Cadmium selenide (CdSe) have been prepared by the reduction of mixed solution of cadmium chloride (CdCl2), sodium selenosulfate (Na2SeSO3) and diethanolamine ((CH2CH2OH)2NH) at temperatures of 80-200°C under Ar atmosphere. Characteristics of CdSe nanoparticles were analyzed using transmission electron microscopy (TEM), x-ray photoelectron spectroscopy (XPS) and x-ray diffraction (XRD) and UV-Vis absorption spectra. CdSe samples prepared at relatively low temperature of below 100°C showed cubic structure while samples synthesized at temperature above 100°C showed hexagonal phase. The increased reaction temperature caused the particle size increase as well as the agglomeration of particles to form a hollow sphere. UV-Vis absorption spectra also showed a red-shift as increasing reaction temperatures due to the gradual growth of CdSe nanoparticles in the solution. The relatively sharp absorption band from samples synthesized at 80 and 100°C can be attributed to homogeneous particle size distribution compared with those of prepared at elevated temperatures. This paper will mainly discuss the phase stability of CdSe nanoparticles as well as the hollow sphere formation.