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Signature Redacted Signature of Author Chemical and Biomedical Sensors Using Two Dimensional Materials by Mantian Xue B.S. Material Science and Engineering University of Illinois at Urbana-Champaign, 2017 Submitted to the Department of Electrical Engineering and Computer Science in partial fulfillment of the requirements for the degree of Master of Science in Electrical Engineering and Computer Science at the MASSACHUSETTS INSTITUTE OF TECHNOLOGY September 2019 ©Massachusetts Institute of Technology 2019. All rights reserved Signature redacted Signature of Author: Department of Electrical Engineering and Computer Science Signature redacted August 30, 2019 Certified by: ................... Tomis Palacios Professor of Electrical Engineering and Computer Science 1) Thesis Supervisor Certified by: ............................ Signatureredacted.... MASSACHUSETTS INSTITUTE / of rECHNOLOGY > Leslie A. Kolodziejski F;- Engineering and Computer Science OCTOC0301 0 32019 Professor of Electrical Chair, Department Committee on Graduate Students LIBRARIES" Two Dimensional Materials Based Sensors for Chemical and Biological Applications by Mantian Xue Submitted to the Department of Electrical Engineering and Computer Science on August 30, 2019, in Partial Fulfillment of the Requirements for the Degree of Masters of Science in Electrical Engineering and Computer Science Abstract We are at the onset of a revolution in chemical and medical sensors. Traditional sen- sors are bulky and difficult to use. Many researchers have started to build easy-to-use in-home healthcare monitoring system such as wearable sweat sensors. In order to make such system practical, sensors need to combine high sensitivity, high selectivity, fast re- sponse time and small signal drift. The sensors also need to cover a wide range of rec- ognizable chemicals and molecules. Two-dimensional materials are perfect candidate as next-generation sensing materials because of their unique electrical, optical, mechanical and chemical properties. In this thesis, the fabrication and device technology of state- of-the-art graphene-based chemical sensor was discussed. A new 2D materials patterning technology and various passivation approaches were also studied. By using these novel technologies, three types of sensing devices that aims to push the development of bet- ter healthcare monitoring system were developed. A graphene-based biosensor for ligand detection was made with high sensitivity and a wide span of detection range. Graphene sensor arrays coupled with various types of ion-selective membranes were also developed. High sensitivity, selectivity and reversibility were achieve for detection of ionized calcium, sodium and potassium in electrolyte. FinallyMoS 2 were explored to amplify the signal and achieve high sensitivity at low concentration as well as an easier measurement scheme. All three sensors will serve as building blocks for the realization of next-generation chem- ical and biomedical sensor systems. Thesis Supervisor: Tomas Palacios Title: Professor of Electrical Engineering 3 Contents 1 Introduction 11 1.1 Project Motivation ..... ....... 11 1.2 Introduction to Two Dimensional Materials ... .. 12 1.2.1 Introduction to Graphene .... 1 13 1.2.2 Introduction toMoS 2 ....... .. .. 16 1.3 Thesis Outline ........ ....... .. .. 19 2 Device Technology 21 2.1 Cleanness of film ..... ........ 21 2.2 Passivation ... ....... ...... 25 2.3 Conclusion . ............... 34 3 Graphene-based Biosensors 36 3.1 Electrolyte-gated graphene field-effect transistors 36 3.2 pH sensing .. ....... ..... 37 3.3 Ligand Detection with GPCR . .. 40 3.3.1 Device Structure . ..... 42 3.3.2 Sensor Response ... ... 43 3.4 Conclusion ............. 46 4 Graphene-based Ion Sensing 47 4.1 Theory of Ion Selective Membrane ... 47 4.2 Sensor Array Structure and Performance 50 4.3 Ca2+ ion sensor . .... ..... ... 53 4.4 Na+ ion sensor ....... ...... 56 4.5 K+ ion sensor .. ........ .... 58 4 4.6 Integration of multiple ion sensor ............ ........... 60 4.7 C onclusion ......................... ........... 62 5 MoS 2-based Sensors 64 5.1 Device Structure ........... ..................... 64 5.2 pH Sensing Mechanism ........ ..................... 65 5.3 Sensor Performance .... ........................... 68 5.4 C onclusion ......... ........................... 69 6 Conclusion and Future Work 70 Bibliography 72 Appendices 83 A Standard Photolithography Recipes 83 B Recipe for graphene-based pH sensor 85 C Recipe for graphene-based ligand sensor 87 D Recipe for graphene-based sensor array 90 E Recipe for back-gated MoS 2 device 93 5 List of Figures 1.1 The family of 2D materials. Figure adopted from [1] ............. 