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Preparation of FexOy/SiO2 nanocomposites by thermal decomposition of some carboxylate precursors formed inside the silica matrix

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Abstract

In this paper we present a study regarding the obtaining of iron oxides embedded in silica matrix, using a modified sol-gel method. This method consists in the formation, inside the silica matrix, of some Fe(III)-carboxylate compounds, resulted in the redox reaction between Fe(NO3)3 and diol.

We have synthesized four gels, starting from tetra-ethyl orthosilicate, Fe(NO3)3·9H2O and different diols: ethylene glycol, 1,2-propanediol, 1,3-propanediol and 1,4-butanediol, for a final composition 50% Fe2O3/50% SiO2. The obtained gels have been thermally treated at 130°C, when the redox reaction Fe(NO3)3-diol took place with formation of the precursors in the xerogels pores. The thermal decomposition of all four precursors took place up to 300°C.

The samples obtained by annealing at 300, 500, 700°C of the four xerogels lead to crystalline phases inside the amorphous silica matrix. γ-Fe2O3/SiO2 may be obtained as unique phase depending on the diols nature. The formation of the precursors inside the silica matrix and the evolution of the crystalline phases were analyzed by thermal analysis, FTIR spectrometry and XRD.

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Correspondence to Oana Ştefănescu.

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Ştefănescu, O., Davidescu, C., Ştefănescu, M. et al. Preparation of FexOy/SiO2 nanocomposites by thermal decomposition of some carboxylate precursors formed inside the silica matrix. J Therm Anal Calorim 97, 203–208 (2009). https://doi.org/10.1007/s10973-008-9687-6

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