X-ray diffraction and electroresistance measurements under high pressure and temperature using a large-volume cell

In this communication we report about original experimental techniques for in-house x-ray diffraction and electrical resistance measurements under high-temperature and high pressure conditions, using large volume cells in the opposite anvil recessed geometry. The high-pressure devices we are currently using are a compact Paris-Edinburgh (PE) V5 150 Tons press and a 50 Tons standard hydraulic press, coupled usually with WC anvils and 10 mm or 7 mm boron-epoxy or pyrophyllite biconical gaskets for x-ray diffraction and resistance measurements respectively. Limiting pressures, using such a non-toroidal sample assembly and WC anvils, are about 10 GPa on samples of large sizes (10-20 mm3). Samples can be heated using an hollow graphite cylinder as a crucible reaching temperatures as high as 2300 K, while the temperature can be measured up to 1300 K by using a K-type thermocouple. The highly automated setup developed for resistance measurements is described in details. In particular, we present electroresistance measurements of Bi melting under pressure and measurements of the Ge and LiF EOS (equation of state) at high temperature and pressure obtained using x-ray diffraction showing the sensitivity of the techniques. The relevance of these experiments to the exploitation of the potential of equipments available at synchrotron radiation facilities is emphasized.