HYDROTHERMAL SYNTHESIS OF MICROPOROUS TIN SULFIDES STUDIED BY REAL-TIME IN-SITU ENERGY-DISPERSIVE X-RAY-DIFFRACTION

Real-time in situ energy-dispersive X-ray diffraction. has been used t o study the synthesis of the open-framework sulfide TMA-SnS-1, under h ydrothermal conditions. The effects of varying the temperature of reac tion, reactant source, and pH of solution on the synthesis have been s tudied. It is found that temperature is the primary factor in determin ing whether crystalline products are formed, while the pH of solution and reactant source were found to be important in determining the rate of reaction and the polytypic structure produced. Evidence has been o btained that in cases where crystalline TMA-SnS-1 is formed, the react ion proceeds via an intermediate disordered lamellar phase, before rea cting further to form the final product.