Electrochemical detection of gas phase chemicals

Patent metadata

Field	Value
Publication number	US-11378547-B1
Application number	US-201916572978-A
Country	US
Kind code	B1
Filing date	Sep 17, 2019
Priority date	Sep 27, 2018
Publication date	Jul 5, 2022
Grant date	Jul 5, 2022

Abstract

We provide an electrochemical sensor in which working microelectrodes are arranged in an array and interconnected in parallel. The working electrodes are arranged so that in use, they are electrochemically coupled to a counter electrode structure through an electrolyte. The sensor also includes a microporous body arranged so that in use, it is situated at a boundary between a gaseous environment and the electrolyte. In another aspect, we provide a method of sensing in which a sample of gas is admitted to a liquid electrolyte maintained by pores of a porous substrate. A voltage is applied to the liquid electrolyte, and an electrical response to the applied voltage is observed, thereby to detect electrochemical evidence of an analyte within the liquid electrolyte.

First claim

We claim:

1. An electrochemical sensor, comprising:
a plurality of working nanoelectrodes arranged in an array and interconnected in parallel;
a counter electrode structure; and
a nanoporous body, wherein:
the counter electrode structure or a further electrode structure is configured to serve as a reference electrode;
at least a portion of the nanoporous body is configured to be exposed to a gaseous environment;
at least a portion of the nanoporous body is configured to contain an electrolyte, a boundary between the gaseous environment and the electrolyte being situated within or adjacent to the nanoporous body;
the working nanoelectrodes are configured to be electrochemically coupled to the counter electrode structure through the electrolyte; and
the nanoporous body is a layer of anodized aluminum oxide (AAO) perforated with an array of mutually parallel nanopores extending from a front face to a back face thereof.

2. The electrochemical sensor of claim 1 , wherein the working nanoelectrodes are situated wholly or partially within nanopores of the nanoporous body.

3. The electrochemical sensor of claim 1 ,
wherein the nanoporous body has a front face configured to be exposed to the gaseous environment, and
wherein the nanoporous body has a back face configured to be exposed to an enclosed fill volume for the electrolyte.

4. The electrochemical sensor of claim 1 ,
wherein the nanoporous body has a front face configured to be exposed to the gaseous environment, and
wherein the nanoporous body is configured to electrochemically couple the working nanoelectrodes to the counter electrode structure through electrolyte contained within nanopores of the nanoporous body.

5. The electrochemical sensor of claim 1 , further comprising a preconcentrator layer configured to release a preconcentrated analyte onto a path between the gaseous environment and the working nanoelectrodes.

6. The electrochemical sensor of claim 5 , wherein the preconcentrator layer is configured to be outside of the electrolyte.

7. The electrochemical sensor of claim 5 , wherein the preconcentrator layer is configured to be within the electrolyte.

8. The electrochemical sensor of claim 5 , wherein the preconcentrator layer comprises a porous metal selected to be electrochemically reactive to an analyte that is to be detected.

9. The electrochemical sensor of claim 5 , wherein the preconcentrator layer comprises a preconcentrator material chosen to capture a desired analyte from the gaseous environment and to preconcentrate the desired analyte.

10. The electrochemical sensor of claim 5 , further comprising an electric heater thermally connected to the preconcentrator layer, whereby energizing the electric heater releases analyte from the preconcentrator layer.

11. The electrochemical sensor of claim 5 , further comprising a pressurizer or depressurizer in fluidic contact with an atmosphere surrounding the preconcentrator layer, whereby activating the pressurizer or depressurizer releases analyte from the preconcentrator layer.

12. The electrochemical sensor of claim 5 , wherein:
the preconcentrator layer comprises a porous metal electrode; and
said porous metal electrode is configured to drive concentration of an analyte upon energizing by a first relative voltage and is configured to drive release of the analyte upon energizing by a second relative voltage.

13. The electrochemical sensor of claim 12 ,
wherein the first relative voltage is between the porous metal electrode and the counter electrode structure, and
wherein the second relative voltage is between the porous metal electrode and the working nanoelectrodes.

14. A sensing method, comprising:
admitting a gas sample to a liquid electrolyte maintained by nanopores of a nanoporous substrate, the nanoporous substrate including a layer of anodized aluminum oxide (AAO) perforated with an array of mutually parallel nanopores extending from a front face to a back face thereof;
applying a voltage to the liquid electrolyte; and
observing an electrical response to the applied voltage, thereby to detect electrochemical evidence of an analyte within the liquid electrolyte.

15. The sensing method of claim 14 , wherein the liquid electrolyte is a product of capillary condensation within the nanopores from an ambient gaseous atmosphere.

16. The sensing method of claim 14 ,
wherein analyte within the gas sample is captured and preconcentrated by a preconcentrator material, and
the sensing method further comprises releasing the preconcentrated analyte from the preconcentrator material into the liquid electrolyte.

17. The sensing method of claim 16 , wherein the releasing of the preconcentrated analyte is performed by heating the preconcentrator material or by causing a change in pressure on the preconcentrator material.

18. The sensing method of claim 16 , wherein the analyte within the gas sample is captured in the liquid phase and preconcentrated by a chemical or electrochemical reaction with the preconcentrator material.

19. The sensing method of claim 16 , wherein the releasing of the preconcentrated analyte from the preconcentrator material is performed by driving an electrochemical reaction.

20. The sensing method of claim 16 , wherein:
the analyte within the gas sample is captured and preconcentrated by at least a first and a second preconcentrator material;
heat or pressure is used to release the preconcentrated analyte from the first preconcentrator material so that it then interacts with the second preconcentrator material; and
an electrochemical reaction is used to release the preconcentrated analyte from the second preconcentrator material into the liquid electrolyte.

Assignees

• Nat Tech & Eng Solutions Sandia Llc

Inventors

• Klavetter Kyle Chris
• Yelton William G
• Nenoff Tina M
• Siegal Michael P
• Perez Carlos R

Classifications

• G01N27/404

  Cells with anode, cathode and cell electrolyte on the same side of a permeable membrane which separates them from the sample fluid {, e.g. Clark-type oxygen sensors} · CPC title

• C25D11/045 Primary

  for forming AAO templates · CPC title

• G01N27/403

  Cells and electrode assemblies · CPC title

• G01N27/301

  Reference electrodes · CPC title

• G01N27/304

  Gas permeable electrodes · CPC title