Structure Evolution in the PbO-ZrO2-TiO2 Sol-Gel System: Part I - Characterization of Prehydrolyzed Precursors

被引:29
作者
Coffman, P. R. [1 ,2 ]
Dey, S. K. [1 ,2 ]
机构
[1] Arizona State Univ, Adv Ceram Proc Lab, Dept Chem, Tempe, AZ 85287 USA
[2] Arizona State Univ, Adv Ceram Proc Lab, Dept Chem Bio & Mat Engn, Tempe, AZ 85287 USA
基金
美国国家科学基金会;
关键词
precursor synthesis; complexation reactions; spectroscopy and analytical chemistry; ferroelectric films;
D O I
10.1007/BF00486168
中图分类号
TQ174 [陶瓷工业]; TB3 [工程材料学];
学科分类号
0805 ; 080502 ;
摘要
In this investigation, several spectroscopic and analytical techniques were used to determine the chemical compositions and structures of the lead, zirconium, titanium, and Pb-(Zr, Ti) alkoxides involved in the sol-gel synthesis of PZT thin films. These techniques included H-1, C-13, and Pb-207 NMR; FT-IR; gas chromatography; Karl Fischer titration; and number-average molecular weights (M-n) determined by cryoscopy. It was found that the titanium precursor had a M-n of 548 and a formula of [Ti(OCH2CH2OCH3)(4)](1.6); the zirconium precursor had a M-n 1015 and a formula of [Zr(OCH2CH2OCH3)(4)](2.6); and the lead precursor had a formula Pb-6(OOCCH3)(5)(OCH2CH2OCH3)(7)center dot 4 H2O and a molecular weight of 2131 (M-n = 2113). It was observed that residual water from the incomplete dehydration of lead acetate trihydrate coupled with released water due to the esterification of acetic acid caused M-O-M (M = Pb, Zr, Ti) bonds in the Pb-(Zr,Ti) alkoxide. Two possible isomeric structures of the Pb-(Zr, Ti) alkoxide have been proposed. They are both cyclic and have a formula of Pb2M'M '' O-2(OR)(8)(ROH)(2), (M'M '' = Zr and/or Ti) and a molecular weight of 1336 (M-n = 1386).
引用
收藏
页码:251 / 265
页数:15
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