The calcination and hydrogen-reduction behavior of Fe- and Ni-nitrate have been investigated. /NiO composite powders were prepared by chemical solution mixing of Fe- and Ni-nitrate and calcination at for 2 h. The calcined powders were hydrogen-reduced at 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 /NiO phase transformed to phase at the temperature of . The activation energy for the hydrogen reduction, evaluated by Kissinger method, was measured as 83.0 kJ/mol.