(a) Schematic of the cell: ❶ 10 mm thick stainless steel clamp-rings [155 mm outer diameter (OD), 125 mm inner diameter (ID)]; ❷ 15 mm Teflon® base (125 mm OD, 100 mm ID); ❸ 0.76 mm thick Kalrez® gasket (100 mm OD, 80 mm ID) with fluid ports; ❹ 4 mm thick TEC 7™ glass counter electrode with fluid ports (100 mm diameter), coated with a conducting film of fluorine-doped tin oxide; ❺ 10 mm thick Si–Cr–Au working electrode (100 mm diameter); clamping screw holes; Luer-Lok® syringe port to inject liquid; , , holes for ionic liquid inlet; Luer-Lok® syringe port to eject liquid; , , holes for ionic liquid outlet; hole for reference electrode. (b) top: schematic of a fully assembled cell; bottom: the actual cell. (c) Schematic of the gold electrode: ❶ 250 nm Au layer, ❷ 25 nm adhesive Cr layer; ❸ 10 mm Si wafer. Inset: the actual gold electrode used in the experiment.
XRR curve for the Si–Cr–Au surface. The measured reflectivity data are presented as circles, with the fit as a continuous. The fit residuals are plotted above. Inset: the corresponding SLD profile of the surface based on the fitted model.
Diffractogram recorded of the gold surface using grazing incidence x-ray diffraction. Each peak corresponds to a distinct crystalline plane.
The setup of NR beamline at ANSTO (Platypus) to probe ionic liquid structures at electrified interface: ❶ origin of the neutron beam; ❷ inlet toward the scattered neutron detector; ❸ sample station; ❹ potentiostat connected to the electrochemical cell; ❺ automatic elevator and rotator for table adjustment. Inset: electrochemical cell (from above), (a) cable to glass counter electrode; (b) cable to gold (working) electrode; (c) silver (reference) electrode; (d) cable to reference electrode; (e) syringe for ionic liquid injection; (f) syringe for ionic liquid extraction.
(a) (top) NR curves for ionic liquid at −1.0 V (△) and (▽) vs silver wire pseudoreference electrode. The lines through the data points are guides to the eye. Also shown is a theoretical curve for no surface excess of either ion. (b) (Bottom) Simulated reflectivity curves for the same system representing surface excesses of either cation or anion, in the 10 Å closest to the Au electrode. Also shown is the test case for no surface excess of either ion.
Theoretical x-ray scattering length densities of all surface components. The absorption terms are not included here.
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