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Room-Temperature Synthesis, Hydrothermal Recrystallization, and Properties of Metastable Stoichiometric FeSe
Room-temperature precipitation from aqueous solutions yields the hitherto unknown metastable stoichiometric iron selenide (ms-FeSe) with tetragonal anti-PbO type structure. Samples with improved crystallinity are obtained by diffusion-controlled precipitation or hydrothermal recrystallization. The r...
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Published in: | Inorganic chemistry 2012-07, Vol.51 (13), p.7370-7376 |
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Main Authors: | , , , , , , , , |
Format: | Article |
Language: | English |
Citations: | Items that this one cites Items that cite this one |
Online Access: | Get full text |
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Summary: | Room-temperature precipitation from aqueous solutions yields the hitherto unknown metastable stoichiometric iron selenide (ms-FeSe) with tetragonal anti-PbO type structure. Samples with improved crystallinity are obtained by diffusion-controlled precipitation or hydrothermal recrystallization. The relations of ms-FeSe to superconducting β-FeSe1–x and other neighbor phases of the iron–selenium system are established by high-temperature X-ray diffraction, DSC/TG/MS (differential scanning calorimetry/thermogravimetry/mass spectroscopy), 57Fe Mössbauer spectroscopy, magnetization measurements, and transmission electron microscopy. Above 300 °C, ms-FeSe decomposes irreversibly to β-FeSe1–x and Fe7Se8. The structural parameters of ms-FeSe (P4/nmm, a = 377.90(1) pm, c = 551.11(3) pm, Z = 2), obtained by Rietveld refinement, differ significantly from literature data for β-FeSe1–x . The Mössbauer spectrum rules out interstitial iron atoms or additional phases. Magnetization data suggest canted antiferromagnetism below T N = 50 K. Stoichiometric non-superconducting ms-FeSe can be regarded as the true “parent” compound for the “11” iron-chalcogenide superconductors and may serve as starting point for new chemical modifications. |
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ISSN: | 0020-1669 1520-510X |
DOI: | 10.1021/ic300798p |