Investigations in high temperature X-ray crystallography

Abstract

The field of X?ray single?crystal structure analysis beyond 1000?°C is, at present, highly underdeveloped and hardly explored. Structure determinations, as are routinely performed at room and low temperatures, have not been carried out at such high temperatures. Modern research in high?temperature technology is producing an ever?increasing number of new and interesting refractory materials. Detailed single?crystal analysis at high temperatures can contribute significantly to a better understanding of these materials—coordination in crystal structures, thermal vibrations, electron densities in atoms, and hence the ionization state of atoms and the nature of chemical bonding at elevated temperatures. There is, therefore, a particular need for high?temperature devices that permit such investigations above the melting point of platinum (~1768?°C). The flame technique does not provide for experimentation under highly controlled conditions of temperature and atmosphere. The ability to reach exceptionally high temperatures, together with the simplicity and low cost of the technique, however, makes the flame approach valuable for obtaining these temperatures, even though the information obtained may be limited in nature.