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The Transformation of Lepidocrocite During Heating: A Magnetic and Spectroscopic Study

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Clays and Clay Minerals

Abstract

Infrared (IR) spectroscopy, in combination with magnetic methods, was used to study the thermally induced transformation of synthetic lepidocrocite (γ-FeOOH) to maghemite (γ-Fe2O3). Magnetic analyses showed that the thermal conversion began at about 175°C with the formation of superparamagnetic maghemite clusters. The overall structural transformation to ferrimagnetic γ-Fe2O3 occurred at 200°C and was complete around 300°C. At higher temperatures, the maghemite converted into hematite (α-Fe2O3). Observation of the transformation from γ-FeOOH to γ-Fe2O3 using variable-temperature IR spectroscopy indicated that dehydroxilation on a molecular level was initiated between 145°C and 155°C. The lag time between the onset of the breaking of OH bonds and the release of H2O from lepidocrocite around 175°C can be explained by diffusive processes. Overall dehydroxilation and the subsequent breakdown of the lepidocrocite structure was complete below 219°C. The comparison of the magnetic and IR data provides evidence that the dehydroxilation may precede the structural conversion to maghemite.

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References

  • Chopelas, A. and Hofmeister, A. M. (1991) Vibrational spectroscopy of aluminate spinels at 1 atm and of MgAl2O4 to over 200 kbar: Phys. Chem. Miner. 18, 279–293.

    Article  Google Scholar 

  • Farmer, V. C. (1974) The Infrared Spectra of Minerals: Mineralogical Society, London.

    Book  Google Scholar 

  • Gehring, A. U. and Karthein, R. (1989) ESR study of Fe(III) and Cr(III) hydroxides: Naturwissenschaften 76, 172–173.

    Article  Google Scholar 

  • Gehring, A. U., Karthein, R., and Relier, A. (1990) Activated state in the lepidocrocite structure during thermal treatment: Naturwissenschaften 77, 177–179.

    Article  Google Scholar 

  • Glemser, O. (1938) Über Darstellung und katalystische Wirksamkeit von reinem 7-FeOOH und daraus gewonnenen γ-Fe2O3: Ber. Dtsch. chem. Ges. 71, 158–163.

    Article  Google Scholar 

  • Gómez-Villacieros, R., Hernán, L., Morales, J., and Tirado, J. L. (1984) Textural evolution of synthetic γ-FeOOH during thermal treatment by different scanning calorimetry: J. Coll. Interf. Sci. 101, 392–1400.

    Article  Google Scholar 

  • Hedley, I. G. (1968) Chemical remanent magnetization of the FeOOH, Fe2O3 system: Phys. Earth Planet. Inter. 1, 103–121.

    Article  Google Scholar 

  • Hofmeister, A. M. (1991) Comment on “Infrared spectroscopy of the polymorphic series (enstatite, ilmenite, and perovskite) of MgSiO3, MgGeO3, and MnGeO3,” by M. Madon and G. D. Price: J. Geophys. Res. 96, 21959–21964.

    Article  Google Scholar 

  • Hofmeister, A. M., Rose, T. B., Hoering, T. C., and Kushiro, I. (1992) Infrared spectroscopy of natural, synthetic, and 18O substituted α-tridymite: Structural implications: J. Phys. Chem. 96, 10213–10218.

    Article  Google Scholar 

  • Joint Committee on Powder Diffraction Standards (JCPDS. (1980) Mineral Powder Diffraction File, Data Book: JCPDS International Center for Diffraction Data, Swarthmore, Pennsylvania.

    Google Scholar 

  • Lebel, P. (1985) Inbetriebnahme und Verwendung einer Curiewaage: Diploma thesis, ETH Zürich, 73 pp.

    Google Scholar 

  • Lewis, D. G. and Farmer, V. C. (1986) Infrared absorption of surface hydroxyl groups and lattice vibration in lepidocrocite (γ-FeOOH) and boethmite (γ-AlOOH): Clay Miner. 21, 93–100.

    Article  Google Scholar 

  • Martin D. H. (1967) Magnetism in Solids: MIT Press, Cambridge, Mass.

    Google Scholar 

  • McDevitt, N.T. and Baun, W. L. (1964) Infrared absorption study of metal oxides in the low frequency region (700-240 cm-1): Spectrochim. Acta 20, 799–808.

    Article  Google Scholar 

  • McMillan, P. F. and Hofmeister, A. M. (1988) Infrared and Raman spectroscopy: in Spectroscopic Methods in Mineralogy and Geology, F.C. Hawthorne, ed., Reviews in Mineralogy 18, 99–160.

    Article  Google Scholar 

  • Morris, R. V., Lauer, H. V., Lawson, C. A., Gibson, E. K., Nace, G. A., and Stewart, C. (1985) Spectral and other physicochemical properties of submicron powders of hematite (α-Fe2O3), maghemite (γ-Fe2O3), goethite (α-Fe-OOH), and lepidocrocite (γ-FeOOH): J. Geophys. Res. 90, 3126–3144.

    Article  Google Scholar 

  • Nakamoto, K., Maargoshes, M., and Rundle, R. E. (1955) Stretching frequencies as a function of distances in hydrogen bonds: J. Am. Chem. Soc. 77, 6480–6488.

    Article  Google Scholar 

  • Schwertmann, U. (1989) Occurrence and formation of iron oxides in various pedeoenvironments: in Iron in Soils and Clay Minerals, J. W. Stucki, B. A. Goodman, and U. Schwertmann, eds., Reidel, Dordrecht, 267–308.

    Google Scholar 

  • Schwertmann, U. and Taylor, R. M. (1972) The transformation of lepidocrocite to goethite: Clays & Clay Minerals 20, 151–158.

    Article  Google Scholar 

  • Serna, C. J., Rendon, J. L., and Iglesias, J. E. (1982) Infrared surface modes in corrundum-type microcrystalline oxides: Spectrochim. Acta 38, 797–802.

    Article  Google Scholar 

  • Subrt, J., Hanousek, F., Zapletal, V., Lipka, J., and Hucl, M. (1981) Dehydration of synthetic lepidocrocite (γ-FeOOH): J. Thermal. Anal. 20, 61–69.

    Article  Google Scholar 

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Gehring, A.U., Hofmeister, A.M. The Transformation of Lepidocrocite During Heating: A Magnetic and Spectroscopic Study. Clays Clay Miner. 42, 409–415 (1994). https://doi.org/10.1346/CCMN.1994.0420405

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  • DOI: https://doi.org/10.1346/CCMN.1994.0420405

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