Complementary sub-micron scanning x-ray Bragg diffraction and fluorescence mapping at 5-ID, NSLS-II

The increasing prevalence of hard X-ray micro- and nano-probes has allowed for versatile sample characterization for a variety of scientific applications. By scanning a probe and simultaneously acquiring different X-ray responses, maps can be constructed of elemental and structural information to investigate sample spatial correlations. Here, we describe recent advancements at the 5-ID, Submicron Resolution X-ray Spectroscopy (SRX) beamline at the National Synchrotron Light Source II (NSLS-II) to incorporate complementary Bragg diffraction with our established X-ray fluorescence mapping. These dual data streams allow for combined structural and elemental mapping of samples, which we utilize for investigating crystal growth in bulk glasses. The complementary diffraction signals provide another contrast mechanism for distinguishing chemically identical but structurally different regions (e.g., congruent crystallization). For crystals larger than the sub-micron beam of SRX, we expand data collection by rotating the crystals or scanning the incident X-ray energy to build 3D reciprocal space maps. These higher dimensional datasets then offer the ability to spatially map crystal lattice parameters and orientation with elemental distributions.