CN116337967A - Preparation method and application of petal-shaped flexible reference electrode - Google Patents
Preparation method and application of petal-shaped flexible reference electrode Download PDFInfo
- Publication number
- CN116337967A CN116337967A CN202211579186.1A CN202211579186A CN116337967A CN 116337967 A CN116337967 A CN 116337967A CN 202211579186 A CN202211579186 A CN 202211579186A CN 116337967 A CN116337967 A CN 116337967A
- Authority
- CN
- China
- Prior art keywords
- electrode
- graphene oxide
- carbon cloth
- reference electrode
- solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/46—Electroplating: Baths therefor from solutions of silver
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
- A61B5/00—Measuring for diagnostic purposes; Identification of persons
- A61B5/24—Detecting, measuring or recording bioelectric or biomagnetic signals of the body or parts thereof
- A61B5/25—Bioelectric electrodes therefor
- A61B5/263—Bioelectric electrodes therefor characterised by the electrode materials
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
- A61B5/00—Measuring for diagnostic purposes; Identification of persons
- A61B5/24—Detecting, measuring or recording bioelectric or biomagnetic signals of the body or parts thereof
- A61B5/25—Bioelectric electrodes therefor
- A61B5/263—Bioelectric electrodes therefor characterised by the electrode materials
- A61B5/265—Bioelectric electrodes therefor characterised by the electrode materials containing silver or silver chloride
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/198—Graphene oxide
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/24—Halogens or compounds thereof
- C25B1/26—Chlorine; Compounds thereof
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/54—Electroplating of non-metallic surfaces
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
- G01N27/301—Reference electrodes
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- General Health & Medical Sciences (AREA)
- Pathology (AREA)
- Molecular Biology (AREA)
- Physics & Mathematics (AREA)
- Veterinary Medicine (AREA)
- Public Health (AREA)
- Inorganic Chemistry (AREA)
- Animal Behavior & Ethology (AREA)
- Surgery (AREA)
- Medical Informatics (AREA)
- Biophysics (AREA)
- Biomedical Technology (AREA)
- Heart & Thoracic Surgery (AREA)
- Nanotechnology (AREA)
- Immunology (AREA)
- General Physics & Mathematics (AREA)
- Biochemistry (AREA)
- Analytical Chemistry (AREA)
- Measurement And Recording Of Electrical Phenomena And Electrical Characteristics Of The Living Body (AREA)
Abstract
A preparation method and application of petal-shaped flexible reference electrode belong to the field of electrochemical preparation of reference electrode. According to the invention, graphene oxide/carbon cloth is taken as a substrate, silver is deposited by an electrochemical method to obtain a graphene oxide/carbon cloth-Ag electrode, then the electrode is chloridized by an electrochemical chloridization method to obtain a petal-shaped graphene oxide/carbon cloth-Ag/AgCl reference electrode, and finally a layer of KCl-PVA-agar conductive hydrogel solution is uniformly coated on the surface of the electrode to obtain the petal-shaped KCl-PVA-agar conductive hydrogel/graphene oxide/carbon cloth-Ag/AgCl reference electrode. According to the invention, graphene oxide/carbon cloth is used as a substrate for the first time, the petal-shaped reference electrode with a nano structure is prepared for the first time, and the surface of the reference electrode is uniformly coated with a layer of hydrogel film.
Description
Technical Field
The invention belongs to the field of electrochemical preparation of reference electrodes, and particularly relates to a preparation method and application of a petal-shaped flexible reference electrode.
Background
In recent years, with the development of flexible wearable sensors, flexible wearable devices with multiple physiological parameters and continuous dynamic measurement capability of motion parameters, soft, light and thin and extensible structures can move along with skin, can realize close contact with the skin in a direct attachment mode, and show excellent repeatability in long-term vital sign monitoring [1] . At present, the flexible sensor can realize measurement of physical quantities such as temperature, heart rate, electrocardio, skin and the like, metabolites, electrolytes, biomolecules and other chemical substances, and can realize percutaneous trans-tissue image signal detection in modes such as ultrasound, X-ray imaging and the like [2] . The reference electrode is used as one of important components of the flexible electronic device, and has the advantages of good tensile strength, light unit weight, good conductivity, high sensitivity, stable chemical performance and the like.
