http://www.cnr.it/ontology/cnr/individuo/prodotto/ID47635

Zirconium and hafnium oxoclusters as molecular building blocks for highly dispersed ZrO2 or HfO2 nanoparticles in silica thin films (Articolo in rivista)

Type

Articolo in rivista (Classe)
Prodotto della ricerca (Classe)

Label

Zirconium and hafnium oxoclusters as molecular building blocks for highly dispersed ZrO2 or HfO2 nanoparticles in silica thin films (Articolo in rivista) (literal)

Anno

2005-01-01T00:00:00+01:00 (literal)

Http://www.cnr.it/ontology/cnr/pubblicazioni.owl#doi

10.1039/b500521c (literal)

Alternative label

Armelao L.; Eisenmenger-Sittner C.; Groenewolt M.; Gross S.; Sada C.; Schubert U.; Tondello E.; Zattin A. (2005)
Zirconium and hafnium oxoclusters as molecular building blocks for highly dispersed ZrO2 or HfO2 nanoparticles in silica thin films
in Journal of materials chemistry (Print); Royal Society of Chemistry, Cambridge (Regno Unito)
(literal)

Http://www.cnr.it/ontology/cnr/pubblicazioni.owl#autori

Armelao L.; Eisenmenger-Sittner C.; Groenewolt M.; Gross S.; Sada C.; Schubert U.; Tondello E.; Zattin A. (literal)

Pagina inizio

1838 (literal)

Pagina fine

1848 (literal)

Http://www.cnr.it/ontology/cnr/pubblicazioni.owl#altreInformazioni

Study performed in the framework of cooperation with different (3) international groups. First thorough study on crystallisation behaviour and evolution of binary zirconia-silica oxide. The manuscript represents a remarkable advance in the field of materials research, and in particular in the development of oxide-based thin films since it presents a new approach to the preparation of thin films characterized by a uniform dispersion of the different components. In fact, the devised method enables to achieve a homogeneous distribution of the host nanoparticles in the silica host matrix. Furthermore, since the cluster are grafted to a partially formed silica network, the nucleation of the host nanoparticles is spatially confined, and the growth of larger particles is avoided. This approach represents a general route to the preparation of homogeneous multicomponent oxide based-materials. Furthermore, a multitechnique approach for the thorough characterization of the films is here presented, which is based on the use of different analytical tools delivering complementary information on the composition, microstructure and morphology of the nanostructured layers. (literal)

Http://www.cnr.it/ontology/cnr/pubblicazioni.owl#url

http://pubs.rsc.org/en/Content/ArticleLanding/2005/JM/b500521c (literal)

Http://www.cnr.it/ontology/cnr/pubblicazioni.owl#numeroVolume

15 (literal)

Rivista

Journal of materials chemistry (Rivista)

Http://www.cnr.it/ontology/cnr/pubblicazioni.owl#pagineTotali

11 (literal)

Note

Scopu (literal)
ISI Web of Science (WOS) (literal)

Http://www.cnr.it/ontology/cnr/pubblicazioni.owl#affiliazioni

Lidia Armelao,a Christoph Eisenmenger-Sittner,b Matthijs Groenewolt,c Silvia Gross,a Cinzia Sada,d Ulrich Schubert,e Eugenio Tondelloa and Andrea Zattina aCNR-ISTM and INSTM, Department of Chemical Sciences, University of Padova, via Marzolo, 1- I-35131, Padova, Italy. E-mail: silvia.gross@unipd.it; Fax: ++39-049-8275161; Tel: ++39-049-8275736 bInstitut fu¨r Festko¨rperphysik-Vienna University of Technology, Vienna, Austria cMax-Planck-Institut fu¨r Kolloid- und Grenzfla¨chenforschung, Golm, Germany dDepartment of Physics, University of Padova, Padova, Italy eInstitute of Materials Chemistry-Vienna University of Technology, Vienna, Austria (literal)

Titolo

Zirconium and hafnium oxoclusters as molecular building blocks for highly dispersed ZrO2 or HfO2 nanoparticles in silica thin films (literal)

Abstract

A novel synthetic route for the preparation of ZrO2 or HfO2 nanoparticles homogeneously dispersed in SiO2 thin films was developed. This route is based on the copolymerisation of organically modified crystalline oxozirconium or oxohafnium clusters (M4O2(OMc)12, M 5 Zr, Hf; OMc 5 OC(O)-C(CH3)LCH2) with (methacryloxymethyl)triethoxysilane (MAMTES, CH2LC(CH3)C(O)O-CH2Si(OCH2CH3)3). These crystalline clusters, which are the precursors for the corresponding metal oxides (MO2), were prepared via the sol-gel route by reaction of zirconium or hafnium butoxide (M(OBu)4) with methacrylic acid. The copolymerisation of the clusters with the methacrylate-functionalised siloxane was photoinitaited by Irgacure 184 and allowed the anchoring of the cluster to the forming silica network. The solution was cast into films by dip-coating and UV cured (10 min, 125 W) to promote the copolymerisation of the methacrylate groups of the cluster with those of the silane. Transparent and homogeneous films 200-450 nm thick were obtained after calcination at 800 uC in air. This route allowed the production of a very homogeneous dispersion of the MO2 precursors inside the silica matrix. The surface and in-depth composition of the thin films was investigated through IR, X-ray photoelectron spectroscopy (XPS) and secondary ion mass spectrometry (SIMS). SIMS and XPS depth profiles evidenced a very homogenous distribution of both zirconium or hafnium throughout the silica films and sharp film-substrate interfaces. The surface morphology of the coatings was investigated through atomic force microscopy (AFM), which showed smooth, homogeneous and crack-free surfaces. Through X-ray diffraction (XRD) the crystallisation of hafnium and zirconium oxides was revealed, while the presence of isolated crystalline nanoparticles having a diameter of 5-10 nm was evidenced by transmission electron microscopy (TEM). A pull-off test indicated a very good adhesion of the films to the substrate. (literal)

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