High-pressure and high-temperature differential scanning calorimeter for combined pressure-concentration-temperature measurements of hydrides

The design and construction of a high-pressure (200 bar) and high-temperature (600 °C) heat-flow differential scanning calorimeter (DSC) for the in situ investigation of the hydrogenation and dehydrogenation reactions of hydrides is presented. In combination with a pressure-concentration-temperature (pcT) system, simultaneous thermodynamic and volumetric measurements become accessible. Due to the high thermal conductivity of hydrogen, only the sample cell and the reference cell are exposed to hydrogen and the remaining system is under ambient conditions. This separation has the advantage that the calibration factor is independent of the hydrogen pressure. The internal empty volume of the combined system is as low as possible to maximize the precision of the pcT measurements. The calorimetric block of the DSC is designed with a silver/copper alloy and the temperature measurements are made resistively with platinum temperature sensors (Pt 100). The instrument was calibrated and its operability was successfu...