High-Throughput Synchrotron X-Ray Experimentation for Combinatorial Phase Matching

Gregoire, J. M. et al. High-throughput synchrotron X-ray diffraction for combinatorial phase mapping. Journal of Synchrotron Radiation 21, 1262-1268, DOI: 10.1107/s1600577514016488 (2014).


Scientific Achievement

Development of new synchrotron X-ray diffraction and fluorescence methods for rapid characterization of material libraries.

Significance & impact

First demonstration of prototype facility capable of meeting the structural characterization requirements for high-throughput material genomic searchers.

 

 

 

  Reprinted with permission from Gregoire, J. M. et al. High-throughput synchrotron X-ray diffraction for combinatorial phase mapping. Journal of Synchrotron Radiation 21, 1262-1268, DOI: 10.1107/s1600577514016488 (2014).  Copyright (2015) International Union of Crystallography.

 

Reprinted with permission from Gregoire, J. M. et al. High-throughput synchrotron X-ray diffraction for combinatorial phase mapping. Journal of Synchrotron Radiation 21, 1262-1268, DOI: 10.1107/s1600577514016488 (2014).  Copyright (2015) International Union of Crystallography.

Top:  Photograph of the combined XRD/XRF experiment on a continuous-composition-spread thin-film library.
Bottom:  left:  Continuous compositional spread of a Bi-V-Fe oxide composition library;  middle:  177 powder patterns from the library that are shown with log-scale intensity;  right:  example of 15 measured compositions revealing the compositions where light absorber phases are formed.

Research Details

Complex technological requirements demand precisely tailored material functionalities, and materials scientists are driven to search for these new materials in compositionally complex and often non-equilibrium spaces containing three, four, or more elements.  The phase behavior of these high- order composition spaces is mostly unknown and unexplored.  High-throughput methods can offer strategies for efficiently searching complex and multi-dimensional material genomes for these much needed new materials and can also suggest a processing pathway for synthesizing them.  However, high-throughput structural characterization is still relatively under-developed for rapid material discovery.

  • High-quality XRD powder patterns of thin film Bi-V-Fe oxide samples were measured with throughput better than 18 s per sample.
  • The optimal configuration for mapping reciprocal space with a single detector image was designed through simulations of the scattering experiments, yielding the highest throughput characterization of these light absorber libraries.

 

Contact:  nslewis@caltech.edu