Journal of Sol-Gel Science and Technology

, Volume 64, Issue 1, pp 251–256 | Cite as

Synthesis of submicrometer zirconium carbide formed from inorganic–organic hybrid precursor pyrolysis

  • Chunlei Yan
  • Rongjun Liu
  • Yingbin Cao
  • Changrui Zhang
  • Deke Zhang
Original Paper


Zirconium carbide (ZrC) was synthesized from inorganic–organic hybrid precursor’s pyrolysis by solution-based processing. Zirconium-containing complexes, which were obtained by chelation of oxide bidentate ligands to zirconium, were used to combine with phenolic resin to form precursors for ZrC. The precursors using specific ligands including acetylacetone, ethyleneglycol, and salicylic acid transformed into pure ZrC at a relatively low temperature (1,550 °C) in addition to that using lactic acid. As a comparison, synthesis of ZrC only using zirconium oxychloride octahydrate (ZrOCl2·8H2O) and phenolic resin was also conducted. The synthesized powders had a small average crystallite size (~300 nm), and a low oxygen content (~2.5 at.%). The conversions from as-synthesized preceramic precursors to ceramics were studied by means of FTIR, SEM, EDS, XRD, and XPS. The oxidation behavior of the synthesized ZrC in air was studied by DSC-TG analysis.


Zirconium carbide Inorganic–organic hybrid precursor Oxide bidentate ligand Carbothermal reduction 



This work was supported by the National Natural Science Foundation of China (No. 51102282).


  1. 1.
    Pierson HO (1996) Handbook of refractory carbides and nitrides. William Andrew Publishing/Noyes, WestwoodGoogle Scholar
  2. 2.
    Minato K, Ogawa T, Sawa K, Ishikawa A, Tomita T, Iida S, Sekino H (2000) Irradiation experiment on ZrC-coated fuel particles for high temperature gas-cooled reactors. Nucl Technol 130:272–281Google Scholar
  3. 3.
    Zhang XH, Qu Q, Han JC, Han WB, Hong CQ (2008) Microstructural features and mechanical properties of ZrB2-SiC-ZrC composites fabricated by hot pressing and reactive hot pressing. Scr Mater 59:753–756CrossRefGoogle Scholar
  4. 4.
    Zhao LY, Jia DC, Wang YJ, Rao JC, Yang ZH, Duan XM, Zhou Y (2010) ZrC-ZrB2 matrix composites with enhanced toughness prepared by reactive hot pressing. Scr Mater 63:887–890CrossRefGoogle Scholar
  5. 5.
    Li YT, Han WJ, Li H, Zhao JB, Zhao T (2012) Synthesis of nano-crystalline ZrB2/ZrC/SiC ceramics by liquid precursors. Mater Lett 68:101–103CrossRefGoogle Scholar
  6. 6.
    Dollé M, Gosset D, Bogicevic C, Karolak F, Simeone D, Baldinozzi G (2007) Synthesis of nanosized zirconium carbide by a sol–gel route. J Eur Ceram Soc 27:2061–2067CrossRefGoogle Scholar
  7. 7.
    Li RX, Zhang Y, Lou HJ, Li JP, Feng ZH (2011) Synthesis of ZrB2 nanoparticles by sol–gel method. J Sol–Gel Sci Technol 58:580–585CrossRefGoogle Scholar
  8. 8.
    Sacks MD, Wang CA, Yang ZH, Jain A (2004) Carbothermal reduction synthesis of nanocrystalline zirconium carbide and hafnium carbide powders using solution-derived precursors. J Mater Sci 39:6057–6066CrossRefGoogle Scholar
  9. 9.
    Yan YJ, Huang ZR, Liu XJ, Jiang DL (2007) Carbothermal synthesis of ultra-fine zirconium carbide powders using inorganic precursors via sol–gel method. J Sol–Gel Sci Technol 44:81–85CrossRefGoogle Scholar
  10. 10.
    Monteverde F, Bellosi A, Scatteia L (2008) Processing and properties of ultra-high temperature ceramics for space applications. Mater Sci Eng A 485:415–421CrossRefGoogle Scholar
  11. 11.
    Xie CM, Chen MW, Wei X, Ge M, Zhang WG (2012) Synthesis and microstructure of zirconium diboride formed from polymeric precursor pyrolysis. J Am Ceram Soc 95:866–869Google Scholar
  12. 12.
    Abe Y, Tomioka H, Gunji T, Nagao Y, Misono T (1994) A one-pot synthesis of polyzirconoxane as a precursor for continuous zirconia fibres. J Mater Sci Lett 13:960–962CrossRefGoogle Scholar
  13. 13.
    Liu HY, Hou XQ, Wang XQ, Wang YL, Xu D, Wang C, Du W, Lu MK, Yuan DR (2004) Fabrication of high-strength continuous zirconia fibers and their formation mechanism study. J Am Ceram Soc 87:2237–2241CrossRefGoogle Scholar
  14. 14.
    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 21:300–304Google Scholar
  15. 15.
    Abe Y, Kudo T, Tomioka H, Gunji T, Nagao Y, Misono T (1998) Preparation of continuous zirconia fibres from polyzirconoxane synthesized by the facile one-pot reaction. J Mater Sci 33:1863–1870CrossRefGoogle Scholar
  16. 16.
    Rodrigues-Filho UP, Gushikem Y, Goncalves MC, Cachichi RC, Castro SC (1996) Composite membranes of cellulose acetate and zirconium dioxide: preparation and study of physicochemical characteristics. Chem Mater 8:1375–1379CrossRefGoogle Scholar
  17. 17.
    Won YS, Kim YS, Varanasi VG, Kryliouka O, Andersona TJ, Sirimanne CT, McElwee-White L (2007) Growth of ZrC thin films by aerosol-assisted MOCVD. J Cryst Growth 304:324–332CrossRefGoogle Scholar
  18. 18.
    Roustila A, Chêne J, Séverac C (2003) XPS study of hydrogen and oxygen interactions on the surface of zirconium. J Alloys Compd 356–357:330–335CrossRefGoogle Scholar
  19. 19.
    Lee D, Choi H, Sim H, Choi D, Hwang H, Lee MJ, Seo SA, Yoo IK (2005) Resistance switching of the nonstoichiometric zirconium oxide for nonvolatile memory applications. IEEE Electron Device Lett 26:719–721CrossRefGoogle Scholar
  20. 20.
    Zhao HS, Liu B, Zhang KH, Tang CH (2011) Microstructure analysis of zirconium carbide layer on pyrocarbon-coated particles prepared by zirconium chloride vapor method. Nucl Eng Des. doi: 10.1016/j.nucengdes.2011.10.001 Google Scholar
  21. 21.
    Shimada S (2002) A thermoanalytical study on the oxidation of ZrC and HfC powders with formation of carbon. Solid State Ion 149:319–326CrossRefGoogle Scholar

Copyright information

© Springer Science+Business Media, LLC 2012

Authors and Affiliations

  • Chunlei Yan
    • 1
  • Rongjun Liu
    • 1
  • Yingbin Cao
    • 1
  • Changrui Zhang
    • 1
  • Deke Zhang
    • 1
  1. 1.National Key Laboratory of Science and Technology on Advanced Ceramic Fibers and Composites, College of Aerospace and Materials EngineeringNational University of Defense TechnologyChangshaChina

Personalised recommendations