TY  - JOUR
A1  - Farla, Robert
T1  - Towards joint in situ determination of pressure and temperature in the large volume press exclusively from X‐ray diffraction
Y1  - 2023-06-21
VL  - 30
IS  - 4
SP  - 807
EP  - 814
JF  - Journal of Synchrotron Radiation
DO  - 10.1107/S1600577523004538
PB  - International Union of Crystallography
N2  - Since high‐pressure devices have been used at synchrotron facilities, accurate determination of pressure and temperature in the sample has been a crucial objective, particularly for experiments that simulate the Earth's interior. However, in some cases using a thermocouple may have a high likelihood of failure or is incompatible with a high‐pressure assembly. To address these challenges and similar issues, we aim to expand a previously proposed solution: to jointly estimate pressure and temperature (<italic>PT</italic>) through <italic>in situ</italic> X‐ray diffraction, to cover a wider range of internal <italic>PT</italic> calibrants tested over larger <italic>PT</italic> ranges. A modifiable Python‐based software is offered to quickly obtain results. To achieve these aims, <italic>in situ</italic> large volume press experiments are performed on pellets of intimately mixed powders of a halide (NaCl, KCl, KBr, CsCl) or MgO and a metal (Pt, Re, Mo, W, Ni) in the pressure range 3–11 GPa and temperature range 300–1800 K. Although the pressure range was chosen for practical reasons, it also covers an equally important depth range in the Earth (down to 350 km) for geoscience studies. A thermocouple was used to validate the <italic>PT</italic> conditions in the cell assemblies. The key results show that choosing the appropriate calibrant materials and using a joint <italic>PT</italic> estimation can yield surprisingly small uncertainties (<italic>i.e.</italic> &lt;±0.1 GPa and &lt;±50 K). This development is expected to benefit current and future research at extreme conditions, as other materials with high compressibility or high thermal pressure, stable over large <italic>PT</italic> ranges, may be discovered and used as <italic>PT</italic> calibrants.</p>
N2  - Research in high‐pressure devices, such as the diamond anvil cell and the large volume press, requires knowledge of the pressure and temperature in the sample. Here, a large volume press and an internal resistive heater were used to generate high load and heat to various combinations of intimately mixed powders of materials. X‐ray diffraction and custom software were used to jointly estimate the pressures and temperatures in the samples and establish calibrants for <italic>in situ</italic> experiments at extreme conditions.<boxed-text position="anchor" content-type="graphic" xml:lang="en"><graphic position="anchor" id="jats-graphic-1" xlink:href="urn:x-wiley:16005775:jsy2vl5008:jsy2vl5008-fig-0001">
UR  - http://resolver.sub.uni-goettingen.de/purl?gldocs-11858/10843
ER  -