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Journal of Materials Science

, Volume 47, Issue 14, pp 5546–5560 | Cite as

Prospects for the incorporation of cobalt into α-Fe2O3 nanorods during hydrothermal synthesis

  • Trevor P. AlmeidaEmail author
  • Michael W. Fay
  • Yanqiu Zhu
  • Paul D. Brown
Article

Abstract

A feasibility study on the incorporation of cobalt into α-Fe2O3 nanorods (NRs) during hydrothermal synthesis (HS) is presented as a function of FeCl3 and CoCl2 concentration, phosphate surfactant concentration and pH value, with samples assessed using X-ray diffractometry, transmission electron microscopy, selected area electron diffraction and energy dispersive X-ray analysis. No evidence was found for the incorporation of cobalt into α-Fe2O3 NRs at low pH, whilst synthesis at intermediate and high pH values favoured the formation of CoFe2O4 NPs. The critical role of pH value over the precipitation, size and phase purity of the nanostructured reaction products is emphasised. At pH ~2, large, well crystalline α-Fe2O3 nanoparticles (NPs) and NRs were grown from FeCl3 solution in the absence and presence of phosphate, respectively, whilst no evidence was found for Co precipitation or incorporation in α-Fe2O3 following HS in the presence of CoCl2. At pH ~8, smaller α-Fe2O3 NPs, as well as Co3O4 and CoFe2O4 NPs were synthesised from FeCl3, CoCl2, or a mixture thereof. HS at pH ~12 produced a mixture of larger CoFe2O4 NPs and α-Fe2O3 NPs depending on the Fe:Co molar ratio. The formation of intermediate metastable (oxy)hydroxide phases is considered pH dependent, providing for a variety of different reaction pathways. Further, inclusion of preformed Co3O4 and CoFe2O4 NPs to the FeCl3 solution at pH ~2 in the presence of phosphate surfactant resulted in the synthesis of α-Fe2O3 NRs with residual Co3O4 and CoFe2O4 NPs attached to their surfaces. The CoFe2O4 NPs encouraged local dissolution leading to the formation of α-Fe2O3 NR surface corrugations.

Keywords

Co3O4 Select Area Electron Diffraction Hydrothermal Synthesis CoFe2O4 NH4H2PO4 
These keywords were added by machine and not by the authors. This process is experimental and the keywords may be updated as the learning algorithm improves.

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Copyright information

© Springer Science+Business Media, LLC 2012

Authors and Affiliations

  • Trevor P. Almeida
    • 1
    • 2
    Email author
  • Michael W. Fay
    • 3
  • Yanqiu Zhu
    • 4
  • Paul D. Brown
    • 1
  1. 1.Division of Materials, Mechanics and Structures, Department of Mechanical, Materials and Manufacturing Engineering, Faculty of EngineeringThe University of Nottingham, University ParkNottinghamUK
  2. 2.Department of Earth Science and EngineeringImperial College LondonLondonUK
  3. 3.Nottingham Nanotechnology and Nanoscience CentreThe University of Nottingham, University ParkNottinghamUK
  4. 4.College of Engineering, Mathematics and Physical SciencesUniversity of ExeterExeterUK

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