New Microthermogravimetric Apparatus. Kinetics of metal sulphidation and transport properties of transition metal sulphides

A novel microthermogravimetric apparatus to study the kinetics of metal sulphur reactions and transport properties of transition metal sulphides has been described. The main feature of this arrangement includes the application of the carrier gas for sulphur vapour transportation and the protection of the balance chamber from sulphur attack. As a consequence, the helix balance could have been replaced by an automatic electronic microbalance and the accuracy of the mass change measurements increased more than two orders of magnitude, up to 10–7 g. The application of two liquid sulphur reservoirs created very stable, strictly defined reaction conditions, and enabled to make rapid changes of sulphur partial pressure in the reaction chamber. It has been demonstrated that all these innovations make it possible to study not only the kinetics of very slow sulphidation processes but also to determine deviations from stoichiometry and defect mobility in transition metal sulphides.