The calcination and hydrogen-reduction behavior of Fe- and Ni-nitrate have been investigated. $Fe_2O_3$/NiO composite powders were prepared by chemical solution mixing of Fe- and Ni-nitrate and calcination at $350^{circ}C$ for 2 h. The calcined powders were hydrogen-reduced at $350^{circ}C$ for 30 min. The calcination and hydrogen-reduction behavior of Fe- and Ni-nitrate were analyzed by TG in air and hydrogen atmosphere, respectively. TG and XRD analysis for hydrogen-reduced powders revealed that the $Fe_2O_3$/NiO phase transformed to $FeNi_3$ phase at the temperature of $350^{circ}$. The activation energy for the hydrogen reduction, evaluated by Kissinger method, was measured as 83.0 kJ/mol.