Solid solution semiconductor(Zn

x

Cd

1-x

S)doped sillica glasses were prepared by sol-gel process and in-situ technique. The absorption edge of above materials shift to short wavelength direction with increasing of Zn contents. The increase of heat treatment temperature is benefit to format of perfect microcrystallite. The photoluminescence spectra excited by short laser pulse consist of two parts: the first at about 500 nm is produced by recombination of electrons and holes which are trapped in the acceptor or donor energy level

and second at about 600 nm is raised from recombination of surface state and defect

also the former is distributed over longer wavelength range which shift to short wavelength direction with increasing of Zn contents

and the intensity of later is reduced by increasing of heat treatment temperature.