International
Tables for
Crystallography
Volume H
Powder diffraction
Edited by C. J. Gilmore, J. A. Kaduk and H. Schenk

International Tables for Crystallography (2018). Vol. H, ch. 2.7, pp. 160-161

Section 2.7.5. Variable-temperature high-pressure devices

A. Katrusiaka*

aFaculty of Chemistry, Adam Mickiewicz University, Poznań, Poland
Correspondence e-mail: katran@amu.edu.pl

2.7.5. Variable-temperature high-pressure devices

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One of the most common interests in extreme conditions combines high pressure and high temperature. Several techniques for simultaneously controlling both pressure and temperature have been developed (Fei & Wang, 2000[link]). The DAC can be heated externally (with respect to the sample chamber between the anvils' culets) when the entire DAC is placed in an oven or in a hot stream of air from an electrical heater (Fourme, 1968[link]; Allan & Clark, 1999[link]; Podsiadło & Katrusiak, 2008[link]; Bujak et al., 2008[link]). External resistance-wire heaters placed immediately around the diamond anvils and the gasket are often used (Bassett & Takahashi, 1965[link]; Takahashi et al., 1982[link]; Adams & Christy, 1992[link]; Eremets, 1996[link]; Moore et al., 1970[link]; Hazen & Finger, 1982[link]; Besson, 1997[link]; Dubrovinskaia & Dubrovinsky, 2003[link]; Fei & Wang, 2000[link]). External heating can routinely operate up to about 673 K. Its main advantages are stability, reliable measurement of temperature and high homogeneity of temperature in the chamber. The disadvantages include the relatively low temperature range and the large mass of the DAC mechanical parts that are heated. Their thermal expansion can cause loss of pressure. This does not apply to the membrane DAC, where a constant thrust from the membrane is transmitted to the anvils. A sophisticated externally heated DAC in an atmosphere of inert gases is capable of operating between 83 and 1473 K (Bassett et al., 1993[link]).

A very small turnbuckle DAC, about 6 mm in diameter, was originally constructed of plastic and hardened beryllium–copper alloy (BERYLCO 25) in order to perform magnetic measurements at low temperature in the small bore of a superconductive quantum interference device (SQUID) (Graf et al., 2011[link]; Giriat et al., 2010[link]). These are at present the smallest designs that can be used for X-ray diffraction studies, with the whole DAC cooled by commercial low-temperature gas-stream attachments. Alireza & Lonzarich (2009[link]) built another miniature DAC for high-pressure magnetic measurements in a SQUID.

Temperatures of several thousand kelvin can be achieved by internal heating, where the sample absorbs the focused light beam of a laser (Bassett, 2001[link]; Ming & Bassett, 1974[link]; Shen et al., 1996[link]) or is heated by a thin wire passing through the chamber or its immediate surroundings, either in the gasket walls (Boehler et al., 1986[link]; Mao et al., 1987[link]; Zha & Bassett, 2003[link]; Dubrovinsky et al., 1998[link]) or in the culets of intelligent diamond anvils (Bureau et al., 2006[link]). Composite resistance gaskets, with a platinum chamber wall acting as a 35 W resistance heater, can increase the temperature to over 2273 K (Miletich et al., 2000[link], 2009[link]). Laser beam(s) focused through the DAC anvil(s) onto the sample (Boehler et al., 2001[link]) can heat it to over 3273 K. This requires that the laser beam, or several beams, or a fraction of their energy, be absorbed in the sample. In order to increase the absorption, the sample can be mixed with another compound, for example gold powder. The main disadvantage of laser heating is inhomogeneous distribution of the temperature within the sample.

Much smaller temperature gradients, of a few kelvin at 2773 K, can be obtained in large-volume presses (LVPs). The multi-anvil LVP has traditionally been applied for the synthesis of diamond, which requires stable conditions of both high pressure and high temperature (Hazen, 1999[link]; Liebermann, 2011[link]). In the LVP, a resistance heater installed inside the chamber can provide stable control of the temperature for days, while the pressure is controlled by a hydraulic press. Owing to the large sample volume, the diffraction pattern can be quickly recorded. Most often, energy-dispersive diffraction is applied for the beams entering and leaving the pressure chamber through the gasket material between the anvils. LVPs are generally very large and heavy, which contrasts with the compact construction of the Paris–Edinburgh and Kurchatov–LLB pressure cells (Besson et al., 1992[link]; Goncharenko, 2004[link], 2006[link]). Both these opposed-anvil cells can be placed in cryostats, and they can be used for either energy- or angle-dispersive diffraction of neutrons or X-rays. The Kurchatov–LLB cell has been optimized for neutron diffraction studies of magnetic structures at high pressure and low temperature (Goncharenko & Mirebeau, 1998[link]; Goncharenko et al., 1995[link]).

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