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In-situ electrochemical X-ray diffraction: A rigorous method to navigate within phase diagrams reveals β-Fe1+xSe as superconductor for all x

DOI: 10.1002/anie.201907426 DOI Help

Authors: Bertold Rasche (University of Oxford) , Minjun Yang (University of Oxford) , Lothar Nikonow (University of Oxford) , Joshaniel F. K. Cooper (ISIS Neutron and Muon Source) , Claire A. Murray (Diamond Light Source) , Sarah J. Day (Diamond Light Source) , Karin Kleiner (Diamond Light Source) , Simon J. Clarke (University of Oxford) , Richard G. Compton (University of Oxford)
Co-authored by industrial partner: No

Type: Journal Paper
Journal: Angewandte Chemie International Edition

State: Published (Approved)
Published: August 2019
Diamond Proposal Number(s): 20638

Abstract: We report the precise postsynthetic control of the composition of β‐Fe1+xSe by electrochemistry with simultaneous tracking of the associated structural changes via in‐situ synchrotron X‐ray diffraction. We access the full phase width of 0.01 < x < 0.04 and identify the superconducting state below 8 K, which in contrast to earlier reports is independent of the composition. However, in a second set of in‐situ X‐ray diffraction experiments, we demonstrate that β‐Fe1+xSe forms a new phase in the presence of oxygen above a 100 °C which has the same anti‐PbO type structure but is not superconducting down to 1.8 K. The latter process can be reversed electrochemically to reinstate the superconducting state. These observations exploit the exquisite control afforded by electrochemistry in contrast with classical approaches of chemical synthesis.

Journal Keywords: Electrochemistry; In-situ X-ray diffraction; Superconductors; iron selenide; Phase transitions

Subject Areas: Chemistry, Physics


Instruments: I11-High Resolution Powder Diffraction