NDLI: Synthesis and characterization of glycol ether and oxime modified precursors of niobium(V) for soft transformation to niobia

Content Provider	SpringerLink
Author	Atal, Mukesh Kumar Jain, Jyoti Dhayal, Veena Nagar, Meena Bohra, Rakesh Rathore, Kuldeep S. Saxena, Narendra S.
Copyright Year	2013
Abstract	A glycol ether modified precursor, [Nb{O(CH$_{2}$CH$_{2}$O)$_{2}$}(OPr$^{i}$)$_{3}$] (A) was prepared by the reaction of Nb(OPr$^{i}$)$_{5}$ with O(CH$_{2}$CH$_{2}$OH)$_{2}$ in 1:1 molar ratio in anhydrous benzene. Further reactions of A with a variety of internally functionalized oximes in different molar ratios, yielded heteroleptic complexes of the type, [Nb{O(CH$_{2}$CH$_{2}$O)$_{2}$}(OPr$^{i}$)$_{3−n}${ON = C(CH$_{3}$)(Ar)}$_{n}$] (1–9) {where Ar = C$_{4}$H$_{3}$O-2, n = 1 [1], n = 2 [2], n = 3 [3]; C$_{4}$H$_{3}$S-2, n = 1 [4], n = 2 [5], n = 3 [6]; C$_{5}$H$_{4}$N-2, n = 1 [7], n = 2 [8], n = 3 [9]}. All the above derivatives have been characterized by elemental analyses, FT-IR, NMR ($^{1}$H, $^{13}$C {$^{1}$H}) and FAB mass studies. Spectral studies of 1–9 suggest the presence of mono- and bi-dentate mode of oxime moieties, in the solution and in the solid states, respectively. FAB mass studies indicate monomeric nature for 3 and dimeric nature for A. TG curves of A and 6 show their low thermal stability. Soft transformation of A and 3 to pure niobia, a and b, respectively have been carried out by sol–gel technique. The XRD patterns of niobia a and b suggest the formation of nano-size crystallites of average size of 10.8 and 19.5 nm, respectively. The XRD patterns also indicate the formation of monoclinic phase of the niobia in both the cases. Absorption spectra of a and b suggest energy band gaps of 4.95 and 4.39 eV, respectively.
Starting Page	88
Ending Page	96
Page Count	9
File Format	PDF
ISSN	09280707
Journal	Journal of Sol-Gel Science and Technology
Volume Number	67
Issue Number	1
e-ISSN	15734846
Language	English
Publisher	Springer US
Publisher Date	2013-05-21
Publisher Place	Boston
Access Restriction	Subscribed
Subject Keyword	Glycol ether modified precursor Internally functionalized oximes Heteroleptic complexes TG curves Ceramics, Glass, Composites, Natural Methods Inorganic Chemistry Optical and Electronic Materials Nanotechnology
Content Type	Text
Resource Type	Article
Subject	Biomaterials Electronic, Optical and Magnetic Materials Condensed Matter Physics Ceramics and Composites Materials Chemistry Chemistry

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