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Self-assembly of iron oxide precursor micelles driven by magnetic stirring time in sol-gel coatings

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2019-06-09
Authors
López Sánchez, Jesús
Rodríguez de la Fuente, Óscar
Serrano, A.
Campo, A. del
Abuín, M.
Salas Colera, E.
Muñoz Noval, A:
Castro, G. R.
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Royal Society Chemical
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The purpose of this work is to fabricate self-assembled microstructures by the sol-gel method and study the morphological, structural and compositional dependence of epsilon-Fe_2O_3 nanoparticles embedded in silica when glycerol (GLY) and cetyl-trimethylammonium bromide (CTAB) are added as steric agents simultaneously. The combined action of a polyalcohol and a surfactant significantly modifies the morphology of the sample giving rise to a different microstructure in each of the studied cases (1, 3 and 7 days of magnetic stirring time). This is due to the fact that the addition of these two compounds leads to a considerable increase in gelation time as GLY can interact with the alkoxide group on the surface of the iron oxide precursor micelle and/or be incorporated into the hydrophilic chains of CTAB. This last effect causes the iron oxide precursor micelles to be interconnected forming aggregates whose size and structure depend on the magnetic stirring time of the sol-gel synthetic route. In this paper, crystalline structure, composition, purity and morphology of the sol-gel coatings densified at 960 degrees C are examined. Emphasis is placed on the nominal percentage of the different iron oxides found in the samples and on the morphological and structural differences. This work implies the possibility of patterning epsilon-Fe_2O_3 nanoparticles in coatings and controlling their purity by an easy one-pot sol-gel method.
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©2019 The Author(s) This journal is © The Royal Society of Chemistry 2019 Artículo firmado por más de diez autores. Dr Paloma Almodovar is acknowledged for her fruitful discussions about CRM and SEM characterization. The authors also acknowledge the Spanish Ministry of Industry, Economy and Competitiveness for financing the project MAT2015-65445-C2-1-R, MAT2017-86450-C4-1-R, MAT2015-67557-C2-1-P, by the Comunidad de Madrid S2013/MIT-2850 NANOFRONTMAG and H2020 AMPHIBIAN Project ID: 720853. The authors are also grateful to the BM25-SpLine staff for their valuable technical support beyond their duties and for the financial support from the Spanish Ministry of Science, Innovation and Universities (MICIU) and The Spanish National Research Council (CSIC) under Grant No. PIE 2010-6OE-013, The ESRF - The European Synchrotron, MICIU and CSIC are acknowledged for provision of synchrotron radiation facilities. A. S. acknowledges the financial support from the Comunidad de Madrid for an "Atraccion de Talento Investigador" contract (No. 2017-t2/IND5395).
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