Materials used as fuel cell electrode should be light, high conductive, high surface area for reaction, catalytic surface and uniformity of porous structure. Nickel is widely used in electrode materials because it itself has catalytic properties. When used as electrode materials, nickel of only a few im on the surface may be sufficient to conduct the catalytic role. To manufacture the nickel with porous structure, Electroless nickel plating on carbon fiber be conducted. Because electroless nickel plating is possible to do uniform coating on the surface of substrate with complex shape. Acidic bath and alkaline bathe were used in electroless nickel plating bath, and pH and temperature of bath were controlled. The rate of electroless plating in alkaline bath was faster than that in acidic bath. As increasing pH and temperature, the rate of electrolee plating was increased. The content of phosphorous in nickel deposit was higher in acidic bath than that in alkaline bath. As a result, the uniform nickel deposit on porous carbon fiber was conducted.