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Continuous supercritical hydrothermal synthesis of iron oxide nanoparticle dispersions and their characterization

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Abstract

Electrostatically stabilized iron oxide nanoparticle dispersions were synthesized using a continuous hydrothermal process at 673 K and 30 MPa. The average size of the primary particles was in the range 5–30 nm. The influence of the flow conditions as well as the composition of the starting material on the dispersion properties was investigated. A new Raman spectroscopic measurement setup was used for the characterization of the structure of the nanoparticles in dispersed form. The use of differential centrifugal sedimentation for the determination of the size distribution of the dispersed particles proved to be convenient and powerful to determine the influence of the investigated parameters on the dispersion properties. For certain compositions of the starting material and flow conditions using a conventional T-union, narrow size distributions concerning both primary particles and agglomerates could be obtained.

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Notes

  1. It is worth noting that the brownish red color was already observed at the time this unit was opened, directly after breaking the airtight packaging cover; there were no apparent color changes afterward. To minimize the exposure to air, the iron(II) acetate was kept in a glove box with an argon atmosphere, and before each experiment, a sufficient amount was bottled airtight in the glove box and was opened under normal atmosphere only once to prepare the aqueous solution.

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Acknowledgments

This work was carried out with the support of the Fraunhofer-Gesellschaft. The assistance of J. Graf, S. Unser, D. Rückert (building up and maintaining the high-pressure pilot plant), J. Schubert, F. Keilmann, C. Mönius, M. Zang (carrying out experimental runs), W. Send, C. Kübel (TEM), U. Förter-Barth, M. Herrmann (PXRD), L. Tercero Espinoza (assistance in programming with “R” for conveniently processing and visualizing data), and G. Irmer (Raman spectroscopy) is gratefully acknowledged.

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Author notes

  1. M. Daschner de Tercero

    Present address: Projektträger Karlsruhe (PTKA), Karlsruhe Institute of Technology (KIT), Hermann-von-Helmholtz-Platz 1, 76344 , Eggenstein-Leopoldshafen, Germany

Authors and Affiliations

  1. Fraunhofer Institute for Chemical Technology ICT, Joseph-von-Fraunhofer-Str. 7, 76327 , Pfinztal, Germany

    M. Daschner de Tercero & U. Fehrenbacher

  2. Institut für Theoretische Physik, Technische Universität Bergakademie Freiberg, Leipziger Str. 23, 09596 , Freiberg, Germany

    C. Röder

  3. Particle Technology, Technische Hochschule Nürnberg, Wassertorstr. 10, 90489 , Nuremberg, Germany

    U. Teipel

  4. Institute for Technical Thermodynamics and Refrigeration, Karlsruhe Institute of Technology (KIT), Engler-Bunte-Ring 21, 76131, Karlsruhe, Germany

    M. Daschner de Tercero & M. Türk

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Daschner de Tercero, M., Röder, C., Fehrenbacher, U. et al. Continuous supercritical hydrothermal synthesis of iron oxide nanoparticle dispersions and their characterization. J Nanopart Res 16, 2350 (2014). https://doi.org/10.1007/s11051-014-2350-1

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