CN113061285A - Preparation method of ultrathin porous stretchable film electrode - Google Patents
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- CN113061285A CN113061285A CN202110215869.8A CN202110215869A CN113061285A CN 113061285 A CN113061285 A CN 113061285A CN 202110215869 A CN202110215869 A CN 202110215869A CN 113061285 A CN113061285 A CN 113061285A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/36—After-treatment
- C08J9/365—Coating
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/04—Homopolymers or copolymers of ethene
- C08J2323/08—Copolymers of ethene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2353/00—Characterised by the use of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
- C08J2353/02—Characterised by the use of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers of vinyl aromatic monomers and conjugated dienes
Abstract
The invention belongs to the technical field of novel flexible electrodes, and discloses a preparation method of an ultrathin porous stretchable film electrode, which comprises the following steps: step one, dissolving a high molecular material in an organic solvent to obtain a uniform high molecular solution; step two, dripping the polymer solution on the surface of the liquid which has the surface tension larger than that of the polymer solution and does not dissolve the polymer material to form an ultrathin liquid film, and spontaneously forming a porous polymer film in the volatilization process of the organic solvent; and step three, preparing a conductive layer on the porous polymer film to obtain the ultrathin porous stretchable film electrode. The preparation method is simple, the cost is low, the electrode thickness can be regulated and controlled within hundreds of nanometers, and the prepared film electrode has better air permeability due to the porous structure and can realize long-time monitoring of human physiological electric signals.
Description
Technical Field
The invention belongs to the technical field of novel flexible electrodes, and particularly relates to a preparation method of an ultrathin porous stretchable film electrode.
Background
The electromyographic signals can reflect the muscle state of a human body in real time, and the long-term monitoring of the electromyographic signals can be applied to the fields of human health monitoring, intelligent artificial limbs, man-machine interaction and the like. The body surface electrode is the most common and widely applied myoelectricity monitoring electrode at present due to the non-invasive property. The gel wet electrode is mainly used in current commercialization, and because the gel wet electrode is easy to lose water, and the user is allergic in the long-term use process, the dry electrode made of flexible materials is concerned by people. However, most dry electrodes are made of airtight high polymer materials, and the prepared electrodes are attached to the body surface to cause sweat accumulation, so that the dry electrodes are easy to generate symptoms such as inflammation and allergy after being worn for a long time, and the long-term use of the dry electrodes is influenced. The methods for improving the air permeability of the electrode mainly include two methods: firstly, a substrate with good air permeability is selected, such as fabric, leather, non-woven fabric and the like. The gas permeability of the electrode is enhanced by preparing the electrode directly on these gas permeable substrates or attaching the electrode thereto. However, such materials generally have poor adhesion to the skin and affect the sensing performance of the electrode. Secondly, the conductive electrode is directly prepared on the skin. For example, the conductive layer is prepared on a soluble substrate, and after the conductive layer is attached to the skin of a human body, the substrate is dissolved, so that the conductive layer is directly prepared on the skin. However, such electrodes are less stable and may lose their sensing properties completely when touched slightly. Therefore, the preparation of the porous ultrathin stretchable film electrode becomes the invention hotspot of the body surface dry electrode.
Disclosure of Invention
Aiming at the problems that the adhesion and air permeability of a dry electrode and skin are difficult to realize simultaneously in the prior art proposed in the background technology and the application of the dry electrode in the long-term monitoring of the body surface myoelectricity is limited, the invention dissolves a high polymer material in an organic solvent, spreads the high polymer material on the surface of a liquid which has higher surface tension than the high polymer solution and does not dissolve the high polymer material to form an ultrathin liquid film, spontaneously forms an ultrathin porous stretchable film in the volatilization process of the organic solvent, and prepares a conductive layer on the ultrathin porous stretchable film to prepare the body surface myoelectricity electrode with excellent adhesion and air permeability.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention dissolves a high molecular material in an organic solvent, the high molecular material is dripped on water surface and spread into an ultrathin liquid film, a high molecular solute is separated out and shrinks to spontaneously form a porous ultrathin film along with the volatilization of the organic solvent, and the ultrathin porous stretchable myoelectric electrode is prepared after a layer of gold is magnetically sputtered on the ultrathin porous stretchable myoelectric electrode.
