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Multiscale structure and dynamics in advanced technological materials

Summary

This project develops and applies metrologies and standards for characterizing microstructure and dynamics in advanced functional materials of technological importance, including heterogeneous or porous materials, over multiple length scales in situ and operando.

Description

USAXS animation

In operando ultra-small-angle X-ray scattering (USAXS), small-angle X-ay scattering (SAXS), and wide-angle X-ray scattering (WAXS) measurements of the precipitate evolution (from USAXS & SAXS) and simultaneous phase evolution (from WAXS) in an advanced nickel-based superalloy heated over 4 hours to 1100 °C.  All features can be quantitatively analyzed.

Click on image to see simultaneous time evolution of small-angle X-ray scattering (precipitate morphology) and X-ray diffraction (phase composition) as function of temperature and time.

New technologies increasingly harness materials phenomena that operate across many length-scales: e.g., in selective gas adsorption, additive manufacturing, new alloy designs, or advanced concretes. To overcome technology barriers, it is no longer sufficient just to characterize the materials. Rather, these multi-scale material processes must be measured and understood under operando conditions. .

The objective of this project is to develop metrologies and standards, provide rigorous structural, thermodynamic and kinetics data for operando multi-scale microstructure and dynamics measurement in advanced functional material systems, and support new and sustainable technologies not fully realized at the present time.

 

Major Accomplishments

Innovative in situ / operando X-ray & neutron scattering methods have elucidated a wide range of multi-scale processes in technological materials, with recent papers in CrystEngCommEnvironmental Science & Technology, Dental Materials, Langmuir, Cement & Concrete Research, Journal of Alloys & Compounds, Journal of Applied Crystallography, Acta Materialia, Nanoscale Advances, Nanomaterials, Fuel,...

Major results have been obtained relevant to Additive Manufacturing processes for metals & alloys – especially in regard to the unexpected appearance of undesired deleterious phases during post-build stress-relief heat treatments in nickel-based super alloys, and also in regard to benchmark measurements for validating modeling and simulation predictions.

Structural & microstructural changes in both natural and advanced manufactured gas sorbents have been correlated with selective gas adsorption & desorption processes relevant to carbon mitigation, enhanced oil & gas recovery, & catalysis.

Our partnership with the APS at Argonne National Laboratory has resulted in the development of a world-leading synchrotron X-ray based materials measurement facility, allowing fully quantitative characterization over the angstrom to micrometer-scale range within a few minutes.  Collaboration with both the APS and NCNR has produced enhanced experimental sample environments for both facilities.

A new NIST Standard Reference Material, SRM 3600, has been issued for the absolute intensity calibration of small-angle X-ray scattering intensity.

 

Created July 6, 2017, Updated March 26, 2025