Cu-In-Se compounds were synthesized by wet chemical route using CuCl, InCl3, and Se as precursors, and CuInSe2 (CIS) was acquired via annealing of Cu-In-Se compounds. As-synthesized compounds exhibited CuSe2-rich phases. The compounds synthesized below 95 degrees C transformed into CIS phase after the annealing above 450 degrees C, however the compounds synthesized above 100 degrees C exhibited different transitions from CuSe2 to Cu2Se. This could be explained by the excessive Se-loss in the surface of big rod. The size of the CIS was about 7.8nm and the elemental ratio of (Cu:In:Se) in the NCs was 1:0.7:2.