Abstract

To attain the complete filling of the channels of MCM-41 with magnetite and maghemite, we have tried out an alternative method to the incipient wetness impregnation. The mesoporous material was instilled with a Fe-carrying organic salt after subjecting the matrix to a silylation treatment. Thus, a solid of 7.7 wt.% iron-loaded MCM-41 was obtained. Different subsequent thermal treatments were used to produce γ-Fe2O3 or Fe3O4. The Mossbauer and magnetic results show that after this method, the as-prepared composite displays a size-distribution of magnetic particles. It is mainly made up of fine particles that display a super paramagnetic relaxation at room temperature and get blocked at ≈2 K for the AC susceptibility time-scale measurements both for γ-Fe2O3 and Fe3O4 particles. For both samples, about 24% of larger iron-containing phases are magnetically blocked at room temperature. For the Fe3O4 particles, this fraction undergoes the Verwey transition at about 110K; in addition, there is a minor Fe(III) fraction that remains paramagnetic down to 4.2 K.

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