Sheet-like reference which is currently more widely usedThe electrode preparation method is screen printing method [3] Ink jet printing method [4] . However, the reference electrode prepared by the two methods has low stability and short service life, and is not beneficial to application in actual life. In the previous studies of the applicant of the present invention [5] PDMS is used as a flexible substrate, agNWs is used for preparing a reference electrode based on silver nanowires, the reference electrode has excellent performance in the aspects of stability, service life, repeatability, storage period and the like, but later research shows that the stability of the reference electrode is not comparable with that of a commercial glass Ag/AgCl reference electrode. Therefore, the primary problem to be solved in the current sheet-shaped reference electrode research field is how to improve the stability of the electrode, so that the electrode reaches the level of the commercial glass Ag/AgCl reference electrode, and the service life and the long-term stability of the electrode are improved.
Disclosure of Invention
Aiming at the defect of the reference electrode prepared by the prior art in performance, the invention aims to disclose a preparation method and application of a petal-shaped flexible reference electrode, namely KCl-PVA-agar conductive hydrogel/graphene oxide/carbon cloth-Ag/AgCl reference electrode, and polyvinyl alcohol (PVA). According to the invention, graphene oxide/carbon cloth is used as a substrate of a reference electrode, silver is deposited by an electrochemical method to obtain a graphene oxide/carbon cloth-Ag electrode, the graphene oxide/carbon cloth-Ag electrode is chloridized by an electrochemical chloridization method to obtain a petal-shaped graphene oxide/carbon cloth-Ag/AgCl reference electrode, and finally a layer of KCl-PVA-agar conductive hydrogel solution is uniformly coated on the surface of the petal-shaped graphene oxide/carbon cloth-Ag/AgCl reference electrode to obtain the petal-shaped KCl-PVA-agar conductive hydrogel/graphene oxide/carbon cloth-Ag/AgCl reference electrode. The electrode prepared by the invention has the advantages of low preparation cost, high tensile strength, light unit weight, good conductivity, stable chemical property, long service life and the like, and can be applied to wearable equipment for monitoring myoelectricity, electrocardio and electroencephalogram.
In order to achieve the above purpose, the invention adopts the following technical scheme:
step 1: and uniformly coating a graphene oxide solution on the carbon cloth substrate to prepare the graphene oxide/carbon cloth flexible substrate.
Step 2: preparation of graphene oxide/carbon cloth-Ag/AgCl reference electrode.
Step 2.1: adopting a three-electrode system, taking a graphene oxide/carbon cloth flexible substrate as a working electrode, taking a saturated calomel electrode as a reference electrode, taking a platinum wire as a counter electrode, and placing the electrodes in AgNO 3 And KNO 3 And (3) in the mixed solution, performing electrochemical deposition by adopting a chronopotentiometric method, and obtaining the graphene oxide/carbon cloth-Ag electrode after deposition.
Step 2.2: the three-electrode system is adopted, the graphene oxide/carbon cloth-Ag electrode is used as a working electrode, the saturated calomel electrode is used as a reference electrode, the platinum wire is used as a counter electrode, the three-electrode system is put into hydrochloric acid solution, and electrochemical chlorination is carried out by adopting a chronopotentiometric method, so that the petal-shaped graphene oxide/carbon cloth-Ag/AgCl reference electrode is prepared.
Step 3: preparation of KCl-PVA-agar conductive hydrogel/graphene oxide/carbon cloth-Ag/AgCl reference electrode.
Dissolving 0.5000g of PVA in 20mL of 80 ℃ ultrapure water, adding 0.3g of agar powder into 20mL of saturated KCl solution, heating to completely dissolve, mixing the PVA solution and the saturated KCl-agar solution to obtain KCl-PVA-agar conductive hydrogel solution, cooling and standing for 6h, immersing a petal-shaped graphene oxide/carbon cloth-Ag/AgCl reference electrode into the conductive hydrogel solution, uniformly coating a layer of hydrogel film on the surface of the conductive hydrogel solution, drying and standing to obtain the petal-shaped KCl-PVA-agar conductive hydrogel/graphene oxide/carbon cloth flexible-Ag/AgCl reference electrode.
