CN115058690A - Manufacturing method of glucose sensor - Google Patents

Manufacturing method of glucose sensor Download PDF

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Publication number
CN115058690A
CN115058690A CN202210567302.1A CN202210567302A CN115058690A CN 115058690 A CN115058690 A CN 115058690A CN 202210567302 A CN202210567302 A CN 202210567302A CN 115058690 A CN115058690 A CN 115058690A
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China
Prior art keywords
evaporation
gold film
glucose sensor
electrode
substrate
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CN202210567302.1A
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Chinese (zh)
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杨印江
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Small Nurse Tianjin Technology Co ltd
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Small Nurse Tianjin Technology Co ltd
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Priority to CN202210567302.1A priority Critical patent/CN115058690A/en
Publication of CN115058690A publication Critical patent/CN115058690A/en
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    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14Metallic material, boron or silicon
    • C23C14/18Metallic material, boron or silicon on other inorganic substrates
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05Metallic powder characterised by the size or surface area of the particles
    • B22F1/054Nanosized particles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/16Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y15/00Nanotechnology for interacting, sensing or actuating, e.g. quantum dots as markers in protein assays or molecular motors
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24Vacuum evaporation
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/58After-treatment
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis

Abstract

The application provides a manufacturing method of a glucose sensor, which comprises the following steps: selecting sand paper as a vapor deposition substrate; placing the evaporation substrate in a vacuum environment, and evaporating a gold film on the evaporation substrate through evaporation; placing the evaporation gold film in the chloroauric acid solution, scanning for multiple times by a cyclic voltammetry method, and generating gold nanoparticles on the evaporation gold film; and placing the evaporation gold film in ozone, irradiating the evaporation gold film by ultraviolet rays, cutting the evaporation gold film by a preset size, taking the cut evaporation gold film as a sensor contact piece, and assembling a working electrode, a counter electrode and a reference electrode in a three-electrode sensor mode to form the glucose sensor. This application passes through abrasive paper as the coating by vaporization substrate in the manufacturing process of coating by vaporization gold film, the flow greatly simplifies, and the yield is high, and the working electrode simple structure who forms has reduced the production degree of difficulty, therefore very big reduce cost.

