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@ARTICLE{Maity:278659,
      author       = {Maity, A. and Dutta, R. and Penkala, B. and Ceretti, M. and
                      Letrouit-Lebranchu, A. and Chernyshov, D. and Perichon, A.
                      and Piovano, A. and Bossak, A. and Meven, Martin and Paulus,
                      W.},
      title        = {{S}olid-state reactivity explored in situ by synchrotron
                      radiation on single crystals: from {S}r{F}e{O} 2.5 to
                      {S}r{F}e{O} 3 via electrochemical oxygen intercalation},
      journal      = {Journal of physics / D},
      volume       = {48},
      number       = {50},
      issn         = {1361-6463},
      address      = {Bristol},
      publisher    = {IOP Publ.},
      reportid     = {FZJ-2015-06984},
      pages        = {504004 -},
      year         = {2015},
      note         = {"final draft post referee" wird nicht zur Verfügung
                      gestellt.},
      abstract     = {In this study we demonstrate the feasibility of following
                      up a chemical reaction by single crystal x-ray (synchrotron)
                      diffraction under operando conditions, carried out in a
                      specially designed electrochemical cell mounted on the BM01A
                      at the European Synchrotron Radiation Facility (ESRF). We
                      investigated in detail the electrochemical oxidation of
                      SrFeO2.5 to SrFeO3 on a spherical single crystal of 70 μm
                      diameter by in situ diffraction at an ambient temperature.
                      Complete data sets were obtained by scanning the whole
                      reciprocal space using a 2M Pilatus detector, resulting in
                      3600 frames with a resolution of 0.1° per data set, each
                      obtained in 18 min. The crystal was mounted in a specially
                      designed electrochemical cell with 1N KOH used as the
                      electrolyte. During the electrochemical oxidation, the
                      reaction proceeds following the phase sequence
                      SrFeO2.5/SrFeO2.75/SrFeO2.875/SrFeO3, structurally
                      accompanied by establishing a complex series of long-range
                      oxygen vacancy ordering, which gets instantly organized at
                      ambient temperature. The topotactic reaction pathway is
                      discussed in terms of the evolution of the twin domain
                      structure. The formation of SrFeO2.875 is accompanied by the
                      formation of diffuse streaks along the [1 0 0]-direction of
                      the perovskite cell, reaching high d-spacings. The diffuse
                      streaks are discussed and are thought to originate from a
                      modified twin structure induced by the SrFeO2.75 to
                      SrFeO2.875 transition, and the associated changes in the
                      domain structure, developed during the oxygen intercalation.
                      We equally analysed and discussed in detail the twin
                      structure of all the title compounds. We confirm the ground
                      state of SrFeO2.5 is able to adopt the Imma space group
                      symmetry, showing stacking faults of the tetrahedral layers
                      along the stacking axis of the brownmillerite unit cell,
                      indicated by the 1D diffuse rods. We showed that in situ
                      single crystal diffraction has huge potential in the study
                      of nonstoichiometric compounds under operando conditions, in
                      order to obtain structural information i.e. about diffuse
                      scattering, and microstructural information related to
                      domain effects such as twinning—information far beyond
                      that which powder diffraction methods allow us to obtain.},
      cin          = {JCNS (München) ; Jülich Centre for Neutron Science JCNS
                      (München) ; JCNS-FRM-II / JCNS-2},
      ddc          = {530},
      cid          = {I:(DE-Juel1)JCNS-FRM-II-20110218 /
                      I:(DE-Juel1)JCNS-2-20110106},
      pnm          = {6G15 - FRM II / MLZ (POF3-6G15) / 6G4 - Jülich Centre for
                      Neutron Research (JCNS) (POF3-623)},
      pid          = {G:(DE-HGF)POF3-6G15 / G:(DE-HGF)POF3-6G4},
      experiment   = {EXP:(DE-MLZ)NOSPEC-20140101},
      typ          = {PUB:(DE-HGF)16},
      UT           = {WOS:000368443100006},
      doi          = {10.1088/0022-3727/48/50/504004},
      url          = {https://juser.fz-juelich.de/record/278659},
}