NIST: National Institute of Standards and Technology 20 articles published in JoVE Chemistry A Synthetic Methodology for Preparing Impregnated and Grafted Amine-Based Silica Composites for Carbon Capture Charlotte M. Wentz1,2, Zois Tsinas1,3, Amanda L. Forster1 1Material Measurement Laboratory, National Institute of Standards and Technology (NIST), 2University of Maryland, 3Theiss Research This work aims to facilitate the development of standardized techniques for impregnating or grafting aminated compounds onto silica substrates, which are often broadly described in the literature. Specific amounts of solvent, substrate, amines, and the values of other important experimental parameters will be discussed in detail. Engineering Measuring the Time-Evolution of Nanoscale Materials with Stopped-Flow and Small-Angle Neutron Scattering Elizabeth G. Kelley1, Michael H. L. Nguyen2, Drew Marquardt2,3, Brian B. Maranville1, Ryan P. Murphy1 1NIST Center for Neutron Research, National Institute of Standards and Technology, 2Department of Chemistry and Biochemistry, University of Windsor, 3Department of Physics, University of Windsor This protocol presents the use of a stopped-flow sample environment to quickly mix multiple liquid solutions in situ during a small-angle neutron scattering measurement and to study kinetic processes on nanometer length scales and second time scales. Chemistry Comparison of Two Different Synthesis Methods of Single Crystals of Superconducting Uranium Ditelluride Sheng Ran1,2,3, I-Lin Liu1,2, Shanta R. Saha1,2, Prathum Saraf1, Johnpierre Paglione1,2, Nicholas P. Butch1,2 1Maryland Quantum Materials Center, Department of Physics, University of Maryland, 2National Institute of Standards and Technology, 3Department of Physics, Washington University in St. Louis Here, we present a protocol to synthesize two types of UTe2 crystals: those exhibiting robust superconductivity, via chemical vapor transport synthesis, and those lacking superconductivity, via molten metal flux synthesis. Engineering Solution Blow Spinning of Polymeric Nano-Composite Fibers for Personal Protective Equipment Zois Tsinas1,2, Ran Tao1,3, Amanda L. Forster1 1Material Measurement Laboratory, National Institute of Standards and Technology, 2Theiss Research, 3Department of Chemical Engineering, Texas Tech University The primary goal of this study is to describe a protocol to prepare polymeric fiber mats with consistent morphology via solution blow spinning (SBS). We aim to use SBS to develop novel, tunable, flexible polymeric fiber nanocomposites for various applications, including protective materials, by incorporating nanoparticles in a polymer-elastomer matrix. Engineering Calibration Procedures for Orthogonal Superposition Rheology Ran Tao1,2, Aaron M. Forster1 1Material Measurement Laboratory, National Institute of Standards and Technology, 2Department of Chemical Engineering, Texas Tech University We present a detailed calibration protocol for a commercial orthogonal superposition rheology technique using Newtonian fluids including end-effect correction factor determination methods and recommendations for best practices to reduce experimental error. Engineering Method Development for Contactless Resonant Cavity Dielectric Spectroscopic Studies of Cellulosic Paper Mary Kombolias1, Jan Obrzut2, Michael T. Postek3,4, Dianne L. Poster2, Yaw S. Obeng3 1Testing and Technical Services, Plant Operations, United States Government Publishing Office, 2Materials Measurement Laboratory, National Institute of Standards and Technology, 3Nanoscale Device Characterization Division, Physical Measurement Laboratory, National Institute of Standards and Technology, 4College of Pharmacy, University of South Florida A protocol for the non-destructive analysis of the fiber content and relative age of paper. Chemistry High Resolution Physical Characterization of Single Metallic Nanoparticles Jessica Ettedgui1,2, Jacob Forstater1,2, Joseph W. Robertson1, John J. Kasianowicz1,3 1Physical Measurement Laboratory, National Institute of Standards and Technology, 2Department of Chemical Engineering, Columbia University, 3Department of Applied Physics and Applied Math, Columbia University Here, we present a protocol to detect discrete metal oxygen clusters, polyoxometalates (POMs), at the