Fig. 2: Operando probing of solid-liquid interfaces on Ni LGNPs using PE-RSoXS.
a Schematic illustrations of the sample chip supporting the three-electrode circuit in the liquid flow cell, along with the corresponding scanning electron microscopy (SEM) image of the Ni LGNPs on the SiNx windows on the sample chip. Scale bar, 200 nm. b Diffraction patterns from charge-coupled device (CCD) images measured at open circuit potential (OCP), 1.2 V and 1.6 V at 852 eV of the photon energy, and c the corresponding diffraction intensity profiles (solid round points) measured at 852 and 860.1 eV, respectively, with the fitting results (crosses). Scattering-derived spectra from the d 3rd, e 4th, and f 5th orders measured at OCP, 1.2 and 1.6 V, respectively, near the Ni L-edge with simulation results based on the finite-element-method (FEM) models. g Cross-sectional models of the gratings for FEM simulations at OCP, 1.2 V and 1.6 V, with the color maps of the components in the models. All the electrochemical measurements were conducted using 0.1 M NaOH aqueous solution flow with a flow rate of 250 µL h−1 at the room temperature without iR correction.
