Solution routes to lead titanate: Synthesis, molecular structure and reactivity of the Pb-Ti and Pb-Zr species formed between various lead oxide precursors and titanium or zirconium alkoxides. Molecular structure of Pb2Ti2(mu(4)-O)(OAc)(2)(OPri)(8) and of PbZr3(mu(4)-O)(OAc)(2)(OPri)(10)

被引:43
作者
HubertPfalzgraf, LG [1 ]
Daniele, S [1 ]
Papiernik, R [1 ]
Massiani, MC [1 ]
Septe, B [1 ]
Vaissermann, J [1 ]
Daran, JC [1 ]
机构
[1] CHIM MET TRANSIT LAB,URA CNRS,F-75230 PARIS 5,FRANCE
关键词
D O I
10.1039/a605266e
中图分类号
O64 [物理化学(理论化学)、化学物理学];
学科分类号
070304 ; 081704 ;
摘要
The reactions between Ti(OR)(4)(R=Et, Pr-i) or [Zr(OPri)(4)((PrOH)-O-i)](2) and various lead oxide precursors [anhydrous Pb(OAc)(2), alkoxides or oxoalkoxides] have been investigated in different experimental conditions (solvent, temperature). Various mixed-metal species have been isolated in high yields and characterized by microanalysis, FTIR and multinuclear NMR (H-1, C-13 and (207)pb) spectroscopies The mixed-metal oxoacetatoalkoxides Pb2Ti2(mu(4)-O)(mu-OAc)(2)(mu-OPri)(5)(OPri)(3) 1 and PbZr3(mu(4)-O)(mu-OAc)(2)(mu-OPri)(5)(OPri)(5) 2 have been characterized by X-ray crystallography at -100 degrees C: for 1, monoclinic, space group C-2/c with a=38.916(17)Angstrom, b=12.045(2)Angstrom, c=19.046(4)Angstrom, beta=112.84(3)degrees, V=8224(4)Angstrom(3), Z=8, R=0.068, R-W=0.076; and for 2, monoclinic space group P2(1)/n with a=10.618(2)Angstrom, b=25.157(11)Angstrom, c=18.611(5)Angstrom, beta=90.35(2)degrees, V=4971(3)Angstrom(3), Z=4, R=0.060, R-W=0.072. Hydrolysis-condensation reactions have been achieved especially for the species having a Pb:Ti stoichiometry appropriate for access to PbTiO3. Effects of the solvent on the temperature of crystallisation and on the particle size are discussed.
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页码:753 / 762
页数:10
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