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Crystal structure and cation distribution in Fe₇SiO₁₀ ("Iscorite")

¹ Institut für Angewandte Geowissenschaften, Technische Universität Darmstadt, Schnittspahnstr. 9, D-64287 Darmstadt, Germany
² Institut für Materialwissenschaften, Technische Universität Darmstadt, Petersenstr. 23, D-64287 Darmstadt, Germany
³ Institut für Mineralogie, Johann Wolfgang Goethe-Universität, Senckenberganlage 30, D-60054 Frankfurt am Main, Germany
⁴ Department of Geosciences, Virginia Tech, Blacksburg VA 24060–0420, USA

^* E-mail: vanaken{at}geo.tu-darmstadt.de

The mixed valence compound Fe²⁺₅Fe³⁺₂SiO₁₀, informally known as "iscorite", has been investigated by high-resolution and analytical transmission electron microscopy (HRTEM & ATEM) including energy-dispersive X-ray microanalysis (EDX) and electron energy-loss spectroscopy (EELS). EDX and EELS measurements confirm the chemical composition of the investigated sample yielding concentration ratios of Fe/Si = 7.1 and Fe³⁺/Fe = 0.29 ± 0.03 which resemble the expected ratios of Fe:Si = 7:1 and Fe³⁺/Fe = 2:7. The lattice parameters of the monoclinic cell given by Smuts et al. (1969) and Modaressi et al. (1985) were confirmed: a = 2.1336 nm, b = 0.30679 nm, c = 0.58744 nm, ß = 98.06°. However, space group I12/m1 (No.12) was found instead of the published space group P12₁/m1 (No.11).

In selected area electron diffraction (SAED) patterns in the orientation [01], streaking of the basic reflections and diffuse diffraction lines located at 1/2 (^* + ^*) parallel to the a direction are observed indicating an intense microstructural disorder. For the first time, we report the occurrence of twins on (200) in "iscorite". These structural modulations observed in SAED patterns and in Fourier-filtering analysis of the HRTEM images result from Fe³⁺/Si-disorder on tetrahedral sites and Fe²⁺/Fe³⁺-disorder on octahedral sites. Therefore, the crystal structure of "iscorite" has been described anew within the non-standard centrosymmetric space group I12/m1 by the use of the single-crystal X-ray diffraction (XRD) data of (Modaressi et al., 1985) in combination with our SAED and HRTEM results.

Key-words: "iscorite", analytical and high-resolution transmission electron microscopy, order-disorder, twinnining, structural modulation.