POLYMERS 1999 PROGRAMS AND ACCOMPLISHMENTS MATERIALS SCIENCE AND ENGINEERING LABORATORY NISTIR 6435 UNITED STATES DEPARTMENT OF COMMERCE TECHNOLOGY ADMINISTRATION NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY UNITED STATES DEPARTMENT OF COMMERCE MATERIALS William M. Daley, Secretary TECHNOLOGY SCIENCE AND ADMINISTRATION Dr. Cheryl L. Shavers, Under Secretary of Commerce for Technology ENGINEERING NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY Raymond G. Kammer, LABORATORY Director T OF C EN OM M M T E R R A C P E E D POLYMERS U N A I C T I E R D E M ST A ATES OF 1999 PROGRAMS AND ACCOMPLISHMENTS Eric J. Amis, Chief Bruno M. Fanconi, Deputy NISTIR 6435 January 2000 TABLE OF CONTENTS EXECUTIVE SUMMARY .............................................................................................................1 Recognizing Leadership in Measurement Science....................................................................3 Recognizing Leadership in Standards Development ...........................................................4 TECHNICAL ACTIVITIES ELECTRONIC PACKAGING, INTERCONNECTION AND ASSEMBLY PROGRAM Overview..............................................................................................................................5 Significant Accomplishments ..............................................................................................6 Characterization of Low-k Dielectric Porous Silica Thin Films .........................................7 Dielectric Properties of Thin Polymer Films and Composites ..........................................10 Optical Polarization Dependent Performance of Photonic Devices ..................................12 Hygrothermal Expansion of Thin Films ............................................................................14 Thermal Properties of Polymer Films and Interfaces ........................................................17 Functionalized Silsesquioxane Cubes as Potential Underfill Encapsulants ......................18 Polymer Electrostriction....................................................................................................21 Electrical and Thermal Properties of Thin Polymer Films ................................................22 Thin-Film Residual Stress Measurement: Application in Determination of In- plane CTE and In-plane Modulus ..........................................................................23 Assembly of IC Chips Utilizing Wafer-level Underfill.....................................................24 Spectroscopic Studies of Polymer Surfaces and Interfaces ...............................................26 Neutron Scattering and the Low Energy Excitations in Polycarbonate Copolymers ........27 Fundamentals of Polymers at Surfaces and Interfaces ......................................................29 Highlight ............................................................................................................................35 POLYMER BLENDS AND PROCESSING PROGRAM Overview............................................................................................................................37 Significant Accomplishments ............................................................................................38 In-Line Optical Characterization of Polymer Extrusion and Blend Morphology..............40 Phase Behavior in Polymer Blends and Polymer Crystallinity .........................................42 Mixing and Structure Formation Under Shear Flow.........................................................46 Fluorescence, Dielectrics and Ultrasonics Monitoring for Polymer Processing ...............50 Theory of Phase Separation and Transport in Polymer Liquid..........................................52 Heterogeneous Dynamics of Polymers and Filled Polymers: Theory and Simulation..............................................................................................................55 Measurements of Polymer-Filler Interactions in Filled Polymers.....................................58 Probing Local Dynamics, Structure and Ordering in Filled Polymers and Nanocomposites....................................................................................................60 Combinatorial Measurements of Polymeric Coatings .......................................................62 Dendrimers with Polymers, Metals, and Small Molecules................................................63 Highlights...........................................................................................................................69 iii POLYMER COMPOSITES PROGRAM Overview............................................................................................................................73 Significant Accomplishments ............................................................................................73 Hybrid Reinforced Polymer Composites ...........................................................................74 Microstructure Studies: Non-destructive Characterization by Optical Coherence Tomography.........................................................................................77 Microstructure Studies: Measurement of Interface Strength after High Speed Processing of Fast Reacting Resins............................................................80 Processing: Fiber Optic Sensors for Process Monitoring ..................................................82 Liquid Composite Molding: Interface Sensitive Optical Fiber Sensor..............................84 Microstructure Studies: Improve the Utility of the Single Fiber Fragmentation Test ...............................................................................................85 Liquid Composite Molding: Lattice Boltzmann Techniques for Process Modeling...................................................................................................88 Processing: Permeability Measurements and Database.....................................................91 Highlights...........................................................................................................................93 POLYMER CHARACTERIZATION Overview............................................................................................................................95 Significant Accomplishments ............................................................................................96 Standard Reference Materials ............................................................................................96 Mass Spectrometry of Polymers ........................................................................................97 Characterization of Polymer Morphology by Microscopy Techniques...........................100 Characterization of Polymers by Spectroscopic Techniques...........................................103 Development of Standard Reference Materials: Non-Newtonian Fluids for Rheological Measurements..................................................................................107 Structural Recovery, Physical Aging and Nonlinear Viscoelasticity of Polymer Glasses .................................................................................................................110 Structural Characterization of Polymers by Small Angle X-Ray Scattering...................111 Hygrothermal Aging Studies of a Commercial Structural Adhesive...............................114 Highlight ..........................................................................................................................117 DENTAL AND MEDICAL MATERIALS PROGRAM Overview..........................................................................................................................119 Significant Accomplishments ..........................................................................................120 Dental Resins Based on Fluorinated Monomers and Oligomers .....................................120 Dental Composites with Improved Interfaces..................................................................124 Improved Adhesive Systems for Bonding to Tooth Structure.........................................128 Bioactive Polymeric Dental Materials with Remineralization Potential based on Amorphous Calcium Phosphate.......................................................................................130 Cure Monitoring of Dental and Medical Resins by Fluorescence Spectroscopy............132 Support for the Biomaterials Integrated Products Industries (BIPI's) .............................134 Highlights.........................................................................................................................139 iv DIVISION MANAGEMENT......................................................................................................141 RESEARCH STAFF....................................................................................................................143 APPENDIX NIST Organization Chart............................................................................................................157 MSEL Organization Chart...........................................................................................................159 Polymers Division Organization Chart........................................................................................161 Certain commercial materials and equipment are identified in this report in order to specify adequately the experimental procedures. In no case does such identification imply recommendation or endorsement