Atmospheric pressure chemical vapor deposition (APCVD) of niobium sulfide coatings was achieved on glass substrates from the reaction of NbCl(5) and S(SiMe(3))(2), tBu(2)S(2), tBuSH, or HSCH(2)CH(2)SH at 250-600degreesC. The niobium sulfide films grown at temperatures above 500degreesC were crystalline, and powder X-ray diffraction showed that two polytypes of NbS(2) were produced. The sulfur precursor used is fundamental to the polytype of NbS(2) obtained; films that are grown from the APCVD reaction of NbCl(5) and S(SiMe(3))(2) or tBu(2)S(2) at 500-600degreesC crystallize into the 1T structure, whereas those grown from the APCVD reaction of NbCl(5) and tBuSH or HSCH(2)CH(2)SH at 500-600 degreesC crystallize into the 3R structure. Energy dispersive X-ray analysis (EDXA) studies gave elemental ratios close to the expected 1:2 ratio for Nb:S. Scanning electron microscopy (SEM) revealed surface morphologies consistent with an island growth mechanism. The films were also characterized using Raman and X-ray photoelectron spectroscopy, both of which showed differences consistent with the formation of the two polytypes, 1T and 3R-NbS(2). (C) Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2004.