Advertisement

Springer Nature is making SARS-CoV-2 and COVID-19 research free. View research | View latest news | Sign up for updates

Carbothermal nitridation synthesis of α-Si3N4 powder from pyrolysed rice hulls

Abstract

The carbothermal nitridation synthesis of α-Si3N4 was studied using a high-temperature tube furnace to react a precursor, comprised of pyrolysed rice hulls (C/SiO2) and additive “seed” Si3N4, with N2. The experimental design for synthesis was a three-level factorial surface response design for determining the effect of temperature (1300–1380°C) and reaction time (1–5 h) on kinetics. In addition, all precursors were reacted at 1460, 1480 and 1500°G for 5 h in order to ensure high conversion suitable for product powder evaluation (composition and morphology). Following excess carbon removal, the product Si3N4 was >95% α-phase and had a surface area of 7.7 m2g−1 with an oxygen content of 3.6 wt% O. The powder was comprised of a bimodal size distribution of submicrometre solid α-Si3N4 crystallites centred at 0.03 and 0.22 μm. No whiskers or high aspect ratio elongated crystallites were found in the powder. The addition of carbon black to the seeded pyrolysed rice hull C/SiO2 mixture had no significant impact on the reaction rate or product powder properties. The reaction was modelled using a nuclei-growth rate expression as

$$\begin{gathered} (kt)^{0.58} = - ln(1 --- X) \hfill \\ k = 1.09 \times 10^{10} exp (--- 50502/T) \hfill \\ \end{gathered} $$

k=1.09×1010 exp (−50502/T) where (1573 K<T<1653 K), (3600<t<18000 s), (0<X<1), andk=rate in s−1.

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

References

  1. 1.

    T. Quadir, R. W. Rice, J. C. Chakraverty, J. A. Breindel, andC. C. Wu,Ceram. Eng. Sci. Proc. 12 (1991) 1952.

  2. 2.

    B. K. Padhi andC. Patnaik,Ceram. Int. 21 (1995) 213.

  3. 3.

    K. Satyanarayana,Res. Ind. 35(12) (1990) 223.

  4. 4.

    D. F. Houston, “Rice Chemistry and Technology” (American Association of Cereal Chemistry, St Paul, MN, 1972) p. 301.

  5. 5.

    S. B. Hanna, N. A. L. Mansour, A. S. Taha andH. M. A. Abd-Allah,Br. Ceram. Trans. J. 84 (1985) 18.

  6. 6.

    S.-W. Kang andS.-S. Chun,J. Kor. Ceram. Soc. 16(2) (1979) 99.

  7. 7.

    N. Kuskonmaz, C. Toy, O. Addemir andA. Tekin, in “Third Euro-Ceramics”, Vol. 1, edited by P. Duran and J. F. Fernandez (Faenza Editrice Iberica, S. L., Spain, 1993) pp. 125–30.

  8. 8.

    J. G. Lee andI. B. Cutler,Am. Ceram. Soc. Bull. 54(2) (1975) 195.

  9. 9.

    Y. Li, L. Liu andS. Dou,J. Inorg. Mater. (Wuji Cailiao Xuebao — Chinese) 6(1) (1991) 45.

  10. 10.

    N. A. L. Mansour andS. B. Hanna,Br. Ceram. Soc. Trans. J. 68(6) (1979) 132.

  11. 11.

    M. Patel andP. Prasanna,Interceram. 40 (1991) 301.

  12. 12.

    I. A. Rahman andF. L. Riley,J. Eur. Ceram. Soc. 5 (1989) 11.

  13. 13.

    R. F. Rodriguez andR. F. J. Narciso,Anal. Quim. 87 (1991) 788.

  14. 14.

    N. K. Sharma andW. S. Williams,J. Am. Ceram. Soc. 67 (1984) 715.

  15. 15.

    J. C. Russ, “Computer-Assisted Microscopy: The Measurement and Analysis of Images” (Plenum Press, New York, 1990).

  16. 16.

    M. Tsukada, J. Naito, T. Masuda andM. Horio,Funtai Kogaku Kaishi 26(3) (1989) 157.

  17. 17.

    M. Avrami,J. Chem. Phys. 7 (1939) 1103.

  18. 18.

    Idem, ibid. 8 (1940) 212.

  19. 19.

    Idem, ibid. 9 (1941) 177.

  20. 20.

    F. C. Tompkins, in “Treatise on Solid State Chemistry”, Vol. 4, “Reactivity of Solids”, edited by N. B. Hannay (Plenum Press, New York, 1976) p. 206.

  21. 21.

    B. V. Erofeyev,C.R. Acad. Sci. URSS 52 (1946) 511.

  22. 22.

    Z. Strnad, “Glass-Ceramic Materials: Liquid Phase Separation, Nuleation and Crystallization in Glasses” (Elsevier, New York, 1986).

  23. 23.

    A. W. Weimer, G. A. Eisman, D. W. Susnitzky, J. W. McCoy andD. R. Beaman,J. Am. Ceram. Soc. (1996) in press.

Download references

Author information

Correspondence to A. W. Weimer.

Rights and permissions

Reprints and Permissions

About this article

Cite this article

Weimer, A.W., Cassiday, J.R., Susnitzky, D.W. et al. Carbothermal nitridation synthesis of α-Si3N4 powder from pyrolysed rice hulls. J Mater Sci 31, 6005–6013 (1996). https://doi.org/10.1007/BF01152152

Download citation

Keywords

  • Hull
  • Surface Response
  • High Aspect Ratio
  • Rate Expression
  • Tube Furnace