Incorporation, Oxidation and Pyrolysis of Ferrocene into Porous Silica Glass: a Route to Different Silica/Carbon and Silica/Iron Oxide Nanocomposites
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This work reports the incorporation of ferrocene into a porous silica glass under ambient temperature and atmosphere.After or during the ferrocene incorporation, the spontaneous formation of ferricinium ions was observed by electronparamagnetic resonance (EPR), UV-visible, X-ray absorption near-edge structure (XANES), and 57Fe Mössbauermeasurements. It was shown that the oxidation of ferrocene molecules to ferricinium ions was promoted by air andthat the Si-O- groups on the surface of the pores act as counteranions. Pyrolysis of the porous glass/ferriciniummaterial under argon atmosphere and variable temperature yields different glass/carbon nanocomposites, whichwere subsequently treated with an HF solution in order to remove the glassy fraction. The resulting insolublecarbon materials were characterized by transmission electron microscopy (TEM), Raman, and EPR spectroscopyand consisted of amorphous carbon when the pyrolysis was carried out at 900 or 1000 C and of a mixture ofcarbon nanotubes and carbonaceous materials at a pyrolysis temperature of 1100 C. When the pyrolysis wasconducted under air, the incorporated ferricinium forms -Fe2O3, and the resulting material is a transparent andhighly homogeneous glass/iron oxide nanocomposite.

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