Skip to main content
SpringerLink
Log in

Synthesis of nanozirconooligocarbosilanes

  • Published:
Inorganic Materials Aims and scope

Abstract

We describe the first chlorine-free synthesis of nanozirconooligocarbosilanes through thermal cocondensation of low-molecular oligocarbosilanes and zirconium tetrakis(diethylamide). The starting reagents, reaction intermediates, and final products have been characterized by 1H, 13C, and 29Si nuclear magnetic resonance, UV and IR spectroscopy, gel-permeation chromatography, thermogravimetry, transmission electron microscopy (TEM), and elemental analysis. The synthesized nanozirconooligocarbosilanes have been used to fabricate ceramic fibers and matrices through thermal and chemical processing. TEM results demonstrate that the particles of zirconium and products of its reactions with silicon, carbon, and nitrogen range in size from 10 to 20 nm in the oligomers and from 20 to 30 nm in the ceramics.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Log in via an institution

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Institutional subscriptions

Similar content being viewed by others

References

  1. Storozhenko, P.A., Tsirlm, A.M., Gubin, S.P., et al., Novel Oxygen-Free Preceramic Polymers: Nanometallopolycarbosilanes and Nanoparticulate Fillers—Unique Materials for Enhancing the Strength and Oxidation Resistance of Carbon-Graphite Composites and Stabilizing High-Strength High-Temperature Ceramics, Membrany, Ser. Krit. Tekhnol., 2005, vol. 28, no. 4, pp. 68–74.

    Google Scholar 

  2. Yajima, S, in Handbook of Composites, vol. 1: Strong Fibers, Watt, W. and Perov, B.V., Eds., Amsterdam: North-Holland, 1985, pp. 201–237.

    Google Scholar 

  3. Gubin, S.P. and Kosobudsky, I.D., Metallic Clusters in Polymer Matrices: A New Type of Metal-Filled Polymers, Vysokomol. Soed., 1985, vol. 27, no. 3, pp. 689–695.

    Google Scholar 

  4. Gubin, S.P., Yurkov, G.Yu., and Kosobudsky, I.D., Nanomaterials Based on Metal-Containing Nanoparticles in Polyethylene and Other Carbon-Chain Polymers, Int. J. Mater. Prod. Technol., 2005, vol. 23, no. 1/2, pp. 2–25.

    CAS  Google Scholar 

  5. Tsirlin, A.M., Popova, N.A., Florina, E.K., et al., RF Patent 2125 579, 1999.

  6. Gubin, S., Moroz, E., Boronin, A., et al., Nanoparticles of Ti and Zr in Organosilicon Polymer Ceramic Precursors, Mendeleev Commun., 1999, no. 2, pp. 59–61.

  7. Gubin, S.P., Tsirlin, A.M., Popova, N.A., et al., Clusters in a Polymer Matrix: IV. Zr-and Ti-Containing Nanoparticles Formed during the Transformation of Oligosilacarbosilane into Poly(carbosilane): Structure and Interaction with the Matrix, Neorg. Mater., 2001, vol. 37, no. 11, pp. 1317–1326 [Inorg. Mater. (Engl. Transl.), vol. 37, no. 11, pp. 1121–1129].

    Article  Google Scholar 

  8. Tsirlin, A.M., Scherbakova, G.I., Florina, E.K., et al., Nano-structured Metal Containing Polymer Precursors for High Temperature Non-oxide Ceramics and Ceramic Fibers—Syntheses, Pyrolyses, and Properties, J. Eur. Ceram. Soc., 2002, vol. 22, pp. 2577–2585.

    Article  CAS  Google Scholar 

  9. Yajima, S., Hasegawa, Y., Hayashi, J., and Iimura, M., Synthesis of Continuous Silicon Carbide Fibre with High Tensile Strength and High Young’s Modulus, Synthesis of Polycarbosilane as Precursor, J. Mater. Sci. 1978, vol. 13, pp. 2569–2576.

    Article  CAS  Google Scholar 

  10. Shcherbakova, G.I., Tsirlin, A.M., Florina, E.K., et al., Polycondensation of Oligocarbosilanes in the Presence of Zircomum Tetrakis(diethylamide), XVII Mendeleevskii s”ezd po obshchei i prikladnoi khimii (XVII Mendeleev Meet., General and Applied Chemistry), Kazan, 2003, vol. 2, p. 448.