More specifically, the preparation method of the substrate in step 1 comprises the following steps: and cutting a piece of carbon cloth into a plurality of specifications of 2cm multiplied by 4cm, and uniformly coating graphene oxide solution on the carbon cloth substrate to prepare the graphene oxide/carbon cloth substrate.
In the method, in the step 1, the concentration of the graphene oxide solution is 2-8mg/mL, and preferably, the concentration of the graphene oxide solution is 6mg/mL.
In the above method, in step 2.1, agNO 3 The concentration of the solution is 0.01-0.1M, KNO 3 The concentration of the solution is 0.1-1.0M, preferably AgNO 3 The concentration of the solution was 0.05M, KNO 3 The concentration of the solution was 0.5M.
In the above method, in step 2.1, silver is deposited by a chronopotentiometric method, the deposition potential is-0.6V, the deposition time is 1800s-3600s, preferably, the deposition potential is-0.6V, and the deposition time is 2400s.
In the above method, in step 2.2, the concentration of the hydrochloric acid solution is 0.05 to 0.15M, preferably, the concentration of the hydrochloric acid solution is 0.1M.
In the above method, in step 2.2, electrochemical chlorination is performed by using a chronopotentiometric method, wherein the chlorination potential is ocp+100mV, ocp+150mV, ocp+200mV, ocp+250mV, ocp+300mV, and most preferably ocp+250mV, and the chlorination time is 2400s-3600s, preferably, the chlorination potential is ocp+250mV, and the chlorination time is 3000s.
The invention simultaneously protects application of the KCl-PVA-agar conductive hydrogel/graphene oxide/carbon cloth-Ag/AgCl reference electrode in the wearable industry, in particular to application in myoelectric monitoring, electrocardiographic monitoring and electroencephalogram monitoring.
The carbon cloth is also called carbon fiber cloth and is formed by carbonizing oxidized polyacrylonitrile fiber fabric or weaving carbon fiber. The carbon cloth has the characteristics of high strength, strong durability, small density, good conductivity, good softness and the like, so the carbon cloth has a very wide application range, for example: for the study of batteries, electron accepting and transferring as a negative electrode; the structure is used for researching super capacitors, and is used as a current collector, an electron transmission structure or a part for collecting current; the method is used for electrochemical substrate materials, metal oxides are deposited on carbon cloth, and the performance of the metal oxides is tested.
Graphene oxide is a non-traditional soft material, and has good hydrophilicity, higher specific surface energy and excellent mechanical properties. Since the basal plane and the edge of the graphene oxide lamellar skeleton have a structure in which a plurality of oxygen-containing functional groups coexist, the conductivity and the band gap of the graphene oxide can be modulated by regulating the types and the numbers of the oxygen-containing functional groups, so that the graphene oxide is widely applied to conductive materials.
The KCl-PVA-agar conductive hydrogel has good conductivity, adhesiveness, softness and ion permeability, and the KCl-PVA-agar conductive hydrogel is used as an encapsulation film to protect the electrode from being damaged, reduce the pollution of the reference electrode, increase the stability of the reference electrode and prolong the service life of the reference electrode.
Compared with the prior art, the invention has the beneficial effects that: the invention takes graphene oxide/carbon cloth as a substrate for the first time, and has the advantages of excellent conductivity, light unit weight, low preparation cost and the like. The KCl-PVA-agar conductive hydrogel with high softness and excellent ion permeability is used as the surface film, so that the pollution of the reference electrode can be reduced, the stability of the reference electrode can be improved, and the service life of the reference electrode can be prolonged. The reference electrode with petal-shaped nano structure is prepared for the first time, and the stability of the reference electrode can be compared with that of a commercial reference electrode. The reference electrode prepared by the invention can be applied to wearable equipment and is used for monitoring myoelectricity, electrocardio and electroencephalogram.
