Microwave‐Assisted Synthesis of MPS 3 Materials (M = Mn, Cd) Using a Dewar‐Ampoule Device

We report on an easy procedure for the synthesis of inorganic solids such as MPS 3 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 MPS 3 compounds. The temperature gradient assures the vapor phase transport to the cold zone. The resulting MPS 3 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)