Fine face-centered cubic (FCC) nickel powders were synthesized by liquid phase reduction with different surfactants. The products were investigated by scanning electron microscopy (SEM), laser particle size analyzer and X-ray powder diffraction (XRD). The results indicate that the type, dosage and relative molecular mass of surfactants significantly impact the purity, dispersion property, particle size, size distribution and morphology of the products. The nonionic surfactants poly ethylene glycol (PEG) and polyethylene glycol sorbitan monostearate (Tween) showed better dispersing ability in the reaction system than the others. The optimal mass ratios of surfactant to Ni are 100 mg/g and 150 mg/g for PEG-600 and Tween-40, respectively. The products obtained in the optimal conditions have ideal morphology and narrow size distribution. Moreover, study on the relative molecular mass effect revealed that with the increase of the relative molecular mass of Tween, the morphology of nickel powders changed from sphere to spiny ball.