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Materials 2013, 6(4), 1467-1484; doi:10.3390/ma6041467
Article

Organized Silica Films Generated by Evaporation-Induced Self-Assembly as Hosts for Iron Oxide Nanoparticles

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1,*
1 Department of Chemistry, University of Cyprus, P.O. Box 20537, Nicosia 1678, Cyprus 2 Institute of Inorganic Chemistry, Graz University of Technology, Stremayergasse 9/4, 8010 Graz, Austria 3 Institute of Advanced Materials, Physicochemical Processes, Nanotechnology and Microsystems (IAMPPNM), Division of Physical Chemistry, National Center for Scientific Research "Demokritos", Aghia Paraskevi Attikis, Athens 153 10, Greece 4 Department of Chemical Engineering, University of Patras, P.O. Box 1414, Patras 265 00, Greece
* Author to whom correspondence should be addressed.
Received: 14 January 2013 / Revised: 26 March 2013 / Accepted: 27 March 2013 / Published: 9 April 2013
(This article belongs to the Special Issue Advances in Sol-gel Derived Materials)
Download PDF [603 KB, 15 April 2013; original version 9 April 2013]

Abstract

In this work, we prepared oriented mesoporous thin films of silica on various solid substrates using the pluronic block copolymer P123 as a template. We attempted to insert guest iron oxide (FexOy) nanoparticles into these films by two different methods: (a) by co-precipitation—where iron precursors are introduced in the synthesis sol before deposition of the silica film—and subsequent oxide production during the film calcination step; (b) by preparing and calcining the silica films first then impregnating them with the iron precursor, obtaining the iron oxide nanoparticles by a second calcination step. We have examined the structural effects of the guest nanoparticles on the silica film structures using grazing incidence X-ray scattering (GISAXS), high-resolution transmission electron spectroscopy (HRTEM), spectroscopic ellipsometry, X-ray photoelectron spectroscopy (XPS), and Raman microscopy. Formation of nanoparticles by co-precipitation may induce substantial changes in the film structure leading, in our adopted process, to the appearance of lamellar ordering in the calcination stage. On the contrary, impregnation-based approaches perturb the film structures much more weakly, but are also less efficient in filling the pores with nanoparticles.
Keywords: oriented mesoporous silica films; grazing incidence X-ray scattering (GISAXS); iron oxide nanoparticles; impregnation; co-precipitation oriented mesoporous silica films; grazing incidence X-ray scattering (GISAXS); iron oxide nanoparticles; impregnation; co-precipitation
This is an open access article distributed under the Creative Commons Attribution License which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.

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Andreou, I.; Amenitsch, H.; Likodimos, V.; Falaras, P.; Koutsoukos, P.G.; Leontidis, E. Organized Silica Films Generated by Evaporation-Induced Self-Assembly as Hosts for Iron Oxide Nanoparticles. Materials 2013, 6, 1467-1484.

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