Chapter-I presents a brief summary of the various thin film deposition techniques, their merits and demerits. The various reports on the electrodeposition of elemental, binary and ternary semiconductors have also been surveyed in this chapter. A review of the basic principles involved in the electrodeposition of the semiconductors is also given Chapter-II and III deal with the development of electrodeposition technique for CuInSe2 films.An alternative route to fabricate CuInSe2 films are explored. This consisted of electroplating a binary system comprising of Cu and In and vacuum evaporating thick selenium film over it for further selenisation treatment. Electrodeposition characteristics of Cu,In and Cu-In in the nonaqueous bath employing ethylene glycol as the solvent are discussed in chapter II. The compositional, structural and morphological analysis of the electrodeposits was also performed and the results have been presented in this chapter. Chapter III deals with the development of rapid thermal annealing technique for the preparation of CuInSe2 films from the Cu-In/Se layers.