単結晶X線回折実験用ガス炎加熱装置と温度測定方法

抄録

Gas-flame heating apparatus for X-ray diffraction studies designed by Yamanaka, Takéuchi and Sadanaga (1981) consists of gas flow controller and microburner set on the stand and provides temperatures higher than 2000°C. Control of the temperature of the sample is carried out by varying the mixing ratio of propane, oxygen and nitrogen gases. The last gas plays a role to regulate the heating temperature and to suppress a fluctuation of the gas-flame especially at low temperatures. It has been demanded to improve the microburner for a more applicable usage for the single-crystal X-ray diffraction studies. A newly devised heating system is composed of a joint assembly of gas-flame and electric resistance heater. Since the assembly is set on the χ-circle of a four-circle X-ray diffractometer, measurement of the diffraction intensities can be made throughout the same samplesetting from room temperature to high temperatures up to 2500°C and can be conducted at more stable and highly desired temperatures. The measurement of the sample-temperatures higher than 1500°C is carried out by a thermocouple of Pt-Rh (20-40%) or Ir-Rh (40%) and an optical pyrometer. For the precise temperature measurement during the collection of intensity data, the sample is mounted on the thermocouple attached to the goniometer head. The thermoelectric current is guided to the regulator and recorder through a ring terminal fixed to the goniometer.