Nickel selenide nano particles has been successfully synthesized from the reaction of Nickel acetate [(CH3COO)2 Ni.4H2O] with sodium selenite (Na2SeO3)in the presence of glycerol as capping agent and hydrazine hydrate (N2H4.H2O)as reductant at 90oC for 6.30hours through a simple thermal reduction process. Doped NiSe: Cois synthesized by chemical Co-precipitation method using Nickel acetate [ (CH3COO)2 Ni.4H2O], Sodium selenite ( Na2SeO3),Cobalt acetate[(CH3COO)2 Co.4H2O] and PVP which act as reductant and capping agent at room temperature. NiSe and doped NiSe:Co were characterized by X-ray diffraction (XRD), Scanning electron microscopy(SEM), Visible Ultra violet spectroscopy (UV), infra red spectroscopy (IR), Energy dispersive X-ray spectroscopy (EDX)and photoluminescence (PL) spectra.