Polymer-protected monodisperse nickel nanoparticles were synthesized by a modified polyol reduction method in the presence of poly ( N-vinyl- 2-pyrrolidone ). These nanoparticles were characterized by transmission electron microscopy (TEM), X- ray diffraction ( XRD ), selected area electron diffraction ( SAED ), as well as vibrating sample magnetometer (VSM). The experimental results show that the addition of PVP and the concentration of NaOH have strong influences on the size, agglomeration and uniformity of nanoparticles. In the presence of PVP and NaOH with low concentrations, monodisperse nickel nanoparticles with average diameters about 42 nm were obtained and characterized to be pure nickel crystalline with fcc structure. Secondary structures such as clusters, loops, and strings resulted from magnetic interactions between particles were observed. The chemical interaction between the PVP and nickel nanoparticles was found by FTIR. The saturation magnetization ( Ms ), remanent magnetization (Mr) and coercivity ( Hc ) of these nickel nanoparticles are lower than those of bulk nickel.