The iron and zinc calcium oxysulfides Ca3Fe4S3O6, CaFeSO and CaZnSO are synthesized by reacting mixtures of CaO and FeS or of CaO and ZnS in an inert atmosphere. Their elemental compositions and lattice parameters are determined by X-ray microanalysis and X-ray diffraction. From the temperature-dependent lattice parameters of oxysulfides (measured up to 1170K) their thermal expansion coefficients are evaluated. Oxidation Ca3Fe4S3O6 and CaZnSO are studied by thermogravimetric analysis when air heated. Oxidation speed temperature coefficients showing that process limiting stage is diffusion are determined.