Investigation of the Pyrolysis and Crystallization of Lead Zirconate Titanate Ceramics Prepared via the Sol Gel Process

Jens Brieger, Rotraut Merkle, Helmut Bertagnolli, Klaus Müller
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引用次数: 5

Abstract

The sol gel process for the preparation of lead zirconate, lead titanate and lead zirconate titanate is studied by various experimental techniques, comprising solid state NMR methods, FT IR spectroscopy, DTA/TG and XRD. Two temperature ranges are examined that cover (i) the pyrolysis step from the solid gel to the amorphous oxide mixture and (ii) the calcination step from the amorphous state to the crystalline ceramics. 13C NMR and FT IR spectroscopy studies primarily are used to monitor the structural changes during the pyrolysis step. 207Pb NMR spectroscopy is employed to examine the development of the short range order at the lead nuclei over the whole temperature range. The latter studies clearly show that the observed changes in the short range order are accompanied by alterations in the long range order, as derived from the XRD data. In addition, 207Pb NMR experiments are performed on ceramic samples that were obtained via the sol gel or the mixed oxide route. It is demonstrated that these samples exhibit significant differences in the short range order, although the long range order was found to be the same, being independent of the actual preparation route.

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溶胶-凝胶法制备锆钛酸铅陶瓷的热解结晶研究
采用固体核磁共振、红外光谱、DTA/TG和XRD等实验技术,研究了溶胶-凝胶法制备锆酸铅、钛酸铅和锆酸铅钛酸盐的工艺。研究了两个温度范围,包括(i)从固体凝胶到非晶态氧化物混合物的热解步骤和(ii)从非晶态到结晶陶瓷的煅烧步骤。13C核磁共振和红外光谱研究主要用于监测热解过程中的结构变化。采用207Pb核磁共振波谱法研究了铅核在整个温度范围内的短程序的发展。后者的研究清楚地表明,从XRD数据中可以看出,观察到的近程变化伴随着远程变化。此外,还对溶胶-凝胶法和混合氧化物法制备的陶瓷样品进行了207Pb核磁共振实验。结果表明,这些样品在近程顺序上表现出显著的差异,尽管发现长距离顺序是相同的,与实际制备路线无关。
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