single molecule limit using a biological nanopore-based electronic platform. The method provides a complementary approach to traditional analytical chemistry tools used in the study of these molecules. Engineering Cutting Procedures, Tensile Testing, and Ageing of Flexible Unidirectional Composite Laminates Amy Engelbrecht-Wiggans1,2, Ajay Krishnamurthy1,2, Faraz Burni1,3, William Osborn1, Amanda L. Forster1 1Material Measurement Laboratory, National Institute of Standards and Technology, 2Theiss Research, 3Chemical and Biomolecular Engineering Department, University of Maryland The goal of the study was to develop protocols to prepare consistent specimens for accurate mechanical testing of high-strength aramid or ultra-high-molar-mass polyethylene-based flexible unidirectional composite laminate materials and to describe protocols for performing artificial ageing on these materials. Chemistry Fabrication and Testing of Photonic Thermometers Nikolai N. Klimov1,2, Zeeshan Ahmed2 1Joint Quantum Institute, University of Maryland, 2Physical Measurement Laboratory, National Institute of Standards and Technology We describe the process of fabrication and testing of photonic thermometers. Chemistry Disentangling High Strength Copolymer Aramid Fibers to Enable the Determination of Their Mechanical Properties Amanda L. Forster1, Viviana Rodriguez Cardenas1, Ajay Krishnamurthy1,2, Zois Tsinas3, Amy Engelbrecht-Wiggans1,2, Nolan Gonzalez1 1Material Measurement Laboratory, National Institute of Standards and Technology, 2Theiss Research, 3University of Maryland The primary goal of the study is to develop a protocol to prepare consistent specimens for accurate mechanical testing of high strength copolymer aramid fibers, by removing a coating and disentangling the individual fiber strands without introducing significant chemical or physical degradation. Engineering Standardized Method for Measuring Collection Efficiency from Wipe-sampling of Trace Explosives Jennifer R. Verkouteren1, Jeffrey A. Lawrence1, Matthew E. Staymates1, Edward Sisco1 1Materials Measurement Science Division, National Institute of Standards and Technology Optimized sampling protocols and the development of new wipe materials can be facilitated by standardized measurements of collection efficiency from wipe-sampling. Our approach for sampling trace explosives uses an automated device to control speed, force, and distance during wipe-sampling followed by extraction of collected explosives. Engineering Dielectric RheoSANS — Simultaneous Interrogation of Impedance, Rheology and Small Angle Neutron Scattering of Complex Fluids Jeffrey J. Richards1, Cedric V. L. Gagnon2, Jeffery R. Krzywon1, Norman J. Wagner3, Paul D. Butler1 1NIST Center for Neutron Research, National Institute of Standards and Technology, 2Department of Materials Science and Engineering, University of Maryland, 3Center for Neutron Science, Department of Chemical and Biomolecular Engineering, University of Delaware Here, we present a procedure for the measurement of simultaneous impedance, rheology and neutron scattering from soft matter materials under shear flow. Engineering Optical Trap Loading of Dielectric Microparticles In Air Haesung Park1, Thomas W. LeBrun1 1Physical Measurement Laboratory, National Institute of Standards and Technology A protocol for launching and stably trapping selected dielectric microparticles in air is presented. Bioengineering Rapid Scan Electron Paramagnetic Resonance Opens New Avenues for Imaging Physiologically Important Parameters In Vivo Joshua R. Biller1,2, Deborah G. Mitchell1, Mark Tseytlin3,4, Hanan Elajaili1, George A. Rinard5, Richard W. Quine6, Sandra S. Eaton1, Gareth R. Eaton1 1Department of Chemistry and Biochemistry, University of Denver, 2Magnetic Imaging Group, Applied Physics Division, Physical Measurements Laboratory, National Institute of Standards and Technology, 3Department of Radiology, Geisel School of Medicine, Dartmouth University, 4Department of Biochemistry, West Virginia University, 5Department of Electrical and Computer Engineering, University of Denver, 6Department of Engineering, University of Denver A new electron paramagnetic resonance (EPR) method, rapid scan EPR (RS-EPR), is demonstrated for 2D spectral spatial imaging which is superior to the traditional