Advanced Materials Characterization

Summary

The Chemical Sciences Division supports the characterization of new, diverse, and technological critical materials. The constant evolution of material science and technology challenge existing methods of metrology and lead to an evolving development and application of improved analytical methods. Our measurement capabilities for chemical compositional characterization are applied to detect elemental signatures, quantify elemental mass, and map its physical distribution. Researchers from across NIST, industry, academia, government are assisted by the application of state-of-the-art techniques, often uniquely available in our Division. The breadth of application supports most program areas involving chemical science metrology.

Description

NIST Center for Neutron Research

Credit: NIST

This program seeks to continually enhance the analytical competence of MML and other major operating units at NIST. Furthermore, the program makes available technical capabilities that U.S. industry and government need in their quest to compete on a global scale through improving methods and abilities, assisting in the research and development of new products, subsequently bringing them safely into the marketplace.

Major Accomplishments

• Optimization and continuing technique development of prompt gamma activation analysis for hydrogen determination in hydrogen storage materials and combinatorial research methods.
• Neutron activation analysis of candidate carbon nanotube reference materials revealed very high levels of contamination from catalysts used to produce the materials resulting in rejection of the material as a RM.
• Quality control for ¹⁰B mass and thickness uniformity in a series of prototype neutron detectors being developed as new instruments for installation at the Spallation Neutron Source (SNS).
• Analytical support in the discovery of a new candidate material for coating the first wall of fusion reactor vessels.
• The nonporous material has a highly critical property of releasing helium during the high temperature anneal cycle rather than eroding away the wall and contaminating the fusion cycle.
• Support of a Ph.D. Thesis on the movement of lithium ions in power cycled lithium batteries. This effort has spawned a second Ph.D. thesis program and is attracting the attention of battery researchers.
• Developed a neutron imaging technique that improves area resolution by 2 or more orders of magnitude over existing imaging detectors. The proposal has attracted the attention of researchers at NIST, in academia, in industry, and in government laboratories.

Additional Technical Details

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We collaborate with other NIST divisions and external researchers to provide chemical compositional measurements in the development of reference materials or research samples of interest. Often, this has required the development of improved abilities for accurate analyses. In other situations entirely new analytical measurement systems are required to achieve the necessary metrological goals. In support of NIST Initiatives and the analytical needs of the nation we have successfully addressed materials problems representing diverse needs while increasing our analytical competence. Examples of recent focus areas include unique quality control support of industrial materials, support of academic research into lithium batteries, development of new instruments targeted to support NIST initiatives and America Competes, and reference materials.

Associated Publications

1. Jahrman, E. P., Weaver, J. L., Govind, N., Perestjuk, M., and Seidler, G. T., "Iron redox analysis of silicate-based minerals and glasses using synchrotron X-ray absorption and laboratory X-ray emission spectroscopy," 577, (2022).  

2. Wang, F., Blanc, L. E., Li, Q., Faraone, A., Ji, X., Chen-Mayer, H. H., Paul, R. L., Dura, J. A., Hu, E. Y., Xu, K., Nazar, L. F., and Wang, C. S., "Quantifying and Suppressing Proton Intercalation to Enable High-Voltage Zn-Ion Batteries," 11, (2021).  

3. Tian, M., Liu, C. F., Zheng, J. Q., Jia, X. X., Jahrman, E. P., Seidler, G. T., Long, D. H., Atif, M., Alsalhi, M., and Cao, G. Z., "Structural engineering of hydrated vanadium oxide cathode by K+ incorporation for high-capacity and long-cycling aqueous zinc ion batteries," 29, 9-16 (2020).  

4. Zangmeister, C. D., Radney, J. G., Vicenzi, E. P., and Weaver, J. L., "Filtration Efficiencies of Nanoscale Aerosol by Cloth Mask Materials Used to Slow the Spread of SARS-CoV-2," 14, 9188-9200 (2020).  

5. Bi, W. C., Huang, J. J., Wang, M. S., Jahrman, E. P., Seidler, G. T., Wang, J. C., Wu, Y. J., Gao, G. H., Wu, G. M., and Cao, G. Z., "V2O5-Conductive polymer nanocables with built-in local electric field derived from interfacial oxygen vacancies for high energy density supercapacitors," 7, 17966-17973 (2019).  

6. Bi, W. C., Wang, J. C., Jahrman, E. P., Seidler, G. T., Gao, G. H., Wu, G. M., and Cao, G. Z., "Interface Engineering V2O5 Nanofibers for High-Energy and Durable Supercapacitors," 15, (2019).  

7. Jahrman, E. P., Pellerin, L. A., Ditter, A. S., Bradshaw, L. R., Fister, T. T., Polzin, B. J., Trask, S. E., Dunlop, A. R., and Seidler, G. T., "Laboratory-Based X-ray Absorption Spectroscopy on a Working Pouch Cell Battery at Industrially-Relevant Charging Rates," 166, A2549-A2555 (2019).  

8. Jahrman, E. P., Holden, W. M., Ditter, A. S., Mortensen, D. R., Seidler, G. T., Fister, T. T., Kozimor, S. A., Piper, L. F. J., Rana, J., Hyatt, N. C., and Stennett, M. C., "An improved laboratory-based x-ray absorption fine structure and x-ray emission spectrometer for analytical applications in materials chemistry research," 90, (2019).  

9. Kalanyan, B., Beams, R., Katz, M. B., Davydov, A. V., Maslar, J. E., and Kanjolia, R. K., "MoS2 thin films from a ((NBu)-Bu-t)(2)(NMe2)(2)Mo and 1-propanethiol atomic layer deposition process," 37, (2019).  