Drawings
FIG. 1 is a scanning electron microscope image of a KCl-PVA-agar conductive hydrogel/graphene oxide/carbon cloth flexible-Ag/AgCl reference electrode;
FIG. 2 is a graph comparing the stability of a KCl-PVA-agar conductive hydrogel/graphene oxide/carbon cloth flexible-Ag/AgCl reference electrode with a commercial hard glass Ag/AgCl reference electrode;
FIG. 3 is a graph of myoelectric monitoring of a person with a KCl-PVA-agar conductive hydrogel/graphene oxide/carbon cloth flexible-Ag/AgCl electrode;
FIG. 4 is a graph of the electrocardiographic monitoring of a person with a KCl-PVA-agar conductive hydrogel/graphene oxide/carbon cloth flexible-Ag/AgCl electrode;
fig. 5 is an electroencephalogram monitoring graph of a human being with a KCl-PVA-agar conductive hydrogel/graphene oxide/carbon cloth flexible-Ag/AgCl electrode.
Detailed Description
The invention is further illustrated below with reference to examples. The experimental methods described in the examples are all conventional methods unless otherwise specified; the experimental reagents and materials are commercially available unless otherwise specified.
Example 1
The preparation method of the KCl-PVA-agar conductive hydrogel/graphene oxide/carbon cloth-Ag/AgCl reference electrode comprises the following specific steps:
step 1: and manufacturing the graphene oxide/carbon cloth flexible substrate.
And cutting a piece of carbon cloth into a plurality of specifications of 2cm multiplied by 4cm, and uniformly coating graphene oxide solution with the concentration of 6mg/mL on the carbon cloth substrate to prepare the graphene oxide/carbon cloth substrate.
Step 2: preparation of graphene oxide/carbon cloth-Ag/AgCl reference electrode.
Step 2.1: and (3) preparing the graphene oxide/carbon cloth-Ag electrode.
Adopting a three-electrode system, taking the graphene oxide/carbon cloth flexible substrate prepared in the step 1 as a working electrode, a saturated calomel electrode as a reference electrode, a platinum wire as a counter electrode, and placing the counter electrode in AgNO of 0.05M 3 And KNO of 0.5M 3 And (3) in the mixed solution, performing electrochemical deposition by adopting a chronopotentiometry, wherein the deposition potential is-0.6V, the deposition time is 2400s, and the graphene oxide/carbon cloth-Ag electrode is obtained after deposition.
Step 2.2: chlorinated graphene oxide/carbon cloth-Ag electrode.
The graphene oxide/carbon cloth-Ag electrode prepared in the step 2.1 is used as a working electrode, a saturated calomel electrode is used as a reference electrode, a platinum wire is used as a counter electrode, the three-electrode system is put into a 0.1M hydrochloric acid solution, and chlorination is carried out by adopting a chronopotentiometric method, wherein the chlorination potential is OCP+250mV, and the chlorination time is 3000s. And (3) preserving the chloridized electrode for one day at room temperature under the dark drying condition, thus obtaining the petal-shaped graphene oxide/carbon cloth-Ag/AgCl reference electrode.
Step 3: preparation of KCl-PVA-agar conductive hydrogel/graphene oxide/carbon cloth-Ag/AgCl reference electrode.
Dissolving 0.5000g of PVA in 20mL of 80 ℃ ultrapure water, adding 0.3g of agar powder into 20mL of saturated KCl solution, heating to completely dissolve, mixing the PVA solution and the saturated KCl-agar solution to obtain KCl-PVA-agar conductive hydrogel solution, cooling and standing for 6h, immersing petal-shaped graphene oxide/carbon cloth-Ag/AgCl reference electrode into the conductive hydrogel solution, uniformly coating a layer of hydrogel film on the surface of the conductive hydrogel solution, drying and standing to obtain petal-shaped KCl-PVA-agar conductive hydrogel/graphene oxide/carbon cloth flexible-Ag/AgCl reference electrode, and scanning electron microscope graph is shown in figure 1.
