In this paper, the 0.1 mol·L−1 FeSO4, NiSO4 mix-solution and 4 mol·L−1 NaOH solution were prepared by FeSO4·7H2O, NiSO4·6H2O and NaOH as raw materials. The Ni-Fe precursor nano-powders were prepared by chemical co-precipitation. The reaction conditions were that dropping speed 50 ml·min−1, pH value of reacting terminal 12, stirring speed 1200 r·min−1, reacting temperature 20°C, and reacting time 40 min. The shape of Ni-Fe precursor nano-powders were nano-stick and nano-ball. Length of Fe50Ni50 precursor nano-stick was 100–150 nm, diameter was 10–30 nm. Diameter of Fe50Ni50 precursor nano-ball was 10–50 nm. The Fe50Ni50 alloy nano-powders were prepared with materials Fe50Ni50 composite oxide by hydrogen co-reduction in closed circular system. The process conditions were that reduction temperature 600°C, reduction time 30 minutes. The Fe50Ni50 alloy nano- powders size was less than 100 nm.