The technical scheme of the invention is specifically that the preparation method of the ultrathin porous stretchable film electrode comprises the following steps:
step one, dissolving a high molecular material in an organic solvent to obtain a uniform high molecular solution;
step two, dripping the polymer solution on the surface of the liquid which has the surface tension larger than that of the polymer solution and does not dissolve the polymer material to form an ultrathin liquid film, and spontaneously forming a porous polymer film in the volatilization process of the organic solvent;
and step three, preparing a conductive layer on the porous polymer film to obtain the ultrathin porous stretchable film electrode.
In the technical scheme of the invention, in the first step, the high molecular material is selected from one or a mixture of more of styrene butadiene block copolymer, hydrogenated styrene butadiene block copolymer and ethylene-vinyl acetate copolymer;
in the technical scheme of the invention, in the first step, the organic solvent is one or a mixture of more of carbon disulfide, chloroform, toluene, dichloromethane, dichloroethane, benzene, tetrahydrofuran, xylene and freon.
In the technical scheme of the invention, in the step one, the concentration of the polymer solution is 1 wt% to 15 wt%, and is preferably 7.5 wt%.
In the technical scheme of the invention, in the second step, the surface tension is greater than that of the polymer solution, the liquid which does not dissolve the polymer material is one or two of water or salt solution, and the salt solution is preferably NaCl solution, KCl solution or NaSO solution4And (3) solution.
In the technical scheme of the invention, in the second step, the dropping amount of the polymer solution is 10-100 μ L, preferably 15-20 μ L.
In the technical scheme of the invention, in the second step, the volatilization rate of the organic solvent is 0.4mg/cm2*min-5mg/cm2And regulating and controlling the pore size of the obtained film from no pore to centimeter-level pore.
In the second step, the thickness of the polymer film is 20nm to 1000nm, wherein the thinnest thickness of the polymer film capable of self-supporting is 100 nm.
In the third step, the method for preparing the conductive layer comprises magnetron sputtering, thermal evaporation, electron beam deposition, spraying method, blade coating method and dip coating method.
The metal material of magnetron sputtering, thermal evaporation and electron beam deposition comprises one or a combination of more of gold, silver, copper, platinum, titanium and iridium. The magnetron sputtering conditions are as follows: argon partial pressure: 3.8Pa, power 150W; the thickness of the sputtering is 7nm to 20nm, preferably 15 to 18 nm. The conditions of thermal evaporation and electron beam deposition are as follows: air pressure less than 3 x 10-3Pa, and the evaporation rate is 0.1-20nm/s, preferably 0.3-0.7 nm/s.
The conductive layer prepared by the spraying method, the blade coating method and the dip coating method adopts conductive nanoparticle aqueous dispersion as a conductive material, and preferably adopts metal nano-material, carbon nano-material and conductive polymer aqueous dispersion as the conductive material. The mass concentration of the conductive nano particle water dispersion liquid is 0.1-20mg/mL, and preferably 0.5-5 mg/mL. The spraying time is 1-20min, preferably 8-10 min.
In the technical scheme of the invention, the ultrathin porous stretchable film electrode prepared in the third step is directly attached to the skin by virtue of van der waals force.
