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Synthesis of polymeric precursors for the formation of nanocrystalline Ti-C-N/amorphous Si-C-N composites

Hering, Nicole ; Schreiber, K. ; Riedel, R. ; Lichtenberger, O. ; Woltersdorf, J. (2001):
Synthesis of polymeric precursors for the formation of nanocrystalline Ti-C-N/amorphous Si-C-N composites.
15, In: Applied Organometallic Chemistry, (10), pp. 879-886. Wiley, ISSN 0268-2605,
[Article]

Abstract

The synthesis of trimethylsilyl-substituted poly(titaniumcarbodiimide) as a novel precursor for titanium carbonitride based ceramic materials is described. The precursor and the subsequent processing steps (cross-linking and pyrolysis) are characterized by IR and Raman spectroscopy, thermal gravimetric analysis and simultaneous mass spectroscopy, electron microscopy and powder X-ray diffraction measurements. The novel polymer is formed by the reaction of TiCl4 or Ti(NEt2)4 with bis(trimethylsilyl) carbodiimide. Subsequent pyrolysis at 1000 °C in argon results in the formation of a ceramic composite material consisting of nanocrystalline TiCN and amorphous SiCN as constituting phases. Using Ti(NEt2)4 as a starting reagent instead of TiCl4, chlorine contamination of the ceramic material can be avoided. The different molecular vibration modes of the metal–nitrogen, metal–carbon and nitrogen– carbon bonds in poly(titaniumcarbodiimides) with trimethylsilyl substituents were calculated using quantum mechanical methods, providing a comprehensive understanding of the measured spectra.

Item Type: Article
Erschienen: 2001
Creators: Hering, Nicole ; Schreiber, K. ; Riedel, R. ; Lichtenberger, O. ; Woltersdorf, J.
Title: Synthesis of polymeric precursors for the formation of nanocrystalline Ti-C-N/amorphous Si-C-N composites
Language: English
Abstract:

The synthesis of trimethylsilyl-substituted poly(titaniumcarbodiimide) as a novel precursor for titanium carbonitride based ceramic materials is described. The precursor and the subsequent processing steps (cross-linking and pyrolysis) are characterized by IR and Raman spectroscopy, thermal gravimetric analysis and simultaneous mass spectroscopy, electron microscopy and powder X-ray diffraction measurements. The novel polymer is formed by the reaction of TiCl4 or Ti(NEt2)4 with bis(trimethylsilyl) carbodiimide. Subsequent pyrolysis at 1000 °C in argon results in the formation of a ceramic composite material consisting of nanocrystalline TiCN and amorphous SiCN as constituting phases. Using Ti(NEt2)4 as a starting reagent instead of TiCl4, chlorine contamination of the ceramic material can be avoided. The different molecular vibration modes of the metal–nitrogen, metal–carbon and nitrogen– carbon bonds in poly(titaniumcarbodiimides) with trimethylsilyl substituents were calculated using quantum mechanical methods, providing a comprehensive understanding of the measured spectra.

Journal or Publication Title: Applied Organometallic Chemistry
Volume: 15
Number: 10
Publisher: Wiley
Uncontrolled Keywords: ceramic materials, pyrolysis, titanium, carbodiimides, vibrational spectroscopy, thermal gravimetric analysis
Divisions: 11 Department of Materials and Earth Sciences
11 Department of Materials and Earth Sciences > Material Science
11 Department of Materials and Earth Sciences > Material Science > Dispersive Solids
Date Deposited: 19 Nov 2008 16:23
Corresponding Links:
Funders: Contract/grant sponsor: Deutsche Forschungsgemeinschaft and Fonds der Chemischen Industrie.
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