WO2023045107A1 - 一种柔性干电极及其制备方法 - Google Patents
一种柔性干电极及其制备方法 Download PDFInfo
- Publication number
- WO2023045107A1 WO2023045107A1 PCT/CN2021/137314 CN2021137314W WO2023045107A1 WO 2023045107 A1 WO2023045107 A1 WO 2023045107A1 CN 2021137314 W CN2021137314 W CN 2021137314W WO 2023045107 A1 WO2023045107 A1 WO 2023045107A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- polymer film
- flexible
- solution
- metal nanowire
- dry electrode
- 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.)
- Ceased
Links
Images
Classifications
-
- 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
- G01N27/327—Biochemical electrodes, e.g. electrical or mechanical details for in vitro measurements
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
Definitions
- the invention relates to the technical field of electrode preparation, in particular to a method for preparing a flexible dry electrode.
- Ag/AgCl wet electrodes are widely used to collect bioelectrical signals due to their excellent electrical properties, however, certain disadvantages greatly limit the use of these electrodes, especially in long-term monitoring.
- the first is that Ag/AgCl electrodes require skin preparation, such as hair cutting, decontamination, and electrolytic gel coating, which is time-consuming.
- conductive gels may dehydrate and coagulate after prolonged use, which may increase detection noise and degrade signal quality. Additionally, the gel has been observed to potentially cause allergic reactions or skin irritation in patients. Due to the hard texture of the overall material of the electrode system, the biocompatibility is poor. The adhesion to the scalp is poor, and micro-movement between the electrode cap and the scalp is easy to occur during use, which directly leads to the loss of signal acquisition and motion artifacts.
- the present invention proposes a method for preparing a flexible dry electrode, which solves or at least partially solves the technical defects existing in the prior art.
- the present invention adopts the following technical solutions:
- a method for preparing a flexible dry electrode comprising the following steps:
- the metal nanowire-polymer film is reacted in a noble metal salt solution to obtain a flexible dry electrode.
- the preparation method of the flexible dry electrode, the preparation method of the flexible pre-PDMS mixture is specifically: mixing the PDMS prepolymer, curing agent and additives and then stirring to obtain the flexible PDMS mixture;
- the preparation method of the metal nanowire solution is as follows: adding the metal nanowire into the alcohol solution to obtain the metal nanowire solution;
- the noble metal in the noble metal salt solution includes one of palladium, platinum and gold.
- the dispersant includes Triton X100, and the mass ratio of the PDMS prepolymer, curing agent and additive is 10:1:(0.03-0.05).
- the metal nanowires include silver nanowires or copper nanowires, and the concentration of the metal nanowire solution is 5 mg/ml.
- the flexible PDMS mixture is coated on the substrate, and the polymer film is formed after curing. on the substrate for 40-120 seconds, and cured at 25-40° C. for 15-24 hours to obtain a polymer film.
- the preparation method of the flexible dry electrode after placing the metal nanowire-polymer film in the noble metal salt solution for reaction, it also includes placing the reacted metal nanowire-polymer film in an ammonia solution in React at 70-80°C for 3-10 minutes to obtain a flexible dry electrode.
- the preparation method of the flexible dry electrode further includes: heating the metal nanowire-polymer film to remove the alcohol solution before placing the metal nanowire-polymer film in the noble metal salt solution for reaction, the Alcoholic solutions include ethanol or isopropanol.
- the metal nanowire-polymer film is reacted in a noble metal salt solution, wherein the reaction temperature is 60-120° C., and the reaction time is 45-120 min.
- the present invention also provides a flexible dry electrode prepared by the preparation method.
- a method for preparing a flexible dry electrode of the present invention has the following beneficial effects:
- the preparation method of the flexible dry electrode of the present invention by coating the flexible PDMS mixture on the substrate, forming a polymer film after curing, then immersing the polymer film in the dopamine hydrochloride solution, and then adding the metal nanowire solution Coated on a polymer film to obtain a metal nanowire-polymer film; then place the metal nanowire-polymer film in a noble metal salt solution, and use the displacement reaction between the noble metal salt solution and the metal nanowire to generate noble metal nanotubes ; Since the present invention uses a flexible PDMS mixture, the resulting polymer film is a flexible film, which has good biocompatibility, good adhesion to the scalp, and reduces the influence of motion artifacts during use.
- the prepared flexible dry electrode has good fit and wearing comfort;
- the preparation method of the flexible dry electrode of the present invention adopts PDMS prepolymers to generate PDMS polymer films.
- PDMS not only has the characteristics of flexibility, but also has excellent biocompatibility.