The principle of the preparation method of the ultrathin porous stretchable film electrode is as follows: when two immiscible liquids are added to a block, a phenomenon of stratification occurs. By utilizing the phenomenon, the invention dissolves the high molecular material in the organic solvent, then the solution is dripped on the liquid surface which has the surface tension larger than that of the high molecular solution and does not dissolve the high molecular material to spread the liquid surface into a film, and the porous high molecular film can be spontaneously formed on the liquid surface after the organic reagent is volatilized. The thickness and porosity of the formed film can be regulated and controlled by controlling the concentration and the dropping amount of the polymer solution and the concentration of the organic solvent in the volatilization space, and then the ultrathin porous flexible stretchable electrode is prepared by preparing the conducting layer on the ultrathin porous film.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention dissolves the high molecular material in the organic solvent, then the surface tension is larger than the high molecular solution, and the liquid surface which does not dissolve the high molecular material is spread to form the ultrathin liquid film, and the ultrathin porous film is formed by self-release after the organic solvent is volatilized. Compared with a solid substrate, the formed film has smaller acting force with the liquid, and the prepared film can be easily fished up, so that the complex transfer process required in the traditional preparation method is avoided, and the maneuvering performance of the electrode is improved.
2. The liquid can be easily spread into a high-quality film with uniform thickness on the surface of the liquid, so the preparation method is simple, the requirement on instruments is low, and the electrode thickness can be regulated and controlled within hundreds of nanometers without complex instruments.
3. The electrode prepared by the invention can be well attached to the skin due to the thickness of the electrode in the order of hundreds of nanometers, and realizes high-performance monitoring of human physiological electrical signals.
4. The film electrode prepared by the invention has better air permeability due to the porous structure, can realize better air permeability when being attached to a human body, and can realize long-time monitoring of physiological electric signals of the human body.
Drawings
FIG. 1 is a schematic diagram of a method for preparing an ultrathin porous membrane electrode according to the present invention.
FIG. 2 is a diagram showing the optical mirror characteristics of ultrathin films with different apertures prepared in example 1 of the present invention. (upper row scale: 1cm, lower row scale: 500 μm).
FIG. 3 is a characterization graph of example 1, wherein FIG. a) is a thickness characterization of an ultrathin porous film; b) characterizing the surface light mirror of the ultrathin porous film; c) the stretchability of the ultrathin porous electrode is characterized; d) the ultrathin porous electrode is attached to the skin in an ultrathin way; e) collecting myoelectricity during movement; f) and after the ultrathin porous electrode is attached to the skin for 24 hours, the skin reacts.
FIG. 4 is a characterization of example 2, wherein FIG. a) a spray coating process is used to prepare a transparent ultrathin porous stretchable electrode; b) SEM characterization of the ultrathin porous stretchable electrode; c) and (3) the ultra-thin porous stretchable electrode is characterized by stretchability.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
The technical solutions in the embodiments of the present invention are clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the scope of the present invention.
Example 1
FIG. 1 is a schematic flow chart showing a method for manufacturing an ultrathin porous stretchable film electrode according to example 1 of the present invention. The preparation method comprises the following steps: dissolving hydrogenated styrene butadiene block copolymer in toluene to obtain polymer solution with mass fraction of 8 wt%, dropwise adding the polymer solution on the surface of 5 wt% NaCl aqueous solution, and controlling the toluene volatilization rate to be 0.40mg/cm2*min，0.7mg/cm2Min and 4.04mg/cm2At min, then fishing out the membrane and transferring17nm gold was sputtered thereon as a conductive layer. Wherein the toluene volatilization rate is 0.7mg/cm2Min gave a film thickness of 108nm and the resulting electrode stretchability exceeded 120%. The myoelectric monitoring instrument has excellent adhesion with skin, and can successfully monitor myoelectric signals in the movement process. Due to its excellent breathability, it does not have any effect on the skin 24h after the skin is attached.
Example 2
Dissolving styrene butadiene block copolymer in toluene to obtain 10% polymer solution, dripping the polymer solution on the surface of 5% NaCl water solution, and controlling the toluene volatilization rate to be 0.7mg/cm2And min, obtaining a film with the thickness of 700nm, and spraying silver nanowires with the concentration of 5mg/mL on the film to be used as a conducting layer. The prepared electrode can successfully collect myoelectricity.
