Porous electrodes for spectroelectrochemistry and x-ray structure analyses

Patent metadata

Field	Value
Publication number	US-10273593-B2
Application number	US-201615221167-A
Country	US
Kind code	B2
Filing date	Jul 27, 2016
Priority date	Jul 27, 2016
Publication date	Apr 30, 2019
Grant date	Apr 30, 2019

Abstract

An electrochemical cell that allows for in-situ structural characterization of amorphous thin film materials during the course of electrolysis using high-energy X-ray scattering (>50 keV). The compact and versatile cell employs a three-electrode configuration and minimizes X-ray scattering contributions from the cell, reference and counter electrodes, as well as the working electrode support. A large surface area working electrode has a physically robust support and is largely transparent to X-rays. This design, which utilizes a three-dimensional working electrode, also greatly improves the intensity and quality of the scattered signal compared to a two-dimensional working electrode. The in-situ cell can be used not only to investigate structural evolution during electrolysis using X-ray scattering (e.g. pair distribution function), but also to perform electrochemical potential-dependent structural analysis by extended X-ray absorption fine structure.

First claim

What is claimed is:

1. An article of manufacture comprising:
an in-situ cell comprising:
at least three electrodes including a working electrode (W.E.), a reference electrode (R.E.), and a cell electrode (C.E.), the C.E. configured to receive current and in electrical communication with the W.E. whereby electrodeposition within the in-situ cell occurs at the W.E., the R.E. in electrical communication with the W.E. and configured to measure potential therebetewen;
the W.E. comprising a glass capillary array having a conformal conductive layer;
a film over the W.E., the W.E. and film defining a W.E. electrolyte region;

an electrolyte system including an electrolyte line and an electrolyte source in fluid communication with the in-situ cell.

2. The article of manufacture of claim 1 , wherein the glass capillary array is a microporous glass capillary array having pores with a diameter of 40 μm or less and at least a 20 mm 2 surface area.

3. The article of manufacture of claim 2 , wherein the conformal conductive layer is less than 70 nm thick.

4. The article of manufacture of claim 1 , wherein the W.E. further comprises a metallic layer deposited on the glass capillary array opposite the conductive layer.

5. The article of manufacture of claim 1 , wherein the conformal conductive layer is less than 50 nm thick.

6. The article of manufacture of claim 1 , wherein the W.E. electrolyte region has a cross-section shape selected from half-moon, semi-elliptical, and semi-circular.

7. The article of manufacture of claim 1 , wherein the film is 7.5 μm thick.

8. The article of manufacture of claim 1 , wherein the electrolyte system further including a stirrer associated with the electrolyte source and configured to stir electrolyte in the electrolyte source.

9. The article of manufacture of claim 1 , wherein the electrolyte system further comprises a pump.

Assignees

• Uchicago Argonne Llc

Inventors

• Kwon Gihan
• Emery Jonathan D
• Kim In Soo
• Martinson Alex B
• Tiede David M

Classifications

• G01N2223/61

  thin films, coatings · CPC title

• C25D17/12 Primary

  Shape or form (C25D17/14 takes precedence) · CPC title

• C25B1/04

  by electrolysis of water · CPC title

• C25D17/02

  Tanks; Installations therefor · CPC title

• G01N23/20

  by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials · CPC title