Abstract

A rapid X-ray diffraction method was proposed for in situ observation of a surface-intermediate structure on a liquid–solid interface. It used a combination of higher-energy monochromatic synchrotron X-rays in grazing incidence and an X-ray two-dimensional detector. Overall patterns were in situ taken, with one-time exposure, of the reciprocal-lattice space of a Au (1 1 1) electrode surface which was fixed at an angular position. We deduced change in crystal domain shapes of surface intermediates as well as its smaller lattice distortion by observing images of reconstructed surface rods during a surface-structural phase transition from the reconstructed surface to the bulk terminated surface. An anisotropic shape of surface-crystal domains was also observed.

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