Example 3
Dissolving ethylene-vinyl acetate copolymer in chloroform to prepare a solution with the mass fraction of 10 wt%, dropwise adding the solution on the surface of deionized water, and controlling the volatilization rate of toluene to be 0.7mg/cm2And min, obtaining a film with the thickness of 600nm, and spraying silver nanowires with the concentration of 5mg/mL on the film to be used as a conducting layer. The prepared electrode has stretchability of more than 200%.
First, result and characterization
FIG. 2 is a diagram showing the characteristics of the optical mirror of the ultrathin film with different aperture diameters in example 1 of the present invention. Wherein, the volatilization rate of toluene in the graph a) is 0.40mg/cm2A film formed at min; b) the toluene volatilization rate is 0.71mg/cm2A film formed at min; c) the volatilization rate of the toluene is 4.04mg/cm2Film formed at min (upper scale: 1cm, lower scale: 500 μm). From fig. 2, it can be seen that the pore size of the obtained ultrathin film is reduced from centimeter level (fig. 2a) to micrometer level (fig. 2b) with the increase of the toluene volatilization rate, and the preparation of a non-porous film can be realized by further increasing the toluene volatilization rate (fig. 2c), which indicates that the method provided by the present invention can realize effective regulation and control of the pore size of the ultrathin stretchable film.
FIG. 3 shows the toluene volatilization rate of 0.7mg/cm in example 12Min gives a characterization of the film with a thickness of 108nm,wherein, figure a) thickness characterization of ultrathin porous films; b) characterizing the surface light mirror of the ultrathin porous film; c) the stretchability of the ultrathin porous electrode is characterized; d) the ultrathin porous electrode is attached to the skin in an ultrathin way; e) collecting myoelectricity during movement; f) and after the ultrathin porous electrode is attached to the skin for 24 hours, the skin reacts. From the graph a), the thickness of the self-supporting film prepared by the invention is 108nm at the lowest, from the graph b), the prepared film has micron-level holes, from the graph c), the stretchability of the ultrathin porous electrode prepared by sputtering 17nm gold as a conductive layer is over 120 percent, from the graph d), the prepared electrode can be attached to the skin in a super mode, and the texture of the skin is clearly visible; from the graph e), it can be seen that the electrode can still effectively collect electromyographic signals in the process of human body movement, and has stronger motion artifact resistance, from the graph f), it can be seen that the electrode has better air permeability, and no inflammation phenomenon appears on the skin after 24h of contact with the human body, while the commercial gel electrode has obvious skin redness phenomenon.
FIG. 4 is a characterization of example 2, wherein FIG. a) a spray coating process is used to prepare a transparent ultrathin porous stretchable electrode; b) SEM characterization of the ultrathin porous stretchable electrode; c) and (3) the ultra-thin porous stretchable electrode is characterized by stretchability. From the graph a), it can be seen that the transparent self-supporting porous conductive electrode can be prepared by the method, from the graph b), it can be seen that AgNWs are randomly arranged on the film, the electrode is a porous electrode, and from the graph c), it can be seen that the stretchability of the prepared electrode exceeds 90%.
The above-mentioned embodiments, objects, technical solutions and advantages of the present invention are further described in detail, it should be understood that the above-mentioned embodiments are only examples of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. A preparation method of an ultrathin porous stretchable film electrode is characterized by comprising the following steps:
step one, dissolving a high molecular material in an organic solvent to obtain a uniform high molecular solution;
step two, dripping the polymer solution on the surface of the liquid which has the surface tension larger than that of the polymer solution and does not dissolve the polymer material to form an ultrathin liquid film, and spontaneously forming a porous polymer film in the volatilization process of the organic solvent;
and step three, preparing a conductive layer on the porous polymer film to obtain the ultrathin porous stretchable film electrode.
2. The method for preparing an ultrathin porous stretchable film electrode as claimed in claim 1, wherein in the step one, the high molecular material is selected from one or a mixture of styrene butadiene block copolymer, hydrogenated styrene butadiene block copolymer and ethylene-vinyl acetate copolymer.
