Microwave-Assisted Synthesis of MPS3 Materials (M = Mn, Cd) Using a Dewar-Ampoule Device

We report on an easy procedure for the synthesis of inorganic solids such as MPS3 materials (M = Mn, Cd) which uses a simple device consisting of a silica ampoule that is divided into a Dewar zone (hot zone) and a nonisolated part (cold zone), which is able to operate inside domestic microwave ovens. This is a rapid and advantageous method applied for the first time to the preparation of inorganic solids. It involves a heat concentration within the Dewar zone that allows the required temperature for the reaction between the components to be reached. In this way, a mixture of S, P, and a transition metal such as Mn or Cd, placed in the Dewar zone gives MPS3 compounds. The temperature gradient assures the vapor phase transport to the cold zone. The resulting MPS3 crystals are deposited within a few minutes in the cold area, in contrast to other conventional procedures requiring long periods of treatment or more complicated procedures for the synthesis of similar products. (© Wiley‐VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2004)