Next Article in Journal
Next Article in Special Issue
Previous Article in Journal
Previous Article in Special Issue
Int. J. Mol. Sci. 2009, 10(11), 4977-4989; doi:10.3390/ijms10114977
Article

Modification of Different Zirconium Propoxide Precursors by Diethanolamine. Is There a Shelf Stability Issue for Sol-Gel Applications?

1,2
, 1
, 1
 and 2,*
Received: 12 October 2009; in revised form: 28 October 2009 / Accepted: 9 November 2009 / Published: 13 November 2009
(This article belongs to the Special Issue Sol-Gel Technique)
View Full-Text   |   Download PDF [943 KB, uploaded 19 June 2014]   |   Browse Figures
Abstract: Modification of different zirconium propoxide precursors with H2dea was investigated by characterization of the isolated modified species. Upon modification of zirconium n-propoxide and [Zr(OnPr)(OiPr)3(iPrOH)]2 with ½ a mol equivalent of H2dea the complexes [Zr2(OnPr)6(OCH2CH2)2NH]2 (1) and [Zr2(OnPr)2(OiPr)4(OCH2CH2)2NH]2 (2) were obtained. However, 1H-NMR studies of these tetranuclear compounds showed that these are not time-stable either in solution or solid form. The effect of this time instability on material properties is demonstrated by light scattering and TEM experiments. Modification of zirconium isopropoxide with either ½ or 1 equivalent mol of H2dea results in formation of the trinuclear complex, Zr{η3μ2-NH(C2H4O)2}3[Zr(OiPr)3]2(iPrOH)2 (3) countering a unique nona-coordinated central zirconium atom. This complex 3 is one of the first modified zirconium propoxide precursors shown to be stable in solution for long periods of time. The particle size and morphology of the products of sol-gel synthesis are strongly dependent on the time factor and eventual heat treatment of the precursor solution. Reproducible sol-gel synthesis requires the use of solution stable precursors.
Keywords: precursor chemistry; molecular structure; nona-coordinated zirconium precursor chemistry; molecular structure; nona-coordinated zirconium
This is an open access article distributed under the Creative Commons Attribution License which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.

Export to BibTeX |
EndNote


MDPI and ACS Style

Spijksma, G.I.; Blank, D.H.A.; Bouwmeester, H.J.M.; Kessler, V.G. Modification of Different Zirconium Propoxide Precursors by Diethanolamine. Is There a Shelf Stability Issue for Sol-Gel Applications? Int. J. Mol. Sci. 2009, 10, 4977-4989.

AMA Style

Spijksma GI, Blank DHA, Bouwmeester HJM, Kessler VG. Modification of Different Zirconium Propoxide Precursors by Diethanolamine. Is There a Shelf Stability Issue for Sol-Gel Applications? International Journal of Molecular Sciences. 2009; 10(11):4977-4989.

Chicago/Turabian Style

Spijksma, Gerald I.; Blank, Dave H. A.; Bouwmeester, Henny J. M.; Kessler, Vadim G. 2009. "Modification of Different Zirconium Propoxide Precursors by Diethanolamine. Is There a Shelf Stability Issue for Sol-Gel Applications?" Int. J. Mol. Sci. 10, no. 11: 4977-4989.



Int. J. Mol. Sci. EISSN 1422-0067 Published by MDPI AG, Basel, Switzerland RSS E-Mail Table of Contents Alert