摘要

We are presenting a simple and inexpensive, in-home made high-temperature (HT) device, suitable for high-temperature in situ investigations of phase transitions, crystallite growth and other thermal features of solid-state materials by X-ray diffraction (XRD). The attachment can be easily mounted on conventional laboratory X-ray diffractometer. The HT-device consists of sample holder and heating element combined together. The unit is made from fused quartz, which temperature resistance is above 1000 degrees C. The sample holder (the front part of the body) can be shaped to match the conventional front packing powder holder for the equipment that is used. The heating element consists of a khantal tape that is mounted on the backside of the body. Different ways of mounting the heating tape can be used to optimize the desired uniform heat distribution within the volume of the packed powder. The length of the heating tape can be adjusted, for tuning its total resistance and accordingly - its heating power. Both the sample holder and the heating element are made "small" to ensure a good thermal exchange and to save energy required for heating. Due to its small size, limited contact with the diffractometer and the good thermal stability of quartz in air, the HT-device does not require water-cooling and can be used for multiple routine in situ measurements up to 950 degrees C. Its functionality was studied on standard reference material (KNO3) and on natural minerals: a mixture of clinoptilolite/opal-cristobalite and Zn-exchanged clinoptilolite. The advantages and limitations of the proposed design are discussed.

  • 出版日期2013