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Highly dispersed mixed zirconia and hafnia nanoparticles in silica matrix: first example of a ZrO2-HfO2-SiO2 ternary oxide system (Articolo in rivista)

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Highly dispersed mixed zirconia and hafnia nanoparticles in silica matrix: first example of a ZrO2-HfO2-SiO2 ternary oxide system (Articolo in rivista) (literal)

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L. Armelao; H. Bertagnolli; D. Bleiner; M. Groenewolt; S. Gross; V. Krishnan; C. Sada; U. Schubert; E. Tondello; A. Zattin (2007)
Highly dispersed mixed zirconia and hafnia nanoparticles in silica matrix: first example of a ZrO2-HfO2-SiO2 ternary oxide system
in Advanced functional materials (Print); Wiley-VCH Verlag, GmbH., Weinheim (Germania)
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L. Armelao; H. Bertagnolli; D. Bleiner; M. Groenewolt; S. Gross; V. Krishnan; C. Sada; U. Schubert; E. Tondello; A. Zattin (literal)

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This work represents a remarkable advance in the field of materials research, and in particular in the development of oxide-based systems since it proposes a new approach for the preparation of bulk mixed oxides (ZrO2- HfO2-SiO2) with a uniform dispersion of the different components. The present work is, at the best of our knowledge, the first example which reports on a ternary system based on these Zr, Hf and Si oxides and describes a new synthetic route which can be applied to the preparation of a wide plethora of mixed oxides. In fact, the devised method, relying on the use of hybrid film to homogeneously embed the precursors of the guest oxides in the silica host matrix, enables to achieve a very uniform distribution of the species in the silica layers. Actually, the Zr- and Hf- clusters are chemically grafted to the partially formed silica network. The starting point is the preparation of inorganic-organic hybrid gels which, upon calcination at high temperature, yield an even distribution of the oxide nanoparticles. The proposed approach represents a general route to the preparation of homogeneous multicomponent oxide based-materials and can be virtually extended to achieve every mixed composition. (literal)

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Dr. S. Gross, Dr. L. Armelao, Prof. E. Tondello, A. Zattin CNR-ISTM, Department of Chemistry University of Padova and INSTM via Marzolo, 1, 35131 Padova (Italy) E-mail: silvia.gross@unipd.it Prof. H. Bertagnolli, Dr. V. Krishnan Institut für Physikalische Chemie, Universität Stuttgart Pfaffenwaldring 55, 70569 Stuttgart (Germany) Dr. D. Bleiner Department of Chemistry, University of Antwerp Universiteitsplein 1, 2610 Wilrijk-Antwerp (Belgium) Dr. M. Groenewolt[+] Max-Planck-Institut für Kolloid- und Grenzflächenforschung Am Mühlenberg 1, 14476 Potsdam, Golm (Germany) Dr. C. Sada Dipartimento di Fisica, Università degli Studi di Padova Via Marzolo, 8, 35131 Padova (Italy) Prof. U. Schubert Institut für Materialchemie, Technische Universität Wien Getreidemarkt 9/2/7 1060 Vienna (Austria) (literal)

Titolo

Highly dispersed mixed zirconia and hafnia nanoparticles in silica matrix: first example of a ZrO2-HfO2-SiO2 ternary oxide system (literal)

Abstract

ZrO2 and HfO2 nanoparticles are homogeneously dispersed in SiO2 matrices (supported film and bulk powders) by copolymerization of two oxozirconium and oxohafnium clusters (M4O2(OMc)12, M=Zr, Hf; OMc= OC(O)-C(CH3)?CH2) with (methacryloxypropyl) trimethoxysilane (MAPTMS, (CH2?C(CH3)C(O)O)-(CH2)3Si(OCH3)3). After calcination (at a temperature >=800 °C), a silica matrix with homogeneously distributedMO2 nanocrystallites is obtained. This route yields a spatially homogeneous dispersion of the metal precursors inside the silica matrix, which is maintained during calcination. The composition of the films and the powders is studied before and after calcination by using Fourier transform infrared (FTIR) analysis, X-ray photoelectron spectroscopy (XPS), secondary ion mass spectrometry (SIMS), and laser ablation inductively coupled plasma mass spectrometry (LA-ICPMS). The local environment of the metal atoms in one of the calcined samples is investigated by using X-ray Absorption Fine Structure (XAFS) spectroscopy. Through X-ray diffraction (XRD) the crystallization of Hf and Zr oxides is seen at temperatures higher than those expected for the pure oxides, and transmission electron microscopy (TEM) shows the presence of well-distributed and isolated crystalline oxide nanoparticles (5-10 nm). (literal)

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