X-Ray Diffraction under Extreme Conditions at the Advanced Light Source

Abstract

Abstract:The more than a century-old technique of X-ray diffraction in either angle or energy dispersive mode has been used to probe materials' microstructure in a number of ways, including phase identification, stress measurements, structure solutions, and the determination of physical properties such as compressibility and phase transition boundaries. The study of high-pressure and high-temperature materials has strongly benefitted from this technique when combined with the high brilliance source provided by third generation synchrotron facilities, such as the Advanced Light Source (ALS) (Berkeley, CA, USA). Here we present a brief review of recent work at this facility in the field of X-ray diffraction under extreme conditions, including an overview of diamond anvil cells, X-ray diffraction, and a summary of three beamline capabilities conducting X-ray diffraction high-pressure research in the diamond anvil cell.

High-pressure polymorphism inl-threonine between ambient pressure and 22 GPa

“…34,35 A total of six diffraction measurements were carried out between 1.26 to 6.67 GPa using a Bruker-Nonius APEX II diffractometer following the collection strategy of Dawson et al 36 Single-crystal diffraction data between 4.0 and 22.3 GPa were measured at room temperature on Beamline 12.2.2 at the Advanced Light Source in Berkeley, California, USA, which has been described in detail elsewhere. 37,38 Crystals measuring ca. 50 μm 3 were cut from larger single crystals and mounted with a ruby sphere in a BX-90 type DAC 39 consisting of 500 μm Boehler-Almax cut diamonds mounted in tungsten-carbide backing seats.…”

A Review of the Melting Curves of Transition Metals at High Pressures Using Static Compression Techniques

“…This technique takes advantage of the extreme hardness and the optical properties of diamond, which is transparent in a very wide wavelength range, from gamma and X-rays to mid-infrared, allowing not only laser irradiation but also coupling with various experimental techniques, both in synchrotron facilities and in laboratories. To demonstrate the versatility of the LH-DAC, one can refer to experimental works on X-ray diffraction (XRD) [149][150][151][152][153][154][155][156][157], X-ray absorption (XAS) [158][159][160][161], X-ray fluorescence (XRF) [162], Mössbauer spectroscopy (SMS) [163,164], inelastic X-ray scattering (IXS) [144][145][146], nuclear inelastic scattering (NIS) [165], nuclear magnetic resonance (NMR) [166], and Raman [167][168][169][170][171] and Brillouin [172][173][174][175] spectroscopies or the synthesis of novel materials [176][177][178][179][180][181][182][183]. Different types of diamond anvil cells exist for different applications, but especially for the LH-DAC, the angular opening of the cell is of crucial importance, especially when coupled with experimental techniques such as XRD or Raman/Brillouin spectroscopies, but also when an off-axis laser heating geometry is in place [61].…”

Equation of State of TiN at High Pressures and Temperatures: A Possible Host for Nitrogen in Planetary Mantles

“…After each heating cycle, the sample was compressed to a new pressure, and the process repeated at a new location on the sample. Room temperature X‐ray diffraction experiments were performed at beamline 12.2.2 of the ALS with a mar345 Image Plate Detector and pinhole (beam size of 5 × 5 µm, exposure time of 120 s, λ = 0.4592 Å) (Stan et al., 2018). The sample‐to‐detector distance was calibrated using 1 bar diffraction of CeO 2 .…”