- Silver nanotubes, platinum nanotubes (Pt NTs) has excellent conductivity, and the prepared flexible dry electrode does not require skin preparation or the use of conductive gel, which saves time and avoids the risk of allergy and skin irritation;
- Fig. 1 is the schematic flow chart of the preparation method of flexible dry electrode of the present invention
- Fig. 2 is a schematic diagram of the preparation method of the flexible dry electrode in Example 1 of the present invention.
- the embodiment of the present application provides a method for preparing a flexible dry electrode, as shown in Figure 1, including the following steps:
- the flexible PDMS mixture is coated on the substrate, and the polymer film is formed after curing, and then the polymer film is peeled off from the substrate.
- the polymer film is peeled from the substrate.
- the pDA layer is polydopamine, its function is to make the hydrophobic polymer film (PDMS film) hydrophilic and increase the adhesion between PDMS and metal nanowires;
- the substrate can be a glass slide, a glass substrate, or the like.
- step S3 before coating the flexible PDMS mixture on the substrate in step S3, it also includes: placing the substrate in acetone, ethanol and deionized solution for ultrasonic cleaning, each cleaning process is ultrasonic for 10 minutes, and then ultrasonically cleaning base to dry.
- the preparation method of the flexible PDMS mixture in step S1 is specifically: mixing the PDMS prepolymer, curing agent and additives and then stirring to obtain the flexible PDMS mixture.
- the PDMS prepolymer and curing agent here are prepolymers and curing agents commonly used in the market, and this application does not improve its specific components.
- the preparation method of the metal nanowire solution is as follows: adding the metal nanowire into the alcohol solution to obtain the metal nanowire solution.
- the noble metal in the noble metal salt solution includes one of palladium, platinum, and gold.
- the noble metal salt can use ethylenediamine platinum chloride, sodium chloroplatinate, ethylenediamine complexes of gold, etc. , correspondingly, palladium nanotubes, platinum nanotubes (Pt NTs) and gold nanotubes were grown on polymer films.
- the additive includes Triton X100, and the mass ratio of PDMS prepolymer, curing agent and added powder is 10:1:(0.03-0.05).
- the flexible polymer can also use PI (polyimide), polyurethane, and the like.
- Additives such as Triton X100 can be used.
- PDMS prepolymers are used to generate PDMS polymer films.
- PDMS not only has the characteristics of flexibility, but also has excellent biocompatibility.
- Platinum nanotubes (Pt NTs) have excellent electrical conductivity.
- the flexible dry electrode requires no skin preparation and no conductive gel, which saves time and avoids the risk of allergies and skin irritation.
- the metal nanowires include silver nanowires or copper nanowires, and the concentration of the metal nanowire solution is 5 mg/ml.
- the silver nanowires (Ag NWs) have a diameter of 45-120nm and a length of 20-50um.
- the metal nanowire-polymer film is placed in the noble metal salt solution to undergo the following reaction:
- platinum nanotubes Pt NTs
- the flexible PDMS mixture is coated on the substrate, and the polymer film is formed after curing.
- the flexible PDMS mixture is coated on the substrate at a speed of 400-800rpm for 40-120s, and the polymer film is formed at 25 Curing at ⁇ 40°C for 15-24 hours to obtain a polymer film.
- the metal nanowire-polymer film after reacting the metal nanowire-polymer film in a noble metal salt solution, it also includes placing the reacted metal nanowire-polymer film in an ammonia solution at 70-80°C for 3- After 10 minutes, the flexible dry electrode was obtained.
- the concentration of the ammonia solution is 0.1M
- the reacted metal nanowire-polymer film reacts with ammonia water to remove the silver precipitate generated in the replacement reaction, such as AgCl
- the specific reaction formula is as follows:
- the metal nanowire-polymer film in the noble metal salt solution before reacting the metal nanowire-polymer film in the noble metal salt solution, it further includes: heating the metal nanowire-polymer film to remove the alcohol solution, and the alcohol solution includes ethanol or isopropanol.
- the metal nanowire-polymer film is reacted in a noble metal salt solution, wherein the reaction temperature is 60-120° C., and the reaction time is 45-120 min.
- the present application also provides a flexible dry electrode prepared by the above preparation method.
- a method for preparing a flexible dry electrode comprising the following steps:
- Fig. 2 has shown the schematic flow chart of preparing flexible dry electrode in embodiment 1, wherein, pDA/PDMS among Fig. 2 represents that in step S3, dopamine self-polymerizes in buffer solution and generates thin polymer (pDA) layer deposition PDMS polymer film surface .
- pDA/PDMS among Fig. 2 represents that in step S3, dopamine self-polymerizes in buffer solution and generates thin polymer (pDA) layer deposition PDMS polymer film surface .
