# US 12,180,609 B2 · Composite array electrode, preparation method thereof and use thereof

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- Number: US 12,180,609 B2
- Document ID: US12180609B2
- Status: Granted
- Kind: B2
- Application number: 17/841,189
- Filed: 2022-06-15
- Published: 2023-05-04
- Granted: 2024-12-31
- Earliest claimed: 2022-06-15
- Assignees: Shenzhen Institutes of Advanced Technology
- Applicants: Shenzhen Institutes of Advanced Technology
- Inventors: Qi Zeng; Tianzhun Wu
- Web page: https://patentgrep.com/patent/US12180609B2

## CPC

- A61B 5/14532: {for measuring glucose, e.g. by tissue impedance measurement}
- C25D 7/12: Semiconductors
- A61B 5/1468: using chemical or electrochemical methods, e.g. by polarographic means
- A61B 5/268: containing conductive polymers, e.g. PEDOT:PSS polymers
- A61N 1/05: for implantation or insertion into the body, e.g. heart electrode (A61N1/06 takes precedence)
- B08B 3/08: the liquid having chemical or dissolving effect
- B08B 7/028: {Using ultrasounds}
- C25D 3/50: of platinum group metals
- C25D 5/02: Electroplating of selected surface areas
- C25D 5/34: Pretreatment of metallic surfaces to be electroplated
- C25D 9/08: by cathodic processes
- C25D 13/22: Servicing or operating {apparatus or multistep processes}
- G01N 27/3278: {involving nanosized elements, e.g. nanogaps or nanoparticles (nanopores G01N33/48721; magnetic beads G01N27/745)}
- H10W 20/40: Interconnections external to wafers or substrates, e.g. back-end-of-line [BEOL] metallisations or vias connecting to gate electrodes
- A61B 2562/028: Microscale sensors, e.g. electromechanical sensors [MEMS]
- A61B 2562/04: Arrangements of multiple sensors of the same type
- A61B 2562/046: in a matrix array
- A61B 2562/125: characterised by the manufacture of electrodes
- A61N 1/0551: {Spinal or peripheral nerve electrodes}
- A61B: DIAGNOSIS; SURGERY; IDENTIFICATION (usefulness limited to only animals A61D)
- C25D: PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- A61N: ELECTROTHERAPY; MAGNETOTHERAPY; RADIATION THERAPY; ULTRASOUND THERAPY (measurement of bioelectric currents A61B; surgical instruments, devices or methods for transferring non-mechanical forms of energy to or from the body A61B18/00; anaesthetic apparatus in general A61M; incandescent lamps H01K; infrared radiators for heating H05B)
- B08B: CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- G01N: INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES (measuring or testing apparatus or processes other than immunoassay, involving enzymes or microorganisms C12M, C12Q)
- H10W: GENERIC PACKAGES, INTERCONNECTIONS, CONNECTORS OR OTHER CONSTRUCTIONAL DETAILS OF DEVICES COVERED BY CLASS H10

## Abstract

Provided are composite array electrode, preparation method thereof and use thereof. The composite array electrode comprises a microelectrode array substrate, and a modification layer formed on a surface of a microelectrode of the microelectrode array substrate, wherein the modification layer comprises a plurality of electrically conductive layers arranged at intervals on the surface of the microelectrode, an insulating layer arranged on the surface of the microelectrode except the electrically conductive layers, and wherein material for the electrically conductive layers comprises one or more of nano platinum, nano iridium, conductive polymer and carbon nanotubes. The composite array electrode effectively eliminates the influence of edge effect such that the electric field distributes uniformly on the microelectrode surface of the composite array electrode, significantly improving electrochemical performance and detection capability of the electrode.

## Claims

### Claim 1

A method for preparing a composite array electrode, comprising:
providing a microelectrode array substrate, the microelectrode of the microelectrode array substrate being provided with an insulating layer on the surface thereof; etching the insulating layer to form a plurality of holes spaced apart and penetrating the insulating layer; and
depositing an electrically conductive material in the holes to form an electrically conductive layer on the surface of the microelectrode by electrodeposition process, the electrically conductive material comprising (i) one or more of nano platinum and nano iridium, and (ii) carbon nanotubes;
wherein the carbon nanotubes are single-walled or multi-walled carbon nanotubes; and the carbon nanotubes have a pore size of 30 to 45 μm.

### Claim 2 (depends on 1)

The method of claim 1, after the step of etching the insulating layer and before performing the electrodeposition process, the method further comprising performing surface pretreatment on the etched microelectrode array substrate, and the step of performing surface pretreatment comprising:
cleaning ultrasonically the etched microelectrode array substrate in an acetone or ethanol solution for 20 to 60 minutes, followed by washing with deionized water and placing in a sulfuric acid solution for electrochemical cyclic voltammetry scanning under a voltage of −0.25V˜1.2V, at a scanning rate of 50˜200 mV/s, for a scanning time of 25˜60 min, until a coincident CV curve is obtained.

### Claim 3 (depends on 1)

The method of claim 1, wherein material for the insulating layer comprises one or more of polyimide, polydimethylsiloxane, polychloro-p-xylene, silica gel, polyurethane, silicone rubber and epoxy resin.

### Claim 4 (depends on 1)

The method of claim 1, when the electrically conductive material comprises nano platinum, the electrodeposition process comprises:
preparing a platinum salt solution; and
placing the surface-pretreated microelectrode array substrate in the platinum salt solution and performing electrodepositing such that an electrically conductive material is deposited in the holes to form the electrically conductive layer on the surface of the microelectrode,
wherein the platinum salt in the platinum salt solution comprises one or more of platinum chloride, ammonium hexachloroplatinate, potassium hexachloroplatinate, sodium hexachloroplatinate, chloroplatinic acid, platinum nitrate, platinum sulfate, potassium tetrachloroplatinate and ammonium tetrachloroplatinate, and the platinum salt solution has a pH of 6.5 to 7.5.

### Claim 5 (depends on 1)

The method of claim 1, when the electrically conductive material comprises nano iridium, the electrodeposition process comprises:
preparing an iridium salt solution; and
placing the surface-pretreated microelectrode array substrate in the iridium salt solution and performing electrodepositing such that an electrically conductive material is deposited in the holes to form the electrically conductive layer on the surface of the microelectrode,
wherein the iridium salt in the iridium salt solution comprises one or more of iridium chloride, chloroiridic acid, sodium hexachloroiridate and potassium hexachloroiridate, and the iridium salt solution has a pH of 6.5 to 7.5.

### Claim 6 (depends on 1)

The method of claim 1, wherein the holes have a cross-sectional shape of one or more of circle, triangle, quadrangle and polygon.

### Claim 7 (depends on 1)

The method of claim 1, wherein the holes have a lateral dimension of 6 to 60 μm.