Heated gas technique for the high temperature single crystal X-ray diffraction

Abstract

A new specimen heating equipment is developed for the four-circle diffractometer and the precession camera. The specimen is heated by a hot gas stream. The temperature can be varied from the room temperature to 1100°C and the atmosphere around the specimen can be controlled by changing the composition of gases for heating. The specimen temperature is stable to ±1°C over the full range of the χ angle. The equipment imposes no significant mechanical restrictions on the angular ranges of the four circles. The absorption of incident and diffracted beam intensities due to the high polymer film, which is used as a heat shield of the specimen, is less than 1%. Installation, adjustment and handling of the equipment are very simple and easy. The use of this equipment has been demonstrated for the high temperature X-ray diffraction experiments of the delafossite-type compound CuAlO₂.