Example 2
Stability comparison of KCl-PVA-agar conductive hydrogel/graphene oxide/carbon cloth-Ag/AgCl reference electrode with commercial hard glass Ag/AgCl reference electrode
The two reference electrodes are subjected to Open Circuit Potential (OCP) test, and the test results are shown in figure 2, and the results show that the test curves of the KCl-PVA-agar conductive hydrogel/graphene oxide/carbon cloth-Ag/AgCl reference electrode and the commercial hard glass Ag/AgCl reference electrode prepared by the invention are very stable and have little difference. From this, the stability of the reference electrode prepared according to the present invention is comparable to that of a commercial hard glass Ag/AgCl reference electrode, which is a level not reached by the reference electrode of the prior art.
Example 3
Application of KCl-PVA-agar conductive hydrogel/graphene oxide/carbon cloth-Ag/AgCl flexible reference electrode in electromyography monitoring, electrocardiograph detection and electroencephalogram monitoring.
Like nerve cells, muscle fibers (cells) also belong to excitable cells. They, when excited, produce action potentials, i.e., conductive potentials that appear across the cell membrane where they are excited. Surface electromyography is a measurement method of bioelectric signals when adjacent myofibers (cells) are activated by placing electrodes on the surface of the skin. At present, most of the surface electromyography monitoring adopts a nano silver/silver chloride electrode, and the electrode has the defects of high manufacturing cost, poor stability and the like. The KCl-PVA-agar conductive hydrogel/graphene oxide/carbon cloth-Ag/AgCl flexible reference electrode has the advantages of low manufacturing cost, high stability, strong signal transmission capability and the like, and is applied to electromyography morphology of the total fibular nerve, the tibial nerve and the superficial fibular nerve measured in surface electromyography monitoring, as shown in figure 3.
Electrocardiograph is a technique for recording the pattern of electrical activity change generated by each cardiac cycle of the heart from the body surface by using electrocardiograph, and is of great importance to the diagnostic analysis of various arrhythmias and conduction blocks by recording the pattern of electrical activity change of the heart by placing measuring electrodes on the surface of the human body. Currently, common electrodes used for biological signal transduction in the electrocardiograph monitoring process are copper alloy silver-plated electrodes, nickel-silver alloy electrodes, zinc-silver-copper alloy electrodes, stainless steel electrodes and the like. The electrode can realize high-performance detection and is widely applied to the existing medical detection, but the manufacturing cost is high. The KCl-PVA-agar conductive hydrogel/graphene oxide/carbon cloth-Ag/AgCl flexible reference electrode has the advantages of low manufacturing cost, stable performance, high safety and strong signal transmission capability, and is more suitable for being applied to a wearable health monitoring system compared with the reference electrode in the prior art. The reference electrode of the present invention was applied to electrocardiographic monitoring, and the results are shown in fig. 4.
Scalp electroencephalogram is a pattern obtained by amplifying and recording spontaneous electrical activity of the brain from the scalp using electrodes. The electroencephalogram does not reflect the electric activity of a certain nerve cell only, but records the total electric activity of a plurality of nerve cell groups in a certain area of the brain represented by the electrode, captures and records some spontaneous rhythmic activities of the brain, and is helpful for the accurate analysis of clinicians. At present, electrodes commonly used in electroencephalogram monitoring are made of stainless steel, gold, platinum or other materials, but long-term direct contact with the gold, platinum or other electrodes can cause skin irritation and discomfort to patients. The reference electrode is more suitable for wearing, and has high safety and stronger signal transmission capability. The reference electrode of the present invention was attached to the scalp of a patient for electroencephalogram monitoring according to the international 10-20 system electrode placement method, and the result is shown in fig. 5.
The above-described embodiments are provided for illustration and description of the present invention only and are not intended to limit the invention to the embodiments described. In addition, those skilled in the art will appreciate that the present invention is not limited to the embodiments described above, and that many variations and modifications are possible in light of the teachings of the invention, which variations and modifications are within the scope of the invention as claimed.
