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Synthesis, characterization, and ceramization of a SiC–ZrC–C preceramic polymer precursor

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Abstract

A silicon- and zirconium-containing polymer precursor (PSZC) for SiC–ZrC–C ceramic was successfully synthesized by chemical reaction of phenol, paraformaldehyde, tetraethoxysilane, acetylacetone, and ZrOCl2·8H2O. The chemical structure, pyrolysis behaviors, and pyrolysis products of PSZC were characterized by the combination of FT-IR, 1H-NMR, TG-DTG, XRD, Raman, SEM, and EDS. It indicates that the obtained PSZC might be Zr–O–Zr and Si–O–Si chain polymer connected by Si–O–Zr bond with hydroxymethyl phenol and acetylacetone as ligands. And the most probable reaction mechanism to form PSZC was proposed. Decomposition of PSZC is completed at 800 °C, and it gives amorphous carbon, SiO2, and ZrO2 with a yield of 70 %. During heat treatment, SiC forms at about 1500 °C, followed by the appearance of ZrC. Defects of the carbon are cumulated to the highest at 1500 °C. Further heating at 1800 °C induces highly crystallized ZrC, SiC ceramic, and structure-ordered carbon with a structure of ZrC and SiC particles uniformly distributed in the carbon matrix.

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References

  1. Cheng GW (2013) An inorganic–organic hybrid precursor strategy for the synthesis of zirconium diboride powders. Int J Refract Met Hard Mater 36:149–153

    Article  Google Scholar 

  2. Li ZQ, Li HJ, Li W, Zhang SY, W J, Guo J (2011) Preparation and ablation properties of ZrC–SiC coating for carbon/carbon composites by solid phase infiltration. Appl Surf Sci 258:565–571

    Article  Google Scholar 

  3. Zhao D, Hu HF, Zhang CR, Zhang YD, Wang J (2010) A simple way to prepare precursors for zirconium carbide. J Mater Sci 45:6401–6405. doi:10.1007/s10853-010-4722-y

    Article  Google Scholar 

  4. Zhu SM, Ding SQ, Xi HA, Wang RD (2005) Low-temperature fabrication of porous SiC ceramics by preceramic polymer reaction bonding. Mater Lett 59:595–597

    Article  Google Scholar 

  5. Li HB, Zhang LT, Cheng LF, Yu ZJ, Huang MH, Tu HB, Xia HP (2009) Effect of curing and pyrolysis processing on the ceramic yield of a highly branched polycarbosilane. J Mater Sci 44:721–725. doi:10.1007/s10853-008-3176-y

    Article  Google Scholar 

  6. Wang YG, Zhu XJ, Zhang LT, Cheng LF (2011) Reaction kinetics and ablation properties of C/C–ZrC composites fabricated by reactive melt infiltration. Ceram Int 37:1277–1283

    Article  Google Scholar 

  7. Yu ZJ, Yang L, Zhan JY, Zhou C, Min H, Zheng Q, Xia HP (2012) Preparation, cross-linking and ceramization of AHPCS/Cp2ZrCl2 hybrid precursors for SiC/ZrC/C composites. J Eur Ceram Soc 32:1291–1298

    Article  Google Scholar 

  8. Li QG, Zhou HJ, Dong SM, Wang Z, He P, Yang JS, Wu B, Hu JB (2012) Fabrication of a ZrC–SiC matrix for ceramic matrix composites and its properties. Ceram Int 38:4379–4384

    Article  Google Scholar 

  9. Xie J, Li KZ, Li HJ, Fu QG, Guo LJ (2013) Ablation behavior and mechanism of C/C–ZrC–SiC composites under an oxyacetylene torch at 3000 °C. Ceram Int 39:4171–4178

    Article  Google Scholar 

  10. Guo SQ, Kagawa Y, Nishimura T, Chung D, Yang JM (2008) Mechanical and physical behavior of spark plasma sintered ZrC–ZrB2–SiC composites. J Eur Ceram Soc 28:1279–1285

    Article  Google Scholar 

  11. Tao XY, Qiu WF, Li H, Zhao T (2010) Synthesis of nanosized zirconium carbide from preceramic polymers by the facile one-pot reaction. Polym Adv Technol 21:300–304

    Google Scholar 

  12. Li YT, Han WJ, Li H, Zhao JB, Zhao T (2012) Synthesis of nano-crystalline ZrB2/ZrC/SiC ceramics by liquid precursors. Mater Lett 68:101–103

    Article  Google Scholar 

  13. Li QG, Zhou HJ, Dong SM, Wang Z, Yang JS, Wu B, Hu JB (2012) Fabrication and comparison of 3D Cf/ZrC–SiC composites using ZrC particles/polycarbosilane and ZrC precursor/polycarbosilane. Ceram Int 38:5271–5275

    Article  Google Scholar 

  14. Pizon D, Lucas R, Chehaidi Foucaud S, Maitre A (2011) From trimethylvinylsilane to ZrC–SiC hybrid materials. J Eur Ceram Soc 31:2687–2690

