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Synthesis and Characterization of a Carborane-containing Precursor for B4C Ceramics

Received: 15 April 2021    Accepted:     Published: 24 May 2021
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Abstract

B4C ceramic is one of widely used ceramics with properties of low density, high hardness, high thermal-stability and high neutron absorption cross-section. However, the high melting point and high hardness of B4C make it difficult to be prepared as materials with complex shape. Precursor derived method is an effective approach to prepare special-shaped ceramics. In the early research of B4C ceramic precursors, highly toxic and unstable decaborane was generally used as the boron source material, and precursors were also unstable and difficult to synthesize. In this work, a new B4C precursor is designed and synthesized, and m-carborane, which has stable chemical properties and high thermal stability, is used as the boron source. Firstly, m-carborane is converted into lithium salt after removing active hydrogen by n-butyllithium. Then, catalyzed by Cu(I), the lithium salt reacts with m-chloroiodobenzene so that monomer, bis(3-chlorophenyl)-m-carborane, is prepared. The monomer is polymerized through Ullmann Coupling reaction at the present of Ni(0) catalyst and Zinc powder, and precursor poly[bis(3-chlorophenyl)-m-carborane] is finally synthesized. The precursor is stable at room temperature in air and soluble in Tetrahydrofuran, with Mw of 1013g/mol, and ceramic yield of 62.20% at 900°C in N2. The precursor pyrolytic product is composed of B4C and graphite after heat treated at 1600°C in inert atmosphere.

Published in Science Discovery (Volume 9, Issue 3)
DOI 10.11648/j.sd.20210903.18
Page(s) 128-132
Creative Commons

This is an Open Access article, distributed under the terms of the Creative Commons Attribution 4.0 International License (http://creativecommons.org/licenses/by/4.0/), which permits unrestricted use, distribution and reproduction in any medium or format, provided the original work is properly cited.

Copyright

Copyright © The Author(s), 2021. Published by Science Publishing Group

Keywords

Precursor, Carborane, B4C

References
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[13] Xiaojuan Zhang, Jing Li, Ke Cao, et al. Synthesis and characterization of B–C polymer hollow microspheres from a new organodecaborane preceramic polymer [J]. Rsc Advances, 2015, 5:86214-86218.
[14] Pender, Mark, J., et al. Transition-Metal-Promoted Reactions of Boron Hydrides. 17. Titanium-Catalyzed [J]. Journal of the American Chemical Society, 2001, 123(49): 12222-12222.
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  • APA Style

    Dexuan Yan, Jiahui Chen, Yu Zhang, Yanzi Gou. (2021). Synthesis and Characterization of a Carborane-containing Precursor for B4C Ceramics. Science Discovery, 9(3), 128-132. https://doi.org/10.11648/j.sd.20210903.18

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    ACS Style

    Dexuan Yan; Jiahui Chen; Yu Zhang; Yanzi Gou. Synthesis and Characterization of a Carborane-containing Precursor for B4C Ceramics. Sci. Discov. 2021, 9(3), 128-132. doi: 10.11648/j.sd.20210903.18

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    AMA Style

    Dexuan Yan, Jiahui Chen, Yu Zhang, Yanzi Gou. Synthesis and Characterization of a Carborane-containing Precursor for B4C Ceramics. Sci Discov. 2021;9(3):128-132. doi: 10.11648/j.sd.20210903.18

