CuInSe2 thin films have been prepared by chemical spray pyrolysis (CSP). Effects of substrate temperature (T(s)), pH and the ion ratio (Cu/In) in the spray solution on the film properties have been investigated, and the following results have been obtained; (i) films deposited with neutralized solution (pH = 4.0) exhibited chalcopyrite structure in contrast to those deposited with unneutralized one (pH = 1.9) having sphalerite structure, (ii) resistivity increased with T(s) for films deposited with the unneutralized solution, while decrease of the resistivity was observed for the neutralized case, and (iii) remarkable increase of resistivity with decreasing Cu/In has been observed. Finally, the effect of pH on the rectifying property in the CuInSe2/CdS heterojunction has been presented.