    Article  Google Scholar 

  15. Liu CQ, Li KZ, Li HJ, Zhang SY, Zhang YL (2014) Preparation and characterization of zirconium-containing ceramic precursor used for impregnation. Acta Polym Sin 1:56–62

    Google Scholar 

  16. Chiang CL, Ma CCM (2004) Synthesis, characterization, thermal properties and flame retardance of novel phenolic resin/silica nanocomposites. Polym Degrad Stab 83:207–214

    Article  Google Scholar 

  17. Tao XY, Qiu WF, Li H, Zhao T, Wei XY (2012) New route to synthesize preceramic polymers for zirconium carbide. Chin Chem Lett 9:1075–1078

    Article  Google Scholar 

  18. Liu CQ, Li KZ, Li HJ, Zhang SY, Zhang YL, Wang B (2014) Synthesis, characterization and ceramization of a carbon-rich zirconium-containing precursor for ZrC ceramic. Ceram Int 40:7285–7292

    Article  Google Scholar 

  19. Wang MC, Yang LJ, Yu CD, Xu CB (2012) Liquid poly(silylacetylene)siloxane resin as a novel precursor of silicon carbide and silicon oxycarbide ceramics. Ceram Int 38:2559-2454

    Google Scholar 

  20. Li HB, Zhang LT, Cheng LF, Wang YG, Yu ZJ, Huang MH, Tu HB, Xia HP (2008) Polymer–ceramic conversion of a highly branched liquid polycarbosilane for SiC-based ceramics. J Mater Sci 43:2806–2811. doi:10.1007/s10853-008-2539-8

    Article  Google Scholar 

  21. Ivanova Y, Gerganova TS, Dimitriev Y, Miranda Salvado IM, Fernandes MHV (2006) Nanostructured hybrid materials as precursors for synthesis of nanocoposites in Si–O–C–N–Zr system. Thin Solid Films 515:271–278

    Article  Google Scholar 

  22. Kongwudthiti S, Praserthdam P, Tanakulrungsank W, Inoue M (2003) The influence of Si–O–Zr bonds on the crystal-growth inhibition of zirconia prepared by the glycothermal method. J Mater Process Technol 136:186–189

    Article  Google Scholar 

  23. Li HB, Zhang LT, Cheng LF, Wang YG, Yu ZJ, Huang MH, Tu HB, Xia HP (2008) Effect of the polycarbosilane structure on its final ceramic yield. J Eur Ceram Soc 28:887–891

    Article  Google Scholar 

  24. Fang YH, Huang MH, Yu ZJ, Xia HP, Chen LF, Zhang Y, Zhang LT (2008) Synthesis, characterization, and pyrolytic conversion of a novel liquid polycarbosilane. J Am Ceram Soc 91:3298–3302

    Article  Google Scholar 

  25. Hua YS, Chen L, Li XF, Gao MJ, MS R, Sun JL (2011) Electrochemical synthesis and characterization of polysilane with zirconium. Acta Polym Sin 6:596–600

    Article  Google Scholar 

  26. Zhou DF, Zhao YL, Hao J, Ma Y, Zhang XY, Su ZM, Wang RS (2013) Effect of ZnCl2 doping on the structure and properties of carbonized phenolic resin material. Chem J Chin U 12:2296–2299

    Google Scholar 

  27. Casiraghi C, Pisana S, Novoselov KS, Geim AK, Ferrari AC (2007) Raman fingerprint of charged impurities in grapheme. Appl Phys Lett 91:233-108

    Article  Google Scholar 

Download references

Acknowledgements

This work has been supported by the National Natural Science Foundation of China under Grant No. 51272213, 51221001, 51202093 and 51402238, and supported by the “111“ project under grant No. B08040 and the Research Fund of the State Key Laboratory of Solidification Processing (NWPU), China (Grant No. 73-QP-2010).

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Authors and Affiliations

  1. State Key Laboratory of Solidification Processing, Carbon/Carbon Composites Research Center, Northwestern Polytechnical University, Xi’an, 710072, People’s Republic of China

    Changqing Liu, Kezhi Li, Hejun Li, Shouyang Zhang & Yulei Zhang

  2. Mechanics, Materials and Structures Research Division, Faculty of Engineering, The University of Nottingham, Nottingham, NG7 2RD, UK

    Xianghui Hou

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  1. Changqing Liu
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  2. Kezhi Li
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  3. Hejun Li
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  4. Shouyang Zhang
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  5. Yulei Zhang
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  6. Xianghui Hou
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Correspondence to Kezhi Li.

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Liu, C., Li, K., Li, H. et al. Synthesis, characterization, and ceramization of a SiC–ZrC–C preceramic polymer precursor. J Mater Sci 50, 2824–2831 (2015). https://doi.org/10.1007/s10853-015-8840-4

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  • DOI: https://doi.org/10.1007/s10853-015-8840-4

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