Protocols for High Temperature Assisted-Microwave Preparation of Inorganic Compounds

Assisted-microwave heating involves the use of a susceptor to initially heat up reactants in a microwave reaction. Once hot, the reactants themselves become directly susceptible to microwave heating and interdiffuse to form products. Assisted-microwave methods are appealing for a wide variety of high temperature solid-state reactions, reaching reaction temperatures of 1500 °C and more. Among the many advantages are that the direct volumetric heating associated with microwaves allows for rapid reaction times while employing significantly less energy than conventional furnace-based preparation. Shorter reaction times and selective heating permit volatile reactants to be incorporated stoichiometrically in the product. Undesirable reactions with containers or enclosures are also minimized. The morphology of powders obtained through microwave reactions are also more uniform and comprise smaller particles than obtained conventionally. This Methods/Protocols article is presented as a user manual for carrying out assisted-microwave preparation of bulk complex oxides in air or reducing atmospheres and sol–gel based processing of complex oxides, air sensitive intermetallics, and transition metal chalcogenides.