continuous wave (CW) technique and opens new venues for in vivo imaging. Results are demonstrated at 250 MHz, but the technique is applicable at any frequency. Engineering How to Build a Vacuum Spring-transport Package for Spinning Rotor Gauges James A. Fedchak1, Julia Scherschligt1, Makfir Sefa1 1Sensor Science Division, Thermodynamic Metrology Group, National Institute of Science and Technology Here we describe how to build a robust spring-transport mechanism for a spinning rotor gauge. This device securely immobilizes the rotor and keeps it under vacuum during transportation. We also describe packaging that minimizes the risk of damage during transport. Tests show our design works for typical shocks during transport. Engineering Advanced Experimental Methods for Low-temperature Magnetotransport Measurement of Novel Materials Joseph A. Hagmann1, Son T. Le1, Curt A. Richter1, David G. Seiler1 1Engineering Physics Division, National Institute of Standards and Technology We describe the methodology of mechanical exfoliation and deposition of flakes of novel materials with micron-sized dimensions onto substrate, fabrication of experimental device structures for transport experimentation, and the magnetotransport measurement in a dry helium close-cycle cryostat at temperatures down to 0.300 K and magnetic fields up to 12 T. Engineering Atomically Traceable Nanostructure Fabrication Josh B. Ballard1, Don D. Dick2, Stephen J. McDonnell3, Maia Bischof4, Joseph Fu5, James H. G. Owen1, William R. Owen1, Justin D. Alexander1, David L. Jaeger4, Pradeep Namboodiri5, Ehud Fuchs1, Yves J. Chabal3, Robert M. Wallace3, Richard Reidy4, Richard M. Silver5, John N. Randall1, James Von Ehr1 1Zyvex Labs, 2Department of Physics, University of Texas at Dallas, 3Department of Materials Science and Engineering, University of Texas at Dallas, 4Materials Science and Engineering, University of North Texas, 5National Institute of Standards and Technology We report a protocol for combining the atomic metrology of the Scanning Tunneling Microscope for surface patterning with selective Atomic Layer Deposition and Reactive Ion Etching. Using a robust process involving numerous atmospheric exposures and transport, 3D nanostructures with atomic metrology are fabricated. Engineering Measuring Material Microstructure Under Flow Using 1-2 Plane Flow-Small Angle Neutron Scattering A. Kate Gurnon1, P. Douglas Godfrin1, Norman J. Wagner1, Aaron P. R. Eberle1,2, Paul Butler2, Lionel Porcar1,3 1Center for Neutron Science, Department of Chemical and Biomolecular Engineering, University of Delaware, 2NIST Center for Neutron Research, National Institute of Standards and Technology, 3Institut Laue-Langevin A shear cell is developed for small-angle neutron scattering measurements in the velocity-velocity gradient plane of shear and is used to characterize complex fluids. Spatially resolved measurements in the velocity gradient direction are possible for studying shear-banding materials. Applications include investigations of colloidal dispersions, polymer solutions, and self-assembled structures. Engineering Fabrication of Uniform Nanoscale Cavities via Silicon Direct Wafer Bonding Stephen R. D. Thomson1, Justin K. Perron2,3, Mark O. Kimball4, Sarabjit Mehta5, Francis M. Gasparini1 1Department of Physics, The State University of New York at Buffalo, 2Joint Quantum Institute, University of Maryland, 3The National Institute of Standards and Technology, 4Cryogenics and Fluids Branch, NASA Goddard Space Flight Center, 5HRL Laboratories A method for permanently bonding two silicon wafers so as to realize a uniform enclosure is described. This includes wafer preparation, cleaning, RT bonding, and annealing processes. The resulting bonded wafers (cells) have uniformity of enclosure ~1%1,2. The resulting geometry allows for measurements of confined liquids and gasses. Engineering Analysis of Contact Interfaces for Single GaN Nanowire Devices Andrew M. Herrero1, Paul T. Blanchard1, Kris A. Bertness1 1Quantum Electronics and Photonics Division, National Institute of Standards and Technology A technique was developed that removes Ni/Au contact metal films from their substrate to allow for the examination and characterization of the contact/substrate and contact/NW interfaces of single GaN nanowire devices.
