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«Oxalate-precursor processing for high quality BaZrO3 Corresponding Author Nigel M. Kirby* Curtin University of Technology Department of Applied ...»

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4.0 Acknowledgments This work was supported by an Australian Postgraduate Award Scholarship and an Australian Institute of Nuclear Science and Engineering Postgraduate Research Award. We wish to acknowledge assistance provided by ANSTO Materials Division, and in particular David Cassidy for help with particle characterisation and thermal analysis. Thanks to Millennium Performance Chemicals for support of this project including supply of raw materials. Rojan Advanced Ceramics Ltd. provided CIP equipment and Michael Smirk of UWA Soil Science and Plant Nutrition assisted with XRF analysis.

References

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21. S.V. ELINSON, K.I. PETROV, Analytical Chemistry of Zirconium and Hafnium, 1969, Ann Arbor Humphrey Science Publishers, London.

22. N.M. KIRBY, A. VAN RIESSEN, C.E. BUCKLEY in “Proceedings of the 2001 Joint AXAA(WA) and WASEM Conference”, 2001, ISBN 0-9586039-2-8, 29.

23. Th. H. DE KEIJSER, J.I. LANGFORD, E.J. MITTEMEYER, A.B.P. VOGELS, J. Applied Crystallography, 1982, 15, 308.

24. N.M. KIRBY, Ph.D. Dissertation, 2003, Curtin University of Technology, Australia.

25. N.M. KIRBY, A. VAN RIESSEN, C.E. BUCKLEY, V.W. WITTORFF, A. TRANG, In preparation.

List of Table Captions Table 1 - Effect of reaction conditions on product stoichiometry for BaCl2, zirconium oxychloride, oxalic acid system using slow addition of reagents during precipitation.

List of Figure Captions Figure 1 - Effect of oxalate excess on product stoichiometry for BaCl2, zirconium oxychloride and oxalic acid system using 1:1 Ba:Zr solution mole ratio. Results for Riedel-de Haën ZrOCl2.8H2O are shown for comparison.

Figure 2 - Control of product stoichiometry in barium acetate, zirconium oxychloride, ammonium oxalate system at ambient temperature, using ammonium oxalate excess and small adjustment of Ba:[Zr+Hf] solution ratio.

Figure 3 – DTA/TGA analysis of precipitate with Ba : [Zr+ Hf] mole ratio = 1.005 ± 0.002.

Figure 4 – XRD of sample after calcination at 1300ºC for 1 hour Ba : [Zr+ Hf] for mole ratio =

0.986 ± 0.002. The expanded view shows the absence of detectable trace secondary phase peaks.

Figure 5 - Effect of calcination temperature on crystallite size and surface area of calcined powders at 0.989 ± 0.002 Ba:[Zr+Hf] mole ratio. Uncertainties are ±2σ.

Figure 6 – TEM micrographs of samples with Ba : [Zr+ Hf] for mole ratio = 0.986 ± 0.002 after calcination at a) 1350ºC for 60 minutes; scale bar = 50 nm, b) 1520ºC for 30 minutes; scale bar = 200 nm and c) 1520ºC for 30 minutes showing agglomeration of crystallites; scale bar = 100 nm.

Figure 7 - SEM micrograph of fracture surface of sintered ceramic showing fine grain size of ceramic. Scale bar = 5 µm.

–  –  –

30 -20 10 -30

-10 -40

–  –  –

Figure 6 a Figure 6b Figure 6c

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