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  • @article{10.11648/j.sd.20210903.18,
      author = {Dexuan Yan and Jiahui Chen and Yu Zhang and Yanzi Gou},
      title = {Synthesis and Characterization of a Carborane-containing Precursor for B4C Ceramics},
      journal = {Science Discovery},
      volume = {9},
      number = {3},
      pages = {128-132},
      doi = {10.11648/j.sd.20210903.18},
      url = {https://doi.org/10.11648/j.sd.20210903.18},
      eprint = {https://article.sciencepublishinggroup.com/pdf/10.11648.j.sd.20210903.18},
      abstract = {B4C ceramic is one of widely used ceramics with properties of low density, high hardness, high thermal-stability and high neutron absorption cross-section. However, the high melting point and high hardness of B4C make it difficult to be prepared as materials with complex shape. Precursor derived method is an effective approach to prepare special-shaped ceramics. In the early research of B4C ceramic precursors, highly toxic and unstable decaborane was generally used as the boron source material, and precursors were also unstable and difficult to synthesize. In this work, a new B4C precursor is designed and synthesized, and m-carborane, which has stable chemical properties and high thermal stability, is used as the boron source. Firstly, m-carborane is converted into lithium salt after removing active hydrogen by n-butyllithium. Then, catalyzed by Cu(I), the lithium salt reacts with m-chloroiodobenzene so that monomer, bis(3-chlorophenyl)-m-carborane, is prepared. The monomer is polymerized through Ullmann Coupling reaction at the present of Ni(0) catalyst and Zinc powder, and precursor poly[bis(3-chlorophenyl)-m-carborane] is finally synthesized. The precursor is stable at room temperature in air and soluble in Tetrahydrofuran, with Mw of 1013g/mol, and ceramic yield of 62.20% at 900°C in N2. The precursor pyrolytic product is composed of B4C and graphite after heat treated at 1600°C in inert atmosphere.},
     year = {2021}
    }
    

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  • TY  - JOUR
    T1  - Synthesis and Characterization of a Carborane-containing Precursor for B4C Ceramics
    AU  - Dexuan Yan
    AU  - Jiahui Chen
    AU  - Yu Zhang
    AU  - Yanzi Gou
    Y1  - 2021/05/24
    PY  - 2021
    N1  - https://doi.org/10.11648/j.sd.20210903.18
    DO  - 10.11648/j.sd.20210903.18
    T2  - Science Discovery
    JF  - Science Discovery
    JO  - Science Discovery
    SP  - 128
    EP  - 132
    PB  - Science Publishing Group
    SN  - 2331-0650
    UR  - https://doi.org/10.11648/j.sd.20210903.18
    AB  - B4C ceramic is one of widely used ceramics with properties of low density, high hardness, high thermal-stability and high neutron absorption cross-section. However, the high melting point and high hardness of B4C make it difficult to be prepared as materials with complex shape. Precursor derived method is an effective approach to prepare special-shaped ceramics. In the early research of B4C ceramic precursors, highly toxic and unstable decaborane was generally used as the boron source material, and precursors were also unstable and difficult to synthesize. In this work, a new B4C precursor is designed and synthesized, and m-carborane, which has stable chemical properties and high thermal stability, is used as the boron source. Firstly, m-carborane is converted into lithium salt after removing active hydrogen by n-butyllithium. Then, catalyzed by Cu(I), the lithium salt reacts with m-chloroiodobenzene so that monomer, bis(3-chlorophenyl)-m-carborane, is prepared. The monomer is polymerized through Ullmann Coupling reaction at the present of Ni(0) catalyst and Zinc powder, and precursor poly[bis(3-chlorophenyl)-m-carborane] is finally synthesized. The precursor is stable at room temperature in air and soluble in Tetrahydrofuran, with Mw of 1013g/mol, and ceramic yield of 62.20% at 900°C in N2. The precursor pyrolytic product is composed of B4C and graphite after heat treated at 1600°C in inert atmosphere.
    VL  - 9
    IS  - 3
    ER  - 

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Author Information
  • Science and Technology on Advanced Ceramic Fibers and Composites Laboratory, National University of Defense Technology, Changsha, China

  • Science and Technology on Advanced Ceramic Fibers and Composites Laboratory, National University of Defense Technology, Changsha, China

  • Science and Technology on Advanced Ceramic Fibers and Composites Laboratory, National University of Defense Technology, Changsha, China

  • Science and Technology on Advanced Ceramic Fibers and Composites Laboratory, National University of Defense Technology, Changsha, China

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