Skip to main content
Log in

Two-Step Gradient Reduction of Zirconia for Making High-Purity Zirconium Powder

  • Technical Article
  • Published:
JOM Aims and scope Submit manuscript

Abstract

Ultra-high pure metallic zirconium powder was successfully obtained through a two-step gradient reduction of nano-ZrO2 in Ar atmosphere. The first reduction by Mg was to remove ~ 85% oxygen, followed by a heat-treatment step to control the particle size and specific surface area of the powder, and the final reduction by calcium was to further purify the powder and decrease oxygen to an extremely low level (0.068 wt.%). The oxygen level in the final powder meets the standard specification of Zr sponge (ASTM B349/B349M-16). Processing parameters, including the reduction temperature, the amount of Mg and MgCl2 and the heat treatment temperature, were investigated. Thermodynamic modeling with the assistance of HSC Chemistry software was carried out to understand the reduction reaction. This study offers a novel process for producing ultra-high pure metallic zirconium powder with the potential to replace the conventional Kroll process.

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

Access this article

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

Instant access to the full article PDF.

Fig. 1
Fig. 2
Fig. 3
Fig. 4
Fig. 5
Fig. 6
Fig. 7
Fig. 8

Similar content being viewed by others

References

  1. D. Knittel and R. Webster, in Proceedings of 5th International Conference Zirconium in the Nuclear Industry, ASTM, Philadelphia, p. 191 (1981).

  2. R. Nielsen, Ullmann’s Encyclopedia of Industrial Chemistry (New York: Wiley, 2005), p. 268.

    Google Scholar 

  3. D.O. Northwood, Mater. Des. 6, 58 (1985).

    Article  Google Scholar 

  4. B. Lustman and J.R. Frank Kerze, The Metallurgy of Zirconium (New York: McGraw-Hill, 1955), p. 19.

    Google Scholar 

  5. W. Kroll, A. Schlechten, and L. Yerkes, Trans. Electrochem. Soc. 89, 263 (1946).

    Article  Google Scholar 

  6. W. Kroll, A. Schlechten, W. Carmody, L. Yerkes, H. Holmes, and H. Gilbert, Trans. Electrochem. Soc. 92, 99 (1947).

    Article  Google Scholar 

  7. L. Xu, Y. Xiao, A. Van Sandwijk, Q. Xu, and Y.J. Yang, Nucl. Mater. 466, 21 (2015).

    Article  Google Scholar 

  8. G.Z. Chen, D.J. Fray, and T.W. Farthing, Nature 407, 361 (2000).

    Article  Google Scholar 

  9. Q.Y. Li, J.H. Du, and Z.P. Xi, Trans. Nonferr. Met. Soc. 17, 560 (2007).

    Google Scholar 

  10. J. Peng, K. Jiang, W. Xiao, D. Wang, X. Jin, and G.Z. Chen, Chem. Mater. 20, 7274 (2008).

    Article  Google Scholar 

  11. D.J. Fray, T.W. Farthing, and G.Z. Chen, Int. Pat. 964, 638 (1999).

    Google Scholar 

  12. K.S. Mohandas and D.J. Fray, Trans. Indian Inst. Met. 57, 579 (2004).

    Google Scholar 

  13. P.S. Pershin, A.A. Kataev, A.A. Filatov, A.V. Suzdaltsev, and YuP Zaikov, Metall. Mater. Trans. B 48, 1962 (2017).

    Article  Google Scholar 

  14. A.M. Abdelkader and E. El-Kashif, ISIJ Int. 47, 25 (2007).

    Article  Google Scholar 

  15. M. Eshed, S. Pol, A. Gedanken, and M. Balasubramanian, Beilstein J. Nanotechnol. 2, 198 (2011).

    Article  Google Scholar 

  16. K.T. Park, H.H. Nersisyan, B.S. Chun, and J.H. Lee, Mater. Res. 26, 16 (2011).

    Google Scholar 

  17. H. Nersisyan, B.U. Yoo, S.C. Kwon, D.Y. Kim, S.K. Han, J.H. Choi, and J.H. Lee, Combust. Flame 183, 22 (2017).

    Article  Google Scholar 

  18. ASTM international, Standard specification for zirconium sponge and other forms of virgin metal for nuclear application, B349/B348M-16.

  19. J.P. Abriata, J. Garcés, and R. Versaci, Bull. Alloy Phase Diagr. 7, 116 (1986).

    Article  Google Scholar 

  20. Y. Zhang, Z.Z. Fang, P. Sun, Y. Xia, M. Free, Z. Huang, H. Lefler, T.Y. Zhang, and J. Guo, Chem. Eng. J. 327, 169 (2017).

    Article  Google Scholar 

  21. Y. Zhang, Z.Z. Fang, Y. Xia, P. Sun, B. Van Devener, M. Free, H. Lefler, and S. Zheng, Chem. Eng. J. 308, 299 (2017).

    Article  Google Scholar 

Download references

Acknowledgements

The authors gratefully acknowledge the financial support from the CSU Start-up Fund and the Hunan Natural Science Fund for Distinguished Young Scholar (2019JJ20031).

Author information

Authors and Affiliations

Authors

Corresponding authors

Correspondence to Yang Xia or Xueyi Guo.

Additional information

Publisher's Note

Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations.

Rights and permissions

Reprints and permissions

About this article

Check for updates. Verify currency and authenticity via CrossMark

Cite this article

Xia, Y., Zhao, J., Dong, Z. et al. Two-Step Gradient Reduction of Zirconia for Making High-Purity Zirconium Powder. JOM 72, 1687–1693 (2020). https://doi.org/10.1007/s11837-019-03958-y

Download citation

  • Received:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s11837-019-03958-y

Navigation