A novel preparation technique for a nanostructured anode for a solid oxide fuel cell is investigated. By mixing nanometer-sized NiO and YSZ powders in a pH-controlled aqueous media, a fine mixture of nanoparticles is successfully obtained through heterocoagulation. The anode prepared from thus prepared mixture has a large triple phase boundary and shows a great improvement in the anode performance by increasing the electric conductivity and effective surface area.