Surfactant-Induced Nonhydrolytic Synthesis of Phase-Pure ZrO2 Nanoparticles from Metal鈥揙rganic and Oxocluster Precursors
详细信息 查看全文
- 作者：Mahmoud A. Sliem ; Diedrich A. Schmidt ; Ang茅lique B茅tard ; Suresh Babu Kalidindi ; Silvia Gross ; Martina Havenith ; Anjana Devi ; Roland A. Fischer
- 刊名：Chemistry of Materials
- 出版年：2012
- 出版时间：November 27, 2012
- 年：2012
- 卷：24
- 期：22
- 页码：4274-4282
- 全文大小：462K
- 年卷期：v.24,no.22(November 27, 2012)
- ISSN：1520-5002
文摘
Nonhydrolytic/non-sol鈥揼el pyrolytic synthesis technique, as a convenient method, was applied to synthesize zirconium oxide nanoparticles (ZrO2 NPs). Pyrolysis of either the mononuclear keto ester/alkoxide complex zirconium bis(isopropoxide)bis(tert-butylacetoacetate) [Zr(OiPr)2(tbaoac)2] (I) or the oligonuclear oxocluster compound [Zr6(OH)4O4(OMc)12] (II, Mc = methacrylate) generated ZrO2 NPs at moderate conditions of 300鈥?00 掳C. Trioctylamine, stearic acid, and/or oleic acid, which act as both solvents and stabilizing agents, were used. Under the adopted process conditions, the stabilizing agent oleic acid plays a vital role in determining the phase of as-synthesized colloidal ZrO2 nanoparticles, which yield the high-temperature tetragonal phase at moderate conditions of 335 掳C. Those as-synthesized samples that contained both monoclinic and tetragonal ZrO2 phases (depending on the choice of the surfactant) were transformed into pure tetragonal phase at 1000 掳C. An unambiguous phase determination of ZrO2 nanoparticles was carried out by the combination of powder X-ray diffraction (XRD) and Raman spectroscopy. Furthermore, the samples were analyzed by transmission electron microscopy (TEM), ultraviolet鈥搗isible (UV鈥搗is) and photoluminescence (PL) spectroscopy, dynamic light scattering (DLS), and Fourier transform infrared (FT-IR) spectroscopy to elucidate the structure, chemical composition, and morphology of the obtained nanoparticles. Also, the phase transformations of the as-synthesized ZrO2 nanoparticles upon annealing were followed via Raman spectroscopy.