Reference to the literature
[1] Late spring snow, wu Ziyue, huang Xian Flexible wearable sensing and Intelligent identification technology research progress [ J ]. Chinese science chemical 2022,52 (11): 1913-1924.
[2]KimDH,LuN,MaR,KimYS,KimRH,WangS,WuJ,WonSM,TaoH,IslamA,YuKJ,KimT,Chowdhury R,YingM,XuL,LiM,ChungHJ,KeumH,McCormickM,LiuP,ZhangYW,OmenettoFG,HuangY,Coleman T,RogersJA.Science,2011,333:838–843
[3]LindnerE,GuzinskiM,KhanTA,etal.Referenceelectrodeswithionicliquidsaltbridge:whenwillthese innovativenovelreferenceelectrodesgainbroadacceptance[J].AcsSensors,2019,4(3):549-561.
[4]CardosoRM,KalinkeC,RochaRG,etal.Additive-manufactured(3D-printed)electrochemicalsensors:Acriticalreview[J].Analyticachimicaacta,2020,1118:73-91.
[5] Sun Jing, wang Qingxiang, shen Guijuan, lang Ming. A method for the preparation and application of a PDMS-based Ag/AgCl microelectrode is described in [ P ]. Liaoning, inc.: CN108195911B,2020-05-19.
Claims (8)
1. The preparation method of the petal-shaped flexible reference electrode is characterized by comprising the following steps of:
step 1: uniformly coating a graphene oxide solution on a carbon cloth substrate to prepare a graphene oxide/carbon cloth flexible substrate;
step 2: preparing a graphene oxide/carbon cloth-Ag/AgCl reference electrode;
step 2.1: adopting a three-electrode system, taking a graphene oxide/carbon cloth flexible substrate as a working electrode, taking a saturated calomel electrode as a reference electrode, taking a platinum wire as a counter electrode, and placing the electrode in AgNO 3 And KNO 3 In the mixed solution, performing electrochemical deposition by adopting a chronopotentiometric method, and obtaining a graphene oxide/carbon cloth-Ag electrode after deposition;
step 2.2: a three-electrode system is adopted, a graphene oxide/carbon cloth-Ag electrode is used as a working electrode, a saturated calomel electrode is used as a reference electrode, a platinum wire is used as a counter electrode, the three-electrode system is put into hydrochloric acid solution, electrochemical chlorination is carried out by adopting a chronopotentiometric method, and a petal-shaped graphene oxide/carbon cloth-Ag/AgCl reference electrode is prepared;
step 3: preparing a KCl-PVA-agar conductive hydrogel/graphene oxide/carbon cloth-Ag/AgCl reference electrode;
dissolving 0.5000g of PVA in 20mL of 80 ℃ ultrapure water, adding 0.3g of agar powder into 20mL of saturated KCl solution, heating to completely dissolve, mixing the PVA solution and the saturated KCl-agar solution to obtain KCl-PVA-agar conductive hydrogel solution, cooling and standing for 6h, immersing a petal-shaped graphene oxide/carbon cloth-Ag/AgCl reference electrode into the conductive hydrogel solution, uniformly coating a layer of hydrogel film on the surface of the conductive hydrogel solution, drying and standing to obtain the petal-shaped KCl-PVA-agar conductive hydrogel/graphene oxide/carbon cloth flexible-Ag/AgCl reference electrode.
2. The method according to claim 1, wherein in step 1, the concentration of the graphene oxide solution is 2 to 8mg/mL.
3. The method according to claim 1, wherein in step 2.1, agNO 3 The concentration of the solution is 0.01-0.1M, KNO 3 The concentration of the solution is 0.1-1.0M, silver is deposited by adopting a chronopotentiometric method, the deposition potential is-0.6V, and the deposition time is 1800-3600 s.
4. The method according to claim 1, wherein in step 2.1, agNO 3 The concentration of the solution was 0.05M, KNO 3 The concentration of the solution is 0.5M, silver is deposited by adopting a chronopotentiometric method, the deposition potential is-0.6V, and the deposition time is 2400s.
