Tricobalt tetraoxide (Co3O4) samples having different thiourea/Co molar ratio of 0, 5 and 10 were prepared by wet chemical synthesis. The effects of thiourea content on the crystal structure-related parameters of Co3O4 were determined. The increase in the amount of thiourea caused a gradual decrease in the lattice parameters and specific surface area and an increase in the crystallinity and crystallite size. The experimental analysis results showed that thiourea content can be used to control the crystal structure-related parameters of Co3O4.