NiS and PdS thin films are prepd. at 10-2 torr from the single-source precursors M(S2COCHMe2)2, M = Ni and Pd. Two different vapor deposition processes, photochem. and thermal, are employed. Gas-phase emission spectroscopy is used during the photochem. deposition to identify the two elemental components of the final materials, the metal atom and sulfur, in the gas phase. NiS and PdS thin films are grown by the thermal process at 300 and 350 °C, resp., on Si and quartz substrates. The NiS films are highly oriented rhombohedral (g) phase, and the PdS films are tetragonal-phase polycryst. The metal sulfide films are grown photolytically by 308 nm laser irradn. of the gas-phase precursors at lower temps. (near the sublimation temp.). The NiS films show no x-ray diffraction patterns, but the PdS films are nonoriented polycryst. tetragonal phase. The films are analyzed by various surface anal. tools including scanning electron microscope, x-ray photoelectron, and Rutherford backscattering techniques.