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Molecular Biology (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
Description
Claims (9)
- 一种柔性干电极的制备方法,其特征在于,包括以下步骤:配制柔性PDMS混合物;提供基底;将柔性PDMS混合物涂覆在所述基底上,固化后形成聚合物膜,将聚合物膜剥离后置于多巴胺盐酸盐溶液中浸泡;配制金属纳米线溶液;将金属纳米线溶液涂覆于聚合物膜上,得到金属纳米线-聚合物膜;将金属纳米线-聚合物膜置于贵金属盐溶液中反应后即得柔性干电极。
- 如权利要求1所述的柔性干电极的制备方法,其特征在于,所述柔性预PDMS混合物的配制方法具体为:将PDMS预聚物、固化剂和添加剂混合后搅拌即得柔性PDMS混合物;和/或,所述金属纳米线溶液的配制方法具体为:将金属纳米线加入至醇溶液中即得金属纳米线溶液;和/或,所述贵金属盐溶液中贵金属包括钯、铂、金中的一种。
- 如权利要求2所述的柔性干电极的制备方法,其特征在于,所述添加剂包括Triton X100,所述PDMS预聚物、固化剂和添加剂的质量比为10:1:(0.03~0.05)。
- 如权利要求2所述的柔性干电极的制备方法,其特征在于,所述金属纳米线包括银纳米线或铜纳米线,所述金属纳米线溶液的浓度为5mg/ml。
- 如权利要求1所述的柔性干电极的制备方法,其特征在于,将柔性PDMS混合物涂覆在所述基底上,固化后形成聚合物膜具体为:将柔性PDMS混合物以400~800rpm的速度旋转涂覆在所述基底上40~120s,并于25-40℃下固化15-24h即得聚合物膜。
- 如权利要求4所述的柔性干电极的制备方法,其特征在于,将金属纳米线-聚合物膜置于贵金属盐溶液中反应后,还包括将反应后的金属纳米线-聚合 物膜置于氨水溶液中于70~80℃下反应3~10min,即得柔性干电极。
- 如权利要求2所述的柔性干电极的制备方法,其特征在于,将金属纳米线-聚合物膜置于贵金属盐溶液中反应之前还包括:对金属纳米线-聚合物膜进行加热以除去醇溶液,所述醇溶液包括乙醇或异丙醇。
- 如权利要求1所述的柔性干电极的制备方法,其特征在于,将金属纳米线-聚合物膜置于贵金属盐溶液中反应,其中反应温度为60~120℃,反应时间为45~120min。
- 一种柔性干电极,其特征在于,采用如权利要求1~8任一所述的制备方法制备得到。
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111111268.9A CN115862952A (zh) | 2021-09-23 | 2021-09-23 | 一种柔性干电极及其制备方法 |
| CN202111111268.9 | 2021-09-23 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| WO2023045107A1 true WO2023045107A1 (zh) | 2023-03-30 |
Family
ID=85652845
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| PCT/CN2021/137314 Ceased WO2023045107A1 (zh) | 2021-09-23 | 2021-12-12 | 一种柔性干电极及其制备方法 |
Country Status (2)
| Country | Link |
|---|---|
| CN (1) | CN115862952A (zh) |
| WO (1) | WO2023045107A1 (zh) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116410517A (zh) * | 2023-05-31 | 2023-07-11 | 河南工业大学 | 一种用于摩擦纳米发电机的介电材料的制备方法 |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105758909A (zh) * | 2016-02-26 | 2016-07-13 | 武汉大学 | 一种基于金纳米管的柔性可拉伸电极及其制备方法与应用 |
| CN106693077A (zh) * | 2017-01-22 | 2017-05-24 | 包磊 | 电子皮肤基底及其制备方法和电子皮肤 |
| CN109821134A (zh) * | 2019-01-18 | 2019-05-31 | 武汉大学 | 一种用于活体的三维网络生物探针及其制备方法与应用 |
| US20200289017A1 (en) * | 2017-06-29 | 2020-09-17 | Knu-Industry Cooperation Foundation | Bio-Electrode For Measuring Bio-Signal And Producing Electrical Activity Based On Nano-Porous Permeable Membrane Having High Specific Surface Area And Method Of Manufacturing The Same |
| WO2021114287A1 (zh) * | 2019-12-13 | 2021-06-17 | 深圳先进技术研究院 | 一种柔性电极及其制备方法 |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106755420B (zh) * | 2015-12-31 | 2020-11-13 | 中国科学院上海微系统与信息技术研究所 | 基于表面活性剂改性pdms的数字pcr芯片和方法 |
-
2021
- 2021-09-23 CN CN202111111268.9A patent/CN115862952A/zh active Pending
- 2021-12-12 WO PCT/CN2021/137314 patent/WO2023045107A1/zh not_active Ceased
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105758909A (zh) * | 2016-02-26 | 2016-07-13 | 武汉大学 | 一种基于金纳米管的柔性可拉伸电极及其制备方法与应用 |
| CN106693077A (zh) * | 2017-01-22 | 2017-05-24 | 包磊 | 电子皮肤基底及其制备方法和电子皮肤 |
