An in Situ Synchrotron-Based Soft X-ray Microscopy Investigation of Ni Electrodeposition in a Thin-Layer Cell

X-ray techniques allow one to carry out imaging with nanometric resolution in situ, during electrodeposition processes. In this paper, we describe the pioneering application of soft X-ray microscopy to Ni electrodeposition from ammonium and chloride solutions. Morphological features typical of the relevant electrochemical process in a thin-layer cell were successfully imaged and followed dynamically as a function of the applied electrochemical polarization. In particular, grainy films, dendrites, and blisters were detected and their locations were rationalized in terms of current density distribution. Furthermore, the electrochemical system implemented at the TwinMic beamline has been proved to support in situ spectroscopic work that will be described in a subsequent publication.