Nanomaterials have attracted considerable, attention in modern-day technology. In this article, sulfide nanoparticles of industrial interest are formed by the sol-gel process using metal chloride precursors dissolved in a mixture of silica gel and organic cellulose network followed by a chemical reaction with hydrogen sulfide gas. Particles are then heated in a vacuum oven. While scanning and transmission electron microscopy are used to study their morphology and structure in the nanometer scale, x-ray photoelectron spectroscopy is employed to understand the bonding chemistry and the stoichiometry of the sulfide particles as a function of H2S exposure and heat treatment. The results from this study are expected to show promising applications and production of other oxides, sulfides and their compounds using sol-gel synthesis are indicated.