Description

Manufacturing method of glucose sensor
Technical Field
The application provides a manufacturing technology of a sensor, and particularly relates to a manufacturing method of a glucose sensor.
Background
With the increasing living standard, diabetes becomes a chronic disease worldwide, and related diseases such as stroke, renal failure, heart disease and the like are brought about. Glucose is the main molecule for diabetes monitoring, and the concentration change of glucose has a crucial effect on human health. Accurate measurement of glucose is also of profound significance for future preventive medical diagnostics, food safety, environmental monitoring, pharmaceutical analysis and biotechnology.
In the prior art, there have been some research results on electrochemical sensors based on gold materials for detecting glucose under neutral conditions, but most blood glucose monitoring is based on rigid-based research, these sensors are difficult to apply to sweat sensors that can be attached to the skin, and require a low detection limit to detect trace amounts of glucose in sweat, which is related to the electrocatalytic activity of the metallic material.
Currently, studies on the mechanism of glucose oxidation in gold electrodes have shown that the surface of gold can induce the production of hydroxyl-adsorbing layers (OHads) to carry out the dehydrogenation step in the mechanism of glucose oxidation reaction. Meanwhile, oxygen functional groups near the Au active surface can also induce OHads through non-covalent interactions. Thus, more OHads can stimulate a faster dehydrogenation reaction, thereby speeding up the overall reaction process. Using the above principles, current technology is able to detect glucose in sweat by using nanogold and a (rGO-PU) support matrix with oxygen-containing functional groups. However, this method requires a catalytic life of one week, and the complicated synthesis process of the nano-hybrid fiber makes the manufacturing process complicated and costly.
Disclosure of Invention
In order to solve one or more problems in the prior art, the present application provides a method for manufacturing a glucose sensor.
The application provides a method for manufacturing a glucose sensor, which comprises the following steps
Selecting sand paper as a vapor deposition substrate;
placing the evaporation substrate in a vacuum environment, and evaporating a gold film on the evaporation substrate through evaporation;
placing the evaporation gold film in the chloroauric acid solution, scanning for multiple times by a cyclic voltammetry method, and generating gold nanoparticles on the evaporation gold film;
and placing the evaporation gold film in ozone, irradiating the evaporation gold film by ultraviolet rays, cutting the evaporation gold film by a preset size, taking the cut evaporation gold film as a sensor contact piece, and assembling a working electrode, a counter electrode and a reference electrode in a three-electrode sensor mode to form the glucose sensor.
Optionally, the sandpaper is 500-mesh or 800-mesh silicon carbide sandpaper.
Optionally, the concentration of the chloroauric acid solution is 0.05-0.2 mol/L.
Optionally, the working time of the cyclic voltammetry is 100s to 500 s.
Optionally, the scanning rate is 0.05-0.15V/s.
Optionally, the number of scanning cycles is 45-55.
Optionally, the evaporated gold film is placed in ozone, and the irradiation time of ultraviolet light is not more than 40 min.
Optionally, the thickness of the evaporated gold film is 100 nm.
Optionally, the performing device of cyclic voltammetry is an electrochemical workstation.
The present application also provides a glucose sensor comprising: the method comprises the following steps: the device comprises a working electrode, a counter electrode, a reference electrode and a contact piece;
the contact piece is composed of an evaporation gold film, wherein the evaporation gold film is provided with a concave-convex structure which is uniformly distributed, and gold nanoparticles which are uniformly distributed on the evaporation gold film.
The application has the advantages over the prior art that:
the application provides a manufacturing method of a glucose sensor, which comprises the following steps: selecting sand paper as a vapor deposition substrate; placing the evaporation substrate in a vacuum environment, and evaporating a gold film on the evaporation substrate through evaporation; placing the evaporation gold film in the chloroauric acid solution, scanning for multiple times by a cyclic voltammetry method, and generating gold nanoparticles on the evaporation gold film; and placing the evaporation gold film in ozone, irradiating the evaporation gold film by ultraviolet rays, cutting the evaporation gold film by a preset size, taking the cut evaporation gold film as a sensor contact piece, and assembling a working electrode, a counter electrode and a reference electrode in a three-electrode sensor mode to form the glucose sensor. This application passes through abrasive paper as the coating by vaporization substrate in the manufacturing process of coating by vaporization gold film, the flow greatly simplifies, and the yield is high, and the working electrode simple structure who forms has reduced the production degree of difficulty, therefore very big reduce cost.
Drawings
FIG. 1 is a flow chart of the fabrication of a glucose sensor according to the present application.
FIG. 2 is a schematic view of the microstructure of the working electrode in the glucose sensor of the present application.
Detailed Description
