Direct mechanochemical synthesis of γ-Fe
3O
4 powders with a planetary-mill from metallic-Fe and FeO(OH)(1:2) in H
2O
2-containing acetone is proposed. At the initial stage of grinding, FeO(OH) particles are kneaded into deformable metallic-Fe forming composite particles. When the metallic-Fe is oxidized to FeO by H
2O
2, the FeO immediately reacts with FeO(OH) to form γ-Fe
3O
4. Almost singlephase γ-Fe
3O
4 is obtained by the grinding at 5s
-1 for 5.0h. The heat of oxidation of iron promotes the formation of γ-Fe
3O
4. The γ-Fe
3O
4 particles are dispersed into the grinding liquid without adhesion to the grinding media. The small amounts of residual Fe and FeO(OH) further react under heat-treatment at 300°C in Ar. The primary particle size of the synthesized γ-Fe
3O
4 is 13-17nm. α-Fe
2O
3 does not form when excess amounts of H
2O
2 are added (H
2O
2/Fe=3.17). Although H
2O as a substitute of H
2O
2 produces γ-Fe
3O
4, the addition of small amounts of oxidation reagents effectively promote the synthesis reactions.
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