An ultra-high-vacuum chamber for high-temperature X-ray diffractometry

Abstract

An attachment to a horizontal goniometer for X‐ray powder diffraction at temperatures up to about 2,000°C in a vacuum in the 10−9 torr range is described. Specimen heating is by direct contact to a resistance strip heater with provision for electron beam heating. Temperature measurement is by thermocouple or optical pyrometer. High‐temperature parameter measurements on vanadium are presented as one of the examples of the capability of the apparatus.

X-ray diffraction

“…Czank and Kleber (77), in addition to a description of their furnace, which is capable of reaching temperatures up to 1500 °C, also discuss the problems of temperature measurement and calibration procedures. Other furnaces reported for powder diffractometry are two capable of reaching 2500 °C (49,125), one used for thermal expansion studies of polymers (340), an ultra-high vacuum chamber plus capability of reaching 2000 °C (197), and the use of solar radiation concentration to achieve temperatures up to about 3000 °C (167, '269). An extensive review of methods of heating sample holders and the problems associated with high temperature diffractometry has been presented by Gerard (117).…”