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Comparison of two soft chemistry routes for the synthesis of mesoporous carbon/β-SiC nanocomposites

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Abstract

We compare the influence of using either molecular or colloidal precursors on the synthesis of a ceramic material containing SiC and porous carbon. Remarkably, the temperature of synthesis for crystalline SiC is independent of the route chosen. The excess carbon in the initial mixture is the source of the excess porous carbon that binds to the crystalline domains of SiC in the final products. Interestingly, increasing the initial area of surface contact between carbon and silicon in the ceramic precursor results in different porosities in the ‘meso’ range. Simultaneous control of the size and the relative amounts of Si and C in the precursors allows control to be exerted over the nature and texture of the final powders. A simple and general mechanism is herein proposed to explain the evolution of the surface area as a function of the volume fraction of residual carbon in the synthesised ceramic.

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Notes

  1. Elem. Anal. Found: C, 41.97; H, 6.82; N, 3.93; O, 35.3; Si, 8.90. Calc. for C42H85N3O23Si3: C, 46.52; H, 7.90; N, 3.88; O, 33.97; Si, 7.77.FTIR νmax/cm−1 3334, 2973, 2927, 2886, 1699, 1531, 1444, 1246, 1056, 949; 13C CP MAS NMR 75 MHz (δ, ppm) 156.9, 103.2, 90.2, 71.7, 58.1, 43.5, 23.2, 18.2, 7.7. 29Si CP MAS NMR 60 MHz (δ, ppm): −45.1 (T0), −52.8 (T1). Level of condensation <12 %.

  2. Elem. Anal. Found: C, 35.43; H, 5.43; N, 4.48; O, 37.7; Si, 10.01. Calc. for C48H80N6O37Si6: C, 38.39; H, 5.37; N, 5.60; O, 39.4; Si, 11.22. FTIR νmax/cm−1 3330, 2934, 2360, 2335, 1693, 1528, 1001, 13C CP MAS NMR 75 MHz (δ, ppm) 158.7, 104.9, 92.1, 73.5, 63.6, 44.4, 24.6, 11.2. 29Si CP MAS NMR 60 MHz (δ, ppm) : −57.4 (T2), −64.4 (T3). Level of condensation >95%. BET surface area <10 m2 g−1.

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Acknowledgements

The authors thank the GNR MATINEX, common to CNRS and CEA, for its financial support as well as M. Georges for his work on the molecular route. The authors also thank the COST network D43 and CM1011 for allowing discussions of all aspects of preparing nanomaterials during annual meetings.

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Authors and Affiliations

  1. ICSM-UMR 5257, CEA/CNRS/UM2/ENSCM Marcoule, BP 17171, 30207, Bagnols-sur-Cèze, France

    Xavier Deschanels, Guilhem Arrachart, Cyrielle Rey, Agnès Grandjean, Guillaume Toquer, Renaud Podor & Thomas Zemb

  2. Centrale Marseille, Aix Marseille Université, CNRS, iSm2 UMR 7313, 13397, Marseille, France

    Damien Hérault

  3. Institut Charles Gerhardt, UMR 5253, Université de Montpellier 2, 34095, Montpellier, France

    Geneviève Cerveau & Robert Corriu

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  1. Xavier Deschanels
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Correspondence to Xavier Deschanels.

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Deschanels, X., Hérault, D., Arrachart, G. et al. Comparison of two soft chemistry routes for the synthesis of mesoporous carbon/β-SiC nanocomposites. J Mater Sci 48, 4097–4108 (2013). https://doi.org/10.1007/s10853-013-7222-z

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