SILAR deposition of CuInSe 2 films was performed by using Cu 2+–TEAH 3 (cupric chloride and triethanolamine) and In 3+–CitNa (indium chloride and sodium citrate) chelating solutions with weak basic pH as well as Na 2SeSO 3 solution at 70 °C. A separate mode and a mixed one of cationic precursor solutions were adopted to investigate effects of the immersion programs on crystallization, composition and morphology of the deposited CuInSe 2 films. Chelating chemistry in two solution modes was deducted based on IR measurement. The XRD, XPS and SEM results showed that well-crystallized, smoothly and distinctly particular CuInSe 2 films could be obtained after annealing in Ar at 400 °C for 1 h by using the mixed cationic solution mode.