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

Abstract

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.

In‐situ Scanning Transmission X‐Ray Microscopy of Catalytic Solids and Related Nanomaterials

“…[60] The cell is equipped with an anode or cathode that can in principle be manufactured of any conductor. In their experiment the group followed the electrodeposition of Ni on an Au film.…”

Fabrication and testing of an electrochemical microcell for in situ soft X-ray microspectroscopy measurements

“…In particular, as a simple demostrative test case, with no claim of specific materials-science interest, we studied Au corrosion in an RTIL electrolyte and we recorded images of mesoscopic features of Au corrosion product organisation. configuration described in [4][5][6][7], since the sealing method is not impacted by the new electrode system. The potential applications are stability of materials for fuel-cells and sensors.…”

“…Of course, the stringent sample requirements of techniques based on transmission of soft X-rays impose severe constraints to in situ operation. As far as electrochemical cells are concerned, two types of concepts have been described so far in the literature: the pioneering two electrode system with polymeric electrolyte proposed in the seminal paper [3] and the Si 3 N 4 -supported, cells with lithographed square electrodes employed by the authors in [4][5][6][7][8][9]. The latter system has allowed in situ dynamic work both with sealed, aqueous electrolytes [4][5][6][7] and with open, room-temperature ionic-liquids (RTIL) [8,9]; nevertheless, the poor current density (c.d.)…”

Development and application of in situ/operando soft X-ray transmission cells to aqueous solutions and catalytic and electrochemical reactions

“…On the other hand, in the soft X-ray region, several groups have developed electrochemical cells for XAS of light elements such as C, N, and O (1s), and Mn and Fe (2p) in fluorescence yields [222,223]. The in situ spatial measurement by scanning transmission X-ray microscope (STXM) is applied to the electrochemical reaction [224][225][226]. However, it is still difficult to measure in operando XAS of electrolytes in transmission mode during the electrochemical reaction.…”