Chemistry and structure of mixed magnesium ferric oxide aerogels

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Abstract
Fine particles of mixed oxides having the composition MgxFe2−2xO3−2x(xbetween 0 and 1.0) were prepared via the sol-gel supercritical drying route (aerogels). Samples were then postprocessed by heating in air at 773 K and 1073 K. The structure and chemistry of the samples were deduced through x-ray diffraction, thermal gravimetric and differential thermal analysis, infrared, and specular UV-visible measurements. Surface areas were measured by the BET method. The volume saturation magnetization and particle volume distribution of MgFe2O4samples were deduced from vibrating sample magnetometer measurements. The samples withx= 0 andx= 0.5 were well-crystallized α–Fe2O3(hematite) and MgFe2O4(magnesioferrite), respectively. Samples with 0 <x< 0.5 consisted of disordered lacunar spinels containing an excess of Fe3+with respect to the spinel stoichiometry and a small amount of Fe2+. Samples heated above 773 K showed progressive segregation of α–Fe2O3. The sample withx= 0.66 was a mixture of a spinel phase and a hydrotalcite-like mixed Fe–Mg hydroxy compound containing methoxy and acetate ions. By heating in air, a monophasic Mg-excess spinel-type structure was obtained. The samples with 0.66 <x< 0.86 were mixtures of a spinel-type phase and another mixed Mg–Fe compound. When heated in air, the samples gave a mixture of MgO (probably containing Fe ions) and MgFe2O4. The saturation magnetization of MgFe2O4samples is comparable to those previously reported, with the as-produced sample having a mean particle radius of 5.5 nm.

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