In-situ SAXS and XRD of SBA-15 in a Diamond Anvil Cell during high-pressure densification

Description

This dataset contains 1D Small Angle X-ray Scattering (SAXS) and 1D X-Ray Diffraction (XRD) patterns for a mixture of gold particles and SBA-15. SBA-15 is a type of periodic mesoporous amorphous silica. The SAXS data has ordered reflection peaks from the SBA-15 mesopore lattice. The XRD data has the First Sharp Diffraction Peak (FSDP) from the SBA-15 and diffraction peaks from the gold particles, particularly the gold [111] reflection which was used to calibrate pressure. The data was measured in-situ in a Diamond Anvil Cell (DAC) during compression, under pressures ranging from ~0-5 GPa. Hydrostatic data was measured when the sample cell was filled with a Pressure Transmitting Medium (PTM) of 4 methanol : 1 ethanol. Uniaxial (i.e., non-hydrostatic) data was measured when the sample cell was filled with only ambient air as the PTM. The SAXS dataset shows the SBA-15 P6mm mesoporous lattice shrinking and becoming increasing disordered during compression. The XRD dataset shows the shift in the FSDP during compression (as well as the shift in the gold [111] reflection). Data is first categorized by which experiment it was a part of; SAXS and XRD data were collected simultaneously so all the hydrostatic data represents a single experiment and all the uniaxial data represents a different single experiment. Data is next categorized by whether it is SAXS or XRD data. Lastly, data is categorized by what pressure it was taken at; XRD/SAXS data labeled with the same pressure was taken at the same DAC pressure setting. README txt files explain the dataset file formats and where the data was collected. This work was supported by the UC Lab Fees Fellowship from University of California Research Initiatives (Contract No. LGF-20-652903); and by the U.S. Department of Energy through the Los Alamos National Laboratory. Los Alamos National Laboratory is operated by Triad National Security, LLC, for the National Nuclear Security Administration of U.S. Department of Energy (Contract No. 89233218CNA000001). Portions of this work were performed at HPCAT (Sector 16), Advanced Photon Source (APS), Argonne National Laboratory. HPCAT operations are supported by DOE-NNSA’s Office of Experimental Sciences. The Advanced Photon Source is a U.S. Department of Energy (DOE) Office of Science User Facility operated for the DOE Office of Science by Argonne National Laboratory under Contract No. DE-AC02-06CH11357.

Steps to reproduce

SBA-15 was purchased from ACS Materials. Pressures were created using a Diamond Anvil Cell (DAC). The hydrostatic measurements used a pressure-transmitting medium (PTM) of 4:1 methanol ethanol and the uniaxial (i.e., non-hydrostatic) measurements used ambient air. Gold particles were put in the sample chamber along with SBA-15 in order to measure the pressure (pressure was measured by calculating the gold FCC lattice size from the XRD data and comparing to the gold equaiton of state). SAXS and XRD datasets were measured at Argonne National Laboratory’s Advanced Photon Source (APS) on HP-CAT (beamline 16-ID-D). XRD data was collected on a Pilatus 100K detector located ~170 mm from the sample with azimuthal coverage of ~40 – 120°. SAXS data was collected on a MAR345 detector located ~3050 mm from the sample. The SAXS background was measured by passing the X-ray beam through a fully assembled DAC without any sample powder or PTM inside the sample chamber.

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