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Induced shape controllability by tailored precursor design in thermal and microwave-assisted synthesis of \(\mathrm{Fe}_{3}\mathrm{O}_{4}\) nanoparticles

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Abstract

The shape of magnetite nanoparticles (NPs) synthesized by thermal (T) and microwave (MW) approaches was controlled by an optimized methodology, which consists of a prior and easy modification of the \(\upalpha\) terminal position belonging to the iron(III) tris(2,4-pentanedionate) precursor. Round, cuboctahedron, flower-like \(\mathrm{Fe}_{3}\mathrm{O}_{4}\) (<10 nm) and bow-like \(\mathrm{FeF}_{2}\) nanostructures have been synthesized in triethylene glycol media, producing polar dispersible NPs. The \(\upalpha\) terminal group was modified from the initial –\(\mathrm{CH}_{3}\) to –\(\mathrm{Ph},\) –\(^{t}\mathrm{Bu},\) and –\(\mathrm{CF}_{3}\) respectively, inducing defined and characteristic shapes of the obtained NPs: round, cuboctahedron, flower-like \(\mathrm{Fe}_{3}\mathrm{O}_{4},\) and bow-like \(\mathrm{FeF}_{2},\) respectively. The two investigated synthetic methodologies, T and MW, produce similar results, except for the precursor containing the aromatic group (–\(\mathrm{Ph}\)), through which cuboctahedron (T) and elongated polycrystalline microwires (MW) were generated. The ensemble of modified ligands has demonstrated to influence the final shape, structure, and composition of the nanocrystals generated. The resulting NPs were studied by high-resolution transmission electron microscopy, X-ray powder diffraction, and thermogravimetric analysis. Data demonstrated a strong relation between the precursor design and the final morphology of the NPs, which could be explained by different precursor–particle interactions during nucleation and crystal growth. The final composition of all nanostructures was the expected \(\mathrm{Fe}_{3}\mathrm{O}_{4},\) except for the fluorinated precursor where \(\mathrm{FeF}_{2}\) was obtained as the main reaction product.

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Acknowledgments

The authors thank the funding of the European Union’s Seventh Framework Program (FP7/2007–2013 under the Grant Agreement number 280432) EUROTAPES and the Spanish Government “MINECO” (MAT2011-28874-C02, CSD 2007-0041, IPT-2011-1090-920000). Thomas Lehnen is also recognized for his contribution to the writing of this manuscript.

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Author notes

  1. Eduardo Solano

    Present address: Department of Solid State Sciences, COCOON, Ghent University, Krijgslaan 281/S1, 9000, Ghent, Belgium

Authors and Affiliations

  1. Departament de Química, Universitat Autònoma de Barcelona, 08193, Bellaterra, Catalonia, Spain

    Alba Garzón-Manjón, Eduardo Solano, Ramón Yáñez & Josep Ros

  2. Institut de Ciència de Materials de Barcelona, ICMAB-CSIC, Campus de la UAB, 08193, Bellaterra, Catalonia, Spain

    Alba Garzón-Manjón, Eduardo Solano, María de la Mata, Roger Guzmán, Teresa Puig, Xavier Obradors & Susagna Ricart

  3. Institució Catalana de Recerca i Estudis Avançats, ICREA, 08019, Barcelona, Catalonia, Spain

    Jordi Arbiol

Authors
  1. Alba Garzón-Manjón
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Correspondence to Eduardo Solano.

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Alba Garzón-Manjón and Eduardo Solano equally contributed to this work.

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Garzón-Manjón, A., Solano, E., de la Mata, M. et al. Induced shape controllability by tailored precursor design in thermal and microwave-assisted synthesis of \(\mathrm{Fe}_{3}\mathrm{O}_{4}\) nanoparticles. J Nanopart Res 17, 291 (2015). https://doi.org/10.1007/s11051-015-3070-x

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