Influence of the lead carboxylate on the molecular composition of its solutions with zirconium and titanium isopropoxides or n-butoxides : 2-ethylhexanoate vs acetate, a way to stabilize the first Pb-Zr carboxylatoalkoxides of 1:1 stoichiometry

The reactions between titanium or zirconium alkoxides namely Ti(OR)4 (R = iPr, nBu) or Zr2(OiPr)8(HOiPr)2, Zr(OnBu)4 respectively and lead 2-ethylhexanoate Pb(O2CC7H15)2 were investigated at room temperature (rt) and by heating. The various compounds were characterized by elemental analysis, FT-IR,...

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Bibliographic Details
Published in:Journal of sol-gel science and technology 2006-08, Vol.39 (2), p.159-167
Main Authors: BRETHON, Anne, HUBERT-PFALZGRAF, Liliane G
Format: Article
Language:English
Subjects:
Adducts
Alkoxides
Catalysis
Chemical analysis
Chemical composition
Chemical Sciences
Chemistry
Colloidal gels. Colloidal sols
Colloidal state and disperse state
Condensation
Exact sciences and technology
General and physical chemistry
Infrared analysis
Lead
Lead isotopes
NMR
Nuclear magnetic resonance
Perovskites
Stoichiometry
Titanium
Transition metals
Zirconium
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Summary:The reactions between titanium or zirconium alkoxides namely Ti(OR)4 (R = iPr, nBu) or Zr2(OiPr)8(HOiPr)2, Zr(OnBu)4 respectively and lead 2-ethylhexanoate Pb(O2CC7H15)2 were investigated at room temperature (rt) and by heating. The various compounds were characterized by elemental analysis, FT-IR, 1H and 207Pb NMR. The mixed-metal species obtained at rt were adducts Pb4Zr4(μ-O2CR′)8(OR)16(OHR)21 and Pb2Ti4(μ-O2CR′)4(OR)162 (R′=CHCHEt(CH2)2Me, R = iPr) independently of the stoichiometry used. The structures of 1 and 2 are based on triangular M2Pb cores (M = Zr, Ti). with 6-coordinate transition metals -as required for perovskites- and 6- or 7-coordinate lead atoms. Similar observations were made with n-butoxides. Thermal and hydrolytic condensation reactions were investigated. Thermal condensation was more difficult for the n-butoxide derivatives than for the isopropoxide ones. Powders derived from the hydrolysis of the Single Source Precursor 1 in various conditions were characterized by TGA, XRD and SEM for the PZ ceramic.
ISSN:0928-0707
1573-4846
DOI:10.1007/s10971-006-9169-x