The following is an example of a specific implementation process provided for explaining the technical solutions to be protected in the present application in detail, but the present application may also be implemented in other ways than those described herein, and a person skilled in the art may implement the present application by using different technical means under the guidance of the idea of the present application, so that the present application is not limited by the following specific embodiments.
The application provides a manufacturing method of a glucose sensor, which comprises the following steps: selecting abrasive paper as an evaporation substrate; placing the evaporation substrate in a vacuum environment, and evaporating a gold film on the evaporation substrate through evaporation; placing the evaporation gold film in the chloroauric acid solution, scanning for multiple times by a cyclic voltammetry method, and generating gold nanoparticles on the evaporation gold film; and placing the evaporation gold film in ozone, irradiating the evaporation gold film by ultraviolet rays, cutting the evaporation gold film by a preset size, taking the cut evaporation gold film as a sensor contact piece, and assembling a working electrode, a counter electrode and a reference electrode in a three-electrode sensor mode to form the glucose sensor. This application passes through abrasive paper as the coating by vaporization substrate in the manufacturing process of coating by vaporization gold film, the flow greatly simplifies, and the yield is high, and the working electrode simple structure who forms has reduced the production degree of difficulty, therefore very big reduce cost.
FIG. 1 is a flow chart of the fabrication of a glucose sensor according to the present application.
Referring to fig. 1, in S101, sand paper is selected as an evaporation substrate.
The coating by vaporization substrate is at the coating by vaporization in-process for the adnexed subbase of coating by vaporization material, and this application adopts abrasive paper as the coating by vaporization substrate, and the material obtains easily, and its unsmooth surface also provides the basis for increasing the surface area of coating by vaporization.
The sand paper is 500-mesh or 800-mesh silicon carbide sand paper, and it can be understood that those skilled in the art can make other selections according to the actual situation, and the sand paper is not limited to 500-mesh or 800-mesh silicon carbide sand paper.
Referring to fig. 1, in step S102, the evaporation substrate is placed in a vacuum environment, and a gold film is evaporated on the evaporation substrate by evaporation.
And cutting the evaporation substrate into the verified size, wherein the cutting size of the evaporation substrate is different according to different specifications of the adopted evaporation machine, and the description is omitted here.
And placing the evaporation substrate in an evaporation machine, vacuumizing the evaporation space, and then carrying out evaporation. The evaporation method is that the material is put in the evaporation base, the material is gasified by heating and condensed on the evaporation substrate, and a uniform evaporation film is obtained.
In the application, the material is metal gold, and the evaporation film is an evaporation gold film.
Referring to fig. 1, in step S103, the evaporated gold film is placed in the chloroauric acid solution, and gold nanoparticles are generated on the evaporated gold film by multiple scans using cyclic voltammetry.
And after the vapor deposition gold film is manufactured, taking down the vapor deposition gold film to form the vapor deposition gold film with the surface having the concave-convex shape, and then placing the vapor deposition gold film in a chloroauric acid solution to attach gold nanoparticles.
The concentration of the chloroauric acid solution adopted in the application is 0.05 mol/L-0.2 mol/L, and preferably, the chloroauric acid solution is 1mol/L and 1.5 mol/L.
Specifically, the attachment of the gold nanoparticles is realized by scanning with cyclic voltammetry, and the specific scanning time is 100s to 500s, preferably 350 s. The scanning speed is 0.05-0.15V/s, and the scanning cycle number is 45-55.
And after gold nanoparticles are separated out by the cyclic voltammetry and attached to the evaporated gold film, finishing the primary production of the evaporated gold film, and then further processing the evaporated gold film to improve the hydrophilicity.
Referring to fig. 1, in step S104, the vapor deposition gold film is placed in ozone, irradiated with ultraviolet light, cut to a predetermined size, and then used as a sensor contact, and a working electrode, a counter electrode, and a reference electrode are assembled in a three-electrode sensor manner, thereby forming a glucose sensor.
The evaporated gold film is subjected to ozone treatment, particularly in an ozone environment, and is subjected to ultraviolet irradiation, so that the hydrophilicity of the evaporated gold film is improved, and the appearance structure of the evaporated gold film is not damaged.
And then cutting the evaporation gold film, installing a preset size and cutting the size into a shape set according to actual needs to form a sensor contact piece.
And finally, assembling the working electrode, the counter electrode and the reference electrode with the vapor deposition gold film and a three-electrode sensor to form the glucose sensor.
Specifically, the glucose sensor is provided with a working electrode and a counter electrode which form a polarization loop, and the reference electrode and the working electrode form a measurement loop.
The present application also provides a glucose sensor comprising: the device comprises a working electrode, a counter electrode, a reference electrode and a contact piece;
the contact piece is composed of an evaporated gold film 101 which is provided with a concave-convex structure uniformly distributed thereon and gold nanoparticles 102 uniformly distributed thereon, as shown in fig. 2.

