Niobium(V) Alkoxides. Synthesis, Structure, and Characterization of [Nb(μ-OCH2CH3)(OCH2C(CH3) 3)4]2, {[H3CC(CH2O)(CH2-μ-O)(C(O) 2)]Nb2(μ-O)(OCH2CH3) 5}2

Timothy J. Boyle*, Todd M. Alam, Duane Dimos, Gregorio J. Moore, Catherine D. Buchheit, Husam Niman Alshareef, Eric R. Mechenbier, Blakely R. Bear, Joseph W. Ziller

*Corresponding author for this work

Research output: Contribution to journalArticlepeer-review

46 Scopus citations

Abstract

We have synthesized and isolated a number of unique niobium alkoxide compounds and introduced them into novel solution processes for the production of lead magnesium niobate oxide (PMN) and niobium-doped lead zirconate titanate oxide (PNZT) materials. A more sterically demanding analogue to Nb(OEt)5 (Et = CH2CH3) was isolated as [Nb(μ-OEt)-(ONp)4]2 (1, Np = CH2C(CH3)3) by alcoholysis exchange. 1 crystallized in an edge-shared bioctahedral dinuclear arrangement with the smaller ligands acting as the bridging moieties. Multidentate ligands such as bis(hydroxymethyl)propionic acid (BHMP-H3) and tris-(hydroxymethyl)ethane (THME-H3) were independently reacted with Nb(OEt)5 to reduce the number of terminal ligands, yielding [(μ-BHMP)Nb2(μ-O)(OEt)5]2 (2) and [(μ-THME)-Nb(OEt)2]2 (3) respectively. For 2, two unsymmetrical "(EtO)2Nb(μ-O)Nb(OEt)3" units are bridged by two tetradentate BHMP ligands. The THME moiety of 3 acts as a chelating, unidentate-bridging ligand forming a symmetrical dinuclear species, wherein each Nb atom possesses two terminal ethoxides. The synthesis, characterization, structural aspects, and solution properties of 1-3 are reported. The resulting morphological and electrical changes in the properties of the resulting electroceramic PMN and PNZT films due to the incorporation of these Nb alkoxides are also reported.

Original languageEnglish (US)
Pages (from-to)3187-3198
Number of pages12
JournalChemistry of Materials
Volume9
Issue number12
StatePublished - Dec 1 1997

ASJC Scopus subject areas

  • Chemistry(all)
  • Chemical Engineering(all)
  • Materials Chemistry

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