Syntheses and characterization of a new class of zirconia precursors of oxime-modified zirconium(IV) isopropoxide |
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| Authors: | Archana Chaudhary Ram Gopal Meena Nagar Rakesh Bohra |
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| Institution: | 1. Discipline of Chemistry, School of Basic Sciences, Indian Institute of Technology Indore, Indore, 452017, Madhya Pradesh, India
2. Department of Chemistry, University of Rajasthan, Jaipur, 302004, Rajasthan, India
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| Abstract: | Some oxime modified complexes of the type Zr{OPri}4?n{L}n] {where, n = 1–4 and LH=(CH3)2C=NOH (1–4) and C9H16C=NOH (5–8)} have been synthesized by the reaction of Zr(OPri)4·PriOH] with oximes, in anhydrous refluxing benzene. These synthesized complexes were characterized by elemental analyses, molecular weight measurements, ESI-mass, FT-IR and NMR (1H and 13C{1H}) spectral studies. The ESI-mass spectral studies indicate dimeric nature for Zr{OPri}2{ONC(CH3)2}2] (2), Zr{OPri}3{ONC10H16}] (5) and Zr{OPri}{ONC10H16}3] (7) and monomeric nature for Zr{ONC10H16}4] (8). Oximato ligands appear to bind the zirconium in side on manner in all the complexes. Thermogravimetric curves of (2) and (8) exhibit multi-step decomposition with the formation of ZrO2, under nitrogen atmosphere. Sol–gel transformations of precursors (5), (6), (7) and (8) in organic medium, yielded nano-sized tetragonal phase of zirconia samples (a), (b), (c) and (d), respectively, on sintering at ~600 °C. All these samples were characterized by Powder XRD patterns and EDX analyses. Surface morphologies of these samples were investigated by SEM images. |
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