PbTiO3 sol-gel process studied by 207Pb-NMR, IR, DTA and XRD

PbTiO3 film and powder materials were obtained from a sol prepared at room temperature by mixing lead (II) acetate trihydrate (LAT) and tetraisopropylorthotitanate (TPOT) in methoxyethanol. The sol-gel process was studied by 207Pb NMR and IR spectroscopy, DTA and XRD measurements. This investigation...

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Bibliographic Details
Published in:Journal of materials science 1995, Vol.30 (12), p.3137-3141
Main Authors: LUO LAN, MONTENERO, A, GNAPPI, G, DRADI, E
Format: Article
Language:English
Subjects:
Chemistry
Colloidal state and disperse state
Exact sciences and technology
General and physical chemistry
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Summary:PbTiO3 film and powder materials were obtained from a sol prepared at room temperature by mixing lead (II) acetate trihydrate (LAT) and tetraisopropylorthotitanate (TPOT) in methoxyethanol. The sol-gel process was studied by 207Pb NMR and IR spectroscopy, DTA and XRD measurements. This investigation shows that an interaction between LAT and TPOT occurs immediately on mixing in solution and, as a result of the interaction, the lead and titanium compounds are indistinctly linked together through bidentate acetate bridging. This linkage remains unchanged during solution reactions and gelation, Pb-O-Ti bonding being absent at this stage. The gel retains its amorphous state on heating at 370 C for 1 h. An unidentified primary crystal phase appears after heating the gel at 400 C for 1 h, and it is transformed into perovskite PbTiO3 crystals at 500 C and higher temperatures. 14 refs.
ISSN:0022-2461
1573-4803