To investigate an effect of phase separation on precipitation characteristics of ZnS microcrystals in ma-trix glass ZnS doped borosilicate glasses for nonlinear optical applications were prepared by melting and pre-cipitation process. ZnS dopant contributed to phase separation promotion which increased the phase separa-tion of the matrix glass within immiscibility region. It was also found that ZnS as phase separation promoter showed a similar contribution for some selected glass compositions in miscibility region. The precipitation of ZnS microcrystals occurred in thephase separable glass compoitions. The radius of ZnS microcrystals in-creased with increasing the heat treatment temperature and Na2O contents of matrix glass composition. The ZnS particle sizes estimated by effective mass approximation ranged from about 30 to 80${AA}$ It was suf-ficiently small to show quantum confinement effect.