Structure evolution in the PbO-ZrO2-TiO2 sol-gel system: Part I - Characterization of prehydrolyzed precursors

P. R. Coffman, Sandwip Dey

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Abstract

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 1H, 13C, and 207Pb NMR; FT-IR; gas chromatography; Karl Fischer titration; and number-average molecular weights (Mn) determined by cryoscopy. It was found that the titanium precursor had a Mnof 548 and a formula of [Ti(OCH2CH2OCH3)4]1.6; the zirconium precursor had a Mnof 1015 and a formula of [Zr(OCH2CH2OCH3)4]2.6; and the lead precursor had a formula Pb6(OOCCH3)5(OCH2CH2OCH3)7. 4 H2O and a molecular weight of 2131 (Mn=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″O2(OR)8(ROH)2, (M′M″=Zr and/or Ti) and a molecular weight of 1336 (Mn=1386).

Original languageEnglish (US)
Pages (from-to)251-265
Number of pages15
JournalJournal of Sol-Gel Science and Technology
Volume1
Issue number3
DOIs
StatePublished - Jan 1 1994

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Keywords

  • complexation reactions
  • ferroelectric films
  • precursor synthesis
  • spectroscopy and analytical chemistry

ASJC Scopus subject areas

  • Electronic, Optical and Magnetic Materials
  • Ceramics and Composites
  • Chemistry(all)
  • Biomaterials
  • Condensed Matter Physics
  • Materials Chemistry

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