High Pressure Single Crystal Diffraction at PX^2

Abstract

In this report we describe detailed procedures for carrying out single crystal X-ray diffraction experiments with a diamond anvil cell (DAC) at the GSECARS 13-BM-C beamline at the Advanced Photon Source. The DAC program at 13-BM-C is part of the Partnership for Extreme Xtallography (PX^2) project. BX-90 type DACs with conical-type diamond anvils and backing plates are recommended for these experiments. The sample chamber should be loaded with noble gas to maintain a hydrostatic pressure environment. The sample is aligned to the rotation center of the diffraction goniometer. The MARCCD area detector is calibrated with a powder diffraction pattern from LaB 6 . The sample diffraction peaks are analyzed with the ATREX software program, and are then indexed with the RSV software program. RSV is used to refine the UB matrix of the single crystal, and with this information and the peak prediction function, more diffraction peaks can be located. Representative single crystal diffraction data from an omphacite (Ca 0.51 Na 0.48 )(Mg 0.44 Al 0.44 Fe 2+ 0.14 Fe 3+ 0.02 )Si 2 O 6 sample were collected. Analysis of the data gave a monoclinic lattice with P2/n space group at 0.35 GPa, and the lattice parameters were found to be: a = 9.496 ±0.006 Å, b = 8.761 ±0.004 Å, c = 5.248 ±0.001 Å, β = 105.06 ±0.03º, α = γ = 90º.

Thermoelastic Properties of Eclogitic Garnets and Omphacites: Implications for Deep Subduction of Oceanic Crust and Density Anomalies in the Upper Mantle

“…The chemical compositions of garnets were obtained as Prp 28 Alm 38 Grs 33 Sps 1 (low Fe) and Prp 14 Alm 62 Grs 19 Adr 3 Sps 2 (high Fe), while the compositions of two omphacites were Quad 57 Jd 42 Ae 1 (low Fe; Quad indicates Ca‐Mg‐Fe pyroxenes; Morimoto, ) and Quad 53 Jd 27 Ae 20 (high Fe; Table S1). Single‐crystal XRD experiments were carried out at experimental station 13‐BM‐C of the Advanced Photon Source, Argonne National Laboratory (Fei et al, ; Kantor et al, ; Rivers et al, ; Zhang et al, ) (supporting information Text S2). The GSE_ADA/RSV software (Dera et al, ) was used to analyze the diffraction data (Figure S1).…”

Crystal-Chemical Properties of Synthetic Almandine-Pyrope Solid Solution by X-Ray Single-Crystal Diffraction and Raman Spectroscopy

“…The wavelength of the incident X-ray was 0.4340 Å, and the beam size was 12 µm × 18 µm. Diffraction images were acquired on Dectris Pilatus 1M detector and calibrated using the ambient LaB 6 as the diffraction standard [14]. Stepped ϕ rotation exposures were collected for the single-crystal sample of different components, with an exposure time of 1 s/deg.…”

Pressure-induced magnetovolume effect in CoCrFeAl high-entropy alloy

“…The sample was thus compressed non-hydrostatically despite the presence of a soft PTM neon. These two runs of experiments were performed at the Advanced Photon Source of Argonne National Laboratory, beamline 13BM-C, GSECARS 38 . The incident X-ray beam was monochromatized to 28.57 keV (wavelength of 0.4340 Å) and focused to a spot size of 18 μm (vertical) × 12 μm (horizontal) (FWHM).…”