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.
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References
D. Knittel and R. Webster, in Proceedings of 5th International Conference Zirconium in the Nuclear Industry, ASTM, Philadelphia, p. 191 (1981).
R. Nielsen, Ullmann’s Encyclopedia of Industrial Chemistry (New York: Wiley, 2005), p. 268.
D.O. Northwood, Mater. Des. 6, 58 (1985).
B. Lustman and J.R. Frank Kerze, The Metallurgy of Zirconium (New York: McGraw-Hill, 1955), p. 19.
W. Kroll, A. Schlechten, and L. Yerkes, Trans. Electrochem. Soc. 89, 263 (1946).
W. Kroll, A. Schlechten, W. Carmody, L. Yerkes, H. Holmes, and H. Gilbert, Trans. Electrochem. Soc. 92, 99 (1947).
L. Xu, Y. Xiao, A. Van Sandwijk, Q. Xu, and Y.J. Yang, Nucl. Mater. 466, 21 (2015).
G.Z. Chen, D.J. Fray, and T.W. Farthing, Nature 407, 361 (2000).
Q.Y. Li, J.H. Du, and Z.P. Xi, Trans. Nonferr. Met. Soc. 17, 560 (2007).
J. Peng, K. Jiang, W. Xiao, D. Wang, X. Jin, and G.Z. Chen, Chem. Mater. 20, 7274 (2008).
D.J. Fray, T.W. Farthing, and G.Z. Chen, Int. Pat. 964, 638 (1999).
K.S. Mohandas and D.J. Fray, Trans. Indian Inst. Met. 57, 579 (2004).
P.S. Pershin, A.A. Kataev, A.A. Filatov, A.V. Suzdaltsev, and YuP Zaikov, Metall. Mater. Trans. B 48, 1962 (2017).
A.M. Abdelkader and E. El-Kashif, ISIJ Int. 47, 25 (2007).
M. Eshed, S. Pol, A. Gedanken, and M. Balasubramanian, Beilstein J. Nanotechnol. 2, 198 (2011).
K.T. Park, H.H. Nersisyan, B.S. Chun, and J.H. Lee, Mater. Res. 26, 16 (2011).
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).
ASTM international, Standard specification for zirconium sponge and other forms of virgin metal for nuclear application, B349/B348M-16.
J.P. Abriata, J. Garcés, and R. Versaci, Bull. Alloy Phase Diagr. 7, 116 (1986).
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).
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).
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The authors gratefully acknowledge the financial support from the CSU Start-up Fund and the Hunan Natural Science Fund for Distinguished Young Scholar (2019JJ20031).
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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
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DOI: https://doi.org/10.1007/s11837-019-03958-y