화학공학소재연구정보센터
Inorganic Chemistry, Vol.34, No.3, 628-632, 1995
Single-Source Precursors of Lead Titanate - Synthesis, Molecular-Structure and Reactivity of Pb2Ti2(Mu(4)-O)(Mu(3)-O-I-Pr)(2)(Mu-O-I-Pr)(4)(O-I-Pr)(4)
The reaction between Ti(O-i-Pr)(4) and [Pb(O-i-Pr)(2)](infinity) or Pb4O(O-i-Pr)(6) offers the mixed-metal oxoalkoxide, Pb-2-Ti-2(mu(4)-O)(mu(3)-O-i-Pr)(2)(mu-O-i-Pr)(4)(O-i-Pr)(4) (1) which has been characterized by crystallography at -120 degrees C. 1 belongs to the monoclinic space group P2(1)/n with a 10.286(14) Angstrom, b = 22.564(4) Angstrom, 18.709(5) Angstrom, B = 97.93(5), V = 4301(6) Angstrom(3), and Z = 4. Compound 1 represents the first example of a structurally characterized "single-source" precursor having a Pb:Ti stoichiometry appropriated for PbTiO3. The 1:1 stoichiometry between the metals is retained by reaction between 1 and acetic acid or acetylacetone (1:2 molar ratio), Pb2Ti2O(OAc)(2)(O-i-Pr)(8) (2) and Pb2Ti2O(acac)(2)(O-i-Pr)(8) (3) being obtained respectively. All compounds have been isolated in high yields and were characterized by microanalysis, FT-IR and NMR (H-1, C-13, and Pb-207). Hydrolysis-condensation reactions of the various species giving lead titanate have been achieved.