4.3 Article

Synthesis routes for multi-shape Fe3O4 nanoparticles through oxidation-precipitation of hematite and modified co-precipitation method without surfactant

Journal

JOURNAL OF DISPERSION SCIENCE AND TECHNOLOGY
Volume 44, Issue 9, Pages 1759-1769

Publisher

TAYLOR & FRANCIS INC
DOI: 10.1080/01932691.2022.2042308

Keywords

Forced hydrolysis; monodispersed particles; magnetite; hematite

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Uniform fine particles of iron oxide with different morphologies were prepared through forced hydrolysis and co-precipitation techniques. The experiment showed that the reaction parameters greatly influenced the uniformity and morphology of the particles. Under optimized conditions, monodispersed magnetite precursor particles with narrow size distribution were obtained. The growth mechanism of the precipitated solids was found to be sensitive to temperature and pH, with high temperature and pH resulting in larger particles, while low temperature and pH leading to smaller particles. Magnetite nanoparticles were directly precipitated through co-precipitation and from the calcination of synthesized hematite at high temperatures. Analysis confirmed the single-phase magnetite structure through SEM, XRD, and FTIR. The response of the prepared particles to temperature and surface group composition was studied using TG/DTA and FT-IR techniques.
Uniform fine particles of iron oxide were precipitated in different morphologies through forced hydrolysis and co-precipitation. The effect of reaction parameters on particle uniformity and morphology was studied, and SEM analysis explored that particle morphological features were strongly affected by the applied reaction conditions. Therefore, monodispersed particles of magnetite precursors with narrow size distribution were prepared under the extensively optimized experimental parameters. The growth mechanism of the precipitated solids was observed to be sensitive to the medium temperature and pH, as high temperature and pH resulted in large particles. In contrast, small particles were precipitated at low temperatures and pH. Magnetite nanoparticles were precipitated directly through co-precipitation under controlled reaction conditions and from the calcination of the as-synthesized hematite at high temperatures. Their SEM demonstrated that calcination at high temperatures affected the particle morphology to a greater extent along with the phase transformation. Similarly, XRD and FTIR analysis of the as-prepared magnetite particles from two routes confirmed the single-phase magnetite. The response of the as-prepared particle systems to the higher temperature and composition of the surface groups was analyzed by TG/DTA and FT-IR techniques.

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