SIGMA, JURNAL SAINS DAN TEKNOLOGI, Vol. 13, No. 2 Juli 2010, ABSTRACT: Nickel sulphide thin films were deposited onto microscope glass slides by chemical bath deposition technique from aqueous solutions containing nickel sulphate and sodium thiosulfate. the effects of pH and bath temperature toward the properties of the thin films were investigated. the deposited thin films were characterized with X-ray diffraction and scanning electron microscopy. for the films deposited at pH 1.5 and 40 C, the X-ray diffraction data suggested the formation of single phase which was NiS with hexagonal structure exhibited a mixture of cubic and hexagonal phase. These observations were supported by scanning electron microscopy results.