5. The method according to claim 1, wherein in step 2.2, electrochemical chlorination is performed by using a chronopotentiometric method, the concentration of the hydrochloric acid solution is 0.05-0.15M, the chlorination potential is ocp+100mV, ocp+150mV, ocp+200mV, ocp+250mV, ocp+300mV, and the chlorination time is 2400s-3600 s.
6. The method according to claim 1, wherein in step 2.2, electrochemical chlorination is performed by chronopotentiometry, the concentration of the hydrochloric acid solution is 0.1M, the chlorination potential is 250mV higher than the open circuit potential, and the chlorination time is 3000s.
7. Use of an electrode prepared by the method of claim 1 in a wearable device.
8. The use of the electrode prepared by the method of claim 1 in electromyographic monitoring, electrocardiographic monitoring and electroencephalographic monitoring.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211579186.1A CN116337967A (en) | 2022-12-07 | 2022-12-07 | Preparation method and application of petal-shaped flexible reference electrode |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211579186.1A CN116337967A (en) | 2022-12-07 | 2022-12-07 | Preparation method and application of petal-shaped flexible reference electrode |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116337967A true CN116337967A (en) | 2023-06-27 |
Family
ID=86888211
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211579186.1A Pending CN116337967A (en) | 2022-12-07 | 2022-12-07 | Preparation method and application of petal-shaped flexible reference electrode |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116337967A (en) |
-
2022
- 2022-12-07 CN CN202211579186.1A patent/CN116337967A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Neuman | Biopotential electrodes | |
| Niu et al. | Surface bioelectric dry Electrodes: A review | |
| Zahed et al. | Flexible and robust dry electrodes based on electroconductive polymer spray-coated 3D porous graphene for long-term electrocardiogram signal monitoring system | |
| CN115337011B (en) | Metal-coated hydrogel electrode and preparation method thereof | |
| CN112450938B (en) | Hydrogel electrode for long-term electroencephalogram acquisition and preparation method thereof | |
| CN108309291B (en) | Flexible contact brain electrode and preparation method thereof | |
| Faham et al. | Electrochemical-based remote biomarker monitoring: Toward Internet of Wearable Things in telemedicine | |
| Varadan et al. | Wireless point-of-care diagnosis for sleep disorder with dry nanowire electrodes | |
| CN109559851A (en) | A kind of graphene electrocardioelectrode and preparation method thereof | |
| WO2020056925A1 (en) | Skin dry electrode | |
| CN110261454A (en) | A kind of nano-porous gold of urine detection dopamine is without enzyme sensing electrode and the preparation method and application thereof | |
| CN116337967A (en) | Preparation method and application of petal-shaped flexible reference electrode | |
| CN116327204A (en) | Preparation method of flexible fishbone-shaped Ag/AgCl reference electrode and application of flexible fishbone-shaped Ag/AgCl reference electrode in wearable industry | |
| Ku et al. | Electro-deposited nanoporous platinum electrode for EEG monitoring | |
| Momota et al. | Fabrication and characterization of inkjet printed flexible dry ECG electrodes | |
| Shen et al. | A gelatin-based hydrogel electrode with high moisturizing ability for wearable EEG recording | |
| Ali et al. | Wearable graphene-based fabric electrodes for enhanced and long-term biosignal detection | |
| KR102173746B1 (en) | Sensor for sensing vital signs | |
| Yoon et al. | A Flexible Electrochemical-Physiological Epidermal Hybrid Patch for Chronic Disease Management | |
| CN114190947A (en) | Non-invasive electroencephalogram sensor based on flexible substrate and preparation method thereof | |
| CN113397551A (en) | Flexible leather electrode material based on liquid metal and preparation method thereof | |
| CN114748064A (en) | Hollow microneedle vertical graphene sensor and preparation method thereof | |
| Song et al. | Performance of a flexible electrode based on natural leather | |
| CN116327202A (en) | Application of flexible electrode in wearable equipment | |
| Zahed et al. | Nanoporous Carbon-Based Wearable Hybrid Biosensing Patch for Real-Time and in Vitro Healthcare Monitoring |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |