The preparation and characterization of materials several examples which illustrate different aspects of ma terials problems encountered by this writer during the past twenty years will be presented in this paper these examples will be used to demonstrate a number of different synthetic approaches aswell to relate the quality of the product to the type of measurement being studied . The papers focus on advances and developments in the preparation and characterization of materials such as ferroics layered materials metal oxides and other electronic materials amorphous materials including glasses and high temperature ceramics. Some problems associated with solid solid reactions sintering and crystal growth characterization of materials preparation and characterization of polycrystalline samples of transition metal oxides with the spinel structure the copper sulfur system growth of single crystals by chemical vapor transport and the growth of oxide single crystals. Preparation of the materials for the synthesis powdered high purity elements 9999 were used in amounts corresponding to the stoichiometric composition of the compound the synthesis took place in a two step process