A new micro-furnace for in situ high-temperature single-crystal X-ray diffraction measurements

A new micro-furnace equipped with an H-shaped resistance heater has been developed to conduct in situ single-crystal X-ray diffraction experiments at high temperature. The compact design of the furnace does not restrict access to reciprocal space out to 2θ = 60°. Therefore, unit-cell parameters and intensity data can be determined to a resolution of 0.71 Å with Mo radiation. The combined use of mineral phases with well characterized lattice expansion (e.g. pure Si and SiO₂ quartz) and a small-diameter (0.025 mm) K-type thermocouple allowed accurate temperature calibration from room temperature to about 1273 K and consequent evaluation of thermal gradients and stability. The new furnace design allows temperatures up to about 1273 K to be reached with a thermal stability better than ±5 K even at the highest temperatures. Measurements of the lattice thermal expansion of pure silicon (Si), pure synthetic grossular garnet (Ca₃Al₂Si₃O₁₂) and quartz (SiO₂) are presented to demonstrate the performance of the device. Its main advantages and limitations and important considerations for using it to perform high-temperature diffraction measurements are discussed.