    Google Scholar 

  11. Shcherbakova, G.I., Tsirlin, A.M., Storozhenko, P.A., et al., Organosilicon Nanometallopolymers for SiC/SiC Composites, X Vserossiiskaya konferentsiya “Kremniiorganicheskie soedineniya: sintez, svoistva, primenenie” (X All-Russia Conf. Organosilicon Compounds: Synthesis, Properties, and Applications), Moscow, 2005, p. 28.

  12. Tsirlin, A.M., Shcherbakova, G.I., Florina, E.K., et al., RF Patent 2258715, 2005.

  13. Bradley, D.C., and Thomas, I.M., Metallo-organic Compounds Containing Metal-Nitrogen Bonds: Part 1. Some Dialkylamino-Derivatives of Titanium and Zirconium, J. Chem. Soc., 1960, pp. 3857–3861.

  14. Tsirlin, A.M., Fedorova, T.V., Florina, E.K., et al., RF Patent 2108 348, 1998.

  15. Andrianov, K.A., Metody elementoorganicheskoi khimii. Kremnii (Methods of Organoelement Chemistry: Silicon), Moscow: Nauka, 1968, pp. 11–13.

    Google Scholar 

  16. Bradley, D.C. and Chisholm, M.H., Transition-Metal Dialkylamides and Disilylamides, Acc. Chem. Res., 1976, vol. 9, pp. 273–280.

    Article  CAS  Google Scholar 

  17. Thomas, I.M., The Preparation of Alkoxides and Triethylsilanolates of Ti, Zr, V, Nb, Ta, and Sn from the Dialkylamides, Can. J. Chem., 1961, vol. 39, pp. 1386–1388.

    Article  CAS  Google Scholar 

  18. Nugent, W.A., Ovenal, D.W., and Holmes, S.J., Catalytic C-H Activation in Early Transition-Metal Dialkylamides and Alkoxides, Organometallics, 1983, vol. 2, pp. 161–162.

    Article  CAS  Google Scholar 

Download references

Author information

Authors and Affiliations

  1. State Research Institute of Chemistry and Technology of Organoelement Compounds, sh. Entuziastov 38, Moscow, 111123, Russia

    P. A. Storozhenko, G. I. Shcherbakova, A. M. Tsirlin, E. K. Florina, E. A. Izmailova, A. A. Savitskii, M. G. Kuznetsova, T. M. Kuznetsova & I. V. Stolyarova

  2. Kurnakov Institute of General and Inorganic Chemistry, Russian Academy of Sciences, Leninskii pr. 31, Moscow, 119991, Russia

    G. Yu. Yurkov & S. P. Gubin

Authors
  1. P. A. Storozhenko
    View author publications

    You can also search for this author in PubMed Google Scholar

  2. G. I. Shcherbakova
    View author publications

    You can also search for this author in PubMed Google Scholar

  3. A. M. Tsirlin
    View author publications

    You can also search for this author in PubMed Google Scholar

  4. E. K. Florina
    View author publications

    You can also search for this author in PubMed Google Scholar

  5. E. A. Izmailova
    View author publications

    You can also search for this author in PubMed Google Scholar

  6. A. A. Savitskii
    View author publications

    You can also search for this author in PubMed Google Scholar

  7. M. G. Kuznetsova
    View author publications

    You can also search for this author in PubMed Google Scholar

  8. T. M. Kuznetsova
    View author publications

    You can also search for this author in PubMed Google Scholar

  9. I. V. Stolyarova
    View author publications

    You can also search for this author in PubMed Google Scholar

  10. G. Yu. Yurkov
    View author publications

    You can also search for this author in PubMed Google Scholar

  11. S. P. Gubin
    View author publications

    You can also search for this author in PubMed Google Scholar

Additional information

Original Russian Text © P.A. Storozhenko, G.I. Shcherbakova, A.M. Tsirlin, E.K. Florina, E.A. Izmailova, A.A. Savitskii, M.G. Kuznetsova, T.M. Kuznetsova, I.V. Stolyarova, G.Yu. Yurkov, S.P. Gubin, 2006, published in Neorganicheskie Materialy, 2006, Vol. 42, No. 10, pp. 1269–1277.

Rights and permissions

Reprints and permissions

About this article

Cite this article

Storozhenko, P.A., Shcherbakova, G.I., Tsirlin, A.M. et al. Synthesis of nanozirconooligocarbosilanes. Inorg Mater 42, 1159–1167 (2006). https://doi.org/10.1134/S0020168506100190

Download citation

  • Received:

  • Issue Date:

  • DOI: https://doi.org/10.1134/S0020168506100190

Keywords

Search

Navigation