4.7 Article

Facile synthesis of morphology and size-controlled α-Fe2O3 and Fe3O4 nano-and microstructures by hydrothermal/solvothermal process: The roles of reaction medium and urea dose

Journal

CERAMICS INTERNATIONAL
Volume 42, Issue 13, Pages 14793-14804

Publisher

ELSEVIER SCI LTD
DOI: 10.1016/j.ceramint.2016.06.111

Keywords

Powders: chemical preparation; X-ray methods; Transition metal oxides; Chemical properties

Funding

  1. General Research Fund scheme of the Research Grants Council of Hong Kong [17206714, 17212015]
  2. Collaborative Research Fund scheme of the Research Grants Council of Hong Kong [C7044-14G]
  3. HKU Strategic Research Themes on Clear Energy and Earth as a Habitable Planet
  4. National Natural Science Foundation of China [51578556]
  5. Natural Science Foundation of Guangdong Province [2015A030308005]
  6. Science and Technology Research Programs of Guangdong Province [2014A020216009]

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This paper reports a systematic study of the influences on the synthesis of alpha-Fe2O3 and Fe3O4 via a hydro/solvothermal process at 200 degrees C. Both the reaction medium and urea dose have been investigated. The products were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), transmission electron microscopy (TEM). Results showed that the reaction mediums, such as water and ethylene glycol, played important roles in forming different types of iron oxides. Pure crystalline alpha-Fe2O3 was formed via the hydrothermal process, and Fe3O4 was obtained through a solvothermal route with ethylene glycol as reaction medium. Increasing urea dose tuned the particle sizes of alpha-Fe2O3 and Fe3O4 from a few hundreds to several tens of nanometers. With addition of urea, the morphology of alpha-Fe2O3 evolved from olive-like to rhomb-like, and Fe304 evolved from hollow sphere, to pinecone-like, and finally into cracked nanostructures. The variations of the surface area of products were mainly dependent on the microstructure and intrinsic features of the iron oxide particles. Results of the mechanistic studies indicated that the generation of CO2 and NH3 via in situ thermal decomposition of urea was crucial for the formation of alpha-Fe2O3 and Fe3O4 nano-and microstructures. The as-synthesized alpha-Fe2O3 and Fe3O4 were used as catalysts for methylene blue degradation in the presence of H2O2, and alpha-Fe2O3 showed a higher degradation efficiency. Our findings demonstrated a promising strategy for the developments of rationally designed iron oxides. (C) 2016 Elsevier Ltd and Techna Group S.r.l. All rights reserved.

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