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  • Author or Editor: Oana Ştefănescu x
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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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Abstract  

Hybrid organic–inorganic materials, silica–diol, were synthesized by the sol–gel process from mixtures of tetraethylorthosilicate (TEOS) and diols: ethylene glycol (HO–CH2–CH2–OH) and 1,3 propane diol (HO–CH2–CH2–CH2–OH), in acid catalysis. The gels have been synthesized for a molar ratio H2O:TEOS = 4:1 and different molar ratios diol/TEOS: 0.25; 0.5; 0.75; 1.0; 1.25 and 1.5. The resulting gels were studied by thermal analysis and FT-IR spectroscopy, in order to evidence the interaction of diols with silica matrix. Thermal analysis indicated that the condensation degree increases with the molar ratio diol/TEOS until a certain value. The thermal decomposition of the organic chains bonded within the silica network in the temperature range 250–320 °C, leaded to a silica matrix with modified morphology. The adsorption–desorption isotherms type is different for the samples with and without diol. Thus, the specific surface areas have values <11 m2/g for the samples without diol and >200 m2/g for the samples with diols, depending on the annealing temperature.

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Abstract

This article presents a study on obtaining Ni, Zn ferrite starting from Fe(III), Ni (II), Zn (II) nitrates and some polyols: 1,2-propane diol, 1,3-propane diol and glycerol. While heating, a redox reaction takes place between nitrate anion and polyol, with formation of carboxylate type precursors. The obtained precursors have been investigated by thermal analysis, FT-IR spectrometry and atomic absorption spectroscopy. The thermal decomposition of the synthesized precursors up to 350 °C leads to the formation of Ni, Zn ferrite as unique phase, evidenced by XRD. The average diameter of the ferrite crystallites, estimated from XRD data, takes values within the range 20–50 nm, depending on the annealing temperature. Transmission Electron Microscopy has evidenced the obtaining of spherical, agglomerated nanoparticles. The magnetic properties of the synthesized samples, measured in cvasistatic magnetic field (50 Hz) are characteristic for the Ni, Zn ferrite nanoparticles, with narrow hysteresis cycle and values of the saturation magnetization <70 emu/g.

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