NiO-Al 2 O 3 -ZrO 2 and Co 3 O 4 -Al 2 O 3 -ZrO 2 catalysts were prepared by three different co-precipitation methods, namely co-precipitation, surfactant-assisted co-precipitation, and surfactant-assisted co-precipitation with ultrasound mixing methods, and their activities were tested in selective CO methanation. Catalysts were characterized using N 2 physisorption, XRD, SEM, TEM, XPS, and TPR-H 2 techniques. CO methanation and selective CO methanation reactions were carried out. Catalysts prepared by surfactant assisted co-precipitation gave high surface area, uniform pore size distributions, and small pores. The NiO-Al 2 O 3 -ZrO 2 catalyst prepared by surfactant-assisted coprecipitation gave 50% CO conversion to CH 4 at 155• C and all CO converted to CH 4 when T > 225 • C. For the selective CO methanation, the CO level decreased below 100 ppm at 200• C over the NiO-Al 2 O 3 -ZrO 2 catalyst prepared by surfactant-assisted co-precipitation.