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Electrochemical cell for neutron reflectometry studies of the structure of ionic liquids at electrified interface
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Image of FIG. 1.
FIG. 1.

(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.

Image of FIG. 2.
FIG. 2.

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.

Image of FIG. 3.
FIG. 3.

Diffractogram recorded of the gold surface using grazing incidence x-ray diffraction. Each peak corresponds to a distinct crystalline plane.

Image of FIG. 4.
FIG. 4.

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.

Image of FIG. 5.
FIG. 5.

(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.


Generic image for table
Table I.

Theoretical x-ray scattering length densities of all surface components. The absorption terms are not included here.


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752b84549af89a08dbdd7fdb8b9568b5 journal.articlezxybnytfddd
Scitation: Electrochemical cell for neutron reflectometry studies of the structure of ionic liquids at electrified interface