A furnace for the in situ study of the formation of inorganic solids at high temperature using time-resolved energy-dispersive x-ray diffraction

The design, construction, and use of a furnace from which time-resolved x-ray diffraction data may be measured from reacting mixtures of solids or of solids and liquids is described. The furnace is a vertical tube design, constructed from commercially available components, and can operate at temperatures of up to 1000 degreesC. The apparatus is designed to heat sample tubes of up to 3 cm diameter. The use of high-intensity synchrotron-generated white-beam x rays allows the tube and its contents to be penetrated; thus x-ray diffraction data can be measured from reactions taking place in laboratory-sized reaction vessels. The energy-dispersive diffraction geometry allows rapid data collection (of the order of seconds); hence reactions can be followed continuously in real time. The use of the furnace is demonstrated by results from experiments performed on Station 16.4 of the Daresbury Synchrotron Radiation Source, UK. Two distinct reaction types are studied, both used to prepare the layered perovskite RbCa2Nb3O10: first, a solid state route at 800 degreesC and second a flux route, performed in molten RbCl, also at 800 degreesC. (C) 2000 American Institute of Physics. [S0034-6748(00)03111-7].