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Issue 22, 2014
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Single-source-precursor synthesis of dense SiC/HfCxN1−x-based ultrahigh-temperature ceramic nanocomposites

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Abstract

A novel single-source precursor was synthesized by the reaction of an allyl hydrido polycarbosilane (SMP10) and tetrakis(dimethylamido)hafnium(IV) (TDMAH) for the purpose of preparing dense monolithic SiC/HfCxN1−x-based ultrahigh temperature ceramic nanocomposites. The materials obtained at different stages of the synthesis process were characterized via Fourier transform infrared (FT-IR) as well as nuclear magnetic resonance (NMR) spectroscopy. The polymer-to-ceramic transformation was investigated by means of MAS NMR and FT-IR spectroscopy as well as thermogravimetric analysis (TGA) coupled with in situ mass spectrometry. Moreover, the microstructural evolution of the synthesized SiHfCN-based ceramics annealed at different temperatures ranging from 1300 °C to 1800 °C was characterized by elemental analysis, X-ray diffraction, Raman spectroscopy and transmission electron microscopy (TEM). Based on its high temperature behavior, the amorphous SiHfCN-based ceramic powder was used to prepare monolithic SiC/HfCxN1−x-based nanocomposites using the spark plasma sintering (SPS) technique. The results showed that dense monolithic SiC/HfCxN1−x-based nanocomposites with low open porosity (0.74 vol%) can be prepared successfully from single-source precursors. The average grain size of both HfC0.83N0.17 and SiC phases was found to be less than 100 nm after SPS processing owing to a unique microstructure: HfC0.83N0.17 grains were embedded homogeneously in a β-SiC matrix and encapsulated by in situ formed carbon layers which acted as a diffusion barrier to suppress grain growth. The segregated Hf-carbonitride grains significantly influenced the electrical conductivity of the SPS processed monolithic samples. While Hf-free polymer-derived SiC showed an electrical conductivity of ca. 1.8 S cm−1, the electrical conductivity of the Hf-containing material was analyzed to be ca. 136.2 S cm−1.

Graphical abstract: Single-source-precursor synthesis of dense SiC/HfCxN1−x-based ultrahigh-temperature ceramic nanocomposites

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Publication details

The article was received on 18 Jun 2014, accepted on 07 Sep 2014 and first published on 10 Sep 2014


Article type: Paper
DOI: 10.1039/C4NR03376K
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Nanoscale, 2014,6, 13678-13689

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    Single-source-precursor synthesis of dense SiC/HfCxN1−x-based ultrahigh-temperature ceramic nanocomposites

    Q. Wen, Y. Xu, B. Xu, C. Fasel, O. Guillon, G. Buntkowsky, Z. Yu, R. Riedel and E. Ionescu, Nanoscale, 2014, 6, 13678
    DOI: 10.1039/C4NR03376K

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