The stiff sodium borosilicate gel doped with Cd(NO3)24H2O and SC(NH2)2 were prepared by using tetraethyl orthosilicate, boricacid, sodium ethoxide, Cd(NO3)2.4H2O and SC(NH2)2 as precursor. The sodium borosilicate glasses doped with CdS microcrystals were preparedby sintering sodium borosilicate transparent bulk gels with CdS which was synthesized byreacting with H2S gas. The micro-struture of gels and glasses doped with CdS microcrystalswere studied by TEM method. The luminescence spectra of nanometer size CdSmicrocrystallites in glass were measured at various temperatures, the inhomogeneosbroadening constant of 150～meV was obtained. The third order nonlinear susceptibilitiesof the CdS microcrystal glass was characterized by Z-scan method, χ(3)is 6.5×10-12 esu.