Study of the Iron-phosphorus-oxygen System by Mössbauer Effect, Neutron Diffraction, Magnetic Susceptibility, and Analytical Electron Microscopy: Some Pitfalls and Solutions in the Analysis of a Complex Mixture
A sample of FePO4 has been characterized by powder X-ray and neutron diffraction techniques, Mössbauer spectroscopy, magnetic susceptibility, and analytical electron microscopy. The analysis by diffraction methods is misleading and indicates that the sample is pure, but analytical electron microscopy shows that the material is triphasic and contains, in addition to FePO4, a glassy component of approximate composition Fe3P5O17 and a small amount of Fe7(PO4)6, a mixed valence compound. The Mössbauer-effect spectra indicate that the material contains approximately 30% of the glass and approximately 2% of Fe7(PO4)6. The Mössbauer spectra give the expected results for FePO4 and confirm that it orders magnetically at 23.8 K. The glassy component orders at ca. 7 K, whereas Fe7(PO4)6 remains paramagnetic down to ca. 10 K. The magnetic susceptibility data show ordering of FePO4 and the glassy component at 24 and ca. 7 K, respectively. The combination of these various techniques has permitted a detailed description of this complex mixture. © 1983 American Chemical Society.
G. J. Long et al., "Study of the Iron-phosphorus-oxygen System by Mössbauer Effect, Neutron Diffraction, Magnetic Susceptibility, and Analytical Electron Microscopy: Some Pitfalls and Solutions in the Analysis of a Complex Mixture," Inorganic Chemistry, American Chemical Society (ACS), Jan 1983.
The definitive version is available at https://doi.org/10.1021/ic00163a007
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© 1983 American Chemical Society (ACS), All rights reserved.