The material of doping transition metal (TM) in chalcogenide compound such as ZnS and ZnSe can be used in sensors, nonlinear optics, optical thin-films and mid-infrared area because of their faster optical response time, wider transparency range of mid-infrared and higher mid-infrared transmittance, low optical loss and phonon energy. In this paper, the ceramic targets of (ZnS/Se)0.4(Co)x(Ga2O3)0.6-x(x=0.1, 0.3 and 0.5) were prepared by high temperature solid state reaction. The mass loss rate, shrinkage rate and molar ration were calculated. XRD, absorption spectrum and AFM&OM were investigated. All of the results are shown that the optimum doping concentration is (ZnS/Se)0.4(Co)0.5(Ga2O3)0.1(namely x=0.5), and the optimum intering temperature are in the range 1000~1200°C. Besides, the zinc-blende structure on ceramics targets was confirmed by XRD. A broad application range from VIS to Mid-infrared was suggested by absorption spectra. The optimal base material ZnSe was proved by AFM and OM. All these results indicate that bulks of (ZnS/Se)0.4(Co)x(Ga2O3)0.6-xare most promising materials in future