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Figure 7
XAS results obtained in situ and in operando by means of the 3D-printed electrochemical devices. Two different types of sample have been considered: electrodes onto which the IrOx film was electrodeposited (a, b, c) and electrodes onto which the IrOx film was photo-electrodeposited (d). (a) Ir LIII XANES spectra acquired in situ at two different potential values: 0.4 V (red line) and 1.4 V (green line) versus RHE. The spectra of IrCl3 (black line) and IrO2 (blue line) standard materials are plotted as references for Ir(III) and Ir(IV), respectively. (bc) Ir LIII normalized XANES spectra acquired at a constant potential value equal to 0.4 V (b) and to 0.8 V (c) under UV–Vis light conditions (red line) and dark conditions (blue line), and the respective differences (black lines) obtained from the subtraction of the spectrum under dark conditions from that acquired under UV–Vis light conditions. (d) Response of the photoanode to the illumination by UV–Vis light when the IrOx layer is prepared by photo-electrodeposition, recorded at a potential of 1.56 V relative to RHE. The signal is different between the XANES spectrum recorded in the presence and that recorded in the absence of the UV–Vis illumination (light − dark).

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