The synthesis of CuBi3 S5 and CuBi3 Se5 and their basic photoelectric properties are reported for the first time. CuBi3 S5 and CuBi3 Se5 were prepared successfully by solvothermal method using hydrazine hydrate (N2 H4 ·H2 O) as the reductant agent in conjunction with solid state reaction method. The resistance dependence of CuBi3 S5 and CuBi3 Se5 on temperature were measured by four-point probe method, the results showed that the CuBi3 S5 has semiconductor nature and CuBi3 Se5 has metal nature. The thermal activation energy of CuBi3 S5 was about 17.1 meV calculated from Arrhenius equation. The Hall effect experiment of CuBi3 S5 was carried out at room temperature, its carrier concentration is about 3.75×1017 cm-3 and Hall mobility is about 14 cm2V-1s-1. CuBi3 S5 is an n-type semiconductor. The diffuse reflectance spectroscopy indicates that the band gap of CuBi3 S5 is about 0.66 eV.