The NiO-ZnO binary materials had been prepared by co-precipitation method. The weight percent of nickel of NiO-ZnO materials were 5, 10 and 20; they were pretreated under air at temperature of 300, 500 and 700°C, respectively. The characterization of NiO-ZnO materials were the thermal gravity analysis(TGA), X-ray diffraction(XRD), N2 adsorption-desorption at 77K, scaning electron microscope(SEM) and temperature-programmed reduction(TPR). The results revealed that surface areas of NiO-ZnO materials order from large to small were 20NiZn(OH)x(66 m2·g-1) > 10NiZn(OH)x(34 m2·g-1) > 5NiZn(OH)x(9 m2·g-1) after being calcined at the temperature of 500°C. Further, NiO-ZnO materials had two main reductive peaks at 390-415°C and 560-657°C, respectively. In all NiO-ZnO materials, 20NiZn(OH)x-C500 material had the highest surface area and the best interaction between NiO and ZnO.