The use of microwave irradiation is already established in sample preparation for analytical work [P. J. Waiter. S. Chalk. and H. M. Kingston, in Microwave-Enhanced Chemistry, Fundamentals, Sample Preparation and Application. p. 55, American Chemical Society, Washington, DC (1997).] and in solution synthesis, of organic compounds (G. Majetich and K. Wheless, ibid., p. 455). The use of microwaves for solid-state synthesis is a fairly recent development but promises advantages in speed and energy efficiency. This paper presents results from a feasibility study into microwave synthesis of some electrochemically active spinel stoichiometries using an unmodified domestic microwave oven. Although much work has been reported about these materials, they are still the subject of intensive interest as potential cathodes in lithium-ion batteries. a cheap and less toxic alternative to LiCuO2. The synthesis Of Li1.025Mn1.975O4 was Seen to be greatly accelerated by microwave: heating. even at low powers. The addition of fluorine juring syntheses using high power had a profound effect on the reaction rate and resultant panicle shape and size. Sample produced using low power from gamma -MnOOH showed unusual needle-like morphologies reminiscent of a chimie-douce process.