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Synthesis of nanocrystalline iron oxide particles by the esterification reaction in the iron(III)/acetate/alcohol system

Marijan Gotić ,  Svetozar Musić 

Ruđer Bošković Institute, Bijenička 54, Zagreb 10000, Croatia


Among the various synthesis routes, solution-based or “wet” chemistry synthesis offers a very good control over particle size, morphology and phase composition of the final product. Forced hydrolysis, microemulsion technique, hydrothermal, sol-gel, polyol and non-hydrolytic syntheses are often utilized. In an earlier work we have shown that nanosize TiO2 (J. Mol. Struct. 481 (1999) 645), V2O5 (unpublished results), Bi2O3 (Matt. Lett. 61 (2007) 709) and Fe-TiO2 nanoparticle (J. Sol-Gel Sci. Technol. 30 (2004) 5) can be successfully synthesized using an esterification reaction between the acetic acid and alcohol. On this route a metal cation was homogeneously hydrolyzed by water molecules generated in situ as follows: CH3COOH + ROH → CH3COOR + H2O. In this work we are presenting new results relating to the synthesis of nanosize iron oxide particles by using the esterification reaction in the iron(III)/acetic acid/alcohol system. Synthesis started from a clear iron(III) organic solution that was stable at room temperature for months. However, at elevated temperature and under the autoclave pressure, a nanocrystalline iron oxide phase was obtained. Control of the phase composition, morphology, aggregation and particle size of obtained iron oxides was achieved by adjusting experimental parameters such as the type of alcohol, the molar ratio of iron(III)/acetic acid/alcohol and temperature. For instance, nanosize magnetite particles arranged in regular spheres were formed in the iron(III)/acetate/ethanol system in autoclave at 180oC (Fig. 1).



Fig. 1 FE SEM images of nanosize magnetite particles arranged in regular spheres and an enlarged detail showing discrete particles on the surface of one sphere.

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Presentation: Oral at E-MRS Fall Meeting 2007, Symposium A, by Marijan Gotić
See On-line Journal of E-MRS Fall Meeting 2007

Submitted: 2007-05-14 16:51
Revised:   2009-06-07 00:44