Claims (10)

1. A method for manufacturing a glucose sensor, comprising
Selecting sand paper as a vapor deposition substrate;
placing the evaporation substrate in a vacuum environment, and evaporating a gold film on the evaporation substrate through evaporation;
placing the evaporation gold film in the chloroauric acid solution, scanning for multiple times by a cyclic voltammetry method, and generating gold nanoparticles on the evaporation gold film;
and placing the evaporation gold film in ozone, irradiating the evaporation gold film by ultraviolet rays, cutting the evaporation gold film by a preset size, taking the cut evaporation gold film as a sensor contact piece, and assembling a working electrode, a counter electrode and a reference electrode in a three-electrode sensor mode to form the glucose sensor.
2. The method of claim 1, wherein the coated abrasive is 500-mesh or 800-mesh silicon carbide coated abrasive.
3. The method for manufacturing a glucose sensor according to claim 1, wherein the concentration of the chloroauric acid solution is 0.05 to 0.2 mol/L.
4. The method for manufacturing the glucose sensor according to claim 1, wherein the cyclic voltammetry is performed for 100s to 500 s.
5. The method of claim 1, wherein the scanning rate is 0.05-0.15V/s.
6. The method of claim 1, wherein the number of scanning cycles is 45 to 55.
7. The method for manufacturing a glucose sensor according to claim 1, wherein the time for irradiating the evaporated gold film with ultraviolet light is not more than 40 min.
8. The method of claim 1, wherein the thickness of the evaporated gold film is 100 nm.
9. The method for manufacturing the glucose sensor according to claim 1 or 4, wherein the executing device of the cyclic voltammetry is an electrochemical workstation.
10. A glucose sensor, comprising: a working electrode, a counter electrode and a reference electrode; the method comprises the following steps: the device comprises a working electrode, a counter electrode, a reference electrode and a contact piece;
the contact piece is composed of an evaporation gold film, wherein the evaporation gold film is provided with a concave-convex structure which is uniformly distributed, and gold nanoparticles which are uniformly distributed on the evaporation gold film.
CN202210567302.1A 2022-05-23 2022-05-23 Manufacturing method of glucose sensor Withdrawn CN115058690A (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0534311A (en) * 1991-07-29 1993-02-09 Anritsu Corp Flavor sensor
CN1339105A (en) * 1999-12-03 2002-03-06 松下电器产业株式会社 Biocapteur
JP2004226358A (en) * 2003-01-27 2004-08-12 Matsushita Electric Ind Co Ltd Biosensor
DE102006020131A1 (en) * 2006-05-02 2007-11-15 Liu, Jinping, Dr.-Ing. Nano- and microstructured biosensor, useful e.g. for detecting biological sample, comprises a substrate with a brush surface, a metal electrode, a permeable membrane and an enzyme membrane
CN103399059A (en) * 2013-07-11 2013-11-20 上海师范大学 Au(111)-like nano-particle non-enzyme glucose sensor electrode, and preparation method and application of same
US20170219511A1 (en) * 2016-01-29 2017-08-03 National Chung Hsing University Enzyme-free glucose detection chip
CN111272849A (en) * 2019-08-20 2020-06-12 深圳硅基传感科技有限公司 Working electrode of glucose sensor and preparation method thereof

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0534311A (en) * 1991-07-29 1993-02-09 Anritsu Corp Flavor sensor
CN1339105A (en) * 1999-12-03 2002-03-06 松下电器产业株式会社 Biocapteur
JP2004226358A (en) * 2003-01-27 2004-08-12 Matsushita Electric Ind Co Ltd Biosensor
DE102006020131A1 (en) * 2006-05-02 2007-11-15 Liu, Jinping, Dr.-Ing. Nano- and microstructured biosensor, useful e.g. for detecting biological sample, comprises a substrate with a brush surface, a metal electrode, a permeable membrane and an enzyme membrane
CN103399059A (en) * 2013-07-11 2013-11-20 上海师范大学 Au(111)-like nano-particle non-enzyme glucose sensor electrode, and preparation method and application of same
US20170219511A1 (en) * 2016-01-29 2017-08-03 National Chung Hsing University Enzyme-free glucose detection chip
CN111272849A (en) * 2019-08-20 2020-06-12 深圳硅基传感科技有限公司 Working electrode of glucose sensor and preparation method thereof

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Application publication date: 20220916