10. Mundy, M. E., Ung, D., Lai, N. L., Jahrman, E. P., Seidler, G. T., and Cossairt, B. M., "Aminophosphines as Versatile Precursors for the Synthesis of Metal Phosphide Nanocrystals," 30, 5373-5379 (2018).  

11. Radney, J. G. and Zangmeister, C. D.,  "Comparing aerosol refractive indices retrieved from full distribution and size- and mass-selected measurements," 220, 52-66 (2018).  

12. Zangmeister, C. D. and Radney, J. G.,  "Absorption Spectroscopy of Black and Brown Carbon Aerosol," 1299, 275-297 (2018).  

13. Kalanyan, B., Kimes, W. A., Beams, R., Stranick, S. J., Garret, E., Kalish, I., Davydov, A. V., Kanjolia, R. K., and Maslar, J. E., "Rapid Wafer-Scale Growth of Polycrystalline 2H-MoS2 by Pulsed Metal-Organic Chemical Vapor Deposition," 29, 6279-6288 (2017).  

14. Zhao, J. J., Kalanyan, B., Barton, H. F., Sperling, B. A., and Parsons, G. N., "In Situ Time-Resolved Attenuated Total Reflectance Infrared Spectroscopy for Probing Metal-Organic Framework Thin Film Growth," 29, 8804-8810 (2017).  

15. Kalanyan, B., Lemaire, P. C., Atanasov, S. E., Ritz, M. J., and Parsons, G. N., "Using Hydrogen To Expand the Inherent Substrate Selectivity Window During Tungsten Atomic Layer Deposition," 28, 117-126 (2016).  

16. You, R., Radney, J. G., Zachariah, M. R., and Zangmeister, C. D., "Measured Wavelength-Dependent Absorption Enhancement of Internally Mixed Black Carbon with Absorbing and Nonabsorbing Materials," 50, 7982-7990 (2016).  

17. Knauf, R. R., Kalanyan, B., Parsons, G. N., and Dempsey, J. L., "Charge Recombination Dynamics in Sensitized SnO2/TiO2 Core/Shell Photoanodes," 119, 28353-28360 (2015).  

18. Kucera, J., Bennett, J. W., Oflaz, R., Paul, R. L., Fernandes, E. A. D., Kubesova, M., Bacchi, M. A., Stopic, A. J., Sturgeon, R. E., and Grinberg, P., "Elemental Characterization of Single-Wall Carbon Nanotube Certified Reference Material by Neutron and Prompt gamma Activation Analysis," 87, 3699-3705 (2015).  

19. Schulz, P., Schafer, T., Zangmeister, C. D., Effertz, C., Meyer, D., Mokros, D., van Zee, R. D., Mazzarello, R., and Wuttig, M., "A New Route to Low Resistance Contacts for Performance-Enhanced Organic Electronic Devices," 1, (2014).  

20. Arpin, K. A., Losego, M. D., Cloud, A. N., Ning, H. L., Mallek, J., Sergeant, N. P., Zhu, L. X., Yu, Z. F., Kalanyan, B., Parsons, G. N., Girolami, G. S., Abelson, J. R., Fan, S. H., and Braun, P. V., "Three-dimensional self-assembled photonic crystals with high temperature stability for thermal emission modification," 4, (2013).  

21. Hanson, K., Losego, M. D., Kalanyan, B., Ashford, D. L., Parsons, G. N., and Meyer, T. J., "Stabilization of [Ru(bpy)(2)(4,4 '-(PO3H2)bpy)](2+) on Mesoporous TiO2 with Atomic Layer Deposition of Al2O3," 25, 3-5 (2013).  

22. Kalanyan, B., Oldham, C. J., Sweet, W. J., and Parsons, G. N., "Highly Conductive and Flexible Nylon-6 Nonwoven Fiber Mats Formed using Tungsten Atomic Layer Deposition," 5, 5253-5259 (2013).  

23. Kalanyan, B., Losego, M. D., Oldham, C. J., and Parsons, G. N., "Low-Temperature Atomic Layer Deposition of Tungsten using Tungsten Hexafluoride and Highly-diluted Silane in Argon," 19, 161-166 (2013).  

24. Ma, X. F., Zachariah, M. R., and Zangmeister, C. D., "Reduction of Suspended Graphene Oxide Single Sheet Nanopaper: The Effect of Crumpling," 117, 3185-3191 (2013).  

25. Wang, H. W., Wesolowski, D. J., Proffen, T. E., Vlcek, L., Wang, W., Allard, L. F., Kolesnikov, A. I., Feygenson, M., Anovitz, L. M., and Paul, R. L., "Structure and Stability of SnO2 Nanocrystals and Surface-Bound Water Species," 135, 6885-6895 (2013).  

26. Couet, A., Motta, A. T., Comstock, R. J., and Paul, R. L., "Cold neutron prompt gamma activation analysis, a non-destructive technique for hydrogen level assessment in zirconium alloys," 425, 211-217 (2012).  

27. Ma, X. F., Zachariah, M. R., and Zangmeister, C. D., "Crumpled Nanopaper from Graphene Oxide," 12, 486-489 (2012).  

28. Paul, R. L. and Lindstrom, R. M., "Preparation and Certification of Hydrogen in Titanium Alloy Standard Reference Materials," 43A, 4888-4895 (2012).  

29. Zangmeister, C. D., Ma, X. F., and Zachariah, M. R., "Restructuring of Graphene Oxide Sheets into Monodisperse Nanospheres," 24, 2554-2557 (2012).  

30. Zeisler, R., Oflaz, R., Paul, R. L., and Fagan, J. A., "Use of neutron activation analysis for the characterization of single-wall carbon nanotube materials," 291, 561-567 (2012).  

31. Paul, R. L., "Measurement of hydrogen in advanced materials by cold neutron prompt gamma-ray activation analysis," 837, 223-229 (2006).