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°C for 2 h. The calcined powders were hydrogen-reduced at 350°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°. The activation energy for the hydrogen reduction, evaluated by Kissinger method, was measured as 83.0 kJ/mol.