13 1.2 (a)The carbon atomic a and 7r orbitals in thesp 2 honeycomb lattice [14] (b) Electronic dispersion in the honeycomb lattice. Left: energy spectrum. Right: zoom in of the energy bands close to one of the Dirac points [13]. (c)Ambipolar electric field effect in single-layer graphene. The insets show its conical low-energy spectrum [2] ............ .......... 15 1.3 (A) Atomic structure for single layer transition metal dichalcogenides (TMDs) in the 2H, 1T, andIT' phases, (B) periodic table of elements involved lay- ered TMDs, (C) evolution of the band structure for 2H-MoS 2 with decreas- ing number of layers, and (D) the schematic representation of the band structure for 2H-MoS 2 . This TMD overview image is reproduced from M anzeli et al. [46] ................................ 17 2.1 Schematics for PMGI/SPR700 bilayer Patterning Process. Green film rep- resents PMGI and orange film represents SPR700 .............. 23 2.2 AFM Images of graphene films on SiO 2 substrate with different photoresist treatm ents ................ .................... 24 2.3 Effect of NMP Treatment with PMMA Processed Graphene film onSiO 2 substrate. (a) PMMA processed graphene, (b) PMMA processed graphene after NMP overnight,(c)microscrope image of patterned graphene film after NM P treatm ent ................................ 25 2.4 AFM images of ALD dielectric on (a)graphene and (b) MoS 2 . Figures adopted from [76] and [78] ........................... 26 2.5 AFM images of ALD A12 0 3 on (a)graphene and (b)MoS 2 surface with Al as the seeding layer ......................... ..... 28 6 2.6 (a)Hysteresis of electrolyte-gated graphene FETs without A1 2 0 3 passiva- tion (b)hysteresis of electrolyte-gated graphene FETs with A1 2 0 3 passivation 29 2.7 Effect of A1203 passivation on electrolyte-gated graphene FETs' I-V char- acteristic ...... ........ ........ ........ ....... 30 2.8 Sensor response and structure of device (a) SU-8 passivation and (b) with oxide passivation . ............ ............. ...... 32 2.9 I-V Characteristics of MoS 2 Back-gated Transistors.(a) Output charac- teristics without oxide, (b)output characteristics with oixde, (c) transfer characteristics without oxide, (d) transfer characterstics with oxide .... 33 2.10 Transfer characteristics of MoS 2 based transistors with different types of passivation. Figure adopted from Yu et al. [78]. ............... 34 3.1 (a)Device structure and measurement setup for electrolyte-gated graphene field-effect transistors. (b)Three most common models to describe electric double layers, figure taken from [36] ...................... 37 3.2 Change in Dirac point with respect to pH value ... ............ 39 3.3 Schematics of 2D lattice of GPCR/S-layer complex. Images taken from R ui Q ing, PhD ..... ............. ............ .... 41 3.4 AFM images to show surface morphology of S-layer and GPCR/S-layer complex on silicon substrate. Images taken from Rui Qing,PhD. ...... 41 3.5 (a)Mask file of the graphene-based ligand sensor with GPCR (b) Measure- ment setup and fluid chamber ......................... 42 3.6 I-V response and schematics upon exposure of CXCL12 ligands with (a) bare graphene, (b) S-layer and (c) GPCR/S-layer complex. Ids is normal- ized to its minimum value. Black stars represent ligand, green lines rep- resent S-layer, orange circles with black stars represent ligand bind with G PCR protein. ............ ............ ......... 44 3.7 Sensor response with respect to ligand concentration demonstrates good linear relation between C/S and C (R2 = 0.992). S is defined as relative change in Dirac point. ............................. 46 7 4.1 (a) Graphene Ca 2+ sensor diagram depicting measurement setup and equi- librium charge distribution. R- represents lipophilic anionic site. (b) schematic diagram showing the electrostatic potential as a function of dis- tance from graphene surface. The dash line indicates the potential distri- bution when zero Ca2+ concentration gradient is present between ISM and electrolyte. (c) idealized graphene Ca2+ sensor I-V characteristic response. 48 4.2 Mask desgin for graphene-based sensor array. Top-right is a zoom-in picture of the sensing area. Insert shows the mask of an individual graphene sensor. Bottom-right is a microscope image of a graphene sensor on the array chip after fabrication .. ........ ......... ........ ..... 51 4.3 (a) I-V characteristics of 244 working electrolyte-gated graphene transis- tors on one chip with Vd, = 300 mV.1uM NaCl solution was used as the electrolyte. (b)distribution of the Dirac points ................ 52 4.4 ((a) Shift if I-V characteristic of a calcium sensor under different concen- tration, (b)slope of the average Dirac point as a function of ionized calcium concentration, error bar indicates the standard deviation. The sample size is 196 and all measurements are taken at Vd, = 300 mV. .......... 54 4.5
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