Abstract
The Fe M2,3-edge spectra of solid solutions of garnets (almandine-skiagite Fe3(Al1–xFex)2[SiO4]3 and andradite-skiagite (Fe1–xCax)3Fe2[SiO4]3), pyroxenes (acmite-hedenbergite (Ca1–xNax)(Fe2+1−xFe3+x)Si2O6), and spinels (magnetite-hercynite Fe(Al1–xFex)2O4) have been measured using the technique of parallel electron energy-loss spectroscopy (EELS) conducted in a transmission electron microscope (TEM). The Fe M2,3 electron energy-loss near-edge structures (ELNES) of the minerals exhibit a characteristic peak located at 4.2 eV and 2.2 eV for trivalent and divalent iron, respectively, prior to the main maximum at about 57 eV. The intensity and energy of the pre-edge feature varies depending on Fe3+/ΣFe. We demonstrate a new quantitative method to extract the ferrous/ferric ratio in minerals. A systematic relationship between Fe3+/ΣFe and the integral intensity ratio of the main maximum and the pre-edge peak of the Fe M2,3 edge is observed. Since the partial cross sections of the Fe M2,3 edges are some orders of magnitude higher than those of the Fe L2,3 edges, the Fe M2,3 edges are interesting for valence-specific imaging of Fe. The possibility of iron valence-specific imaging is illustrated by Fe M2,3-ELNES investigations with high lateral resolution from a sample of ilmenite containing hematite exsolution lamellae that shows different edge shapes consistent with variations in the Fe3+/ΣFe ratio over distances on the order of 100 nm.
Published Version
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