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Nanostructured (CoxFe1– x)3–yO4 spinel – mechanochemical synthesis

  • E. Wu , S. J. Campbell EMAIL logo , W. A. Kaczmarek , M. Hofmann and S. J. Kennedy
Published/Copyright: February 7, 2022
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International Journal of Materials Research
From the journal International Journal of Materials Research Volume 94 Issue 10

Abstract

The effects of wet-milling mixtures of α-Fe2O3 and cobalt hydroxide Co(OH)2 over a range of Co/Fe ratios for 215 h have been investigated by neutron diffraction and Mössbauer spectroscopy. The starting materials were mixed according to the stoichiometric formula (CoxFe1 –x)3O4 for values of x = 0.037, 0.071, 0.133, 0.234 and 0.380 (i. e., from ≈ Co0.1Fe2.9O4 to the cobalt spinel CoFe2O4). These studies reveal the formation of a nanostructured, mixed Co–Fe spinel phase with non-stoichiometric composition (CoxFe1– x)3 –yO4; the defect spinels have refined values xc = 0.04, 0.08 and 0.14 for the mixtures with the lowest Co content (x = 0.037, 0.071 and 0.133) and defect concentrations in the range y ≈ 0.1 –0.2. Both the spinel phase and un-reacted α-Fe2O3 are found to occur in the neutron diffraction patterns and Mössbauer spectra for the high Co content mixtures x = 0.234 and x = 0.380. Rietveld refinements of the neutron data indicate that the Co atoms predominantly occupy the octahedral B sites with vacancies also found to be located on the octahedral B sites. Analyses of the Mössbauer spectra of the milled samples confirm the existence of vacancy defects in the B sites and reveal that the vacancies cause similar effects to those of the Co ions, leading to a higher average charge state per iron atom.

Keywords: Nanostructured ferrites; Mössbauer spectroscopy; Neutron diffraction; (CoxFe1 –x)3 –yO4
Prof. Stewart J. Campbell School of Physical, Environmental and Mathematical Sciences, UNSW at ADFA The University of New South Wales Australian Defence Force Academy Canberra, ACT 26000, Australia Tel.: +61 2 6268 8767 Fax: +61 2 6268 8786

(* present adress: Institute of Metal Research, Chinese Academy of Sciences, China)

(* former adress: Rutherford Appleton Laboratory, ISIS Facilities, UK)

Dedicated to Prof Dr. Dr. h. c. Herbert Gleiter on the occasion of his 65th birthday

  1. It is a pleasure to acknowledge the pioneering and definitive research undertaken by Prof. Dr. H. Gleiter in the field of nanostructured materials, and to acknowledge the contribution which he has made in helping to shape the direction of the work of SJC and his colleagues. We thank Dr. A. Studer, ANSTO, for helpful assistance with some of the neutron diffraction experiments. This work is supported in part by a grant from the Australian Research Council leading to the award of a Research Associateship. The project is also supported by a grant from the Australian Institute of Nuclear Science and Engineering.

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Received: 2003-04-01
Published Online: 2022-02-07

© 2003 Carl Hanser Verlag, München

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  2. Articles/Aufsätze
  3. From atomistics to macro-behavior: structural superplasticity in micro- and nano-crystalline materials
  4. Interface stress in nanocrystalline materials
  5. Microstructure, frequency and localisation of pseudo-elastic fatigue strain in NiTi
  6. Intercrystalline defects and some properties of electrodeposited nanocrystalline nickel and its alloys
  7. Positrons as chemically sensitive probes in interfaces of multicomponent complex materials: Nanocrystalline Fe90Zr7B3
  8. Annealing treatments to enhance thermal and mechanical stability of ultrafine-grained metals produced by severe plastic deformation
  9. Nanoceramics by chemical vapour synthesis
  10. Deformation mechanism and inverse Hall – Petch behavior in nanocrystalline materials
  11. Simulations of the inert gas condensation processes
  12. Unconventional deformation mechanism in nanocrystalline metals?
  13. Alloying reactions in nanostructured multilayers during intense deformation
  14. Impact of grain boundary character on grain boundary kinetics
  15. Nanostructured (CoxFe1– x)3–yO4 spinel – mechanochemical synthesis
  16. Nanostructure formation and thermal stability of nanophase materials prepared by mechanical means
  17. Low-temperature plasma nitriding of AISI 304 stainless steel with nano-structured surface layer
  18. New materials from non-intuitive composite effects
  19. On the line defects associated with grain boundary junctions
  20. Young’s modulus in nanostructured metals
  21. The kinetics of phase formation in an ultra-thin nanoscale layer
  22. Notifications/Mitteilungen
  23. Personal/Personelles
  24. News
  25. DGM Events
https://doi.org/10.1515/ijmr-2003-0204
Keywords for this article
Nanostructured ferrites; Mössbauer spectroscopy; Neutron diffraction; (CoxFe1 –x)3 –yO4

Articles in the same Issue

  1. Frontmatter
  2. Articles/Aufsätze
  3. From atomistics to macro-behavior: structural superplasticity in micro- and nano-crystalline materials
  4. Interface stress in nanocrystalline materials
  5. Microstructure, frequency and localisation of pseudo-elastic fatigue strain in NiTi
  6. Intercrystalline defects and some properties of electrodeposited nanocrystalline nickel and its alloys
  7. Positrons as chemically sensitive probes in interfaces of multicomponent complex materials: Nanocrystalline Fe90Zr7B3
  8. Annealing treatments to enhance thermal and mechanical stability of ultrafine-grained metals produced by severe plastic deformation
  9. Nanoceramics by chemical vapour synthesis
  10. Deformation mechanism and inverse Hall – Petch behavior in nanocrystalline materials
  11. Simulations of the inert gas condensation processes
  12. Unconventional deformation mechanism in nanocrystalline metals?
  13. Alloying reactions in nanostructured multilayers during intense deformation
  14. Impact of grain boundary character on grain boundary kinetics
  15. Nanostructured (CoxFe1– x)3–yO4 spinel – mechanochemical synthesis
  16. Nanostructure formation and thermal stability of nanophase materials prepared by mechanical means
  17. Low-temperature plasma nitriding of AISI 304 stainless steel with nano-structured surface layer
  18. New materials from non-intuitive composite effects
  19. On the line defects associated with grain boundary junctions
  20. Young’s modulus in nanostructured metals
  21. The kinetics of phase formation in an ultra-thin nanoscale layer
  22. Notifications/Mitteilungen
  23. Personal/Personelles
  24. News
  25. DGM Events
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