High-temperature experiments using a resistively heated high-pressure membrane diamond anvil cell

Rev Sci Instrum. 2013 Sep;84(9):095114. doi: 10.1063/1.4821622.

Abstract

We describe a reliable high performance resistive heating method developed for the membrane diamond anvil cell. This method generates homogenous high temperatures at high pressure in the whole sample for extended operation period. It relies on two mini coil heaters made of Pt-Rh alloy wire mounted around the diamond anvils and gasket, while temperature is monitored by two K-type thermocouples mounted near the sample. The sample, diamonds, and tungsten-carbide seats are thermally insulated from the piston and cylinder keeping the cell temperature below 750 K while the sample temperature is 1200 K. The cell with the heaters is placed in a vacuum oven to prevent oxidation and unnecessary heat loss. This assembly allows complete remote operation, ideally suited for experiments at synchrotron facilities. Capabilities of the setup are demonstrated for in situ Raman and synchrotron x-ray diffraction measurements. We show experimental measurements from isothermal compression at 900 K and 580 K to 100 GPa and 185 GPa, respectively, and quasi-isobaric compression at 95 GPa over 1000 K.