Hydrothermal Synthesis of Microporous Tin Sulfides Studied by Real-Time in Situ Energy-Dispersive X-ray Diffraction

Abstract

Real-time in situ energy-dispersive X-ray diffraction has been used to study the synthesis of the open-framework sulfide TMA−SnS-1, under hydrothermal conditions. The effects of varying the temperature of reaction, reactant source, and pH of solution on the synthesis have been studied. It is found that temperature is the primary factor in determining 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 obtained that in cases where crystalline TMA−SnS-1 is formed, the reaction proceeds via an intermediate disordered lamellar phase, before reacting further to form the final product.