The main objective of this proposal is better understanding of underlying atomic and molecular processes involved in the microstructural evolution of polycrytalline TiS2 and other powders synthesized using the thi-sol-gel process previously proposed by the P.I. A secondary objective is to investigate the electrochemical properties of the resulted thin layer, the influence of heat treatment and of charging on the particulate microstructure. The effects of particle size, shape, crystallite size, orientation and stoichiometry on the elctrochemical properties and the mechanisms involved in the evolution of the microstructure will be investigated using differential thermal and thermogravimetric analyses, scanning and transmission electron microscopy. If successful, the research may provide a method to synthesize an engineered microstructure with optimal electrochemical properties. Applications include electrochemical batteries. The preliminary test have indicated a dramatic increase of the number of charging cycles for a given reduction in performance.