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Correlation between synthesis parameters and properties of magnetite clusters prepared by solvothermal polyol method

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Abstract

The solvothermal polyol reaction is one of the most common methods known in the literature to synthesize magnetite nanoparticles and especially clusters. Despite this, its reaction mechanism is still not definitely determined. In the course of this work, a polyol reaction with sodium acrylate as stabilizer was used as a representative example. By using analytic tools such as TEM/SEM, XRPD, FTIR and Raman spectroscopy, XPS and magnetization measurements, the influence of several reaction parameters was examined, some of them for the first time for this type of reaction. The results detailed here have consequences for reproducibility as well as scale-up for this reaction. Using NMR techniques, the surface coating of the clusters was also analyzed. It was found that the coating consists of a variety of molecules, not just the stabilizer added in the reaction. By varying the temperature, it was possible to produce maghemite clusters instead of magnetite ones. Finally, on the basis of detailed analysis of intermediates, a possible reaction mechanism was formulated and used to explain several of the earlier findings.

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Acknowledgements

The authors wish to thank Sorina Ciupe for IR measurements, Dr. Lucian Barbu-Tudoran and Septimiu Tripon for some TEM measurements, Dr. Björn Kobin (Humboldt-Universität Berlin) for TGA measurements, Dr. Andrea Zehl (Humboldt-Universität Berlin) for elemental analysis and Dr. Cristian Leostean for XPS and magnetization measurements.

Funding

This work was supported by Grants of the Romanian National Authority for Scientific Research and Innovation, CNCS/CCCDI-UEFISCDI Project No. PN-III-P2-2.1-PED-2016-0168 and Project No. PN-III-P1-1.2-PCCDI-2017-0062, Contract No. 58, within PNCDI III. It was partially supported through the infrastructure obtained in the project Research Center and Advanced Technologies for Alternative Energies—CETATEA—623/11.03.2014.

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  1. National Institute R&D for Isotopic and Molecular Technology, 67-103 Donat Street, 400293, Cluj-Napoca, Romania

    Alexander Bunge, Alin Sebastian Porav, Gheorghe Borodi, Teodora Radu, Adrian Pîrnău, Camelia Berghian-Grosan & Rodica Turcu

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Bunge, A., Porav, A.S., Borodi, G. et al. Correlation between synthesis parameters and properties of magnetite clusters prepared by solvothermal polyol method. J Mater Sci 54, 2853–2875 (2019). https://doi.org/10.1007/s10853-018-3030-9

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