Nickel particles were prepared form nickel chloride by hydrazine reduction in sodium dodecyl sulfate (SDS)-polyvinylpyrrolidone (PVP) clusters. XRD proof shows that the nickel particles are face centric structural with an average radius of 16 nm. TEM image implies that nickel particles merge with each other in the course of growth. SEM images indicate that the nickel particles are spherical and formed by linear nickel crystals, whose radius are about 20 nm, in accordance with the result of XRD analysis. With the increase of SDS concentration, the size of nickel particle decreases, implying that SDS-PVP complex could control the particle size.