| US20200289017A1 (en) * | 2017-06-29 | 2020-09-17 | Knu-Industry Cooperation Foundation | Bio-Electrode For Measuring Bio-Signal And Producing Electrical Activity Based On Nano-Porous Permeable Membrane Having High Specific Surface Area And Method Of Manufacturing The Same |
| CN109821134A (zh) * | 2019-01-18 | 2019-05-31 | 武汉大学 | 一种用于活体的三维网络生物探针及其制备方法与应用 |
| WO2021114287A1 (zh) * | 2019-12-13 | 2021-06-17 | 深圳先进技术研究院 | 一种柔性电极及其制备方法 |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116410517A (zh) * | 2023-05-31 | 2023-07-11 | 河南工业大学 | 一种用于摩擦纳米发电机的介电材料的制备方法 |
| CN116410517B (zh) * | 2023-05-31 | 2025-05-02 | 河南工业大学 | 一种用于摩擦纳米发电机的介电材料的制备方法 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115862952A (zh) | 2023-03-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110453260B (zh) | 一种用于汗液检测的可穿戴传感器及其制备方法 | |
| Peng et al. | Electrochemical fabrication of functional gelatin-based bioelectronic interface | |
| CN107115559B (zh) | 在医用金属表面制备纳米银抗菌涂层的方法 | |
| CN110651183A (zh) | 金属支柱装置结构以及在电化学和/或电催化应用中制造和使用它们的方法 | |
| CN104233436B (zh) | 一种壳聚糖/明胶/纳米银导电抗菌生物材料及其制备方法 | |
| US20250215228A1 (en) | Thermo-reversible conducting hydrogels and their use for epidermal electrodes or standalone transmitter | |
| WO2024109839A2 (zh) | 一种柔性石墨烯电极及其制备方法和应用 | |
| WO2023045107A1 (zh) | 一种柔性干电极及其制备方法 | |
| CN106950267A (zh) | 一种柔性电极制备方法及柔性电极 | |
| US20230397870A1 (en) | Conductive Hydrogel-Based Wearable Health Monitors | |
| CN108195911B (zh) | 一种可重复性使用基于PDMS的Ag/AgCl微电极的制备方法和应用 | |
| KR100367164B1 (ko) | 금속도금 전처리제 및 그것을 사용하는 금속도금 방법 | |
| CN103983675A (zh) | 以不锈钢针为基底的铂和聚苯胺复合纳米纤维三维功能结构葡萄糖传感器及制备方法 | |
| CN113647952A (zh) | 基于银/氯化银纳米线制成的柔性干电极及其制备方法 | |
| CN115627504A (zh) | 一种复合材料、微电极及其制备方法和应用 | |
| CN113933371B (zh) | 一种柔性生物传感器电极的制备方法 | |
| CN113916957B (zh) | GPBCs/CC及其葡萄糖传感器和应用 | |
| CN111110222A (zh) | 一种生物蛋白柔性皮肤贴服式电极及其制备方法 | |
| CN114469844A (zh) | 一种抗菌微针及其制备方法 | |
| CN108395565B (zh) | 一种纳米多孔sebs薄膜的制备方法 | |
| CN109171699B (zh) | 一种蚕丝微针电极及其制备方法 | |
| Komorsky-Lovrić et al. | Abrasive stripping square wave voltammetry of some natural antioxidants | |
| JP2005033991A (ja) | 高分子アクチュエータ素子 | |
| CN112626583B (zh) | 一种导电基体软界面的构筑方法、微电极及应用 | |
| CN109920604A (zh) | 一种可拉伸式导电薄膜的制备方法 |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| 121 | Ep: the epo has been informed by wipo that ep was designated in this application |
Ref document number: 21958218 Country of ref document: EP Kind code of ref document: A1 |
|
| NENP | Non-entry into the national phase |
Ref country code: DE |
|
| 122 | Ep: pct application non-entry in european phase |
Ref document number: 21958218 Country of ref document: EP Kind code of ref document: A1 |
|
| 122 | Ep: pct application non-entry in european phase |
Ref document number: 21958218 Country of ref document: EP Kind code of ref document: A1 |
|
| 32PN | Ep: public notification in the ep bulletin as address of the adressee cannot be established |
Free format text: NOTING OF LOSS OF RIGHTS PURSUANT TO RULE 112(1) EPC (EPO FORM 1205 DATED 01.10.2024) |
|
| 122 | Ep: pct application non-entry in european phase |
Ref document number: 21958218 Country of ref document: EP Kind code of ref document: A1 |