NNIN Annual Report

March 2011 – Dec 2011

Cooperative Agreement ECCS-0335765

Prof. Roger T. Howe Prof. Dan Ralph Dr. Lynn Rathbun NNIN Director Principal Investigator NNIN Deputy Director Stanford University Cornell University Cornell University

Participating Institutions: Arizona State University, Cornell University, Georgia Institute of Technology, Harvard University, Howard University, Pennsylvania State University, Stanford University, University of California at Santa Barbara, University of Colorado, University of Michigan, University of Minnesota, University of Texas at Austin, University of Washington, and Washington University in St. Louis

NNIN Annual Report p.1 March 2011-Dec 2011 Table of Contents

Contents 1.0 Introduction to the Report ...... 14 2.0 NNIN Overview ...... 14 2.1 Approach and Usage ...... 15 2.2 Practices for User Support ...... 18 2.2.1 User Facilities ...... 18 2.2.2 NNIN Project Support, Process Support and Training ...... 18 2.3 Overview for 2011 ...... 19 2.3.1 Activities and Usage ...... 19 2.3.2 Facilities Expansion ...... 21 2.3.3 Examples of Scientific Impact from 2010 ...... 22 2.4 Network Management ...... 24 2.5 Network and Site Funding-Year 9 ...... 26 2.6 Network Performance ...... 27 2.6.1 Program Breadth ...... 30 2.6.2 Lab Use(text to be updated) ...... 31 2.6.3 Cumulative Annual Users ...... 32 2.6.4 Average Monthly Users ...... 36 2.6.5 User Fees(text to be updated) ...... 37 2.6.6 Hours per user ...... 43 2.6.7 New Users ...... 44 3.0 NNIN Education and Human Resources Programs ...... 46 3.1 Objectives and Program Challenges ...... 46 3.2 Coordination and Collaboration...... 48 3.2.1 Scope of Program and “Countable” Activities...... 48 3.3 NNIN Major National Programs: REU, iREU and RET ...... 49 3.3.1 REU Program ...... 49 3.3.2 iREU Program ...... 52 3.3.3 iREG-International Research Experience for Graduates ...... 56 3.3.4 RET Program ...... 56 3.3.5 iWSG...... 58 3.4 Other Education Programs ...... 62 3.4.1 Teacher Workshops ...... 62 3.4.2 NanoTeach ...... 63 3.4.3 Other K-12 outreach ...... 64 3.4.4 NanoExpress ...... 65 3.4.5 NNIN Education Portal ...... 65 3.4.6 Nanooze ...... 65 3.5 Technical Workshops--Laboratory Oriented ...... 66 3.6 Symposia and Advanced Topics Workshops ...... 67 3.7 Diversity Related Efforts and Programs ...... 67 3.7.1 Diversity in NNIN REU Program ...... 68 3.7.2 Diversity in NNIN RET Program ...... 68 3.7.3 Showcase for Students: An NNIN Diversity Program ...... 68

NNIN Annual Report p.2 March 2011-Dec 2011 3.7.4 Laboratory Experience for Faculty Program ...... 69 3.8 Assesment and Evaluation ...... 70 3.9 Program Summary ...... 71 4.0 NNIN Computation Program ...... 72 4.1 Codes at the Sites ...... 72 4.2 Hardware Update at Harvard ...... 73 4.3 NNIN/C Impact in Science and Education ...... 73 4.4 Research Highlights ...... 74 4.4.1 Dynamics of Polymers in Flowing Colloidal Suspensions ...... 75

4.4.2 Ambipolar field effect in the ternary topological insulator (BixSb1–x)2Te3 by composition tuning ...... 75 4.4.3 MEMS Capacitive Accelerometer for Health Monitoring Applications ...... 76 4.4.4 Polymeric Nanocarriers for Local and Systemic Delivery of Drugs to the Lungs via Oral Inhalation...... 77 4.4.5 Adaptable Two-Dimension Sliding Windows on NVIDIA GPUs with Runtime Compilation ...... 77 4.4.6 How Easy is it to Tear Graphene? ...... 78 4.4.7 Thermal Transport in InAs Nanowires ...... 78 4.4.8 Towards Organic Energy Storage ...... 79 4.4.9 Graphane Under Pressure...... 79 4.5 Progress on New Computation Initiatives ...... 80 4.5.1 Virtual Vault for Interatomic Potentials ...... 80 4.5.2 Virtual Vault for Pseudopotentials Development ...... 81 4.5.3 GPU Initiative ...... 81 4.6 Collaborative Projects ...... 82 4.6.1 Defence Threat Reduction Agency Grant Award ...... 82 4.6.2 Center for Integrated Nanotechnologies, Sandia National Laboratory ...... 82 4.6.3 Thermal Transport in Crystalline and Disordered Materials ...... 83 4.7 Workshops and Training Activities ...... 83 4.7.1 NNIN/C Role in Training and Courses at NNIN sites ...... 83 4.7.2 Advanced Modeling and Simulation of Micro/Nano Electro Mechanical Systems (MEMS/NEMS) and Nano/Micro-fluidic Devices, University of Michigan: ...... 84 4.7.3 NNIN/C Workshop: ENCON1 Synergy Between Experiment and Computation in Energy – Looking to 2030 ...... 84 4.7.4 EM.CUBE workshop at Michigan ...... 85 4.7.5 Pan-American Advanced Studies Workshop on Computational Material Science for Energy Generation and Conversion ...... 85 4.7.6 Modeling and Simulation of Nano/Microsystems Contest ...... 86 5.0 NNIN GeoSciences Initiative...... 87 5.1 Introduction: ...... 87 5.2 Tasks and Accomplishments ...... 87 5.2.1 Task 1: Outreach to Geo Community ...... 87 5.2.2. Tasks 2 & 3: Initiate Collaborative Projects and Disseminate Information: ...... 88 5.2.3 Task 4: Geosciences User Expansion at NNIN ...... 92 6.0 Society and Ethical Implications of Nanotechnology ...... 93 6.1 Vision and Goals ...... 93 6.2 SEI Activities...... 93

NNIN Annual Report p.3 March 2011-Dec 2011 6.2.1. NNIN SEI REU Participation: ...... 93 6.2.2 NNIN SEI Brochure: ...... 94 6.2.3 SEI Orientation “Train the Trainer” Workshops for NNIN Labs: ...... 94 6.2.4 SEI Orientation Web Module ...... 95 6.2.5 SEI Featured Ethical Column: ...... 95 6.2.6 Additional, Ongoing Activities: ...... 95 6.2.7 SEI Publications and Presentations from NNIN SEI Princpals...... 96 7.0 Site reports ...... 98 7.1 Arizona State University Site Report ...... 98 7.1.1 Site Overview ...... 98 7.1.2 Project Highlights ...... 98 7.1.4 Education & Outreach ...... 99 7.1.5 SEI Training ...... 100 7.1.6 ASU-Selected Site Statistics (2011) ...... 101 7.1.7 ASU User Institutions (2011) ...... 102 7.2 Cornell University NNIN Site Report ...... 103 7.2.1 Overview ...... 103 7.2.2 Users and User Base ...... 103 7.2.3 Technical Highlights ...... 103 7.2.4 Focus Areas/Assigned Responsibilities ...... 106 7.2.5 Equipment and Facilities...... 108 7.2.6 Site Usage and Promotion Activities ...... 109 7.2.7 Education Contributions...... 109 7.2.8 Computation Contributions (CNF/C) ...... 112 7.2.9 Social and Ethical Issues in Nanotechnology ...... 114 7.2.10 Staffing ...... 114 7.2.11 Selected Cornell Site Statistics (2011) ...... 116 7.2.12 Cornell User Institutions (2011) ...... 117 7.3 Georgia Tech Site Report ...... 118 7.3.1 Research Highlights ...... 118 7.3.2 Growth of the Ga Tech NRC Facilities, Equipment and Capabilities ...... 119 7.3.3 Diversity Activities ...... 120 7.3.4 Special Focus/Leadership: Education: ...... 120 7.3.5 Georgia Tech Selected Site Statistics (2011) ...... 123 7.3.6 Georgia Tech User Institutions (2011) ...... 124 7.4 Harvard University Site Report ...... 125 7.4.1 Facility Overview ...... 125 7.4.2 Nanocompuation (NNIN/C) Summary ...... 125 7.4.3 Research Highlights ...... 125 7.4.4 Facility and Operations Highlights ...... 128 7.4.5 Equipment Highlights ...... 128 7.4.6 Staff Highlights ...... 131 7.4.7 Education and Outreach ...... 131 7.4.8 Society and Ethics ...... 134 7.4.9 Selected Harvard Site Statisitcs ...... 135 7.4.10 Harvard Site User Institutions (2011) ...... 136 7.5 Howard University Site ...... 137 7.5.1 Overview ...... 137

NNIN Annual Report p.4 March 2011-Dec 2011 7.5.2 Progress in Attracting New Users: ...... 137 7.5.3 Staff ...... 138 7.5.4 Education ...... 138 7.5.5 New Equipment ...... 140 7.5.6 Nanotechnology Seminar Series ...... 140 7.5.7 Renovations of HNF ...... 141 7.5.8 Research Highlights ...... 141 7.5.9 Howard Site Statistics (2011) ...... 149 7.5.10 Howard User Institutions (2011) ...... 150 7.6 Penn State University Site Report ...... 151 7.6.1 Site Description and Technical Capabilities ...... 151 7.6.2 External and Internal Research Highlights ...... 151 7.6.3 Facilities, Acquisitions, and Operations ...... 152 7.6.4 Education, Outreach and SEI ...... 154 7.6.5 Penn State Selected Statistics (2011) ...... 156 7.6.6 Penn State User Institutions (2011) ...... 157 7.7 Stanford University Site Report ...... 158 7.7.1 Facility Overview ...... 158 7.7.2 Equipment ...... 158 7.7.3 Staffing ...... 159 7.7.4 Research Highlights ...... 159 7.7.5 Educational/Computational/Societal and Ethical Implications of Nanotechnology Highlights...... 161 7.7.6 Selected Stanford Use Statistics (2011) ...... 163 7.7.7 Stanford User Institutions (2011) ...... 164 7.8 University of California Santa Barbara Site Report ...... 165 7.8.1 Site Overview ...... 165 7.8.2 Research Examples ...... 165 7.8.3 Operations and Capital Acquisitions ...... 167 7.8.4 Education, Diversity, and SEI ...... 168 7.8.5. USCB Selected Statistics ...... 170 7.8.6 UCSB User Institutions (2011) ...... 171 7.9 University of Colorado Site Report ...... 172 7.9.1 Summary ...... 172 7.9.2 Technical Focus Areas ...... 172 7.9.3 Research Highlights ...... 172 7.9.4 Operations ...... 173 7.9.5 Diversity oriented initiatives ...... 175 7.9.6 Education oriented contributions ...... 175 7.9.7 Society and ethics oriented activities ...... 176 7.9.8 Selected Univ. of Colorado Site Statistics (2011) ...... 177 7.9.9 University of Colorado User Institutions (2011) ...... 178 7.10 University of Michigan Site Report ...... 179 7.10.1 Technical Focus Area ...... 179 7.10.2 Research Highlights ...... 180 7.10.3 Acquisitions, Changes and Facility Operations ...... 183 7.10.4 Diversity Oriented Contributions ...... 184 7.10.5 Educational ...... 184

NNIN Annual Report p.5 March 2011-Dec 2011 7.10.6 SEI highlights ...... 185 7.10.7 University of Michigan Selected Statistics (2011) ...... 187 7.10.8 University of Michigan User Institutions (2011) ...... 189 7.11 University of Minnesota Site Report ...... 190 7.11.1 Summary of Initiatives and Activities ...... 190 7.11.2 Selected External and Internal Highlights ...... 190 7.11.3 Equipment and Facility Highlights ...... 192 7.11.4 Diversity ...... 193 7.11.5 Education Outreach Efforts Summary: ...... 193 7.11.6 SEI Activities ...... 195 7.11.7 Minnesota Selected Site Statistics (2011) ...... 196 7.11.8 University of Minnesota User Institutions (2011) ...... 198 7.12 University of Texas Site Report ...... 199 7.12.1 Technical leadership areas: Initiatives and Activities ...... 199 7.12.2 Acquisitions, Changes, Operations ...... 200 7.12.3 Diversity Activities ...... 200 7.12.4 Education ...... 200 7.12.5 Social and Ethical Issues (SEI) ...... 201 7.12.6 University of Texas Selected Site Statistics (2011) ...... 203 7.12.7 University of Texas User Institutions (2011) ...... 205 7.13 University of Washington Site Report ...... 206 7.13.1 Overview ...... 206 7.13.2 Aquatic and Geo Sciences News ...... 206 7.13.3 Research Highlights ...... 207 7.13.4 Equipment, Facility and Staff Highlights ...... 208 7.13.5 Educational Highlights ...... 208 7.13.6 SEI Highlights ...... 209 7.13.7 University of Washington Selected Statistics (2011) ...... 210 7.13.8 Univ. of Washington User Institutions (2011) ...... 211 7.14 Washington University in St. Louis Site Report ...... 212 7.14.1 Overview ...... 212 7.14.2 Research Project Highlights ...... 212 7.13.3 Equipment and Operation ...... 214 7.14.4 Staff ...... 216 7.14.5 Education and Other Activities ...... 216 7.14.6 Washington University at St. Louis Selected Site Statistics ...... 218 7.14.7 Washington University at St. Louis User Institutions ...... 219 Appendix 1: NNIN Network and Site Directors and Coordinators ...... 220 Appendix 2: NNIN Highlights 2011 ...... 221 Appendix 3: NNIN Publications (following) ...... 221

NNIN Annual Report p.6 March 2011-Dec 2011 Table of Figures

Figure 1: Map of location of NNIN Sites...... 15 Figure 2: Overview of NNIN operations. Its community, resources and a schematic of approach to service...... 15 Figure 3:: (a) Graphene membranes mounted on a SiN scaffold, (b) grain boundary imaged within a graphene membrane. (scale bar 0.5 nm). (c) color-coded depiction of grain orientations within one graphene membrane. (scale bar 500 nm)...... 22 Figure 4: (a) Schematic of ABEL, a nanofluidic trap that confines a biomolecule at a nanochannel crossing and (b) ABEL snapshots of antenna protein showing conformation changes upon illumination...... 23 Figure 5: (right) Conductance variation with gate voltage Vg for (left) bilayer and (right) trilayer graphene devices at 4.2 K. Upper and lower curves are taken before and after current annealing, respectively. Inset: SEM image of a suspended graphene device (left) Conductance oscillations as a function of inverse magnetic field at

gate Vg = 3, 4, 5, 6,7, 7.5, 8, 8.5, 9, and 9.8 V (bottom to top); the traces are offset for clarity...... 23 Figure 6: (left) Overlay of piezoresponse data on the topology map of a 2 μm2 area for correlation study; (right) (a) vertical and (b) lateral piezoresponse correlation of a 1 μm2 area quantum dot...... 23 Figure 7: Network Management Structure...... 24 Figure 8: Approach to collection of information by the network...... 28 Figure 9: Network User Distribution by Technical Area...... 30 Figure 10: User Lab Hours by NNIN Site. Note different sites count hours in different ways – equipment time where equipment has charges associated with it, or clean room time...... 31 Figure 11: Cumulative Users at each site. (March-Dec) ...... 32 Figure 12: NNIN Outside Users by Site...... 33 Figure 13 NNIN users by site in a multi year comparison...... 34 Figure 14: Network wide research usage by year...... 35 Figure 15: Average Monthly Users...... 36 Figure 16: Average Monthly Outside Users ...... 36 Figure 17: User Fee Recovery by Site and Type for 10 month period of 2011...... 37 Figure 18 NNIN major sources of funding: NSF (NNIN Main Cooperative agreement and ARRA only) and user fees...... 38 Figure 19: Average academic user fees for local and external academic users ...... 39 Figure 20: Average fees for Outside academic users...... 40 Figure 21: Average academic fees per hour at NNIN facilities...... 41 Figure 22: Average Industrial User Fees by Site ...... 42 Figure 23: Average industrial user fees per hour of usage in the 10 month period of 2011. ..42 Figure 24: Laboratory hours per academic user (local and external)...... 43 Figure 25:: Training load for new users (internal and external)...... 44 Figure 26: Ratio of New Users to Cumulative Annual users by site...... 45 Figure 27: NNIN Education Events and Participants...... 47

NNIN Annual Report p.7 March 2011-Dec 2011 Figure 28: REU convocation ...... 50 Figure 29: REU convocation poster session ...... 50 Figure 31: iREU Belgium ...... 53 Figure 30: iREU 2011 Germany ...... 53 Figure 32: iREU Delft ...... 54 Figure 33: iREU France ...... 54 Figure 34: Pictured left to right Yuki Matsuoka and Seiya Suzuki...... 56 Figure 35a: Histograms of scores of participants during the teaching part of IWSG3 ...... 62 Figure 36: Georgia counties and states where GT has reached teachers ...... 63 Figure 37: Nanoexpress at the Boston Museum of Science...... 65 Figure 38: 5 most recent issues of Nanooze ...... 66 Figure 39: "Nanooze Lab" at Disneyland Innoventions, celbrating the International Year of Chemistry ...... 66 Figure 40: Showcase for Students Demonnstration ...... 68 Figure 41: a) Snapshot of a single chain (blue beads) with a cohesive energy ε=2.08 unfolding in a sheared colloidal suspension (red spheres) with Φ=15% and r¬c= 5. (b) Typical extension sequences as a function of time for a collapsed polymer at different colloid volume fractions Φ=0%, 15%, and 30%. The other parameters are

γτ = 2 and rc= 5...... 75 Figure 42: Ab initio band structure calculations of Bi2Te3, (Bi0.75Sb0.25)2Te3, (Bi0.50Sb0.50)2Te3, (Bi0.25Sb0.75)2Te3 and Sb2Te3 show qualitative agreement with ARPES measurements (b, bottom row), with gapless SSB consist of linear dispersions spanning the bulk gap observed in all the compositions. The

difference in EF between calculated and measured band structures reflects the carriers arising from defects and vacancies in the crystals...... 76 Figure 43 :a) A 3-D model of the capacitive comb-drive accelerometer; (b) SEM picture of the fabricated serpentine spring; (c) Profile of maximum deformation of the proof- mass and serpentine springs in z and x direction, respectively ...... 76 Figure 44 a) Structure of PAMAM dendrimers (generation 2 and 3) before and after equilibration – ca. 15 ns. Bottom: Structure of G3 PAMAM dendrimer grafted with different densities of PED1000 ...... 77 Figure 45: A comparison of the average per-frame processing times for the three implementations ...... 77 Figure 46: Phase AFM image show the region before and after an indentation measurement performed near a grain boundary (at location indicated by blue dot). Scale bars: 150 nm ...... 78 Figure 47 MD simulation of the effect of a void on the strength of a small bicrystalline graphene sheet (Panel c). MD simulation of decreased breaking strength due to shearing in the presence of a grain boundary.: ...... 78 Figure 48 Isolating the nanowires for thermal measurements requires multiple fabrication steps to achieve the proper setup. The calculated phonon dispersions for zincblende (ZB) and wurtzite (WZ) nanowires are also shown Experimental data points for ZB InAs are ...... 79 Figure 49: Simulation for energy storage application ...... 79

NNIN Annual Report p.8 March 2011-Dec 2011 Figure 50: Various Graphane structures found during the evolutionary search ...... 80 Figure 51.: Virtual Vault for Interatomic Potentials Schema...... 80 Figure 52: Molecular spectroscopy in nano-environments...... 82 Figure 53: Predicted thermal conductivity in SiGe alloys with embedded Si or Ge nanoparticles based on T-matrix and Born approaches. The thermal conductivity reaches a minimum for nanoparticles with a 10 nm diameter. (A. Kundu et al, Phys. Rev. B, 84. 125426 (2011) ...... 83 Figure 54 :Advanced Modeling and Simulation of Micro/Nano Electro Mechanical Systems and Nano/Micro-fluidic Devices- April 2011 NNIN/C Workshop Attendees at Michigan...... 84 Figure 55: Daniel Nocera describes the “Artificial Leaf” at ENCON1: Synergy Between Experiment and Computation in Energy – Looking to 2030...... 84 Figure 56: NNIN/C@ Michigan EM.CUBE Workshop ...... 85 Figure 58 Modeling and simulation of nano/microsystems contest at Michigan- ...... 86 Figure 57: Participants at the 2012 PASI-CMS4E Workshop ...... 86 Figure 59: NNIN Booth at AGU conference...... 88 Figure 60: Array of Au/Hg working microelectrodes...... 89 Figure 61: Current geosciences and environmental science users (a total of 140 geo users from 8 NNIN sites) by technical category...... 92 Figure 62: Rachel Brockhage (middle row, right) participated as a SEI REU intern at Cornell and Nina Hwanng (top row, center) participated at University of Colorado-Boulder...... 93 Figure 63: NNIN Participates and Helps Sponsor First Congress on Teaching Societal and Ethical Implications of Research ...... 94 Figure 64: NNIN Poster Session at SEI Congress and Business Meeting...... 95 Figure 65: NNIN Participates and Helps Sponsor First Congress on Teaching Societal and Ethical Implications of Research...... 98 Figure 66 Schematic of DNA translocation methodology ...... 98 Figure 67 PDMS channel with inlet and outlet ports on top of one electrode array...... 98 Figure 68: Single photon counting module ...... 99 Figure 69: VP Joe Biden met with innovators in DNA sequencing, including ASU’s Stuart Lindsay (center)...... 99 Figure 70: 4th grade lesson plan ...... 99 Figure 71: ASU Outreach Activity ...... 99 Figure 72: ASU Site Statisics ...... 101 Figure 73: Grain boundries in Graphene (Park, McEuen, Muller) ...... 103 Figure 74: Block co-polymer templates (Wiesner, Thompson, Muller) ...... 104 Figure 75: Microfabricated structure to study cancer cell metastasis and migration (Austin)...... 104 Figure 76: Spin polarization memory element (Kent)...... 105 Figure 77: Ab ignition calculations of charge transfer and excition dissociation in lead salt nanocrystals (Hanrath and Wise) ...... 105 Figure 78: Reconfigurable microfluidic switches (Erickson) ...... 106 Figure 79: Hitachi FIB ...... 108

NNIN Annual Report p.9 March 2011-Dec 2011 Figure 80: Primax uEtch Vapor HF ...... 108 Figure 81: AJA Sputter System ...... 108 Figure 82: Zygo NewView 7300 ...... 109 Figure 83: 2011 CNF REU group ...... 109 Figure 84: Nanooze ...... 110 Figure 85: TCN Short Course ...... 110 Figure 86: Junior FIRST Lego event ...... 112 Figure 87: Rachel Brockhage, SEI REU student ...... 114 Figure 88: CNF Site Statistics ...... 116 Figure 89: Tissue Scaffold (Dean, Uehlin) ...... 118 Figure 90: Nanoplasmonic sensor ...... 118 Figure 91: Micrograph of tumor membranes ...... 119 Figure 92: PDMS microwell arrays ...... 119 Figure 93: GSR Particles ...... 120 Figure 94 Georgia Tech Selected Site Statistics ...... 123 Figure 95: Overview of the pH based actuation mechanism...... 126 Figure 96: (left) Micrograph of highly regular inverse-opal structure; (right) multilevel encryption displaying different letters for different ethanol-water mixtures...... 126 Figure 97: Massachusetts-based Lilliputian Systems power cell. The company has demonstrated mobile device recharging stations based on the technology...... 127 Figure 98: Boston-based FastCAP researchers, and capacitor based battery (inset)...... 127 Figure 99: New Hall measurement system...... 129 Figure 100: New 125 kV e-beam lithography system...... 129 Figure 101: New XeF2 etcher...... 129 Figure 102: Direct-write lithography systems...... 129 Figure 103: Representative atomic resolution data from atom probe system...... 130 Figure 104: Cross-section polisher...... 130 Figure 105: Cambridge 8th grade students learn about nanotechnology through interactive demonstrations...... 131 Figure 106: CNS Microscopist Carolyn Marks leads demonstrations for John D. O’Bryant students...... 131 Figure 107: Tech Savvy participants construct a water drop maze from hydrophobic and hydrophilic materials...... 132 Figure 108: Education Specialist Jorge Pozo leads demonstrations at Salud Y Familia...... 132 Figure 109: Professor Howard Stone gives children instructions for illustrating electric current during the 2011 Holiday Lecture...... 132 Figure 110: Energy Workshop ...... 133 Figure 111 Selected Harvard Site Statistics ...... 135 Figure 112: Harvard User Institutions ...... 136 Figure 113: Auriga CrossBeam Workstation ...... 137 Figure 114: Libra TEM...... 137 Figure 115: Nanotalk on the radio WHUR ...... 139 Figure 116: MOCVD ...... 140 Figure 117: Laser Engraver ...... 140

NNIN Annual Report p.10 March 2011-Dec 2011 Figure 118: Xray diffractometer ...... 140 Figure 119: Renovation of LK Downing Hall at Howard University ...... 141 Figure 120: Howard Selected Site Statistics ...... 149 Figure 121: Columnar ChG thin film deposition system developed at Penn State. Optical and FESEM images of ChG CTF on a fingerprint...... 151 Figure 122 :Left: A chip containing resonant micro-PZT membranes for biosensing. Right: Microfluidic chamber with on-board electronics...... 151 Figure 123: Packaged PZT-based pyroelectric detector array integrated on ROIC along with IR image collected using this device...... 152 Figure 124: Top: FESEM of graphene RF transistors of varying gate lengths. Bottom Bottom: Device data demonstrating 10X improvement in FET frequency response...... 152 Figure 125: Selected Penn State Site Statistics...... 156 Figure 126: Stanford Nanostructures Integration Lab n-SiL ...... 158 Figure 127: The Bosch Group ...... 159 Figure 128: Nanotechnology-enabled Artificial Kidney...... 160 Figure 129: Lateral NEM Switch Technology for Robust, Low-Power Digital Systems...... 160 Figure 130: Volumetric Intracardiac Ultrasound Imaging ...... 160 Figure 131: Electrically Pumped Photonic Crystal Laser ...... 160 Figure 132 3D-FPGA ,:Prof. S. Wong ...... 161 Figure 133 Selected Stanford Site Statistics ...... 163 Figure 134: CWDM Laser Spectrum of 50 Gb/s Hybrid Silicon Photonic Transmitter ...... 166 Figure 135: 50 Gb/s Hybrid Silicon Photonic Transmitter ...... 166 Figure 136:: Device circuit and micrograph of two Josephson phase qubits with a tunable coupler. The two qubits are shown in red and blue in the circuit, and boxes b and c in the lower micrograph ...... 166 Figure 137: Electrode and CNT SEM images ...... 166 Figure 138: Resonance Frequency and conductance measurements versus gate bias...... 167 Figure 139: Selected Site Statistics from UCSB ...... 170 Figure 140: a) Surface profile of the double helix mask design. (b) Measured surface profile of the fabricated phase mask. c) Typical fluorescence image of micro-tubules limited by the classical diffraction-limited criteria. d) A 3D image using a double helix point ...... 173 Figure 141: a) Number of users by year, b) Hours of use by year and c) User research areas for 2011 ...... 174 Figure 142: Selected Colorado Site Statistics ...... 177 Figure 143: SystemAttendees of the Symposium on Advanced Modeling Methods of MEMS/NEMS and Micro/Nanofluidic Devices ...... 180 Figure 144: Left: Uniform nano gold array fabricated by PVD gold onto nano- polystyrene beads coated surface. Right: Preliminary sensor response...... 180 Figure 145- Top: Profile of maximum deformation of the proof-mass and serpentine springs; Bottom: Completed 1.5 mm x 1.5 mm capacitive accelerometers...... 181 Figure 146: Top: Schematic of picowatt calorimeter. Left: Measured temperature oscillations...... 181

NNIN Annual Report p.11 March 2011-Dec 2011 Figure 147: Microfluidic biochip for trapping WBCs. Fluorescent image shows WBCs trapped in the device...... 181 Figure 148: Left: Schematic diagram of the proposed neural probe integrated with waveguides and SEM images of the fabricated probes...... 182 Figure 149: Microfabricated probes for scanning thermal microscopy ...... 182 Figure 150 :Left: MEMS deformable mirror mounted for easy implementation into focus control imaging applications. Right: Topside view of a mirror released in XeF2. 182 Figure 151: Structure of G3 PAMAM dendrimer grafted with different densities of PEG1000...... 182 Figure 152: JBX-6300FS Electron Beam Lithography System ...... 183 Figure 153: SEM and EDS mapping of Si, O, Au, Pb, and C on samples with patterned PZT film...... 183 Figure 154: Olympus BX51 Fluorescent microscope installed on vibration isolation table. ... 183 Figure 155: 2011 Spring Nanocamp ...... 184 Figure 156: SEI Seminar organized for the local community ...... 185 Figure 157: University of Michigan Selected Site Statistics ...... 187 Figure 158: Scematic of DNA sequencing scheme ...... 190 Figure 159 191 Figure 160 191 Figure 161 Post array for study of DNA dynamics ...... 191 Figure 162: Rendering of new Facility ...... 192 Figure 163 University of Minnesota Statistics ...... 196 Figure 164: IntelliJet Drop Pattern Generator in hard disk drive applications by Molecular Imprints Inc...... 199 Figure 165: Perfecta MR5000, Nanoimprint lithography 6025 semiconductor mask replication. Throughput: 4-mask replicas/ h...... 199 Figure 166: Astrowatt high efficiency ultra thin solar cells to be stringing on a 5inch module...... 200 Figure 167: MRC U Texas operations team ...... 200 Figure 168: Science Teacher Association of Texas (STAT), 2011 conference at Dallas ...... 201 Figure 169: 400,000 kilowatt-hours solar energy field at MRC UT Austin ...... 201 Figure 170: University of Texas Site Statistics ...... 203 Figure 171: SEM image and EDS analysis of interplanetary dust...... 206 Figure 172 ERS barcodes of 3 different strains of V. parahaemolyticus ...... 206 Figure 173: AFM image of the protonic field effect transistor developed by Rolandi...... 207 Figure 174: 3D rendering of a ring resonator showing optical mode propagation through a waveguide...... 207 Figure 175: Schematic of two-state model with detachment during assembly and disassembly (rates k3 and k4, respectively), and interconversion between states...... 207 Figure 176:. Devices on CVD-grown graphene show the scalability of the structure (left). The magnified image of a typical device (top right) and a map of the generated photocurrent (bottom right) are shown...... 207 Figure 177: PdS “Los Nanobots” team presenting their project to their mates and the UW- NNIN staff...... 208

NNIN Annual Report p.12 March 2011-Dec 2011 Figure 178 University of Washington Selected Statistics ...... 210 Figure 179: SEM image of the aluminum nanowire optical filters deposited directly on top of the CCD imaging sensor ...... 212 Figure 180: Mechanistic illustration of Fe(II)-induced recrystallization of Ni-substituted hematite...... 213 Figure 181: Prototype magnet system developed by Pulse Therapeutics, Inc. for use with magnetic nanoparticles in the treatment of stroke patients...... 213 Figure 182: Transmission electron micrograph of palladium colloid...... 214 Figure 183: TEM and SEM images of superparamagnetic magnetite nanoparticles...... 214 Figure 184: TEM images of gold nanoplates with 400nm edge length before (left) and after (center) purification and gold nanoplates with edge length of 200nm (right)...... 215 Figure 185: Biomass growth of Arabidopsis seedlings in the presence and absence of silver nanoparticles left). Silver uptake by mature Arabidopsis plants (right)...... 215 Figure 186: Silver nanocubes (left) and their absorbance in solution at different silver concentrations (center). A linear relationship between silver nanocube concentration and absorbance has been demonstrated (right)...... 215 Figure 187: Washington University Selected Site Statistics ...... 218

NNIN Annual Report p.13 March 2011-Dec 2011 1.0 Introduction to the Report This report summarizes the activities and progress over ten months during the 8th year of the operation of the National Nanotechnology Infrastructure Network (NNIN), from March 1, 2011 through Dec. 31, 2011, which is the 3rd year following its five-year renewal in 2009. NNIN is funded via a cooperative agreement between Cornell University and NSF; the current award period extends through Feb. 28, 2014. Some highlights of 2011 include: 1 The three institutions joining NNIN in 2009, Arizona State, Colorado – Boulder, and Washington University, St. Louis, are becoming fully functioning nodes with increasing usage of their nanofabrication facilities, as well through their participation in network-wide activities. The network has seen its usage grow to over 5600 users (10 months), of which 1847 are external academic or industrial users. 2 All of the ARRA-funded fabrication tools purchased in 2010 are installed at sites throughout the network and are providing both new capabilities and higher reliability; 3 Initiatives toward the geo- and ocean science communities are bearing fruit, with new collaborations leading to research in new sensing capabilities. 4 In January 2011, the third International Winter School for Graduate Students was held in India, with U.S. students learning from leading nanotechnology researchers at IISc_Bangalore, followed by a week of educational outreach in rural villages. In January 2012, the 4th International Winter School was held at UNICAP in Brazil. 5 NNIN enabled high-impact research in all subdisciplines of nanotechnology, including nanomaterials and the nano-bio interface. The network has unique strengths – its diverse technical capabilities afforded through the laboratory and technical personnel, its unique user community with technical diversity and unparalleled reach as the largest community of nano-oriented researchers, and the academic strength and geographic reach that it can leverage through its place in the national research and development investments. These newer efforts in education and outreach activities include the development of an international perspective in the U.S. nanotechnology graduate student community, in helping open and explore new science and engineering frontiers through advanced symposia and workshops, and in the development of societal and ethical consciousness through citizenship-building, as well as research studies to assess the implications of nanotechnology, all draw on the reach and the resources of the network This report documents NNIN’s activities and highlights for ten months of 2011. It includes statistics of usage and particularly focuses on progress and activities that NNIN initiated in the renewal term after 2009. Earlier reports have described NNIN functions and operations extensively and these will not be described here in detail.

2.0 NNIN Overview The National Nanotechnology Infrastructure Network (NNIN) is a collective of fourteen university-based facilities with the mission to enable rapid advancements in nanoscale science, technology and engineering through open and efficient access for fabrication. The core mission of the NNIN is to provide a distributed, facilities-based infrastructure resource that is openly accessible to the nation’s students, scientists and engineers from academe, small and large companies, and national laboratories. It enables them to design and fabricate nano-scale structures, devices, and systems for characterizing material properties and device and system performance, through providing access to fabrication tools and processes in leading academic cleanrooms, along with the hands-on training and consultation with

NNIN Annual Report p.14 March 2011-Dec 2011 experts that is essential for success. NNIN’s goal is to bring newcomers to experimental nanotechnology to a point of being able to fabricate on their own, at an affordable cost and with the minimum training period. NNIN also supports its core mission through computational scientists and computing facilities at several of its nodes. These experts in modeling and simulation collaborate with nanoscience and engineering experimentalists to accelerate research in materials science, nanoscale metrology, and device structures. NNIN’s computational infrastructure is open to academic and industrial users from outside the host institutions. We also leverage our extensive infrastructure resources and geographic and institutional diversity to conduct other

activities with broad impact: in education, in enhancing Figure 1: Map of location of NNIN Sites diversity in the technical disciplines, in the societal and ethical implications, and in the health and environmental issues associated with nanotechnology.

2.1 Approach and Usage NNIN’s approach for supporting research and development has been to focus its efforts on serving the external user who is not part of the academic community at the host institution. As a result, we use the resources provided by NSF to support the staff members that train users, assist them with their research and development tasks, and maintain the equipment and process resource. These staff, made possible by the NSF funds, often leveraged by university support. Nanotechnology resources are optimized through the identification of the technical strengths at each of the nodes, which reflect the intellectual strengths of the host institution. When coupled with geographic diversity, this community approach also enables a balanced and broad set of capabilities for the nation’s nanotechnology researchers. The network is focused on providing the infrastructure for nanotechnology research by the external user community: the students and professionals from non-NNIN institutions. In NNIN’s view, infrastructure consists of much more than advanced equipment. While an extensive set of state-of-the- art equipment is a necessary condition, it is not sufficient for the operation of an effective distributed user facility. Key to NNIN’s operation and thus a key part of the “infrastructure” are the committed staff who enable the effective use of the nanotechnology tool set and who have a focus on service to external users. NNIN’s facilities are all committed to this open-access culture and operate as an organization supporting and complementing each other, so that the network can be effective across the breadth of Figure 2: Overview of NNIN operations. Its community, resources and a schematic of approach to service. NNIN Annual Report p.15 March 2011-Dec 2011 nanotechnology’s subdisciplines, as well as geographically. NNIN supports researchers having a wide range of experience, from novice to experts, by sharing with them the breadth of tools, along with a breadth of knowledge on integrated process design and execution, where a large number of material and environmental interactions can occur. Essential to each nanofab’s efficient and productive operation is the training of users on a large variety of equipment, maintaining a high level of equipment uptime, supporting the users by open sharing process knowledge and previous experience, and by keeping the facilities open 24 hours a day. Some projects are simple, requiring only one fabrication step or access to a single advanced instrument; others can be very complex, requiring integration of multiple process steps and the use of novel materials. Openness to new materials is also a key feature on NNIN facilities. Nanotechnology extends to all forms of condensed matter and fabrication technology in order to build structures, devices, and systems. The ability and willingness to process new materials is critical for many emerging applications of nanotechnology, and is particularly critical at this time where problems and research challenges related to energy conversion and storage and the biosciences are expanding the materials being explored in nano-scale science and engineering. A broad array of techniques applicable to a diverse palate of materials is necessary and is made available through NNIN facilities. To support this growing set of materials in shared nanotechnology facilities without cross- contamination occurring requires both thorough training of the user community and a vigilant staff that closely monitors critical tools and processes. Our approach for achieving our objective of effective and efficient project execution by external users is summarized by our commitment to provide: • A true practice of openness at all sites, based on serving external users, • A state-of-the-art equipment resource, distributed across the sites, and supported by a high level of technical staff expertise, • A commitment to technical excellence that focuses on bringing key instrumentation and knowledge and training to users, especially new users, • The effective and leveraged usage of scarce equipment and staff resources, which is made possible by a critical mass of users across the network, • A geographically distributed resource, with distributed technical responsibilities, building upon the research and technology strengths of each site, while serving the broadest community, and • A synergistic set of local and national activities to support education of users, potential users, human resource development, and provide public outreach. Each NNIN site has technical area responsibilities that are tied to the technical area strengths of the institution. NNIN sites, thus, do not provide identical capabilities but do provide a set of common, essential fabrication techniques, complemented by specialized technical area capabilities. We can provide world-leading expertise that is unique to each site, based on its own toolset and history, interests of the local faculty, and resources. The network is a distributed set of laboratories, each with distinctly local flavor, but all work toward a common goal, with a common approach. This shared vision is critical to the operation of the network. To achieve this vision, all sites have committed to the following common principles: • Open and equal access to all projects independent of origin, • Single-minded commitment to serving external users, • Commitment to support interdisciplinary research and emerging areas, • Openness to new materials, techniques, processes, and applications, • Commitment to deepening social and ethical consciousness,

NNIN Annual Report p.16 March 2011-Dec 2011 • Facility control, rather than ownership by individual faculty ownership, of fabrication tools, instruments, and other resources, • Commitment to maintaining high equipment uptime and availability • Commitment to comprehensive training and staff support, • Facility governance dedicated to national networked support, independent of interference from other local organizations at the site, and • Commitment to having no intellectual-property barriers to facility access. These principles are critical to NNIN’s operational success and they distinguish NNIN facilities from other research facilities, which try to support external user access as a secondary rather than a primary mission. This approach also avoids any conflicts of interest that arise in conduct of research when multiple investigators are pursuing similar directions. These principles have served NNIN well and have allowed it to make a major contribution to the nation’s nanotechnology research and development infrastructure. NNIN efficiently utilizes its resources by tying intellectual strengths at a particular host university to leadership responsibilities for serving related disciplines through its site. This strategy assures that state- of-art instruments and advanced knowledge as well as extensive experience are available to external users. The table shows the matrix of leadership and contributory responsibilities of the sites within the network.

Table 1---NNIN sites and technical competencies and leadership areas. L=Leadership, x=assigned technical areas

Scale

Organic Interface

ics, MEMS Optics &

Sciences -

Bio & IntegratedBioSystems & Chem. Molecular& Tech. Electron Bio Life& Sciences Materials Physical & Sciences Computation Geo Support/Tool Res. Man’f Dev Remote Usage Support Inorganic Energy Precision Sciences & Engineering Environment Health & Society Ethics & Education Diversity Outreach Cornell x x L x L L x x L x x L L L x Stanford x x L x L L x x L x x x x L L x Georgia Tech x x L x x x L L Michigan L x x L L x x x x Harvard x L x x L x x x x UCSB x L x x L L Minnesota x x x x L x x Penn State L x x x x x x Texas L x L x x Washington x L L x x x x Howard x x x L ASU x x x L x L WUStL x x L x L Colorado x x L L x L Together, these practices have established NNIN as a model of a distributed, shared laboratory environment that embraces interdisciplinary research and builds upon the nano-science and nanotechnology expertise resident at each of our member sites. This infrastructure support for

NNIN Annual Report p.17 March 2011-Dec 2011 nanotechnology research enables NNIN to play a leading role in the development of the scientists, engineers and high-technology work force of the future. 2.2 Practices for User Support Our practices to support and train users, especially new users, continue to evolve with learning and experience. External user support, training, and procedures are our focus; internal users obviously benefit, because of the efficiencies created. The procedures are not straightforward to implement in a conventional university laboratory environment where multiple conflicting interests co-exist. Through the leadership of NNIN derived from its experience over the past 8 years, and its documented impact on nanotechnology research, both locally and nationally, the NNIN sites have adopted and implemented these methods. This section summarizes the NNIN user-support practices. 2.2.1 User Facilities The facilities of NNIN are resource facilities; i.e., the primary mission of NNIN and its individual sites are to facilitate the research of others. The NNIN sites are specifically not research centers and NNIN is not a research program. This fact distinguishes its operating philosophy from that of other center-based programs, including STCs, ERCs, NSECs, MRSECs, etc., which are primarily research centers. While the facilities of these research centers may be available to some collaborators, they are primarily maintained to support the research mission of the center; furthermore, such research centers rarely have the staff or user support mechanisms in place to assist users from unaffiliated research groups. The NNIN facilities therefore do not have a particular research thrust or a portfolio of research thrusts. NNIN does not fund research at the site by resident faculty or staff, with the exception of its society and ethics program. Similarly, NNIN does not directly fund user projects from outside users. The NNIN’s goal of providing a national nanotechnology infrastructure resource is accomplished by providing equipment, processes, staff support, and instruction to all feasible projects at each of the fourteen nodes. The user base thus defines the direction of their research in NNIN; we thus avoid the conflicts that arise between conducting research and supporting research. At most of the host universities, there are resident research programs — NSECs, MRSECs, STCs, ERCs, etc., as well as non-NSF centers — which use the facilities heavily and provide critical knowledge and information. These programs, related “research centers”, and their associated students provide much of the technology base, process development, and process characterization at each site, which is critical to the success of diverse user projects. A prime tenet of NNIN is, however, that all users are equal and the facility is equally open to all. NNIN sites are expected to separate research tasks from the user facility tasks so that even researchers from competing research programs have fair and equal access to all site technologies. The NNIN facility staff is distinct from any associated research staff. This separation is a cornerstone of NNIN operation and distinguishes the NNIN from other organizations. NNIN also removes intellectual property concerns by placing the responsibility for protecting confidential information on the user. External users are expected not to share information that they wish to protect for patents or as trade secrets. Being academic facilities, within the academic community – both internal and external – NNIN fosters an environment of sharing so that researchers can be productive in uncovering new knowledge, rather than duplicating results known to other practitioners. 2.2.2 NNIN Project Support, Process Support and Training NNIN facilities are primarily hands-on facilities. Users are trained by the staff to become self-sufficient. However, NNIN also serves users remotely, without the user needing to visit a site. Remote access to NNIN typically involves execution of a selection of reproducible and specialized processes and process sequences that are essential to a variety of tasks, but aren’t themselves the focus of the research. Examples of these processes are fabrication of thin low-stress membranes, selective etches, deep silicon etches, thin-film coatings, and fine-line lithography, etc.). These processes can be performed for a remote

NNIN Annual Report p.18 March 2011-Dec 2011 user by an NNIN-supported staff member. The NNIN, however, does not operate as a foundry for complex integration of materials and processes. The execution of a complex multi-step process sequence is itself a research project and must be performed by the user. Most users, from academia or industry, are performing research and development and wish to be part of the hands-on process of research, in order to learn from the staff, and become self-sufficient researchers. Each site is responsible for providing sufficient staff resources to enable comprehensive training and support for external research projects. Currently, NNIN trains approximately 2000 new users per year, with almost 6000 different users taking advantage of NNIN laboratory facilities each full year. Safety training, including a component devoted to the development of societal and ethical consciousness, is mandated for all users prior to any activity in the laboratory. Each external user project is assigned to a staff mentor who is the primary contact for technical support. Instruction in all phases of nanotechnology is provided as necessary in addition to direct equipment instruction. The NNIN staff act only as facilitators; the technical and intellectual direction of each project remains with the user. As projects progress, users become more independent of NNIN staff support, many to the point of being self-sufficient. NNIN staff remains available, however, to provide support as necessary. Accommodating large numbers of new users arriving weekly and training them to operate safely and creatively in a shared-facility environment is the most critical aspect of network operation. With a high level of training and process support delivered by a dedicated professional staff, complex technologies such as e-beam lithography and complex multi-step integrated processing procedures can be made available to a large user community in an efficient and timely manner. At the same time, new techniques and processes, developed either by the staff or by the user community, can be efficiently and effectively made available for the mutual benefit of all users, at the site, and across the network. 2.3 Overview for 2011 The past year was the third year following NNIN’s renewal in 2009. The three new sites, Arizona State, Colorado – Boulder, and Washington University, St. Louis, have become thriving nodes with increasing usage of their nanofabrication facilities, as well through their participation in network-wide activities. While the rest of this report will explain the past year’s activities and accomplishments more detail, some of the salient milestones of the diverse network activities included: 2.3.1 Activities and Usage Note: since this report covers the 10 month period March 2011-Dec.2011, most usage numbers are quoted on a 10 month basis. Updated full annual data will be provided at the annual review a. Network usage: The network usage is increasing in the high single digit rate per year and over the 2011 10 month period, 5646 users directly employed the resources of NNIN. The usage is broadly distributed across disciplines. During this 10 month period 1909 new users were trained in the use of a large instrument set. Average costs incurred by academic users, who came from 188 universities, was approximately $3200 for the 10 month period. This cost continues to be an affordable sum for research projects. Over 350 small companies and 89 large companies, with over 885 industrial scientists, are using the facilities for their research and development efforts. The graduate student community of 4600 users of NNIN reflects between 15 and 25% of experimental science and engineering student community that potentially needs the type of resources NNIN provides. NNIN, through its 14 advanced nanotechnology facilities and associated staff, continues to make a significant impact on both the academic community and on the economic development front. b. Research and development impact: The network’s contributions are reflected in over 3100 publications that appeared over a year-long period and collected in July, 2010. Highlights of the

NNIN Annual Report p.19 March 2011-Dec 2011 research and development span the breadth of intellectual interests. Examples include fundamental measurements such as of single phonons, persistent currents in normal metals, attonewton measurements of dielectric fluctuations, mechanical control of spin states in single molecules, single photon sources for quantum explorations; biological applications such as use of single-walled nanotubes for DNA sequencing, use of nanoporous membranes for hemofiltration; energy applications such as self-pumping and self-breathing fuel cells, thin crystalline as well as nanowire solar cells and information technology-related applications, such as MEMS based mobile projectors, and new forms of phase transition memories. c. Advanced Scientific Computation and Modeling: In excess of 100 advanced research users working at the limits of discipline and at interdisciplinary boundaries are employing the knowledge of the NNIN computation staff and the one-of-kind academic software available from NNIN. Their effort is reflected in 27 publications in leading journals – Nature Chemistry, Nano and Physical Review Letters, etc. The cumulative impact of NNIN computation effort since its start in 2004 is reflected in about 11 citations per publication over 120 publications, with an h index of 22. A user, Zoe Boekelheide, graduate student at UC Berkeley, won the 2011 Group on Magnetism and Magnetic Materials (GMAG) Dissertation Award sponsored by the American Physical Society for her work on the effects of nanoscale structure on magnetic and transport properties of chromium and chromium-aluminum alloys. The virtual vault, a trusted repository of critically important but difficult to obtain scientific information, now includes over twelve different pseudopotential databases, ten pseudopotential generators, four pseudopotential generators, and links to key references on pseudopotentials. d. Education and outreach: The portfolio of NNIN’s activity encompasses a wide spectrum of age groups and technical knowledge. Through its diverse events, NNIN reached nearly 34000 individuals (in person) during the 2010 year. i. Symposia and Workshops: NNIN organized four major symposia during 2011, where leading practitioner and visionaries assemble for talks and discussions of challenges and in defining future directions. They included: Materials and Manufacturing for Energy and Electronics, held at UT Austin and co-organized with Penn State, NNIN Symposium on Frontiers in Nanoscale Transistors and Electronics held at UCSB, Bio-inspired Engineering, held at Harvard, and Synergy Between Experiment and Computation in Energy – Looking to 2030, a symposium organized at Harvard as part of the NNIN/C computational nanotechnology effort. In addition, NNIN organized numerous workshops with technical education objectives. ii. Nanooze is a children’s magazine, a website resource, and a hands-on museum-quality exhibit for elementary to middle-school age children. Ten issues of the print edition are now available and nearly 100,000 copies of each issue are distributed by direct mailing upon request. In October 2011, Nanooze Labs, a 1500 sq ft interactive museum display, opened at Disneyland in Anaheim, CA, celebrating the International Year of Chemistry. It will be seen by hundreds of thousands of visitors during its one year engagement. iii. REU (Research Experience for Undergraduates), a hands-on nanotechnology research experience across the breadth of disciplines had 85 participants across the network. iv. iREU (international Research Experience for Undergraduates) provides an advanced research experience for exceptional students selected out of our prior year’s REU program. This program gives them not only a more advanced exposure to nanotechnology research, but also provides them with experience in an international

NNIN Annual Report p.20 March 2011-Dec 2011 context, helping them develop as globally aware scientists. The 2011 program consisted of 15 students at partner laboratories in France, Germany, Belgium, and the Netherlands. v. iWSG (international Winter School for Graduate Students), a technical and global awareness activity in which a technically advanced emerged area is taught internationally together with a society and ethics component with exposure to technological limitations and successes in the third world environment. The January 2011 edition was taught at IISC Bangalore by five US faculty on the subject of nanofabrication. Thirteen nationally selected graduate students participated, together with more than 100 students from across India. vi. iREG (international Research Experience for Graduates), a reciprocal program of partnership with NIMS brought 5 Japanese graduate students and were hosted at NNIN laboratories for a summer research experience. Georgia Tech, University of Michigan and University of Texas participated in this year’s program. The costs of the travel, housing, and stipend for the participating students are borne entirely by NIMS. vii. LEF (Laboratory Experience for Faculty), a summer REU-like program for underrepresented faculty or faculty at under-represented serving institutions had 6 participants hosted at Georgia Tech, Stanford, Michigan, Minnesota, and Texas (2). This program helps the faculty establish viable research programs and provides a nanotechnology experience, which can be incorporated into their classroom environment. viii. Nanotechnology Showcase is a day-long event consisting of lectures and hands on experience activities designed for increasing awareness among underrepresented undergraduates. NNIN held a Showcase at Society of Hispanic Professional Engineers Annual Conference in Anaheim in October reaching more than 200 undergraduate students. e. Societal and ethical implications of nanotechnology: Our SEI effort participated in the training of over 1900 new users through discussions, presentations, and training modules, reaching the community of new NNIN users. Details of these accomplishments, as well as other NNIN activities, are given in subsequent sections of this report and in some cases in the individual site reports. 2.3.2 Facilities Expansion In August, Penn State’s new nanofabrication facility, housed in the Millenium Science Complex, was dedicated. The University of Minnesota’s new Physics and Nanotechnology Building began construction in October. Finally, a $6.6M renovation and expansion of the Stanford Nanofabrication Facility (SNF) began in December, of which $4.2M was provided by an NSF ARI-R2 grant. This project will create a separate laboratory, adjacent to the SNF and accessible to NNIN, for bringing synthetic nanostructures into the mainstream of nanofabrication. Since 2004, ten major facilities expansions or constructions have taken place at NNIN sites. In total, eight entirely new facilities (Cornell, UCSB, Harvard, Michigan, Washington University at St. Louis, and University of Colorado, Georgia Tech, Penn State) and extensive renovations represent an investment by universities and state governments of over $600M. The affiliation with NNIN is an important force in justification of these expenditures by state and universities, since sustainable operations of the resources becomes possible through the critical mass of users that come via NNIN participation. NNIN is a key factor in the business model that makes these facilities affordable. While these expenditures are made to enhance the local university’s capabilities and stature, NNIN and its users receive enormous benefit from these significant investments in infrastructure.

NNIN Annual Report p.21 March 2011-Dec 2011 2.3.3 Examples of Scientific Impact from 2010 Over 2500 publications reported research results enabled by NNIN in 2011, which span across the breadth of the engineering, physical, and life science disciplines. In many of these publications, external users were able to exercise the capabilities of NNIN to fabricate materials, structures, devices, or systems that advanced the state of nano-science and engineering. A publication list over the period July 2010 – June 2011 is available as supplementary material to this annual report. The papers range from fundamental measurements of nano-scale phenemena to molecular and supra-molecular scale structures that demonstrate new nanofabrication technologies or nano-device designs to applications in many fields of science and engineering. Several examples, selected from nearly 300 research highlights at the fourteen NNIN nodes, demonstrate the breadth of NNIN’s impact on nanoscale science and engineering. These particular examples show outstanding research that advances understanding of the fundamental material structures and physical properties of matter at the nanoscale. A recent paper by Profs. Jiwoong Park, Paul McKuen and David Muller and co-authors from Cornell demonstrates that grain boundaries in single-layer graphene can be imaged in a TEM, if the graphene is mounted on a SiN scaffold. The patchwork quilt of poly-crystalline graphene is pictured in the false-color image. In addition, they were able to perform nano-indentation as well as imaging using an AFM on graphene suspended over a shallow cavity formed by patterning thin films of oxide and gold on silicon. The grain boundaries were found to degrade the mechanical properties of graphene significantly, in contrast to their minimal impact on graphene’s electrical properties.

Figure 3:: (a) Graphene membranes mounted on a SiN scaffold, (b) grain boundary imaged within a graphene membrane. (scale bar 0.5 nm). (c) color-coded depiction of grain orientations within one graphene membrane. (scale bar 500 nm).

Prof. William Moerner’s group at Stanford has recently developed an active nanofluidic technique to trap individual biomolecules. The device is called an anti-brownian electrokinetic trap (ABEL) and utilizes the active control of the electrokinetic flows in a nanochannel intersection, using position information from the fast optical imaging of a fluorescent group on the molecule. ABEL has been used to study the photophysics of single antenna proteins in photosynthesis, revealing heterogeneity that has not been observed in coarser imaging techniques.

NNIN Annual Report p.22 March 2011-Dec 2011 Figure 4: (a) Schematic of ABEL, a nanofluidic trap that confines a biomolecule at a nano-channel crossing and (b) ABEL snapshots of antenna protein showing conformation changes upon illumination.

Prof. Wenzhong Bao from UC Riverside measured magnetoconductance oscillations in suspended bi- and trilayer graphene, the fabrication of which made use of the UC Santa Barbara NNIN node. The conductance minima are observed at all integer filling factors between 0 and 8, as well as a small plateau at 1/3. The trilayer graphene device shows persistent conductance features, which could suggest the onset of symmetry breaking of the first few Landau levels and fractional quantum Hall states.

Figure 5: (right) Conductance variation with gate voltage Vg for (left) bilayer and (right) trilayer graphene devices at 4.2 K. Upper and lower curves are taken before and after current annealing, respectively. Inset: SEM image of a suspended graphene device (left) Conductance oscillations as a function of inverse magnetic field at gate Vg = 3, 4, 5, 6,7, 7.5, 8, 8.5, 9, and 9.8 V (bottom to top); the traces are offset for clarity.

P. Phillips of the University of Michigan has used piezoresponse force microscopy (PFM) to image InGaN quantum dots fabricated in the Lurie Nanofabrication Facility, Michigan’s NNIN site. This technique can provide a quantitative measure of the large lattice mismatch between InN and GaN and its effect on the on the optoelectronic properties of the quantum dot.

Figure 6: (left) Overlay of piezoresponse data on the topology map of a 2 μm2 area for correlation study; (right) (a) vertical and (b) lateral piezoresponse correlation of a 1 μm2 area quantum dot.

NNIN Annual Report p.23 March 2011-Dec 2011 2.4 Network Management As a large group of university-based laboratories in a very diverse technical area encompassing nearly all the areas of science and engineering serving a user community spanning academia, industry and national laboratories, and a multifaceted outreach mission, a cohesive, responsive and stream-lined management is essential for the NNIN to achieve its network goals and for the standards for operation and support of users to be maintained. Management is responsible for coordination of intra-network activities and for various levels of reporting to NSF, NNI, and others. The management structure of NNIN also has to take into account the large number of network university sites, the individuality of universities and their environment and yet has to be flexible, responsive and adaptive to the evolving environment of nanotechnology research. Our management structure and procedures follow the format outlined in the NNIN proposal.

Network Director Network Executive Network Advisory Board Committee

NNIN Deputy Director

Site Directors Education & Outreach Coordinator

Computing Coordinator

Society & Ethics Coordinator

Figure 7: Network Management Structure.

In October 2011, Prof. Sandip Tiwari, Cornell, stepped down as Director of NNIN, a postion he had held since the inception of NNIN. Prof. Roger Howe of Stanford assumed the position of NNIN Director. Other than the change of Director, all other management functions remained at Cornell. Since the NNIN Cooperative Agreement is between Cornell and NSF, a Cornell Faculty member must be PI on the award, for financial accountability reasons. Upon consultation with NSF, Prof. Dan Ralph assumed the role of PI, with Roger Howe as co-PI. Functionally, however, Prof. Howe is Director of NNIN, and all financial and management functions remain at Cornell, under Dr. Lynn Rathbun, NNIN Deputy Director. Figure 5 shows the broad outline of the organizational structure. Prof. Roger Howe, the NNIN Network Director and Co-Principal Investigator, is the point of contact with NSF, and is responsible for implementing the network policies and program in conjunction with the co-PI, Prof. Dan Ralph of Cornell. Dr. Lynn Rathbun, Cornell University, serves as Deputy Director and coordinates the daily activities and communication with network sites. Four Network Coordinators are responsible for the broad outreach activities areas across the network. • Education & Outreach: Dr. Nancy Healy, Georgia Tech, • Society & Ethical Implications in Nanotechnology: Prof. Katherine McComas, Cornell,

NNIN Annual Report p.24 March 2011-Dec 2011 • Computation and Modeling: Dr. Mike Stopa, Harvard, and For the purpose of implementation of the program and policies, the Network Director and the Program Manager interact directly and regularly with the site directors and the coordinators of thrust activities. The Site Directors are responsible for the operation of individual sites. A complete list of Site Directors is provided in Appendix. The network management hosts a conference call with the Site Directors as a group at least once every two months. The Network Executive Committee (NEC), chaired by the Network Director, sets the vision, policies, operating procedures, evolution, and manages the allocation of the NNIN resources. NEC has 3 permanent members — the Network Director and the site directors at Cornell and Stanford — and 3 members elected from the other sites. The Network Coordinators also participate in the Network Executive Committee discussions. The NEC meets monthly by conference call, or more often, if necessary. For 2011, the Network Executive Committee consisted of • Prof. Roger Howe (Stanford University), ex-officio • Prof. Dan Ralph (Cornell University), ex-officio • Prof. Khalil Najafi (University of Michigan, term expires 2013) • Prof. Steve Campbell (University of Minnesota, term expires 2012) • Prof. Mark Rodwell (UCSB, term expires 2012) In Feb, 2012, Prof. Theresa Mayer (PSU) and Prof Bart van Zeghbroeck (Colorado) were elected to replace Prof. Campbell and Prof. Rodwell. The Network Director and the Network Executive Committee receive advice from the Network Advisory Board (NAB), an independent body of leaders and thinkers of the disciplines and communities that the network serves. The NNIN advisory board represents eminent scientists, engineers, and administrators. The advisory board members are a cross-section representative of the nanotechnology user areas and are individuals with stature, experience and independence that can help the network evolve through critical advice and guidance of programs, activities, vision and future directions. The members of the Network Advisory Board are:

Dr. Samuel Bader; Assoc. Div. Director, Materials Science Division, Argonne National Lab Dr. Carl Kukkonen; CEO, ViaSpace Technologies Prof. George Langford; Dean of College of Arts and Sciences, Syracuse University Dr. Jim McGroddy; Retired Senior VP, Research, IBM Prof. Hans Mooij; Chairman, Kavli Institute of Nanoscience, Delft Univ. of Technology Prof. Paul Peercy; Dean of Engineering, U. Wisconsin Dr. Kurt Petersen; Entrepreneur and consultant Dr. Tom Theis; Director of Physical Sciences, IBM Research Prof. Vivian Weil; Director, Center for the Study of Ethics in the Professions, Illinois Institute of Technology, Chicago

The advisory board met in New York City in April 2011 and is consulted by phone and group email by the NNIN Director for advice at critical times.

NNIN Annual Report p.25 March 2011-Dec 2011 2.5 Network and Site Funding-Year 9 NNIN is funded by a primary cooperative agreement between NSF and Cornell University at the level of $17.0 M/yr for years 6-10. Almost all of these funds are distributed to sites for local programs, mostly for laboratory support. Some funds are retained at the NNIN office for network management. Other funds are retained at the NNIN office for network wide programs. Those program funds are either spent directly from the management office on programs or distributed to sites as supplements to execute national programs at the local sites. As we enter year 9, it has become clear that more funds have been retained in the management budget than have been necessary. As a result, the year 9 allocation for management has been reduced; Necessary management functions will be funded by carry forward from prior years. Funds which would have been allocated to management functions have been redistributed into the site budgets on a uniform basis, an increase of $72,000 at each site. All centrally managed programs will continue with adequate funds to support them. On a percentage basis, this choice favors the smaller sites where the increase in funds will have the most impact. At this time, this is expected to be a one time adjustment; Placing this adjustment in year 9 will allow the funds to be spent in a manner that will have maximum user impact before the end of the award in 2014. The budget distribution by site is outlined in Table 2.

Table 2 NNIN Annual Funding by Prior Baseline Budget Year 9 Budget Request Site Cornell $2,675,000 $2,747,000 Stanford $2,675,000 $2,747,000 Georgia Tech $1,590,000 $1,662,000 Michigan $1,275,000 $1,347,000 UCSB $875,000 $ 947,000 Harvard $825,000 $ 897,000 U. Minnesota $775,000 $847,000 Penn State $750,000 $822,000 U. Washington $725,000 $797,000 U. Texas $700,000 $772,000 Howard Univ. $550,000 $622,000 Arizona State $500,000 $572,000 U. Colorado $500,000 $572,000 Wash. Univ. in St. Louis $500,000 $572,000 Network Coordination $372,855 $ 0 Network Activities and Programs $1,712,145 $1,077,000 (central)

Total $17,000,000 $17,000,000 The NNIN Activities budget is for network-scale activities, including participant support for various programs (REU, iREU, LEF, iWSG, Showcases), network booths at outreach activities and professional meetings, support of Symposia and Workshops, Advisory Board and Annual Meeting, etc. Much of this budget is sub-awarded to sites annually, amounts in addition to those shown above as the”baseline”. The mix of activities funded under this budget changes annually based on new initiatives and feedback on existing programs and initiatives. Retaining these funds at the network level, at least initially, gives maximum flexibility in meeting the changing program needs. A more complete explanation of funding and program allocation is given in the Budget Justificaiton for

NNIN Annual Report p.26 March 2011-Dec 2011 year 9 funding supplied to NSF. 2.6 Network Performance For NNIN to deliver the greatest possible value to the national user community and the nation, it is essential that the network be a dynamic organization that rewards performance and systematically adapts to changing circumstances and emerging opportunities. During formation of NNIN, we committed to making funding allocations yearly based on productivity metrics and on the basis of leadership contributions in research service in areas of assigned responsibilities and the other NNIN thrust areas. A balanced evaluation requires understanding of responsiveness to user needs, the quantity and quality of output from the individual sites, the needs of different types of usage, and the changing requirements of new and rapidly developing fields. Sites are expected to allocate resources in accordance with the assigned focus areas and are held specifically accountable for success in those areas. We distinguish experimental R&D usage, i.e. research usage, from educational usage that is in support of our broader outcome objectives. Research usage is in support of a specific research task, supported by research funds whose end result are publications for academic users, or new technology and commercialization-oriented development for the industrial users, and new knowledge for both. Educational and other broader area usage has as its goals training or knowledge dissemination. Technical workshops that we conduct, e.g., are in educational usage. On the other hand, an external user, who comes to facilities, gets trained and uses resources to accomplish his or her own technical tasks, is a research user when we count in our user statistics for experimental support. We also collect statistics related to Scientific Computation and Modeling activities separately because of the different nature and needs of this activity. Evaluating performance in this context is a complex task since it must balance between the nature of the activity and its requirements and needs and an appropriate evaluation of the contribution. Research user support and educational user support require different resources and scientific computation users also require a very different type of attention and support. Similarly, within research user support activity, different tasks may require different levels of time and intensity of commitment from staff as well as of the level of complexity of instrumentation. Thus, data needs to be looked at in a variety of ways in order to assess the performance. In addition to quantitative measures, a qualitative evaluation of the enabled research also sets a different context of performance evaluation. Impact of the activity is also critical, and hence quality and quantity of research contribution enabled by site activities, particularly in the area of site focus, is an important consideration in performance evaluation. NNIN focuses on collecting information that helps with forming a balanced and relatively complete picture of the network operation. For research quality, this includes collection of highlights of research and development, related publications and presentations, the impact of the scientific research, as well as quantitative measures that look at research and educational user service. A list of publications resulting from network efforts during a one-year period is attached to this report together with research highlights. The different components of the NNIN mission – research-user services, computation and web-based services, education and outreach, and the societal and ethical thrust – each require separate measures to evaluate productivity, quality of contributions, and user satisfaction. The quantitative data shown in the following sections primarily relates to support of the user research mission. NNIN sites also vary considerably in size and scope of effort related to NNIN. Consequently, the level of funding and the resultant expectations vary accordingly with the following guidelines:

• The range and volume of service that each site can, now and in the near future, provide to outside research users in specific technical areas assigned to it;

NNIN Annual Report p.27 March 2011-Dec 2011 • The infrastructure needs of the technical focus areas that are supported by each site; • The infrastructure needs for the educational efforts and educational user activities, activities that are different in character than research support activities; • The level of responsibilities and range of activities that each site undertakes with regard to the NNIN education and outreach thrust, the computing and web-infrastructure thrust, and the societal and ethical issues thrust. In the following, we summarize the performance of the network and the sites. Figure 8 shows some of the major elements of the information collection. Since each user and each site is different, none of the metrics tells a complete story in itself. In particular, aspects of the quality of the research or the quality of the customer service are not captured well by any of the quantitative metrics. It is also acknowledged that the scope and type of use varies significantly from site to site, and that some types of users/fields have significantly different use profiles (e.g. a simple characterization or thin film deposition user vs. a user doing complex process integration for a MEMS or electronic device). The information summarized here is for experimental research lab usage only. These are related to the projects where a user is trained and performs independent research, uses the variety instruments in the laboratory, and is the primary focus of the network research support activity. These data therefore do not include any educational “user”, people who attended workshops, and other significant activities, or local students taking using any resources for class-room learning, etc. These statistics do not include Computation and Modeling Users; although a significant number require close work with our Computation Domain Experts, and doing in theory what we also do in experiments, they are evaluated separately as this activity is distinct and available only at four sites currently.

Figure 8: Approach to collection of information by the network.

Data collection from network sites for usage, demand, type of usage, and impact. Our focus is on the external user support from the facilities.

Primary Metrics Primary Metric Data submitted • External usage • Cumulative Users by Sites monthly • Average Monthly Users • Lab Time • User Fees • Publications • Highlights • … Broken Down By

Secondary Metrics • All Users Computed from primary metrics • Outside Users • External hours/user • Outside Academic Users • User fees per user • Technical Area • Fees per hour • Site • Area resource requirements • Combinations of above No single “best” indicator

NNIN Annual Report p.28 March 2011-Dec 2011 Primary usage data are submitted monthly by each site to NNIN management. All graphs are subject to the accuracy of the data supplied by the sites. Unless otherwise noted, all data is for the ten-month period from March 2011-Dec. 2011. Data will be updated after March 1, 2012 to reflect the full year. Persons exclusively using NNIN Computation resources for scientific simulations are not counted as part of the NNIN Users. We collect that data separately. As used here, “users” refers to laboratory users only.

NNIN Annual Report p.29 March 2011-Dec 2011 2.6.1 Program Breadth NNIN’s mission in support of experimental nanotechnology spans the entire range of nanotechnology disciplines and applications, from complex fabrication of structures such as in MEMS, biosciences, optics and electronics, to synthesized molecular scale structures and creation of materials assemblies for advanced studies. Figure 6 shows the distribution of users by field (10 months, cumulative users) across the network. Overlap between technical areas is inevitable and many users could be assigned to multiple categories. None the less, the broad coverage of nanotechnology subareas is apparent. Materials is a broad category when specific engineering application is not intended; it is the largest in usage and users from Chemistry, Physics and Materials Sciences are usually pursuing projects in this category. GeoSciences is an area where usage is increasing with outreach effort on our part and increasing interest and recognition in the ocean and environmental sensors community. NNIN continues to place an effort in building up usage in this area. Our focus is on leveraging sensors and microsystems knowledge to help the scientists and engineers in water and environment research communities .

Figure 9: Network User Distribution by Technical Area. Network User Distribution 10 months ( March 2011-Dec 2011) 1400 Cumulative Users: Unique Users since March 1, 1200 Each user counts once. Count resets each March. Actual active research users only 1000

800

Users 600

400

200

NNIN Annual Report p.30 March 2011-Dec 2011 2.6.2 Lab Use(text to be updated) Laboratory hours are counted by one of two means at NNIN sites; either direct use equipment time, or clean room time. The former does not include lab use for non-charged equipment or other general lab time but does count multiple simultaneous equipment use. The latter counts just time in the lab, which could be used for a single piece of equipment, or multiples or none. Thus, while there is correlation between the two measures, they are different in between sites. We accept this variation in counting methods as part of the uncertainty, and have not standardized to one approach because of the expense and time involved and questions that will still remain – sites have numerous essential equipment that incur no charge while a clean room in itself provides ability to access a large number of tools simultaneously. However, laboratory hours are an important way to track intensity of laboratory activity at each site and across the network.

Figure 10: User Lab Hours by NNIN Site. Note different sites count hours in different ways – equipment time where equipment has charges associated with it, or clean room time.

120,000 Lab Hours by NNIN Site and User Type 10 months March 2011-Dec 2011

100,000 foreign state and fed gov large company small company 80,000 pre-college 2 year college 4 year college other university 60,000 local site academic Hours

40,000

20,000

The chart in Figure 10 represents total lab hours during the ten-month period (Mar. 2011 - Dec. 2011). The size of each NNIN facility and its associated funding varies significantly and each includes different amounts of “associated” facilities (e.g., characterization facilities [large materials characterization resources are not included in NNIN]). Nonetheless, they reveal information about the size, scope and character of each laboratory’s activities when looked at together with user numbers and their antecedents in academic (local or external) and industrial research. The activity at all laboratories is dominated by local usage. The local users are a vital foundation and critical element of the facilities. The local users develop the processes, provide quite often the initial impetus for new technology development, and provide the rigor and reproducibility that becomes the knowledge and training foundation for the external user.

NNIN Annual Report p.31 March 2011-Dec 2011 2.6.3 Cumulative Annual Users Cumulative Annual Users is a primary user counting metric employed by NNIN; this is often just referred to as “users”. This is each unique experimental research user counted once during the time period, using March as the starting time for every yearly cycle. This number monotonically increases during the year, reaching the maximum at 12 months (at the end of February of NNIN funding calendar) when the counter is reset for the next year. This measures the number of different people that the site has served; a user who visits once counts the same as one who visits many times over the year. Figure 11 shows the distribution of users across the network by site and institution type. This figure can also be contrasted with the chart for laboratory hours (either laboratory time or equipment time) (Figure 10). There is considerable variation in the number of users and in their distribution between sites, and this should be considered together with the technical focus responsibility area at the specific site. In this metric, each user counts the same regardless of whether he/she uses the facility 4 hours per year or 400 hours per year. To gain a fuller picture of the effectiveness of each site one has to look at other metrics, such as intensity of usage, as a supplement to this information.

Figure 11: Cumulative Users at each site. (March-Dec)

Cumulative Users (2011 10 months) by site 1200 foreign state and fed gov 1000 large company small company pre-college 800 2 year college 4 year college other university 600 local site academic

Cumulative Users Cumulative 400

200

As discussed in the introduction, NNIN’s effort is organized around the theme of serving the external user – a focus we believe leads to crucial benefits in quality, efficiency, and local community and external community effects that are essential to bringing the maximum benefits to progress in nanotechnology from an infrastructure. External users are the most important component of the NNIN effort together with the focus on external users in assigned areas of technical responsibility within the network. This enables effective use of limited

NNIN Annual Report p.32 March 2011-Dec 2011 funds with the maximum efficiency in equipment usage and delivery and sharing of critical technical knowledge and expertise. Figure 12 show the distribution of outside (external) users only, i.e. local site users have been removed for clarity. Nearly all sites continue to make progress towards the objectives. Six major sites of the network (Cornell, Stanford, UCSB, Michigan, Georgia Tech, and Harvard) all have 140 or more outside users each in the 10 month period, with both academic and industrial users benefiting from the network.

Figure 12: NNIN Outside Users by Site.

Cumulative OUTSIDE Users (2011 10 months) by site 450 foreign 400 state and fed gov large company 350 small company pre-college 300 2 year college

250 4 year college other university 200

Cumulative Users Cumulative 150

100

NNIN Annual Report p.33 March 2011-Dec 2011

Building up usage at a site is a multiyear enterprise based on network and site outreach and user successes that reinforce confidence in the site’s capabilities. Particularly for the new or smaller sites, it takes considerable time to grow effective and sustainable usage and vibrant user base. The new sites to the network are the ones with the smaller usage and it is important to also view the progress in network usage since the inception of NNIN in 2004. Figure 13 shows the trends in usage of the network at the sites. In this figure, the data for current year is for a 10 month period. Many of the larger, older sites, are operating at or near saturation, given current resources. This user number is also tied to the type of needs, its usage needs in equipment and in staff, and the intensity, i.e. hours of usage per user.

Figure 13 NNIN users by site in a multi year comparison. NNIN "Annual" User Trends 1200 12 month 2004 12 month 2005 1000 12 month 2006 12 month 2007 12 month 2008 800 12 month 2009 12 month 2010 10 month 2011 600

400

200

NNIN Annual Report p.34 March 2011-Dec 2011

Figure 14 shows total network usage (Users) in each of the 8 years of NNIN- broken down by user type, i.e. local and external academic, and industrial. Data for 2011 are only for 10 months. It shows a continuing increase in network usage across all types over the 8 year history of the network. . For the full 12 months it should be over 6000 users.

Figure 14: Network wide research usage by year.

Network Users Each Year by Type 6000

5000

4000

12 months 10 months 3000 foreign state and fed gov 12 months 12 months 12 months 12 months 12 months 12 months large company 2000 small company

Cumulative Users per year pre-college 2 year college 1000 4 year college other university local site academic 0 2004 2005 2006 2007 2008 2009 2010 2011 (10 months)

NNIN Annual Report p.35 March 2011-Dec 2011 2.6.4 Average Monthly Users Usage needs to be looked at from a variety of perspectives as remarked earlier. The metric of average monthly users, i.e., number of unique users each month, e.g., is indicative of “how busy” a site is (Figure 15). The larger NNIN sites also show a larger number of average monthly users. Figure 16 shows this demand from external users, the user populace that NNIN places its emphasis on.

Figure 15: Average Monthly Users. 500 Average Monthly Users -10 months-2011 450 foreign 400 state and fed gov large company 350 small company pre-college 300 2 year college 4 year college 250 other university local site academic 200

150

100

Figure 16: Average Monthly Outside Users 180 Average Monthly Outside Users -10 months-2011

160 foreign

state and fed gov 140 large company 120 small company pre-college 100 2 year college 4 year college

80 other university

NNIN Annual Report p.36 March 2011-Dec 2011 2.6.5 User Fees(text to be updated) Lab use fees supplement the NNIN funding at all sites. Of course, all users, both internal and external, pay user fees. Fees are charged on per user or per hour basis with the exact structure varying by site. The user fee rates at each site are set at local discretion following the federal and university regulations for cost centers. Some of the NNIN site programs are connected to existing and sometimes larger facilities and programs. As such, no attempt has been made to standardize fees across the network since cost structures are different at different locales. NNIN only expects that external academic users receive the same rate as local academic users, and that NSF funds be allocated to support open academic usage. Thus, industrial users pay the full cost of usage, while the academic users benefit from lower costs that the NSF support makes possible. In short, academic fees cover the incremental costs of operation while the industrial users are charged at higher rates to reflect full cost recovery and reflecting effort that does not compete with commercial enterprises. User fees provide a mechanism for allocating costs to different activities. The NNIN mission is to make

Figure 17: User Fee Recovery by Site and Type for 10 month period of 2011.

$4,500,000 User Fee Recovery (10 months 2011) $4,000,000

$3,500,000 foreign state and fed gov $3,000,000 large company small company $2,500,000 pre-college 2 year college

Dollars $2,000,000 4 year college other university $1,500,000 local site academic

$1,000,000

$500,000

successful research and development happen through open and effective usage of these facilities by the national user community. NNIN funds largely pay for the staff and training infrastructure required to support this outside user effort and not for operation of existing facilities. The level of expense recovery obviously varies with the size of the user base as well as the type of user, e.g. industrial users are an important source; examination of total fee recovery yields little new information. The amount of user fees collected at each site is shown in Figure 17 (10 months). There can be several explanations for low fee recovery from outside users, among them: a) low number of outside users, and b) low average level of use by outside users. At least four sites, however, show that company usage is an important component of achieving their sustainability. In particular, it points to the large relative small company fee recovery at UCSB. In almost all cases, overall user fee recovery is an important part of facility operation budgets.

NNIN Annual Report p.37 March 2011-Dec 2011

Figure 18 shows the overall high leverage of the NSF investment over the years. Each dollar of the NSF cooperative agreement is more than matched by user fees. Both user fees and the NSF support are critical to operation of NNIN. Note this charge does not reflect university or state funding to the sites. This can be significant, particularly in the case of university-funded buildings and equipment. Neither does it include any federal awards directly to the sites, such as from MRI awards.

Figure 18 NNIN major sources of funding: NSF (NNIN Main Cooperative agreement and ARRA only) and user fees. Historical NSF Funding and User Fee Income--Entire Network NSF Coop ARRA Local Academic Other Academic Industrial and Gov $30,000,000 Annual---except 2011 user fees (10 months)

$25,000,000

$20,000,000

$15,000,000

$10,000,000

$5,000,000

$0 2004 2005 2006 2007 2008 2009 2010 2011

NNIN Annual Report p.38 March 2011-Dec 2011 One of the requirements of a successful user facility/network is that it be affordable. This is particularly critical for academic research where the effort is paid largely by various government grants. Because of the economies of scale and the critical mass of users, NNIN is able to keep academic use charges low. Figure 19 compares the local academic (NNIN institution) and outside academic average user fees per user over the ten-month period (total academic fees/ total # of academic users). Note the difference here is not in the rates ($/hour fees), but in the intensity of use. All academic users are charged the same rates. In general, local academic users tend to be more intensive users than outside academic users.

Figure 19: Average academic user fees for local and external academic users $Fees per Academic User ( 10 months) March 2011-Dec 2011

$6,000 inside/user $ 3,268 average per 10 months (March-Dec 2011) outside academic /user across all academic users $5,000

$4,000 month periodmonth 10 $3,000

$2,000

$1,000 Lab feesduring

NNIN Annual Report p.39 March 2011-Dec 2011 Figure 20 shows a subset of the same date, the average user fees per user for just outside academic users. By NNIN mandate, local users and outside users pay the same rates for use; the variation from the total for all academic users reflects different levels and types of usage and intensity of that usage. While there is some variation between sites, the most striking part is that the average external academic user paid approximately $2100 during the 10 month reporting period, a level that is quite affordable for access to an extremely large set of research enabling tools. This is an average; many heavy users paid significantly more, and many light to moderate users paid significantly less. Figure 19 and 20 together also show that the usage recovery from internal academic user is about twice that of external academic user, and for sites an important component of their sustainability.

Figure 20: Average fees for Outside academic users. $4,500 $ Fees per Outside ACADEMIC User (10 months 2011) $4,000 Stanford Minnesota $3,500 UCSB G Tech U.Wash. $3,000 U. Michigan ASU Cornell $2,500 $2,144 network average (10 months) PSU Howard Texas $2,000 Harvard WUSTL $1,500 Colorado

$1,000

$500

NNIN Annual Report p.40 March 2011-Dec 2011 Similarly, average fees per hour (Figure 21) are clustered around $30 per hour, a quite reasonable and accessible fee for high technology equipment.

Figure 21: Average academic fees per hour at NNIN facilities. Academic Fees per Hour (10 month) March 2011-Dec 2011 $140

$120 *ASU: includes significant proportion of "remote/foundry" processing done by staff

$100 inside/hr outside/hr $80 $30 per hour average

$60

$40

$20

The point of these figures is not any individual variation, either between sites, or between local and outside users at a given site; there is far too much variation in complexity of projects and the available equipment sets to draw those conclusions (although actually most use falls in the $20-40 per hour range, a quite tight and reasonable result). One should thus not conclude that one site’s fees are too high or too low from this data – a larger fraction of usage of expensive tools, electron beam lithography or deep ultra violet lithography – can skew these data. Similarly any difference between “average rates” between inside and outside at a given site are due to differences in use profile (type of equipment) and not due to differences in actual rates. In addition, there are certainly individual users who are at both 4x the average and 1/4 the average making for a broad distribution. It does show, however, that access to NNIN facilities for an “average” user is quite affordable. The full out average over all sites for all academic users at around $3000 is quite within the budget of most research grants.

NNIN Annual Report p.41 March 2011-Dec 2011 In contrast, the average cost for an industrial users (small and large company) is $8608 for the 2011 ten- month period (Figure 22) or approximately $85 per hour (Figure 23), again with a broad distribution both within sites and across sites, but extremely manageable for the complex resources that the NNIN sites provide to the industrial users. Again, the equipment use profile varies significantly across the sites

Figure 22: Average Industrial User Fees by Site $20,000 $ Fees per Industrial User- 10 months (March 2011-Dec 2011) $18,000

$16,000 SNF UMN UCSB $14,000 GT UW $12,000 Umich ASU CNF $10,000 $8608 Average Cost (10 months) PSU Howard $ Fees $ Texas $8,000 Harvard WUSTL $6,000 Colorado

$4,000

$2,000

resulting in some of the intra-site variation. The major point is that equipment resources are affordable and accessible.

Figure 23: Average industrial user fees per hour of usage in the 10 month period of 2011. $200 Average Industrial User Fees per Hour ( 10 months 2011) $180 $85/hr Average Industrial rate (10 months) $160 Stanford Minnesota UCSB $140 G Tech U.Wash. $120 U. Michigan ASU Cornell $100 PSU Howard $80 Texas Harvard WUSTL $60 Colorado

$40 $per hour (industrial)

$20

For outside users we do not believe that the relative costs of NNIN facilities are a major factor in selection of a facility. Technical capabilities of the sites, technical alignment with the users requirements, and geographical considerations are significantly more important considerations.

NNIN Annual Report p.42 March 2011-Dec 2011 2.6.6 Hours per user Hours per user is a particularly enlightening metric as it reflects intensity of use, with the caveat that different sites collect data on hours of specific equipment usage) or clean room time. A site can more easily sustain a large number of users doing small processes than a similar number of users doing complex processing. Hours per user is an average secondary metric, gathered by dividing lab hours in a particular category by the cumulative annual users in that category. Average usages of 100’s of hours per user would indicate a facility with more complex processing and a concomitant larger impact upon the facility and its resources. A hundred hour of usage is more than a couple of weeks of dedicated effort by the user. Average usages of <25 hours indicate a group of users who place a significantly smaller burden on the facility. That use may still in fact be critical to a given project but it requires fewer resources to support incrementally. Results across the network, for both internal and external academic users, are shown in Figure 24. It is obvious that there is considerable difference between sites in the intensity of use by an “average” user. Note, in some cases, this derived metric is the ratio of two small numbers and thus the metric is less enlightening for sites with a small number of users. In most cases, intensity of use by internal users is higher than for external users, reflecting the higher availability for routine and unplanned use.

Figure 24: Laboratory hours per academic user (local and external).

Hours per Academic User - 10 months- March 2011-Dec 2011 300 Hours per Inside(academic) user Hours per Outside academic user 250

Average 108 hours per academic user (both types) ( 10 months) 200 Note: some sites report equipment hours, others report lab hours

150

100

NNIN Annual Report p.43 March 2011-Dec 2011 2.6.7 New Users Each facility is constantly accepting new users. This is part of the trend of growth and of turnover as projects succeed and graduate. New users require training, hand holding at least initially, and intense staff commitment during the initial periods of visit and start up. The number of new users is thus an excellent metric for measuring the demand for NNIN resources. Here (Figure 25) we show the number of new users trained in FY2010 by site. Note that some sites average 3-6 new users (inside + outside) per week, a load involving a significant amount of user training and associated staff support.

Figure 25:: Training load for new users (internal and external). New Users 10 months (March 2011-Dec 1011) 200

180 Inside Outside 160

140

120

100

In addition, there needs to be a balance between new users and total users. Figure 26 shows the ratio of new users to total users in FY2011 at each site. A ratio that is too low could indicate a stagnant facility with little growth or replenishment. A high ratio hand could indicate a rapidly growing facility. On the other hand, a ratio too high could also indicate an excessive turnover often associated with short-term, low impact projects.

NNIN Annual Report p.44 March 2011-Dec 2011

Figure 26: Ratio of New Users to Cumulative Annual users by site. Ratio of New Users to Total Cumulative Annual Users ( 10 months 2011) 0.7 Inside 0.6 Outside

0.5

0.4

0.3

0.2

0.1

NNIN Annual Report p.45 March 2011-Dec 2011 3.0 NNIN Education and Human Resources Programs

3.1 Objectives and Program Challenges In completing its eighth year of operation, the NNIN Education and Outreach (NNIN E&O) program continues to offer and strengthen numerous activities at the local, network, and national level. NNIN has as its goals a wide variety of educational outreach that spans the spectrum of K-gray, i.e. school aged children through adult professionals. NNIN has established the following goals for its network-based educational outreach and human resource development: • Educate a dynamic workforce • Support the spreading of the benefits of nanoscale science and engineering (NSE) to new disciplines where it has meaningful impact • Be a resource for all ages and educational background o K-12 o Undergraduates o Graduate students o Post-docs, faculty, government/industry o General population From these overarching goals, specific programmatic objectives have been established that impact national or local efforts. These include: • developing and distributing activities to encourage K-12 students to enter science and engineering fields; • developing resources to inform the public about NSE; • developing activities and information for undergraduates regarding careers in nanoscience; • developing tools and resources for undergraduates and graduate students that focus on teaching and learning and research; • designing programs to ensure the inclusion of underrepresented groups; • developing programs for technical workforce development; and • developing programs and resources for K-12 teachers This report provides updates on our accomplishments and current programs that are both local and national in focus. To attain each of the NNIN’s education objectives, a variety of innovative activities has been defined, developed, and implemented. NNIN E&O components include network-wide programs to address needs at the national scale and more specific efforts for communities that are local to network sites. Table 3 illustrates the type of programs offered by NNIN and the scope across the network. The various facets of the NNIN E&O program are reviewed in following sections of this report.

NNIN Annual Report p.46 March 2011-Dec 2011 Table 3. Local and National NNIN education activities and program. Site Specific Activities Network-wide Activities Local Scope Local Activities – Site Specific Network Activities - Local Scope Facility tours User support & training Community days Diversity Open house K-12 education- school programs Seminars/Public lectures Summer & after school camps School programs K-12 2 and 4 year colleges National Scope Site Activities - National Scope Network Activities - National Scope Workshops National Conferences & Meetings Technical Training Research Experience for Undergrads Teacher Training Research Experience for Teachers K-12 instructional materials (NSF award) Hands-on demos & experiments NNIN Education portal Undergraduate education User support Lab Experience for Faculty (LEF) Diversity Nanooze Open Textbook

Figure 24 summarizes events that NNIN has conducted yearly since 2005 and reported through our web- based recording system (Education Events Manager). The graphs demonstrate how the program continues to maintain a high level of activity since we began collecting data on events in 2005. Figure 24 also shows that we maintain our capacity in the number of events offered across the network sites. In 2011, we directly reached more than 25,000 individuals. This number does not indlcude the NNIN education portal (http://www.education.nnin.org), the nanooze web site, the print version on Nanooze (~100,000), nor the Nanooze the Exhibit at Epcot and Disneyland.

Figure 27: NNIN Education Events and Participants NNIN as a networked resource has geographic reach and technical strengths that are derived from the diversity of subject strengths and facility strengths, and within our universities the strengths arising from the collective of faculty and students. This national and diverse scope is unparalleled and not reproducible in any other center-based programs. NNIN has chosen to place an emphasis on deriving

NNIN Annual Report p.47 March 2011-Dec 2011 maximum impact from the strength of these resources. Our efforts use an approximate guide of 2/3 of our effort devoted to national outreach and impact and 1/3 on local/state outreach and impact. 3.2 Coordination and Collaboration The challenges of any large-scale activity center on coordination and communication. Each NNIN site has a full-time or part-time education coordinator. The NNIN site education coordinators have established a communications network which effectively allows us to refine our work plans, establish short and long- range plans, and ensure continuous communication and collaboration among the sites. The network coordination of NNIN E&O occurs from the Georgia Institute of Technology and Dr. Nancy Healy serves as the NNIN Education Program coordinator. She is assisted at the site by Joyce Palmer Allen and Katie Hutchison (position vacant since 11/1/11). Communication methods include phone, e-mail, and face-to- face meetings.Large education programs are coordinated in cooperation with the NNIN Deputy Director (Dr. Lynn Rathbun) and assistants at Cornell. The education site coordinators meet once a year at one of the NNIN sites for a minimum of two days. The NNIN E&O program has reached a point where sharing of ideas, approaches, and materials is a regular practice among the sites and often occurs outside our scheduled meetings. During the past year, the coordinators met at the University of Minnesota September 28-29, 2011. Minutes of all meetings are available. Coordinators also meet informally at various professional meetings/conferences and the Research Experience for Undergraduates convocation. An additional challenge is keeping accurate records of our activities and resources. Because of the wide variety of activities across the sites, it is important to know the types of activities, the duration, the impact in terms of numbers served, etc. In 2005, NNIN launched the Education Events Manager (EEM), a web-based electronic database for tracking activities and participatns. All sites are required to regularly update the system by posting their events and activities. Tracking of events is done by Georgia Tech and Cornell which can monitor entries and use the system to generate reports. 3.2.1 Scope of Program and “Countable” Activities In a large distributed program like NNIN, consistently counting activities and even determining what activities to include as part of the NNIN program is a major task. NNIN is fairly strict about determining what is and what is not part of NNIN Education Program activities. All of our campuses have multiple nanotechnology programs supported by other funds. While synergies and collaboration are good, double counting is not. We want to be sure that those activities that NNIN reports and the sites report are actually activities for which NNIN is responsible for and for which NNIN contributes signficant resources. We do this without taking credit for activities which are supported by other centers. To be counted as part of NNIN, activities must user include signficant NNIN staff effort and use significant other NNIN resources (funds, equipment, facilities, modules, activites). We specifically exclude activities and programs supported by or organized by separately funded centers unless there is signficant NNIN involvement. For example, we count our own REU and RET participants, but the REU programs and REU participants from other centers are not part of the NNIN Education activity, they are merely users. Similarly, we do not include any activites in support of the normal education program of our own institutions (.e.g laboratory courses, course development, tours for acadmeic classes, etc); Not that those are not important, but rather they would occur independent of NNIN and thus do not really represent an NNIN impact. Neither do we include any equipment instruction, orientation, safety training; those are considered part of the normal research endeavor. Likewise department colloquia and symposia are not counted. Our EEM system allows management to filter out any such activities that are reported. While NNIN certainly makes some contribution to these other activities and takes advantage of synergies, we believe our program is extensive and intensive enough that including these peripheral activities in our reports does no one any good.

NNIN Annual Report p.48 March 2011-Dec 2011 3.3 NNIN Major National Programs: REU, iREU and RET 3.3.1 REU Program The NNIN has developed, operated, and managed a highly successful Research Experience for Undergraduates (REU) Program in nanotechnology since 1997 (begun under National Nanofabrication Users Network (NNUN)). This program is a coordinated network activity which has ~80-90 students participating each summer across 14 NNIN sites.This program is entirely funded out of NNIN Cooperative agreement funds; We do not have support from the NSF REU program. In 2011, the NNIN management budget allocated funds to sites to assure a minimum of 5 students were hosted at each of the 14 sites, for a total of 85 interns. The technical diversity of our laboratories allows us to offer a program covering the broad range of nanotechnology fields, from biology and chemistry to electrical and mechanical engineering. Our program offers a well-supervised independent research project for a 10 week summer period. While individual sites are responsible for daily project supervision, there is strong network coordination to assure a uniform program with high expectations. Our program features a central on-line application process for the entire network program as well as specific program expectations for projects, interns, project directors, and mentors. The NNIN REU draws top quality participants from a diverse applicant pool. Due to the visibility and size of our program, we have been successful in recruiting a large number of women, minorities, and students from non-research institutions (non-doctoral granting). Our program remains a popular choice among students with completed 814 applications received in 2011. We have been committed to providing research opportunities to students who have the most to gain from the NNIN REU experience - 75% of the 2007, 69% of the 2008, 65% of the 2009, 48% of the 2010, and 58% of the 2011 participants had no prior orgainzed summer research experience (REU type internships). Table 4 shows the demographic make-up of applicants, participants, and their type of home institution for 2009, 2010, and 2011.

Table 4. 2009-2011 NNIN REU Program Demographics

# of applicants Applicant Pool # Participants Appl. Success Participation (%) Rate ‘09 ‘10 ‘11 ‘09 ‘10 ‘11 ‘09 ‘10 ‘09 ‘10 ‘11 ‘09 ‘10 ‘11 Overall 625 756 814 74 80 86 12% 11% 11% Gender* Women 213 245 289 34% 33% 36% 40 37 43 19% 15% 15% 54% 46% 51% Men 412 505 525 66% 67% 64% 34 43 42 9% 9% 8% 46% 54% 49% Race/Ethnici ty Minorities** 103 128 168 19% 19% 21% 14 13 24 13% 10% 14% 19% 18% 28% Non- 446 550 646 81% 81% 79% 59 61 62 13% 11% 10% 81% 82% 72% Minorities** Inst. Type*** Ph.D. Level 406 506 549 65% 67% 67% 52 57 63 13% 11% 11% 70% 71% 74% Master’s 114 101 119 18% 14% 15% 10 15 11 9% 15% 9% 14% 19% 13% Level Bacc. Level 85 119 115 14% 16% 14% 11 8 9 13% 7% 8% 15% 10% 11% Assoc. Level 18 24 29 3% 3% 4% 1 0 2 5% 0% 7% 1% 0% 2% * Not all report gender; * *Race/Ethnicity is only for students who reported this information. +Carnegie Ratings: The Carnegie Foundation ratings of high education institutions are used as the measure of institutional size diversity. Some Ph.D. institutions may not offer advanced degrees in the sciences and engineering.

NNIN Annual Report p.49 March 2011-Dec 2011 Of particular interest is the high number of female participants in the last three years. Women are participating at a much higher rate compared to their number of applicants. The breadth of our program helps us meet these goals; there are considerably more women in biology and biomedical engineering than in some of the more traditional engineering fields. Minority student participation increased in 2011 after two years of level participation rates in 2009 and 2010, which reflects the applicant pool. This is a return to results seen prior to 2009, which had a higher participation rate than the applicant pool of underrepresented students. The REU program is funded from the central NNIN activities budget, with supplemental fund transfers to sites to cover the per student costs at a rate of $7,500 participant support per student. Sites can have as few as 5 or as many as 10 participants. The NNIN REU program culminates with the NNIN REU Convocation which is a “mini” scientific conference attended by all site coordinators and REU interns (Fig. 28). The 2011 convocation was held August 10-13, 2011 Figure 28: REU convocation at Georgia Institute of Technology. At the convocation, each student presents his/her research results to fellow NNIN REU participants and NNIN staff. Students do both oral and poster presentations (Fig. 29), which assist them in developing their presentation skills. For many of our students, this is their first scientific presentation. We simultaneously webcast these presentations which allows faculty, graduate student mentors, and staff from the sites, as well as any other interested viewers, to view the convocation. To complete the program, all students write a research report that is published as the NNIN REU Research Accomplishments. The archived webcasts and the Accomplishments are online at http://www.nnin.org/nnin_reu.html. Each year we survey our interns as part of our program evaluation. We consistently receive very high ratings for our program including the quality of research, support by faculty and graduate student mentors, and technical training and support (among others). Table 5 highlights the technical components of our 2011 program. Comparison of 2011 results to previous years indicates consistency of the scores. Analysis of past results shows that the scores vary by approximatley +.20 which clearly demonstrates that the sites adhere to program expectations and offer a high quality program from year to year.

Figure 29: REU convocation poster session

NNIN Annual Report p.50 March 2011-Dec 2011 Table 5. NNIN REU Participant post-program survey. NNIN Post Survey 2011 Question Avg. Question Avg. Did the program offer you a substantial 4.2* How well did the program provide you 4.3 independent research project with a strong with an understanding of the graduate intellectual focus? research life? Were you able to execute the research project 4.2 How well did the program provide you 4.1 using the available equipment and facilities? with an understanding of careers in nanotechnology? Did you consider your project a "good" project- 4.0 Did the program assist you in making 4.2 interesting, right scale, right complexity, etc. future educational & career choices? Were you reasonably able to complete the 3.7 How likely is it that you will choose a 3.5 project? career in nanotechnology? Were you satisfied with how much you were 3.7 How likely is it that you will go to 4.3 able to complete, given the time constraints? graduate school in science/engineering? Did you receive significant scientific interaction 3.8 Did the program assist you in developing 4.0 with the faculty member/ senior staff in charge presentation and writing skills? of your project? Were you included in group meetings and 4.3 Was the Convocation a worthwhile 4.5 seminars? experience? Did the program provide you with experience 4.4 Would you recommend the program to a 4.7 that allowed you to see the breadth of friend? nanotechnology applications? How well did the program assist you in learning 4.4 How likely is it that when you return to 4.6 to use advanced equipment and processes in your home campus that you will share nanotechnology? your experiences with fellow students and faculty? How well did the program assist you in 4.1 How do you rate the overall quality of the 4.5 understanding the scientific basis of program? nanotechnology equipment & processes?

How well did the program provide you with an 3.8 Did you think that your experience with 4.4 exposure to the social and ethical issues related the program was positive? Would you do to nanotechnology, and research in general? it again?

* Likert Scale 1-5; 1 = poor/no 5= superior/very yes

Since its inception in 1997, the NNIN REU program has had nearly Table 6. Academic/Career paths 1,000 participants. As noted above, the program began under the NNIN REU Longitudinal Study NNUN and expanded to twelve sites with the inception of the NNIN, Degree/Career 1997-2007 and to 14 following renewal in 2009. The NNIN REU is a long-term Doctorate 50% investment in human resource development. The career plans of the Master’s 24% participatns play out only five or more after participation, particularly Baccalaureate 13% for those who persue a graduate degree research path. In 2006, we M.D./J.D./MBA 13% began a longitudinal study to determine the educational and career path of interns who participated in the early (pre-2003) years of the program; since then, that window has been gradually expanded to include all participants between 1997- 2007, encompassing all past participatns who are more than 4 years out of the program. This is an ongoing, labor-intensive study which has significance for not only the NNIN REU program but to other undergraduate research-experience programs, as well. We have chosen this time period because participants will have graduated from their home institutions and will have entered or completed additional education and/or entered into the workforce. Of the 597

NNIN Annual Report p.51 March 2011-Dec 2011 participants from 1997-2007, 386 (65%) have completed the online survey. Locating part participants is sometimes a challenge, but we have had reasonable success at it and we are careful to gather sufficient information from current participants to facilitate future contact. Academic and career results are shown in Table 6. Ninety-five percent of the respondents have remained in science and engineering with approximatley 50% reporting their current position involves nanotechnology (broadly defined). The results presented in Table 6 have shown little variabilit,y as the number of responses has increased from the initial sample of ~200. While we continue to look for more respondants, we do not expect the general conclusions to vary significantly with additional data. 3.3.2 iREU Program Each summer, the NNIN REU program described above provides the introductory research experience for approximately 80 students described above. The training and experience these students receive is excellent and they are highly sought by employers, graduate schools, and other internship programs. While they almost all perform well, from observations over the summer it is clear that 15-25% are very high quality students and have an exceptional ability and commitment to research These are destined to be future research leaders; with the right experience, we believe they can become research leaders in nanotechnology. In 2008, we established the NNIN international REU (iREU) to further the nanotechnology experience of these exceptional individuals. NNIN established this program because we believe that globally aware scientists and engineers should be a priority in the 21st century. In this program, selected students are offered a “2nd summer” REU-like experience in the laboratories of one of our international partners, generally a National Laboratory in Europe or Japan. This program is only open to our prior year REU students – we are effectively using our REU program as a “filter” to select only the very best students for this enhanced research experience, as determined by their activity during the REU experience. Our traditional partners for this program have been the National Institute for Materials Science in Tsukuba, Japan and the Forshungszentrum Julich in Germany. We have supplemental funding from the NSF International Research Experience for Students program (IRES) for five participants at NIMS in Japan. NNIN management program funds support the other iREU participants. The students spend approximately 11 weeks at the international laboratories working on more advanced nanotechnogy research projects.. NNIN provides travel, stipend, housing, and a food allowance. This program is slightly more expensive than REU ( ~$11,000 per participant) but all the laboratory and project supervision costs are borne by our international partners. We have completed 4 summers of this program; our international partners have been well pleased with the arrangement and have been eagar to maintain and even expand the partnership. Students are selected and assigned to projects in January. The March 2011 earthquake and resulting tsunami in Japan significantly modified our plans for 2011; upon consulation with our partners and with NSF, we suspended the program in Japan for 2011, repositioning the selected students to other sites. In April 2011 we quickly added two additional European sites to our already established two European sites and added extra projects at other sites to accommodate the students who we had selected for Japan. In the end, our partners for 2011 were the Forshungsentrum Jülich (FZJ) (a Helmholz Research Institute) in Germany, IMEC in Belgium, TU Delft in The Netherlands, and Ecole Nationale Supérieure des Mines de Saint Etienne in France. We express great appreciation for our partners at each of these sites who stepped up on short notice to host students who had been scheduled to go to Japan. These 4 sites hosted a total of 16 participants--7, 4, 3, and 2 students, respectively (Figure 25 - 28).

NNIN Annual Report p.52 March 2011-Dec 2011

Participants in 2011 included: Germany • Zachary Connell, University of Nebraska • Brian Benton, University of Minnesota • Kevin Chen, Arizona State • Steven Chase, Rose-Hulman Institute • Brian Chung, UC Santa Barbara • Clara Chow, U. of Wisconsin Madison • Mark Brunson, San Fransisco State

Figure 30: iREU 2011 Germany

Belgium • Joseph Smalley, Pennsylvania State University • Emily Hoffman, Case Western • Diana Wu,MIT • Sibu Kiruvilla, University of Illinois

Figure 31: iREU Belgium

NNIN Annual Report p.53 March 2011-Dec 2011 The Netherlands • Margeaux Wallace, Cornell University • Evan Mirts, Truman State University • Lauren Cantley, Grinnell University

Figure 32: iREU Delft

France • Fiona O’Connell, Loyola University • Michelle Pillers, Southern Methodist Univ

Figure 33: iREU France

“I absolutely loved the iREU experience, and I would gladly be a participant again! I recommend it to anyone and everyone who has even minimal interest in research, as research today is a completely international entity. Thank you for the opportunity!.”, Sibu Kiruvilla 2011 iREU Belgium “I loved everything about this program. A most sincere thanks to the entire NNIN REU staff for providing me with this opportunity to travel the world for nanotechnology research! It's a journey I will certainly never forget.” Brian Chung 2011 iREU Germany

Despite the last minute rearrangement of projects due to the disaster in Japan, all the students had sucessful research experiences. Their research is reported along with our REU project reports in the NNIN REU Research Accomplishements (www.nnin.org/nnin_reu.html). We will be returning to Japan in

NNIN Annual Report p.54 March 2011-Dec 2011 the summer of 2012. This program provides an excellent career growth opportunity for the participants. iREU interns have indicated that their prior NNIN REU experience allowed them to meet the challenges of a more advanced project, work in a different research environment, and live and work with colleagues from another culture. Consistent with the goals of the program, the participants indicated that they would pursue other international programs in their future education and career paths, something that would likely not have happened otherwise. We will watch how this plays as their careers develop. The iREU also established important international linkages for the NNIN with our “sister organizations” if Europe and Japan.. Of the 52 participants in the 4 years of this program, 26 are in graduate school and 13 are still undergraduates; the remainder are employed but some of them intend to return to graduate school The 26 in graduate school include 5 NSF fellows, a testament to the high quality of the participants and the boost that participation in this program offers. We will continue to track the career paths of these students. In 2011, we undertook a follow-up survey of all of the participants with 46 of the 52 responding. Table 7 summarizes the results of the iREU follow-up survey. The results clearly demonstrate the positive impact this program has on the partcipants.

Table 7. Post iREU Survey 2011 (4 years of participants)

Question Avg.

My REU experience was important in securing my current position (grad school, work) or in 4.5 successfully performing in current position

The program helped me feel confident to work in an international setting 4.8

The program helped me feel confident to work with international colleagues 4.8

The program helped me develop relationsips with international researchers and colleagues 4.6

The program helped me understand the global nature of science and engineering 4.6

The program helped me to develop an interest in working internationally 4.5

I consider my participation to have a positive influence on my future educational or career 4.9 choices

The porgram helped me to develop a global perspective regarding research and society 4.8

* Likert Scale 1-5; 1 = poor/no 5= superior/very yes

NNIN Annual Report p.55 March 2011-Dec 2011 3.3.3 iREG-International Research Experience for Graduates As an integral part of our relationship with NIMS Japan for hosting our iREU program, NNIN hosts a number of graduate students from Nanonet, the Japanese equivalent of NNIN, which is managed by NIMS. In 2011, 5 graduate students from Japan came to NNIN sites; two to Georgia Tech and one each to the University of Michigan, University of Texas, and University of Colorado. • Yoshihiro Nakano, Tohoku University; worked at Georgia Figure 34: Pictured left to right Yuki Tech with Prof. Farrokh Ayazi on the project “Vibration Matsuoka and Seiya Suzuki. Energy Harvesters” • Ko Nakagawa, Hokkaido University; worked at Georgia Tech with Prof. Roasrio Gerhardt on the project “Development of Optimal Surface Coating Techniques for High- throughput, Dense-multiplexed Nanophotonic Biosensor Arrays in Lab-on-a-chip Applications” • Yuki Matsuoka, Toyota Technological Institute; worked at the University of Michigan with Prof. John Hart on the project “Carbon Nanotube Microsensors and Microactuators for Biomedical Microsystems” • Seiya Suzuki, Toyota Technological Institute; worked at the University of Colorado with Prof. Thomas Schibli on the project “Graphene-based Ultrafast Electro-optical Modulators” • Yoichi Ogata, Japan Advanced Institute of Science and Technology; worked at the University of Texas with Professor Brian Korgel on the project “Photovoltaic Devices Made of Silicon Nanowire Fabric”

Each of these students was at the NNIN sites for 8-10 weeks during which time they were treated much like our REU students. In particular, they were integrated both socially and technically with the REU students, which added greatly to their experience. Unlike undergraduate REU students, these graduate students come with a significant prior skill set and more focused scientific interests. During this time they integrated into the appropriate research group, were trained in equipment and techniques, and contributed to both their own research project and the overall goals of the research group. Four of the students were able to participate in the NNIN REU convocation in Atlanta, further enriching their experience. Since 2008, 18 students have been hosted at eight NNIN sites: Penn State (x2), University of Texas (x4), Harvard, UCSB, Cornell (x2), Georgia Tech (x4), University of Michigan (x3), and University of Colorado. NIMS and Nanonet are highly pleased with the program and the interactions developed with this exchange. The goal of this program is much the same as iREU, that is, to increase awareness of the global nature of research. In this, it has been very successful. These students interact strongly with our resident REU students, which results in considerable synergy between the REU, iREU, and iREG programs. 3.3.4 RET Program Five sites participate in an NSF-funded Research Experience for Teachers (RET) Program which began in March 2006. While separately funded, RET is tightly woven into the NNIN Education Program. The initial NNIN REU program (2006-2008) was funded by a separate NNIN award with 5 participating sites. A second three-year NSF award was received in May 2009 and supports the current program. Georgia Tech (lead), Harvard, Howard, Penn State, and UCSB host the teachers. In 2011, we had 20 participants:

NNIN Annual Report p.56 March 2011-Dec 2011 11 women (55%), 9 men (45%) and 45% from underrepresented populations. This is consistent with the entire six-year program which had 116 diverse participants: 54% women; 46% men, and 42% from underrepresented populations. Some sites leveraged the RET award with NNIN funds to support additional participants (5) in 2011 (and other years). We achieved our goal of having teachers from minority populations. We have also been highly successful in having teachers who teach at schools with high-minority populations: ~70% of the schools have a high percentage of underrepresented populations (race, ethnicity, and socioeconomic status). The summer of 2011 was the final year of the existing NNIN RET award. A followup program has been proposed by Georgia Tech, with a somewhat different line-up of participating sites. Although it is funded separately, the NNIN RET program is an integral part of the NNIN Education Program. It is directed out of the NNIN Education Office, is implemented by the NNIN Education Coordinators at participating sites, and the work product of the RET program forms a major part of the nanotechnology education resources distributed by NNIN. Not all sites, however, participate in this program for financial, geographical or programatic reasons. For example, due to the follow up required, a long term successful RET program requires a high concentration of teachers within commuting distance. This is not practical at many sites. Each RET participant completes a post- survey based on one developed by the RET Network. The survey was modified to reflect specific questions regarding NSE. Results from some of our survey questions are in Table 8. These reflect some of the results that address the issues of whether the program provided a research experience, had an impact on teaching, and was an overall positive experience.

Table 8. Examples of NNIN RET Post Survey Results 2011 (n=13) Avg.* Program was responsive to professional development needs 3.9 Program provided opportunities to engage in inquiry/research activities that I will adapt for classroom use 3.9 I collaborated in ongoing research with site staff 3.5 I operated instruments, equipment, & other technologies 3.7 Program increased interest in research & ways that STEM can be applied. 4.0 I gained greater understanding of the applications of STEM to everyday life. 4.0 I acquired greater understanding of fundamental concepts in STEM 3.7 I became familiar with new materials & equipment that I can use in my teaching. 3.8 I learned innovative ways to use standard materials and equipment in my field. 3.8 I increased my knowledge of current issues in STEM research 3.8 Mentor’s knowledge of roles & responsibilities of teachers in STEM 3.8 Mentor’s interest in helping you develop a plan to improve education in STEM 3.9 Would you recommend the NNIN RET program to your colleagues? 3.8 Please rate the NNIN RET program as a professional development program 4.6/5.0 Likert scale 1-4 1= not at all; 2= small extent; 3= moderate extent; 4= great extent

The results indicate that teachers were actively engaged in research that they can adapt for their classrooms, a main goal of the program. The project mentors showed that they had an understanding of teacher roles and responsibilities and wanted to help the teachers in improving education. Teachers also indicated that they increased their knowledge of current issues in STEM research. Overall, the program received very high ratings. During the school year, each site supports the teachers in their classroom to help introduce NSE into their courses. The RET program culminates at the National Science Teachers Association (NSTA) annual

NNIN Annual Report p.57 March 2011-Dec 2011 meeting. All participants from the five sites meet for a half-day session (NNIN RET Share-a-Thon ) where classroom materials are shared and critiqued. Teachers interact with their fellow NNIN RETs which builds a sense of community. Each participant develops an instructional unit for his/her classroom, which is then reviewed and field tested before placement on the NNIN education portal (http://www.education.nnin.org). In addition, the RETs “work” at the NNIN exhibit booth at NSTA and interact with attendees as experts in bringing NSE into the classroom Lessons and modules developed by the NNIN RET participants are an important part of the expanding set of nanotechnology education resources offered by NNIN. RET modules are edited, reviewed, and vetted, and eventually posted on the NNIN education web portal, making them available for wider use. These activities also become an important part of the activities NNIN uses at its various workshops, camps, and public engagement activities. In spring 2011, we began a new survey that would examine how participants (post-NSTA meeting) were interacting with their site and what they thought about the program several months later. This survey was done with the 2010 participants and will be done in late spring 2012 with the 2011 participants. Some results are below: Table 9. 2011 Follow-up survey of 2010 RET program (n=16) Avg. I have continued to interact with my NNIN RET site 3.2* I would like to maintain my interaction with the RET site beyond this school year 3.6 I plan to continue offering NSE in my teaching 3.7 I have shared my summer experience with colleagues 3.7 I have been in contact with my project mentor/advisor 3.2 I learned how NSE can be integrated into standards-based science 3.8 I believe that it is important for students to know something about NSE 3.8 What was the level of interest or reaction by your students to your lesson? 3.8 *Likert scale 1-4 1 = not at all 4= great extent

Most encouraging with these results is that the teachers plan to continue offering NSE-focused lessons and that their students demonstrate a high level of interest with these lessons. Ninety-two percent of respondents indicated yes to the question: “Do you think your RET experience has had any impact on student interest in STEM?” Written responses included:

• Many students are now interested in pursuing a career in engineering • Students are eager and amazed about the wide array of NSE applications • Students see my experience, ask questions about it, and many want similar experiences for themselves • Students respect my ideas more when they know I have had a research experience • It has promoted inquiry into the field and career offerings

Seventy percent indicated that they would use additional NSE materials (beyond the lesson they developed) in their classroom. We interpret this to mean that they feel confident to include NSE in their teaching and that they understand how it fits into a standards-based curriculum – something we stress throughout the program.

3.3.5 iWSG The international Winter Schools for Graduate Students (iWSG) are organized jointly by NNIN and institutions in develping countries with the goal of promoting international bridge-building and understanding by bringing together students and faculty in an intense teaching and societal experience. Each year, approximately10 US graduate students and 5 US faculty participate in a rigorous course in an

NNIN Annual Report p.58 March 2011-Dec 2011 emerging and research-intensive interdisciplinary nanotechnology topic. This course lasts six days and includes laboratory sections. This is followed by travel to a rural, underdeveloped part of the country (~4-5 days) where students spend time observing, experiencing and discussing the societal challenges and the part science and technology can play in a developing society. A large group of students from the host

Table 10. Evaluation results for iWSG 2011* AVG. To what extend did the Winter School: Avg. Give you a broad perspective of fabrication & its challenges 4.5 Introduce the context of fabrication and its current R&D context 4.1 Provide broad understanding of oxidation and chemical deposition processes 4.2 Provide introduction to vacuum equipment and physical deposition 4.5 Discuss and help you understand the variety of optical lithographic techniques 4.4 Discuss and help you understand electron beam and soft lithography 4.3 Provide and understanding of wet etching and dry etching techniques 4.3 Discuss underpinnings of chemical precursors and related deposition 3.1 Discuss and introduce stress and defect evolution in films & crystals 4.7 Help you understand implantation and annealing 4.8 Discuss & helped you understand optical characterization techniques 4.1 Provide an understanding of how processes are integrated for MEMS 3.3 Provide an understanding of how MEMS devices are characterized 3.3 Provide an understanding of process integration for CMOS 2.9

country participate in the course part and a smaller group joins in the rural experience

NNIN Annual Report p.59 March 2011-Dec 2011 Discuss and helped you understand other in-process characterization (AFM, SEM, etc.) 4.2 Present in an understandable way the context of technology in Indian environment 3.8 Help you see differences in perspective of how problems of living are viewed from Indian 4.2 perspective *Likert scale: 1 = not at all; 5 = great extent

The third iWSG took place at IISc-Bangalore, India during January 3-15, 2011 with the societal experience in Dharmasthala. Thirteen graduate students from across US institutions participated in this event. The subject of the teaching was “Science and Technology of Nanofabrication”. The rural experience focused on early education and rural needs. The participants visited such places ad the Rural Development and Self Employment and Training Institute, local schools, and an energy cooperative,among others. This year they also brought education demonstartions/hands-on activities to do with local school children. Participating students were selected from a nationwide solicitation and included: • Julie Bert, Stanford University • Michael Junkin, University of Arizona • Blair Brettman, MIT • A.J. Kumar, Harvard University • David Carlton, Univ. California, Berkeley • Vincent Lee, Columbia University • Matt Gibson, University of Michigan • Jonilyn Longenecker, Cornell University • Joseph Grogan, Penn. State University • Sarah Lukes, Montana State University • James Pikul, University of Illinois • Kasey Phillips, Harvard University • Thomas Woodson, Georgia Tech

Participating US faculty and personnel included: • Prof. Sandip Tiwari, Cornell University • Prof. Steve Campbell, University of Minnesota • Prof. Bart Vanzeghbroeck, University of Colorado • Dr. Bojan Ilic, Cornell University • Prof. Karl Böhringer. University of Washington • Dr. Larry Goldberg, National Science Foundation US students completed an evaluation instrument for the event and the results are presented in Table 11. Overall, the course received very good ratings including providing a broad perspective to the field and its challenges as well as allowing participants to interact across international boundaries and see the other world perspectives. This latter was an important goal of the program in that we are seeking to develop globally aware scientist through this experience (an important focus of the program). Participants in the field trip portion of the trip completed an essay on their thoughts and observations. These essays indicated that students were extremely positive about the workshop and the field trip. The visits to rural villages in India were “eye-opening” events for all participants and helped them to see how technology connects and potentially can help the poorest people in the world. Sample comments by the US participants are in the text boxes to the right. The comments reveal the various impacts that the rural experience had on the students.

Figure 30. Scenes from the 3rd iWSG that was held at IISc, Bangalore, India and its post-teaching societal activities.

NNIN Annual Report p.60 March 2011-Dec 2011 The 4th International Winter School was conducted in January 2012 in the São Paolo state in Brazil in conjunction with our partner UNICAMP, the University at Campinas. Fifteen US participants were selected from graduate schools across the country. Student participants included

• Arrielle Optowsky, U. Wisconsin • Meredith Lee, Stanford • Jared Schwede, Stanford • Kevin Luke, Cornell • Romy Fain, Cornell • Joseph Young, Rice • Tatyana Sheps, UC Irvine • Kishore Padmaraju, Columbia • Morgan Stanton, WPI • Jenna Hagemeir, UCSB • Anna Shneidman,Harvard • Brian Lambson, Berkeley • Zephram Marks, U. Colorado • Sonia Buckley, Stanford

• Jaime Teherani, MIT

They were joined by 7 US faculty and about 50 participants from South America. The technical part of the course was on Optoelectronics with basic and advanced lectures on topics including lasers, waveguides, LEDs,VCSELs, modulators, detectors, non-linear optics, and optoelectronic circuits.

US Faculty included

• Prof. Bard van Zedgbroeck, U. Colorado, (technical organizer) • Prof. Connie Chang-Hasnain, U.C. Berkeley • Prof. Michal Lipson, Cornell University • Prof. Michael Hochberg, U. Washington • Prof. Kent Choquett, Univ. Illinois • Prof. Alex Gaeta, Cornell • Dr. Laura Grossenbacher, U. Wisconsin (Social and Ethical Issues Coordinator)

For the second week field trip, 15 US student participants, 3 faculty, and 4 Brazilians ventured into rural parts of Brazil including visits to the Atlantic rain forest. A high point of the experience was several hands- on science demonstration activities done by our students in 2 rural villages, primarily using kids and modules developed as part of the NNIN Education program.

In Fall 2011, we instituted a new survey to follow-up with participants in the iWSG to gain information on how they perceived the technical and societal portions of the course years to months after their participation. To date, 24 of the 33 participants (from the first 3 years) have completed the survey. This survey will become ongoing which will annually request participants to complete it several months after their participation. Results for the technical and societal pieces of the survey are presented in Tables 11 and 12 below. The results demonstrate that the technical portion of the course did an effective job in presenting the technical aspects and that the topics have been at the forefront of new knowledge. It does appear that participants would like to have more time for discussion and this will be taken into account with future international offerings. The societal portion of the program received very high marks and clearly demonstrates that exposure to the underdeveloped world is extremely important in developing a global perspective in these young scientists and engineers. Ninety percent of the respondents indicated that the IWSG was time well spent in their academic career and 68% indicated that the experience has had an impact on their views of technology and society.

Table 11. Technical Portion Questions iWSG 2011* (participants from IWSG 1,2,3) Avg. The course was the correct level for my background and experience 3.6 The presenters were very knowledgeable and added to my understanding of the topic 4.5

NNIN Annual Report p.61 March 2011-Dec 2011 The course provided the right balance of lecture, labs, and discussion 3.4 The course provided the host country's perspective on the topic 4.0 The course provided an effective forum to discuss critical technical issues 3.3 The course duration was sufficient for the topics covered 4.2 The course topic was timely and provided current and cutting-edge information 4.3

Table 12. Societal Portion Questions iWSG 2011*(participants from IWSG 1,2,3) Avg. It allowed me to identify/perceive the world context of technology 4.7 It allowed me to see how technology can help improve the lives of under-served 4.6 It allowedli me to put my research in the context of the global arena 4.1 It allowed me to have discussions with the foreign participants about technology and 4.8 It openedi up my understanding of technology and the impact on society 4.6 It has influenced my future in terms of my career choices 4.1 *Likert scale 1-5 1 = poor/no 5 = superior/very yes The winter school is a comprehensive education program whose content is archived at the NNIN education portal. See, e.g. http://www.nnin.org/nnin_iwsg_2010_bangalore.html for the latest course. Included in this education are quizzes to assess the learning. These also give an opportunity to compare the knowledge acquisition of the participants. Figure 35a shows distribution of scores from the iWSG3 of the US participants, and the non-local Indian participants through 17 quizzes.

Figure 35a: Histograms of scores of participants during the teaching part of IWSG3 3.4 Other Education Programs 3.4.1 Teacher Workshops NNIN (Georgia Tech) has developed and provided teacher workshops on nanoscale science and engineering (NSE). The intent of these activities is to give teachers the background and tools necessary to increase student awareness and interest in science and technology in general and NSE in particular. We believe it is very important to provide professional development training for teachers in order to move NSE into classrooms to help meet the projected workforce demands of nanotechnology.

NNIN Annual Report p.62 March 2011-Dec 2011 Georgia Tech has offered a variety of workshops which range from two hours to one week which focus on how NSE can be included in standards-based science curriucla. All of the instructional materials are tied to National Science Education Content Standards or state standards if the workshop is offered at a state meeting. This is done to ensure that teachers are using standards-based units. Georgia Tech workshops in 2011 were presented at the annual meetings of the Georgia Science Teachers Association, Texas Science Teachers Association (with University of Texas), National Science Teachers Association, and California Science Teaches Association. Other venues were at Tennessee Technological University, University of Texas Health Science Center (San Antonio), and American Association for Engineering Education. Figure 36 shows the states and Georgia counties where NNIN has reached at least one

Figure 36: Georgia counties and states where GT has reached teachers teacher in a workshop (typically more than one per shaded area). These workshops have proved extremely popular, beyond the capacity of the GT site to provide. Because of this, NNIN sites are now encouraged to either exhibit or present at their state science teachers’ association meeting to inform teachers about NSE and its inclusion in the science curriculum.The office at Georgia Tech assists with these regional events when requested to leverage the existing expertise of the network. The University of Texas (with assistance from the NNIN Education Office) exhibited at the Texas Science Teachers Assocation annual meeting in November which had over 7,800 attendees. UCSB provided workshops at the October meeting of the California Science Teachers Association and Stanford asssited UCSB and GT with the exhibit booth. The University of Michigan and University of Minnesota both offered workshops and an exhibit booth at their state science teachers association meetings. Stanford provides hands-on activities, lectures, and facility tours to teachers attending the weeklong Summer Institute for Middle School Teachers. This demonstrates that the NNIN sites are willing to assist with this increasing demand for teacher professional development programs offered by the network. Georgia Tech uses pre and post surveys to determine if the workshop participants have gained understanding of the nano-concepts presented. Using these data, the workshops have been refined over time. For example, in a lesson on the tools of NSE teachers were shown AFM images and they indicated on the post surveys that an AFM can see nanoscale objects. The lesson was changed to stress that nanoscale materials are below the visible spectrum of light (thus optical microscopes cannot be used) and that we must use different methods to image and interpret materials at that scale. With this approach, a majority of teachers understood how and why we use an AFM to observe the nanoscale. 3.4.2 NanoTeach In September 2008, NSF (DRK-12) funded the Mid-Continent Research for Education and Learning’s (McREL) NanoTeach project. Stanford, Georgia Tech, and University of Colorado at Boulder (MRSEC) are the university partners for this professional development program. Since its inception, the NNIN sites

NNIN Annual Report p.63 March 2011-Dec 2011 at Stanford and Georgia Tech have been involved in the development of the two week professional development pilot workshop which occurred July 12-23, 2010 with the pilot follow-up occurring July 21-22, 2011. NanoTeach (http://www.mcrel.org/NanoTeach/index.asp) uses a combination of face-to-face and online professional development experiences for high school science teachers who teach physical science topics. The primary goal of NanoTeach is to prepare teachers to use an instructional design framework to integrate NSE content into their curriculum in significant ways. The Stanford site has developed remote access events for NanoTeach and also provides content support. Georgia Tech developed a PowerPoint on the Big Ideas in Nanoscale Science and Engineering: A Guidebook for Secondary Teachers (Stevens, et. al, 2009), developed posters on the Big Ideas, provided content and instructional materials support, and recruited NNIN site researchers to present webinars. Both NNIN sites are active in evaluating pre- and post-survey answers and providing content support for the instructional model. This fall, NanoTeach began the fourth year of this five year program and the NNIN sites have been active in developing the next phase of the implementation as well as in recruiting school districts. The next phase will require 150 participants in a two-pronged approach: one group will receive a two week workshop and one group will receive all materials but will not be in a facilitated group and will operate as a self study. Gwinnett County in Georgia (the state’s largest district; 16th in the nation) is one of the sites being recruited for summer 2012. 3.4.3 Other K-12 outreach Numerous outreach activities have occurred in 2011 including K-12 field trips to facilities, visits to schools, summer/weekend camps, workshops, and demonstrations. In order to provide these activities, the NNIN sites have developed hands-on activities (http://www.nnin.org/nnin_k12teachers.html), demonstrations, and presentations on NSE. We also adopt and adapt activities developed by other centers and programs such as University of Wisconsin-Madison MRSEC & NSEC, Nanosense (SRI), NISE Net, among others. Hands-on summer, weekend, or after-school camps/programs to engage students in NSE are offered by numerous sites in addition to school on-site visits and tours. These camps/programs focus on middle and high school students and have a variety of formats (1day to one week) and content (chip camps, introduction to nano, biomedical, etc.). In addition, most sites provide on-site activities for visiting school groups as well as the general public. These typically involve lectures, hands-on activities, demonstrations, lab tours, and cleanroom tours. Most include discussions on career and educational opportunities to encourage students to consider careers in STEM and in particular NSE. Sites are also involved in career days at schools, family science nights, science fairs, and community days. Examples of some of these program for 2011 include: • UCSB “Chip Camps” provides hands-on nanofabrication to students from area high schools. • University of Michigan offers NanoCamp (parent and student versions) and support of SWE Summer Engineering Explorations Camp • University of Minnesota’s Science participated in Engineering Day and NanoNights at the Science Museum of Minnesota • University of Washington hosted tours of the facility to school groups • Stanford provides support for the Summer Institute for Middle School Teachers by hands-on activities, demos and a tour of the cleanroom facilities • Arizona State has been developing fourth grade lessons in collaboration with a local elementary school • Harvard presented demonstrations at Salud y Familia and at Cambridge Public Schools Eight grade Science and Engineering Showcase

NNIN Annual Report p.64 March 2011-Dec 2011 • Cornell participates annually at the Lower Hudson Valley Engineering Expo and the FIRST Junior LEGO® Event • Washington University has mentored high school students to provide an experience of working in the nanotechnology research facility by having them assist in research with the lab technicians • University of Colorado offered “Experience Nano” to elementary students • Georgia Tech hosted a variety of middle and high school students for an introduction to nano • Penn State participated in the campus Exploration Days with demos • University of Texas provided activities for a middle school science club At the September 2009 coordinators meeting it was agreed that all sites would seek materials from NISE Net to host a NanoDay event beginning in 2010. In 2010, 13 sites participated and 9 in 2011. Sites are either the primary sponsor of the NanoDays event or host in collaboration with a local science center or museum. 3.4.4 NanoExpress Figure 37: Nanoexpress at the Boston Museum of Science. Howard University launched the NanoExpress in summer 2006. This is a mobile laboratory which presents the world of nanotechnology to schools and the general public. The NanoExpress (Figure 37) is a mobile van with 208 square feet of lab space designed to facilitate hands-on experiments but also capable of doing nanotechnology research. Experimental areas include: Introduction to Passive Nanoparticles, Introduction to Self Assembly, Introduction to Micro and Nanofabrication, “Chips are for Kids”, Instruments for NanoScience, Shape Memory Alloys, and Soft Lithography. Undergraduate, graduate lab assistants, and RETs help supervise experiments. In 2011, NanoExpress visited D.C. area schools, Black Engineers of the Year, Exxon Science Camp, Howard Homecoming, National Society of Black Engineers and various universities. 3.4.5 NNIN Education Portal The NNIN education portal (http://www.education.nnin.org) serves as another avenue in reaching a variety of audiences by offering information for children and adults. There are general interest articles, links to additional resources, and lessons (primarily by RETs) for teachers. Multimedia resources and the “Open Textbook” are also available for undergraduates and graduate students. 3.4.6 Nanooze NNIN produces and distributes a children’s science magazine related to physical sciences and particularly nanotechnology. Editorially the content is produced by Prof. Carl Batt of Cornell, with printing and distribution handled by the NNIN office at Cornell. Nanooze began as a web based magazine (http://www.nanooze.org/), with kid-friendly text, topics, and games. It is designed for grades 5-8 but we have found that even high school students enjoy the magazine. The web edition of Nanooze is available in English, Spanish, and Portuguese on the web. Nanooze has evolved into an 8 page printed “magazine” that is distributed irectly to schools in hard copy; we are currently producing a 4 issue series on atoms and molecules, in conjuction with the International Year of Chemistry. A total of 10 issues are available, each with colorful graphics and interesting stories written at an accessible level. They are used as enrightment material at all levels from elementary to high school and beyondTeachers may request classroom packs of any or all of these issues. Through a variety of distribution mechanisms, including

NNIN Annual Report p.65 March 2011-Dec 2011 NNIN’s exhibit booth at NSTA, over 100,000 copies were distributed to upper elementary through high school students in 2011 (more than 800,000 copies have been printed).. PDF versions can also can also be downloaded from the web site for local printing. Additional details are available in the Cornell site report.

Figure 38: 5 most recent issues of Nanooze

In addition, NNIN has two 1500 sq.ft. interactive ”museum” displays that are currently deployed at Disney World Epcot and at Innoventions in Disneyland Anaheim. There exhibits were developed under other programs, but now fall under the “Nanooze” brand. They promote nanotechnology and Nanooze to hundreds of thousands of visitors each year.

3.5 Technical Workshops--Laboratory Figure 39: "Nanooze Lab" at Disneyland Innoventions, celbrating the International Year of Oriented Chemistry The NNIN is committed to workforce development training through a variety of activities which have been developed and implemented across the network. Training and development activities focus on undergraduate and graduate students, industry and government personnel, and faculty from other institutions. Information on these workshops is found on the NNIN website and upcoming events are advertised on the home page so that individuals can find quick links to the technical workshops. A variety of multimedia is also available on the website including talks, symposia, short courses, and equipment training - http://www.nnin.org/nnin_multimedia.html. Individual sites also offer online training materials which are downloadable. Many of these video demonstrations and lectures are downloaded by individuals worldwide for use in classrooms and training activities. Technology and Characterization at the Nanoscale (TCN) is a workshop offered twice a year by Cornell. The content of TCN is designed to encompass all nanotechnology techniques relevant to current research in the field. While traditional topics in nanotechnology - thin films, lithography, pattern transfer (etching), and characterization - provide the basic structure of the course, we include emerging technologies and new approaches in nanotechnology. Nano-imprint lithography, bottom-up nanofabrication, carbon nanotubes, soft lithography, and surface preparation for biology applications are among the topics addressed. The University of Minnesota provided several workshops during the past year. The workshops included 7th Annual Minnesota Nanotechnology conference as well as shortcourses on: E-beam Lithography, Micromachining, and Thin Films. The University of Michigan presented IntelliSuite a workshop on MEMS/Microfluidic Design and Analysis Tool and a short course on Advanced Techinques in Atomic

NNIN Annual Report p.66 March 2011-Dec 2011 Force Microscopy. Georgia Tech hosted an intersite workshop on graphene as well as two NanoFans(Nano Focusing on Advanced NanoBio Systems) a twice yearly forum to connect the medical/life sciences/biology and nanotechnology communities. The two workshops were on Nano/Microtechnology in Neuroscience and on Nanomedicine. (http://www.mirc.gatech.edu/ nanofans.php). The University of Colorado hosted a one day workshop on graphene and a three-day workshop entitled “Introduction to Nanofabrication.” They also hosted a one day workshop on Graduate School Advising that brought to CU several participants from the international Winter School (IWSG) to provide advise to the participants. The University of Texas provided a workshop entitled “Surface Measurement Systems.” 3.6 Symposia and Advanced Topics Workshops NNIN has over recent years held a number of special focused advanced topic workshops or symposia which bring together significant contributors in fields covered by NNIN. In general, the purpose of these special workshops is to explore emerging areas in which NNIN may be able to make significant contributions. They aim to foster interactions with NNIN and interactions between the participants, and are one source of information to guide NNIN management in new initiatives. With the recent renewal, NNIN recommitted to these special symposia with a goal of 4 major events per year. Only one was held in 2011 with two scheduled for January 2012. Arizona State University offered “Organic/Inorganic Interfaces and their Health Science Applications” January 13-14, 2011. The prupose was to increase awareness of the ASU role as the technical lead for organic/inorganic interfaces and to foster collaboration with neighboring schools. The symposium comprised three sessions addressing topics related to: 1) Sensor Elements; 2) System Level Integration; and 3) Cellular Interfaces and Control. Approximately 100 participants attended the two day symposium to hear 23 speakers, including 15 from external universities. Presentation subjects ranged from pore- based DNA sequencing and graphene chemical sensors, to fully integrated environmental monitors for personal health care, and CMOS based sensing of cultured cells. A lively student poster competition took place on Thursday evening with the external speakers judging the posters to pick the top three finalists. In January 2012 a total of 4 different major symposia were held. These included

• Materials and Manufacturing for Energy and Electronics, held a UT Austin and co organized with Penn State,

• NNIN Symposium on Frontiers in Nanoscale Transistors and Electronics held at UCSB, • Bio-inspired Engineering, held at Harvard

• Synergy Between Experiment and Computation in Energy – Looking to 2030, a symposium organized at Harvard as part of the NNIN/C computational nanotechnology effort Reports from these major symposia will be posted on the NNIN web site. 3.7 Diversity Related Efforts and Programs A primary focus of NNIN E&O is inclusion of underrepresented populations and this theme runs throughout the education goals and objectives of the NNIN. While there are specific outreach activities that focus on underrepresented populations, inclusion is an underlying objective of all of our outreach programs. Discussed below are some of the specific programs that are occurring which highlight some of our inclusion activities. Individual sites make every effort to ensure participation by underrepresented groups in the K-12 programs. With our data management system, gender and ethnicity are being tracked for all activities (when possible). Sites that are located in diverse areas of the country have the best opportunities for

NNIN Annual Report p.67 March 2011-Dec 2011 recruiting underrepresented participants to the events. However, all sites make an effort for reaching out to diverse populations. For example, the University of Michigan exhibits each year at the regional National Society of Black Engineers conference and UCSB works with students and teachers in high minority (Hispanic/Latinos) schools as well as the MESA (Mathematics Engineering Science Achievement) program at UCSB. MESA is a national program that works with educationally disadvantaged students so they can excel in math and science. 3.7.1 Diversity in NNIN REU Program Our REU program places a special emphasis on providing research opportunities for women and minorities. Specifically, the program requirements indicate, “Sites are encouraged to select applicants who are female, minority members, or from non-research institutions.” The REU program has quantifiable benchmarks regarding participants which include 50% women participants, 20% from underrepresented minorities, 50% from schools with no Ph.D. program in science and engineering, and 50% from outside the 100 largest research universities. The results reported in the REU section of this report demonstrate that women typically have a higher participation rate in our program in comparison to the applicant pool and in 2011 we had 51% female participation in the REU program with 49% in 2010 and 54% in 2009, very close to our 50% benchmark. Minority students participated at a higher rate than the applicant pool with 28% participating in 2011 from an applicant pool of 19%. This is greater than to our benchmark of 20%. This is an increase after two consecutive years of having minority participation rate the same as the application rate. We continue to fall short of our benchmark of having 50% of the interns come from schools with no Ph.D. program in science and engineering with 26% of our interns coming from these schools in 2011. We typically have two-thirds of our applicants coming from Ph.D. granting institutions which is then reflected in the participation percentage of around 67-70% each year. 3.7.2 Diversity in NNIN RET Program The NNIN RET program recruits teachers who are themselves from underrepresented groups or teach at schools with a high percentage of underrepresented students or low socio-economic status. In 2011, the 20 RETparticipants were - 11 women (55%), 9 men (45%), and 45% from underrepresented populations. Our RET program has been very successful in including teachers who teach at schools with high-minority populations - >70% of RET schools have a high percentage of underrepresented populations. The 2011 data are consistent a six-year total of 116 diversity participants: with 54% women and 42% from underrepresented populations. 3.7.3 Showcase for Students: An NNIN Diversity Program NNIN has developed the Showcase for Students which is an all day workshop on nanotechnology with morning lectures and activities and demonstrations in the afternoon. This event features a series of talks in the morning about the career and education opportunities in NSE. The afternoon session consist of a variety of high-tech and low-tech demonstrations of nanotechnology instrumentation and concepts. NNIN has an array of portable nanotechnology instrumentation, including AFM, STM, SEM, and a variety of optical microscopes. These are set up for live demonstrations for the students to visit and interact with. In addition, staff from NNIN sites bring smaller items that can be used to demonstrate nanotechnology concepts. These include Figure 40: Showcase for Students shape memory alloys, nanotechnology products, quantum dots, Demonnstration hydrophobic and hydrophilic materials, carbon nanotubes, and microfluidic devices. The focus is on

NNIN Annual Report p.68 March 2011-Dec 2011 undergraduate students who attend conferences sponsored by underrepresented professional science and engineering organizations. NNIN held one workshop in 2011 at the Society for Hispanic Professional Engineers Annual Conference in Aneheim, CA in October. We reached approximately 250 students at the event. The afternoon demonstration session is particularly well-received by attendees and they have indicated that they enjoy learning about nanotechnology but also interacting with NNIN researchers and staff who support the technical/demonstration session. An exit survey at the presentation and demonstration portions yielded the following results:

Table 13. Question (n=24)* Avg.* I learned about the interdisciplinary nature of nano 4.5 I learned about current nano applications/research 4.6 I learned about nano education paths 4.4 I learned about careers in nano 4.4 I learned about tools of nano 4.5 I enjoyed the nano demonstrations 4.8 I recommend NNIN repeat this at future SHPE conferences 4.8 *Some respondents only attended one session

**Likert scale 1-5 with 5 highest

3.7.4 Laboratory Experience for Faculty Program In fall 2007, NNIN introduced a new program, the NNIN Lab Experience for Faculty. The program focuses on supporting underrepresented faculty or faculty from minority serving institutions to perform research at one of our facilities. In some cases, the participants may become NNIN users in the future; in others, they will relate their experience to their students. Either way, NNIN has an impact on participation of underrepresented populations in nanotechnology. This program runs annual, in the summer in parallel with out REU program. Six awards of $13,000 each (covering stipend, travel, housing, and lab expense) were made to Stanford, University of Michigan, University ofTexas (x2), University of Minnesota, and Georgia Tech. Faculty spent 8-10 weeks in the summer of 2011 undertaking their own research project in nanoscale science. Table 14 summarizes the faculty and their projects.

Table 14. NNIN 2011 LEF participants.

Faculty Participant Home Institution NNIN Site Project

Prof. Zachariah Oommen Albany State University Georgia Tech Surface Chemistry of Gunshot Residue (GSR) Particles by X-ray Photoelectron Spectroscopy (XPS)- Complement to Electron Microscopy; Federal BallistiClean Prof. Kim Lewis Rensselaer Polytechnic University of Electrode Fabrication for Single Institute Michigan Molecule Transistors

Prof. A. Serdar Sezen Saint Cloud State University of Development of miniature tactile University Minnesota sensors capable of detecting tissue elastic properties Prof. Christi Madsen Texas A&M University University of Texas Integrated Optics

Prof. Haiyan Wang Texas A&M University University of Texas Processing and Characterization of Multifunctional Ceramic Nanocomposites

Prof. Unyoung (Ashley) Santa Clara University Stanford University Microfluidic Multi-target Cell Sorter Kim for Point-of-Care Testing

NNIN Annual Report p.69 March 2011-Dec 2011 Beginning in fall 2011, we sent a request to all LEF participants to complete a short follow-up survey to gain information on the technical aspects of the program with the results presented below. To date, 19 of the 24 participants have completed the survey. The results indicate that the LEFs were easily integrated into the facilities and had good support for the cleanroom and site staff allowing them to complete their project.

Table 15: LEF Follow-up Survey Results – Fall 2011 Technical Aspects Avg.*

Were you able to easily establish a working relationship with the site to develop your project? 4.4

Did you develop a good working relationship with your host NNIN faculty member 4.4

Were you able to execute the research project using the available equipment and facilities? 4.2

Please rate the quality and availability of the overall facility. 4.4

Did site staff provide assistance, if needed, to help develop your project? 4.4

Please rate the availability of necessary equipment in other labs, if necessary. 4.3

Support by cleanroom staff 4.5

Support by site education staff 4.7 *Likert scale 1-5 with 1= Poor/No and 5 = Superior/Very Yes We also asked them questions about their interactions with the host site and NNIN. As can be seen in the table below, many of the participants have continued interaction with the site with 2/3rd still users of the facility and the same number using the experience to enrich their teaching. While 42% have presented their results at a conference, very few have published their results.

Table 16 LEF Follow-up Survey Results – Fall 2011 No Yes NA I have continued to interact with NNIN site faculty/staff. 16% 84% 0% I am still a user of an NNIN facility. 32% 63% 5% The results of my research have lead to a conference presentation 47% 42% 11% The results of my research have lead to a publication 74% 16% 10% The results of my research has lead to a funding opportunity 74% 10% 16% My students now use the NNIN facility 47% 47% 6% My students are aware of my research conducted at the NNIN site. 0% 100% 0% My students are considering or have applied for graduate school at the NNIN 37% 42% 21% I have shared my LEF experience with colleagues at my institution. 5% 95% 0% Have you used your LEF experience to enrich your undergraduate courses 37% 63% 0% Have you recommended undergraduate students to the NNIN REU program. 37% 47% 16% 3.8 Assesment and Evaluation NNIN has developed a variety of evaluation instruments for its major programs which include: REU, RET, iREU, LEF, past REUs, iWSG, teacher workshops (pre and post), camps (pre and post), and school visits (pre and post). Instruments have been shared among all of the sites which can adopt and adapt them for their particular programs. In 2008, NNIN developed a logic model and evaluation plan with the assistance of an external consultant (Tom McKlin, The Findings Group). The model and plan were presented in the 2008 annual report. We use the plan to ensure that we are collecting the correct data to assess the impact and quality of our outreach endeavors. Data presented in this report represent some of our findings using our instruments and other data collection methods.

NNIN Annual Report p.70 March 2011-Dec 2011 In Janualy 2012, NNIN assembled a team of experienced science education profesionals to conduct an independent focused review of the NNIN Education Program. This group included: Prof. Doug Huffman, College of Education, University of Kansas; Prof. Frances Lawrenz , Associate Vice President for Research at the University of Minnesota; .Dr. Lis Palmer, Aspen Associates; and Prof. Deb Newberry, Dakota County Technical College. While generally praising the quality and breadth of the NNIN Education Program they stressed the need to develop and implement a more rigourous assessment scheme for our activities. We will act on this recommendation as we move forward. 3.9 Program Summary NNIN’s education program Is widely recognized as a leader within the nanotechnology and academic research center community. NNIN has and will continue to offer a variety of education and outreach activities at the local and national level. Table 12 below summarizes the major network wide programs.

Table 17. Summary of NNIN Network-wide Programs. Program Participants Purpose Status REU Undergraduates Research experience for a diverse population Upcoming 16th summer of undergraduates; introduction to in 2012 nanotechnology research & careers iREU Undergraduates – Develop globally aware scientists and Upcoming 5th summer former NNIN REU engineers from the most successful REU in 2012 participants participants iREG Graduate students International outreach; reciprocity for iREU Upcoming 4th summer from Japan (NIMS) Japan; No cost to NNIN in 2012 RET Middle and high Introduce teachers to nanotechnology and 6th and final year 2001- school science experimental design; develop 12; new proposal teachers nanotechnology classroom activities submitted 8/2011 LEF – Lab Underrepresented Increase diversity in NNIN user base and in Upcoming 5th summer Experience for faculty and/or faculty STEM/ nanotechnology pipeline in 2012 Faculty from minority serving institutions SFS – Undergraduates Expose diverse population of undergraduates Plan to offer 1-2 times Nanotechnology to education and career opportunities in per year Showcase for nanotechnology Students Nanooze Upper elementary Stimulate and maintain interest in STEM at a Up to issue #10. and middle school young age Classroom packs students widely distributed in 2011 iWSG Graduate students Develop globally aware scientists and Third two week engineers; Provide technical workshops in workshop held in nano to US and foreign students; Encourage Bangalore, India in international collaboration January 2011.

NNIN Annual Report p.71 March 2011-Dec 2011 4.0 NNIN Computation Program Nanoscience, as we know it, would not be possible without computation. Numerical calculations are crucial for every stage of nanoscale research, including device design, analysis of experimental data, and complex predictive simulations. The computation project of the National Nanotechnology Infrastructure Network, (NNIN/C), enables nanoscience research by providing on-site domain experts, access to computing resources, a broad suite of simulation tools, numerous workshops, and unique cyberinfrastructure resources. This framework has led to an active and expanding NNIN/C user community that regularly generates seminal research and high-impact publications. Since its inception in 2004, the NNIN/C has focused on a broad range of simulation expertise and tools to address the spectrum of research projects in the nanoscale regime. While other NSF funded projects such as the Purdue Nanohub operate under a similar mandate, the computational effort of the NNIN/C is unique due to the fact that it is embedded at leading nanofabrication user facilities across the country. At each site, Ph.D. level research liaisons work directly with users to help them overcome the initial learning curve associated with new simulation approaches so that these tools can be an effective part of their research plan. These experts provide insight on multiple aspects of nanoscience, including MEMS and NEMS devices, electronic structure of materials, nanoscale thermal and electronic transport, semiconductor devices, and advanced parallel computing architectures (i.e. GPUs). This unique juxtaposition of simulation and fabrication efforts helps us reach and impact the efforts of a cross-section of nanoscale researchers that may be missed by other on-line or remote simulation efforts. This effort exceeds that of desktop capabilities, provides expert staff to assist new users in simulation approaches, and also serves as a gateway to larger NSF computational grid facilities such as XSede. In addition, the NNIN/C also provides targeted simulation workshops, cyberinfrastructure resources like the Virtual Vault for Nanoscience, and access to unique computing resources like the GPU cluster at Harvard. The success of NNIN/C is measured by its ever-increasing user numbers, by the popularity of NNIN/C sponsored events (such as the over 130 participants at the recent Conference on the Synergy Between Experiment and Computation in Energy at Harvard University) and, most notably, by the number and strength of the publications resulting from NNIN/C support – manifested by an incredible h index of 24 after only seven years. Since its inception in 2004, NNIN/C has stressed the synergy and close interaction between experiments and simulations and has thereby enabled cutting edge research and scientific and engineering discoveries in all fields of nanoscience. This report describes code and hardware additions, publication statistics and specific highlights, sponsored workshops and advanced projects – such as the virtual vault for nanoscience and the GPU project – during the past year of the project. References are given to the NNIN/C webpage where a complete record of publications and a list of codes, for example, can be found. 4.1 Codes at the Sites Nanoscale science pertains to the regime where the number of atoms or molecules under study are too numerous for a single-atom/molecule treatment, on the one hand. On the other hand, the number and arrangement of atoms is also neither regular (periodic) nor sufficiently large for meaningful statistical (thermodynamic) analysis. The foundations of nanoscale computation consist of electronic structure codes, which are initially appropriate for small atom number or periodic systems, and molecular dynamics codes, which are statistical insofar as they typically require ensembles of initial conditions and treat systems interacting with heat baths. Additionally, photonics and phononics codes address the primary bosonic degrees of freedom of nanoscale matter, processing or fabrication codes treat the physics of ion implantation (among other areas), and multiscale or finite element tools treat microfluidics, which while larger than the nanoscale often interfaces with nanoscale structures and are important in their own right.

NNIN Annual Report p.72 March 2011-Dec 2011 The complete list of codes, listed in a matrix according to site, can be found at: http://www.nnin.org/nnin_computation_code_matrix.html. This year, the University of Michigan underwent a major “ramp-up” of its code base and added the following tools:

Table 18: New Simulation Tools added at the University of Michigan site Molecular Dynamics Electronic Structure CFD and Finite Element Tools LAMMPS QUANTUM ESPRESSO* ELMER DL_POLY ABINIT* TAHOE NAMD Octopus FEBio DESMOND GAUSSIAN CFD-ACE+ GULP CPMD Gerris CP2K OPENFOAM MOSAICS IntelliSuite MCCS Towhee Free CFD Nanophotonics Codes Multiscale Tools/Fabrication DDSCAT Quasicontinuum MULTEL CADD Meshfree Methods LibMultiScale Unitah OCTA IntelliSuite

4.2 Hardware Update at Harvard The NNIN/C Project at Harvard University has announced the purchase of a new computational cluster for the general use of NNIN/C members, both locally and nationwide. The new equipment, will consist of 480 nodes with each of the 80 Intel Xeon X5650 processors hosting six cores and having 24GB of memory. The new cluster will be hosted and maintained by the Faculty of Arts and Sciences Research Computing group, headed by Dr. James Cuff. 4.3 NNIN/C Impact in Science and Education The NNIN/C continues to have an important impact on research activities both at nodes in the NNIN/C and other institutions across the United States. Since its inception, NNIN/C user activities have been measured based on the number of researchers who obtain accounts and perform research on NNIN/C computational facilities. However, this measure unfortunately does not capture consulting activities or collaborative work which also leads to a measurable impact in research. Since the computational liaisons are embedded at nanofabrication facilities, these direct exchanges can occur quite often. Other major nanotechnology simulation efforts, like the NCN, measure user number based on the number of researchers who log into the Nanohub site. In order to develop similar statistics, the NNIN/C will be moving to a platform where researchers interested in consultations or computing resources can fill out a standard request form. During this current transition period, we have listed user statistics both in terms of the old measure (researchers using computing resources at NNIN/C) and the new framework (consulting, collaborations, and local resourcess.). In addition, we have listed seperately the number of participants at each site that have taken part in educational activities (conferences, workshops, courses).

NNIN Annual Report p.73 March 2011-Dec 2011 Table 19: User Statistics for the different NNIN/C sites

Total Users (consulting, Users with computing time on Educational collaborations, computing NNIN/C resources Participants time)

Internal External Internal External Harvard 38 41 34 22 130 Cornell 30 29 29 10 65 Stanford 63 32 40 13 10 Michigan 14 12 8 9 94 4.4 Research Highlights The NNIN/C initiative focuses on providing doctorate level expertise and consultation, cutting-edge simulation tools, and computing resources to help researchers succeed. The effectiveness of this effort can be measured through the publications of NNIN/C users and the impact they have had in the scientific community. During 2011 and early 2012, 34 publications resulted from NNIN/C users in leading journals such as Nature Nanotechnology, Proceedings of the National Academy of Sciences, Nano Letters, and Physical Review Letters. Since the NNIN/C program started in 2004, there have been 160 publications through the NNIN/C program that have been cited a total of 2036 times with an average of 15.19 citations/paper. Five of the papers have 95 or more citations. The total collection of NNIN/C papers has a Hirsch or h index of 24 which indicates that 24 papers have 24 or more citations. (Citation data and statistics obtained from Thomson Reuters ISI Web of Knowledge). A full list of NNIN/C publications is available at the NNIN website: at http://www.nnin.org/nnin_computation_publications.html During 2011, several NNIN/C users also received awards or accolades for their research using NNIN/C computing resources. • Zoe Boekelheide (University of California at Berkeley) won the American Physical Society, Group on Magnetism and Magnetic Materials (GMAG) Dissertation Award for 2011. Her work focuses on the effects of nanoscale structure on magnetic and transport properties of chromium and chromium-aluminum alloys. • Nicholas Moore and colleagues at Northeastern University won the best paper award for the use of GPUs in scientific computing at the 2011 Symposium on Application Accelerators in High Performance Computing (SAAHPC 2011). • Joshua Taillon won the 2011 Best Overall Materials Science and Engineering Senior Thesis at Cornell University for his thesis “Ab Initio Discovery of Novel Crystal Structure Stability in Barium and Sodium-Calcium Compounds under Pressure”.

NNIN Annual Report p.74 March 2011-Dec 2011 4.4.1 Dynamics of Polymers in Flowing Colloidal Suspensions Hsieh Chen and Alfredo Alexander-Katz, Physical Review Letters 107, 128301 (2011). Understanding the dynamic behavior of dilute polymers in flow has been an active research area during the last decades because of its direct relevance to the rheological properties of polymer solutions, as well as to the emerging technologies of single-chain analysis of DNA molecules. More recently, it has also been discovered that the dynamics of globular (or collapsed) polymers directly correlates with the functionality of certain proteins in blood that are crucial during the blood clotting cascade. The properties of very dilute polymer solutions are important to understanding the physical origin of the dynamics of polymers in flow, but in most applications one does not Figure 41: a) Snapshot of a single chain (blue have single polymers. Instead, one would typically have a beads) with a cohesive energy ε=2.08 unfolding in dense solution and in many cases a mixture with colloidal a sheared colloidal suspension (red spheres) with Φ=15% and r¬c= 5. (b) Typical extension particles. Thus, it is of interest to understand how the sequences as a function of time for a collapsed dynamics of the single chains is modified under these polymer at different colloid volume fractions conditions. In this Letter we study such a scenario by Φ=0%, 15%, and 30%. The other parameters are γτ = 2 and rc= 5. exploring how polymers behave in sheared colloidal suspensions. To attack this problem we consider the simplest model that we believe captures the essential physics of the problem, namely, a monodisperse colloidal suspension with a homopolymer undergoing shear flow, and simulate it using hydrodynamic simulations. The particular question we address here is how the unfolding and refolding cycles of the polymers in shear flow are affected by the presence of the colloids. A representative snapshot of our simulation results is presented in Fig. 40(a), where we show a stretched chain (blue beads) in a sea of colloids (red spheres) undergoing shear flow. The polymer extension Rs is defined as the projected polymer length along the flow direction as illustrated. In Fig. 40(b) we present three time sequences of the extension of the collapsed polymers (with ε = 2.08 ) at the same sheer rate γτ = 2 but with different colloidal volume fractions.

4.4.2 Ambipolar field effect in the ternary topological insulator (BixSb1–x)2Te3 by composition tuning Desheng Kong, Yulin Chen, Judy J. Cha, Qianfan Zhang, James G. Analytis, Keji Lai, Zhongkai Liu, Seung Sae Hong, Kristie J. Koski, Sung-Kwan Mo, Zahid Hussain, Ian R. Fisher, Zhi-Xun Shen & Yi Cui,

"Ambipolar field effect in the ternary topological insulator (BixSb1–x)2Te3 by composition tuning", Nature Nanotechnology 6, 705–709 (2011).

Topological insulators exhibit a bulk energy gap and spin-polarized surface states that lead to unique electronic properties, with potential applications in spintronics and quantum information processing. However, residual bulk charge carriers originating from crystal defects or environmental doping mask the contribution of surface carriers. By tuning the ratio of bismuth to antimony, this work demonstrates that the bulk carrier density can be reduced by over two orders of magnitude, while maintaining the topological insulator properties. The experimentally observed ARPES measurements are qualitatively reproduced by ab initio band structure calculations in which the linear SSB dispersion around the Γ point in all compositions confirms their topological non-triviality. As a result, a clear ambipolar gating effect in

(BixSb1–x)2Te3 nanoplate field-effect transistor devices has been observed, similar to that observed in graphene field-effect transistor devices. The manipulation of carrier type and density in topological

NNIN Annual Report p.75 March 2011-Dec 2011 insulator nanostructures demonstrated in this work paves the way for the implementation of topological insulators in nanoelectronics and spintronics.

Figure 42: Ab initio band structure calculations of Bi2Te3, (Bi0.75Sb0.25)2Te3, (Bi0.50Sb0.50)2Te3, (Bi0.25Sb0.75)2Te3 and Sb2Te3 show qualitative agreement with ARPES measurements (b, bottom row), with gapless SSB consist of linear dispersions spanning the bulk gap observed in all the compositions. The difference in EF between calculated and measured band structures reflects the carriers arising from defects and vacancies in the crystals.

4.4.3 MEMS Capacitive Accelerometer for Health Monitoring Applications Tolga Kaya, Central Michigan University Professor Tolga Kaya and his research group at Central Michigan University have been using both the computation and fabrication resources at the Michigan site of the NNIN to design and fabricate a novel, three direction MEMS capacitive accelerometer for health monitoring applications. COMSOL Multiphysics was used to study the working principle and the dynamic performance of the accelerometer. In the first step, the motion of the proof-mass was investigated by coupling the squeeze-film gas damping to the structural dynamic of the accelerometer. The modified Reynolds equation for perforated plate was implemented into COMSOL model to capture the proof-mass out-of- plane deflection. The maximum design acceleration considered was 5g in all directions.

A modal analysis was also used to find the Figure 43 :a) A 3-D model of the capacitive comb-drive fundamental modes of vibration and frequencies, in accelerometer; (b) SEM picture of the fabricated serpentine spring; (c) Profile of maximum deformation of the proof-mass and serpentine springs in z and x direction, respectively

NNIN Annual Report p.76 March 2011-Dec 2011 order to avoid resonance and identify the device range of operation. At the end, a series of three- dimensional electrostatic finite element analysis was conducted to calculate the mutual capacitance between the moving and fixed fingers when the proof-mass is subjected to an in-plane design acceleration. 4.4.4 Polymeric Nanocarriers for Local and Systemic Delivery of Drugs to the Lungs via Oral Inhalation. Sandro DaRocha, Wayne State University Professor Da Rocha’s group at Wayne State University is using the NNIN/C at Michigan resources to investigate polymeric nanocarriers such as dendrimers for local and systemic delivery of drugs to and through the lungs via oral inhalation.(fig. 43). In this study, PEGylation is a very attractive procedure, as it can be used to modulate the interaction of the carriers with the biological environment, including transport modulation and protection of the therapeutic cargo from degradation. In this Figure 44 a) Structure of PAMAM dendrimers (generation 2 and work they have used numerical simulations 3) before and after equilibration – ca. 15 ns. Bottom: Structure of G3 PAMAM dendrimer grafted with different densities of using to determine the effect of PEGylation on PED1000 the structure of dendrimer nanocarriers, with atomic-level detail. 4.4.5 Adaptable Two-Dimension Sliding Windows on NVIDIA GPUs with Runtime Compilation Nicholas Moore, Miriam Leeser and Laurie Smith King. (Winner, Best Paper Award: Symposium on Application Accelerators in High Performance Computing (SAAHPC), July 2011) [In 2009 NNIN/C embarked on an ambitious project to support high performance computing research that takes advantage of new, massively parallel computer architectures, specifically the devices known as General Purpose Graphical Processing Units, or GPGPUs or GPUs for short. NNIN/C, together with the NSF-funded Cyber-Enabled Discovery and Innovation Project at Harvard, purchased a cluster of GPU machines called “orgoglio” (see “GPU Initiative”, below). One of the principal new participants in the project is Dr. Miriam Leeser at Boston University, who is currently transitioning her code to be tested on orgoglio. This work is a sample of the groundbreaking research in the field by Dr. Leeser.] For some classes of problems, NVIDIA CUDA abstraction and hardware properties combine with problem characteristics to limit the specific problem instances that can be effectively accelerated. As a real- world example, a twodimensional correlation-based template-matching MATLAB application is considered. While this problem has a well known solution for the Figure 45: A comparison of the average per-frame common case of linear image filtering—small fixed processing times for the three implementations templates of a known size applied to a much larger image—the application considered here uses large arbitrarily sized templates, up to 156-by-116 pixels, with small search spaces containing no more than

NNIN Annual Report p.77 March 2011-Dec 2011 703 window positions per template. Our CUDA implementation approach employs template tiling and problem-specific kernel compilation to achieve speedups of up to 15 when compared to an optimized multi-threaded implementation running on a 3.33 GHz four core Intel Nehalem processor. Tiling the template enables exploiting the parallelism within the computation and shared memory usage. At the same time, problem-specific kernel compilation allows greater levels of adaptability than would otherwise be possible. 4.4.6 How Easy is it to Tear Graphene?

C. S. Ruiz-Vargas, H. L. Zhuang, P. Y. Huang, A. M. van der Zande, S. Garg, P. L. McEuen, D. A. Muller, R. G. Hennig, and J. Park, “Softened Elastic Response and Unzipping in Chemical Vapor Deposition Graphene Membranes”, Nano Letters, 11, 2259 (2011).

Graphene has proposed as a candidate material for flexible electronic devices due to both its superior mechanical properties (i.e. large Young’s modulus and high breaking strength) and its extremely high electrical conductivity. Graphene grown on copper using chemical vapor deposition (CVD) offers one Figure 46: Phase AFM image fabrication route that could lead to mass production of graphene devices. show the region before and after an indentation However, it has been noted recently that CVD graphene grown on copper measurement performed near consists of a large number of grains separated by lines of atomic defects. a grain boundary (at location indicated by blue dot). Scale This raises the question of how these grain boundaries will affect the structural bars: 150 nm strength of these CVD graphene sheets. In this work, the researchers modeled the tensile behavior of graphene sheets using the molecular dynamics code, LAMMPS. They found that grain boundaries in general reduce the strength of graphene sheets and that the presence of subnanometer voids near the grain boundaries can reduce the sheet strength even further. These simulations confirmed the results of nanoindentation studies of graphene sheets done at Cornell. The experimental work for this project was done in the clean room facilities at the Cornell Nanoscale Facility.

4.4.7 Thermal Transport in InAs Nanowires

F. Zhou, A. L. Moore, J. Bolinsson, A. Persson, L. Froberg, M. T. Pettes, H. Kong, L. Rabenberg, P. Caroff, D. A. Stewart, N. Mingo, K. A. Dick, L. Samuelson, H. Linke, and L. Shi, “Thermal conductivity

of indium arsenide nanowires with wurtzite and zinc blende phases”, Physical Review B, 83, 205416 (2011).

How do you predict the thermal conductivity of a material that doesn’t exist in nature? In its bulk form, InAs takes on a zincblende crystal structures. However, for very thin InAs nanowires, the wurtzite crystal structure is more stable. During thermal transport measurements, Li Shi’s group at the University of Texas noticed that the thermal conductivity of the wurtzite InAs nanowires was much less Figure 47 MD simulation of the effect of a than that of slightly larger zincblende InAs nanowires. However, they void on the strength of a small were not sure if this was due to the change in crystal structure or due bicrystalline graphene sheet (Panel c). MD simulation of decreased breaking strength due to shearing in the presence NNIN Annual Report of a grain boundary.: p.78 March 2011-Dec 2011 to changes in the surface properties of the nanowire.

Figure 48 Isolating the nanowires for thermal measurements requires multiple fabrication steps to achieve the proper setup. The calculated phonon dispersions for zincblende (ZB) and wurtzite (WZ) nanowires are also shown Experimental data points for ZB InAs are Analytical thermal conductivity models require information on sound velocity and the phonon dispersion of a material. This is readily available for zincblende InAs, but not for the theoretical wurtzite InAs. Using density functional perturbation theory, Derek Stewart (CNF) calculated the phonon dispersion for both the zincblende and wurtzite forms of InAs. Arden Moore, a graduate student at the University of Texas, then used the branch-specific phonon dispersion data in the Brillouin zone to construct a numerical model for thermal conductivity in wurtzite crystals. The results showed that the zincblende and wurtzite crystals have similar thermal conductivities and that the real source of the difference in thermal transport is due to the surface conditions of the nanowires. 4.4.8 Towards Organic Energy Storage

S. E. Burkhardt, S. Conte, G. G. Rodriguez-Calero, M. A. Lowe, H. Qian, W. Zhou, J. Gao, R. G. Hennig, and H. D. Abruna, “Towards organic energy storage: characterization of 2,5-bis(methylthio)thieno[3,2- b]thiophene”, Journal of Materials Chemistry, 21, 9553 (2011)

Alternative energy sources such as solar and wind hold great potential for addressing some of the future global energy requirements. However, these energy sources are inherently intermittent, which highlights the need for new energy storage materials with high energy and power densities. Conjugated conducting polymers have fast charge-discharge rates which make them very attractive for high power applications. Unfortunately these materials Figure 49: Simulation for energy storage have general low specific capacities. One route to alleviate application this problem is to functionalize these materials with pendant redox units that boost the energy density while maintaining the rapid charging and discharging rates. In this work, S.E. Burkhardt and his colleagues have used a combination of experimental and simulation approaches to study 2,5- bis(methylthio)thieno[3,2-b]thiophene. They find encouraging evidence that this redox unit could provide high energy density for electrical storage energy devices. 4.4.9 Graphane Under Pressure

X.-D. Wen, L. Hand, V. Labet, T. Yang, R. Hoffmann, N. W. Ashcroft, A. R. Organov, A. O. Lyakhov, “Graphene sheets and crystals under pressure”, Proceedings of the National Academy of Sciences, 108, 6833 (2011).

NNIN Annual Report p.79 March 2011-Dec 2011 Using an evolutionary search algorithm combined with density functional calculations, X. D. Wen and his collaborators conducted an extensive search for possible graphane structures over a wide range of pressures. Graphane is a graphene sheet that is fully saturated with hydrogen. Under normal atmospheric conditions, layers in graphitic structures are held together with weak van der Waals bonds. By varying the system pressure, these researchers were able to systematically study how the bonding interaction between the layers changed. They found five different graphane structures that had low enthalpies for a particular pressure regime. Four were also found to be more stable than benzene. Similar to diamond, all graphane structures were found to be insulating up to 300 GPa.

Figure 50: Various Graphane structures found during the evolutionary search 4.5 Progress on New Computation Initiatives 4.5.1 Virtual Vault for Interatomic Potentials In September of 2009, the National Science foundation awarded a grant to the “Knowledge-Base for Interatomic Models,” (KIM). KIM is a program to test, validate and store interatomic model potentials for use in molecular dynamics calculations, which are at the heart of many biological and chemical simulation approaches. The principal investigators, Ellad Tadmoor, University of Minnesota, James Sethna, Cornell University and Ryan Elliott, University of Minnesota, plan to work with NNIN/C to make the database, which is a major output of their research, available to the nanoscience computing community. (Fig. 51) Atomistic simulations using empirical interatomic potentials are playing an increasingly important role in realistic scientific and industrial applications in many areas including advanced material design, drug design, renewable energy, and nanotechnology. The predictive capability of thes approaches hinges on the accuracy of the interatomic model used to describe atomic interactions. Modern potentials are optimized to reproduce experimental values and electronic structure estimates for the force and energies of representative atomic configurations deemed important for the problem of interest. However, no standardized approach exists yet for comparing the accuracy of interatomic models, or Figure 51.: Virtual Vault for Interatomic Potentials Schema. estimating the likely accuracy of a given prediction. In addition, a lack of standardization in the programming interface of interatomic potentials and the lack of a

NNIN Annual Report p.80 March 2011-Dec 2011 systematic infrastructure for archiving them makes it difficult to use potentials for new applications and to reproduce published results. These limitations are preventing the field of atomistic modeling from realizing its true scientific and technological potential. The Knowledgebase of Interatomic Models (KIM) is a four-year NSF Cyber-Enabled Discovery and Innovation (CDI) program which seeks to address the limitations described above in two stages: • Development of an online infrastructure consisting of a web portal, repository and processing pipeline. • Development of a framework for evaluating the transferability and precision of interatomic models. 4.5.2 Virtual Vault for Pseudopotentials Development The CNF hosts the Virtual Vault for Pseudopotentials for the NNIN/C. The NNIN database provides the global scientific community with access to pseudopotentials used in a wide range of electronic structure codes (See http://www.nnin.org/nnin_comp_psp_vault.html .) The clearinghouse consists of a PHP-SQL database of pseudopotentials that can be accessed online, containing over 800 pseudopotential files drawn from different pseudopotential codes including Quantum Espresso, Abinit, and Qbox. Users can interface this data through an online periodic table to find information related to a particular atom. Users can also search the database based on a given element and compare available pseudopotentials based on criteria such as exchange-correlation functional, pseudopotential class (i.e. ultra-soft, norm- conserving), parent electronic structure code, and more. This database provides the first centralized resource for pseudopotentials that spans multiple electronic codes. Numerous websites in the electronic structure community now provides links to the Vault as a valuable resource. In addition, members in the community have also begun to donate their own pseudopotentials to the database. In 2011, additional search mechanisms were added to the Vault interface. Derek Stewart has also been working with Joseph Bennett (Rutgers University) to add a suite of optimized pseudopotentials to the Virtual Vault. 4.5.3 GPU Initiative The Graphical Processing Unit, highly parallel computing initiative of NNIN/C got underway in 2009 with the installation of the Orgoglio cluster. Since then, several users have made remarkable research achievements based on the use of Orgoglio. In particular, the research group of Dr. Alfredo Alexander- Katz published: “Dynamics of Polymers in Flowing Colloidal Suspensions,” Hsieh Chen and Alfredo Alexander-Katz, Physical Review Letters 107, 128301 (2011),and the research group of Dr. Miriam Leeser at Boston University has begun transitioning her code on GPU algorithms to the Orgoglio cluster (see Research Highlights, above). The cluster specifications are as follows: • Single quad-core Xeon ‘Harpertown’ processors at 3 GHz • 16 GB of EEC DDR2 800 RAM • Two Tesla C1060 GPUs (each with 4GB of RAM) • (total of 24 nodes/motherboards, 96 cores, 192 GB RAM, 48 S1070 cards). • QLogic 24-Port 9024 DDR InfiniBand networking between the nodes. The field of high performance computing has been transformed by the advent of GPU computing and the introduction of the CUDA programming language by Nvidia. On January 10-14, 2011, the Institute for Mathematics and it’s Applications (IMA) at the University of Minnesota held a major workshop entitled High Performance Computing and Emerging Architectures. NNIN/C director Michael Stopa was an invited participant and presented a poster detailing high performance computing in NNIN/C.

NNIN Annual Report p.81 March 2011-Dec 2011 4.6 Collaborative Projects 4.6.1 Defence Threat Reduction Agency Grant Award In February of 2010 the Defense Threat Reduction Agency granted an award (Contract No HDTRA1-10 1-0046) for a proposal on Coherent Molecular Profiling Using Nano-Structured Environments submitted by Dr. Alan Aspuru-Guzik in collaboration with NNIN/C director Michael Stopa and Research Scientist Semion Saykin. The project calls for the development of analytical and numerical approaches to describe interaction of analyte molecules with excitations in nanostructured environments, as well as describing the influence of the nanostructured environment on the ground state properties of molecules. As an example the researchers explore several model systems for better understanding of the physical processes involved. The models were selected to benefit from our ongoing experimental collaborations. As described by Dr. Eric Moore, Chief of Basic and Supporting Sciences for DTRA, the mission areas of DTRA are: (1) to provide a robust fundamental knowledge base for countering current and future Chemical and Biological (CB) threats through scientific discoveries leading to technological breakthrough; (2) to provide fundamental scientific understanding of CB threat agents with specific attention to information gaps or requirements pertinent to the DoD, DHS, and other Intelligence Agencies. This is accomplished through two components: the Life Sciences Branch and the Physical Sciences Branch. The Annual DTRA meeting was held in Las Vegas, NV from November 14-18, 2011 and Stopa and Saykin participated with a poster presentation on recent results on coherent molecular profiling. Aspuru-Guzik, Saykin and Stopa described a method for employing the coherent interaction between, in particular, molecules and surfaces plasmons in metal nanoparticles and surfaces (so-called “plexcitons”) to extract spectroscopic information which is unavailable in the ensemble-averaged classical limit, required to identify analytes.

Figure 52: Molecular spectroscopy in nano-environments. 4.6.2 Center for Integrated Nanotechnologies, Sandia National Laboratory Project Title: Multiscale Calculation of the Strained, Multi-band Electronic Structure of Semiconductor Nanowires: Hetero-interfaces Investigators: Michael Stopa (Harvard University) in collaboration with N. Modine (CINT) The purpose of this work is to apply the computational tools developed in previous stages of this collaboration to calculate the effects of the inhomogeneous strain at hetero-interfaces on the electronic structure in an epitaxially grown quantum wire. Specifically, within a multi-band k·p model, we calculate the variation of the band edges as well as the coupling between different angular momentum components of a band as a function of position. The structures we will consider begin with a wire with a simple interface between, for example, Si and Ge (or alloys thereof), but may also extend to more complex structures such as core-shell nanowires. The strain will be taken as input from the result of molecular dynamics calculations which give the equilibrium position of the atoms when, for instance, a compositional change along, say, the z direction is made during the growth of the wire.

NNIN Annual Report p.82 March 2011-Dec 2011 A new project, based on previous work, was begun in 2011 which combined two calculations of the strain field in an epitaxially grown nanowire: a molecular dynamics simulation with atomic resolution, on the one hand, and a continuum elasticity model calculation minimizing the elastic free enrgy, on the other hand. 4.6.3 Thermal Transport in Crystalline and Disordered Materials Project Title: Collaborative Research: Ab-Initio Computation of Thermal Transport in Crystalline and Disordered Materials: Investigators: Derek Stewart (Cornell University) and Prof. David Broido (Boston College) In 2011, Dr. Derek Stewart received a National Science Foundation research grant “Collaborative Research: Ab Initio Computation of Phonon Thermal Transport in Crystalline and Disordered Material” (CBET-1066406). This grant will fund a collaborative effort between Dr. Stewart at Cornell and Prof. David Broido at Boston College on first principles thermal transport in low thermal conductivity materials, such as thermoelectrics. Accurate theoretical modeling of the lattice thermal conductivity is essential to numerous fields including microelectronics cooling, thermoelectrics, and even Figure 53: Predicted thermal conductivity in SiGe alloys with embedded Si or Ge nanoparticles based on planetary science. The Cornell site will focus on T-matrix and Born approaches. The thermal calculating ab initio harmonic and, where required, conductivity reaches a minimum for nanoparticles with a anharmonic interatomic force constants (IFCs) for the 10 nm diameter. (A. Kundu et al, Phys. Rev. B, 84. 125426 (2011) materials and structures to be investigated. These calculations will be based on density functional perturbation theory. The IFCs are required inputs for phonon dispersions, phonon density of states, and phonon thermal transport calculations from which the lattice thermal conductivity is obtained. The materials to be studied in this project include lead chalcogenides, I-V-VI2 semiconductors, and nanoparticle-in-alloy-structures. The first principles approach has already demonstrated excellent agreement with measured high thermal conductivities of group IV semiconductors. The materials to be studied in this project are unified by their exceptionally low thermal conductivities and therefore provide an excellent test of the robustness of the theory.The tools developed through this grant will be made available through the NNIN and tutorials on their use will be featured in future NNIN/C workshops. 4.7 Workshops and Training Activities The education activities of the NNIN/C in 2011-2012 included numerous workshops and training classes organized at various sites. These events are designed to help eliminate the learning curve associated with simulation approaches and also encourage greater interaction between experimental and simulation groups. 4.7.1 NNIN/C Role in Training and Courses at NNIN sites Stanford: Training classes with weekly discussions meetings at Stanford were geared toward the education of novice users on the applications of various modeling tools., These classes with approximately 10 participants were specially designed to engage the local and external experimental community to use simulation in conjunction with lab work. Basic and advance topics to study novel material properties were adressed to help them improve device performance and fabrication. Cornell: During the 2011 Cornell Spring semester, Derek Stewart worked with Prof. Richard Hennig (MSE, Cornell) on a simulation module for a Solid State Chemistry course (CHEM 6070). Approximately 25 students participants in this modules and students used the CNF cluster during tutorial sessions.

NNIN Annual Report p.83 March 2011-Dec 2011 4.7.2 Advanced Modeling and Simulation of Micro/Nano Electro Mechanical Systems (MEMS/NEMS) and Nano/Micro-fluidic Devices, University of Michigan: The Symposium brought together leading researchers to review recent progress and latest Figure 54 :Advanced Modeling and Simulation of Micro/Nano Electro Mechanical Systems and Nano/Micro- developments and review future challenges in the fluidic Devices- April 2011 NNIN/C Workshop Attendees at field. The NNIN/C symposium was a success with 50 Michigan. attendees from 15 institutions (fig. 54). The attendees contributed freely in discussions and remained engaged throughout the duration of the symposium. It is hoped that the attendees will go on to share their new learning with colleagues at their institution.

4.7.3 NNIN/C Workshop: ENCON1 Synergy Between Experiment and Computation in Energy – Looking to 2030 In January of 2012, NNIN/C held a major workshop at Harvard University on the synergy between experiment and computation in research related to energy. According to the program for the workshop: Society’s ceaseless demand for clean, renewable energy resources, as populations grow and as poorer nations undergo increased industrialization, will remain one of the prime motivating forces of research for the foreseeable future. Much of this research relies on both experimental and computational studies, and the synergy between them. In addition, many of the current studies focus on physical effects at the nanoscale or at multiple length scales including the nanoscale. The workshop, which featured 18 distinguished invited speakers and over 120 registered participants overall, focused on four main research thrusts: organic photovoltaics, self-assembly, catalysis and fuel cells. These sessions were each organized by experts in those areas. Organic photovoltaics: (Organized by Tim Kaxiras, Harvard, and Ala Aspuru-Guzik, Harvard) Organic and nanoparticle/organic photovoltaic solar cells have the promise of a low manufacturing cost. At this moment, these solar cells have relatively low efficiencies. This section of the conference will concentrate on the physical mechanisms of solar energy absorption in these materials to understand them at the microscopic level and learn about possible strategies for improving their efficiency, Figure 55: Daniel Nocera describes the “Artificial Leaf” at ENCON1: Synergy Between Experiment thereby making them cost-effective. The goal is to and Computation in Energy – Looking to 2030. understand and predict the effects of material morphology on the exciton, electron and hole-transport properties of the device. Speakers: Konstantinos Fostiropoulos (Helmholtz-Zentrum Berlin ), Shane Yost (MIT MSE), Alan Aspuru-Guzik (Harvard), Tim Kaxiras (Harvard). Self-organization: (Organized by Alfredo Alexander-Katz, MIT) Self assembly, the process in which molecules self-organize in a particular morphology, can play a decisive role in many energy applications where order at a particular length scale is desired. In theis conference we will explore synergies between

NNIN Annual Report p.84 March 2011-Dec 2011 experiment and simulation in this area, and discuss the challenges and opportunities that remain ahead. Speakers: Bradley Olsen (MIT ChemE), Juan Jose de Pablo (Wisconsin ChemE) , Mark Bathe (MIT) Alfredo Alexander-Katz (MIT). Catalysis: (Organized by Ted Betley, Harvard) Inorganic chemistry can have an impact on all phases of the energy landscape: catalysis, conversion, and storage. This portion of the colloquium will discuss the frontier of all three of these areas showcasing new design strategies for homogeneous and heterogeneous, molecular and solid-state catalysts. Finally, new design strategies for extended solids will be described for energy storage and novel catalytic materials.Speakers: Daniel G. Nocera (MIT), Matthew Kanan, (Stanford), Bart Bartlett, (Michigan), Mircea Dinca (MIT), Ted Betley (Harvard). Fuel Cells: (Organized by Sergio Granados-Focile, Clark University) The performance and durability challenges for materials used in fuel cells will be addressed with a particular focused on the catalyst and ion-transporting layers. Work on developing materials for traditional water-mediated and water-free ion transport will be discussed emphasizing the benefits of synergy between computational and experimental collaborations. Speakers: Yu Morimoto (Toyota Central R&D Labs., Inc., Electrochemistry Div.), Mark Mathias (General Motors Research & Development), Peter N. Pintauro (Vanderbilt University), Thomas Zawodzinski (UT-Knoxville and ORNL), Sergio Granados-Focil (Clark). 4.7.4 EM.CUBE workshop at Michigan EMAG Technologies presented its EM.CUBE suite of electromagnetic modeling and RF design tools at the NNIN/C computation site at Michigan. This workshop introduced EM.CUBE’s modular simulation environment for solving a wide range of electromagnetic radiation, coupling, scattering, propagation and compatibility problems with many applications in communication and radar systems, electronic sensors, high speed digital circuits, biological systems, remote sensing, electronic warfare. This hands-on workshop had 22 attendees from 3 different institutions (Fig.56). Figure 56: NNIN/C@ Michigan EM.CUBE Workshop 4.7.5 Pan-American Advanced Studies Workshop on Computational Material Science for Energy Generation and Conversion Dr. Derek Stewart received a $100K National Science Foundation grant (#1123536) to host a Pan- American Advanced Studies Institute on Computational Materials Science for Energy Generation and Conversion (CMS4E) in Santiago, Chile from January 8-22nd. Additional funding was also obtained from the NNIN, Office of Global Naval Research, the International Center for Materials Research, and two Cornell centers (CCMR and EMC2). This two week school brought together over 40 graduate students and post-doctoral researchers from the United States (12 states), Chile, Argentina, Mexico, Colombia, and Brazil. The workshop provided lectures in first principles approaches, molecular dynamics, optical techniques, and finite element approaches. Advanced topics included piezoelectrics for energy harvesting, lithium battery design, and engineering thermal properties of materials for thermoelectrics. In addition, students participated in daily hands-on sessions to gain experience in various simulation approaches. Computational resources on the Texas supercomputer, Ranger, were made possible through a NSF XSede computing time grant. Lectures and tutorials developed through this course will be made available on the CNF and NNIN websites

NNIN Annual Report p.85 March 2011-Dec 2011 Pan American Advanced Studies Institute “Computational Material Science for Energy Generation and Conversion”, Pontifica Universidad de Chile, Jan. 9th -20th, 2012, Santiago, Chile http://www.cnf.cornell.edu/cnf_pasi2012.html

Figure 57: Participants at the 2012 PASI-CMS4E Workshop

4.7.6 Modeling and Simulation of Nano/Microsystems Contest The objective of this contest was to provide publicity and promotional support to new developments, recent progress, and advances in the modeling and simulation of Micro/Nanosystems. The emphasis was on current challenges in understanding of the multi-physics/multi-scale phenomena that govern such systems functionality. Twenty researchers have uploaded the requirement materials (two-page abstract, poster and animations) for the contest. The top three winners of 2011 contest were selected and awarded by NNIN/C at Michigan.

Figure 58 Modeling and simulation of nano/microsystems contest at Michigan-

NNIN Annual Report p.86 March 2011-Dec 2011 5.0 NNIN GeoSciences Initiative

5.1 Introduction: Several reports produced by NSF-sponsored committees have identified sensors, sensing materials, and sensing systems as one of the major needs for ocean, atmosphere, earth and space observatories. Over the past decade, there has been significant advances in the development of nano and micro devices and sensing systems for automotive, industrial, medical, and environmental applications. Yet, these advances have not permeated the geoscience community. One of the goals of the NNIN-Geo program is to bring together researchers from these two communities and help provide enabling technological solutions to long-standing problems in geosciences. NNIN’s focused activity in geosciences (NNIN-Geo) was initiated in 2009 under the leadership of two sites: University of Michigan and University of Washington. The first step was to hire a domain expert with significant experience in geosciences. This position was funded for the University of Michigan and filled in September 2010 with the recruitment of Dr. Hélène Craigg. The primary goals of the NNIN-Geo program are: 1. to reach out to the geosciences community, raise awareness of NNIN, and disseminate information about the network’s tools, capabilities and researchers; 2. to promote research collaborations between select geo and micro/nano researchers with the aim of generating success stories in nano-enabled geosciences; 3. to disseminate results from these collaborations to the broader geo community in order to encourage more researchers to consider using nanotechnologies and NNIN capabilities; 4. to expand the NNIN user base by training users from the geo community on network tools. 5.2 Tasks and Accomplishments NNIN-Geo intends to accomplish the above goals within five years. A summary of progress for the first three years is provided below. 5.2.1 Task 1: Outreach to Geo Community Over the past year, NNIN-Geo conducted a number of outreach activities and participated in several meetings and events. • The new NNIN@Michigan website (http://www.lnf.umich.edu/nnin) is now live and includes a geosciences section containing information on NNIN capabilities, examples of supported projects, and a list of geosciences and environmental sciences funding opportunities. • A comprehensive tri-fold brochure on NNIN and nanotechnology as an enabling tool for geosciences was prepared and printed. This brochure is now the main promotional NNIN-Geo material. • Two meetings focusing on freshwater systems were organized in collaboration with U. Michigan: the Sustainable Waters Initiative Research Meeting (Mars 18, 2011 – Ann Arbor MI) and the MI H2Objective Conference: Research Shaping Michigan’s Water Future (September 29-30, 2011 - Detroit, MI). Dr. Craigg attended both meetings and held a booth during the MI H2Objective Conference. Participation in these meetings is essential for networking and a better understanding of sensor needs by freshwater scientists. A major outcome was the organization of a brainstorming session on environmental sensors for the Great Lake community at U. Michigan (December 12, 2011). The meeting was held between NNIN-Geo (Khalil Najafi and Helene Craigg), Yogesh Gianchandani (Wireless Integrated MicroSensing and Systems Institute, U. Michigan) and 8 researchers from different institutions such as the Cooperative Institute for Limnology & Ecosystems Research, and the NOAA-Great Lake Environmental Research

NNIN Annual Report p.87 March 2011-Dec 2011 Laboratory and the Great Lakes Observing System. The Great Lake community has expressed a strong desire to collaborate. Therefore, this introductory meeting will be followed in 2012 by more extensive meetings in order to initiate concrete projects A booth staffed by U. Michigan and U. Washington personnel showcased NNIN at the American Geophysical Union 2011 Fall meeting (AGU 2011; December 4-10, 2011 - San Francisco, CA) (Figure 1). Informative material such as Figure 59: NNIN Booth at AGU conference. flyers emphasizing nanotechnologies and sensors suitable for geosciences applications and the tri-fold brochure were distributed. About 70 new contacts were established with geoscientists of all disciplines. NNIN will also have a booth at the Ocean Sciences Meeting 2012 (February 20-24, 2012; Salt Lake City, UT). During this meeting, a two-hour workshop with break out sessions on nanotechnology in geosciences will be held. The geosciences curriculum for undergraduate students does not currently include a significant amount of material related to nanotechnology. Prof. David Mogk from the U. Montana and the NSF program “On the Cutting Edge: for the professional development for geosciences faculty” is interested in developing educational resources in collaboration with NNIN. As a first step, we are discussing a workshop on how to teach nanotechnology for geo undergraduate students at the Goldschmidt conference in 2012 (Montreal, Canada). Meanwhile, digital resources are being prepared for the “On the Cutting Edge” website.

5.2.2. Tasks 2 & 3: Initiate Collaborative Projects and Disseminate Information: 5.2.2.1 Update on the “Nano-enabled Sensing Microsystems for Geo Sciences” workshop (Feb 2010, U. of Michigan) In order to develop a geo community user base, we have been working at initiating projects involving researchers from both the geo and micro/nano communities. A first step was taken in February 2010 with a U. Michigan workshop entitled “Nano-enabled Sensing Microsystems for Geo Sciences.” At the conclusion of the workshop, five white papers were written and three were later converted to formal proposals. Two proposals have been funded by NSF and NOAA. A third was submitted as a collaborative proposal to NSF OTIC program but was not funded. Here is the update on these projects: Sensors for Multi-functional and Autonomous Analysis of Geofluids: A New Approach to the Design and Performance of Chemical Sensors in Extreme Environments Investigators: Yogesh Gianchandani (U. Michigan) and Bill Seyfried and Kang Ding (U. Minnesota) The project focuses on hydrothermal vents at mid-ocean ridges. Even though these systems have been studied for a long time, the lack of performing and reliable chemical sensors limits the quantitative studies. The proposal targets the improvement of chemical components measurement associated with hydrothermal vent fluids using high performance miniaturized sensor assembly and ultimately the development of on-board signal processing. The Michigan team has visited the Minnesota Geosciences team. They jointly have revised MEMS design concept based on Geosciences goal and properties of structural materials. The sensor design is finished. The

NNIN Annual Report p.88 March 2011-Dec 2011 fabrication of customized YSZ disks, MacorR ceramic backing, and other components are completed. The device integration process using microfabrication-based techniques is done. Preliminary test results obtained by the Michigan team suggest that the sensor can provide pH measurement of a solution in a regular laboratory settings, indicating the validity of the sensor design. A project review meeting between the Michigan team and the Minnesota Geosciences team was held at Michigan, and further evaluation of the sensor has been planned under extreme conditions and/or real deep sea settings. The work is submitted to a conference for publication by the whole team. EAGER Proposal, starting date: 8/1/10. Total Funding: $101,805, which is split roughly evenly. IDC has been waived at U. Minnesota, and reduced to 11% at U. Michigan. Raman-based Barcoding for the Identification of Toxic Marine Pathogens and Phytoplankton Investigators: Qiuming Yu (U. Washington), Vera L. Trainer and Mark S. Strom (West Coast Center for Oceans and Human Health), Mark L. Wells (U. Maine) A Raman-based barcoding technique for the identification of toxic marine pathogens and phytoplankton was developed using a unique quasi-3D plasmonic nanostructure arrays that can be specifically tuned to enhance the detection of bacteria or small molecules via surface-enhanced Raman spectroscopy (SERS). The investigators have demonstrated that the biochemical information embedded in microorganisms’ cell walls can be used for the rapid identification of pathogens. Seven strains of the marine pathogen vibrio parahaemolyticus were used to demonstrate the power of the approach. The high sensitivity and reproducibility provided by the unique SERS-active substrates enabled the construction of a color SERS barcoding for each strain. Unknown samples and mixtures of two out of seven strains were quickly identified by comparing SERS barcoding patterns. Furthermore, strains belonging to the same genomic group exhibited common characteristic peaks, indicating correlation of genomic and phenotypic variation. Two NNIN REU students contributed to the project. Two proposals have been submitted USDA and DTRA, two papers have been published and one manuscript is in preparation (see section 5.2.2.3).

Proposal funded by NOAA Oceans and Human Health Initiative (OHHI 2010), starting date: 8/1/10. A Microfabricated Protein-Based Array for Electrochemical Detection of Bioavailable Metals in Aquatic Environments Investigators: François Baneyx (U. Washington); Thomas Dichristina (GeorgiaTech); Karen Orcutt (U. Southern Mississippi); Becky Peterson (U. Michigan); Martial Taillefert (GeorgiaTech) The goal of this project is to design, build and field-test a revolutionary sensor for multiplex, real- time and on-demand quantification of bioavailable metals in Figure 60: Array of Au/Hg aquatic environments. This transformative project will be working microelectrodes. conducted by an interdisciplinary team with synergistic expertise in molecular biology (Dichristina), protein and molecular engineering (Baneyx), nanosensor design (Orcutt), analytical electrochemistry (Taillefert) and microfabrication (Peterson). The sensor platform will harness the metal-selective transport properties of biological efflux pumps and the light-activated proton pumping power of bacteriorhodopsin to import and concentrate specific metal cations from the aquatic environment and into a microfabricated assay chamber. It will rely on built-in microelectrodes for high-sensitivity voltammetric quantification of metal ions. An NSF-OTIC proposal was submitted in 2010 ($3M total request) but the project was not

NNIN Annual Report p.89 March 2011-Dec 2011 funded. The team is planning to resubmit a series of smaller proposals. H. Craigg, B. Peteron and M. Taillefert have worked on the sensing part of the device. Arrays of Au/Hg working microelectrodes were designed and fabricated at U. Michigan (Fig 2) and electroplated and tested by M. Taillefert at Geogia Tech. A NNIN REU student contributed to the project. Microfluidic Chamber of Microbe Culture has been identified as a fourth project and is in its early stages of data gathering Inverstigators: Euisik Yoon (U. Michigan); Clara Chan (U. Delaware); Peter Hesketh (GeorgiaTech) Only an extremely small fraction of environmental microbes have been studied so far due to challenging growth conditions. Microfluidic devices appear to offer new opportunities for microbe cultures and study. Prof. Euisik Yoon shipped samples of his microfluidic chips to Prof. Clara Chan for initial testing of microbe culture and viability. Prof. Yoon was invited by Prof. Chan to give a talk at the Delaware Biotechnology Institute (DBI) seminar series in September and talked about his platform technologies with several researchers. We hope to further promote this collaboration and encourage the parties involved to explore funding opportunities. Discussions on NSF Science and Technology Center (STC) One of the outcomes of the February 2010 Workshop at the U. Michigan was a discussion between Professors Mark Wells (U. of Maine), Khalil Najafi (U. Michigan), and François Baneyx (U. Washington) about the possibility of submitting a NSF STC proposal on the theme of nano-enabled aquatic sciences with U. Maine as lead institution. Early 2011, Ana Barros (Duke U.) and Katherine McMahon (Wisconsin U.) were brought on board as hydrological cycle expert and freshwater microbiology specialist, respectively. Annette deCharon (COSEE-OS director, U. Maine) and David Mogk (co-PI of the NSF “On the Cutting Edge” program, Montana State U.) agreed to lead the education and outreach section of the STC. The research thrusts focused on the study of physiological phenomena in freshwater and oceans across spatial and temporal scales using microsensors. Although the discussions were very productive, we came to the conclusion that, in order to demonstrate the viability of an compelling STC, we first need to show the potential success of nanotechnologies as enabler for aquatic sciences. We have decided to submit the STC preproposal at the next NSF call. Meanwhile, we will keep working on developing smaller individual research projects as step stones for a more compelling STC research thrusts. 5.2.2.2 Highlighted Collaborative Projects and Areas for Development A number of geoscientists are using the capabilites offered by the 14 NNIN sites (see section 5.2.3). Highlight of geoscience projects conducted at U. Michigan and U. Washington are provided below. Analysis of Cometary Material Investigator: Don Brownlee (Astronomy Department, U. Washington) In 2006, the first direct samples of cometary material were brought back to earth by the NASA Stardust spacecraft. Comets are among the most primitive bodies in the solar system and they preserve records of chemical processes that occurred during the formation of our sun and planets. The general morphology and elemental/mineral composition of the particles have been determined in-part by back-scatter SEM and Energy Dispersive X-ray Spectroscopy (EDS) at U. Washington. Data from these analyses are essential to understand the formation of solar systems, the interstellar distribution of elements and compounds, and the “life cycle” of comets. Mineralogical samples preparation Investigator: Pamela Burnely (Department of Geoscience, U. Nevada Las Vegas)

NNIN Annual Report p.90 March 2011-Dec 2011 Diamond Anvil Cells are high-pressure devices able to reproduce the pressure and temperature conditions of the Earth mantle in a small pressure chamber (typically 400 µm diameter or less). To conduct a new type of deformation experiments, samples preparation technique suitable for DAC needs to be developed. The adaptation of the high precision dicing saw located at the U. Michigan is under way in order to cut alumina and olivine samples to the desired size and shape. Investigator: Jane Niu (Department of Earth and Environmental Sciences, U. Michigan) The study of uranium reduction precipitation features on pyrite by in-situ fluid tapping AFM requires a mirror-finish polish surface. Natural pyrite samples will easily develop an oxidation layer that alters the sample surface. Nanofabrication polishing techniques such as chemical mechanical polishing technique are an efficient way to remove this layer and provide the surface finishes needed for this study. A specific process to polish pyrite samples is under development. Oxygen sensor to study coral bleaching Investigator: Mark L. Wells (School of Marine Sciences, U. Maine) Coral bleaching is a common issue of tropical reefs. Stress is suspected to be one of the triggers. A primary indicator of stress is diminished photosynthesis of the symbiotic algae; the main food source for many corals. One approach to assess the influence of stress is to measure changes in oxygen production/release at the coral/water interface. M. Wells proposes to create and test a compact sensing unit that can be deployed in reef systems for integrated assessment of photosynthetic production, thereby providing quantitative assessment of the timing and degree of coral stress, using established fiberoptic sensing technology, combined with NNIN inspired engineering. A proposal will be submitted to the NSF-Ocean Technology and Interdisciplinary Coordination program this year. Quantified ostracod surface morphology is a measure of ontogenetic change Investigators: Janice Pappas and Daniel Miller (Museum of Paleontology, U. Michigan) The surface morphology of ostracods can reveal important information about sex, ontogenetic stage and past salinity and climatic changes. Laser interferometry technique will be used for quantified surface metrology study. The result will provide a relationship between carapace surface roughness and ontogenetic parameters as well as a searchable database and digital library. The method is innovative of paleontological studies and will provide new data not accessible with traditional observation method. Two researchers have started working on the project. They have tested the laser interferometer microscope at U. Michigan to collect data and a proposal was submitted 01/16/11 to the NSF paleontology directorate, sedimentary geology and paleobiology program. Total funding asked: $296,678 for three years. The proposal was not funded and will be resubmitted. Experimental investigations of carbon in Earth’s core Investigator: Jie Li (Department of Earth and Environmental Sciences, U. Michigan)

The global carbon cycle may involve iron carbide (Fe3C or Fe7C3) as a dominant component of the inner core, although experimental data on the phase relation of the Fe-C binary system are limited

to 70 GPa. Sound velocity data are only available for Fe3C, under conditions up to 68 GPa at 300 K

and up to 47 GPa at high temperatures. Density measurements on Fe3C and Fe7C3 have reached ~ 200 GPa in pressure, although limited to 300 K in temperature. The investigator proposes to extend the data coverage into the core pressure regime and up to 2000 K. The new data will help understanding the effect of carbon on the melting behavior, density and sound velocities of iron under core conditions, thus enabling us to conduct stringent test of the carbon-rich inner core

NNIN Annual Report p.91 March 2011-Dec 2011 scenarios. Nanofabrication and analyzing techniques will be used to prepare the micro size samples before and after multi-anvil and diamond anvil cell experiments. The techniques will include high-precision dicing, focus ion beam, electron probe analysis, and patterning. A proposal was submitted 01/06/12 to the NSF Division of Earth Sciences, Petrology/Geochemistry program. Total funding asked: $482,673 for three years 5.2.2.3 Disseminate research results Publications “Understanding the Effects of Dielectric Medium, Substrate, and Depth on Electric Fields and SERS of Quasi-3D Plasmonic Nanostructures”, Jiajie Xu, Pavel Kvasnička, Matthew Idso, Roger W. Jordan, Heng Gong , Jiří Homola and Qiuming Yu, Optics Express, 19, 20493, (2011). “Light Transmission and Surface-enhanced Raman Scattering of Quasi-3D Plasmonic Nanostructure Arrays with Deep and Shallow Fabry-Pérot Nanocavities”, Jiajie Xu, Phillip Guan, Pavel Kvasnička, Heng Gong, Jiří Homola, and Qiuming Yu, J. Phys. Chem. C. 115, 10996 (2011). “In-situ Strain-level Identification of Vibrio Parahaemolyticus Based on Biochemical Information Embedded in Cell Walls Using SERS”, Jiajie Xu, Jeff W. Turner, Matthew Idso, Stanley V. Biryukov, Laurel Rognstad, Heng Gong, Mark Wells, Vera Trainer, Mark S. Strom, and Qiuming Yu, PNAS, to be submitted (2012). Conferences A Chemical Detector for Gas Chromatography Using Pulsed Discharge Emission Spectroscopy on a Microchip: Xin Luo; Weibin Zhu; Bhaskar Mitra; Jing Liu; Thomas Liu; Xudong Fan; Yogesh Gianchandani. Paper presented at the American Geophysical Union (AGU) 2011 Fall meeting in the session of “Micro/Nano Sensing Technology for Extreme Environments.” 5.2.3 Task 4: Geosciences User Expansion at NNIN Across the network, more than 140 users who listed their technical field and/or affiliation as “Geosciences and Environmental Sciences” have been active in 2011. Figure 3 shows the Figure 61: Current geosciences and environmental science users (a total of 140 geo users from 8 NNIN sites) by technical category. distribution of these users according to nanotechnology needs. We believe that our geo activities during the past year have been very effective and expect that users will grow in number as the activities listed above bear fruit.

NNIN Annual Report p.92 March 2011-Dec 2011 6.0 Society and Ethical Implications of Nanotechnology

6.1 Vision and Goals The Societal and Ethical Issues (SEI) component of NNIN seeks to increase national capacity for exploring the societal and ethical issues associated with nanotechnology. A particularly important part of this effort is to increase the awareness of SEI within the large NNIN user community. The NNIN SEI effort acts as a resource for education and information for our user community. As the largest single group of nanotechnology researchers in the world, NNIN has both a unique opportunity and a unique obligation to assure that its users have full awareness of the societal implications of their work and their associated ethical obligations. To accomplish this goal, the SEI component has developed an infrastructure for conducting research and disseminating information about SEI. That infrastructure serves both the NNIN and the broader community interested in nanotechnology. Since its renewal, NNIN has placed particular emphasis on making the NNIN user base available as a research resource to social scientists for surveys and interviews, as well as internal educational activites for the NNIN user base.

6.2 SEI Activities Figure 62: Rachel Brockhage (middle row, right) participated as a SEI REU intern at Cornell and Nina Hwanng (top 6.2.1. NNIN SEI REU Participation: row, center) participated at University of Two NNIN REU students worked on SEI related projects during Colorado-Boulder. the summer of 2011 (Fig. 62).. Ms. Nina Hwanng, a chemistry major from Rice University, worked at the University of Colorado- Boulder site and examined the Ethical, Societal, and Legal Implications of Nanotechnology. Specifically, working with Dr. Carl Mitcham and mentorship of Lupita Montoya, Ms. Hwanng conducted a comparative study of how three countries – The Netherlands, United State, and China – historically addressed the regulation of new technologies. The final report “looks at past examples because history shapes a culture and creates different standards for what is or is not ethical. Other important comparisons include how legislation, education of the public, and safety of nanomaterials are addressed by each country. Cornell University also hosted an REU student during the summer of 2011, Ms. Rachel Brockhage, a biology major from Grove City College (Pennsylvania). As an SEI REU intern, Rachel assisted Dr. Katherine McComas and graduate student mentor Chris Clarke with an online survey of NNIN users about their views on the role funding sources and conflicts of interest (COI) play in their research. This survey was in follow-up to a 2011 article Dr. McComas published in Science and Engineering Ethics. The 2011 survey investigated:: • Overall views of NNIN users on these two issues (e.g., the extent they are seen as problematic in their field of nanotechology research); • Reactions to hypothetical scenarios about how funding sources and COI could potentially influence when, where, and how nanotechnology scholars conduct, published, and share their research;

NNIN Annual Report p.93 March 2011-Dec 2011 • Intentions to recognize and respond to COI in one’s own research; • Who is seen as resonsible for doing so (i.e., oneself, one’s supervisor, etc). • Perceived normative influence on such behavior (i.e., the extent one believes that colleagues/co- workers expect one to recognize and respond to COI in one’s research). Ms. Brockhage assisted with the project in a number of ways, including developing survey questions; conducting data analysis; and helping draft a journal manuscript, which will be submitted for publication in early 2012. In addition to the survey, Ms. Brockhage also worked with Dr. Robert McGinn (Stanford), McComas, and Clarke to develop and pilot test an REU SEI Survey that can be used annually at the REU Convocation to evaluate the SEI learning that is occuring via NNIN’s REU program. 6.2.2 NNIN SEI Brochure: To increase the visibility of the SEI activities at NNIN, we produced a brochure for dissemination at conferences, meetings, and other appropriate venues. 6.2.3 SEI Orientation “Train the Trainer” Workshops for NNIN Labs: NNIN has a user base of well over 5000 users each year and trains over 2000 new users each year. Early on, it was identified that a need was to build the capacity of each of the NNIN sites to conduct an interactive SEI orientation. Following up the first two “Train the Trainer” workshops (at Cornell in January 2010 and Washington University-St. Louis in October 2010, we conducted a third meeting for the SEI Orientation leaders or their representatives. To both highlight the work we’re doing at NNIN and interact with the Figure 63: NNIN Participates and Helps broader SEI community, the workshop coincided with the Sponsor First Congress on Teaching Societal and Ethical Implications of Research First “Congress on Teaching Social and Ethical Implications of Research,” that took place in Phoenix, AZ, on Arizona State University’s campus from November 10- 11, 2011. In addition to attending two days of talks on SEI research, education, and outreach, representatives from 12 sites participated and presented in a NNIN Poster Session highlighting how each NNIN lab targets their ethics training for their diverse users. The posters were well received by the rest of the Congress and sparked new ideas and discussion during our business meeting.

NNIN Annual Report p.94 March 2011-Dec 2011

Figure 64: NNIN Poster Session at SEI Congress and Business Meeting.

6.2.4 SEI Orientation Web Module We are working with Cornell Information Technologies (CIT) to produce an interactive web module version of the SEI PowerPoint for use at all 14 NNIN facilities. The web module will not only serve as a valuable resource for all the sites (especially those that do not directly specialize in SEI research) but also provide the foundation for additional modules targeted to continuing facility users, such as SEI “refresher” training opportunities. We expect to have a draft version available by early 2012. 6.2.5 SEI Featured Ethical Column: In April 2011, the NNIN website featured its first Ethical Column, written by Dr. Robert McGinn. The intent is for the column to spark interest and discussion with the broader SEI community. See http://sei.nnin.org/sei_featured_question.html. 6.2.6 Additional, Ongoing Activities: • Promoted the visibility of NNIN as a site for SEI research on nanotechnology via web sites, list serves, conferences, publications. • Advertised the SEI Research “Seed” and Travel grants • Maintained open and frequent communication between SEI contacts at NNIN sites to facilitate SEI research, address any challenges, and discover any opportunities for network collaboration. • Maintained the SEI website as a key destination for current research and conference alerts. Also,

NNIN Annual Report p.95 March 2011-Dec 2011 looking into the use of Ethics Core as a way to increase exposure to NNIN SEI efforts. • Exposed graduate students, tomorrow’s leaders, to societal and ethical questions related to Third World contexts through multi-day field experience during the international Winter Graduate School. • Presented research at academic and professional conferences. 6.2.7 SEI Publications and Presentations from NNIN SEI Princpals • Publications

• Brainard, S., Allen, and Savath. Factors and perspectives influencing nanotechnology career development: Comparison of male and female academic nanoscientists Article submitted and accepted for review in the Journal of Engineering Education. • McComas, K. (2011). Researcher views about funding sources and conflicts of interest in nanotechnology. Science and Engineering Ethics (online version available Feb. 19, 2011). • McComas, K. A., & Besley, J. C. (2011) Fairness and nanotechnology concern. Risk Analysis, 31, 1749-1761. • McGinn, R. (2011). What Makes Safety In the Nanotech Lab an ‘Ethical Issue’? Retrieved January 2, 2012, from http://sei.nnin.org/sei_featured_question.html. • Thursby, J., & Thursby, M. (2011). University-industry linkages in nanotechnology and biotechnology: Evidence on collaborative patterns for new methods of inventing. Journal of Technology Transfer, 36, 605-623.

• Presentations • Brainard, S. (2011, November). Career Pathways of Female and Male Nanoscientists. Presented at S.Net 2011, Tempe, AZ • McComas, K., & Healy, N. (2011, June). Incorporating societal and ethical issues of nanotechnology into an integrated user network – Results from the National Nanotechnology Infrastructure Network. Paper presented at the American Society for Engineering Education Annual Conference and Exposition, Vancouver, BC, Canada. • McGinn, R. (2011, February 25). “Ethics and Nanotechnology” at the Ethics Workshop, organized by the Center for Probing the Nanoscale, Stanford University. • Thursby, J., & Thursby, M. (2011). “University-industry linkages in nanotechnology and biotechnology: Evidence on collaborative patterns for new methods of inventing,” Rise of Nanotechnology: Implications for the Economy, Society, and the Environment, Harvard University, Cambridge, MA., May 2011.

• Other Activities:

• Brainard: Funded by NSF, Center for Workforce Development held a Nano and Gender Workshop at AAAS in Washington DC. The workshop brought together leading national researchers in the social sciences and nanosciences to provide direction to the NSF on how nanotechnology can benefit from the increased participation of women faculty. See http://www.aaas.org/news/releases/2011/0610women_nanotech.shtml

o Monograph summarizing the results and recommendations from the Nano and Gender Workshop published and disseminated nationally.

o Nature Alerts published a brief summary of the Nano and Gender Workshop and Nature Journal is planning on publishing an article in the next edition. See http://www.nature.com/naturejobs/science/articles/10.1038/nj7353-669b

NNIN Annual Report p.96 March 2011-Dec 2011 • Thursby: “We are currently working on a project with Karin Hoisl of Ludwig Maximillian University and Dietmar Harhoff on citation patterns in nanotechnology.”

• McGinn: Assisted with the development and piloting of first REU SEI survey at the summer 2011 NNIN REU Convocation at Georgia Tech. Based on the pilot, the survey will be revised in time for next year’s NNIN REU Convocation.

NNIN Annual Report p.97 March 2011-Dec 2011 7.0 Site reports

7.1 Arizona State University Site Report 7.1.1 Site Overview The ASU site is one of three new schools that joined the NNIN in March 2009. The facility is operated as the ASU NanoFab by the Center for Solid State Electronics Research, and maintains ~20,000 sq. ft. of laboratory and office space, including a 4,000 sq. ft, class-100 cleanroom. The technical focus of the ASU NanoFab within the NNIN is the interface between organic and inorganic materials. The facility also manages a general purpose semiconductor and MEMS processing capability. The NanoFab has a full time staff of six process and equipment engineers, one NNIN domain expert, and a part-time education and outreach coordinator. 7.1.2 Project Highlights The number of users at ASU continues to grow. For the period March to December 2011 we have a total of 101 users from ASU, an increase of six over the same period last year. To date we have attracted two additional external users bringing the total to 34 through December 2011. The largest growth in external use is from small business users, comprising 21 researchers from 16 companies. A summary of a few of the external projects is presented below. Plasma Lithography for Cell Networks Formation: Junkin and Wong, University of Arizona; A versatile plasma lithography technique has been developed to generate stable surface patterns for guiding cellular attachment. The technique has been applied to create cell networks including those that mimic natural tissues and has been used for studying several, distinct cell types. In particular, the method has been applied to form diverse networks with different cell types for Figure 65: NNIN Participates and transformative investigations in collective cell migration, intercellular Helps Sponsor First Congress on signaling, tissue formation, and the behavior and interactions of Teaching Societal and Ethical Implications of Research. neurons arranged in a network. Translocation DNA Sequencing: Petrossian, NABsys Inc.; NABsys aims to make whole-genome DNA sequencing fast, inexpensive, and accurate enough to be used in clinical care. The approach builds on existing solid-state technologies to create a whole- genome sequencing technology that employs electronic detection, does not depend on a polymerase, and obtains DNA sequence information Figure 66 Schematic of DNA translocation methodology over hundreds of thousands of bases. ASU NanoFab fabricated components of this system include fluidic devices for DNA dynamics experimentation and optimization. DC Bias – AC Electroosmotic Pump: Ciocanel and Islam, Northern Arizona University; The DC bias – AC electroosmotic micropump can be used to induce bi-directional fluid flow in MEMS devices. The structure of the device consists of an array of electrodes deposited on a Si wafer and a PDMS channel, with an input and output port, deposited on top of the electrode’s array. The device features range from micro- to macro-scale, making the Figure 67 PDMS channel with inlet and outlet ports on top of one electrode fabrication very challenging. The electrodes’ width ranges between array.

NNIN Annual Report p.98 March 2011-Dec 2011 40 and 120μm, while the channel’s length and width are in the tens of millimeter range. Single Photon Counting Module: Nguyen and Grubisic, Laser Components DG Inc.; New Single Photon Counting Modules have been developed to offer a unique combination of high detection efficiency (> 70%) over wide wavelength range, wide dynamic range and ease of use for photon counting applications. Dark counts of 10 photons per second have been achieved in the best devices to date. Module performance is based on Laser Components’ ultra-low-noise VLoK silicon avalanche photodiode developed using the full suite of advanced tools available within the ASU NanoFab. Figure 68: Single photon counting module Internal users also had a successful year with a number of groups reporting new finding in high impact journals such as Science and Nature. Researchers in Stuart Lindsay’s group in the ASU Biodesign Institute and collaborators at Columbia University and Oak Ridge National Laboratory are using carbon nanotubes to sequence DNA. The National Institutes of Health identified the work as a major contribution towards the “$1000 Genome” project, and Lindsay along with other NIH funded researchers were invited to meet Vice President Biden at the White House. 7.1.4 Education & Outreach ASU has developed a 4th Grade science lesson plan to introduce Figure 69: VP Joe Biden met with children to basic concepts of size and scale as it relates to innovators in DNA sequencing, including ASU’s Stuart Lindsay (center). Nanotechnology. (Fig. 70). The lesson has been developed in line with the Arizona 4th Grade Science Standards, specifically focusing on Strand 3, PO2: "Describe benefits and risks related to the use of technology“. Entitled “Nanosilver socks: no more stinky feet?” The lesson plan consists of two 50 minute classroom sessions that have been completed at Fountain Hills Charter School (FHCS) and Navajo Elementary School. The town of Fountain Hills is the nearest population center to the Fort McDowell Yavapai Nation and FHCS has a significant Hispanic and Native American population, as does Navajo Elementary, a Title 1 school with a STEM focus. A total of 83 students and four 4th grade teachers participated in the classroom sessions and a similar number is expected when the lessons are implemented again this year. One of the lessons can be viewed at Figure 70: 4th grade lesson plan http://www.youtube.com/watch?v=JMOPkQm32oc&hd=1 . The ASU node of the NNIN continues to work closely with the NSF supported Center for Nanotechnology in Society (http://cns.asu.edu/) implementing an informal science communication (ISC) program called “Taking to the Streets”. The program was initially developed around the NISENet Nanodays Kits, which help facilitate discussions about nanotechnology primarily with K-12 children and their teachers/chaperones. After a short training in basic presentation skills, engaging the public in a museum setting

Figure 71: ASU Outreach Activity NNIN Annual Report p.99 March 2011-Dec 2011 and learning objectives of the Nanodays kits, students are scheduled to host tables at the AZ Science Center on a monthly basis (more frequently as time and resources permit) throughout the year, with a special emphasis during NanoDays each Spring. When possible, visits also coincided with the height of school fields trips to the AZ Science Center. This audience is specifically K-12 students, their parents and/or teachers/chaperones. As they are ready, students are also encouraged to develop their own table demonstrations about their own research, then “take it to the people”. The ISC program also hosts a tent at the 3-day Spring Tempe Art Festival, another opportunity to engage a wider cross section of the general public in discussion around nanotechnology, which also coincides with Nanodays. Both at the AZ Science Center and the Tempe Art Festival, children and their parents enthusiastically engage with us each time we visit, adding useful insights through their comments and questions that help us continue to improve the SEI and outreach activities. 7.1.5 SEI Training NanoFab users are required to take an hour-long course on the latest health and safety issues associated with nanofabrication lab work. The SEI component is now an additional 30 minute segment to this training. The short time span is used to convey a few very basic lessons and to let lab users know about a wide array of resources available through CNS and other venues that can help them to wrestle with the ethical implications of their work. The main goal of this process is to help the researchers see that there are direct links between what they do in the lab and the big picture, including the affects it will have on people they will never meet. To further emphasize this point, and to make it directly meaningful, the SEI leader engages the researchers to describe their work and do a thought exercise. We have SEI researchers skilled at taking small technical ideas and fleshing out the potential uses (or misuses) of such ideas, how regulatory frameworks grow up around such products, and how disadvantaged communities can be further disenfranchised by specific technologies, and how small adjustments to design can lead to dramatically different affects on people’s values. Over time, the researchers slowly become active participants in this part of the discussion, and acknowledge an increase awareness of the potential impacts of their specific work past the lab walls. The SEI training is implemented by Brenda Trinidad, a doctoral student in CNS. The SEI training and other related activities were presented at the Congress on Teaching Social and Ethical Implications of Research held on the ASU campus during 10-11 November, 2011.

NNIN Annual Report p.100 March 2011-Dec 2011 7.1.6 ASU-Selected Site Statistics (2011) a) Historical Annual Users

ASU Historical Users 160

12 months 140

120 10 months foreign state and fed gov 100 large company small company 80 pre-college 2 year college 4 year college Joined NNIN FY09 Users in period Users 60 other university local site academic

0 FY04 FY04 FY05 FY05 FY06 FY06 FY07 FY07 FY08 FY08 FY09 FY09 FY10 FY10 FY11 FY11 Local Other Local Other Local Other Local other Local other Local other Local Other Local Other

b) Lab Hours by Institution Type C User Distribution by Institution Type

ASU Lab Hours March 2011- Dec 2011 10 months ASU Lab Users March 2011- Dec 2011 10 Months

large company 4% large company foreign small company small company 0% 25% 0% 12% foreign other university 0% 1% other university 9%

local site local site academic academic 75% 74% 136 users- 10 months

10,037 Hours-10 months

d) Average Hours per User ( in 10 months) e) New Users

180 50 ASU Hours per User 10 months March 2011-Dec 2011 ASU New Users-March 2011-Dec 2011 10 Months 160 45

140 40 35 120 30 100 25 80

New Users 20

Hours per user per Hours 60 63 New Users in 10 Months 15

40 10

20 5

0 0

Figure 72: ASU Site Statisics

NNIN Annual Report p.101 March 2011-Dec 2011 7.1.7 ASU User Institutions (2011) Academic Small Company Large Company Louisiana State University Ambature Amtech Northern Arizona University First Point Scientific ASM America Duke University Freeform Wave Technology Engis Corporation University of Minnesota-Morris GaNotec/Soitec Phoenix Research FujiFilm Laboratory University of Missouri-Columbia INanoBio University of Nebraska NabSYS Olin College of Engineering Sonata Biosciences University of Arizona Park Electrochemical Wichita State SEMTEC SJT Micropower Laser Components DG Inc NthDegree Technologies

NNIN Annual Report p.102 March 2011-Dec 2011 7.2 Cornell University NNIN Site Report 7.2.1 Overview CNF serves as an open resource to scientists and engineers from a broad range of nanotechnology areas, with emphasis on providing complex integration capabilities as well as support of the SEI initiative, Computation and other specific thrust areas within NNIN. CNF has operated as a dedicated user facility since 1977 so 2012 marks CNF’s 35th anniversary. In addition to technical management and administrative staff, it currently has a technical staff of 21 who maintain the equipment and baseline processes, while assisting users at all levels - particularly focusing on the needs of our external user community. CNF maintains a full spectrum of processing and characterization equipment, with emphasis on electron beam lithography at the smallest dimensions, and a wide array of deposition and etching resources necessary to handle the needs of a wide spectrum of materials. CNF continues to be an interdisciplinary facility with activities fairly evenly spread across physical sciences, engineering, and life sciences. Both the replacement of old tools and the addition of new capabilities keep CNF at the technology forefront. 7.2.2 Users and User Base CNF served over 615 users in 2011 (10 months) projecting to approximately 680 for the full year, one of the largest user bases in NNIN, with a large fraction of outside users. Our users clocked over 53,000 hours of lab usage during this 10 month period and over 60,000 for the year. Within the outside user base, CNF has a particularly strong outside academic user presence, from large universities and small colleges around the country. There were 48 such academic institutions along with 40 companies, 5 international institutions and 2 government labs during this period. Users came from 28 states and 4 foreign countries. CNF has a refined process for integration of new users in the laboratory with an emphasis on best safety practices. New users are accepted into the CNF each Monday. Basic orientation is accomplished within two intense training days to allow rapid initiation of projects. 163 new users were trained in CNF during the 10 month period (March-December 2011) 7.2.3 Technical Highlights Research reports are provided annually for many projects and are published as the CNF Research Accomplishments and online at http://www.cnf.cornell.edu/cnf5_research.html . This year we reported over 800 publications, conference presentations, and patents from among our users. Here we highlight some of the most significant examples of research enabled by CNF in the past year.

• In Nature, the Park, McEuen, and Muller groups at Cornell have developed new techniques to characterize and optimize the properties of single-atom thick graphene sheets made by chemical vapor deposition.(fig. 73). By mounting graphene on silicon nitride scaffolds and imaging in a scanning transmission electron microscope, they determined the location and identity of every atom at graphene grain boundaries. They also used diffraction-filtered imaging to rapidly map the location, orientation, and Figure 73: Grain boundries in Graphene (Park, McEuen, Muller) shape of hundreds of grains and boundaries simultaneously. They were able to show that grain boundaries severely weaken the mechanical strength of graphene membranes but do not as drastically alter their electrical properties.

NNIN Annual Report p.103 March 2011-Dec 2011 • In Science, the Wiesner, Thompson, and Muller groups at Cornell have reported the growth of single- crystal nanostructures within nanoporous templates made using block copolymers (Fig. 74). The researchers place the block-copolymer templates on a silicon substrate, fill the templates with amorphous silicon or NiSi, and then use a laser pulse to melt and crystallize the added material. The nanoscale confinement in the template allows for controlled growth of single-crystal epitaxial nanostructures. These results suggest a general strategy for growing single-crystal nanostructures for a wide variety of applications, including energy conversion and Figure 74: Block co-polymer templates (Wiesner, Thompson, Muller) storage. • In the Proceedings of the National Academy of Sciences, the Austin group at Princeton used microfabricated chips with a three dimensional topology, fabricated at CNF, to study metastasis, the process whereby cancer cells spread from their site of origin to colonize distant parts of an organism. The chip consists of lowlands and isolated square highlands, which stand hundreds of microns above the lowlands. Metastatic prostate cancer cells were studied as they invaded the highlands. The experiments reveal that these two types of highly metastatic cells have vastly different invasion rates. This microfabricated device shows promise to be a real-time platform for in vitro quantitative studies of cell invasion for a broad arrange of cancer cells.

Figure 75: Microfabricated structure to study cancer cell metastasis and migration (Austin). • In a cover article in IEEE Transactions on Biomedical Engineering, a collaboration centered at the Veterans Administration and MIT published performance tests of a miniaturized, hermetically encased, wirelessly operated retinal prosthesis developed for preclinical studies in the Yucatan minipig. The prosthesis attaches conformally to the outside of the eye and electrically drives a microfabricated thin-film array of electrodes that is implanted into the subretinal space to make electrical connections to the retinal nerves. Operation of the retinal implant has been verified in two pigs for up to five and a half months by detecting responses of the pigs to signals generated by the implanted device. • In two papers published in Physical Review Letters, Yuki Sato from the Rowland Institute at Harvard has reported experiments using arrays of nanoscale apertures in silicon nitride membranes to study the quantum-mechanical flow of superfluid helium through the array. By applying a variable phase difference across the array using a heat gradient, he observed patterns of constructive and destructive interference for superfluid flow through different apertures. He also studied the dynamics of the superfluid flow under sufficiently strong AC driving to enter a

NNIN Annual Report p.104 March 2011-Dec 2011 nonlinear dynamical regime, where he observed a dynamical bifurcation – an abrupt transition between two different flow states. • In Applied Physics Letters, the Kent group from NYU has developed a magnetic memory element that uses a spin-polarizing layer magnetized perpendicularly to a free layer to achieve large spin-transfer torques and ultrafast energy efficient switching (Fig. 76). A magnetic tunnel junction on top of the free layer reads out its orientation. The switching can be driven by 500 ps current pulses, occurs via a precessional reversal mechanism, and requires an energy of less than 450 fJ. • In Nature Nanotechnology, the Park group at Cornell Figure 76: Spin polarization memory element (Kent). has studied carbon nanotube devices optimized for optical studies. By measuring the absolute intensity of Rayleigh scattering of light from individual nanotubes, they showed that single-walled carbon nanotubes act as ideal optical wires. The nanotubes display a uniform peak optical conductivity of ∼8 e2/h, suggesting universal behavior similar to that observed in the low-frequency electrical conductance of nanotubes. • In Nano Letters, the Hanrath and Wise groups at Cornell used both the computational and cleanroom facilities of the CNF to examine charge transfer and exciton dissociation in coupled lead salt nanocrystals under illumination when two nanocrystals are connected by different linker molecules(fig. 77). As part of this work, ab-initio calculations were done on the CNF computational cluster to determine the HOMO-LUMO energy levels of different length nBDT bi- linker molecules connecting lead salt nanocrystals and how these energy levels affect the transfer rate between the nanocrystals. Evidence was found for two different types of transfer mechanisms.

Figure 77: Ab ignition calculations of charge transfer and excition dissociation in lead salt nanocrystals (Hanrath and Wise) • In Nano Letters, the Craighead group at Cornell has developed a high-throughput “Print-and- Peel” method to generate multicomponent biomolecular arrays with sub-100 nm nanoscale feature widths. The researchers start with a paralene template containing nanoscale openings on a substrate. An inkjet printer aligned to the template then prints on top of the paralene and through the holes in the paralene. After printing, the parylene is peeled off to reveal uniformly patterned nanoscale features, despite the imperfect morphologies of inkjet spots. The

NNIN Annual Report p.105 March 2011-Dec 2011 researchers further patterned combinatorial nanoarrays by performing a second print-run superimposed over the first, thereby extending the multiplexing capability of the technique. • In Optics Express, The Erickson group at Cornell has demonstrated reconfigurable optical switches based on using flowing liquids to dynamically change the optical index of refraction (fig. 78). By controlling the flow of two liquids with different indices of refraction within a microfluidic device, they can create liquid-core/liquid-cladding optical waveguides. By adjusting the relative pressure of the flows, they can steer the liquid core to switch between different channels, thereby also switching the path of the flow of light traveling within the waveguide. The chip-based geometry allows external optical fibers to be coupled efficiently to reconfigurable fluidic devices to make complex reconfigurable photonic systems.

Figure 78: Reconfigurable microfluidic switches (Erickson) 7.2.4 Focus Areas/Assigned Responsibilities As one of the largest nodes in NNIN, CNF has been assigned special leadership responsibilities in the network for: Electronics, Optics, and MEMs; for Computation; for SEI activities; and for Education, as well as broad responsibility to support all NNIN technical areas. CNF actively supports users and provides specialized and generalized resources as discussed below. Leadership areas: • Electronics, Optics, MEMS: CNF has extensive facilities and processes to support the traditional areas of Electronics, Optics, and MEMS. CNF has the most advanced e-beam lithography facilities in the network and is positioned to maintain that leadership for several years with future upgrades and system acquisitions. In 2012 we are expecting delivery of a new flagship tool, the JEOL JBX 9500FSZ, that is currently being built. These, along with other advanced photolithography capabilities (described below), support fabrication of advanced electronics, optics, and MEMS structures and a growing number of life sciences projects. CNF also has a broad silicon CVD/oxidation capability with up to 20 process tubes. We continue to acquire and develop processeses for leading edge tools such as a Graphene/ Carbon Nanotube Furnace from FirstNano. A Primaxx Vapor HF etch system, and a new AJA Orion 8 RF/DC Sputter Deposition System. Recent acquisitions such as the Suss mask and bond aligner, a high speed Heidelberg Laser writer for mask making, a Veeco Dimension Icon atomic force microscope, and Suss Gamma (described below) have all added capabilities that are sought by both academic and industrial users. Students and Post Docs nearby centers such as the Cornell Center for Nanoscale Systems (CNS), the Cornell center for materials research (CCMR), and the Cornell High Energy Synchrotron Source (CHESS), help provide a critical mass of research and technology in advanced materials and device structures. We also maintain support for fluidics capabilities for the life sciences through our life sciences liaison, Dr. Beth Rhoades, our new

NNIN Annual Report p.106 March 2011-Dec 2011 VersaLaser cutting tool and a short course offering on PDMS casting (co-instructed with the Nanobiotechnology Center staff). CNF staff are particularly skilled in complete process integration issues involving deposition, etching, and lithography. • Computation: CNF is one of four NNIN nodes with major nanotechnology computation capabilities. CNF has invested in computational resources and a nanotechnology computation technical liaison (Dr. Derek Stewart) to support and expand facilities for users. Details of the expanded hardware, software, and outreach for the CNF computational program are described in a separate section below. • Social and Ethical Issues in Nanotechnology: CNF is a major site for NNIN SEI activity. Both the NNIN SEI Coordinator for the network and research associate are based at Cornell and paid from Cornell site funds. Detailed SEI activities for the year are discussed below. • Education: CNF has extensive education activities, primarily directed to the university level and above but with significant outreach among younger students as well. These are covered in the Education section below. Other Assigned Areas: • Life Sciences: CNF actively supports projects involving biological applications of nanotechnology. To provide discipline specific support for life sciences users, CNF has a technical liaison (Dr. Elizabeth Rhoades). The Cornell Nanobiotechnology Center (NBTC), a parallel user facility, helps provide a critical mass of nanobiology users who contribute to the technology base available to users. Current CNF projects include considerable work in biosensors and microfluidics. CNF maintains a number of processes which significantly or exclusively support nanobiotechnology (e.g., molecular vapor coating, parylene deposition, embossing, PMDS casting, and microcontact printing). CNF has implemented an extensive process and sample compatibility study with input from NBTC staff. A lab demonstration on soft materials was added to our TCN course this year and a quarterly short course on PDMS stamping was developed and jointly conducted with the NBTC staff. • Materials and Materials Analysis: CNF supports a broad range of materials and materials related research both in-house and through facilitated access to electron microscopy facilities within the Cornell Center for Materials Research (CCMR). STEM, TEM and Dual Beam FIB facilities can be accessed by our users via CCMR. Within CNF are housed excellent SEM facilities in the form of two Zeiss Gemini series digital field emission microscopes. To assist users in true nanoscale probing of materials and device structures, CNF has a Zyvex nanomanipulator system, allowing probing within a SEM with 1 nm motion resolution. CNF’s Dimatix materials ink jet printer supports a novel fabrication process with organic and inorganic materials “inks”, on rigid and flexible substrates. Along with the Reynolds Tech cluster tool for deposition of organic conductive coatings, we have made significant strides in establishing an organic electronics capability. The Oxford ALD continues to serve materials research with highly conformal metal nitrides, hafnia and, aluminum oxide and silicon dioxide film deposition with monolayer control. Our Woolam spectroscopic ellipsometer, newly acquired Zygo optical profiler, and Filmetrics thin film mapper all support film characterization for both organic and inorganic thin and thick film materials. • Remote Processing: Remote usage serves as a way to engage future users, achieve higher tool utilization, and enhance the NNIN network value to users. Remote processing is generally limited to single steps or short process sequences that have a high probability of success. In this reporting period, over 75 remote jobs were completed. While mask making, lithography, and thin film deposition are the most common remote requests, more complex structures are being accomplished. We also make use of inter-site capabilities. For example, shipping a user’s wafers

NNIN Annual Report p.107 March 2011-Dec 2011 to U. Michigan or UCSB for etching or to Stanford, Georgia Tech, and Harvard when a CNF system is down for repairs. We have gotten excellent cooperation from the other NNIN sites when users require this backup support. 7.2.5 Equipment and Facilities CNF operates in a suite of labs in Duffield Hall, a state of the art research building on Cornell’s Engineering College part of campus. CNF user facilities include a 16,000 sq. ft. clean room, but also include wet and dry non-cleanroom labs for additional chemistry and biology support facilities. There is also a characterization lab, a CAD room, and an ion implantation laboratory. In addition, CNF has nanoscale computation facilities (hardware, software, and support) that specialize in assisting users in interfacing with the various modeling programs. CNF maintains a broad set of processing and characterization tools with emphasis on patterning at the smallest dimensions. Our two 100keV ebeam lithography tools are the cornerstone of our materials patterning capabilities; they are supported by contact lithography (3), steppers (3), mask makers (2), 16 dry etch tools of various types, and extensive thin film deposition and inspection capabilities. In total, over 90 major processing tools are available. • In 2011, CNF was active in upgrading and adding process equipment and computing resources. We are preparing for a next generation electron beam lithography system from JEOL, the JBX 9500 FSZ. This will be first major advance in EBL in a decade and will likely set the standard for the next decade. In addition our two year new JBX 6300FS e-beam system was upgraded to 50 MHz and added a motorized aperture. • We were able to replace our ailing FEI FIB with a nice small footprint Hitachi FB 2000A purchased from Corning Inc. (Fig. 79) • We received and installed a SUSS MicroTec Gamma Coat,Bake, and Develop robotic track system. The system allows automated pre and post exposure processing for advanced photolithography users. The system also is equipped with an AltaSpray system that allows spray application of photoresist – especially useful for coating wafers with extreme topography where spin coating is not practical. Figure 79: Hitachi FIB • Through a joint development agreement with SUSS Microtec, CNF has received a hardware addition for the SUSS MA6 aligner that performs substrate conformable imprint lithography (SCIL), Microoptics for shaping illumination printing, and GenISys LayOut Lab software for 3D simulation of proximity lithography. • To provide a dry method of MEMS release, we installed a Primaxx µEtch dry HF vapor etch system. This is a new product sized for the research community that is based on proven technology in larger systems. (Fig. 80) • To improve the work flow in the photolithography area we acquired Figure 80: Primax uEtch Vapor HF several new hotplates, ovens and a new vented cabinet. This along with some rearrangement of the spinner hoods should Figure 81: AJA Sputter System improve the ergonomics and increase the number of fixed and adjustable bake options for photoresists. • To improve the availability of sputter deposition targets we have augmented our existing tool with an AJA Orion 8 system with both DC and RF sputter capability. This increases our available targets from 3 to 8 at any given time.(fig. 81)

NNIN Annual Report p.108 March 2011-Dec 2011 • ASML has generously donated and installed a 3D align (backside alignment) system onto our PAS 5500/300C DUV stepper. • Our VersaLaser cutting tool has demonstrated great flexibility in patterning thin materials including paper, plastics, metals, etc. from CAD layouts. • A new ZYGO NewView 7300 optical profiler with dynamic MEMS software has replaced a retired system (fig. 82). The new system is far more capable that can produce highly sensitive 2-D height maps, 3-D reconstructions, and record strobe effect movies of moving MEMs parts • Our acquisition of the Suss DSM-8 will allow the contact aligners and the ASML stepper to quantify the back to front alignment errors. • Several Cornell grad students worked with Phil Infante to develop a catalytic Graphene growth process on copper. The system is now available to users for CNT and graphene growth. • We have purchased and are in the process of installing a major Oxford 100 upgrade that includes a new PLC and expansion of the gas handling capabilities. The major focus will be to allow exploration of new process gases that

vary the fluorine to carbon ratios. Figure 82: Zygo NewView 7300 7.2.6 Site Usage and Promotion Activities CNF distributes a set of eight professionally designed color brochures covering each of the primary technical areas. These brochures are widely distributed as a marketing tool to potential users both in NYS and around the country. We also distribute a professionally produced tri-fold brochure as a “light” alternative for wide mailings and trade show distribution and are just completing the art work for an updated version. CNF staff manned the NNIN Promotional Booth at AVS, MRS, EIPBN, and APS. CNF annually publishes its annual CNF Research Accomplishments consisting of research reports from many of its users. One hundred and forty three reports were featured in the 2010-2011 edition, which is available on request from CNF or via the CNF web site at http://www.cnf.cornell.edu/cnf_2011ra.html. “The Nanometer”, the CNF glossy newsletter was also published and distributed to 1400 users, former users, corporate supporters, and visitors. Recent issues of the NanoMeter are available at http://www.cnf.cornell.edu/cnf5_nanometer.html The visibility of CNF is enhanced by Cornell’s use of Duffield Hall as a venue for campus events. Numerous visits by company executives and government leaders to campus have been accompanied by visit and tour requests. In 2011 alone, CNF hosted over 1100 visitors in 31 corporate visits and over 130 academic, educational and government visits and events. This is over and above our users and external outreach activities that engaged an additional 2580 participants . 7.2.7 Education Contributions CNF supports a broad range of educational activities, primarily at the undergraduate, graduate, and professional levels. • Research Experience for Undergraduates: Research Experience for Undergraduates: CNF plays a leadership role and participates actively in the NNIN REU program. In summer 2011, CNF hosted twelve students including eight women (fig. 83). Cornell staff

Figure 83: 2011 CNF REU group

NNIN Annual Report p.109 March 2011-Dec 2011 also provide most of the administrative support for the entire network REU program including advertising, processing of over 1000 applications, initial interaction with participants, and preparation and printing of the REU research accomplishments for the 14 sites. CNF also underwrites the laboratory charges for all the cleanroom and tool charges incurred by the Cornell faculty-hosted REU participants. • Nanooze: As part of its national educational outreach CNF has committed to producing and distributing Nanooze, a children’s science magazine relating to physical sciences and particularly nanotechnology. Nanooze (http://www.nanooze.org/) is a both web-based and printed magazine, with kid-friendly text, topics, and navigation. Nanooze is predominantly the work of Prof. Carl Batt and his former student Clarissa Lui, with support from CNF. Nanooze is available in English, Spanish and Portuguese. This year a new issue (our tenth) was printed and distributed highlighting the roles of atoms in materials, Nanotech applications, and celebrating 2011 as the “Year of Chemistry”. (fig. 84) Three more issues related to chemistry are in production, all in recognition of the International Year of Chemistry.Issue 10 also features Q&A with Nobel Prize winner Harry Kroto, recognized for the discovery of the C60 “Buckeyball”. Circulation has Figure 84: Nanooze grown to nearly 100,000 copies per issue as requests from classroom teachers continue to grow. CNF employs an undergraduate who works every week to keep up with the requests for classroom kits. • TCN – Technology and Characterization at the Nanoscale: TCN is CNF's introductory course to Nanotechnology. The course is open to the public and aims to educate students, industrial personnel, technology managers and entrepreneurs with an interest in Nanotechnology. (fig.85). CNF offers the TCN semiannually during the summer and winter recess, so that interested students from universities and industry can easily participate. Combined, about sixty students and scientists participate in the two courses offered per year, representing Biomedical Engineering, Optics, Physics and Applied Physics, Material Science, Chemical Engineering, Environmental Health and Safety, and Electrical Engineering. On average, about one third of the participants are Cornell graduate students, one third are graduate students from universities other than Cornell, and one third are undergraduate students, teachers, and industrial participants. The content of the TCN is designed to encompass a wide range of nanotechnology techniques relevant to current research in the field. While traditional topics in nanotechnology - thin films, lithography, pattern transfer (etching), process integration, and characterization - provide the basic structure of the course, we include emerging technologies and new approaches in nanotechnology. Nano-imprint lithography, bottom-up nanofabrication, carbon nanotubes, soft lithography, and surface preparation for biology applications are among the topics addressed. The printed notes for the TCN course have been developed over 17 years and are a highly valued resource. The course includes lectures and laboratory Figure 85: TCN Short Course

NNIN Annual Report p.110 March 2011-Dec 2011 demonstrations as well as hands-on photolithography sessions. The evaluation forms for the TCN conducted after the June course showed that 85% of the participants rated the lectures and 90% rated the lab course good to excellent. 100% would recommend the course to others. The TCN course will next be offered in June 2012. In addition to preparation time, this course occupies most of the CNF staff for the three-day duration of the course. • CNF Annual Users Meeting: On September 15, 2011 CNF hosted its annual user symposium and executive user committee meetings. Presenters included keynote speaker Philip • Clarkson Workshop: CNF hosted a hands on workshop for 10 graduate students from Clarkson University. Prof. Cetin Cetinkaya at Clarkson conducts a one semester Nanotechnology course that prepares students for the CNF lab experience. • CIPT Workshop: On July 12, 2011CNF staff conducted CNS Institute for Physics Teachers, a one day lab event for 26 teachers who participated in the program Beth Rhoades and Mike Skvarla from CNF coordinated the event with Julie Nucci from CNS. • Microfluidics and Surface Modification Mini-Courses: A hands on lab course in microfluidics was offered twice in 2011 as a joint effort between the CNF and the Nanobiotechnology Center (NBTC). The 3-day course covered the fabrication, assembly and uses of microfluidic devices. It was taught by Beth Rhoades, the Life Sciences Liaison of the CNF, and two staff members from the NBTC. Cornell researchers who have made microfluidic devices at the NBTC and CNF made short presentations and showed their research devices to the attendees. Attendees came from the Cornell and external academics. A second mini-course was added following a similar schedule has been developed for surface modification for biotechnology. • Wafer Bonding and Lithography Workshop: In collaboration with SUSS MicroTec, CNF staff hosted and helped conduct a workshop that investigated and demonstrated recent technology developments in temporary and permanent wafer bonding, spray coating methods, substrate conformable imprint technology, and microoptics for proximity printing. The one day workshop combined classroom and cleanroom experiences. About 30 attendees came from industry, academia, and staff from other NNIN sites to meet with SUSS engineers who travelled from Germany for the day. • BEAMeeting at CNF: CNF hosted software developers and application engineers from GenISys to present the various features and usage concepts of software modules now in use at CNF, such as Beamer and Layout Lab. 45 users and staff attended the sessions that included both presentations and active workstation sessions. A second hands on workshop is scheduled for mid-February 2012. • Computational Workshop: CNF computation liaison, Derek Stewart. received a National Science Foundation grant to host a Pan-American Advanced Studies Institute on Computational Materials Science for Energy Generation and Conversion in Santiago, Chile from January 8-22nd 2012. Additional funding was also obtained from the Office of Global Naval Research, NNIN, the International Center for Materials Research, and several other Cornell centers. CNF staff provided the administrative support for the travelers. This two week school brought together over 40 graduate students and post-doctoral researchers from the United States, Chile, Argentina, Mexico, Colombia, and Brazil. The workshop provided lectures in first principles approaches, molecular dynamics, optical techniques, and finite element approaches. Advanced topics included piezoelectrics for energy harvesting, lithium battery design, and engineering thermal properties of materials for thermoelectrics. Lectures and tutorials developed through this course will be made available on the CNF and NNIN websites. • Junior FIRST LEGO® League: The CNF sponsored a Junior FIRST LEGO League (Jr.FLL) Expo for 50 kids ages 6 - 9 from 9 teams (Fig. 86). The teams came in from a wide area covering Rochester to Ithaca, NY. The theme of this year's expo was Snack Attack, dealing with Food

NNIN Annual Report p.111 March 2011-Dec 2011 Safety. Beginning in the fall, the teams had to take a "hands on" approach to the topic of food safety by exploring how proper preparation and storage can help keep us healthy. Teams learn about simple machines as they build a model made of LEGO® elements with a motorized moving part, and will create a team Show-Me Poster to represent their Snack Attack findings. Teams from around the area presented their LEGO model and poster and received an award for their work. Staff from CNF organized the event and served as Figure 86: Junior FIRST Lego event project reviewers. This event was also partially underwritten by a grant from the Shell Oil Company. 7.2.8 Computation Contributions (CNF/C) During 2011, the computational effort at the Cornell Nanoscale Facility continued to help foster nanoscale research and education through direct consultation and access to a wide array of simulation tools on the CNF cluster.

• Publications 2011: Work on the CNF cluster resulted in 11 research articles in 2011 and 2 articles currently under review, bringing the total number of publications to 59 since the cluster came online in February 2005. The full collection of papers has h-index of 16 and has currently been cited 753 times. The 2011 papers include articles published in the Proceedings of the National Academy of Sciences, Nano Letters, Journal of the American Chemical Society, Physical Review B, and the Journal of Materials Chemistry. Recent research topics include thermal transport in InAs nanowires, graphane sheets under pressure, improved energy storage devices, new thermoelectrics based on nanoparticle embedded alloys, and grain boundaries in graphene sheets. • Cluster User Statistics for 2011: In addition to usage by several veteran CNF cluster users, 20 new users obtained accounts in 2011. In 2011, the CNF cluster had 39 active users, 29 Cornell users and 10 external users. The outside users for 2011 included researchers from Lawrence Berkeley National Laboratory, Tuskegee University, UC Berkeley, SUNY Albany, and Alfred University. • New NNIN/C Counting Approach for 2011: Using the new NNIN/C counting approach that includes both cluster users and consulting with users on projects (collaborations, simulation advice, code distribution, etc), in 2011 the CNF had 59 total users with 29 outside users. This number does not include the 25 students that used the cluster for a Cornell Solid State Chemistry course. • User Awards Zoe Boekelheide (University of California, Berkeley) won the American Physical Society, Group on Magnetism and Magnetic Materials (GMAG) Dissertation Award for 2011. Her work focuses on the effects of nanoscale structure on the magnetic and transport properties of chromium and chromium-aluminum alloys. She has performed numerous simulations of CrAl alloys on the CNF cluster that resulted in a 2010 Physical Review Letters article and another article currently in review at Physical Review B. Also, Joshua Taillon, an undergraduate who was using the CNF cluster for his research, won the 2011 Best Overall Senior Thesis for Material Science and Engineering at Cornell. (J. Taillon, "Ab Initio Discovery of Novel Crystal Structure Stability in Barium and Sodium-Calcium Compounds under Pressure", Senior Thesis, Cornell University (2011) ) A paper on the work will probably come out some time this year. • Educational Outreach: During the 2011 Cornell Spring semester, Derek Stewart worked with Prof. Richard Henning (MSE, Cornell) on a simulation module for the Frank DiSalvo’s Solid State Chemistry course (CHEM 6070). Approximately 25 students participated in this module and

NNIN Annual Report p.112 March 2011-Dec 2011 students used the CNF cluster during class tutorials. • Research Grants: Dr. Derek Stewart received a National Science Foundation research grant “Collaborative Research: Ab Initio Computation of Phonon Thermal Transport in Crystalline and Disordered Material” (CBET-1066406). This grant will fund a collaborative effort between Dr. Stewart at Cornell and Prof. David Broido at Boston College on first principles thermal transport in low thermal conductivity materials, such as thermoelectrics. The tools developed through this grant will be made available through the NNIN. • Outreach Grants: Dr. Derek Stewart received a $100K National Science Foundation grant (#1123536) to host a Pan-American Advanced Studies Institute on Computational Materials Science for Energy Generation and Conversion in Santiago, Chile from January 8-22nd. Additional funding was also obtained from the Office of Global Naval Research, NNIN, the International Center for Materials Research, and several other Cornell centers. This two week school brought together over 40 graduate students and post-doctoral researchers from the United States, Chile, Argentina, Mexico, Colombia, and Brazil. The workshop provided lectures in first principles approaches, molecular dynamics, optical techniques, and finite element approaches. Advanced topics included piezoelectrics for energy harvesting, lithium battery design, and engineering thermal properties of materials for thermoelectrics. In addition, students participated in daily hands-on sessions to gain experience in various simulation approaches. Computational resources on the Texas supercomputer, Ranger, were made possible through a NSF XSede computing time grant. Lectures and tutorials developed through this course will be made available on the CNF and NNIN websites.[Pan American Advanced Studies Institute “Computational Material Science for Energy Generation and Conversion”, Pontifica Universidad de Chile, Jan. 9th -20th, 2012, Santiago, Chile (see description above) http://www.cnf.cornell.edu/cnf_pasi2012.html] • Virtual Vault for Pseudopotentials Development : The CNF hosts the Virtual Vault for Pseudopotentials for the NNIN/C. The NNIN database provides the global scientific community with access to pseudopotentials used in a wide range of electronic structure codes (See http://www.nnin.org/nnin_comp_psp_vault.html .) The clearinghouse consists of a PHP-SQL database of pseudopotentials that can be accessed online, containing over 800 pseudopotential files drawn from different pseudopotential codes including Quantum Espresso, Abinit, and Qbox. Users can interface this data through an online periodic table to find information related to a particular atom. Users can also search the database based on a given element and compare available pseudopotentials based on criteria such as exchange-correlation functional, pseudopotential class (i.e. ultra-soft, norm-conserving), parent electronic structure code, and more. This database provides the first centralized resource for pseudopotentials that spans multiple electronic codes and numerous websites in the electronic structure community now provides links to the Vault as a valuable resource. In addition, members in the community have also begun to donate their own pseudopotentials to the database. In 2011, additional search mechanisms were added to the Vault interfaction. In addition, Derek Stewart has been working with Joseph Bennett (Rutgers University) to add a suite of optimized pseudopotentials to the Virtual Vault. • Cluster Simulation Options: Two new software packages were added to the CNF computational resources available for users in 2011. In addition, several simulation codes were updated to their most recent version. Currently, CNF users have access to over 30 different computational packages for topics including nanophotonics, fluidics, molecular dynamics, and electronic transport in nanostructures. In addition, the computational branch at the CNF continues to provide the only public access point for the UT Quant code which is used to calculate C-V characteristics for MOS structures. In 2011, this code was requested from researchers at

NNIN Annual Report p.113 March 2011-Dec 2011 institutions in the United States, France, and India. • Continued Impact of the New Hardware on the CNF Cluster: The Cornell Nanoscale Facility purchased 20 new computing nodes and a new master node in July 2010. These nodes are constantly in high demand by the CNF cluster users with usage often at or above optimal capacity. A future expansion in computational resources would help alleviate this issue and potentially increase the number of users. • New software added in 2011 o XBand – Graphical user interface for band structure calculations developed by the Universitat Munchen. o Phonon Focusing Software – these packages determine how phonons are focused along particular crystal directions. o Software updated to Newer Versions: VASP, Gaussian 2009, Quantum Espresso, OpenMX, QuantumWise ATK/VNL, LAMMPS 7.2.9 Social and Ethical Issues in Nanotechnology Social and Ethical Issues (SEI) activities form an integral part of NNIN training at its 14 sites where we aim to develop social and ethical consciousness both within user community and the broader nanotechnology community. • SEI at CNF: CNF continues to conduct a weekly 30-minute face-to-face SEI Orientation for all new lab users. These materials are used to stimulate discussion seeking out the opinions of the users. The orientation consists of an interactive PowerPoint presentation adapted from a previous version developed by Dr. Debasmita Patra, a former Postdoctoral Research Associate at CNF and the Department of Communication. The orientation covers various topics, including: an overview of pertinent ethical issues in nanotechnology research, including privacy and the equitable distribution of risks and benefits of particular applications; an overview of pertinent risk- based aspects of nanotechnology, including toxicology and similarities/differences with past technologies such as asbestos and biotechnology; a discussion of research on public perceptions of nanotechnology; a survey of strategies for communicating the risks and benefits of nanotechnology; examples of ongoing work that is addressing SEI, including interdiscipinary courses for undergraduate and graduate students at various universities as well as the “Responsible Research in Action” posters developed by Dr. McComas and previous CNF REU intern, Chloe Lake, in 2010. • SEI REU: CNF hosted one of the two NNIN SEI REU interns, Ms. Rachel Brockhage, a biology major at Grove City College (Pennsylvania) (fig. 87). As an SEI REU intern, Rachel assisted Dr. Katherine McComas (NNIN SEI Coordinator) and graduate student mentor Chris Clarke with an online Figure 87: Rachel Brockhage, survey of NNIN users about their views on the role funding SEI REU student sources and conflicts of interest (COI) play in their research. This survey was in follow-up to a 2011 article Dr. McComas published in Science and Engineering Ethics.In addition to the survey, Ms. Brockhage participated in the weekly “new user lunches” that CNF conducts and facilitated informal SEI discussions at the lunches. She was invited to discuss her efforts at the 2011 Congress on Societal and Ethical Implications in Tempe, AZ, November 9-11 (see photo). 7.2.10 Staffing CNF has a staff of 29 technical and administrative professionals, all dedicated to CNF/NNIN user

NNIN Annual Report p.114 March 2011-Dec 2011 functions. All staff members are supported entirely by CNF core funding and user facility funds.Average tenure at CNF is over 10 years. In late 2011 Daniel Woodie, the CNF Lab Use Manager and Safety Coordinator left CNF to become the Safety Manager for the Cornell College of Engineering. We are currently conducting a search for a replacement staff member, but were fortunate to have talented and experienced staff members who were able to step up and serve in these capacities. Daron Westly is now serving as the CNF Lab Use Manager and Phil Infante as our Safety Coordinator. We also hired on an interim basis a former CNF staff member, Daniel McCollister to help fill in with the lab responsibilities until we complete our search.

NNIN Annual Report p.115 March 2011-Dec 2011 7.2.11 Selected Cornell Site Statistics (2011) a) Historical Annual Users

foreign Cornell Site Historical Users state and fed gov 450 12 months large company 10 months small company 400 pre-college 2 year college 4 year college 350 other university local site academic

300

250

Annual Users 200

150

100

b) Lab Hours by Institution Type C User Distribution by Institution Type

Cornell Site Lab Hours 10 months Cornell Site User Distribution 10 Months March 2011-Dec. 2012 (March 2011-Dec 2011) Large State and Fed State and Fed Company Gov Gov Large Company Foreign 2% 0% 1% 1% Small 2% Company Foreign Small Company 10% 14% 1%

Other Local Site Academic University Other University 56% Local Site 27% 30% Academic 56% 615 unique users in 10 months 53072 Hours in 10 months

d) Average Hours per User ( in 10 months) e) New Users

120 Cornell Site--Average Hours per User 140 Cornell Site New Users (10 months) 120 100

100 80 163 New Users in 10 Months

Hours 80 60 60 New Users 40 40 20 20

0 0

Figure 88: CNF Site Statistics

NNIN Annual Report p.116 March 2011-Dec 2011 7.2.12 Cornell User Institutions (2011) Other University Small Company Large Company Binghamton University Advanced Diamond Tech. API Defense Inc. City College of New York Advion BioSystems, Inc. ASML Clarkson University Agiltron Inc. Corning, Inc. Clemson University Applied Pulsed Power, Inc. GE Global Research Center Columbia University BinOptics Corp Hysitron Inc Georgia Institute of Technology BioArray Solutions Ltd Ortho Clinical Diagnostics Harvard University Boston MicroSystems, Inc. Suss MicroTec Indiana University Calient Optical Components Xerox Corporation Lehigh University EIC Biomedical MIT EigenPhase Technologies New York University Faraday Technology, Inc. North Carolina State University Illuminaria, LLC International North Carolina State University Kionix, Inc. Ecole des Mines de Saint Etienne Northeastern University MCB Clean Room Solutions University of Toronto Northwestern University McCollister Nanofab Services University of Waterloo Old Dominion University Mezmeriz Inc. Oregon State University MicroGen Systems, LLC Princeton University Mitegen, LLC Rensselaer Polytechnic Institute NABsys, Inc. State and Federal Rochester Institute of Tech. NanoMas Technologies MIT Lincoln laboratory Stony Brook University Odyssey Scientific Syracuse University optofluidics, Inc. Texas A&M University Orthogonal Inc. University at Albany Pacific Biosciences University at Buffalo PC Mirage LLC University of Arkansas Phoebus Optoelectronics, LLC Univ. of Colorado at Boulder Promerus, LLC University of Connecticut Resource Management Tech. University of Idaho Tornado Medical Systems US, Inc. University of Kentucky Transonic Systems Univ. of Maryland - College Park Widetronix, Inc University of Pennsylvania University of Rochester University of South Carolina University of Washington Utah State University Vanderbilt University Yale University

NNIN Annual Report p.117 March 2011-Dec 2011 7.3 Georgia Tech Site Report 7.3.1 Research Highlights Nanolithography: The Nanolithography Facility continues to successfully operate with a JEOL JBX- 9300FS Electron Beam System.Both academic and industrial users have successfully engaged at Georgia Tech to achieve their research goals. Research project were either started or continue with 53 total users for 2011. Users came from US and foreign academic institutions, US companies, and the US government. Tissue Engineering of a Ligament, Derrick Dean and Andrew Uehlin (University of Alabama - Birmingham): This investigation incorporates the fabrication of a tissue scaffold designed to support unique, hierarchical cellular development for use in studies of a bioengineered ligament and bone- ligament interface. Biomolecule deposition via the JetLab II inkjet printing system is utilized to immobilize various bioinks on an aligned fibrous polymer matrix, creating hierarchical, spatially organized structures that are capable of inducing zone-specific cellular responses. To date, nanoscale particles of hydroxyapatite have been printed over a spatial distribution gradient on an aligned, electrospun poly(lactic) acid fiber tissue scaffold. This morphology is mimetic of the gradual increase in cellular mineralization as the ligament transitions into bone. Future studies

will include the addition of bioinks comprised of various growth Figure 89: Tissue Scaffold (Dean, Uehlin) factors and additional biological response modifiers to further promote hierarchical cellular development.

Hybrid Nanoplasmonic Photonic On-chip Sensors, Ali Adibi (Georgia Institute of Technology): Integrated nanoplasmonic photonic sensors are designed and implemented for on-chip sensing (Fig. 90). The purpose of the novel integrated plasmonic photonic platform is to realize a lab-on-chip system for efficient light-matter interaction. This leads to a low-cost, highly sensitive, and portable sensing device for applications in point of care diagnostics in far reaching areas with limited resources, and also for chemical and environmental sensing. Different components of this sensing platform are fabricated using electron beam nanolithography, ICP etching, metal evaporation, and lift-off using the tools at GT-NRC.

The device is fabricated on a Si wafer with layers of oxide, and Figure 90: Nanoplasmonic sensor nitride as the photonic component. The plasmonic component is implemented using gold nanoparticles.

Analysis and characterization of albumin and dextran microparticles carrying encapsulated membranes, Periasamy Selvaraj and Sanjay Srivatsan (Dept. of Immunology and Cancer Biology, School of Medicine, Emory University): The research work focuses on the tumors modified by transfecting genes for immunostimulatory molecules such as B7 and cytokines are now considered as a potential therapeutic tumor vaccine. However, transfection is not always efficient and can be difficult with many cell types, especially freshly isolated tumor cells from patients. Moreover, transfection of genes requires the introduction of vectors of viral origin which is not desirable for human therapeutic purposes. Using recombinant techniques, the authors have developed many immunostimulatory molecules and currently use protein transfer to express these molecules to develop cancer vaccines for breast cancer and melanoma.

NNIN Annual Report p.118 March 2011-Dec 2011 Cancer's central feature of immune escape presents a problem yet to be solved. In an attempt to create a novel cancer vaccine system, a murine T-cell lymphoma cell line was grown in mass and lysed to yield tumor membranes. These tumor membranes were then encapsulated in cyclodextrane or cross-linked albumin microspheres. To ensure that the encapsulation of tumor membranes did not interfere the geometry or size of the microspheres Variable Pressure SEM was conducted. The micrograph at the right (fig. 91) shows that the encapsulating tumor membranes does not affect the geometry nor does it affect Figure 91: Micrograph of tumor the size drastically. membranes

Fabrication of SU-8 Posts for creating PDMS Microwell Arrays for Immunological Studies, J. Christopher Love and Ayca Ozkumur (Department of Chemical Engineering, Massachusetts Institute of Technology): This research aims to explore the heterogeneity present in populations of cells and characterize the dynamic biological responses of individual cells subjected to defined perturbations. We have developed a process for analyzing large numbers of individual living cells quantitatively and dynamically, based on soft lithography of microwell arrays. These arrays were utilized to measure multiple characteristics of single cells, and from those data, aimed to construct detailed profiles that describe the state and evolution of the cell itself or the multicellular population of which it is a member. The applications of this technology include clonal selection for bioprocess manufacturing, discovery of new immunotherapies, and immunological monitoring for diagnosis and biomedical research in clinical immunology. Particular areas of emphasis in clinical immunology presently are infectious diseases and autoimmune disorders.

To improve the existing single-cell analysis platform, the authors plan to test new designs for creating microwell arrays. The master molds fabricated will be used to make a series of new PDMS devices that will be tested for Figure 92: PDMS microwell arrays performance assessment.

7.3.2 Growth of the Ga Tech NRC Facilities, Equipment and Capabilities Tool installation in the inorganic cleanroom is approximately 80% complete, with more room for future capabilities. Future capabilities for the organic cleanroom include a GLP lab for pre-clinical trials for vaccine delivery. Building expansion, currently in schematic design, will include two of the three laboratory floors, space for visiting NNIN scholars/users, and a nano-imaging suite, which will be part of the NNIN user facility in the Marcus Nanotechnology Building.

During the past year, the Georgia Tech IEN has acquired a number of innovative capabilities. This has been achieved in part by purchasing high-quality equipment and performing nearly all of the installation in-house.

Thin film deposition has improved via installation of a Denton Discovery sputtering system which is configured for the deposition of magnetic materials and is capable of RF co-sputtering, DC sputtering, and application of an RF bias voltage to the substrate. The Oxford Plasmalab System 100 is a high- density ICP PECVD that has been equipped with a substrate heater table that operates up to 400°C to allow for improved silicon dioxide film quality. Etching capabilities available in the Marcus

NNIN Annual Report p.119 March 2011-Dec 2011 Nanotechnology Building have been enhanced by the acquisition of a Unaxis 790 RIE system with chlorine chemistry for shallow silicon etching.

Lithography has been enhanced by the addition of a Suss Altaspray Spray Coater to conformally coat challenging, high aspect ratio structures. In addition, a Microtech LW405A laser writer has been added to increase the in-house mask production capability and capacity.

Characterization capabilities have been expanded, including the purchase of a new Woollam M2000 spectroscopic ellipsometer that collects 570 wavelength measurements simultaneously with a large spectral range (375nm-1690nm). The Keyence VHX-600 digital microscope has been upgraded with a new low-magnfication lens & stand that allows for the acquisition of image data from 25X-250X while the other stand allows 250X-2500X. The IonTOF 5 Time-of-Flight Secondary Ion Mass Spectrometer (ToF-SIMS) which has bismuth, cesium, and oxygen sources has been upgraded to the latest software version on a new control computer and new offline analysis software. The new Biacore T200 Surface Plasmon Resonance (SPR) tool is a versatile, label-free system with exceptional sensitivity that provides high quality kinetics from fast on-rates to very slow-off rate. The addition of a Zetasizer particle sizing system allows for quantification of nanoparticle size distributions from 0.5nm to 10um.

7.3.3 Diversity Activities During Summer 2011, Dr. Zachariah Oommen from Department of Forensic Science and Criminal Justice, Albany State University, GA worked on “Surface Chemistry of Gunshot Residue (GSR) Particles by X-ray Photoelectron Spectroscopy (XPS) and Time of Flight Secondary Ion Mass Spectrometry (ToF SIMS) - Complement to Electron Microscopy (SEM/EDX).” Gunshot residue particles that are discharged out of the firearm cartridge during firing along with smoke and fire are composed of unburnt and partially burnt particles either in the elemental form or molecular form. The hot gases and vapors coming out of the gun settle down at the surroundings or shooters hand and are specific to residues produced by the discharge of a gun. The particles (GSR) thus produced are collected and analyzed for the characteristics of the constituents. The objective is to determine whether or not a suspect fired a gun and hence to distinguish between real GSR particle and environmental contaminants. Scanning electron microscope equipped with energy dispersive x-ray spectrometer is used to detect the morphology and chemical composition of the discharged particles. Lead (Pb), Barium (Ba) and Antimony (Sb) are identified in the lead based GSR particles. Sodium (Na), Potassium (K), Aluminum (Al) and Calcium (Ca) are identified in the lead free based primers. The same specimens are further subjected to XPS and ToF SIMS analysis with a view to identify the respective surface chemistry, molecular nature and molecular Figure 93: GSR Particles mass of the GSR particles. The binding energies of the identified elements are shifted to higher values showing that these elements in GSR particles are in the oxidized form. Again the ToF SIMS shows peaks correspond to oxides of lead, barium and calcium apart from the elemental masses. 7.3.4 Special Focus/Leadership: Education: The NNIN’s Education and Outreach Office is housed at Georgia Tech. The staff consist of the NNIN education coordinator who oversees network, national and local efforts, a full-time assistant education coordinator whose primary focus is GT initiatives and a full-time education assistant (position vacant since 11/1/2011). Georgia Tech’s education program is a very active outreach program with more than 46 events directly reaching over 6,200 individuals. Our focus encompasses a variety of K-12 student programs, including on

NNIN Annual Report p.120 March 2011-Dec 2011 and off-site school programs; teacher professional development workshops; and presentations at local and regional science teacher meetings. We also offer professional workshops and have developed a program titled NanoFans – Nano Focusing on Advanced NanoBio Systems. The goal of the forum is to connect the medical/life sciences/biology and nanotechnology communities. NanoFans seeks to reach out to researchers in the biomedical/life sciences areas to inform them about what nanotechnology can offer them in the advancement of their research. The series offered two events: May 27, 2010 – Nanotechnology Application in Cardiology and November 18, 2010 – Nanotechnology in Drug Delivery. Approximately 240 participated in the events. We also hosted an inter-site workshop on graphene focused on current research trends. Georgia Tech is the lead on an NSF awarded RET program which includes Harvard, Howard, Penn State, and UCSB. During summer 2011, four teachers undertook research during their six-week experience at Georgia Tech and have designed classroom instructional units for use in high school science classes. These materials will be posted on the NRC website and are linked to Georgia Performance Standards thus making them a useful resource for Georgia science teachers (http://www.mirc.gatech.edu/education/instructional_units.php). The teachers also present their experience at the Georgia Science Teachers Association annual meeting. Georgia Tech also supported seven REU interns during summer 2011. One of these students will participate in the NNIN International REU in summer 2012. Georgia Tech also hosted two Japanese graduate students during the summer as part of the NNIN’s international Research Program for Graduate Students. The students came to us through NanoNet (Japan) and the National Institute of Materials Science in Tsukuba, Japan. They spent a total of 10 weeks doing research with faculty and graduate students. We also hosted one faculty participating in NNIN’s Lab Experience for Faculty (LEF) program which encourages nanoscale research by women and minorities. Our participant came from Albany State University in Georgia. We were also the host site for the NNIN REU convocation which had 115 participants over the four day event held at the Marcus Nanotechnology Building. In October, 2008 GT joined MCREL and Stanford’s NNIN site on a new NSF-funded (DRK-12) project titled NanoTeach. This 5 year, professional development program will develop a combination of face-to- face and online professional development experiences for high school science teachers. During 2011, Georgia Tech evaluated pre and post-survey answers and providing content support for the instructional model. We have also been active in developing the next implementation phase as well as in recruiting school districts. Georgia Tech was very active in providing teacher professional development workshops on how to include standards-based nanotechnology lessons into the science curriculum. We delivered workshops at national, regional, and local events for elementary, middle and high school teachers. Bio-Outreach: NRC technical liaisons attended, exhibited, and/or presented at numerous bio-related events in 2011. Events included Pittcon, APS, MRS, US-India Business Summit, Savannah Ocean Exchange, AVS. We also offer professional workshops and have developed a program titled NanoFans – Nano Focusing on Advanced NanoBio Systems. The goal of the forum is to connect the medical/life sciences/biology and nanotechnology communities. NanoFans seeks to reach out to researchers in the biomedical/life sciences areas to inform them about what nanotechnology can offer them in the advancement of their research. The series offered two events: May 18, 2011 – “Nano- and Micro-Technology in Neurology” and November 18, 2010 – “Nanomedicine. Approximately 235 reserachers participated in the events. Nano@Tech is a joint NRC education/outreach and research program.The featured speakers for the twice-a-month seminars come from all of the disciplines involved in nanotechnology research (including the social sciences), and the seminars represent an excellent opportunity for cross-pollination and

NNIN Annual Report p.121 March 2011-Dec 2011 collaboration forming.Attendees include faculty, graduate and undergraduate students from Georgia Tech and other local campuses, and professionals from the corresponding scientific community.Nano@Tech members (more than 500 on the mailing list) also support the NNIN Education and Outreach Office at Georgia Tech by providing volunteers for K-12 outreach activities.Since January 2008, 60 seminars have been held in this program and the attendance has steadily doubled over that time period.Most of these seminars have been captured on video and archived on the SMARTech website (http://smartech.gatech.edu/handle/1853/14205) where they have been viewed or downloaded as many as 2000 times. Finally, this past year began a new component of Nano@Tech with the inclusion of student mini-seminars each semester. Direct-2-Discovery (D2D), a program focusing on enabling student-to-researcher interactions in STEM by connecting classrooms to Georgia Tech researchers using sophisticated, high-definition videoconferencing technologies, was awarded $200k from the Arthur Vinings Davis foundation, and continues to reach middle and high schoolers throughout the US. ---End of Georgia Tech text report---

NNIN Annual Report p.122 March 2011-Dec 2011 7.3.5 Georgia Tech Selected Site Statistics (2011) a)Historical Annual Users

GaTech Cumulative Users- Historical

12 months 500 10 months foreign state and fed gov large company 400 small company pre-college 2 year college 4 year college 300 other university local site academic

200 Cumulative Annual Users

100

b) Lab Hours by Institution (10 months) c) User Distribution by Institution Type

Georgia Tech Lab Hours March 2011- Dec 2011 10 Months GaTech Users - March 2011 - Dec 2011 10 months

small company pre-college 2% state and fed gov 0% 4 year college 0% large company 2% large company state and fed gov small company 5% 1% 0% 8% foreign other university 2% 5% foreign 1% 4 year college 5%

other university local site 14% academic local site 65% 77593 Hours-10 months academic 89% 600 users - 10 months

d) Average Hours per User( in 10 months) e)New Users

200 200 Ga Tech Hours per user - March 2011-Dec 2011 10 Months 180 180 Ga Tech New Users Trained- March 2011-Dec 2011 (10 months) Does not include new remote users 160 160 140 140 120 120 100 100 80 80 New Users

Hours per User per Hours 60 60 40 40 20 20 0 0

Figure 94 Georgia Tech Selected Site Statistics

NNIN Annual Report p.123 March 2011-Dec 2011 7.3.6 Georgia Tech User Institutions (2011) Outside US Academic Small Companies Large Companies Boston University Accelent Massachusetts General Clemson C3 International Bard C R College of Wooster CardioMEMS CSP Technologies Covenant College CyOptics, Inc. Emory University EnGeniusMicro Honeywell Univ. of Central Florida Eotron Lockheed Martin Auburn H2Scan Milliken and Company Clark Atlanta University L-3 MVA Scientific Clemson Lehigh Technologies SanDisk Cornell MedShape Solutions Sensor Electronic Tech Kennesaw State University Molecular Imprints Solvay Advanced Polymers, LLC MIT Optical Filter Source WL Gore Morehouse School of PCB Piezotronics St Joseph's Hospital Medicine Oklahoma State University Physical Optics Corp. Kimberly Clark University of Georgia Toppan Interamerica U Missouri ViscidTech International Univ of South Carolina Open Cell Technologies Asahi Glass Univ. Alabama-Birmingham Icon Interventional CNRS University of Denver CorMatrix University of Florida Enumeral University of South Florida Epitaxial Performance Alloys UT Austin Western Michigan University State and Federal UNCC NASA - KSC Southern Poly State University NASA Ames Binghamton University US Army

NNIN Annual Report p.124 March 2011-Dec 2011 7.4 Harvard University Site Report 7.4.1 Facility Overview Year 8 (2011-2012) was another significant year of growth in users and capabilities for the Harvard University site. Highlights include a record number of users overall, record number of industrial users, and our all-time highest percentage of external users. During this review period several new instruments were added to our laboratories, and an Education and Outreach Specialist joined the staff. Numerous events were held at the Harvard site, particularly two major symposia held in January 2012: one in computational approaches to energy research (complimenting Harvard’s role as lead for NNIN/C), and the other in bio-inspired engineering (complimenting Harvard’s active Chemical Nanotechnology focus area). 7.4.2 Nanocompuation (NNIN/C) Summary Harvard continued as the headquarters for the NNIN computation technical area (NNIN/C) led by Dr. Michael Stopa who directs the network-wide computation efforts. NNIN/C provides high performance computing for advanced nanotechnology applications as well as support for experimental and theoretical studies. A fuller report of NNIN/C is given elsewhere, but highlights for computation at the Harvard site follow. This year, the Harvard node of NNIN/C continued to provide computational hardware, software tools and, most importantly, domain expertise to users internal to and external to Harvard University. Hardware. Regarding hardware support, the Harvard site continues to support users with access to both traditional processor clusters and also GPUs. The Graphical Processing Unit (GPU) parallel computing initiative of NNIN/C began in 2009 with the installation of the “Orgoglio” cluster at Harvard. In the years since, the user base continually grown and produced several interesting research accomplishments (see “Research Highlights” below). The Orgoglio cluster is one of only about ten such systems in the United States. It consists of quad-core Xeon ‘Harpertown’ processors running at 3 GHz and Tesla C1060 GPUs (a total of 96 cores and 48 GPU cards). The interconnects are QLogic 24-Port 9024 DDR InfiniBand. In addition, NNIN/C at Harvard University has announced the purchase of a new computational cluster for the general use of NNIN/C members, both locally and nationwide. The new equipment, which has been priced by Dell at $149,990, will consist of 480 nodes with each of the 80 Intel Xeon X5650 processors hosting six cores and having 24GB of memory. The system will be interconnected with gigabit Ethernet for rapid parallel processing, in addition to availability for use on serial jobs. The new cluster replaces the previous twin 112 node AMD Opteron clusters, which have now been taken out of service. Events. The largest NNIN/C event held this period was a three day conference in January 2012 on research topics in Energy computation, attended more than 100 researchers. This conference, “Synergy Between Experiment and Computation in Energy Research – Looking to 2030” followed in the tradition of past NNIN/C events by combining contributions for leading computational researchers with those of experimentalists. The conference was based around the four focus topics: fuel cells, catalysis, self- assembly and organic photovoltaics. More than fifteen internationally-renowned speakers presented at this major event. 7.4.3 Research Highlights The Harvard site continues to support a very broad range of research activities, spanning nano-materials, low-dimensional physics, microfluidic medical diagnostics, renewable energy, and optics. Graphene and diamond also continued as significant themes. Bio-inspired and bio-interface projects were numerous during the past year, fueled in part by the researchers of the Boston-based Wyss Institute for Biologically Inspired Engineering. Representative bio- related projects conducted this year included “Bio-MicroElectroMechanical (BioMEM) Device for Rapid Pathogens Detection,’ “Characterization of Bio-derived Optical Structures,” “Plasmonic Bio-Detectors,”

NNIN Annual Report p.125 March 2011-Dec 2011 “Research on Cephalopod Inspired Adaptive Photonic Systems,” “Bio-Inspired Dynamic Optical Devices,” and “Technologies for Design and Fabrication of Novel Bio-Polymeric Materials”. Two interesting examples of bio-inspired design come from the Aizenberg group at Harvard and the Wyss Institute. The first demonstates mechanical acutation based on pH. The group has developed a bio-inspired hybrid materials system by utilizing pH-responsive hydrogel as the “muscle” that dynamically and reversibly actuates embedded microstructures while the sample is submerged (Fig. 95). The chemo-mechanical actuation system is designed to provide uniform directional bending over a large area by utilizing

Figure 95: Overview of the pH based actuation mechanism. asymmetric “microfin” structures which have a structurally-determined preferred bending orientation. Such a chemically responsive, reversibly actuating surface that functions in a fluidic environment shows promise for applications ranging from propulsion to microfluidics. A second project from the Aizenberg group uses patterned, reactive surfaces to create a novel liquid identification system. (Fig. 96) They developed a technique in a highly ordered 3D photonic crystal, generating complex wettability patterns. When immersed in a liquid, the pores are selectively infiltrated in a unique spatial pattern – creating an optical fingerprint of that liquid through the color contrast between wetted and non-wetted regions. A remarkable selectivity of wetting is observed over a very broad range of fluidic surface tensions. These properties, combined with the easily detectable optical response, allow this system to be used as a colorimetric indicator for liquids based on wettability. This strategy of modifying the behavior of the liquid- surface interfaces through nanopatterning is common to many current projects. An example of this approach with high relevance to world health is the Figure 96: (left) Micrograph of highly regular inverse-opal project by the Karnik group at MIT related to “Vapor- structure; (right) multilevel encryption displaying different Trapping Membrane for Water Desalination”. The letters for different ethanol-water mixtures. availability of clean water is a major challenge that the world will face in this century. Reverse osmosis is the process of choice when energy efficiency is an issue, and the Karnik group is developing new membrane technologies for seawater desalination based

NNIN Annual Report p.126 March 2011-Dec 2011 on short hydrophobic nanopores that trap vapor; transport of water across the pores occurs when applied pressure exceeds the osmotic pressure. In another liquid-surface interface project, this time related to hydrogen fuel generation, the Mazur group from Harvard is investigating the use of laser-patterned titanium films for water splitting. This group can produce a range of nano-patterned surfaces depending on laser conditions and treatment with reactive gasses. Several groups are currently pursuing technologies for energy storage. One of the most advanced projects is that of local Massachusetts-based start-up Lilliputian Systems Inc. (LSI) which is developing a revolutionary miniature fuel cell for the $50 billion portable power market(Fig.97). LSI is pursuing a radically different technical approach (relative to other fuel cells) by implementing its fuel cell in silicon, using thin-film Solid Oxide Fuel Cell (SOFC) technology and Micro Electrical Mechanical System (MEMS)-based fabrication methods. Lilliputian is based less than 30 minutes from the Harvard campus, and are frequent users of the facility. Figure 97: Massachusetts-based Lilliputian Systems Another approach to energy storage is being developed power cell. The company has demonstrated mobile by Boston-based FastCAP, who use carbon nanotubes to device recharging stations based on the technology. improve an energy storage device called an ultracapacitor(Fig. 98). Unlike batteries, which store energy via chemical reactions, ultracapacitors store energy in electric fields. The devices possess enormous advantages over conventional battery technologies, including extremely long lifespans (over a million cycles, as compared to 10,000 for conventional batteries), unsurpassed ruggedness and durability, and low environmental impact due to their non- toxic internal components. However, ultracapacitors have fallen short of batteries in one key metric: energy density. FastCAP's ultracapacitor technology addresses this key metric by improving the internal electrode structures and the processes to produce them – improvements which allow them to combine the benefits of ultracapacitors and conventional batteries into one device, with none of the drawbacks of either technology. In the area of GPU-based nanosimulation, Dr.

Figure 98: Boston-based FastCAP researchers, and capacitor based Miriam Leeser of nearby Northeastern battery (inset). University has been active in the area of architecture considerations of GPU computation. Dr. Miriam Leeser is an internationally renowned researcher in massively parallel computing. She recently gave the keynote talk at International Workshop on Highly-Efficient Accelerators and Reconfigurable Technologies entitled: “The Challenges of Writing Portable, Correct and High Performance Libraries for GPUs or How to Avoid the Heroics of GPU Programming,” May 2011. From Dr. Leeser’s Abstract: Heterogeneous and homogeneous multicore processor architectures (NVIDIA Fermi, AMD Radeon, Intel Sandy Bridge, AMD Fusion) have emerged demonstrating significant increases in throughput in scientific applications over traditional single core processors. Each of these new processing

NNIN Annual Report p.127 March 2011-Dec 2011 elements varies widely in their processing capabilities, performance, memory systems, development environments, programming languages and debugging tools. In this rapidly increasing design space, programming for these platforms has become much more complex, error prone, and architecture dependent. Designing portable high-performance applications that can function properly across widely varied systems has become paramount. This work extends the Tasks and Conduits framework (originally developed at MIT Lincoln Laboratory) to support GPUs and heterogeneous platforms using NVIDIA CUDA and OpenCL. Running an application of Monte Carlo simulations of photon propagation, we have achieved 22x speedup porting the application from a single CPU core to a GPU with a change of only 5 source lines of code (SLOC) in addition to the GPU kernel. 7.4.4 Facility and Operations Highlights The laboratory spaces of the CNS facility were expanded through the commissioning of two new laboratory areas. The first change was to establish a new scanning probe microscopy facility. This new laboratory area has improved vibration characteristics compared to the initial SPM location, and the relocating of our existing SPM equipment and has already resulted in improvements in data. The second addition opened during this period is a new sample preparation laboratory which allows more working area for users with general sample work outside of the CNS cleanrooms. Our Biomaterials/cell culture facility was upgraded with several pieces of new or replacement equipment. The new cell counter, cell culture microscope, and warm water bath support projects that require the incubation and analysis of cell cultures. The major areas of research supported by the biomaterials facility are bioMEMS, biosensors, 3D cell cultures, and tissue engineering. Our ability to support user requirements for data analysis was improved by an on-site training session on VGStudio MAX software. This event held over three days in June 2011 was taught on by Dr. Daniela Handl from Volume Graphics and attended by several CNS staff members and MicroCT users. CNS infrastructure was also improved with software updates to both our laboratory access network and to our administrative business systems. In the laboratory, our “CNS Laboratory Equipment Access Network” (CLEAN) access management system was expanded to include several additional instruments such as our mask aligners, and new network and system monitoring routines were created that provide 24/7 alerts of system problems to our IT staff. Numerous minor modifications were made to the capability of the CLEAN system to manage instrument reservations and usage-reporting. A major modification was made to our administrative enterprise systems, improving their ability to convert the reservation and equipment logon/logoff data directly into electronic invoices. This electronic invoicing flow now allows for paper-free billing for equipment, using only the user-provided reservation and logon/logout history to produce both an electronic feed to automatically bill on-campus users through the Harvard accounting system, and to produce a second electronic feed which is delivered to a central campus A/R facility for billing of off- campus clients. Some of these results will be submitted for presentation to the UGIM2012 meeting at Berkeley in July 2012. These investments in enterprise automation are essential for the Harvard site to continue to support the ever-increasing number of researchers enrolling in our User Program. 7.4.5 Equipment Highlights During this review period several new instruments were added to the CNS portfolio, including those listed below: H2 generator. A major safety improvement to our cleanroom was accomplished when our new HOGEN S10 H2 generator was commissioned in nanofabrication facility. This system eliminates the need of expensive, dangerous, high pressure cylinders of hydrogen in the laboratory. With the flow capacities up to 4.7 SLPM, the generator provides high grade H2 gas for multiple processes in the cleanroom, including CVD film deposition, dry etching, diamond CVD growth, and inert gas mixing. With this generator installation, a SiH4/H2 mixing gas line was also added into the PECVD process to satisfy the need of a-Si

NNIN Annual Report p.128 March 2011-Dec 2011 growth for solar cell applications. Hall Effect Measurement System. In 2011 our film characterization capabilities were improved when a new MMR Hall and Van der Pauw Measurement System was installed in the nanofabrication facility(fig. 99). This system can be used to analyze the electrical properties of semiconducting films in the temperature range of 80 K-730 K with a variable magnetic field up to 1.4 Tesla (14,000 G). The system reports resistivity, sheet resistance, majority carrier type and concentration, mobility, and Hall coefficient as a function of temperature with a user friendly software package.

Upgrade of Elionix EBL system. To satisfy the growing usage Figure 99: New Hall measurement system. requirement of e-beam lithography, CNS upgraded the current 100 kV Elionix e-beam lithography system (ELS-7000) to the ELS-F125 system (Fig. 100). With the world’s first 125 keV acceleration voltage, the F125 can achieve a 1.7 nm beam diameter and write line width of 5 nm or less. Due to the higher writing current and faster scan electronics, the writing speed increased 6-10 times compared with the ELS-7000, providing CNS with much-needed increased throughput to support the site’s high demand for e-beam lithography. The new system was commissioned in late 2011 and already supports 50 users trained to run the system independently. Figure 100: New 125 kV e-beam lithography system. XeF2 etcher. Our support of the many MEMS projects in CNS was improved with the commissioning of a new XeF2 (xenon difluoride) isotropic silicon etch sytem (Fig. 101). XeF2 vapor phase etching exhibits nearly infinite selectivity of silicon to photoresist, silicon dioxide, silicon nitride and aluminum. Leveraging the strong equipment engineering skills within the Center, CNS staff designed and built the XeF2 etcher entirely “from scratch” at a fraction of the cost of a commercial system. Etch performance shows high etch uniformity, and the user interface is simple and intuitive. Direct laser lithography system. CNS added direct-write capability to our ensemble of lithography equipment with the trial addition of a Figure 101: New XeF2 etcher. Heidelberg “Small MicroLithography Engine” (SMiLE) system (Fig. 102). SMiLE is a microscope-based optical lithography direct write system, using a 390 nm LED UV light source. This system uses a DMD micro-mirror array to generate patterns, with up to 1 micrometer resolution in fine mode, and 3 micrometer resolution in standard mode. This system is suitable for direct writing applications, and for low volume mask making. Atom-Probe Tomography System: In January 2012 CNS acquired a Cameca 3D Atom Probe, which was awarded under NSF MRI Award 1040243. This new generation probe supports imaging atoms and identifying them one-by-one in a wide variety of Figure 102: Direct-write lithography systems. materials, including compound semiconductors and non-conducting oxides. Atom-probe tomography (APT), allows scientists and engineers to analyze specimens in three dimensions with atomic resolution, offering key insights into how a material’s nanostructure affects its

NNIN Annual Report p.129 March 2011-Dec 2011 mechanical and electrical properties. Information acquired by APT allows researchers to link phenomena that occur on the nanoscale to properties at the macro scale. The APT system enables material analysis in three dimensions with atomic resolution, offering key insights relating properties (brittleness, heat transfer, irradiation damage, carrier lifetime) to underlying nanostructural factors. APT’s ultra-high mass resolution enables it to differentiate between elements and their isotopes. Its pulsed-laser allows the 3-D analysis of composition and structure at atomic resolution in non-conductive systems such as ceramics, semiconductors, organics, glasses, oxide layers and even biological materials. (fig. 103) Specific applications include: 3-D Nanoelectronic and Optoelectronic devices, Nanocrystals and Nanowires, Heterostructures, III-V materials, Oxide semiconductors, High-temperature oxides, High-k dielectrics, Dopant distribution, Layer roughness, Thin films and coatings, Metallic Figure 103: Representative atomic resolution data from atom probe system. alloys, Superalloys, Precipitates and Carbides, Grain and phase boundaries, Cluster analysis, Dielectrics, Soft materials, Polymers and Biological samples (more difficult to prepare but possible). New Solid Ink Printer: Our support of the many microfluidic projects was improved through the commissioning of a new solid ink printer which enables users to fabricate paper-based microfluidic devices. Paper-based microfluidic devices work similarly to lateral flow assays. This technology provides an inexpensive and versatile platform for disposable biological and diagnostic assays, especially suitable for resource-starved regions of the world (the technique was developed by the Whitesides Group at Harvard University). The Xerox 8570 printer is a wax-based solid ink printer. Each ink droplet is about 50 to 60 micrometers. The wax, which is compatible with most aqueous solutions over a range of pH levels, forms a hydrophobic barrier to delineate the “walls” of the channels and reservoirs. Printing can be done on Whatman No. 1 chromatography papers, polyester-cellulose blend papers, ITW Technicloth, etc. The paper substrate serves as the “pump” medium using capillary action to generate fluid flow. The Cross Section Polisher: Our SEM sample preparation capability was improved through the commissioning of a new cross-section polisher that utilizes a broad argon ion beam for preparation of pristine cross-sections (Fig. 104). It is especially suitable for preparing ultra clean edges of materials such as multilayer thin films found in nanophotonic devices. Other techniques have the problem that they tend to smear the layers, and not produce atomically smooth cross sections. The new tool enables users to readily image cross-sections on the SEM. The CP is suited for preparation of any type of material or composite, especially specimens that are close to impossible to prepare mechanically. Examples include paper, solar and other thin films, very hard materials like diamond, soft materials like solder, and various polymers. Photoluminescence Spectroscopy System: In early 2012 the commissioning of a new photoluminescence system will allow Figure 104: Cross-section polisher. improved material characterization capability, augmenting our existing Raman and FT-IR systems. This new PL can be used to characterize material band gaps by looking at the radiative transitions after stimulation. A Quantel Q-switched Nd:YAG laser with 4 ns pulses is installed in LISE G04. The fourth

NNIN Annual Report p.130 March 2011-Dec 2011 harmonic of the laser (266nm) is used to stimulate photoluminescence from samples. A McPherson 2035 spectrometer with an Andor Newton EMCCD camera is used for signal detection. When the system is fully commissioned it will be capable of time dependent and temperature dependent (4K to 300K) measurements. 7.4.6 Staff Highlights During this review period, Jorge Pozo joined CNS as an Education and Outreach Specialist. Jorge Pozo, a 2010 biology graduate of Northeastern University, is also a decorated Army veteran who served in Operation Enduring Freedom in Afghanistan and is pursuing a Master's in Biotechnology at the Harvard Extension School. Under the direction of Dr. Kathryn Hollar, Jorge has been instrumental in expanding CNS education, diversity and outreach efforts during the reporting period. CNS also added an undergraduate intern supporting the cleanroom operation, and an undergraduate intern supporting the user administration office. Three additional hires to support the growing user community are planned for the upcoming year if funding can be arranged. 7.4.7 Education and Outreach Beyond training and technically supporting our very large population of NNIN users and other technical professionals, CNS staff members continued to support both broad educational activities and public outreach during the past year. In 2011-2012, CNS hosted or participated in activities that reached over 2000 K-12 students, teachers, families, members of the general public, and technical professionals. In many cases, we have partnered with school districts and organizations with large populations of students who are traditionally Figure 105: Cambridge 8th grade students learn underrepresented in science and engineering. Below about nanotechnology through interactive are highlights from the 2011-2012 education and demonstrations. diversity program.

K-12 and Public Programs Cambridge 8th Grade Science & Engineering Showcase. In May 2011, CNS and the Harvard School of Engineering & Applied Sciences hosted the first annual Cambridge 8th Grade Science & Engineering Showcase at Harvard (Fig. 105). Over 400 8th grade students from Cambridge Public Schools presented their science and engineering fair projects at Harvard, and participated in presentations and tours of Harvard research facilities. CNS staff hosted tours of the CNS facilities, led demonstrations, Figure 106: CNS Microscopist Carolyn Marks and also served as “questioners” during student leads demonstrations for John D. O’Bryant poster presentations. In addition, one of the classes, students. taught by former NNIN RET William McDonald, presented projects on “Demonstration of Self-Assembly by GeoMags” and “Engineering Structures with GeoMags,” based on an NNIN K-12 classroom module developed by Mr. McDonald.

NNIN Annual Report p.131 March 2011-Dec 2011 Targeted High School Partnerships: CNS has partnered with the John D. O’Bryant School for Mathematics and Science in the Boston Public Schools to support students in the school’s Engineering Pathways Program, and to provide science fair support for interested students (Fig. 106). The O’Bryant is one of three exam schools in the Boston Public Schools, and serves a diverse population (66% of students are from groups underrepresented in science and engineering). To kick off the partnership, 30 students and teachers visited CNS prior to the start of the school year for tours and demonstrations by CNS staff.

Boston STEP-Up Program: CNS is currently collaborating with Boston Public Schools to host the science portion of a series of visits by elementary schools in the Boston Public School District. Targeting 4th-6th grade students in underperforming schools, the STEP-Up program is an early intervention program designed to increase college and career awareness in at-risk populations. CNS is hosting 9 schools through the STEP-Up program, with an anticipated impact on over 270 students. CNS staff lead tours and

hands-on demonstrations, and talk informally about careers in science and nanotechnology. Figure 107: Tech Savvy participants construct a water drop maze from hydrophobic and hydrophilic Tech Savvy: In Summer 2011, CNS and SEAS hosted 30 materials. middle school girls from the greater Boston area as one of the sites in a week-long summer camp, Tech Savvy. (Fig. 107). Throughout the week, girls spend one day at each of the partner universities. At Harvard, NNIN RET Marianne Dunne and Education Specialist Jorge Pozo led a nanotechnology-based engineering design project in which the girls first ranked various fabrics (including Nanotex™- treated fabrics) according to their hydrophobic or hydrophilic characteristics. The girls then constructed a water-drop maze in which hydrophobic fabrics were the channels for a Figure 108: Education Specialist Jorge Pozo leads water drop, while hydrophilic fabrics constituted the maze demonstrations at Salud Y Familia. barriers and “dead ends.” As part of the activities, CNS staff also led an interactive tour of CNS facilities.

Salud Y Familia: Through this one-day information fair on health and science in October 2011, CNS Education Specialist Jorge Pozo introduced ~200 individuals from the Boston Latino community to the role nanotechnology has in the development new consumer products, as well as nanotechnology’s potential for improving healthcare. (Fig. 108)

Holiday Lecture for Families: CNS collaborates with SEAS, the NSEC and MRSEC to host an annual science-themed holiday lecture for families each December( Fig. 109). The theme of the December 2011 lecture was “Powerful Potential: Figure 109: Professor Howard Stone gives children instructions for illustrating electric current The Gift of Energy.” The highly interactive lecture was targeted during the 2011 Holiday Lecture.

NNIN Annual Report p.132 March 2011-Dec 2011 to ages 7 and up, with the goal of inspiring family discussions of science to continue after the lecture. Children received t-shirts that illustrate a scientific concept, and helped demonstrate that concept during the lecture. Over 800 people attended this year’s lecture.

Nanodays: CNS staff participated in Nanodays events at the Museum of Science in Boston, leading demonstrations and activities. NISE-Net Nanodays kits were also used in other outreach activities throughout the year. Undergraduate training and outreach As in years past, this June CNS staff conducted orientations and presentations for the 70 visiting undergraduate interns who were on campus. These students were largely beyond the five supported directly by the NNIN program and included those supported by our NSF NSEC and MRSEC. Subsequent to this orientation, many of these students conducted research activities in the CNS laboratories as part of their REU projects. Additionally, to encourage the use of facilities by undergraduates, CNS offers a 1-year cleanroom scholarship for any undergraduate (including non-Harvard students) performing research under the supervision of a faculty member.

Education specialist Jorge Pozo and Director of Educational Programs Kathryn Hollar have also publicized the NNIN REU program at several diversity conferences, including the annual conferences of the National Society of Black Physicists and National Society of Hispanic Physicists; the Society for Advancement of Chicanos and Native Americans in Science; the Annual Biomedical Research Conference for Minority Students; the Mexican American Engineering Society; and the Society for Hispanic Professional Engineers (as part of the SHPE NNIN workshop on nanotechnology). CNS also co- hosted a group of minority students from UC-Berkeley, the Cal NERDS, during a recent visit to Harvard in which they explored Figure 110: Energy Workshop summer and graduate opportunities. In October 2011 CNS conducted a poster contest soliciting material suitable for describing research projects conducted in the CNS laboratories to visiting school-age children. A Kindle Fire was offered as a grand prize, and the contest resulted in >40 submissions, the best of which were mounted in the LISE building. Workshops for technical professionals Beyond the technical events that are offered specifically for the CNS user community and employees, CNS conducts an on-going series of technical events open to the public and advertised generally in the Boston area. During the past 12 months CNS organized more than 50 public events which attracted >1700 attendees. This year the two largest of these were the two January 2012 symposia mentioned previously: “Energy - Synergy Between Computation and Experiment” attended by >100, and the “International Bio-Inspired Engineering Symposium 2012,” attended by >200. CNS hosted workshops each attended by >50 people in the areas of surface analysis, plasma etching, atomic layer deposition (ALD), low-pressure chemical vapor deposition (LPCVD), and physical vapor deposition (PVD). As in previous years, again during the summer of 2011 CNS staff conducted a free and public series of instructional classes in cleanroom technology. This “Nanofabrication Summer School” included 10 instructional sessions on cleanroom facilities, photolithography, mask design, E-beam lithography, RIE, CVD, PVD, ALD, metrology, scanning probe microscopy, and packaging process. In June, CNS hosted a one-day workshop entitled, “The world’s fastest AFM system and applications.” This event included a half- day of technology talks and discussion, and a half-day of system demonstrations. About 50 attendees, including some from out-of-state, attended this workshop.

NNIN Annual Report p.133 March 2011-Dec 2011 Several formal courses for non-Harvard students were conducted in CNS laboratories and were instructed by CNS staff members. Offered through the Harvard Extension School, these courses are typically held in the evenings as continuing education for the local community and do not require an application. During summer 2011, CNS Materials Facilities manager Dr. Fettah Kosar taught a 7-week- long summer course titled, “Introduction to Fabrication of Microfluidic and Lab-on-a-Chip Devices,” which was fully enrolled at 15 students. The course covered the field of miniaturization of pharmaceutical, biological, chemical, and biomedical assays. It served as an introduction to the facilities, tools and techniques used for the fabrication of microfluidic and lab-on-a-chip devices and reviewed some of the latest advances in this field. During the 2011 fall semester, CNS managers Dr. Jiangdong Deng and Dr. David Bell taught the course “Nanofabrication and Nanoanalysis,” also through the Harvard’s Extension School. This laboratory course explores the concepts of nanotechnology through nanofabrication and nano-analysis. Through fabricating real devices in the cleanroom students learned the complete nanofabrication processes from CAD design to fabricated structure. Several analysis techniques were applied to the devices and structures which were fabricated in class. For the second year, Dr. Fettah Kosar went off-campus to the University of Notre Dame in order to teach an invited 3-day course in microfluidics and soft-lithography techniques. This course had classroom and laboratory components, and was hosted by Prof. Bilgicer. In January 2012 a workshop in “X-ray Imaging and Tomography” was led by Materials group manager Dr. Kosar. X-ray imaging and computed tomography (CT) techniques are employed in many disciplines to non-destructively image and measure the internal structures of objects. This workshop will provide an introduction to the basic theory and practice of X-ray imaging and CT at micrometer length scales. It will take the students from the basics of X-ray generation to the methods of using X-rays to image internal features of samples and creating 3D images. The event was open to the public and no prior knowledge of X-ray imaging was required. On a lighter note, in January 2012 Dr. Kosar – who is also a pilot - conducted a public workshop on “Fundamentals of Aerodynamics” focusing on the fundamental understanding of the laws of aerodynamics and aeronautics. The concepts presented in this course were reinforced with three Saturday afternoon trips to local parks and airports for model and full scale demonstrations. 7.4.8 Society and Ethics John Sweeney, CNS Health and Safety Officer and SEI trainer attended a Congress at Arizona State University on “Teaching Social and Ethical Implications on Research”. John also presented a poster on SEI strategies from the Harvard site. The poster was based on Cornell SEI work available to John through the network of SEI coordinators. The new poster information is now shared each week at the CNS SEI training, which is a 20 minute segment of the mandatory all-user introductory safety training. This is the third time that the SEI training has been changed to better meet the needs of the NNIN program. --End of Harvard Text Report---

NNIN Annual Report p.134 March 2011-Dec 2011 7.4.9 Selected Harvard Site Statisitcs a)Historical Annual Users

Harvard Cumulative Users-Historical 600 12 months 10 months

500

400

Accurate Prior Year 300 Data Not Available Foreign State and Fed Gov Large Company 200 Small Company Pre-college 2 year college

100 4 year college

Cumulative Annual Users Annual Cumulative Other University Local Site Academic

0 FY04 FY04 FY05 FY05 FY06 FY06 FY07 FY07 FY08 FY08 FY09 FY09 FY10 FY10 FY11 FY11 Local Other Local Other Local Other Local Other Local Other Local Other local other local other

b) Lab Hours by Institution Type c) User Distribution by Institution Type

Harvard Users March 2011-Dec 2011 10 months Harvard Lab Hours March 2011-Dec 2011 10 Months

Small Company Large Company Foreign 9% Large Company Small Company 3% 0% 0% 12% Pre-college 4 year college 0% 1% 4 year college Other University 1% 16% Local Site Academic Local Site 75% Academic 57%

Other University 96,546 Hours 10 months 27% 976 Users - 10 months

d) Average Hours per User( in 10 months) e)New Users

180 180 Harvard New Users March 2011-Dec2011 10 months Harvard Hours per user March 2011 -Dec 2011 10 Months 160 160

140 140

120 120

100 100

80 80 Hours

60 New Users 60

40 40

20 20

0 0

Figure 111 Selected Harvard Site Statistics

NNIN Annual Report p.135 March 2011-Dec 2011 7.4.10 Harvard Site User Institutions (2011) Outside US Acacemic Small Companies Large Companies Boston College 1366 Technologies Alcatel-Lucent Boston University Agiltron American Superconductor Brown University AJA International Dow Chemical Bunker Hill Community College Applied NanoFemto Technologies EMD Chemicals, Inc. Case Western Reserve University Avedro, Inc. National Semiconductor Contra Costa Community College Axsun Technologies Novartis Cooper Union Bandgap Engineering Varian Semiconductor Equip. Cornell University Boston Microsystems, Inc. Schlumberger-Doll Research CUNY City College of New York Chemicro Engineering Dartmouth College Custom Nanotech, LLC. Eastern Nazarene College DNA Medical Institute Other Beth Israel Deaconess Franklin W. Olin College of Eng. E Ink Corporation Medical Center Howard University EOS Photonics Brigham and Women's Hosp. Massachusetts Institute of Tech. FastCAP Systems Corporation Children's Hospital Middlebury College GVD Corporation Dana Farber Cancer Institute Montana State University HabSel, Inc. Mass. General Hospital Mount Holyoke College Hybrid Silica Technologies, Inc. New York University Hyperion Catalysis International Small Companies Northeastern University Ingrain, Inc. (continued) Oklahoma State University Lightspin Technologies, Inc. Semprus Biosciences Rice University Lilliputian Systems, Inc. SiEnergy Systems, LLC. Rowan University Living Proof, Inc. SiOnyx, Inc. Simmons College Lumarray, Inc. Solid State Scientific Corp. SW Indian Polytechnic Inst. MC10, Inc. Sun Catalytix Stanford University Mears Technologies, Inc. Technic, Inc. Texas A&M University Microscale, Inc. TIAX, LLC. Tufts University Milli Sensor Systems Trelleborg Offshore Boston University of California - San Diego NABsys, Inc. Z Corporation University of Connecticut New England Analytical, Inc. Zena Technologies, Inc. Univ. of Illinois - Urbana Nth Degree Technologies ZS Genetics, Inc. Univ. of Massachusetts - Amherst OptoGration, Inc. Univ. of Mass. - Dartmouth Optron Systems, Inc. Univ. of Massachusetts - Lowell Paratek Microwave, Inc. Univ. of Mass. Medical School Pendar Medical University of Miami Pixtronix University of New Mexico Qmagiq, LLC. University of Puerto Rico Quanterix Corporation University of Rochester Radiation Monitoring Devices, Inc. Washington University in St. Louis Ramgoss, Inc. Wellesley College Sand 9, Inc. Worcester Polytechnic Institute Figure 112: Harvard User Institutions

NNIN Annual Report p.136 March 2011-Dec 2011 7.5 Howard University Site 7.5.1 Overview The National Nanotechnology Infrastructure Network (NNIN) has changed the model for user based research facilities in the US and at Howard University. The Howard Nanoscale Science and Engineering Facility (HNF) has been the vehicle and has lead to the Howard University Program for the Expansion of Research and Education in Nanotechnology (HUPEREN). Last year of funding under this program (HUPEREN) had included a major piece of capital equipment ( SEM/FIB Auriga from Carl Zeiss @1.5 million), funds for new faculty in the area of nanotechnology, lab fees for Howard faculty interested in Figure 113: Auriga CrossBeam Workstation using HNF, and small renovations of HNF. A picture of the Auriga is shown in Figure 113.. The AURIGA™ the new CrossBeam® Workstation (FIB-SEM) from Carl Zeiss SMT delivers on the nanoscopic scale and is install in LK Downing Hall. The system required more than five month to obtain a fully operational state and train a group users. As part Howard University Program for the Expansion of Research and Education in Nanotechnology (HUPEREN) a ‘state of the art’ Libra transmission electron microscope (TEM) use also purchased at a cost of over $600,000.This (TEM) uses electron translucent specimens with images directly projected on a screen or camera. Resolution better than 0.1 nm are now achievable, delivering atomic scale resolution. It is also fully operational and users of HNF can obtain user time. Several users have been trained. 7.5.2 Progress in Attracting New Users:

The HNF staff is quite aware of their mission to bring in Figure 114: Libra TEM outside users. This year we have had over a 200 users as of January 2012. This represents a 10% increase in the number of users (this is with the cleanroom shutdown for about one month with the new rennovations of LK Downing Hall). We believe that with the additional equipment and resources from HUPEREN, HNF will also add to the number of users. Two additional programs in the area of nanotechnology have been funded including the Center for Environment Implications of Nanotechnology with Duke University, Carnegie Mellon University, Howard University, and Virginia Tech University. Howard has also been rewarded an NSF-Integrative Graduate Education and Research Traineeship Program (IGERT) in the area of Environmental Nanotechnology. HNF is working actively to advertise and market to outside users from various populations and regions. We have been working with the Washington DC Small Business Development Center at Howard University and School of Buisness new “Gadget Center”. These potential users include private companies, government labs and other universities in the area and the nation though NNIN. (The statistics show the addition of several small business users and with the new clean space we are sure this number will increase in the next year.) Some of the new users this year include: • Carnegie Institution of Washington- Geophysical Laboratory • Aqua Nanotechnologies

NNIN Annual Report p.137 March 2011-Dec 2011 • Phantom Works-Boeing Corporation • Norfolk State University • Syracuse University • George Washington University • Williams College • Center for Aesthetic Modernism 7.5.3 Staff The staff support by HNF during 2011 include the following: Name Title % NNIN support James Griffin Lab Manager 30% Tony Gomez Support Technician 100% Crawford Taylor Research Associate 100% To be named Admin Assistant 100% Nefertiti Patrick-Boadley, PhD Admin/Research Associate 100% Tina Brower, Ph.D. Post-Doc 0 % Maoqi HE, Ph.D. Senior Research Associate 0 % William Rose, PhD Senior Research Associate 100% Chichang, Zhang, Ph.D. Post-Doc 0 % Andy Hai Tang Associate Lab Manager 0 % Jude Abanulo, Ph.D. Post-Doc/Lecturer 0 % 7.5.4 Education HNF has an impressive portfolio of educational activities across K-Grey, both formal and informal. The NanoExpress presents the complex and fascinating world of nanotechnology to the general public from K-Grey. The campaign was designed to provide information on the current state of research and development potential in nanotechnology. It also aims to promote the dialogue between the world of science and the general public. The NanoExpress is a trailer with a lithography area, 208 square feet of lab space and undergraduate and graduate lab assistants who help supervise hands-on experiments (Fig. 82). The NanoExpress touched over 8,911visitors and experimenters this year. Experimental areas include: Introduction to Passive Nanoparticles, Introduction to Self Assembly, Introduction to Micro and Nanofabrication, “Chips are for Kids”, Instruments for NanoScience and Technology and Shape Memory Alloys.The university purchased a new truck for the NanoExpress and WHUR the provided a new look. The NanoExpress was on the road for more that 40 days this year. The lectures and laboratory format has been very well received at elementary, junior and high schools (15), two year college and universities (6), adult groups, national conferences, museums, etc. The highlight of the 2011 Nanoexpress program was the fall, Historical Balck college and University Tabcoo Road Tour in November to three HBCUs in one week and we introduce over 500 students to Nanotechnology and the students performed nano technology experiments. Below is a list of some of the places the NanoExpress attended in 2011:

NNIN Annual Report p.138 March 2011-Dec 2011 EVENT Location # of Participants Cardoza High School Washington, DC 100 Dunbar High School Washington, DC 73 KIPP Schools Philadelphia Washington, DC 118 Booker T. Washington High Washington, DC 48 Georgetown -JSHS Washington, DC 140 Hampton University Hampton, VA 175 Va State University Petersburg, VA 220 Norfolk State U. Norfolk, VA 125 NSBE Region @ Baltimore, MD 650 American Society of Nanomedicine Shady-Grove, MD 120 Howard NanoExpress Day Washington, DC 74 Howard Homecoming Washington, DC 250 Smart Lighting Summer Program Washington, DC 15 US Black Engineer Baltimore, MD 3200 Boston Science Museum Boston MA 1000 Port Discovery Baltimore, MD 800 National Youth Medical Forum Washington, DC 29 CrossRoad Adventist School Washington, DC 45 Annunciation Catholic School Washington, DC 120 Exxon Summer Camp Washington, DC 25 Leadership Alliance Program Providence ,RI 1 Summer Program Washington, DC 35 TOTAL 7363

NanoTalk- (HUR Radio Channel 141 Sirius –XM) “Under the leadership of visionary General Manager Jim Watkins and the talented WHUR team, the Howard University Radio Network has become a trailblazer in radio,” said Howard University President Sidney A. Ribeau. “We are excited about the new frontiers and the opportunities that this venture holds for Howard University, our students, the community and the

world.” H.U.R. Voices embodies the mission of Howard University—to Figure 115: Nanotalk on serve “America and the Global Community”—by offering exciting, the radio WHUR educational and entertaining original programming that examines issues that affect people of color, including a unique mixture of talk radio, local and national news, and great music. On December 1, 2011, Gary L Harris launched his new radio show called, “Nanotalk”. Nanotalk is the technical newstalk show that examines topics related to science, engineering and technology. Nanotalk can be heard: ON-AIR: Wednesday 9am-10am RE-AIR: Saturday 4pm-5pm / Monday 12pm-1pm

Host Gary Harris provides technical information that is timely and relevant to the everyday listener. Nano Talk introduces the HURVOICES listener to the world of technology that is not discussed on a daily basis. Dr. Nancy Healy, NNIN Educational Coordinator has been a guest and we are planning on other

NNIN Annual Report p.139 March 2011-Dec 2011 members of NNIN to appear on the show. Sirius XM Radio is America's satellite radio company. SiriusXM broadcasts more than 135 satellite radio channels of commercial-free music, and premier sports, news, talk, entertainment, traffic, weather, and data services to over 21 million subscribers. SiriusXM offers an array of content from many of the biggest names in entertainment, as well as from professional sports leagues, major colleges, and national news and talk providers.

7.5.5 New Equipment The NNIN mission is to “enable rapid advancements in science, engineering and technology at the nanoscale by efficient access to nanotechnology infrastructure”. New major equipment acquired during the year include: We have finally completed the construction of the gas handling system and MOCVD (Thomas Swann- Aixtron) reactor with the help Structured Materials Industries in Piscataway, NJ. This reactor MOCVD reactor can build up many layers, each of a precisely controlled thickness, to create a material which has specific optical and electrical properties. Using this Figure 116: MOCVD technique it's possible to build a range of semiconductor photodetectors and lasers, the devices that lie at the heart of the information revolution. Users of the HNF can get a their MOCVD epi-layers grown here a new service for HNF (starting in early spring). Several users at HNF have requested a laser engraver. We have purchased a

Epi-Log Helix 24 50 watt CO2 laser. The Laser can engraving and cutting wood, acrylic, plastic, marble, fabric , glass & more. The will aid in the cheap MEMs projects like paper MEMs. Double Crystal Scintag Pad-V X ray Diffractometer It includes the goniometer and the other components listed, and it is a complete operating Scintag PAD-V X-Ray Diffraction system. Incorporated in this system are the following components: Figure 117: Laser • High voltage power supply Engraver • High voltage variable controller and input cable • High precision THETA and 2-THETA goniometer • Goniometry drive motor cable • Germanium Detector and liquid nitrogen Dewar • X-Ray tube housing • High voltage X-ray tube cable Several users have requested X-ray services. We have also submitted a Major Equipment Request to NSF with several groups at Howard for the acquisition of a small angle x-ray scattering (SAXS) system that will give us unprecedented resolution of particle size, shape, and interparticle interactions at length scales ranging from 1 to 100nm under the MRI Program 2012. The PI is Dr. Kimani A. Stancil who was part of the Laboratory Experience Faculty (LEF) program in Figure 118: Xray 2011. diffractometer 7.5.6 Nanotechnology Seminar Series The Howard Nanoscale Science and Engineering Facility sponsors a monthly Nanotechnology Seminar Series. The seminar schedule are submitted to the ScienceNet local internet newsletter sent to the Washington area science and engineering community. The series is sometimes co-sponsored with other organizations on campus. The following is a list of seminars in 2011:

NNIN Annual Report p.140 March 2011-Dec 2011 • “Fabrication and Characterization of Semiconducting Oxide Nanomaterials Using Horizontal Vapor Phase Growth Technique,” Dr. Gil Nonato C. Santos, Physics Department, De La Salle University, Taft Ave. Manila • “Simulations of the Solid Phase of Krypton and Argon on a Carbon Nanotube”, Silvina Gatica, Howard University, Department of Physics • “3rd American Society for Nanomedicine ASNM Annual Meeting”, 3rd American Society for Nanomedicine ASNM Annual Meeting, Dr. Roger Tsien, Nobel Prize Laureate 2008, will be the keynote speaker of the conference, co sponsor ASNM • “Nanotechnology in the 2010s: The Teen Years”, Pedro Alvarez, George R. Brown Professor of Engineering & Chair of the Department of Civil and Environmental Engineering, Rice University; Omid Farokhzad, Associate Professor, Brigham and Women’s Hospital, Harvard Medical School; Debra Kaiser, Supervisory Materials Research Engineer & Division Chief Ceramics, National Institute of Standards and Technology (NIST); David Kestenbaum, National Public Radio, Moderator. co-sponsor AAAS

• “How Science and Technology Can Accelerate the Development of Africa”, Dr. Cheick Modibo Diarra, Africa Chairman, Microsoft Corporation co-sponsor with College of Engineering • " Sustainable Energy and Environmental Justice”, Howard SEEDS Chapter of the Ecological Society of America, co-sponsor with Physics Department • “Fabrication and Characterization of Semiconducting Oxide Nanomaterials Using Horizontal Vapor Phase Growth Technique”, Dr. Gil Nonato C. Santos, Physics Department, De La Salle University, Taft Ave. Manila

• “Growth of SiC and Silicon Nanowires”, Karina Moore, Howard University • “Nanoscale Materials for Alternative Energy”, Prof. Richard Robinson, Cornell University, Materials Science Department, co-sponsor with Physics Department • “Next Generation of Advanced Polymeric Materials and Filtration Systems for Sustainable Water Purification", Mamadou S. Diallo, Ph.D.,Environmental Science and Engineering, CalTech, , co- sponsor with NSF-CREST 7.5.7 Renovations of HNF The entire LK Downing Hall is under going a face lift which includes painting, new bathrooms, new high tech lobby, new alarm system, etc. the total cost of these renovations in approximately three million dollars. Shown below is the outside of the building during renovations. The estimated time of completion is May 2012. 7.5.8 Research Highlights The main research thrusts for HNF are: Electronics and Materials - wide band gap devices and applications to nanotechnology. Characterization Science - the universally required tool for advancing research and technology across the physical, biological, materials and medical sciences and engineering disciplines. Nanofiltration membranes and technology - Figure 119: Renovation of membrane processes such as reverse osmosis (RO), nanofiltration (NF), LK Downing Hall at Howard University ultrafiltration (UF) and microfiltration (MF), which have applications in the fields of biotechnology, food science, chemical engineering, medical applications like artificial kidneys and

NNIN Annual Report p.141 March 2011-Dec 2011 more recently, environmental and geosciences engineering. Nanobubbles at Water-Solid Interfaces: Calculation of the Contact Angle Based on a Simple Model,. H. Elnaiem1 , D. Casimir1, P. Misra1 and S.M. Gatica: Nanobubbles have been found to form at the interface of water and solid surfaces. We examine the conditions for such bubbles to form and estimate the pressure inside the bubble based on thermodynamic considerations. Using a simple model we calculate the contact angle for a wide range of temperatures and hypothetical substrates possessing a continuous range of strengths. We show that as the temperature increases the shape of a bubble changes continuously from a spherical cap with low curvature to a complete sphere. An equivalent effect results from either increasing the strength of the solid or decreasing the surface tension. A model of a substrate formed by layers of materials is proposed to obtain a nanobub- ble with a particular contact angle. A Biocompatible SiC RF Antenna for In-vivo Sensing Applications, Shamima Afroz, S.W. Thomas University of South Florida: In recent years, considerable progress has been made in developing implantable biosensors that can continually monitor different health care issues such as glucose levels of a diabetic patient etc. However, to be truly beneficial, the implanted sensor must be able to function properly for an extended period of time. The biosensors developed thus far can only remain functional up to 10-30 days or months after their implantation in the body. Contributing factors for this loss of functionality include the degradation and fouling of the sensor, and the changes in the tissue surrounding the sensor such as fibrosis and inflammation. While researchers explore potential solutions to improve the current implantable biosensors, there is an urgent need to investigate alternative technologies and material of choice. Silicon carbide (SiC) is one of the few semiconducting materials that combine biocompatibility and great sensing potentiality. SiC chemical inertness, superior tribological properties, and well known hemocompatibility, make it a very promising candidate for in-vitro and in-vivo biosensors, biologically interfaced neural networks and intelligent implantable medical devices. The goal of this research is to develop, fabricate and characterize a fully biocompatible (SiC) RF antenna sensor that can remain functional in the body for years and will not require additional encasing. For example, this antenna sensor can be used as a continuous glucose monitoring sensor. Another application of this antenna would be a communicating device to other implantable sensors using telemetry unit integration. Development of titanium needle probes for neural recording, H. Yoon, D. C. Deshpande, V. K. Varadan, T. Kim, E. Jeong, and R. E. Harbaugh: The aim of this research is to develop a mechanically flexible and strong neural probe with microelectrode array for future clinical applications in neural prosthetics and neurological disorder fields. This research specifically focuses on the development of neural recording electrodes with iridium oxide (IrOx) electrodes on a titanium needle probe and discusses the fabrication techniques and their evaluation for physical properties and electrochemical performance. Microfabrication processes, such as inductive coupled plasma etching, were used to deeply etch the Ti needle structures on titanium foils, and microelectrode arrays with iridium oxide films were formed by electrochemical deposition for low impedance neural recording. Mechanical and electrochemical analyses were performed to verify the viability of Ti needle probes in vitro. The final section of this paper addresses the issue of magnetic resonance imaging artifacts of titanium needle probes, and test results are compared with similarly fabricated Si needle probes. The advantages of using a titanium needle probe are discussed in the application of neural probe electrodes, as well. Modification of sheet metal forming fluids with dispersed nanoparticles for improved lubrication, Mohsen Mosleh, Neway D. Atnafu (HowardU.) and John H Belk and Orval M. Nobles (Boeing Company): Sheet metal working fluids are used for reducing wear of forming sheets and dies and lowering friction at the die/workpiece interface. The reduction of friction and wear results in fewer defects and improved geometric and surface finish quality. In this paper, nanoparticles of several materials with known solid lubrication properties such as molybdenum disulfide (MoS2), tungsten disulfide (WS2), and

NNIN Annual Report p.142 March 2011-Dec 2011 hexagonal boron nitride (hBN) were dispersed in commercial sheet metal forming fluids by sonication and their tribological properties were evaluated using laboratory tribotesting. The sheet metal materials were titanium and carbon steel whereas 440C balls were used as the counterfaces to represent the die material. The experimental results indicated that in 440C ball-titanium sheet pairs sliding in the presence of the modified oil with nanoparticles, the wear volume of titanium sheets was reduced by as much as 25- 30% in certain nanoparticle particle concentrations. In the 440C ballsteel sheet sliding pairs, the wear volume of the 440C balls was reduced by as much as 55-65% using the modified fluid. The friction coefficient of ball-titanium systems was reduced by as much as 10% in some cases, but it showed no noticeable improvement in 440C ball-steel pairs using the modified fluid. Mechanisms by which modified oils with dispersed nanoparticles improve tribological behaviour are discussed. ZnO Nanowires Growth, Maoqi He, J. Halpern, and G.L.Harris: We have grown ZnO nanowires on Au particles by passing molecular oxygen over Zn metal. The growth system was the same as we use for growing nitrides. In a typical experiments, as shown about 1 g of Zn (6 9s pure) was put in a BN boat. Oxygen gas was passed over the boat at a flow rate of 2 sccm. Gold particles, about 2 nm across were used as a growth catalyst. They were placed on a Si substrate, which was located downstream between 10-50 mm from the Zn source. Both the Zn and the substrates were placed in quartz liner. The quartz liner was put in 1 m long quartz process tube, the center half of which was inserted into a tube furnace. The Zn was located at the center of the three zone furnace. After evacuation oxygen at 2 sccm and 10 sccm Ar used as a carrier gas flowed through the system. The temperature of furnace was raised to 870oC for 1 hour while maintaining the pressure at 10 to 15 Torr. Nanowires and combs were observed to grow only in the region where the gold particles had been deposited. The teeth on the combs are 100 nm to 200 nm in diameter and 10-15 μm long. Synthesis and Characterization of Graphene Materials and Films , R.D. Little and JW Mitchell; The investigation of the synthesis and functional derivitization of graphene, a one dimensional nanomaterial, was continued using vigorous oxidation of graphite in highly corrosive acids and oxidizing mixtures of permanganate. Methods were optimized to preclude the formation of the previously observed emulsions. Repeatable synthesis of 0.25 to 0.5 gm quantities of graphine oxide is permitting collaborations with external research partners. Graphene has unique properties that pose great potential for the use of surface absorbate/surface interactions, and the exploitation of electric field effects at surfaces to advance the analytical characterization science of nanomaterials. Hosten's and Mitchell's groups are interested in the investigation of graphene influence on surface plasmon resonance enhancements in silver nanoparticlestructures and the enhanced vibrational detection of molecutes by SERS. Graphene Oxide Normal Raman Spectra, R.D. Little and JW Mitchell; The normal Raman (NR) spectrum of graphene oxide (GO) is available. Pure graphene is known to give a signal at ca. 1565 cm-1. When the order of graphene is disrupted the 1565 cm-1 signal exhibits a blue shift and a second band centered at ca. 1360 cm-1 appears. The G band is centered at 1600 cm-1, while the D band emerges at 1365 cm-1. The oxidation of the graphene to form GO introduced oxygenated functional groups (i.e. hydroxyls, epoxides) to the surface of the layer. The encircled bands at 891, 981, and 1054 cm-1 are in good agreement with literature values for C-O stretching of various compounds. The weak feature at 620 cm-1 is due to the C-C=C bending of the GO sheet. The spectrum labeled GO liquid is the NR spectrum of the aqueous storage solution atop the GO suspension. This shows no discernible features. Electric field dependence of quantum efficiencies of Ag/n-Si composites in the infrared at room temperature, Chichang Zhangand C. Bates: Bates and Mitchell initiated fundamental studies and experimental scrutiny respectively of the surface charge and electric field distribution at surfaces of Ag-Si nanocomposites, doped silicon, and patterned silicon wafers. Room temperature quantum efficiencies of 2 μm thick Ag/n-Si composite films as a function of electric field are calculated for incident radiation wavelengths of 3, 5, 8, and 14 μm using a previously derived formula. With energies smaller than the Ag–

NNIN Annual Report p.143 March 2011-Dec 2011 Si Schottky barrier height, the signal current is carried by electrons tunneling through the barrier. For composites with Ag particle size of 5 nm, in an applied electric field of 2×106 V/cm, the quantum efficiencies are between 10% and 35%, depending on the wavelength. They increase rapidly with electric field and asymptotically approach a large fraction of the absorbed incident radiation in the Ag particles. Synthesis and Characterization Science of Nanomatter, R.D. Little and JW Mitchell; Thorough characterization science must establish the chemical and physical status of manufactured nanomaterials for assessing their environmental and biological effects, and monitoring their transformation during controlled laboratory experiments that simulate environmental conditions within various ecosystems. Mitchell is engaging the chemical engineering synthesis and characterization science of nanomaterials for bionanomolecular and intracellular research. Silver nanoparticles, stabilized with different molecular functionalities, are chemically engineered at scaled levels under pristine atmospheric and aqueous conditions. The most suitable processes for generating biocompatible formulations are being examined. Few, if any, previous investigations have examined the mass action effect chemistry and chemical dynamics occurring over the long term in aqueous nanoparticle systems with the objective of controlling conditions for the preservation of chemical purity and physical stability. Following synthesis, even under precisely controlled conditions , a resulting multicomponent nanoparticle system is produced with a quasi chemical equilibrium existing between excess Ag+ and stabilizer, nanoparticle oxides of Ag2O, AgO, clusters of neutral silver nanoparticles Ag0NP, Ag2NP, mixed ionized and zero valent clusters Ag NG+, and mixtures of AgNP's with different molar ratios of the stabilizing molecule Ag(NP)x. The equilibrium state may also be process temperature sensitive. Research to determine the stability of silver nanoparticles in aqueous media is paramountly important in view of the rapid application of silver in commercial products. Following the Centers pivotal work in the synthesis, and characterization of extremely stable Ag, - NP's, work continues to perfect quantitative techniques for measuring Ag, - NP's at 10-8 molar levels and below. Resonance light scattering investigations have examined all of the necessary factors impacting accurate measurements. Additionally, the most sensitive spectrophotometric methodology currently known for determining Ag + at ppb levels has been refined for determination of free Ag+ in prepared silver nano particle systems. The tetrabomophenathaline system is now used in the group for assessing the purity and percentage completion of chemical procedures to generate nanoparticles. The improved determination of Ag+ in nanoparticles formulation by application of the fluorescence enhancement of Cd sulfide quantum dots were investigated and completed. High Resolution Field Emission Scanning Electron Microscopy of Nanomaterials, JW Mitchell; Ultra high resolution (20nm) SEM micrographs of Ag PVP nanoparticles were obtained on a Zeiss SEM- FIB focused ion beam system to evaluate the instrumentation for acquisition by Howard University. Micrographs of synthesized silicon nitride nanowires in the corresponding nanopowder matrix were also acquired. The exceptionally clear micrographs elucidate the size distribution, physical homogeneity, and verified the solid-liquid-vapor growth mechanism of nanowires. Acquisition of a system is being pursued vigorously in collaboration with the Department of Biology. Bismuth spin filter, Prof. Tito Huber, Ajibola Adeyeye, Patrice Jones, and Yakushia Hill; Spin transport has generated much interest for applications such as storage, logic, and quantum computing. Our approach to spintronics is to exploit the spin-dependent transport inherent in mesoscopic structures and nanostructures that exhibit Aharonov-Bohm (AB) interference phenomena in the presence of a magnetic polarization can be intrinsic or be induced by an applied magnetic field. Such devices could also be useful for energy conversion because they imply unobstructed transport of entropy represented by the large degree of ordering inherent in a spin polarized current.Ultrafine Nanostructured Composites for Cooling Applications, Our objective is to advance the development of better solid state coolers that can be used in night vision goggles and infrared cameras. The cooling principle is not based on compressors that are noisy and large but is based on a thermoelectric semiconductors.[1] Solid state operation is silent

NNIN Annual Report p.144 March 2011-Dec 2011 and semiconductor technology is miniaturizable. Thermoelectric (TE) composites have the advantage of low thermal conductivity that improve substantially the thermoelectric figure of merit.[2] Statement of the problem studied: Nanostructured composites and nanowire arrays of traditional thermoelectrics like Bi,

Bi1-xSbx and Bi2Te3 have metallic Rashba surface spin-orbit bands featuring high mobilities rivaling that of the bulk for which topological insulator behavior has been proposed.[3] These surface bands appear because surfaces break the inversion symmetry, because there is a surface electric field that couples to electronic spin. The question that we addressed is the influence of the new surface in fine thermoelectric composites. We find that in fine composites, the surface bands participate and can dominate the transport properties of fine composites. [4] We have presented experimental results that show how to measure and test the relevance of the surface bands and have shown that these bands have to be considered in electronic transport. In the past, the spin-orbit surface bands were not considered. In fact typically confinement models [5] do not consider the surface bands from the outset. Since fine composites feature both surface charges and quantum confinement, in the future the two effects will have to be considered together. Summary of important results: In, 2010 we have made significant advances in the study of the thermopower of the surface bands by developing methods for analyzing magnetoresistance and thermopower and we also prepared samples that allowed us to measure all the relevant parameters (thermopower and mobility) together. In essence, we studied electronic transport and thermopower of Bi nanowires.[6,8] We found that individual nanowires and composites of Bi nanowires realize surface-only electronic transport since they become bulk insulators when they undergo the bulk semimetal- semiconductor transition as a result of quantum confinement for diameters close to 50 nm. We studied 20-, 30-, 50- and 200-nm trigonal Bi nanowire arrays. Shubnikov-de Haas magnetoresistance oscillations caused by surface electrons and bulklike holes enable the determination of their densities and mobilities. Surface electrons have high mobilities exceeding 20000 cm2sec-1V-1. This mobility is substantial, it is 2/3 of the value that is found for unsuspended graphene with significantly less charge densities.[8] How can charges that are on the surface of a solid have such high mobilities? The answer is that there are very few opportunities for scattering for these charges! Also, the theory of topological insulators is based on the observation that in some selected cases (semiconducting BiSb, for example or BiTe) there is also time reversal symmetry [3] and in these special cases the mobility is predicted to be extraordinarily high. In Bi nanowires, we find also that surface charges contribute strongly to the thermopower, dominating for temperatures T< 100 K. The surface thermopower is −1.2 T μV/K2, a value that is consistent with theory, raising the prospect of developing nanoscale thermoelectrics based on surface bands. The thermal conductivity of Bi nanowires has been measured and the results indicate that the phonon thermal conductivity is negligible compared with the electronic term in our case. We have prepared a manuscript,[9] that is posted in arxiv the open source journal, where we present an evaluation of the thermoelectric figure of merit in this case. At low temperatures, the values of optimal hypothetical material (please see the manuscript for a detailed account of this work) of surface states and of 50-nm Bi and of 45-nm Bi (0.95)Sb(0.05) exceed that of the other materials that are known to display excellent TE

properties at low temperatures CsBi(4)Te(6) and Bi1-xSbx . From this study it appears that nanowire arrays and composites based on nanowires of traditional TEs Bi, BiSb and also of other TEs that exhibit topological insulator behavior will be of practical interest for cooling. References 1. H. J. Goldsmid in “Electronic Refrigeration” (Pion Limited, London, 1986). 2. R. Venkatasubramanian, E. Siivola, T. Colpitts and B. O’Quinn. Nature, 413, 597 (2001). 3. M. Z. Hasan and C. L. Kane, Rev. Mod. Phys. 82, 3045 (2010). 4. T. E. Huber, A. Nikolaeva, D. Gitsu, L. Konopko, C.A. Foss, Jr., and M.J. Graf. Applied Physics Letters 84, 1326 (2004). 5. L. D. Hicks and M. S. Dresselhaus, Phys. Rev. B 47, 16631 (1993).

NNIN Annual Report p.145 March 2011-Dec 2011 6. L. Konopko, T. Huber and A. Nikolaeva. J. Low Temp. Physics. 158, 523 (2010) 7. T. E. Huber, A. Adeyeye, A. Nikolaeva, L. Konopko, R. C. Johnson, and M. J. Graf. Phys. Rev. B83, 235414 (2011). 8. K. I. Bolodin, K. J. Sikes, Z. Jiang, M. Klima, G. Fudenberg, J. Hone, P. Kim and H. L. Stormer, Solid State Comm. 146 351 (2008). 9. arxiv 1108.3356. "Thermoelectric prospects of nanomaterials with spin-orbit surface bands" by T. E. Huber, K. Owusu, S. Johnson, A. Nikolaeva L. Konopko, R. C. Johnson, M. J. Graf (Submitted to JAP on 16 Aug 2011). Developments in Nanoparticulate Drug Delivery Systems for Cancer Chemotherapy: Emmanuel O. Akala, Oluyomi Okunola and Simeon Adesina: Department of Pharmaceutical Sciences, School of Pharmacy, Howard University; A lot of progress has been made in the understanding of cancer biology and to design effective anticancer bioactive agents.However, at the moment, there is an imbalance between the knowledge of cancer biology and the success achieved in cancer treatment: efforts in the treatment of cancer have not met with much success. One of the main reasons for this situation is the inadequacies in the ability to administer bioactive agents so that they selectively reach the desired targets (cancer cells) with no damage to healthy cells. This limitation is also true of contrast agents for imaging applications. Thus to increase efficacy per dose of the therapeutic agent and contrast agent formulation, there should be efforts in the direction of targeting selectivity. To help meet the goal of eliminating death and suffering from cancer by 2015, the National Cancer Institute (NCI) is engaged in efforts to harness the power of nanotechnology to radically change the way we diagnose, image and treat cancer. In developing a cancer nanotechnology plan, NCI identifies major challenge areas of emphasis. This work highlights the developments in cancer nanotherapeutics (from first generation to the third generation nanoparticles for anticancer drug delivery systems). The efforts of our research group in fabricating multifunctional polymeric nanoparticles.

High Speed Switching Characteristics of Pt/Ta2O5/Cu Memristive Switch, P. Shrestha, A. Ochia, K.P. Cheung, J. P. Campbell, H. Baumgart and G. Harris: Accurately measure the transient details of switching memristive switch is crucial to the elucidation of the switching mechanism. Such high-speed measurements often plagued by artifacts. Here we describe a measurement technique capable of capturing Set/Reset characteristics of memristive switches with high accuracy. It can accurately measure the transient current during the Set/Reset operation with rise time as short as 2 ns. The circuit is designed to cycle through (Set/Reset) and sense (read the state) rapidly to enable the study of endurance. The sense circuit is able to measure currents as low as 30 pA yielding accurate measurement of the

resistance in the off state up to 1.6 GΩ. Pt/Ta2O5/Cu memeristive switches are examined that exhibit ON 4 4 and OFF state resistance (Ron and Roff) ratio of >10 and endurance cycles of >6x10 . Cancer Nanotechnology Center at Howard University, Paul C. Wang, Biochemistry Department, College of Medicine, Howard University; Nanotechnology is expected to revolutionize the diagnosis and management of cancer and will ultimately lead to personalized medicine.A multipronged effort from basic scientists, engineers and clinicians will be necessary for fulfilling this promise. Howard University is a premier HBCU with a rich tradition of producing scientists, engineers and clinicians with Ph.D. and other advanced degrees. The Cancer Nanotechnology Center at Howard University for training highly skilled and motivated researchers to propel this exciting field forward and reap rich rewards for mankind. The center is in the early stages of its development and will be relying on the support of the HNF. There are several other schools involved including George Washington University, Catholic University (Biomedical Engineering), and several other HBCUs. Synthesis of amphiphilic triblock copolymers as multidentate ligands for biocompatible coating of

NNIN Annual Report p.146 March 2011-Dec 2011 quantum dots, Tongxin Wanga Rajagopalan Sridharb, Alexandru Korotcova, Andy Hai Ting, Kyethann Francisc, James Mitchellc, Paul C. Wang: One barrier to the application of current tri- octylphosphine oxide (TOPO) based quantum dots (QDs) for biomedical imaging is that the TOPO on TOPO-QDs can be replaced by the proteins in living system, which may cause the degradation of QDs and/or deactivation of protein. In order to develop biocompatible optical imaging agents, a novel triblock copolymer, designed as a multidentate ligand, was synthesized to coat quantum dot nanocrystals (QDs). The copolymer consists of a polycarboxylic acid block at one end and a polythiol block at the other end with an intervening cross-linked poly(styrene-co-divinylbenzene) block bridging the ends. The multiple mercapto groups from the polythiol block act as multidentate ligands to stabilize QDs, while the polycarboxylic acid block improves the water solubility of QDs and offers reaction sites for surface modification or conjugation with bimolecules. The cross-linked poly(styrene- co-divinylbenzene) block provides a densely compacted hydrophobic shell. This shell will act as a barrier to inhibit the degradation of QDs by preventing the diffusion of ions and small molecules into the core of QDs. This new multidentate polymer coating facilitates the transfer of QDs from organic solvent into aqueous phase. The QDs directly bound to multidentate mercapto groups instead of TOPO are less likely to be affected by the mercapto or disulfide groups within proteins or other biomolecules. Therefore, this research will provide an alternative coating material instead of TOPO to produce QDs which could be more suitable for in vivo use under complex physiological conditions. Center for the Environmental Implications of Nanotechnology(CEIN), Kimberly Jones, Civil and Environmental Engineering, Howard University; The Center will address interactions of naturally derived, incidental and engineered nanoparticles and nanostructured materials, devices and systems (herein called “nanomaterials”) with the living world. Headquartered at Duke University, CEINT is a collaboration between Duke, Carnegie Mellon University, Howard University, and Virginia Tech and investigators from the University of Kentucky and Stanford University. Doping GaN Nanowires with Mn for Magnetic Applications, J.B.Halpern, C. Thomas, M. He, G.L. Harris and J. Griffin, Howard University; Using Mn metal power as a Mn source, NH3, as a reactive gas and N2 as a carrier gas we have been able to grow and dope nanowires of GaN. The purpose of doping the GaN nanowires with Mn is to produce nanowires that are magnetic and can be used in spintronics. GaN and Mnpowder are heated for two hours at 850ºC. The length of the wires was measured with typical values between 20 to 200µm. the diameter of the wires range from 20 to 200nm. The flow rates ofthe gases, growth temperature and distance from the source will be presented in detail. EDS and local photoluminescence have been performed of the as grown samples. Over 5% on Mn was found in the GaN wires. The PL spectrum indicates the presentsof both GaN and a impurity level associated with Mn in GaN. We will also report on the structural, magnetic and electrical properties of these nanowires. This work is being supported by NSF under the Partnership for Research and Education in Materials Program. Morphology and chemical composition of airborne Saharan dust during the AEROsol and Ocean Science Expeditions (AEROSE) Geoscience and Remote Sensing Symposium, Effiong, Esther B.; Morris, Vernon R.; Nalli, Nicholas R.: Howard University, NOAA Center for Atmospheric Sciences Washington, DC The morphology and chemical composition of aerosols associated with Saharan dust outbreaks between July 2006 and 2009 off-shore of the African continent above the tropical North Atlantic Ocean is investigated. Conducted aboard the NOAA research ship Ronald H. Brown (RHB). The trans-Atlantic AEROsol and Ocean Science Expeditions (AEROSE) are a series of intensive atmospheric field campaigns designed to investigate the surface chemistry and provide a unique data set to characterize the impact and microphysical evolution of Saharan dust during mobilization as a signature to different source regions. Elemental composition results for the 2006 AEROSE samples based on energy dispersive X-ray microanalysis system indicate a well-mixed dust-urban plume regime and reveal

NNIN Annual Report p.147 March 2011-Dec 2011 the presence of Al, C, Ca, Cd, Cl, Fe, K, Mg, Na, O, Pb, S, and Si; while the 2009 samples being predominantly dust aerosols were dominated by crustal elements such as Al, Ca, Cl, Cu, Fe, K, Mg, Na, O, P, S, Si, Sn, Ti, and Zn. The secondary electron images for both years reveal a variety of morphologies, but were dominated by chain-like association of spherules and non-spherical particles. Raman Microscopy affords an interpretation of the surface chemical processing and mixing state and revealed the presence of significant hydrocarbons in 2006, and sulfate for both years. Back trajectories show an outflow of air masses from Mauritania, Senegal, and a weak outflow from Algeria-Mali border for 2006 and Libya for 2009. Surface state effects on the thermopower of 30- to 200-nm diameter bismuth nanowires, T. E. Huber,A. Adeyeye, Nikolaeva,L. Konopko, R.C. Johnson, and M. J. Graf,: Many thermoelectrics like Bi and Bi(2)Te(3) exhibit Rashba spin-orbit surface bands [1] for which topological insulator behavior consisting of ultrahigh mobilities [2] and enhanced thermopower for solid-state energy conversion has been predicted. Most of the experimental evidence comes from angle resolved photoemission spectroscopy. There are few experimental realizations that demonstrate this behavior in electronic transport. Bi nanowires realize surface-only electronic transport since they become bulk insulators when they undergo the bulk semimetal-semiconductor transition as a result of quantum confinement for diameters close to 50 nm. We have studied 20-, 30-, 50- and 200-nm trigonal Bi wires via coupled measurements of resistance and thermopower from 4 K to 300 K.[3] In this work, the wires were also studied via low temperature magnetoresistance for fields up to 9 T. Shubnikov-de Haas magnetoresistance oscillations caused by surface electrons and bulklike holes enable the determination of their densities and mobilities. For 50 nm, a high degree of suppression of the bulklike contribution is achieved; in other words in 50-nm nanowires the surface conduction dominates over holes. Surface electrons are observed to have high mobilities exceeding 2 m2sec-1V-1 and to contribute strongly to the thermopower, dominating for temperatures T< 100 K. The surface thermopower is −1.2 T μV/K2, a value that is consistent with theory raising the prospect of developing nanoscale thermoelectrics of high figure of merit based on surface bands. In this presentation, we will review electronic transport including thermopower in topological insulators and also present our recent work where, using the same procedures as in [3], we test Te and Sn doped Bi nanowires in order to further improve the thermoelectric properties of the nanowires. References [1] Ph. Hofmann, Prog. Surf. Sci. 81, 191 (2006). [2] M. Z. Hasan and C. L. Kane, Rev. Mod. Phys. 82, 3045 (2010). [3] T.E. Huber, A. Adeyeye, A. Nikolaeva, L. Konopko, R.C. Johnson and M.J. Graf. Phys. Rev. B 83, 235414 (2011).

NNIN Annual Report p.148 March 2011-Dec 2011 7.5.9 Howard Site Statistics (2011) a)Historical Annual Users

Howard Cumulative Users-Historical 180 12 Months 10 Months 160

140

120 foreign state and fed gov 100 large company small company pre-college 80 2 year college 4 year college 60 other university local site academic

40 Cumulative Annual Users Annual Cumulative

0 FY04 FY04 FY05 FY05 FY06 FY06 FY07 FY07 FY08 FY08 FY09 FY09 FY10 FY10 FY11 FY11 Local Other Local Other Local Other Local Other Local Other Local Other Local Other Local Other

b) Lab Hours by Institution Type c) User Distribution by Institution Type

Howard Lab Hours March 2011-Dec 2011 (10 Months) Howard Lab Users March 2010-Dec 2010 (10 Months)

small company pre-college small company 1% large company 4% state and 4% large company 0% 2 year college fed gov 0% pre-college state and fed gov 0% 3% 4% 3% 2 year college 4 year college 2% 2% other university 15% 4 year college 0% local site other university local site academic 13% academic 75% 74%

196Users--10 months 17,746 Hours---10 months

d) Average Hours per User( in 10 months) e)New Users

80 Howard Hours per User 10 months March 2011-Dec 2011 Howard New Users 10 months March 2011-Dec 2011 300 70

250 60

200 50 97 new users 40 150

New Users 30 Hours per user per Hours 100 20 50 10

0 0

Figure 120: Howard Selected Site Statistics

NNIN Annual Report p.149 March 2011-Dec 2011 7.5.10 Howard User Institutions (2011)

Academic Small Company Cornell University Epitaxial Technologies John Hopkins U. Global Sustainability Alternatives University of Michigan Harris Aesthetics Geroge Washington U. Carnegie Institution of Washington Univ. of South Florida Georgetown Univ. Medical Center Large Company Lincoln University Lockheed Martin Norfolk State Ubiversity Boeing Company Univ. of North Texas Syracuse University Pre-College Wiiliams College Frank W. Ballou High School BlackFeet Comm College Bowie High School Harvard University Dunbar High School Gallaudet University Coolidge High School Calif. State Ponoma Archbishop Carroll High School Yale University Benjamin Banneker High School Prince George Community College

NNIN Annual Report p.150 March 2011-Dec 2011 7.6 Penn State University Site Report 7.6.1 Site Description and Technical Capabilities The Penn State NNIN site provides users with access to facilities that enable fabrication of a wide range of electrical, optical, and microelectromechanical devices to support fundamental and applied research in diverse fields spanning electronics to medicine. The primary focus of the Penn State Nanofabrication Laboratory within the NNIN is to provide specialized instruments and technical support in the areas of chemical and molecular-scale nanotechnology and complex ferroelectric oxide device micro- and nanofabrication. To support chemical and molecular-scale nanotechnology, we provide self assembled monolayer-based chemical patterning methods and deterministic nanomaterials assembly techniques from Penn State Materials Research Science and Engineering Center. The strong coupling between traditional top-down nanofabrication and bottom-up molecular self assembly provides a unique capability within the NNIN that can be used in applications where it may be necessary to flexibly derivatize surfaces with specific chemical and biological functionality. In addition, our site continues to build on Penn State’s strength in complex ferroelectric oxide material thin film deposition and device processing. We have established a comprehensive and integrated set of instruments to support the more stringent fabrication requirements associated with these material systems, which include Pb-based oxides. We work closely with Penn State faculty in the Smart Materials Integration Laboratory to develop and document robust baseline processes for complex oxide microelectromechanical system (MEMS) devices. The Penn State site has also invested in developing several deposition and processing capabilties that are new to the network, including infrared chalcogenide glasses, nanolithography on curved surfaces, and large area graphene. The specialized technical capabilities offered by the Penn State site were advertised at workshops, technical meetings, and on the NNIN web site. 7.6.2 External and Internal Research Highlights Columnar Chalcogenide Thin-Films for Fingerprint ID: A. Lakhtakia, R.C. Shaler, R.J. Martín-Palma, M.A. Motyka, and D.P. Pulsifer, Penn State University, University Park, PA Visualization of fingerprints obtained from physical evidence taken from crime scenes for subsequent comparison typically requires the use of physical and chemical techniques. Researchers at the Penn State NNIN site have developed a new conformal- evaporated-film-by-rotation technique to deposit dense columnar thin films (CTFs) on latent fingerprints on different types of surfaces. Thermal evaporation of chalcogenide (ChG) glass using Figure 121: Columnar ChG thin film this technique leads to the formation of a dense CTF on the deposition system developed at Penn State. Optical and FESEM images of fingerprint, thereby capturing the topographical texture with high ChG CTF on a fingerprint. resolution. (Fig 121) MEMS Membrane Devices Incorporating PZT for Biosensing Applications: F. Mathieu and L. Nicu, Laboratory for the Analysis and Architecture of Systems (LAAS), French National Center for Research (CNRS), University of Toulouse, Toulouse, FR Researchers at LAAS-CNRS, Toulouse, France are developing resonant micro-membranes to detect pathogenic agents that mimic bacteriological threats. Each micro-fabricated chip includes several Figure 122 :Left: A chip containing circular micro-membranes for multiplexed sensing. The actuation resonant micro-PZT membranes for and sensing scheme is based on the integration of a biosensing. Right: Microfluidic chamber with on-board electronics. NNIN Annual Report p.151 March 2011-Dec 2011 Pb(Zr0.30Ti0.70)O3 (PZT) piezoelectric thin film and a boron-doped Si piezo-resistor, respectively. The fully integrated device includes a fluidic cell and onboard electronics. The devices were fabricated using the Penn State NNIN baseline PZT process. In addition, staff members at LAAS-CNRS, the NNIN staff, and Penn State faculty members are collaborating to develop methods to manufacture PZT based nanodevices with high yield. (Fig. 122) Low-Cost Pyroelectric Detector Arrays: H. Beratan, Bridge Semiconductor, Pittsburg, PA The Penn State NNIN site is being used to deposit, pattern, and etch doped Pb(Zr0.30Ti0.70)O3 (PZT) pyroelectric films to develop infrared focal plane arrays for uncooled thermal imaging systems. Video frame-rate infrared imaging has been demonstrated upon integration with CMOS read-out integrated circuit (ROIC) electronics. (Fig. 123) . Ultimately, image quality is expected to be superior to other uncooled thermal imagers, including resistive Figure 123: Packaged PZT-based pyroelectric detector array integrated on bolometers. This process is currently being transitioned to a ROIC along with IR image collected foundry for commercialization. using this device. Epitaxial Grapene Transistors for High Frequency Applications: J. Robinson and D. Snyder, Penn State Electro-Optics Center, Freeport, PA Researchers at the Penn State Electro-Optics Center have demonstrated significant advancements in the growth of device quality epitaxial graphene on substrates up to 100mm in diameter. By eliminating the graphene-SiC interface through a process of hydrogenation the carrier mobility increases from an average of 800 cm2/Vs to >2000 cm2/Vs. Graphene transistors fabricated at the Penn State NNIN site using this epitaxial graphene show an increase in the current saturation from 750 to >1300 mA/mm, and in the transconductance from 175 mS/mm to >400mS. Figure 124: Top: FESEM of graphene RF transistors of The resulting graphene transistors demonstrate a 10X varying gate lengths. Bottom Bottom: Device data demonstrating 10X improvement in FET frequency improvement in the extrinsic current gain response response. with optimal extrinsic current-gain cut-off frequencies of 24 GHz or greater (Fig. 124). The epitaxial graphene wafers are being made available to external users through the Penn State NNIN site. 7.6.3 Facilities, Acquisitions, and Operations Facilities: The Penn State Nanofabrication Laboratory consists of approximately 6000 sq. ft. of clean room space and over 3000 square feet of supporting non-clean laboratory space located at our Materials Research Institute, Materials Research Laboratory, and Electrical Engineering West Building. Penn State took possession of the 275,600 gross sq. ft. Millennium Science Complex (MSC) in October 2011. The Penn State NNIN site is currently being relocated into a 10,000 sq. ft. class 100/1000 clean room with an additional 6500 sq. ft. of non-clean support space beneath the cleanroom. The move will be complete in July 2012. This building will bring together the core user instrument laboratories and the faculty/center research laboratories that support our NNIN focus areas, which will allow the Penn State site to better serve the network in the future. Acquisitions: Several new instruments are being added to Penn State NNIN site when the new MSC

NNIN Annual Report p.152 March 2011-Dec 2011 cleanroom opens. The new instruments bring significant improvements in patterning, thin film deposition, metrology and wet chemical cleaning and etching. The tools and capabilities are described below:

• Thermco 2604 Atmospheric Oxidation and LPCVD System: This four stack unit was purchased with NNIN ARRA funds, and it will provide wet and dry thermal oxide, silicon nitride, and doped/undoped polysilicon capabilities to the laboratory.

• Wave 4W-LANS Custom Multiple Target Ion Beam Deposition System: This programmable, load locked, multi-target, ion beam assisted deposition system was purchased with NNIN ARRA funds, and is equipped with an ultra low energy high intensity ion source, water cooled rotational stage for up to 100mm substrates, ports for in situ ellipsometry, and a residual gas analysis system. Processes are being developed to deposit novel infrared materials, including vanadium oxide and ChG’s.

• Vistec 5200ES Electron Beam Lithography System: This advanced nanolithography instrument was purchased with support from an NSF MRI award, and it will enable direct patterning of features on substrates having a variety of sizes and thicknesses, with demonstrated sub-10 nm pattern resolution and sub-15 nm stitching and overlay accuracy. It is equipped with a z-lift stage that allows software-controlled dynamic stage height adjustments for patterning on substrates with extreme topography and curvature, which will provide a unique capability in the NNIN. The system is currently being installed in the new MSC cleanroom.

• WAFAB Custom Electroplating Bench: The fully integrated, multi-bath plating bench was purchased with NNIN ARRA funds. Each of the three baths have rate controlled filtered circulation and customized electrode fixtures for plating 150 mm wafers to pieces.

• Lithography Systems: Several lithography tools acquired from Motorola Labs are being installed, including a GCA 8500 i-Line optical stepper, SVG coat/bake and bake/develop tracks, two Brewer Science resist apply and bake tracks, a Blue M oven, and a Fusion resist UV/thermal curing and processing station.

• Wet Chemistry and Lithography Benches: As part of the MSC cleanroom fitout, 10 custom WAFAB wet chemistry benches ( 3 acid/base clean, 3 solvent clean, 1 KOH/TMAH etch, 1 complex spin apply, 1 spin on diectric apply and 1 tube cleaning) and 7 custom WAFEB lithography benches (3 resist apply, 3 develop, 1 integrated hot plate) were purchased and installed.

• FEI Nova Nanosem 630 Field Emission Scanning Electron Microscope: This tool provides low voltage, high resolution (1.6nm resolution at 1kV), and variable pressure capabilities to image uncoated insulating and life science specimens. The system is equipped with elemental mapping via an energy dispersive spectrometry for detecting elements down to Boron.

• ZYGO NewView™ 7300 Optical Profilometer: The system provides non-contact, nondestructive optical profilometry capable of producing highly accurate, 3D surface topography measurements at heights from 0.1nm to 20 mm, with vertical resolution to 0.1 nm. It is ideally suited for measuring step heights and critical dimensions as well as statically or dynamically measuring MEMS devices.

• ADT 7100 Series proVectus™ Dicing System: The system is a versatile dicing saw equipped with a DC-brushless, 1.2 kW, Front-mounted, Air-bearing, closed-loop turntable Spindle optimized for multi-angle dicing of thin substrates with tight tolerance. The system easily cuts complex shapes on samples up to 8" in diameter. Operations: Oversight of the Penn State NNIN site is provided by the Materials Research Institute, which was established in 1996 to support interdisciplinary materials and device research and outreach to industry. The unit reports directly to the Vice President for Research and brings shared resources

NNIN Annual Report p.153 March 2011-Dec 2011 including information technology, outreach, and web design personnel as well as professionals who have experience coordinating workshops and industrial outreach events. 7.6.4 Education, Outreach and SEI Education: The Penn State Nanofabrication Laboratory undertook activities to (1) introduce K-12 students to nanotechnology, nanofabrication, career opportunities, and educational pathways; (2) provide training to teachers about the discipline of experimental sciences and enhance their enthusiasm for having students pursue careers in science; and (3) provide hands-on nanotechnology summer research with state-of-the-art equipment for undergraduate students. The Penn State NNIN hosted a science teacher from Park Forest Middle School in State College PA, a science teacher from Central Cambria High School in Cambria PA, and a physics teacher from St. Hubbert High School for Girls in Philadelphia PA. The teachers researched the antibacterial properties of Ag nanoparticles applied to bandages under the supervision of Dr. Christine Keating, a professor in the Department of Chemistry, and Dr. Steven Keating, a Senior Lecturer, in the Biochemistry and Molecular Biology department. The teachers created engaging, hands-on and affordable lessons to introduce high school students to the field of nanotechnology and to demonstrate its relevance to their lives. The RET program supported 2 female teachers. Penn State hosted 5 undergraduate students for the summer NNIN REU program. In addition to training students to operate the equipment necessary to complete their summer projects, the students participated in weekly professional development training, weekly seminars, a Penn State symposium with several REU programs, and the NNIN convocation. The REU program supported 2 women and 2 underrepresented minority students. The Pennsylvania Nanofabrication Manufacturing Technology program offered an 18 credit capstone semester to 22 associate and 31 baccalaureate students from across PA. The defining feature of the partnership is the sharing of the nanofabrication facilities, staff, and faculty at Penn State with educational partners across the Commonwealth. As part of the NSF National Center’s Work, the nanofabrication facility and staff participate in the educator workshops, which are targeted at community college instructors across the country where “Teaching Cleanroom” was taught. Five on-site workshops were taught, with 49 educators attending the 5 workshops. Outreach: The Penn State NNIN site continues outreach activities to inform potential users in academia, national laboratories, and industry of our general technical capabilities and specific focus areas. Our user outreach activities for 2011 are summarized below:

• Tradeshow/Conference displays: The Penn State NNIN site advertised its capabilities at the ONR International Workshop on Acoutic Transduction Materials and Devices in March 2011, and the Center for Dielectric Studies Spring Meeting in April 2011. These meetings were aattended by by over 200 participants, representing over 50 companies. The NNIN site provided a display at the Pennsylvania Regional Nanotechnology for Industry Conference that was held in May 2011 at Drexel University in Philadelphia, PA. The display was visited by nearly 100 attendees.

• Special Events: The Penn State NNIN participated in Penn State Exploration Day 2011, which showcases science activities to students in grades K-12. This event featured interactive activities, multimedia presentations, student developed displays and activities, and planetarium shows. Over 2,000 people attended the event.

• Facility Tours:The Penn State NNIN provided more than 20 outreach tours for over 200 participants. A sample of academic and industrial participants included Quest Integrated, SciTech Solar LLC, Princeton University, George Washinton University, Boeing, Tsinghua University, China, Sunlight

NNIN Annual Report p.154 March 2011-Dec 2011 Photonics, Washington University, and Deltronic Crystal Industries.

• Industrial Visits: The Penn State NNIN site was described at nanotechnology-focused industrial and government visits: Office of the Under Secretary of Defense for Intelligence, the National Magnetic Field Lab, PPGPhillips Ultrasound Division, Pratt Whitney, CyOptics, Boeing, Deltonic Crystal Industries Inc.. These visits were attended by scientists, engineers, and executives. SEI: The Penn State NNIN site developed and integrated new SEI material into the User Orientation sessions. The material includes a slide show and a reader entitled “Overview of the Etchical Dimensions of Scientific Research,” authored by Dr. Erich Schienke, Assistant Professor of Science, Technology and Society at Penn State. The material is formatted for iPads and other tablet devices for easy viewing. In collaboration with Dr. Richard Doyle, a Professor of Rhetoric and Science Studies in the English Department, the Penn State NNIN continued its efforts to assemble all SEI interested groups at Penn State into a central organization. The intent of this effort is to promote scholarship in the area of SEI, and to bolster research programs and proposals in nanotechnology related SEI research. ------End of Penn State Text Report-----

NNIN Annual Report p.155 March 2011-Dec 2011 7.6.5 Penn State Selected Statistics (2011) a)Historical Annual Users

Penn State Historical Users

500 12 months 450 10 months

400

350 foreign state and fed gov large company 300 mo) small company

10 pre-college 250 2 year college 4 year college 200 other university local site academic 150

100

Users in Period or (annual in Users 0 FY04 FY04 FY05 FY05 FY06 FY06 FY07 FY07 FY08 FY08 FY09 fy09 FY10 FY10 FY11 FY11 Local Other Local Other Local Other Local other local other Local other Local Other Local Other

b) Lab Hours by Institution Type c) User Distribution by Institution Type

Penn State Lab Hours - March 2011-Dec 2011 10 months Penn State Lab Users March 2011- Dec 2011 10 months

Small Company small company 9% 4 year college Large Company 6% large company 0% 2% 4% 4 year college 1% Other University 2% other university 5%

Local Site Academic 87% local site academic 84% 37,573Hours- 10 Months 425 users--10 months

d) Average Hours per User( in 10 months) e)New Users

160 200 Penn State Hours per User - March 2011-Dec 2011 10 months Penn State New Users - March 2011-Dec 2011 10 months 140 180 160 120 140 100 120 80 100 80 60 New Users

hours per user per hours 60 40 40 20 20 0 0

Figure 125: Selected Penn State Site Statistics

NNIN Annual Report p.156 March 2011-Dec 2011 7.6.6 Penn State User Institutions (2011) Outside US Academics Small US Companies Large US Companies Alfred University Advanced Cooling Tech. FCI USA, LLC Arizona State University AGR International Inc Air Products And Chemicals Inc Carnegie Mellon University Bio Armor Inc B. Braun Medical Inc City College of New York Bridge Semiconductor Corp BTU International Clarion University of PA Concurrent Technologies Corp. Corning Inc Cornell University Flexible Medical Systems, LLC Eastman Kodak Harvard University ImTech, Inc. FLIR Systems, Inc. Johns Hopkins University Leversense, LLC GEIT Louisiana Tech University Pellion Technologies, Inc. Lexmark International, Inc MIT Ramtron International Corp. Philips Healthcare Norfolk State University Scitech Associates, LLC Philips Lumileds Texas A & M University Silberline Spectrum Control Inc. University of Akron SilcoTek Corporation Standard Steel LLC University of Illinois Spectrum Devices University of Maryland Strategic Polymer Sciences, Inc. State and Federal Uni. of N.Carolina at Charlotte Titan Spine, LLC Government NASA Marshall Space Flight University of Pennsylvania TRS Ceramics Center University of Pittsburgh TRS Technologies University of Rochester Unilife Corp X-ray Diffraction Services

NNIN Annual Report p.157 March 2011-Dec 2011 7.7 Stanford University Site Report 7.7.1 Facility Overview The Stanford Nanofabrication Facility was awarded funds under the NSF-sponsored ARI-R2 program that is allowing a number of critical building infrastructure items to be upgraded. Stanford University has added to that amount to fund a variety of deferred maintenance activities. Key elements that will allow us to support the needs of the research community include: • Improved electrical and process cooling water capacity to better meet future equipment needs. • Improved humidity control in lithographic patterning areas of SNF to allow better control of exposure and developing processes. • Addition of several new gas cabinets, lines, and valve manifold boxes to better support future research needs and to allow better isolation of tools sharing a single gas cylinder. Key elements of the renovation that will allow us to improve the overall safety of this shared research operation include:

• Installation of a new, more comprehensive toxic gas monitoring system. • Installation of double-contained hydrofluoric acid waste piping.

• Installation of a new scrubber to treat the effluent of LPCVD tools. The renovation includes the expansion of shared laboratory space into a former workshop area. The Nano-Structures Integration Laboratory, or “n-SiL” will complement the existing main Fab by providing resources for processes not allowed in a cleanroom, such as nanoparticle synthesis and surface modification. The new n-Sil will facilitate integration of “bottom-up” bulk nanosynthesis with nanofab “top-down” approaches to device construction. While the renovation grant supports only construction of the infrastructure for the n-SiL (namely lab utilities and fume hoods), Stanford’s Nano- science and Nanotechnology Initiative will support acquisition of new equipment to outfit the lab. In addition, SNF plans to hire a Ph.D. chemist to provide dedicated technical support for the lab and its researchers. Managed by SNF, the new n-SiL will be an open, shared resource for researchers to explore new materials and structures.(fig. 126) This renovation project has undergone detailed planning during the past year and actual clean room construction is taking place between December 15, 2011 and February 1, 2012. The n-SiL will be complete in late February. Figure 126: Stanford Nanostructures Integration Lab n-SiL 7.7.2 Equipment During the past year, SNF has installed the following pieces of research equipment that were purchased with NNIN ARRA funds:

NNIN Annual Report p.158 March 2011-Dec 2011 • A Cambridge Nanotech Fiji 202, dual chamber ALD tool, with enhance ozone and plasma deposition capabilities. • An IntlVac multi-target ebeam evaporator. • An IntlVac multi-target sputtering tool with a broad range of reactive sputter capability. • A PlasmaTherm capactively-coupled PECVD tool for silicon-based, doped/undoped films including silicon carbide. • A PlasmaTherm inductively-coupled PECVD tool for low temperature deposition of silicon-based films. More recently, we have purchased, but not yet installed, four new plasma etch tools with funding provided by Stanford University. In addition, NNIN capital funds have been used to modify and bring up two Thermco oxidation furnaces, replace two RTA systems, refurbish an SVG 8800 dual coat track system, and update/replace two dual stack spin rinse dryers. 7.7.3 Staffing After a nationwide search, the SNF recruited Dr. John Bumgarner as the Operations Director in July 2011. John has implemented a “functional area” structure that aligns maintenance and process staff into one group for each area, with a single supervisor. In addition, he has instituted a daily pass-down on tool status, which has already improved the up-time of key fabrication tools. The position of installation engineer has also been established, in order to make tool start-ups smoother by coordinating the facilitization and permitting processes. Dr. Bumgarner brings 30 years of post-bachelor’s experience to SNF, having come to us from SRI International, where he was doing government-funded research, while managing two MEMS fabs, one in Largo, Florida and one in Menlo Park, California. Previously he has worked at Kyma Technologies, a start up in GaN, as Engineering VP, at Intel as Process Integration, Yield, Team Lead and Group Leaders at PTD in Oregon and at the Fab22 start-up in Arizona, and at GE Neutron Devices as a Development Engineer. He has a Ph.D. in SiC technology with Prof. Bob Davis at North Carolina State University, and an M.S. and B.S. from Northwestern University, all in materials science and engineering. 7.7.4 Research Highlights Some research project highlights for this year include: From industry: Alces Technology, Inc.- CMOS-Compatible Laser MEMS Microdisplay The Bosch Group.- ALD-Metal Bolometer and Capacitive Pressure Sensors (Fig.127)) Corium International, Inc.- Microstructures for Transdermal Drug Delivery DxRay, Inc.- Silicon Nanowire Arrays as Silicon Photomultipliers (SiPMs) for Medical Imaging OndaVia, Inc.- Portable Raman Spectroscope Based Instrument with Figure 127: The Bosch Group Single-Use eSERS Cartridges for Field Measurements NuPGA/Monolithic 3D, Inc.- Low Temperature Junctionless Transistor Suitable for Monolithic 3D From non-Stanford academics: Prof. Unyoung Kim - Biotechnology, Santa Clara University - Concentrating and Detecting Waterborne

NNIN Annual Report p.159 March 2011-Dec 2011 SNM Pathogens for Resources-limited Settings Chip Blood Prof. Luke Theogarajan - Electrical and Computer Engineering, University of California, Santa Barbara - Graphene Nanopores on CMOS PTFE Prof. Shuvo Roy - Bioengineering – University of California, San Francisco - Grafts Nanotechnology-enabled Artificial Kidney (Fig. 128) From Stanford: Profs. C. Chidsey - Chemistry, and D. Goldhaber-Gordon – Physics - High- Yield Nanoscale Molecular Junctions Figure 128: Nanotechnology- enabled Artificial Kidney Prof. G.T.A. Kovacs - Electrical Engineering - Microfluidic Impedance Spectroscopy. Profs. J. Harris and D.A.B.. Miller - Electrical Engineering - Ge/SiGe Quantum Well Waveguide Modulator. Profs. M. Brongersma - Materials Science & Engineering and D.A.B. Miller - Electrical Engineering - Nanometer-scale Two Conductor Waveguides for On- Chip Optical Interconnects.

Profs. S. Mitra, R.T. Howe, and H.-S. P. Wong - Electrical Engineering - Figure 129: Lateral NEM Lateral NEM Switch Technology for Robust, Low-Power Digital Systems. (Fig. Switch Technology for Robust, 129) Low-Power Digital Systems Prof. B.T. Khuri-Yakub - Electrical Engineering - Volumetric Intracardiac Ultrasound Imaging (Fig. 130) Prof. W.E. Moerner – Chemistry - Anti-Brownian Electrokinetic Traps for Studying Cooperativity in Individual Multi-Subunit Enzymes. Prof. B. Pruitt - Mechanical Engineering - Self-sensing, Coaxial-Tip Scanning Probes. Prof. K. Saraswat - Electrical Engineering - High Mobility III-V PMOS. Figure 130: Volumetric Intracardiac Prof. J. Vuckovic - Applied Physics - Electrically Pumped Photonic Ultrasound Imaging Crystal Laser (Fig. 131) Prof. S. Wong - Electrical Engineering - 3D-FPGA (Fig. 132) Prof. R. Zare – Chemistry - High-Throughput Selective Single-Cell Capture Prof. X. Zhang - Mechanical Engineering - Passivation Studies for Efficient Silicon Wire Radial Junction Solar Cells Computational research highlights for 2011 include Prof. Yi. Cui and Dr. Q. Zhang, Material Sciences and Engineering, Stanford University - Topological Insulators. Figure 131: Electrically Pumped Photonic Crystal Laser Prof. R. T. Howe and Dr. C. Gupta, Electrical Engineering, Stanford University - Quantum Tunneling Biomolecular Sensor Platform.

NNIN Annual Report p.160 March 2011-Dec 2011 Figure 132 3D-FPGA ,:Prof. S. Wong

Prof. Y. Nishi, Dr. S.-G. Park, Dr. H. Lee, and Dr. B. Magyari-Köpe, Electrical Engineering, Stanford University – Resistive Switching Mechanisms in Transition Metal Oxides Based Random Access Memory Devices. Prof. E. Reed, Materials Science and Engineering, Stanford University - Engineered Piezoelectricity in Graphene. Prof. K. Saraswat, J. Harris, and Y. Nishi and Dr. B. Magyar-Köpe, Electrical Engineering, Stanford University – GeSn Technology: Extending the Ge Electronics Roadmap. 7.7.5 Educational/Computational/Societal and Ethical Implications of Nanotechnology Highlights Education/Outreach Activities SNF was again involved in a variety of different educational and outreach activities. In the 5-year NanoTeach program, funded by NSF through a DLR grant and by NNIN and involving the Georgia Tech site and Mid-continent Research for Education and Learning (McREL), SNF is developing and testing a combination of workshop and online professional development experiences for high school science teachers to incorporate nanotechnology into their curriculum. This past year SNF assisted the Pilot Testing teachers in their incorporation of nanoscience content into their classrooms, provided expertise in the assessment component, participated in the 2nd-year Pilot Testing workshop, and began to plan for the the 2-year Field Testing with 150 teachers across the country. SNF again participated in the week-long Summer Institute for Middle School Teachers, organized by the NSEC Center for Probing the Nanoscale at Stanford. SNF also took part in the People-to-People program, including a seminar, demonstrations, and live virtual webcam cleanroom tour to 180 US and international high school students. In addition SNF hosted numerous local school groups, including middle schools, high schools, and our local community college, for presentations, demonstrations and tours of the facility. For these we have develped a photolithograpy demonstration/activity in which photograph images are etched into silicon wafers for the students. In the area of mass media, SNF has been working with Silicon Run Productions in their NSF- funded program to produce a film on nanoscience and nanofabrication, which is due out March. SNF hosted 6 REU students last summer, and as part of the NNIN Laboratory Experience for Faculty program, Professor Ashley Kim from Santa Clara University worked on “Microfluidic multi-target cell sorter for point-of-care testing,” in Prof. R. T. Howe’s group. SNF staff also contributed to NNIN activites at national and state conferences such as the Society for Hispanic Professional Engineers in Anaheim and the California Science Teacher Association Conference in Pasadena.

NNIN Annual Report p.161 March 2011-Dec 2011 Computational Infrastructure The Stanford NNIN Computing Facility (SNCF) consists of a 64 node, 512 CPU Linux computer cluster and supported the research work of a total of 53 users (40 internal and 13 external). Users on the cluster utilized a wide range of simulation packages to describe and analyze various properties of technologically important materials. The simulation tools installed on the cluster were chosen to offer users a multiscale approach from an atomistic description to realistic device structures. Electronic structure methods based on Density Functional Theory (DFT), Configuration interaction (CI), Coupled Cluster (CC), Many Body Perturbation (MP), Quantum Monte Carlo (QMC), force field methods based on molecular dynamics, and multiscale methods for photonics were incorporated to address complex scientific problems at different length scales. The research projects encompass a wide range of areas, including nanoelectronics, spintronics, new materials for topological insulators, photonics and plasmonics, photovoltaics, catalysis, new memory materials, bio-sensors, biological processes in cells, as well as ultrafast processes in materials, with users from chemistry, chemical engineering, electrical engineering, biological engineering, and materials science and engineering. Societal and Ethical Implications of Nanotechnology Prof. Robert McGinn directs the SEI team at SNF which consists of Drs. Michael Deal and Mary Tang, with participation of other SNF staff members as needed. In November of 2010, we began incorporating an on-line ethics survey in our new-user orientation program. The survey is designed to gauge the level of ethical development among our new incoming researchers – as well as provoke them to consider various ethical implications of their work. After 14 months, over 150 incoming SNF researchers and students have contributed to this survey. Prof. Robert McGinn and the SEI team are using the results to identify topics and define focus areas that will inform SEI educational efforts targeting new researchers. For Spring quarter of 2011, Prof. McGinn and the SEI team introduced a new class to the Stanford curriculum, E 204, “Research Ethics for Engineers and Scientists.” This course is one of only two Stanford classes recognized by the University as meeting NSF’s requirements for instruction in the Responsible Conduct of Research. The course take the form of a seminar/discussion in which each session focuses on a specific topic and is usually led by guest speakers knowledgeable in the field. Some topics of particular note: • Ethics in nanotechnology, led by Prof. Malcom Beasley, Prof. Emeritus in Applied Physics at Stanford and chairman of the Bell Labs commission investigating data fraud allegations in the Hendrik Schoen case. • Ethics of authorship in papers, conference presentations, and patents, led by Prof. R. T. Howe, Electrical Engineering, and NNIN Director. • Responsible conduct in a shared lab community, led by Drs. Michael Deal and Mary Tang, Senior Research Associates with SNF. Prof. McGinn actively participates in NNIN SEI activities: presenting at the Congress on Teaching SEI, at Arizona State, Nov. 2011; contributing an essay to the SEI website, "What Makes Safety In the Nanotech Lab an ‘Ethical Issue’?; working with Cornell’s SEI team to develop an ethics questionnaire for the 2011 REU students. Prof. McGinn has also represented NNIN in giving a talk entitled “Ethics and Nanotechnology” at the Center for Probing the Nanoscale: Ethics Workshop at Stanford University, in February, 2011. --End of Stanford Text report---

NNIN Annual Report p.162 March 2011-Dec 2011 7.7.6 Selected Stanford Use Statistics (2011)

SNF Cumulative Users-Historical 700 12 months

10 months 600 foreign state and fed gov large company 500 small company pre-college 2 year college 400 4 year college other university local site academic 300

200

100 Cumulative Annual Users Annual Cumulative

0 FY04 FY04 FY05 FY05 FY06 FY06 FY07 FY07 FY08 FY08 FY09 FY09 FY10 FY10 FY11 FY11 Local Other Local Other Local Other Local other Local other Local Other Local Other Local Other

b) Lab Hours by Institution Type c) User Distribution by Institution Type

Stanford Users March 2011-Dec 2011 10 months Stanford Lab Hours March 2011-Dec 2011 10 Months

small company large company 15% 3% large company 3% other university small company 4% 15%

other university 5% local site local site academic academic 78% 77%

65,630 hours in 10 months 585 unique users in 10 months

d) Average Hours per User( in 10 months) e)New Users

160 80 Stanford Hours per User March 2011-Dec 2011 10 months Stanford New Users March 2011-Dec 2011 10 months 140 70

120 60

100 50

80 40

60 New Users 30 Hours per per user Hours 40 20

20 10

0 0

Figure 133 Selected Stanford Site Statistics

NNIN Annual Report p.163 March 2011-Dec 2011 7.7.7 Stanford User Institutions (2011) Other Academic Small Company Large Company Harvard University A M Fitzgerald & Associates Agilent Middlebury College Acorn Technologies Hewlett Packard Naval Postgraduate School Active Optical MEMS Hitachi GST North Carolina State University Active Optical Networks IBM Princeton University Aerospace Missions Corp Intel Corp Saint Louis University AG MicroSystems JDS Uniphase San Jose State University Akxel Microsystems SRI International Santa Clara University ALCES Technology Swarthmore College Alion Foreign Alpha and Omega UC Berkeley Semiconductor Universitat Basel UC San Francisco Amprius University of Calgary University of Prince Edward UC Santa Barbara Areva Island UC Santa Cruz Arrayed Fiberoptics UCLA ASML Industry Small Company (Continued) University of Michigan Asylum Research OndaVia University of Riverside Banpil Photonics Pacific Biosciences University of Washington Ben Chui Consulting Phoenix Biosystems University of Wyoming BeSang Inc. Physical Optics Corp Calarrudo Consulting Pradeep Nataraj Consulting Corium International QuSwami Small Company (continued) Cranepine Medical REC Technology US Kovio DxRay-SBIR RPIC Systems Kumetrix Eksigent Technologies Sensorin LuxVue Technology EPIR Technologies Siargo LW Microsystems ePowersoft Silexos MagArray First Solar Silicon Light Machines Mcube Glide/Write Single Cell Technology Microcess GLO USA SiPhoton M-Tech Instrument Grandis Solar Junction Nano and Micro Technology Halcyon Molecular Strataglass Nano Liquid Devices Heliofarm TetraSun NanoGram Integrated Plasmonics ThinSilicon Nanolabz Intermolecular Tricorntech Nanosys Intevac Twin Creeks Technologies NetCrystal InVisage Unity Semiconductor NthDegree Tech Worldwide Jacksons Processing Solutions Veloctron Nupga Kaiam Voxtel Kateeva Wostec Wuzi Zhichao Medical Devices Yung Chieh Tan Zeno Semiconductor

NNIN Annual Report p.164 March 2011-Dec 2011 7.8 University of California Santa Barbara Site Report 7.8.1 Site Overview UCSB's Nanofabrication facility draws upon the strengths of UCSB's internal research in compound semiconductor electronic and optoelectronic devices in the GaAs, InP and GaN-based materials systems; polymer and organic electronic and photonic devices; quantized electron structures and THz physics; spintronics, single electronics, and quantum computation; quantum optics; MEMS/NEMS, bio- instruments, and microfluidics. Of note are the National Research Council Rankings of Research Doctoral programs, by department, in the US. According to the overall rankings, The UCSB Materials department ranks first in the nation, the Electrical Engineering and Chemical Engineering departments rank in the top 5, and the Physics and Mechanical Engineering departments rank in the top 8 nationwide. The UCSB Nanofabrication facility operates out of a 12000 ft2 class 100/1000 cleanroom environment. UCSB has extensive facilities and research for nanotechnology including: electron beam lithography down to <10nm resolution; optical projection lithography to below 150nm; advanced ICP etch tools for a wide range of materials including ceramics, dielectrics, metals, silicon, SiC, III-V nitrides, III-V phosphides, and III-V arsenides; thin film deposition techniques including evaporation, RF and DC reactive sputtering, ion beam deposition, atomic layer deposition, and ICP-based PECVD; Field Emission SEM and EDX; Scanning Phase Microscopy. The facility is open to processing the widest variety of materials possible, with few restrictions, to facilitate research over the widest possible range. UCSB fosters a very collaborative research environment between researchers in many disciplines including Materials Science, Chemistry, Physics, Biology, Chemical, Electrical, and Mechanical Engineering. UCSB houses a wide range of well-funded centers of excellence in areas of electronics, optoelectronics, energy efficiency, materials, biology and physics. These centers are funded by a wide variety of government agencies and industrial partners and often involve significant academic collaborations not reflected directly in user statistics. The centers include: The Optoelectronics Technology Center, The Solid State Lighting and Energy Center, The NSF-funded Materials Research Laboratory,the Mitsubishi Chemical - Center for Advanced Materials, the Institute for Energy Efficiency, The Institute for Collaborative Biotechnologies, The California Nanosystems Institute, the Center for Polymers and Organic Solids, the Institute for Terahertz Science and Technology, the Center for Energry Efficient Materials (CEEM), and the Center for Spintronics and Quantum Computation. Researchers from these centers utilize the nanofabrication facility and provide resources and knowledge that benefit the entire user community. Many of the centers coordinate weekly and other special technical seminars and workshops. To leverage these resources, links to the research centers are posted on the UCSB Nanofabrication Facility website and talks are often advertised by fliers outside the facility entrance so that our large multi-disciplinary user community is invited and encouraged to attend these events. As a center of excellence for electronics and compound semiconductors, the UCSB site is hosting and coordinating an exploratory symposium on electron device research entitled “Frontiers in Nanoscale Transistors and Electronics”. The workshop has invited speakers form around the nation from academia and industry. Guided by critical system and circuit requirements, this symposium will define candidate devices, associated materials, and process technologies for future generations of electron devices. This workshop will address the problems and difficulties when working with: future digital systems (VLSI) as these migrate to few-nm device dimensions and wireless communications systems as these migrate towards THz frequencies. 7.8.2 Research Examples The primary mission of the facility is to provide the resources and expertise to enable research into devices on the micro and nano-scale. Research results over a wide range of disciplines are obtained by internal and external researchers of the UCSB facility. Below are three highlights of projects using the

NNIN Annual Report p.165 March 2011-Dec 2011 laboratory from different research groups and affiliations. External Small Company User: Optics/Electronics: Heterogeneous Photonic Integrated Circuits: Aurrion, Inc. Aurrion, a start-up company in Santa Barbara, is commercializing a semiconductor integration platform that enables all the elements of photonics systems to be fabricated on a single chip using control and cost-structure of silicon foundries. This technology is disruptive to the current photonics industry, therefore, in both its ability to change the economics of photonics manufacturing and its ability to Figure 134: CWDM Laser Spectrum of 50 Gb/s Hybrid Silicon Photonic push photonic integration on a growth curve similar to Moore’s law. Transmitter Aurrion believes that such integration will be critical to the next generations of military systems and communication systems. Figures 134 and 135 show fabricated hybrid laser output spectra and a schematic of the integrated 50Gb/s transmitter chip. (IEEE Journal of Selected Topics in Quantum Electronics, 17(3), 671-688, 2011) . Internal User: Physics/Electronics: Fast Tunable Coupler for

Superconducting Qubits: Martinis, Cleland Groups, UCSB Figure 135: 50 Gb/s Hybrid Silicon Photonic Transmitter A major challenge in the field of quantum computing is the construction of scalable qubit coupling architectures. Here, UCSB researchers demonstrate a novel tunable coupling circuit that allows superconducting qubits to be coupled over long distances. They show that the interqubit coupling strength can be arbitrarily tuned over nanosecond time scales within a sequence that mimics actual use in an algorithm. The coupler has a measured on/off ratio of 1000. The design is self-contained and physically separate from the qubits, allowing the coupler to be used as a module to connect a variety of elements such as qubits, resonators, amplifiers, and readout circuitry over distances much larger than nearest-neighbor. Such design flexibility is likely to be useful for a scalable quantum computer..(Fig. 136) (Phys. Figure 136:: Device circuit and micrograph of two Josephson phase qubits with a tunable Rev. Lett. 106, 060501 2011) coupler. The two qubits are shown in red and blue in the circuit, and boxes b and c in the lower External Academic User: Physics/MEMS/Electronics: Electromechanical resonance behavior of suspended single-walled carbonnanotubes under high bias voltages, Cronin Group, Electrical Engineering and Physics Depts, USC In this work USC researchers characterize the nanoelectromechanical response of suspended individual carbon nanotubes under high voltage biases. They observe an abrupt upshift in the mechanical resonance frequency of approximately 3 MHz at high bias. The upshift is attributed to the Figure 137: Electrode and CNT SEM images onset of optical phonon emission, which results in a sudden contraction of the nanotube due to its negative thermal expansion coefﬁcient. This, in turn, causes an increase in the tension in the suspended nanotube, which upshifts its mechanical resonance frequency. The upshift is reported as consistent with Raman spectral measurements, which show a sudden downshift of the optical phonon modes at the

NNIN Annual Report p.166 March 2011-Dec 2011 same high bias voltages. Using a simple model for oscillations on a string, the researchers estimate the effective change in the length of the nanotube to be ∆L/L ≈ −2 × 10−5 at a bias voltage of 1 V.( J. Micromech. Microeng. 21 (2011) 085008). (Figs. 137 and 138). 7.8.3 Operations and Capital Acquisitions The UCSB facility hosted 521 research users over the span of Mar. through Dec. 2011.This includes 50 external academic and government users, 133 small company users, and 39

large company users for a net 44% external cumulative user base, the same as in 2010.The external academic user Figure 138: Resonance Frequency and numbers have been consistent from 50 in 2010 to 48 through conductance measurements versus gate bias Dec. 2011. Average lab hours per month have remained near 6000.The number of cumulative remote users has remained steady at 45. The number and hours of remote users per month is 7.5 and 56 respectively, or roughly 7.5 hours per month per remote user. Consultation and technical discussions of the UCSB profesional staff with outside users is not recorded as this service is provided to all users at no additional cost. There were 38 new projects since last reporting, bringing the total number of new external research projects is up to 232 since the inception of the NNIN, 107 of them from academic/government institutions (6 foreign) and 125 from industry(1 foreign). Colleague referral and internet searches were responsible for most of the new projects in 2011. The UCSB facility continues to house a diverse community comprised of significant numbers of users from Physics (12%), Materials (20%), Electronics (23%), MEMS/Mechanical Engineering (11%), and Optics (29%). UCSB continues to improve process offerings and user capacity through capital purchases.These purchases expand process and metrology capability and increase capacity to accept new users. In 2011, installed systems include: • ASML 5500/300C DUV (248nm) stepper. Purchased and received in 2010. Installation completed Sept. 2011. This equipment expands optical lithography to the deep sub-micron (0.1-0.2um) regime and increases capacity in the lab. For users wanting large areas of deep-sub micron lithography, this tool provides a cost effective option against e-beam lithography. The system accommodates piece parts. User training is expected to begin in February 2012. (facility funded) • Logitech Orbis Chemi-Mechanical Polisher (CMP) system. This system enables fine polishing for many materials used in the facility (Si, GaAs, InP, GaN, Diamond, Metals, Oxides, etc.) and for self-aligned planarization techniques not available with other fabrication methods. Logitech’s experience with piece parts makes this technique available to a large number of UCSB researchers. Logitech is providing full process support with direct access to their applications experts by our researchers. (NNIN and facility funded) • Olympus LEXT, DUV, and general inspection (with fluorescence) microscopes. The LEXT microscope is a laser scanning confocal microscope that provides 3-D imaging and metrology (x,y,z, roughness) measurements of processed surfaces using an all-optical measurement. The DUV scope uses 248nm light to capture very high resolution (sub-100nm) images for wafer/process inspection. These two microscopes supplement SEM, AFM, and Profilometer measurement tools for many users. The general inspection scope was added to alleviate wait times for normal inspection, with the added benefit of fluorescence imaging capability. (facility funded) The UCSB facility had no new hires in 2011, but expects 1 new position for 2012.

NNIN Annual Report p.167 March 2011-Dec 2011 7.8.4 Education, Diversity, and SEI In 2011, UCSB hosted the annual NanoDays exhibition at the Santa Barbara Museum of Natural History, providing hands-on activities for 897 community members of the general public. This event reached all ages, including building a giant model of a carbon nanotube, using an actual atomic force microscope (AFM) to see the nanoscale features of a butterfly wing, to using a scanning electron microscope (SEM) to see the hairs on a bee’s leg. UCSB also provided the SEM, AFM, and technical personnel as part of NNIN’s outreach event to the annual SHPE (Society of Hispanic Professional Engineers) held in Anaheim California in October. UCSB also offers hands-on educational clean room experience to pre-college students as an introduction to nanotechnology. In 2011, these 2-day chip camps reached 57 students and 6 teacher and community members, providing opportunities for females (56%) and underrepresented (59%) students to learn basic nanofabrication processing techniques. Chip camps serve as a pipeline for students into longer research experiences.

In 2011, UCSB provided research experiences that actively engaged 6 college students, and 4 secondary science teachers in a clean room laboratory, so they could contribute to real-world nanoscale research. These activities are part of the larger NNIN REU and RET programs. All research experiences are similar in that they participate in nanotechnology related research over a summer, and later they present it through an oral presentation, a poster presentation, and through a written report (or, in the case with teachers, curriculum is developed based on that research). The experiences differ in the target participants, and the length of time during the summer. The particulars of these programs are summarized below.

Undergraduate Research Experiences (REU): • Research Experience for Undergraduates (REU) recruits 6 students (17% females) from all over the US. As an example of the breadth of topics, here are three of the research titles from 2011: “Sub-wavelength Photonic Grating Couplers Using Electron Beam Lithography”, “Nanomechanical Properties of Structured Biopolymer Networks”, “Nanoscale Diamond Lenses for Atomic-Scale Sensing” Research Experience for Teachers (RET): • 6-week summer research for local secondary science teachers: 3 male, 1 female, 1 Hispanic. In this part of the program, teachers do research and then develop curriculum based on that research

• classroom follow-up: 424 high school students: 49% females; 54% minority. Here, the NNIN coordinator directly views, in the classroom setting, the activities developed during the summer portion of the program. • curriculum dissemination at the National Science Teachers Association annual conference: we brought 4 teachers: 1 female; 1 Hispanic. At the NSTA conference, teachers who participated in UCSBs 2010 RET program shared their curriculum with other teachers. Educational programs also incorporated SEI components into the learning experience. At the 2011 NanoDays exhibition, NISE network SEI-related posters and brochures were handed out and two volunteers from the UCSB Center for Nanotechnology in Society (CNS) were there to promote SEI awareness and to answer questions. For the chip camps, 1 hour CNS driven exercises focusing on SEI- related scenarios and problem solving in groups was done. Also, for overnight chip camps, students were encouraged to play a game of Nanoventure, which explores the connections between science, specifically nanotechnology, and society In support of SEI activities geared towards the research community, UCSB has engagement on several

NNIN Annual Report p.168 March 2011-Dec 2011 fronts. New users are currently directed to a video presentation on the main NNIN SEI site as part of their lab orientation. UCSB has also supported a 4 part lecture series, sponsored by the UCSB Office of Research, on general research ethics by direct emailings and advertisement of the talks to the facility’s 500+ person user base. The talks have highlighted various research ethics issues including data fabrication, ethics in stem cell research, and ethics in neuroscience research. The nanotech website contains front page links for getting more SEI information at the main NNIN-SEI website, the Center for Nanotechnology and Society (CNS) at UCSB, and the UC Center for Environmental Implications of Nanotechnology. Posters, produced by Cornell, meant to stimulate SEI nanotechnology issues are displayed outside the cleanroom entrance and in visible locations within the laboratory. An assessment of the SEI activities was done through an informal survey and was presented in poster format at the SEI national congress at ASU in Tempe, AZ, in November.

NNIN Annual Report p.169 March 2011-Dec 2011 7.8.5. USCB Selected Statistics a)Historical Annual Users

UCSB Cumulative Users-Historical 450 foreign 12 months state and fed gov 400 large company small company 10 months pre-college 350 2 year college 4 year college 300 other university local site academic

250

200

150

100

Cumulative Annual Users Annual Cumulative 50

0 FY04 FY04 FY05 FY05 FY06 FY06 FY07 FY07 FY08 FY08 Fy09 Fy09 FY10 FY10 FY11 FY11 Local Other Local Other Local Other Local other Local other local Other Local Other Local Other

b) Lab Hours by Institution Type c) User Distribution by Institution Type

UCSB Lab Hours March 2011-Dec 2011 10 months UCSB Lab Users March 2011-Dec 2011 10 Months

state and fed gov foreign large company 0% 1% 4% large company small company 8% foreign 29% 1% small company 26%

local site academic local site 63% academic other university 56% 3% other university 9%

521 Users- 10 months 60,231 Hours- 10 months

d) Average Hours per User( in 10 months) e)New Users

200 80 UCSB Hours per User March 2011-Dec 2011 10 Months UCSB New Users March 2011-Dec 2011 10 months 180 70 160 60 140 120 50 100 40 80 New Users 30 Hours per user per Hours 60 20 40 10 20 0 0

Figure 139: Selected Site Statistics from UCSB

NNIN Annual Report p.170 March 2011-Dec 2011 7.8.6 UCSB User Institutions (2011)

Outside US Academic Small US Companies Large US Companies California Institute of Technology AdTech Optics Autoliv George Washington University Advanced Nanostructures Avery Dennison Montana State University Advanced Scientific Concepts Bruker Metrology Pennsylvania State University Aerius Photonics Cree Stanford University Applied Nanostructures, Inc DuPont Displays University of Arizona Asylum Research Emcore University of California, Berkeley Aurrion FLIR University of California, Los Angeles Avio Scientific Hewlett-Packard University of California, Riverside Bridgelux Hughes Research Laboratories University of California, San Diego Calient Networks InfraredVision Technology Corp University of California, Santa Cruz Cbrite Intel University of Central Florida Freedom Photonics JDSU University of Colorado Boulder Inlustra Technologies Lockheed Martin, SB Focal Plane University of Notre Dame Innovative Micro Technologies Northrop Grumman Corporation University of Southern California Invenios Raytheon Vision Systems University of Texas Austin, MRC Kaiam Corporation University of Washington Kavana Technology International Washington State University LED Engin Centre Investigacions Nanociencia Washington University St. Louis LuxVue Laboratoire de physique at chimie des INSA dept de denie physics Wayne State University MEMS Precision Tech University of Augsburg Ostendo Technologies VisIC Technologies Polyfet RF Devices Praevium Research State & Federal QmagiQ JPL rubbix Lawrence Livermore National Laboratory Serry Enterprises Simax Solar3D Soraa SpectraFluidics Spectrolab Superconductor Tech., Inc. TelAztec Transphorm

NNIN Annual Report p.171 March 2011-Dec 2011 7.9 University of Colorado Site Report 7.9.1 Summary In its third year of operation, the Colorado Nanofabrication Laboratory (CNL) experienced further growth of number of users, percentage of external users and user hours. The cumulative number of users increased1 by 42% to 142 and the hours of use increased by 26% to 20,600. The number of external users almost doubled from 21 to 41, increasing the percentage of external users from 21% to 29%. Capabilities of the Laboratoy have been increased through further process development and addition of new materials such as platinum, magnesium, tetracene and graphene. An atmospheric pressure CVD furnace was installed for growing graphene on copper foil. The education and outreach activities were expanded. A workshop on Graphene was held in October 2011. New education and outreach activities include the Graduate School Advising Workshop which included the students that attended the NNIN international Winter School in Bangalore, India. 7.9.2 Technical Focus Areas The technical focus areas are linked to local research strengths in precision measurements and energy. Initiatives in each area are discussed next: Precision measurements Related research activities in Colorado are concentrated at NIST and JILA, a joint institute supported by NIST and the University of Colorado. We started continued interactions with both institutions. Discussions with current and potential users and targeted process development has resulted in 8 users from JILA and Cold Quanta, a JILA spin off. Our graphene growth system is expected to attract additional users from this community. Energy Energy research in Colorado is rapidly growing with a clear focus at NREL and multiple Colorado-based initiatives such as RASEI, a multi-university research initiative, the Center for Revolutionary Solar Photovoltaics (CRSP) and the Renewable Energy Materials Science and Engineering Center (REMRSEC) at the Colorado School of Mines (CSM). The REMRSEC at CSM has been identified as a complementary NSF-funded research effort in Colorado. Their focus is on materials including nanoparticles and chalcogenides for thin film solar cells, advanced membranes and clathrates for hydrogen storage. NREL has a long track record pursuing photovoltaics and hold numerous records for highly-efficient solar cells. They are set up as an independent research unit with their own funding and facilities, but welcome interaction with Universities across the globe. First users from local energy startups have been attracted, including researchers from Ampulse Solar (2) and Ravenbrick (1). Interaction with NREL is primarily through local users that are funded through NREL or collaborate with NREL researchers with an occasional NREL staff member using the facility. Two users from CSM have been trained and have become frequent visitors of the facility. Ongoing research includes thin film solar, adaptive window coatings and nanoparticles. 7.9.3 Research Highlights Research activities of the users are primarily in MEMS, optics, materials and electronics. Research in our focus areas, energy and precision measurements, are linked to materials/optics and optics/MEMS respectively. The following are examples of research results that were obtained by users of the CNL

1 All data are projections for year 3 (3/1/2011 – 2/28/2012) based on 11 month data (3/1/2011 – 1/31/2012)

NNIN Annual Report p.172 March 2011-Dec 2011 facility during the past year:

• Ultrastrong adhesion of graphene membranes, Prof. J. Scott Bunch et al., University of Colorado. The adhesion energy of graphene sheets to a silicon dioxide substrate was measured using a pressurized blister test, resulting in an adhesion energy of 0.45 J/m2 for monolayer graphene and 0.31 J/m2 for samples containing two to five graphene sheets. These values are larger than the adhesion energies measured in typical micromechanical structures and are comparable to solid–liquid adhesion energies. This is attributed to the extreme flexibility of graphene, which allows it to conform to the topography of even the smoothest substrates, thus making its interaction with the substrate more liquid-like than solid-like.

• Super resolution 3D microscopy using double helix point spread functions implemented with a phase mask, Prof. R. Piestun et al., University of Colorado. The technique of Stochastic Optical Reconstruction Microscopy (STORM) has been implemented in three dimensions using a double helix point spread function, resulting in full 3D imaging with super resolution. This technique uses a phase mask as shown in Figure 140a) and b). The mask was fabricated with a maskless lithography system using gray scale exposure yielding a continuously varying phase. The resulting image is compared in Figure 140c) and d), illustrating both the higher resolution and 3D capability of the technique.

a) b) c) d)

Figure 140: a) Surface profile of the double helix mask design. (b) Measured surface profile of the fabricated phase mask. c) Typical fluorescence image of micro-tubules limited by the classical diffraction-limited criteria. d) A 3D image using a double helix point

7.9.4 Operations Focus of year three was: 1) Solving vibration and EMI issues due to the close proximity of the E-beam lithography activity to a growing number of vacuum systems. 2) Installation of additional equipment and development of related process with a specific emphasis on what that benefits current users and supports focus areas, and 3) Increasing external visibility of CNL and promotion of use by external researchers. A 750 sq ft satellite facility was set up to accommodate E-beam writing and AFM characterization. This facility is located in a cleanroom in the second basement of the building and has immediately reduced the vibration and EMI issues users experienced in the main facility. The facility provides E-beam writing using a converted JEOL JSM-5910LV SEM, enabling users to fabricate feature as small as 50nm. Additional equipment that became available to the users includes a 3” graphene furnace for atmospheric growth of graphene on copper foil, a Tylan 4-tube furnace for silicon porocesses (oxydation, diffusion and metal anneal), a rapid thermal anneal system (RTA), and a high temperature (1800oC) inductively heated how wall reactor for annealing of implanted layers in silicon carbide and the conversion of tantalum to tantalum carbide. Two upgrades were added: an STM upgrade to the Nanosurf AFM, providing atomic

NNIN Annual Report p.173 March 2011-Dec 2011 resolution imaging on conducting surfaces and a light source upgrade for the maskless lithography system. Some smaller investments were made to make the lab more robust including the acquisition of a second profilometer (Alphastep 500) and a nitrogen generator. Additional equipment was obtained from researchers across campus, who donated their used equipment to the CNL user facility. This includes a Viper SLA system that came with $16k for refurbishing, an additional ball bonder and a Shimadzu spectrophotometer, which was upgraded with a new computer. Process development is a key component for a successful user facility. We aim to provide a base-line process for any tool and work with users to develop their own research specific processes. This year we added processes for the growth of graphene on copper foil and transfer to another substrate, deposition of high density and low stress PECVD nitride, deposition of magnesium, tetracene, and platinum. This year we also transitioned into developing process modules, such as the formation of suspended

membranes (SiO2, Si3N4, silicon) on a silicon wafer and selective gold electroplating. As the facility has been renovated and upgraded, the operational focus is further shifting towards attracting external users, especially those performing research in our focus areas. Visibility of the facility has been increased through education and outreach activities, additions to the website, a targeted mailing to local industry and word of mouth. We have already seen an uptick in general inquiries, have provided SBIR support letters to local small business, confirming open access and have provided multiple tours of the facility. As we pole new users, we find that in addition to the above efforts, word of mouth still plays a significant role. By now, we have points of contact at most Universities along the front range. They are typically users of the lab and have been instrumental in recommending our facility to their faculty. Further targeted advertizing is planned, with an increased focus on local industry. A specific target is start-ups and small businesses funded by SBIR and venture funds, which we plan to access through the local technology transfer offices, chambers of commerce, incubators and industry associations such as the Colorado Photonics Industry Association. CSM and NREL were specifically targeted as they represent a significant group of potential users with research activities that match our energy focus area. Interaction and joint activities were pursued with the REMRSEC at CSM and the photovoltaics researchers at NREL, including lab tours, discussion of the facilities and a joint poster session. The operational changes and improvements have resulted in a sustained growth of the number of users and hours of use as illustrated with Figure 141.

Geology Education 1% 1% Other 25,000 Medicine 1% 1% 200 Chemistry 4% 20,000 150 Physics MEMS 15,000 8% 5 year 30% 100 5 year target 10,000 Electronics target 13% 50 External UserHours 5,000

Number of Users External Number of Users users users Materials 0 0 17% Optics 24% 2008 2009 2010 2011 2012 2013 2008 2009 2010 2011 2012 2013 Year Year

Figure 141: a) Number of users by year, b) Hours of use by year and c) User research areas for 2011

NNIN Annual Report p.174 March 2011-Dec 2011 The figure illustrates the sustained growth the facility experienced during the last three years. The number of users increased to 142 which is a 42% increase over last year. At this rate we expect to meet and exceed our 5-year goal of reaching 200 users in 2013. Annual use of the facility has increased to 20,600 hours a 26% increase, already exceeding our five year goal by 4,600. Growth of user hours was less than last year as the number of heavy users in research areas such as MEMS has saturated and their relative numbers have declined. Still we expect the hours of use to grow to 30,000 for 2013. Of the 142 current users, 30% perform research on MEMS, with optics (24%), material science (18%) and electronics (13) representing 84% of all users. Newly trained users are spread between MEMS (15%), electronics (9%), optics (28%) and material science (26%). External users almost doubled from 21 to 41 compared to last year, with an even split between academic and industrial users. The percentage of external users also increased compared to last year from 21% to 29%. The category of remote access users grew from 4% to 9%, while reaching users across the US. 7.9.5 Diversity oriented initiatives Overall, we have aimed to be inclusive in all of our activities, particularly with respect to underrepresented groups, specifically hispanics and woman. Outreach activities have been identified as a prime opportunity to promote diversity, from the REU program, the Symposia, to Nanodays, and K-12 oriented presentations and activities. Inclusion of women has been straightforward so far, while inclusion of minorities has been identified as requiring further improvement. We are currently working with the Society of Hispanic Engineers to advertize opprtunities for Hispanic science and engineering students at CNL and to bring outstanding students to our campus with travel grants. 7.9.6 Education oriented contributions Our main focus in education is on establishing educational activities that can be repeated on an annual basis, thereby continuously improving their scope, quality, effectiveness and efficiency from year to year. This year’s REU program included 6 NNIN REU’s, one NNIN REU working on SEI, and one international student from Japan. One REU student funded by a single PI NSF REU grant was also included in the CNL REU group activities. The PI/mentor training was further expanded this year. Three full-day REU events were organized jointly with the REU program of the REMRSEC at CSM, including technical presentations, lab tours, a poster session, an SEI discussion and one-on-one interaction. The students also particpated in the newly established graduate school advising workshop. In addition, student attended bi-weekly user meetings and self-organized social activities during weekends. This summer, three of last year’s REU students also participated in the NNIN iREU program in Germany (2) and the Netherlands (1). Two former REU students are now graduate students at the Univeristy of Colorado. Links were established between current and prior REU students through social networking sites, enabling students to exchange information and experiences regarding research and graduate school. The annual workshop covering basic nanofabrication processes was held for the third time June 8-11, 2010. Separate lectures on lab safety and SEI were included with dedicated time for discussion. The lectures were recorded and are available to registered users throughout the year as streaming video with slides. The hands-on lab experiments are available as supplemental training for CNL users. A graduate school advising workshop was held June 14, 2011. The format included short presentations, a panel session and one-on-one Q&A sessions in small groups. Eight of last year’s participants of the NNIN iWSG in Bangalore, Inda were brought in as a resource.Through a series of presentations, they provided information about their University and talked about their personal graduate school experience. Topics covered included the application process, standardized tests, the selection of graduate schools, field of

NNIN Annual Report p.175 March 2011-Dec 2011 research and potential thesis advisor. The option of delaying graduate school for study abroad or other foreign activities such as peace corps or engineers without borders received quite a bit of attention. A total of 44 students participated in the event. Based on feedback received, we plan to make this an annual event, open it up to a broader range of students and include junior faculty as well as recent graduates employed in industry and national labs as speakers and panel members. A workshop on Graphene was held Friday, October 7, 2011 in Boulder, CO. The workshop was prompted by the realization that multiple users were independely performing research involving graphene. The purpose of the workshop was to bring these researchers together and to gauge the need for a dedicated graphene CVD system at CNL. The workshop consisted of 4 oral presentations, a panel session, networking opportunities and a lab tour. A total of 40 people registered for the workshop. As a result of the workshop, the decision was made to install a graphene CVD system and to develop an atmospheric growth process on copper foil. A special effort was made by CNL staff to participate in other NNIN and local outreach activities, including the REU convocation at Georgia Tech, the Society for Hispanic Professional Engineers Meeting in Anaheim, presentations at Evergreen Middle School, the first Congress on Teaching the Social and Ethical Issues of Research at Tempe, AZ, and participation in the international Winter School for Graduate students in Campinas, Brazil. The experience gained from these activities will be used in our own education and outreach activities. 7.9.7 Society and ethics oriented activities Our society and ethics oriented activities were further refined and have become an integrated part of most education, outreach and training activities. Creating awareness and promoting discussion are the two main objectives we seek. The SEI material was first included in the annual workshop in June 2010 and is being incorporated into all user training. REU posters highlighting SEI activities, including the awareness posters developed by Cornell have been posted in the facility. SEI training of individual lab users consists of viewing one of the SEI videos and completing the SEI quiz. Additonal SEI material is posted on the CNL website for further reading/exploration. All users also take a short refresher training as they renew their lab membership each March. SEI training of larger groups of new users is incorporated in the annual workshop and REU student training. Here we have separate lecturs on lab safety and SEI with ample time for discussion. SEI seminars are included in the biweekly user meetings, ranging from a discussion of case studies and research practices, to an SEI webcast. The graduate school advising workshop naturally sparked a range of SEI issues as students formulated their choices in life and discussed the benefit of joining the peace corps/engineers without borders. This year we hosted one SEI REU, who was co-advised by Prof. Carl Mitcham at CSM and Prof. Lupita Montoya, a junior CU faculty member with an interest in environmental sciences. As part of CNL’s participation in the international winter school in Brazil, we added two SEI lectures to the program, presented by Prof. Laura Grossenbacher. She also promoted discussion of students’ experiences during the second week, providing discussion and writing assignments and moderating group discussions. ---End of Colorado Site Text Report---

NNIN Annual Report p.176 March 2011-Dec 2011 7.9.8 Selected Univ. of Colorado Site Statistics (2011) a)Historical Annual Users

Historical Users--Colorado Site--by Institution Type 100 10months foreign 90 state and fed gov 12 months

80 large company

small company 70 pre-college 12 months 60 2 year college Users 4 year college 50 other university Joined NNIN local site academic 40 in FY09

0 FY04 FY04 FY05 FY05 FY06 FY06 FY07 FY07 FY08 FY08 FY09 FY09 FY10 FY10 FY11 FY11 Local Other Local Other Local Other Local other Local other Local Other Local Other Local Other

b) Lab Hours by Institution Type c) User Distribution by Institution Type

Colorado Lab Hours March 2011-Dec 2011 10 months Colorado Lab Users March 20110- Dec 2011 10 Months

Small company Pre-college 16% Small company Large company 0% Large company 12% 1% 0% State and fed gov Pre-college State and fed gov 4 year college 0% 0% 0% 2% 2 year college Foreign 1% Other university 2% 6% 4 year college 3% Other university Local site 10% academic Local site 72% academic 18,084 lab hours total 71% 132 total users 13774 Hours-10 Months 94 users - 10 months

d) Average Hours per User( in 10 months) e)New Users

500 40 Colorado Hours Per User---March 2011 to Dec 2011 (10 months) U. Colorado------New Users--March 2011-Dec 2011 10 Months 450 35 400 30 350

300 25 56 New Users in 10 Months

250 20

200 New Users 15 Hours per user per Hours 150 10 100 5 50

0 0

Figure 142: Selected Colorado Site Statistics

NNIN Annual Report p.177 March 2011-Dec 2011 7.9.9 University of Colorado User Institutions (2011)

Outside US Academic Small Company Large Company Colorado School of Mines Aymont Technology, Inc. Research Electro-Optics Colorado State University BiOptix Montana State University Chiaro Technologies LLC Olin College of Engineering ColdQuanta Inc University of Arizona InRedox LLC International University of denver Mircoflux LLC Toyota Technological University of Miami Phase Three Product I tit t J University of Pennsylvania RavenBrickDl LLC t State and Federal University of San Diego Redefine Technologies Inc JILA University of Texas at Austin TDA Research, Inc. Washington State University Vescent Photonics Winona State University

NNIN Annual Report p.178 March 2011-Dec 2011

7.10 University of Michigan Site Report 7.10.1 Technical Focus Area The Michigan Lurie Nanofabrication Facility (LNF) focuses primarily on micro electro mechanical systems (MEMS), complex integrated microsystems, and micro and nanotechnology. Applications of integrated sensors/actuators and microsystems include health care, biology and biochemistry, medical implantable microsystems, chemistry, environmental monitoring, and homeland and infrastructure security. Michigan’s continued efforts on geosciences include outreach to the geoscience community, new collaborations between geo and nano researchers, and support for new users from the geo community. Our outreach activities include participation in several meetings (American Geophysical Union 2011 Fall meeting, Sustainable Waters Initiative Research Meeting, Michigan H2Objective Conference: Research Shaping Michigan’s Water Future, and the upcoming Ocean Sciences meeting). Some of these led to a brainstorming session on environmental sensors for the Great Lakes community between NNIN-Geo, U- Michigan WIMS2, and researchers from the Cooperative Institute for Limnology & Ecosystems Research, the NOAA-Great Lakes Environmental Research Laboratory and the Great Lakes Observing System. As a follow-up to white papers developed during the “Nano-Enabled Sensing Microsystems for Geosciences” workshop held at U. Michigan in February 2010, several collaborative projects have continued between geosciences and nanotechnology researchers. Design, fabrication and integration for the project on “Micromachined Sensors for Multi-functional and Autonomous Analysis of Geofluids: A New Approach to the Design and Performance of Chemical Sensors in Extreme Environments” (U. Michigan and U. Minnesota) has been completed. Preliminary test results obtained by the Michigan team suggest that the sensor can provide pH measurement of a solution in regular laboratory settings, indicating the validity of the sensor design. Further evaluation of the sensor is now planned under extreme conditions and/or real deep sea settings. As part of a second project on “A Microfabricated Protein-Based Array for Electrochemical Detection of Bioavailable Metals in Aquatic Environments” (U. Washington, U. Southern Mississippi, U. Michigan and GeorgiaTech), initial work on arrays of Au/Hg working microelectrodes was done: microelectrodes were designed and fabricated at U. Michigan and electroplated and tested at Georgia Tech. An NNIN REU student contributed to the project. In addition, the new NNIN@Michigan website (http://www.lnf.umich.edu/nnin) includes a section for the geoscience community, with information about NNIN capabilities, examples of supported projects, and relevant funding opportunities. Since July 2010, NNIN/C@Michigan has provided support to researchers and engineers who tackle science and engineering problems at the micro/nanoscale, which can provide orders of magnitude performance improvement over current MEMS/NEMS technologies. We have been especially involved with the experimental user community and many of the projects that are using the NNIN/C@Michigan resources have both computational and experimental aspects, very often within one of the NNIN facilities. We have successfully established a very fruitful relationship with small universities and private companies in the region. The program has also provided strong technical support and thorough instruction on software tools so as to permit even novice users to progress rapidly to the solutions of their own unique research problems. The NNIN/C@ Michigan domain expert provided consulting expertise to researchers in a wide range of fields such as modeling, analyzing data, managing data collections, and producing scientific visualizations that aid in the knowledge discovery process. The research projects encompass a wide range of computational techniques, including continuum approaches (finite element, finite volume and boundary element methods), atomistic approaches (Molecular Dynamics, Monte Carlo) and multiscale methods

NNIN Annual Report p.179 March 2011-Dec 2011 (coupled atomistic/continuum). These, and many other techniques, have been successfully carried out with parallel computing. We continued our efforts to reach out towards the modeling community with workshops on MEMS/NEMS modeling and simulation at both local and national levels. We held a national symposium on Advanced Modeling Methods of MEMS/NEMS and Micro/Nanofluidic Devices in April 2011. The Symposium brought together 50 leading researchers from 15 different institutions to review recent progress latest developments, and review future challenges in the field. In Figure 143: SystemAttendees of the Symposium on Advanced Modeling Methods of MEMS/NEMS and Micro/Nanofluidic Devices addition, we also continued to host free, local workshops to inform users of MEMS/NEMS modeling community’s activities and to provide a platform for networking amongst researchers interested in MEMS/NEMS development. Finally, we organized a Modeling and Simulation of Nano/Microsystems Contest, with the objective to provide publicity and promotional support to new developments, recent progress, and advances in the modeling and simulation of Micro/Nanosystems. The emphasis was on current challenges in understanding of the multi-physics/multi-scale phenomena that govern such systems functionality. Over 20 submissions were received from several US and international institutions and the judging process is underway at the time of the report. The Michigan site of the NNIN has also continued expanding its experimental user community through many different events and activities: seminars and workshops on and off-site, participation in technical conferences, partnerships and discussions with local business organizations, etc. By hiring a dedicated person for marketing and user outreach and leveraging onsite graphic design personnel, we have been able to lead significant efforts in marketing/communication for the Michigan site of the NNIN: new enhanced website, professionally designed marketing material, booths at numerous technical shows and meetings. We believe that, although a direct return rate is always difficult to evaluate and quantify, all these efforts are crucial in disseminating the NNIN message and making the NNIN better known among the researchers who could benefit from it. As a consequence, the LNF user community has again significantly grown over this past year, both in number of users and in terms of the number of research groups and organizations served. During these past 10 months, we have trained 52 new external onsite users, and now serve 145 external users (an increase of 27% over the previous year) from 79 organizations, 43 of which are new. Several of these organizations are making use of the off-site processing capabilities in which researchers send samples to be processed by NNIN@Michigan staff. These researchers often have their own fabrication facility and only need a single processing step, for instance because of specific capabilities available at our site (DRIE, wafer bonding, deposition of non-standard material, etc), and it can be most efficient to send samples to our facility. 7.10.2 Research Highlights Below are a few highlights for this past year from some of the LNF users. Prof. Cameron’s group at the University of Toledo department of Bioengineering has been using the LNF as part of their efforts on biomedical optics for medical Figure 144: Left: Uniform nano gold array fabricated by PVD gold onto nano- polystyrene beads coated surface. Right: Preliminary sensor response. NNIN Annual Report p.180 March 2011-Dec 2011 diagnostics and sensing. His groups has fabricated Localized Surface Plasom Resonance (LSPR) sensors chips to serve as a reliable, portable and sensitive biosensor platforms. Prof. Kaya and his research group at Central Michigan University have been using both the computation and fabrication resources at the Michigan site of the NNIN to design and fabricate a novel, three- direction MEMS capacitive accelerometer for health monitoring applications. COMSOL Multiphysics was used to study the working principle and the dynamic performance of the accelerometer. In the first step, the motion of the proof-mass was investigated by coupling the squeeze-film gas damping to the structural dynamic of the accelerometer. The modified Reynolds equation for perforated plate was implemented into COMSOL model to capture the proof-mass out- of-plane deflection. The maximum design acceleration was considered 5g in all directions. The magnitudes of von-mises stresses in the serpentine springs were calculated for the predictions of fracture Figure 145- Top: Profile of maximum failures under maximum design acceleration and deflections. A modal deformation of the proof-mass and analysis was also used to find the fundamental modes of vibration and serpentine springs; Bottom: Completed frequencies, in order to avoid resonance and identify the device range 1.5 mm x 1.5 mm capacitive accelerometers. of operation. At the end, a series of three-dimensional electrostatic finite element analysis was conducted to calculate the mutual capacitance between the moving and fixed fingers when the proof-mass is subjected to an in-plane design acceleration. Prof. Chronis’s group at the University of Michigan has been developing inexpensive lab-on-a-chip device for point-of-care monitoring of HIV/AIDS in the resource limited settings of the world. This biochip (microfluidic device) can perform CD4+ T-cell counting for HIV/AIDS monitoring, and a cell trapping biochip with a novel 3D trapping architecture has been developed for capturing human white blood cells (WBCs), with a high (> 90%) trapping efficiency. This biochip can be integrated with an on-chip microscopy technique, hence eliminating the need for bulky and expensive external Figure 147: Microfluidic biochip for trapping WBCs. Fluorescent image shows microscopy setup. WBCs trapped in the device. Prof. Reddy of the University of Michigan’s Nanoscale Transport LAB has been working on a project to achieve room-temperature picowatt resolution calorimetry, necessary for fundamental studies of nanoscale energy transport. They have reported a microfabricated device capable of <4 pW resolution—an order of magnitude improvement over state-of-the-art room temperature calorimeters. This was achieved by the Figure 146: Top: incorporation of two important features: (i) thermal isolation of Schematic of picowatt the active area of the device by thin and long beams and (ii) a calorimeter. Left: Measured temperature bimaterial cantilever thermometer capable of a temperature oscillations. resolution of 4 µK integrated into the microdevice.

NNIN Annual Report p.181 March 2011-Dec 2011 Prof. Yoon’s group at the University of Michigan has fabricated a neural probe which can selectively optically stimulate target neurons from an integrated optical waveguide and also monitor extracellular neural signals in electrical recording sites. The waveguide is composed of SU-8 core and oxide cladding layer to guide a light from optical source. A U-groove has been formed at the end of the waveguide for easy alignment with an optical fiber. The coupling loss Figure 148: Left: Schematic diagram of the proposed neural probe between the optical fiber and integrated with waveguides and SEM images of the fabricated probes. waveguide has been measured below - 3.7 dB with a waveguide loss of -0.22 dB/mm. Picocal is a local company which has been using the LNF for several years to develop a family of micro- cantilevers for high-throughput scanning probe microscopy. Simultaneous thermal, frictional, and electrical measurements can be obtained with MEMS probes, and scanning thermal allows the Figure 149: imaging of temperature changes and thermal Microfabricated properties at a scale not possible using traditional probes for scanning thermal microscopy methodologies like IR microscopy. Multiprobe arrays provide high throughput. At Montana State University, Prof Dickensheet’s group has Figure 150 :Left: MEMS deformable mirror been working on MEMS mounted for easy Deformable Mirrors for Focus implementation into focus Control Imaging Applications control imaging applications. Right: and used the LNF to Topside view of a mirror complement the capabilities of released in XeF2. their own facility. Prof Da Rocha’s group at Wayne State University is using the NNIN/C@Michigan resources to investigate polymeric nanocarriers such as dendrimers for local and systemic delivery of drugs to and through the lungs via oral inhalation. In this study, PEGylation is a very attractive procedure, as it can be used to modulate the interaction of the carriers with the biological environment, including transport modulation and protection of the therapeutic cargo from degradation. In this work they have used numerical simulations using to determine the effect of PEGylation on the structure of dendrimer nanocarriers, with Figure 151: Structure of G3 PAMAM dendrimer atomic-level detail. grafted with different densities of PEG1000.

NNIN Annual Report p.182 March 2011-Dec 2011 7.10.3 Acquisitions, Changes and Facility Operations The Lurie Nanofabrication Facility now occupies about 12,000 sq.ft and several new pieces of equipment have been acquired and/or installed during this past year, including our new JEOL JBX-6300FS. The unique features developed specifically on this tool for the LNF will allow the possibility of writing on non-planar substrates and substrates with high topological variations. This is made possible through the use of a Mitaka-Ryokosha Scanning Laser probe microscope which allows non-contact 3-D mapping of surfaces with nanometer-scale precision. The same Laser Probe Microscope nicely complements the LNF’s metrology capabilities. Other exclusive capabilities available on this JBX- 6300FS include the ability to pattern on transparent substrates, a Figure 152: JBX-6300FS Electron Beam 50MHz beam scanner, and write fields of up to 2mm X 2mm. Lithography System The JBX-6300FS has been released to the LNF community during this past year. Our analytical and characterization capabilities have also been increased over this past year. The Quantax 200 is a Silicon drift detector (SDD)-based EDS system, which has given the LNF new analytical capabilities to complement the Hitachi SU8030 FE SEM. The SDD (30cm2) detector requires no liquid nitrogen cooling, has lower dead time and orders of magnitude higher throughput and higher count rate than older detectors. The increased sample rate reduces the possibilitiy for sample damage and shortens acquisition time considerably. It also has a small volume interaction cross-section which improves the spatial resolution of the instrument. The superior capabilities of the Quantax 200 allow the user to detect thin films of the order of 3nm in just seconds. It also has automated mapping capabilities, easy to learn software, is very reliable, and extremely accurate. Users can detect the chemical composition of their films in seconds, and complements the topographic information they acquire in the SEM. It has been a welcome addition to the LNF. Users can do a point, line or map the whole sample in short time. It can detect elements from beryllium on up Figure 153: SEM and EDS to the heaver elements. mapping of Si, O, Au, Pb, and C on samples with patterned PZT In addition, we have enhanced the capabilities of our existing AFM by adding Tunneling AFM (TUNA) capability. This allows LNF users to measure current (down to femto-amperes) flowing between the tip and the sample upon the application of a voltage gradient (±10V). LNF users are further characterizing the electrical response of their nano structures using this attachment, such as I-V curves in nano wires, leakage current mapping, and electric field mapping. As part of the development of capabilities for the growing bio- community of LNF users, we have installed an Olympus BX51 Fluorescent microscope. This state-of-the-art vibration-isolated and environmentally-enhanced microscope is completely computer controlled and allows the user to perform routine measurements completely and automatically. It is a top down microscope designed for the MEMS fabrication user in mind, but also can be configured Figure 154: Olympus BX51 Fluorescent microscope installed on vibration isolation table. NNIN Annual Report p.183 March 2011-Dec 2011 for the bio-MEMS user. It has a motor-driven automated and programmable stage, motorized lens turret, and fluorescent cubes exchange. This allows the user to program hours of data acquisition automatically. In addition, it has DIC, DF and a high-speed camera to record movies in microfluidic devices or devices with movement. The microscope has been installed in a part of the LNF where we will have the ability to provide for a CO2 enriched atmosphere and complete darkness. The LNF has also continued process development on its new deep glass etcher: the SPTS’ Omega® APS process module. This advanced etcher has been proven to etch glass, quartz, graphite and PZT. Etch depths of 200 microns in glass have been achieved with etch rates nearing 1 micron per minute. Development of a deep etch process for silicon carbide has begun and etch rates near 2 microns per minute have been achieved thus far. In addition, the APS improves upon the dielectric etch applications previously in use. The combination of low pressure, high flow, high density, and high bias, allow process tunability not previously available at the LNF. This has equal applications in submicron work and nanofabrication as well. High aspect ratio submicron etch capabilities have been demonstrated. 7.10.4 Diversity Oriented Contributions To increase underrepresented minority participation in nanotechnology, we sponsored a booth and a 90- minute presentation at the NSBE regional meeting in Milwaukee, WI, and supported the NNIN Showcase for Students event at the SHPE conference held in Anaheim, CA. We have increased our interactions with intramural organizations, such as Women in Science and Engineering (WISE) and the Center for Engineering Diversity and Outreach, to support diversity initiatives in K-12. The LNF also continued its participation in the Laboratory Experience for Faculty (LEF) in 2011 with Prof. Kim Lewis from Rensselaer Polytechnic Institute working in collaboration with Prof Cagliyan Kurdak from the Physics department at the University of Michigan on electrodes for single molecule transistors. 7.10.5 Educational The LNF has continued its education mission through diverse programming that reflects the K-Gray spectrum of learning. K-12 and general public: A one-day Nanocamp was held for middle and high school students in the spring of 2011. During this camp students were exposed to fundamental concepts of nanotechnology in modules that utilized hands-on demonstrations. As this event was held in support of the NISEnet NanoDays program, numerous activities provided throught NISEnet were integrated into Nanocamp modules. One of the hightlights of this event for the students is the opportunity to work inside the cleanroom facitly to pattern and etch Au-coated wafers. A new module focused on bionanotechnology was developed in partnership with an Emerging Frontiers in Research and Innovation research program led by Ron Larson (George Granger Brown Professor of Chemical Engineering, and Professor of Mechanical Engineering and Macromolecular Science and Engineering). This event was also used as an opportunity to engage a broader audience by closing the event with a dynamic presentation for nanocamp participants and their families. The presentation delivered Max Shtein (Associate Professor of Material Science and Figure 155: 2011 Spring Nanocamp Engineering) was entitled “Better Lighting Through Nanotechnology”. A facility tour was also provided to all family members.

NNIN Annual Report p.184 March 2011-Dec 2011 Onsite efforts for elementary and secondary institutions included visits by high school students consisting of opportunities to participate in hands-on activities inside the cleanroom, a comprehensive behind-the- scenes tour of laboratory support systems, and panel discussions with undergraduate volunteers. Elementary students were introduced to the bottom-up approach to nanofabrication through games focused on self-assemblly in addition to learning how to don cleanroom suits. In addition, we also participated in Honey Creek Community School science nights and afterschool enrichment programs at Cody High School located in Detroit, MI. In our continued effort to assist K-12 teachers introduce nanotechnology into their classrooms, we have hosted a session at the 58th Annual Conference of the Michigan Science Teachers Association at the end of February 2011 in partnership with Prof. Dean Aslam from Michigan State University. The session focused on the disseminiation of network modules and novel methods to explore nanotechnology concepts in the classroom with hands-on activities based on Legos.

A sponsored award was given to select middle and high school students at the Southeastern Michigan Science Fair where we also served as judges. All winners of the sponsored award were guaranteed admission to the upcoming NanoCamp program. Undergraduate Students We have developed a partnership with the University of Michigan Undergraduate Research Opportunities Program (UROP). We provide introductory talks on nanotechnology and assist with developing/supporting nanotechnology related research projects. In addition, 6 undergraduate students participated in the NNIN REU program this summer, and one Japanese graduate student from the NNIN iREG program also worked at the LNF during the summer. Graduate Students and Professionals We organized several workshops and seminars on topics including advanced AFM techniques, deep RIE and high aspect ratio etching, and computation techniques for NEMS, MEMS and micro/nanofluidics were collectively attended by more than 150 faculty, industry professionals and graduate students. In addition, we provided support to faculty from regional institutions such as Central Michigan University and Oakland University. This included giving introductory lectures and providing hands-on demonstrations inside our cleanroom. We also supported regional sections/chapters of professional organizations, such as AVS, to increase the visibility of the network among various professional communities. NNIN@Michigan staff provided extensive support to the AVS Michigan 38th Spring Symposium which was held at Wayne State University in Detroit, MI. 7.10.6 SEI highlights NNIN@Michigan has implemented an SEI program for new users by leveraging network resources and best practices outlined in the network orientation user manual. We have found this approach affords flexibility to work within the specific attributes of our site (i.e. number of users, staff resources, user backgrounds) and establishes a firm baseline of exposure for the diverse user community. Additionally, we have continued to promote ethics throughhout the facility by maximizing the Figure 156: SEI Seminar organized for the local community visibility of posters, highlighting sustainability efforts and incorporating relevant terminology in our

NNIN Annual Report p.185 March 2011-Dec 2011 communication with users on various issues. Highlights from the past year included a seminar entitled "Rethinking science and technology innovation for the 21st century" by Prof. Andrew Maynard from the University of Michigan Risk Science Center. We were able to personalize our interactive discussions with new users by referencing our site-specific data found in the work of Robert McGinn entitled “Ethics and Nanotechnology: Views of Nanotechnology Researchers.” Our REU program was supplemented with more SEI related activities which included the development of a group presentation on Nanoethics and written summaries on engineering and professional ethics. Dr. Pilar Herrera-Fierro presented an overview of our laboratory sustainability initiatives at the Michigan Green Chemistry and Engineering Conference. Over the next year, we will continue to advance our SEI program by exploring strategic initiatives with stakeholders from the Risk Science Center.

NNIN Annual Report p.186 March 2011-Dec 2011 7.10.7 University of Michigan Selected Statistics (2011) a)Historical Annual Users

Michigan Cumulative Users-Historical

300 12 months

foreign 10 months 250 state and fed gov large company small company pre-college 200 2 year college 4 year college other university local site academic 150

100

50 Cumulative Annual Users Annual Cumulative

0 FY04 FY04 FY05 FY05 FY06 FY06 FY07 FY07 FY08 FY08 FY09 FY09 FY10 FY10 FY11 FY11 Local Other Local Other Local Other Local other Local other Local Other Local Other Local Other

c) User Distribution by Institution Type

Michigan Lab Hours - March 2011- Dec 2011 10 months Michigan Users - March 2011 - Dec 2011 10 months

small company large company 13% 1% State and Fed Large Company Foreign Gov 3% 2% other university 1% 3% Small Company 18% `

Other University 13% Local Site local site Academic academic 63% 82%

83,701 Hours-10 months

398 Users --10 months

d) Average Hours per User( in 10 months) e)New Users

300 Michigan Hours per User - March 2011-Dec 2011 (10 months) 80 Michigan New Users March 2011-Dec 2011 10 Months 250 70

60 200 50 150 40

100 New Users 30 Hours per User per Hours

20 50 10

0 0

Figure 157: University of Michigan Selected Site Statistics

NNIN Annual Report p.187 March 2011-Dec 2011

NNIN Annual Report p.188 March 2011-Dec 2011 7.10.8 University of Michigan User Institutions (2011) Outside US Academics Small Companies Large Companies Central Michigan University Advanced Micro Fab, LLC IMRA America, Inc. Cornell University Atactic Johnson&Johnson Kent State University Avto Metals PPG Industries MIT Baker Calling Stryker Instruments Miami University DeNovo Sciences Toyota Michigan State University Dexter Research Center Universal Display Corporation Oakland University ElectroDynamic Applications, Inc Watlow Electric Manufacturing Ohio State University Energy Conversion Devices Purdue University ePack US and State Government Rensselaer Polytechnic Inst. Evigia Systems, Inc. Air Force Research Lab Rice University Fraunhofer Institute Pacific Northwest National Lab Smithsonian Astrophysical Stanford University Grid Logic Observatory Texas A&M University H2scan UCLA Inos Technologies International University of Michigan Dearborn Integrated Sensing Systems A*Star IME University of Minnesota Intellisense Abbott Point of Care University of Nebraska k-Spaces Associates Holographics Canada University of Texas Austin LabSys JCP Processing & Consulting University of Toledo Lakeshore Cryotonics University of Washington Lumedyne Technologies University of Wisconsin Madison MEMS IC, Inc Wayne State University MEMStim Western Michigan University Midwest MicroDevices Small Companies (cont.) Yale University Nanoselect, Inc Silicon Designs Neuronexus Technologies Silicon Resources Nokomis Solid State Research, Inc Ovonyx Sonetics Ultrasound, Inc. PicoCal, Inc. STIgma Free Picometrix Structured Microsystems Promerus Technova Corp Radiation Monitoring Devices Translume Silicium Energy Visca LLC

NNIN Annual Report p.189 March 2011-Dec 2011 7.11 University of Minnesota Site Report 7.11.1 Summary of Initiatives and Activities The Minnesota node focuses on serving a large set of external users in a variety of areas including electronics, MEMS and alternative energy. A primary performance metric is the number of users, especially external users. The node engages in an aggressive recruiting process. Over the last year our number of users increased about 10%, as it has for the last three years. We now have users from more than 50 external universities or companies. External academic recruitment has been particularly effective with an increase of nearly 30% over the previous year. The amount of lab fees that we receive per external user, however, is low. This puts a significant burden on our staff in terms of training and providing service to these users. Dr. Jim Marti joined us as an external user coordinator and has been working to increase our number of new users. Major new capability area for the lab include lithography, especially our new 100 keV Vistec direct write electron beam lithography tool. This system was acquired after a successful grant application to the National Science Foundation’s Major Research Instrumentation program. It is on line and serving nearly two dozen users. Most work in the areas of nanophotonics, nanoelectronics, nanomechannics, and nanomagnetics. Minimum feature sizes down to 6 nm have been demonstrated. We have begun to market this system to bring in new external users for this and other tools in the facility. Other major tool acquisitions are listed below. Several of these stem from the NNIN MRI award. The major advance for the node, however, is the acquisition of University and State of Minnesota funds to build a new Physics and Nanotechnology building across the street from the Electrical Engineering building which houses the current cleanroom facilities. The building will house a new cleanroom with 5000 square feet under filter. Most of the nano systems will be moved to the new facility beginning in late 2013 when it opens. The current facility will continue to operate to support MEMS research as well as serving as a teaching facility. 7.11.2 Selected External and Internal Highlights Single Molecule Tunneling with Sub-molecular Resolution for DNA Sequence and Fragment Sizing Applications (Economist cover) Professor Joshua Edel from the Imperial College of London has developed a simple method to fabricate tunneling junctions aligned to a nanopore and proof-of-principle experiments demonstrating simultaneous detection of DNA translocations using both tunneling and ionic currents in a nanopore platform. The process involved the alignment of a nanopore and a nanoelectrode couple using high resolution lithography and Focused Ion Beam techniques. It was found that nanometer-scale pores (nanopores) are versatile single- molecule sensors for the label-free detection and structural analysis of biological polymers such as DNA, RNA, polypeptides, and DNA- Figure 158: Scematic of DNA sequencing scheme protein complexes in solution. MEMS-based Nanoindentation Transducers Using the Nanofabrication Center at the University of Minnesota, Hysitron, a leading manufacturer of nanomechanical test instrumentation, has developed a MEMS based transducer. The transducer has high precision actuation and high bandwidth dynamic characteristic as well as low noise level in displacement and force measurements. The advantages of this MEMS transducer for nanomechanical tests such as nanoindentation and topography scanning are tremendous since it has high bandwidth

NNIN Annual Report p.190 March 2011-Dec 2011 actuation, good controllability and can be used in many challenging environments such as in high vacuum and under high temperature. Owing to its small scale, the MEMS transducer can be used in instruments allowing extremely small space for transducer placement such as inside transmission electron microscope holders. Polymer-Based Sensing

Professor Michele Miller from Michigan Technological University has Figure 159 developed and optimized an inexpensive high performance integrated gas sensor system. The chemical and structural behaviors of the material were incorporated into the design optimization procedure. The device is prepared from a polymer matrix with a sensing probe coating. The sensor shows good dynamic performance even when operating at atmospheric pressure. The device has a steady state fluorescence response of the polymer in the presence of a test analyte (HF).

Figure 160 DNA Electrophoresis in Microfabricated Devices Professor Kevin Dorfman (Chemical Engineering at the University of Minnesota) developed new microscale methods for separating long DNA. His group built channels and observed single-DNA dynamics as well as studied separation resolution. Professor Dorfman was able to elucidate the role of the curved field lines on DNA dynamics and demonstrated the ability to separate DNA in sparse, ordered post arrays. He developed a method to fabricate sparse arrays of nanoposts without the need for conventional nanopatterning steps (e.g., e-beam lithography). He also developed a method to selectively grow ZnO nanowires into a separation microchannel and Figure 161 Post array for study of DNA studied the collision of a single DNA molecule with an isolated small dynamics post, confirming theoretical predictions.

NNIN Annual Report p.191 March 2011-Dec 2011 7.11.3 Equipment and Facility Highlights New Clean Room Minnesota has begun construction of a new Physics and Nanotechnology building. This will include a new clean room. The facility (5000 ft2 under filter, 10000 ft2 gross) will more than double our existing space. The new facility, across the street from the current cleanroom, is open to a meeting area and atrium, providing outstanding visibility for the nano activities (right). The existing facility will continue to operate focusing on MEMS and teaching, while the new facility will be focused on nano. Completion of the facility including acceptance of the cleanroom is expected in late 2012. Figure 162: Rendering of new Facility Heidelberg Laserwriter Using University of Minnesota funds, a Heidelberg DWL 200 laserwriter was purchased. The primary use of this tool will be to replace our optical pattern generator photomask fabrication system which is no longer supported by the manufacturer. The DWL 200 can define features down to 0.6um, and write a 5 inch mask plate in a few hours. In addition to maskmaking, the DWL 200 can be used for direct writing on a variety of substrates, from pieces to full wafers. We purchased the 3D lithography option, which will be useful for researchers working in micro-optics. A second option for backside alignment was purchased, which will be useful for those working in MEMS processing. Advanced Vacuum Etcher A Vision 320 reactive ion etcher (RIE) was purchased with ARRA funds. This is a batch RIE tool with a heated graphite electrode large enough for a 12 inch wafer. The tool will be primarily used for etching of

silicon dioxide, silicon nitride, and silicon using fluorine gases such as CF4, CHF3, and SF6. This is a workhorse system that will greatly increase our capacity for these commonly used processes. AJA International Sputter Deposition System AJA model ATC-2200 was purchased with ARRA funds. This multi-gun system is designed for sputtering a wide variety of materials, including metals, dielectrics, magnetic and optical materials. The tool has 6

magnetron sputter guns, loadlock loading, Ar, N2 and O2 gas capability, substrate heating to 500ºC, and optional substrate RF bias for pre-cleaning and for deposition. Samples sizes ranging from pieces to 8 inch diameter wafers can be accommodated through the loadlock loading system. The computer control system can be set up to run a fully automated deposition process. This is a workhorse system that will greatly increase our capacity for these commonly used processes. Cleanroom Facility Temperature Control Upgrade A major improvement to the temperature stability of the cleanroom was completed, allowing temperature control of +/- 0.1ºF. The upgrade involved installation of a heat exchanger to isolate the cleanroom temperature control process water from the university chilled water system. This prevents debris from the main university system from getting into the cleanroom system and causing cooling coil fouling. This upgrade was done with internal funding.

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7.11.4 Diversity Extended Tours & Presentations 1. Saint Paul Public Schools Exploration Day, March 9, 2011. NFC’s Outreach Coordinator, Dr. Jim Marti, presented an introduction to nanoscale and science/technology topics to 30 4th – 8th grade students from the St. Paul School District. Fifty percent of participants were from minority groups traditionally underrepresented in STEM careers. 2. Exploring Careers in Engineering and Physical Science (ECEPS), June 14, 2011 Dr. Marti gave tours of the NFC and presented a 2.5 hour class on nanotechnology to a group of 25 high school girls from schools around the Twin Cities metro area. This class was part of a University- sponsored Exploring Careers in Science and Engineering event aimed at attracting a more diverse population to the fields of science and engineering. Recruiting a more Diverse User Group Throughout the year in 2011, Dr. Marti contacted minority and female faculty members at several colleges and universities around the state of Minnesota to invite applications to NNIN’s Laboratory Experience for Faculty (LEF) Program. These contacts helped the NFC reach out to new potential users and to build a more diverse user group. One faculty member, Prof. Gina Samuelson of the St. Catherine University in St, Paul, has expressed interest in the program for the summer of 2012. Dr. Marti located a faculty sponsor at the University of Minnesota and got the two faculty members in touch to set up a summer research program. The Minnesota NNIN site plans to nominate Prof. Samuelson for the 2012 NNIN LEF Program. 7.11.5 Education Outreach Efforts Summary: 1. Saint Paul Public Schools Exploration Day, March 9, 2011 NNIN Outreach Coordinator Jim Marti presented an introduction to nanoscale and science/technology topics to 30 public school children attending "Exploration Day" at the University of Minnesota’s College of Science and Engineering. Students ranged from 4th – 8th grade and 50% of participants were from under represented minority groups. Topics covered included scale, types of nanotechnology, applications, lithography, activities on nanocoatings and self-assembly. Demonstrations and activities included magic sand, nano pants, self-assembly. Becky von Dissen served as tour guide/campus escort for groups. 2. National Science Teachers Association Meeting, San Francisco, March 12, 2011 The NNIN’s Jim Marti presented a workshop to 45 secondary school science teachers on using a photolithography demonstration kit, developed at the Minnesota NNIN site, for teaching lithography concepts in secondary schools. 3. Science and Engineering Day, March 29, 2011 This event, held by the College of Science and Engineering, works to attract industry to campus to celebrate Science and Engineering Day and hear about innovations and current research in a variety of fields. Steve Campbell provided a lecture on "Nano Applications and University-Based Resources" touting the NFC’s capabilities and resources for external academic and industry users; Jim Marti and Becky von Dissen staffed a booth exhibit with a display about NNIN and the Nanofabrication Center with emphasis on highlighting our work with external users. 4. Nano Night at the Science Museum of Minnesota, March 29, 2011 The NNIN’s Jim Marti and Jennifer Kuzma participated in a panel discussion on nanotechnology in food

NNIN Annual Report p.193 March 2011-Dec 2011 and consumer products with an emphasis on SEI. 35 general public participants attended. 5. NanoDays 2011 on campus, March 30, 2011 Jim Marti set up an activities table at the University’s student union during peak attendance hours to engage a general audience (students and visitors) with demonstrations of nanotechnology concepts and topics. About 30 people stopped by the table to learn and hear more about the demonstrations. 6. Minnesota Science Teacher Association Conference on Science Education, April 1, 2011 Becky von Dissen and Jim Marti traveled to attend the conference in Mankato, MN to host table/booth promoting NNIN and nanotech, and presented a session to 14 middle-school and high-school teachers on incorporating nano into classroom. Jim Marti presented a session to 14 middle-school and high-school teachers on incorporating nanoscience and technology into the classroom. About 20 people stopped by the booth which provided Nanooze magazines and a summary page describing the NNIN Education Portal website for their reference. 7. NNIN REU Summer Internship, summer 2011 Five NNIN REU students were selected to spend their summer at the U of Minnesota. Interns and projects included: Francisco Pelaez, DNA Barcoding in Nanochannels; Leah Laux, Microfluidics Immune System-on-a-Chip; Nathaniel Sheehan, Nanopatterned Graphene Device Fabrication and Characterization; Lauren Otto, High-throughput Fabrication of Metallic Nanostructure for Surface Plasmon Resonance Biosensing; Laura Windmuller, Nanoparticle Contamination Control and Metrology for Extreme Ultraviolet Lithography Systems. 8. Exploring Careers in Engineering and Physical Science (ECEPS), June 14, 2011 Jim Marti presented an introduction to nanotechnology class to about 25 female high school students. 9. Dakota County Technical College High School Nano Class, June 20, 2011 Jim Marti presented an introduction to photolithography to 10 high school students participating in a week-long summer nanotech class. 10. Exploring Careers in Engineering and Physical Science (ECEPS), June 22 & June 29, 2011 The NNIN’s Jim Marti conducted a tour of the Nanofabrication Center for groups of 45 and 25 students in the ECEPS program. 11. 7th Annual Minnesota Nanotechnology Workshop, November 15-16, 2011 This two-day workshop at the University of Minnesota offers presentations and discussions on topics including materials, devices, energy and medicine. The workshop, which was attended by approximately 200 people, also included a reception and poster session after Tuesday's talks. The reception allowed opportunities to network, view the poster exhibit, and talk one-on-one with researchers about their work. This workshop reaches more than 50 undergraduate and community/technical college students. It exposes them to this research and these discussions and allows them to network and discover education options in nano and related science/engineering areas. Three special introductory short courses were offered to workshop attendees during the 2011 event: 12. Micromachining: November 15 (12 attendees) This course was aimed at those in the fields of precision manufacturing and small scale devices. The objective was to educate designers of medical devices, precision mechanisms, and other devices on the ability of microlithography to fabricate very small structures. The course presented an introduction to surface and bulk micromachining, MEMS structures, and photolithography, and attracted 15 attendees. 13. Making Nano-structures with Electron-beam Lithography: November 16 (10 attendees) Electron-beam lithography (EBL) is currently the only mature technology capable of true nanoscale

NNIN Annual Report p.194 March 2011-Dec 2011 patterning, and as a result is a critical tool in the nanotechnologist's toolbox. The Vistec EBPG5000+ EBL system recently acquired by the NFC is a state-of-the-art tool that uses a focused beam of electrons accelerated to 100 keV to pattern features 10 nanometers wide and smaller. This course will cover the principles of electron-beam lithography as well as the capabilities of the EBPG5000+, and includes a hands-on demonstration of the tool's patterning capabilities. Ten people attended the short course, 14. Thin Film Coatings: November 15 (12 attendees) Thin films are used in many industries, from optics to electronics to medical devices. This course will introduce the processes of thin film deposition and characterization. Class members will learn about thin film applications and the most common thin film deposition methods, then get hands-on experience by depositing and testing thin films using the tools in the NFC. This course attracted 12 attendees. 7.11.6 SEI Activities

During early 2011, a polished Social, Ethical, Implications (SEI) Discussion and Module were created, ready to be delivered to Nanofabrication Center (NFC) users at the University of Minnesota. The main content for the Guide and Module was researched, assembled, and refined by Humphrey School of Public Affairs student Jonathan Brown, and reviewed and critiqued by Humphrey School faculty member Dr. Jennifer Kuzma, during summer and fall 2010. Information and discussion from NNIN SEI workshops held in January 2010 (hosted by Cornell University) and October 2010 (hosted by Washington University in St. Louis), and SEI presentations/discussions with two groups of REU students during summer 2010 assisted with content generation and editing. The final SEI Module consists of the SEI Discussion powerpoint slides , a pre- and post-survey for attendees, and worksheets containing discussion questions presented in the session.

The first SEI session was conducted as a 60-minute pilot in March 2011. Since the pilot, the Module was approved for further implementation in all follow-up sessions. Throughout the remainder of 2011, sessions have been conducted about one to two times per month and will continue at such a rate indefinitely, dependent upon the number of new NFC users. All sessions have been led by Jonathan, lasted between 1.5 to 2 hours, and had groups sizes ranging between 2-12 attendees. Format for all sessions has been as follows: introductions, pre-survey, 20-30 minute informational overview, 60-90 minute group discussion of prepared SEI questions/issues, and post-survey. For groups six attendees or larger, group discussion involves first tackling the given question/issue in groups of two to three and then sharing ideas with the larger group later on. For groups five or smaller, group discussion consists of individuals jotting down notes on a sheet a paper explaining the question/issue and then discussing the question/issue as a whole group. The aforementioned format will continue to be used, though questions/issues covered and information presented may be adjusted periodically.

In November 2011, Dr. Kuzma attended the NNIN SEI Workshop at the SEI Congress on Teaching. She presented a poster drafted by Jonathan, explaining the SEI Module conducted at the University of Minnesota, the methods employed, and select results from the pre- and post-surveys.

---End of University of Minnesota Text Report----

NNIN Annual Report p.195 March 2011-Dec 2011 7.11.7 Minnesota Selected Site Statistics (2011) a)Historical Annual Users

Minnesota Cumulative Users-Historical 600 12 months

500

foreign 400 state and fed gov large company small company pre-college 300 2 year college 4 year college other university (significant change 10 months in scope of NNIN facility) 200 local site academic Cumulative Annual Users Annual Cumulative

100

0 FY04 FY04 FY05 FY05 FY06 FY06 FY07 FY07 FY08 FY08 FY09 FY09 FY10 FY10 FY11 FY11 Local Other Local Other Local Other Local other Local other local other Local Other Local Other

b) Lab Hours by Institution Type c) User Distribution by Institution Type

Minnesota Lab Hours March 2011-Dec 2011 10 Months Minnesota Lab Users March 2011-Dec 2011 10 Months

small company large company state and fed gov 9% small company foreign 3% 0% 6% large company 1% 3% 4 year college foreign 4 year college 1% 1% 1%

other university 6% other university local site 14% academic local site 72% academic 83%

16,586 Hours--10 months 272 users--10 months

d) Average Hours per User( in 10 months) e)New Users

100 90 Hours per User March 2011-Dec 2011 10 Months Minnesota New Users March 2011-Dec 2011 10 Months 90 80 80 70 70 60 60 50 50 40 40 New USers

Hours per User per Hours 30 30 20 20

10 10

0 0

Figure 163 University of Minnesota Statistics

NNIN Annual Report p.196 March 2011-Dec 2011

NNIN Annual Report p.197 March 2011-Dec 2011 7.11.8 University of Minnesota User Institutions (2011) Outside US Academic Small Companies Large Companies Bethel University Advanced Research Corp. BF Goodrich Carleton College American Medical Entegris Macalester College Aveka, Inc. Medtronic, Inc. North Dakota State University BH Electronics, Inc. Seagate Technology University of Evansville Bioforce Nanosciences Valspar Univ. of Wisconsin - Stevens Point Chameleon Scientific Clemson University Hysitron, Inc. Iowa State University IIIAN Company, LLC Michigan Technological University Kevin Roberts Consulting International MIT Koral Labs ETH Zurich Montana State University Physical Electronics Imperial College London Olin College of Engineering Polyera Corp University of Trieste Purdue University Sage Electrochromics Saint Cloud State University SVT Associates, Inc. State & Federal South Dakota State University TLC Precision Wafer Tech. Argonne National Laboratory Texas A&M Vixar University of California San Diego Univ.California Santa Barbara University of Iowa University of Nebraska - Lincoln University of Texas Austin University of Texas El Paso University of Wisconsin - Madison Washington University in St. Louis

NNIN Annual Report p.198 March 2011-Dec 2011 7.12 University of Texas Site Report 7.12.1 Technical leadership areas: Initiatives and Activities The UT-Austin technical leadership areas comprise nanofabrication instrument design and process research through techniques such as nano-imprint lithography (NIL), electron beam lithography and chemical & molecular-scale methods with major emphasis on materials and manufacturing. Three examples of successful Austin-based manufacturing company are presented. MRC supported their developments by hosting these starts up and by providing scientific exchange and access to equipment. Some of these starts up are yet to make the necessary breakthrough to present manufacturing viable products. Besides to become independent entities, some of these starts-up uses MRC for supporting their productions. Examples of advanced research undertakings in the MRC in industrial areas are described below. Jet-and-Flash Imprint Lithography for HDD Storage One of the core-strengths of the MRC for nano-imprint patterning involves Jet-and-Flash Imprint Lithography (J- FIL™) methods. At MRC imprint processes are conducted on the IMPRIO100 tool, acquired in 2005 from the MRC- hosted start-up Molecular Imprints Inc. (MII). MII is one of the successful U Texas spin off from co-inventors Profs. C G Willson and S V Sreenivasan. Created in 2003, MII is the industry leader for nanoimprint production systems with Perfecta MR5000, a $4M system for template replication of 6025 masks and with NuTera HD7000, a dual side imprint system that demonstrate a throughput as high as 300 Figure 164: IntelliJet Drop Pattern disks/h for patterned media hard disk drives (HDD). The Generator in hard disk drive applications by revolutionary MII techniques are based on a Jet Drop Pattern Molecular Imprints Inc. Generator (resist version of a inkjet printer module) that optimizes the consumption of photoresist by replacing the spin coating step with a resist drop pattern exactly matching the pattern layout. The resulting HDD, with a patterning cost less than 50¢ / plates for the 20x nm and beyond are implemented to provide data storage at densities exceeding 1012 bits/in2. MRC supports MII development activities by offering a suite of state-of-the–art metrology tools and jointly acquire RIE equipment. A portion of MII employees are users of the MRC cleanroom to sustain production lot analyzes and samplings. Test & Measurement for the Photovoltaic (PV) Industry Atonometrics Inc. an Austin-based start up company wasfounded in 2007 by W Stueve and benefited from the MRC infrastructure and research environmment. With 2 former graduates students from MRC, Atonometrics started developing test and measurement technology designed to help PV manufacturer scale up production. After 3 Figure 165: Perfecta MR5000, years hosted in the MRC building, the company got her own Nanoimprint lithography 6025 semiconductor mask replication. location. Atonometrics with close to 20 employees offer unique Throughput: 4-mask replicas/ h. equipment for PV module reliability testing in high-volume manufacturing environments, and a range of test and measurement services

Nanofabrication for Clean and Renewable Energy Dharmesh Jawarani and Leo Mathew, co-founded AstroWatt, an Austin-based venture backed company,

NNIN Annual Report p.199 March 2011-Dec 2011 developing a proprietary solar cell technology. To meet the growing global demand for renewable energy Astrowatt developped and fabricates at MRC ultra thin (25 micron), high efficiency (15%) c-Si photovoltaic solar cells. This novel solar cell architecture has been obtained using the MRC facilities by a patented exfoliation process : Semiconductor on Metal (SOM). The advanges of using a thin substate for fabricating solar cells are multiples: higher efficiency by design, lowest cost due to less material utilized, emergence of newer applications due to the flexible thin crystalline silicon. The Astrowatt solar cell are prefectly manufacturable in a Figure 166: Astrowatt high efficiency standard semiconductor plants. Astrowatt is now focusing on working ultra thin solar cells to be stringing on a 5inch module. around the handling issue with thin 25 microns substrates to obtain a viable manufacturing products. This technology has also been demonstrated for other substrates such as Ge and GaAs in different research groups at UT. 7.12.2 Acquisitions, Changes, Operations The Microelectronics Research Center of The University of Texas at Austin recently acquired a new set of state-of-the-art instruments that complement its existing nanofabrication strengths, while also expanding capabilities for manufacture and test of nanoscale devices and materials. Some of the new tools are: • Oerlikon sputtering system with 3 targets of 4 inch, running at a vacuum of 5e -7 Torr. The 1-m3 chamber could accommodate up to 4 wafers of 4 inch and provide a film uniformity of 5% wafer-to- wafer and run-to-run. This system replaced our 25 years old Varian sputtering tool for Al metallization. • Different equipment donated to the MRC UT Austin had been installed, tested and open to the share access. Among those, we count an Asher, a Leizt optical microscope with BF and DF capabilities, a CHA E-beam evaporator with four 12cc pockets. Figure 167: MRC U Texas operations team To serve over 300 MRC annual cleanroom facility users, the team led by Prof. Banerjee comprises 8 technicians and engineers. 7.12.3 Diversity Activities The University of Texas participated in the NNIN-sponsored Laboratory Experience for Faculty (LEF) program, which enabled research experience for faculty member belonging to a minority serving institution. In summer 2011, two professors from Texas A & M at College Station (Texas): Prof. Haiyan Wang and Prof. Christi K. Madsen were hosted at the MRC to advance their research programs. MRC contributes to education programs that focus on under-represented communities in science and engineering. MRC Graduate Research Assistant Michael Ramon participated in the Society of Hispanic Engineers (SHPE) Conference. On 27 Oct 2011, Michael Ramon, helped to set up and demonstrate the use of AFM, SEM and various microscope at the Anaheim 2011 conference. This event involved discussions with the attendants in the career fair and the nanotechnology showcase. The audience of this conference included more than 5,000 students, professionals, corporate representatives, educators and community leaders from all over the United States. 7.12.4 Education Since 2004, MRC has accommodated Research Experience for Undergraduate (REU) scholars. Last

NNIN Annual Report p.200 March 2011-Dec 2011 summer UT Austin supervised 5 undergraduate students along the NNIN REU program. The REU participants consisted of three females and two males, working with UT professors and postdoctoral and graduate students, acting as mentors on research projects in diverse areas such as simulation, biomedicine and nanoelectronics. In addition to the REU students, UT Austin also hosted a graduate student from the Japanese Nanonet (a network similar to NNIN, guided by the National Institute for Materials Science, NIMS). The visiting students engaged in developing shape-Specific FePt Nanocrystals for - Transfer S p in Torque in Magnetic Tunnel Junctions (Kai He), synthesis of Few Layer Graphene Films of Large Lateral Dimensions (Claire Spradling), Fabrication and Testing of Voltage- Tunable - InfraredPlasm onic (Ting M etam Chia aterials Chang), in SynthesisM id of Silicon and Germanium Nanowires (Yoichi Ogata), Utilizing Solution-Grown Silicon Nanowires in Photovoltaic Devices (Elizabeth Fullerton), Growth and Characterization of Graphene for Use in Graphene Effect Transistors (Bethany Robinson). UT-Austin’s education program organized 4 minor events (tours) and contributed to 3 major national events in 2010. • On 17-19 Nov 2011, U Texas co-exhibits with Georgia Tech a NNIN booth at the largest science teacher conference of the nation with 5,907 attendees. The NNIN booth was set-up for this 3 days conference in the giant convention center at Dallas. Hands-on activities were proposed. Nancy Healy and Joyce Palmer (Georgia Tech) jointly with Marylene Palard (Texas), distributed more than 6,000 Nanooze magazines and promoted nanotechnology to the teachers who visited the Figure 168: Science Teacher Association of Texas booth. The goal was to explain to elementary, (STAT), 2011 conference at Dallas middle and high school level teachers how to include nanotechnology to the scientific curriculum they are teaching. • MRC UT-Austin offered cleanroom tours during the year. During these guided tours, MRC specialists gave a synopsis of micro and nano fabrication, equipment and applications. Individuals from dissimilar age groups and different professional areas attended the tours: summer camp students, K-12 students and teachers, Associate Vice Chancellor for Research at UT System, Oakridge National Lab –Consortium, and Industry and External University conference participants. 7.12.5 Social and Ethical Issues (SEI) The MRC safety coordinator, Darren Robbins, schedules twice-a-week orientation sessions for new users. The SEI component is embedded in this training, and is fulfilled using an in-house developed presentation that discusses the benefits and risks of using nanomaterial, analyzing the case of silver nanocrystals as antibiotic and therapeutic tools in Figure 169: 400,000 kilowatt-hours solar energy living beings. With MRC 1.75 acres solar energy system field at MRC UT Austin installed in June 2011, emphasis on renewable energy using nanoscale processes for PV powers is given during SEI orientation. A comprehensive review of safety procedures (emergency exits, cleanroom protocol to dispose acids, solvent and other chemicals, safety gear to handle chemicals, etc.) follows the Social and Ethical Issues (SEI) discussion. Questions and comments from the new trainees are stimulated during the discussion.

NNIN Annual Report p.201 March 2011-Dec 2011 On 27-29 Nov 2011, U Texas contributed to the NNIN SEI workshop. It was a true exchange between scientists and researchers with philosophers and ethicists. Dr. Sushant Sonde was the Texas representative at these 2 days conference hosted by the University of Arizona. This SEI meeting served to know more about the approach adopted in other sites, and guided MRC UT Austin on how to improve and ignite SEI discussions in our site. ---End of Texas Text Report--

NNIN Annual Report p.202 March 2011-Dec 2011 7.12.6 University of Texas Selected Site Statistics (2011) a)Historical Annual Users 350 Texas Cumulative Users- Historical

300 12 months

foreign 10 months 250 state and fed gov large company small company pre-college 200 2 year college 4 year college other university 150 local site academic

100

50 Cumulative Annual Users Annual Cumulative

0 FY04 FY04 FY05 FY05 FY06 FY06 FY07 FY07 FY08 FY08 FY09 FY09 FY10 FY10 FY11 FY11 Local Other Local Other Local Other Local other Local other local other Local Other Local Other

b) Lab Hours by Institution Type c) User Distribution by Institution Type

Texas Lab Hours March 2011- Dec 2011 10 Months Texas Lab Users - March 2011-Dec 2011 10 Months large company 1% foreign large company 1% small company foreign 1% 20% small company 1% 20%

2 year college local site 1% academic 69% other university local site 13% academic 65% other university 8%

260 Users -10 months 43,083 Hours - 10 months

d) Average Hours per User( in 10 months) e)New Users

300 120 Texas Hours per User March 2011-Dec 2011 10 months Texas New Users- March 2011-Dec 2011 10 months 250 100

200 80

150 60 New Users 100

Hours per User per Hours 40

50 20

0 0

Figure 170: University of Texas Site Statistics

NNIN Annual Report p.203 March 2011-Dec 2011

NNIN Annual Report p.204 March 2011-Dec 2011 7.12.7 University of Texas User Institutions (2011) Outside U.S. Academic Small companies Large companies Trinity Univ (San Antonio) Astrowatt Toppan Global Masks Samsung Austin UT Arlington Cerium Labs Semiconductor Texas A&M Displaytip Rice University Illumitex Inc. University of San Antonio MetaMaterials UT Houston Molecular Imprints International King Abdullah University of Science and Technology Nanohmics Inc (KAUST) NanoMaster Nanomaterials Characterization Group NanoMedical Systems Inc. Other The Methodist Hospital Optical Filter Sources System, Houston, Texas Quantum Logic Devices Sematech Sheetak Stellar Micro Devices PrivaTran

NNIN Annual Report p.205 March 2011-Dec 2011 7.13 University of Washington Site Report 7.13.1 Overview The University of Washington NNIN node (UW-NNIN) has primary responsibilities in the areas of biological and life sciences, society and ethics (SEI), and in connecting the network to the aquatic and geoscience communities. UW-NNIN employs a technical staff of 9 and consists of the Nanotech User Facility (NTUF) and Microfabrication Facility (MFF). NTUF occupies 3,000 sq ft of newly renovated laboratory space equipped with tools and facilities targeted towards the investigative needs of nanobio users. It also provides complementary e-beam lithography, deposition and soft and photolithography services. The adjacent MFF occupies 15,000 sq ft of space and provides access to e-beam lithography, photolithography, thin-film deposition, plasma and chemical etching, and metrology. In July 2011, ownership of the MFF was transferred from the state of Washington Technology Center to the University of Washington which has embarked on an extensive program of facility and equipment upgrades (see below). Over the reporting period, UW-NNIN served 387 users coming from the local site, 11 other academic institutions, 25 small and 9 large companies. 7.13.2 Aquatic and Geo Sciences News Together with U. Michigan, and with the support of Cornell, Stanford and Georgia Tech, U. Washington has primary responsibility in connecting the network and its users with the aquatic and geoscience communities. As part of an ongoing effort to raise NNIN awareness, U. Michigan and U. Washington staff held a well-attended booth at the 2011 American Geophysical Union (AGU) Fall Meeting in San Francisco. These efforts are starting to pay off: over the current reporting cycle, 11 users and one company performed geoscience-related research at UW-NNIN. Among these, Don Brownlee (UW Astronomy) analyzes cometary and interplanetary material brought back to earth by the 2006 NASA Stardust mission. Comets are among the most primitive bodies in the solar system and preserve records of chemical processes that occurred during the Figure 171: SEM image and EDS analysis of interplanetary formation of our sun and planets. The morphology and elemental/mineral dust. composition of interplanetary dust particles is being examined at UW-NNIN to inform astronomers’ theories on the formation of solar systems, the interstellar distribution of elements and compounds, and the “life cycle” of comets (Fig.171). Thanks to a white paper elaborated during the 2010 “Nano-Enabled Sensing Microsystems for Geosciences” U. Michigan workshop, Qiuming Yu (U. Washington), Vera Trainer (NOAA), Mark Strom (West Coast Center for Oceans and Human Health) and Mark Wells (U. Maine) received funding from NOAA-OHHI to develop Raman-based barcoding techniques for the identification of marine pathogens. Using Prof. Yu quasi-3D plasmonic nanostructure arrays, the group demonstrated that biochemical information embedded in the pathogens’ cell wall could be used to identify strains of Vibrio parahaemolyticus by surface-enhanced Raman spectroscopy (SERS) with high sensitivity and reproducibility. This has allowed for the construction of SERS “barcodes” for each strain (Fig. 172). With this approach, unknown samples and mixtures of multiple strains can be quickly identified. Furthermore, barcodes can be used to correlate genomic and phenotypic variation among strains. Proposals to expand upon this work have been submitted to USDA and DTRA. Two papers Figure 172 ERS barcodes of 3 different strains of V. parahaemolyticus

NNIN Annual Report p.206 March 2011-Dec 2011 (one of which having a 2011 NNIN REU as co-author) have been published and one manuscript is in preparation. 7.13.3 Research Highlights Marco Rolandi (UW MSE) reported in Nature Communications the development a protonic field effect transistor (H+-FET) that controls the flow of protons instead of electrons, making it a good potential starting point for bio-interface devices.In biology, it is generally the movement of ions, instead of electrons, that controls processes such as ATP synthesis and the opening of channels in cell walls to allow transport of materials into and out of living cells. Protons (H+) play a key role in ATP synthesis.The H+-FET consists of maleic chitosan fibers bridging the source and drain of the transistor, which are made Figure 173: AFM image of the of proton-conducting PdHx. Maleic chitosan is a biodegradable, non- protonic field effect transistor toxic polysaccharide chitin derivative that is extracted from squid pen. developed by Rolandi. Over 50 news and media outlets including the New York Times, IEEE Spectrum, MRS Materials360, Popular Science, Materials Today and Engadget picked up the story. In research performed at the U. Washington and Cornell NNIN sites, Michael Hochberg (UW EE) has built silicon waveguides for mid- infrared (MIR) wavelengths at 5.5 µm (Fig. 174). Such waveguides had not been demonstrated past 3.5 µm before. The working ring resonators were fabricated using silicon-on-sapphire material and direct-write electron beam lithography. MIR wavelengths have applications in thermal imaging, spectroscopy, and bio-sensing. The Figure 174: 3D rendering of a ring ability to fabricate MIR silicon photonics with nanometer precision resonator showing optical mode propagation through a waveguide. creates opportunities for new complex systems at these wavelengths. The mitotic spindle is an exquisite molecular machine that organizes and separates Figure 175: Schematic of chromosomes during cell division. To uncover its two-state model with detachment during assembly mode of action, an interdisciplinary group consiting and disassembly (rates k3 of Sue Biggins (Fred Hutchinson Cancer Research and k4, respectively), and interconversion between Center), Jeffrey Ranish (Institute for Systems states. Biology), and Charles Asbury (UW Physiology and Biophysics) have reconstituted spindle function by employing tools to manipulate individual molecules. In a Nature article the group showed that chromosome-spindle attachments behave like Chinese ‘finger-traps’ (i.e., that they are more stable when pulled). This helps explain why division is so accurate as improper attachments, which lack tension, are selectively destabilized (Fig. 175). The pn junction is the backbone of most Figure 176:. Devices on CVD-grown graphene show electronic and optoelectronic devices. The the scalability of the Xiaodong Xu group (UW Physics) has structure (left). The magnified image of a typical fabricated pn junctions in monolayer device (top right) and a map graphene using a local top gate and a of the generated global bottom gate to electrically bias photocurrent (bottom right) are shown. different areas of graphene to form the junction. This device structure has been demonstrated both on individual graphene flakes and on large sheets of chemical vapor deposition grown

NNIN Annual Report p.207 March 2011-Dec 2011 graphene. With these devices, they study the ultrafast response of Dirac fermions with pump-probe photocurrent techniques for applications in new light harvesting and light detecting technologies. 7.13.4 Equipment, Facility and Staff Highlights Equipment – A Fischione 1050 Ion Mill was delivered in August and made available to users in September 2011. This advanced mill is designed to thin semiconductors, ceramics, and metals to electron transparency for TEM studies. It greatly enhances UW-NNIN materials and nanostructure sample preparation capabilities. A Filmetrics F50UVX thin-film analyzer (reflectometer) was delivered in December and comissioned in January 2012. The tool measures index of refraction and thickness/uniformity of thin films between 5 nm and 250 μm and is a critical component of establishing statistical process controls. It is equiped with a near infrared option to facilitate the characterization of silicon-on-insulator (SOI) wafers. Staff – The transfer of MFF from the Washington Technology Center to U. Washington was accompanied by significant personnel changes starting with the appointment of Electrical Engineering Prof. Karl Böhringer as Faculty Director and the recruitment of Dr. Michael Khbeis as Associate Director. With 15 years in semiconductor fabrication, 2.5/3-D integration, and advanced packaging research and development experience from the Department of Defense and Matsushita Semiconductor, Dr. Khbeis brings a wealth of experience to the facility. Two staff members (Mike Hjelmstad and Paul Schilling) were retained and three new engineers were hired. Rick Bojko, who has extensive expertise in EBL from Cornell, Westinghouse Research, Northrop Grumman, Seagate Technogology and most recently the UW Nanophotonics Lab, was hired as JEOL EBL specialist. Steve Potter, a 35-year veteran of the semiconductor industry, specializing in III-V compound semiconductor manufacturing with M/A-COM and TriQuint Semiconductor was hired to support physical vapor deposition (PVD) and EBL operations. Finally, Kris Lawler, whose background in fabrication technologies from the Opto-Electronic and Lightwave Engineering Group at NCSU was hired for general equipment support. At NTUF, Scott Braswell was appointed TEM specialist and Lindsey Maier joined the staff as SEM/EBL specialist in April 2011. Lindsey previously worked with Semion on Focused Ion Beam tools. 7.13.5 Educational Highlights In cooperation with the MDITR STC, UW-NNIN expanded its series of web-based video training modules. These now includes SEM operation, TEM operation, EBL, Raman microscopy, mask writing, ellipsometry, and liquid mode AFM for biological applications. The latter video was created by external users from Seattle University. All videos are posted on You Tube or Jove and are indexed on the UW-NNIN site at https://depts.washington.edu/ntuf/facility/training.php#video. As of January 2012, they had been viewed nearly 105,000 times. The special REU program for students enrolled in the North Seattle Community College (NSCC) Nanotechnology AAS-T degree program continued in 2011. This year, two NSCC interns conducted research in cryo-etching and low-temperature deposition of gate dielectrics by ALD. UW-NNIN also supported the continuation of Penn State’s ATE National Nanotechnology Applications and Career Knowledge (NACK) Center by helping NSCC establish the Seattle’s Hub for Industry-driven Nanotechnology Education (SHINE).

Figure 177: PdS “Los Nanobots” As in previous years, UW-NNIN arranged for multiple lab tours for team presenting their project to their elementary, middle and high school students. In a special treat, two mates and the UW-NNIN staff. student groups participating in the First LEGO Robotics competition (http://www.firstlegoleague.org/) visited the site prior to competition.

NNIN Annual Report p.208 March 2011-Dec 2011 Puesta del Sol’s M.E.N.T.E. (Movimiento y Exploración de Nuevas Tecnologías en Equipo) 4th grade team presented their project – “Los Nanobots” – on preventing milk from spoiling using nanobots (Fig. 177). The second group, “Hot Plasma”, consisted of 6th graders from Tyee Middle School and other private institutions in Bellevue, WA. This group’s research interest was in the detection of reversing of DNA in GM foods by using nanobots. 7.13.6 SEI Highlights UW-NNIN SEI activities are coordinated by the Center for Workforce Development (CWD) which is interviewing nanoscientists and nanoengineers at five NNIN sites to examine: 1) career pathways of men and women scientists; 2) perceptions on risks and benefits of nanotechnology; and 3) views on promoting social and ethical awareness in the nanotechnology community. Interviews focused on career pathways, perceptions of risk, and public awareness have been conducted with NNIN faculty at Cornell, Stanford, Georgia Tech and U. Washington. Eighteen faculty were added this year for a total of 59 faculty interviewed and more will be included this coming year. Preliminary findings indicate that: • The interdisciplinary aspect of nano is highly attractive to both men and women working in the field • At every stage of their careers except graduate school, fewer men than women acknowledge receiving mentoring. Full one in five men claim to never have been mentored. Yet, despite this, more men than women claim to be currently acting as mentors • Roughly twice as many women as men view their engagement in nanotechnology as secondary, or see nano primarily useful as a tool, rather than being the central focus of their scientific interests. Over the reporting period, CWD presented a paper at S. Net 2011 and submitted a manuscript to the Journal of Engineering Education entitled “Factors and perspectives influencing nanotechnology career development: Comparison of male and female academic nanoscientists”. CWD also held a NSF-funded Nano and Gender Workshop at AAAS in Washington DC that brought together leading national researchers in the social sciences and nanosciences to provide direction to the NSF on how nanotechnology can benefit from increased participation of women faculty. A monograph summarizing results and recommendations has been published and disseminated nationally. Nature Alerts published a brief summary of the Nano and Gender Workshop. The Societal and Ethical Issues in Nanotechnology class fulfills NSF-NNIN requirements for ethical education. Training is now a mandatory step in new user registration and training sessions are usually held monthly depending on user demand. Class curricula has been developed through several iterations of instructors, including an education and outreach coordinator, and graduate students in electrical engineering, philosophy, and chemistry.

----End of University of Washington Text Report---

NNIN Annual Report p.209 March 2011-Dec 2011 7.13.7 University of Washington Selected Statistics (2011) a)Historical Annual Users

Univ. Washington Cumulative Users-Historical

400 12 months

350 10 months

300 foreign state and fed gov 250 large company small company pre-college 200 2 year college 4 year college other university 150 local site academic

100 Cumulative Annual Users Annual Cumulative 50

b)Lab Hours by Institution Type c)User Distribution by Institution Type

Univ. Washington Lab Hours March 2011-Dec. 2011 10 months Univ. Washington Users by Type- March 2011-Dec 2011 10 Months

large company small company 3% 11% large company 4 year college state and fed gov state and fed gov 1% 12% 0% 1% foreign small company foreign 1% 23% 0% other university local site 3% academic 60% local site 2 year college academic 3% 80% 4 year college 375 unique users--10 months 1% other university 1% 14,444 hours--10 months

d) Average Hours per User( in 10 months) e)New Users

250 Univ. of Washington Hours per user- March 2011-Dec 2011 10 months 140 Univ. of Washington New Users- March 2011- Dec 2011 10 months

200 120

100 150 80

100 60 New Users Hours per User per Hours 40 50 20

0 0

Figure 178 University of Washington Selected Statistics

NNIN Annual Report p.210 March 2011-Dec 2011 7.13.8 Univ. of Washington User Institutions (2011) Academic Small Companies Large Companies Bradley University Component Concepts Aerojet North Seattle CC EnerG2 Google, Inc. Pacific Lutheran University EO Space Heideberg Plasma Technologies Seattle University EO Tron Janicki Industries University of Maine Gigoptics Lockheed Martin -- Aculight Western Washington University GoNano Technologies Microsoft Halo Source Inc. PCB Piezotronics MEMS Group Healionics Corp. Sharp Labs of America Impinj Intel Integrated Photovoltaics Inc. MicroGreen Polymers, Inc Microvision International Modumetal Aalborg University (Denmark) NanoICE Al Azhar University-Gaza Centre for Cellular and Molecular New Light Industries Biology (India) Harbin Institute of Technology Nortis (China) Paine Electronics Revalesio Corp RJC Enterprises Other Silicon Designs inc Arctic Medical (nonprofit) Spiration Fred Hutchinson Cancer Center Stratos Biosystems Stratos Genomics Targeted Growth VisionGate

NNIN Annual Report p.211 March 2011-Dec 2011 7.14 Washington University in St. Louis Site Report 7.14.1 Overview The Nano Research Facility (NRF), a new NNIN node at Washington University in St. Louis, completed the third-year of operation. The focal areas are in nanomaterial environmental health and safety; applications in medicine (nanomedicine), and in environmental and energy applications. In addition to our existing characterization equipment (see www.nano,wustl.edu ), we solidified capabilities in the class 100/1000/10,000 clean rooms (2,150 sqft) and leveraged the new reactive ion etching system to bring in additional users. We expanded our unique capabilities in the synthesis of functional nanomaterials and included superparamagnetic nanoparticles and gold nanoplates to our portfolios for potential applications in drug delivery and surfaced enhanced raman spectroscopy; we have begun development of an approach to evaluate the growth inhibiting effects of silver nanomaterials on plants by monitoring the biomass growth of arabadopsis in the presence of silver nanoparticles; and we added an additional capability, fluorescence microscopy, to the NRF Bio-imaging Lab. As a new node in the NNIN community, NRF is growing by providing unique technical capabilites in nanotechnology research at the intersection of public health and the environment, anticipating specific needs from the research community, and improving user training and support. We have actively promoted NNIN to the regional research and industry community by attending regional workshops and providing tours and demonstrations to local schools and companies. In Fall 2011 NRF welcomed visitors from companies including Boeing, Monsanto, TSI, and Rusnano. The NNIN serves as a catalyst to change the research and education landscape at Washington University and in the St. Louis region. By providing open facilities with multi-diciplinary tools as well as staff support and expertise NRF encourages collaboration across all fields of research. As a shared facility NRF is also uniquely suited to serving as a location for interdisciplinary lab courses in micro/nano-fabrication and advanced characterization techniques. NRF has also proven to be a valuable resource to local start-up companies such as Pulse Therapuetics Inc. where NRF’s unique nanomaterial synthesis capabilities and expertise have been a key component to their success thus far. 7.14.2 Research Project Highlights Highlight 1: Sensing NRF has cultivated an open and shared research environment to provide expertise in imaging, elemental analysis and device fabrication. Multiple user groups at Washington University have utilized NRF in the development of unique sensors with applications from pollutant detection to medicine to homeland security. i) Stuart Solin’s group from Physics is developing GaAs based van der Pauw devices that may be used for cell identification by exploiting geometrical-driven conductance shifts that can be used to map Figure 179: SEM image of the charge distribution on van der Pauw a surface. ii) In Electrical System aluminum nanowire optical filters deposited directly on top of the CCD Engineering Lan Yang’s group was studying chemical and biosensing imaging sensor applications of whispering gallery mode optical resonators with a goal to accurately detect and determine the size of single particles. iii) Srikanth Singamaneni’s group in Mechanical Engineering and Materials Science was investigating self assembly of gold nanoparticles for biosensing. Self-assembly of gold nanoparticles using aminothiols generates plasmonic coupling between adjacent particles, greatly enhancing sensitivity. iv) Viktor Gruev’s group from Computer Science and Engineering has created polarization imaging sensors with aluminum nanowires that can capture linear polarization properties of the imaged environment in real-time and in high resolution (see Figure 179). Polarization sensors applications range from underwater imaging, to classification of chemical isomers, to

NNIN Annual Report p.212 March 2011-Dec 2011 non-contact fingerprint detection. v) Barani Raman’s group in Biomedical Engineering is developing microsensor arrays for chemical sensing using thin films of thiol-conjugated gold na. noparticles with a goal of being able to diagnose non-small cell lung cancer from the volatile organic compound compostion of a patient’s breath sample. Highlight 2: Environment To meet it’s commitment to nanotechnology and the environment NRF provides a high level of technical expertise and user support in the area of environmental studies. Making use of this expertise are Washington Unviersity groups studying air quality, mineral science, environmental transport, and water quality. i) Jay Turner’s group in Energy, Environmental and Chemical Engineering (EECE) is studying air quality near refinery facilties by Figure 180: Mechanistic illustration of Fe(II)-induced measuring the concentrations of rare earth elements that are present in recrystallization of Ni-substituted catalysts used in the cracking process of crude oil. ii) Jeffrey Catalano’s hematite. group at Earth and Planetary Science was studying Fe(II)-activated trace element cycling through crystalline iron oxides (see Figure 180). Such cycling affects micronutrient availability, contaminant transport, and the distribution of both redox sensitive and redox-inactive trace elements in natural and engineered systems. iii) Young–Shin Jun’s group in EECE is investigating the fate and transport of hematite and galena nanoparticles in simulated wastewater treatment systems. iv) The Robert Criss lab in Earth and Planetary Sciences was studying the hydrology and geochemistry of urban and rural watersheds in east-central Missouri. v) The Biswas and Giammar groups in Energy, Environmental and Chemical Engineering have examined the characteristics of combustion aerosols such as fly ash from coal. The detailed studies on understanding the structure of fly ash helps establish impacts on the environment and develop strategies to alleviate any deleterious impacts. Feedback is also provided to combustion scientists to design advanced coal combustion technologies that alter the characteristics of the fly ash so they are more re-usable, and have minimal deleterious impacts. Highlight 3: Medicine NRF is dedicated to facilitating nanotechnology reseach in the field of public health and to that end has focused on supporting the thriving regional medical community. i) Pulse Therapuetics Inc. is developing a technology to improve stroke outcomes by providing a minimally-invasive, compact, and safe magnetic technology to the emergency room which will mechanically amplify the effects of clot-busting drugs in the treatment of stroke. They have devoloped a magnet system for delivering magnetic nanoparticles synthesized by NRF to the site of the clot (see Figure 181). ii) Eric Figure 181: Prototype magnet system developed by Pulse Leuthardt’s group at the Consortium for Translational Research in Therapeutics, Inc. for use with Advanced Imaging and Nanomedicine at Washington University has magnetic nanoparticles in the treatment of stroke patients. utilized the NRF to fabricate an electroencephalography microgrid that can be attached to a standard brain retractor for monitoring of a patient’s brain state during surgery. iii) Mikhail Berezin’s group at Washington University School of Medicine is developing optically active near-infared contrast agents for early diagnostics and targeted therapies including gold fluorescent nanoparticles for image guided laser ablation of tumors and activatable fluorescence nanoparticles for imaging of reactive oxygen species and nitric oxide in acute lung injuries. iv) Kakkattukuzhy Isaac’s group at Missouri University of Science and Technology is developing a multifunctional microfluidics device without channels based on electrochemical

NNIN Annual Report p.213 March 2011-Dec 2011 magnetohydrodynamics for lab-on-a-chip applications. v) At Saint Louis University Alessandro Vindigni’s group utilizes microfluidics devices fabricated at NRF in their studies of DNA repair and genome stability, including the structure, function, and regulation of RecQ helicases. Highlight 4: Synthesis The NRF continues to provide unique services in the synthesis of nanoparticles via both top-down and bottom-up approaches. This expertise in nanoparticle synthesis and characterization provides a solid support base for users conducting research in the area of nanoparticle synthesis. i) Dean Campbell at Bradley University studied the synthesis of catalytic palladium colloids within silicone polymer matrices. These systems could combine the catalytic capabilities of the colloidal metal nanoparticles with the ability to recover the catalytic particles at the end of the reaction (see Figure 182). ii) The Epstein and Xu groups at Brandeis University are evaluating the fundamental effects of the localization of active species in non-equilibrium soft materials during chemomechanical conversion by utilizing heterogeneous micro-BZ gels generated using templates created via soft lithography techniques. iii) Daren Chen’s group at Washington University is developing methods to synthesize TiO2 and SiO2 nano-agglomerates using a diffusion Figure 182: Transmission burner. iv) Richard Axelbaum’s group at Washington University is studying electron micrograph of the synthesis of lithium-manganese-nickel-oxide nanoparticles generated palladium colloid. using spray pyrolysis for use as cathode materials in lithium ion batteries. v) Pratim Biswas’s group at Washington University is synthesizing titanium dioxide thin flims for applications in solar driven carbon dioxide reduction and water splitting. v) The Biswas group has been using the facility to characterize their novel, 1-D nanostructures for solar energy applications. A patented Aerosol Chemical Vapor Deposition technique is used to make these single crystal 1-D nanostructures that are very effective in light harvesting devices. The applications focus on solar PV systems; photoreduction of carbon dioxide and water splitting applications. vi) The Biswas group also uses flame aerosol reactors (FLAR) and furnace aerosol reactors (FUAR) in the synthesis of nanomaterials. A key application has been the collaborative work with toxicologists to establish the effects as a function of particle size, crystallinity and other characteristics. 7.13.3 Equipment and Operation In 2011, NRF installed the following tool:

• Cary 50 UV-Vis Spectrometer provides the capability to monitor the progress of nanoparticle synthesis reactions by examination of localized surface plasmon resonance peaks. (Supported by the NSF-NNIN 2011) In 2011, NRF has developed the following new capabilities:

• Superparamagnetic Nanomaterials: NRF has demonstrated the capabilities to produce monodispersed superparamagnetic magnetite nanoparticles with an ability to maneuver the size from 100 nm to 800 nm (see Figure 183).

• Gold Nanoplates: NRF has demonstrated the capability to produce and Figure 183: TEM and SEM images of superparamagnetic magnetite nanoparticles.

NNIN Annual Report p.214 March 2011-Dec 2011 purify gold nanoplates of triangular or hexagonal configuration with edge length control from 50nm to 1µm (see Figure 184).

Figure 184: TEM images of gold nanoplates with 400nm edge length before (left) and after (center) purification and gold nanoplates with edge length of 200nm (right). • Unconventional Concentration Measurement: NRF is developing routine procedures for measurement of the concentration of silver nanoparticles in aqueous suspensions by UV-Vis Spectrometery. Utilizing the Beer-Lambert law the concentration of silver nanocubes in a solution can be estimated with a quick 1 minute measurement. For applications not requiring exact concentration analysis this is provides considerable time and resource savings over atomic spectrometery techniques which can take hours to complete (see Figure 185).

Figure 185: Biomass growth of Arabidopsis seedlings in the presence and absence of silver nanoparticles left). Silver uptake by mature Arabidopsis plants (right).

• Toxicity Evaluation: NRF has continued work towards establishing our own toxicity core. Specifically, we are developing procedures for screening plant growth inhibition in the presence of nanoparticles using a model plant (Arabidopsis) system. In a typical process, Arabidopsis seeds are grown in the presence of silver nanocubes in water or a nutrient solution. Differences in biomass growth between controls and plants grown with nanocubes could reflect inhibition effects

Figure 186: Silver nanocubes (left) and their absorbance in solution at different silver concentrations (center). A linear relationship between silver nanocube concentration and absorbance has been demonstrated (right).

of the silver nanoparticles. The uptake of nanoparticles by plants has been examined by transmission electron microscopy and inductively-coupled plasma mass spectrometry.

NNIN Annual Report p.215 March 2011-Dec 2011 Preliminary results indicate that the presence of silver nanoparticles has an inhibiting effect on early stages of plant biomass growth and that mature plants uptake a high percentage of nanoparticles available in solution (see Figure 138). In order to better standardize procedures we are exploring collaboration opportunites with Missouri Botanical Gardens. 7.14.4 Staff The director of NRF, Dr. Dong Qin, left her position this year to begin her appointment as Associate Professor of Materials Scinece and Engineering at Georgia Tech. Pratim Biswas, PhD., and chair of the department of Energy, Environmental, and Chemical Engineering replaced Dr. Qin as Director of NRF. Dr. Yujie Xiong also left his position as NRF Lab Manager to become Professor of Chemistry at the University of Science and Technology of China. He was replaced in June 2011 by Kate Nelson who originally joined NRF in March 2010 to provide support in environmental engineering applications and analytical chemistry techniques. Research engineer Brent Riggs left NRF to pursue a career with Samsung and was replaced in April 2011 by Nathan Reed. Mr Reed, who has a bachelor degree in Integrative Biology and previous work experience with thin films at Deposition Research Laboratory, Inc., joined the NRF technical team to provide expertise in cleanroom applications. Research engineer Kristy Wendt left NRF to pursue opportunities at the Washington University in St. Louis School of Medicine and was replaced in September 2011 by Howard Wynder, who has over 20 years of experience in biological imaging applications including fluorescense microscopy, electron micrsocopy, and ultramicrotomy. Jinho Park, with an M.S. in Chemical Engineering from Washington University in St. Louis, joined the NRF technical team in September 2011 to provide expertise in nanoparticle synthesis. 7.14.5 Education and Other Activities NRF has been an active participant in NNIN educational events including the NNIN Showcase for Students at the Society for Hispanic Professional Engineers and the USA Science and Engineering Festival at Washington DC, as well as local educational events such as Nanodays at the St. Louis Science Center. NRF routinely provides lab tours and demonstrations for undergraduate and graduate classes at Washignton University as well as local high school classes. We provided additioanl assistance to the Washington University undergraduate biology course, “Phage Hunters”. The Phage Hunters class is a laboratory research based biology course focused on isolating and characterizing bacterial phages in local soils. NRF provided live demonstrations of transmission electron microscopy for each student’s phage samples. The collected images were used by the student’s to classify the phages using measured head and tail size and morphology. NRF continues to host six undergraduate students for summer research through the NNIN-REU program. NRF also hosted three additional undergraduate students for summer research (supported by NSF-NUE). These students receive valuable experience by working side-by-side with graduate students and post- docs in Washington University in St. Louis labs engaged in nanotechnology research. As part of NRF’s SEI initiative these students receive additional nanotechnology safety and ethics training as well as research communication guidance from NRF staff. NRF hosted one high school science teacher for a summer research project as part of a Research Experience for Teachers program (supported by NSF-NUE). The teacher worked alongside NRF staff to develop protocols for evaluating the inhibition of plant growth in the presence of nanoparticles. NRF hosted two high school interns for summer research (supported by NSF-NNIN 2011). The interns

NNIN Annual Report p.216 March 2011-Dec 2011 worked side-by-side with NRF staff on toxicity evaluation and unconvential concentration measurement projects to gain research experience. ---End of Washington University at St. Louis Text Site Report--

NNIN Annual Report p.217 March 2011-Dec 2011 7.14.6 Washington University at St. Louis Selected Site Statistics a)

Washington University Historical Users 160

10 months 140

12 months 12 months 120

100 foreign

state and fed gov Users 80 large company Joined NNIN in FY09 small company 60 pre-college

2 year college 40 4 year college

other university 20 local site academic

0 FY04 FY04 FY05 FY05 FY06 FY06 FY07 FY07 FY08 FY08 FY09 FY09 FY10 FY10 FY11 FY11 Local Other Local Other Local Other Local other Local other Local other Local Other Local Other

b)Lab Hours by Institution Type cUser Distribution by Institution Type

Washington University User Hours (10 months FY11) WUSTL Users by Type- March 2011-Dec 2011 10 Months

Small Company 5% Large Company Small Company 2% 4 year college 4% 4 year college Large Company State and Fed 1% 0% 1% Gov foreign Other University 0% 0% 4% Foreign 0% Other University 3%

Local Site Academic 89%

Local Site 4662 Hours-10 months Academic 90%

146 users - 10 months

d) Average Hours per User( in 10 months) e) New Users

80 70 Washington University Hours per User ---10 months FY11 Washington University New Users--10 months--FY11 70 60

60 50

50 70 New Users in 10 Months 40 40 30

30 New Users

Hours per user per Hours 20 20

10 10

0 0

Figure 187: Washington University Selected Site Statistics

NNIN Annual Report p.218 March 2011-Dec 2011 7.14.7 Washington University at St. Louis User Institutions Academic Small Company Large Company Brandeis University AIST-NT Inc. Boeing University of Missouri VSG Inc UTC Power Missouri University of Pulse Therapeutics, Inc. Dynalabs Science & Technology Saint Louis University Covidien/Mallinckrodt

State and Federal International Pacific Northwest National Research Council National Laboratory Canada

NNIN Annual Report p.219 March 2011-Dec 2011 Appendix 1: NNIN Network and Site Directors and Coordinators Prof. Roger T. Howe, Stanford University, Network Director and Co-PI [email protected] Dan Ralph, Professor, Department of Physics, Principal Investigator [email protected] Dr. Lynn Rathbun, Cornell University, Deputy Director [email protected] Dr. Nancy Healy, Georgia Tech NNIN Education Coordinator [email protected] Dr. Michael Stopa, Harvard University, NNIN Scientific Computation Coordinator [email protected] Prof. Katherine McComas, Dept. of Communications; NNIN SEI Coordinator [email protected]

Arizona State University Site Trevor Thornton, Professor, Department of Electrical Engineering, (Site Director) [email protected]

Cornell University Site Dan Ralph, Professor, Department of Physics, (Site Director) [email protected]

Georgia Institute of Technology James Meindl, Professor, School of Electrical and Computer Engineering (Site Director) [email protected]

Harvard University Roy Gordon, Professor of Chemistry(Site Director) [email protected]

Howard University Gary Harris, Professor, Department of Electrical and Computer Engineering (Site Director) [email protected]

Pennsylvania State University Theresa Mayer,Professor, (Site Director) [email protected]

Stanford University Roger Howe, Professor, Department of Electrical Engineering (Site Director) [email protected]

University of California, Santa Barbara Mark Rodwell, Professor, Department of Electrical and Computer Engineering (Site Director) [email protected]

University of Colorado Bart van Zeghbroeck, Professor, Department of Electrical Engineering (Site Director) [email protected]

University of Michigan Khalil Najafi, Professor, Department of EE and CS (Site Director)

NNIN Annual Report p.220 March 2011-Dec 2011 [email protected]

University of Minnesota Steve Campbell, Professor, Department of Electrical Engineering (Site Director) [email protected]

University of Texas, Austin Sanjay Banerjee, Professor, Department of Electrical and Computer Engineering (Site Director) [email protected]

University of Washington Francois Baneyx, Professor, Department of Chemical Engineering (Site Director) [email protected]

Washington University in St. Louis Pratim Biswas , Professor, Environmental and Chemical Engineering [email protected]

Appendix 2: NNIN Highlights 2011

Appendix 3: NNIN Publications (following)

End of NNIN Annual Report

NNIN Annual Report p.221 March 2011-Dec 2011