Maghemite (γ‐Fe2O3) is a metastable iron oxide phase and usually undergoes fast phase transition to hematite at elevated temperatures (>350 °C). Maghemite nanoparticles were synthesized by the polyol method and then intercalated into a highly swollen (>100 nm separation) nematic phase of hectorite. A composite of maghemite nanoparticles sandwiched between nanosheets of synthetic hectorite was obtained. The confinement of the nanoparticles hampered Ostwald ripening up to 700 °C and consequently the phase transition to hematite is suppressed. Only above 700 °C γ‐Fe2O3 nanoparticles started to grow and undergo phase transition to α‐F2O3. The structure and the phase transition of the composite was evaluated using X‐ray diffraction, TEM, SEM, physisorption, TGA/DSC, and Mößbauer spectroscopy.
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