Croatica Chemica Acta, Vol. 71 No. 3, 1998.
Original scientific paper
XRD and Laser Raman Spectroscopy Investigation of the Stability of Low Temperature t-ZrO2
Goran Štefanić
; Ruđer Bošković Institute, P. O. Box 1016, 10001 Zagreb, Croatia
Svetozar Musić
; Ruđer Bošković Institute, P. O. Box 1016, 10001 Zagreb, Croatia
Biserka Gržeta
; Ruđer Bošković Institute, P. O. Box 1016, 10001 Zagreb, Croatia
Stanko Popović
; Department of Physics, Faculty of Science, University of Zagreb, P. O. Box 162, 10001 Zagreb, Croatia
Andreja Sekulić
; Ruđer Bošković Institute, P. O. Box 1016, 10001 Zagreb, Croatia
Abstract
The influence of precipitation pH and the presence of Na+ impurities on the stability of metastable t-ZrO2 were investigated. Zirconia samples with a high t-ZrO2 phase content were crystallized from zirconium hydroxide precipitated at pH 13, 7 and 2.5. The obtained samples were subjected to the influence of temperature, pressure and γ-irradiation. The influence of these treatments on the metastable t-ZrO2 were investigated using XRD and laser Raman spectroscopy. The results of phase analysis showed that the change in the pH of zirconium hydroxide precipitation significantly changed the sensitivity of the metastable t-ZrO2 to temperature and pressure. The metastable t-ZrO2 was most stable in the sample obtained from zirconium hydroxide precipitated at pH 2.5 and most unstable in the sample obtained from zirconium hydroxide precipitated at pH 7. The presence of Na+ impurities decreased the stability of metastable t-ZrO2. All the samples were shown to be stable under high γ-irradiation. The capability of laser Raman spectroscopy for the quantitative analysis was examined by comparing the values of the m-ZrO2 volume fraction (nm) obtained by this technique with the corresponding values obtained by XRD. It was concluded that the relation proposed by Clarke and Adar, J. Am. Ceram. Soc. 65 (1982) 284., was correct but the reliability of the m values estimated by the laser Raman spectroscopy was not high, especially in the region of 0.15 < nm < 0.70. The reason for the low reliability in this region is discussed.
Keywords
Hrčak ID:
132406
URI
Publication date:
1.10.1998.
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