The reactions between Ti(OR)
 4
 (R=Et, Pr
 i
) or
[Zr(OPr
 i
)
 4
(Pr
 i
OH)]
 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 (
 1
H, 13
C and 207
Pb)
spectroscopies. The mixed-metal oxoacetatoalkoxides
Pb
 2
Ti
 2
(µ
 4
-O)(µ-OAc)
 2

(µ-OPr
 i
)
 5
(OPr
 i
)
 3
 1 and
PbZr
 3
(µ
 4
-O)(µ-OAc)
 2

(µ-OPr
 i
)
 5
(OPr
 i
)
 5
 2 have
been characterized by X-ray crystallography at -100 °C: for 1,
monoclinic, space group C
 2
 /c with
a=38.916(17) A, b=12.045(2) A,
c=19.046(4) A, β=112.84(3)°,
V=8224(4) A
 3
 , Z=8, R=0.068,
R
 w
=0.076; and for 2, monoclinic, space group
P2
 1
 /n with a=10.618(2) A,
b=25.157(11) A, c=18.611(5) A,
β=90.35(2)°, V=4971(3) A
 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
PbTiO
 3
 . Effects of the solvent on the temperature of
crystallisation and on the particle size are
discussed.

Synthesis and structure of barium-titanium and calcium-titanium bimetallicalcoholates

Solution routes to lead titanate: synthesis, molecular structureand reactivity of the Pb–Ti and Pb–Zr species formed betweenvarious lead oxide precursors and titanium or zirconium alkoxides.Molecular structure of Pb2Ti2(µ4-O)(OAc)2(OPri)8 and ofPbZr3(µ4-O)(OAc)2(OPri)10

The reactions between titanium alkoxides Ti(OR)4 (R=Et,iPr) and strontium β-diketonates Sr(β-dik)2 (β-dik=thd, acac) were investigated. The various Sr−Ti species, Sr2Ti2(β-dik)4(OR)8, have a 1∶1 Sr∶Ti stoichiometry and were characterized by elemental analysis, FT-IR and by single-crystal X-ray diffraction for Sr2Ti2(μ3-OiPr)2(μ-OiPr)4OiPr)2(thd)4(1). The hydrolysis-polycondensation reactions of the various species were investigated and the resulting powders analyzed by light scattering and XRD. While acetone was found to have little influence on the hydrolysis reactions of the Sr−Ti species, polycondensation of Ti(OiPr)4 in neat acetone offers a trinuclear enolate Ti(μ3-O)2(OCMe=CH2)3(OiPr)5(iPrOH)(4). Comparisons between the Ba−Ti and Sr−Ti systems are given.

Synthesis and structure of barium-titanium and calcium-titanium bimetallicalcoholates

Citations

Solution routes to lead titanate: synthesis, molecular structureand reactivity of the Pb–Ti and Pb–Zr species formed betweenvarious lead oxide precursors and titanium or zirconium alkoxides.Molecular structure of Pb2Ti2(µ4-O)(OAc)2(OPri)8 and ofPbZr3(µ4-O)(OAc)2(OPri)10

The quest for single-source precursors for BaTiO3 and SrTiO3

The Synthesis and Solution Stability of Alkoxide Precursors

5 – Metal Oxo-alkoxides

Related Papers (5)

The System Titanium-Calcium

Synthesis of Well-Isolated Barium Titanium Trioxide Nanocubes.

Barium titanium silicon iron composition intermediate alloy

Preparing Titanium Powders by Calcium Vapor Reduction Process of Titanium Dioxide

Method for obtaining titanium-aluminium alloy from oxide titanium-containing material