Abstract: In this paper, Raman scattering spectra under low temperature were used to analyze and compare the phonons of Cd_0.96Zn_0.04Te surface lattice and elemental deposits on the surfaces, which had been treated by 4 different typical methods. By investigating the anti Stokes part in range -220-90 cm^-1, some results were concluded: mechanical polishing brings a damaged surface layer, where damage and defect accumulate; after BM solution treatment, the best surface perfection was obtained; LB solution can further improved roughness and leakage current of the Cd_0.96Zn_0.04Te surface, and then ion bombardment leaves behind much defects on the surface, but it ensures the metal/Cd_0.96Zn_0.04Te contact for good adhesion. It is shown Raman spectrum under low temperature is very effective in chemical identifying the elemental deposits and analyzing quality transformation of material surface, and then can be used in optimizing surface treatment technique for good surface quality.