3. The method as claimed in claim 1, wherein in the step one, the organic solvent is selected from one or more of carbon disulfide, chloroform, toluene, dichloromethane, dichloroethane, benzene, tetrahydrofuran, xylene, and freon.
4. The method for preparing an ultrathin porous stretchable film electrode as claimed in claim 1, wherein in the step one, the concentration of the polymer solution is 1 wt% to 15 wt%, preferably 7.5 wt%.
5. The method as claimed in claim 1, wherein in the step two, the surface tension is greater than that of the polymer solution, and the liquid not dissolving the polymer material is one or both of water and a salt solution, and the salt solution is preferably NaCl solution, KCl solution or NaSO solution4And (3) solution.
6. The method for preparing an ultrathin porous stretchable film electrode as claimed in claim 1, wherein in the second step, the dropping amount of the polymer solution is 10 μ L-100 μ L, preferably 15-20 μ L.
7. The method of claim 1, wherein the organic solvent is volatilized at a rate of 0.4mg/cm in the second step2*min-5mg/cm2And regulating and controlling the pore size of the obtained film from no pore to centimeter-level pore.
8. The method as claimed in claim 7, wherein in the second step, the thickness of the polymer film is 20nm to 1000nm, and the thinnest thickness of the self-supporting polymer film is 100 nm.
9. The method for preparing the ultrathin porous stretchable film electrode as claimed in claim 1, wherein in the third step, the method for preparing the conductive layer comprises magnetron sputtering, thermal evaporation, electron beam deposition, spraying, blade coating, and dip coating;
preferably, the metal material for magnetron sputtering, thermal evaporation and electron beam deposition comprises one or a combination of more of gold, silver, copper, platinum, titanium and iridium;
preferably, the magnetron sputtering conditions are as follows: argon partial pressure: 3.8Pa, power 150W; the thickness of the sputtering is 7nm-20nm, preferably 15-18 nm;
the conditions of thermal evaporation and electron beam deposition are as follows: air pressure less than 3 x 10-3Pa, the evaporation rate is 0.1-20nm/s, preferably 0.3-0.7 nm/s;
preferably, the conductive layer prepared by the spraying method, the blade coating method and the dip coating method adopts conductive nanoparticle aqueous dispersion as a conductive material, and preferably adopts metal nano-materials, carbon nano-materials and conductive polymer aqueous dispersion as a conductive material;
the mass concentration of the conductive nano particle water dispersion liquid is 0.1-20mg/mL, and preferably 0.5-5 mg/mL. The spraying time is 1-20min, preferably 8-10 min.
10. The method for preparing an ultra-thin porous stretchable film electrode according to claim 1, wherein the ultra-thin porous stretchable film electrode prepared in the third step is directly attached to the skin by van der waals force.
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| CN202110215869.8A CN113061285B (en) | 2021-02-26 | 2021-02-26 | Preparation method of ultrathin porous stretchable film electrode |
| PCT/CN2021/137592 WO2022179252A1 (en) | 2021-02-26 | 2021-12-13 | Method for preparing ultra-thin porous stretchable thin-film electrode |
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| CN114081499A (en) * | 2021-11-23 | 2022-02-25 | 吉林大学 | Flexible breathable surface electromyography electrode with two gradient holes and preparation method thereof |
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| WO2022179252A1 (en) * | 2021-02-26 | 2022-09-01 | 中国科学院深圳先进技术研究院 | Method for preparing ultra-thin porous stretchable thin-film electrode |
| CN116041777A (en) * | 2023-01-10 | 2023-05-02 | 四川大学 | Photovoltaic power generation material, power generation device, preparation method and application of power generation device |
| WO2023097765A1 (en) * | 2021-12-01 | 2023-06-08 | 中国科学院深圳先进技术研究院 | Stretchable multifunctional sensor, and manufacturing method therefor and application thereof |
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| WO2022179252A1 (en) | 2022-09-01 |
| CN113061285B (en) | 2021-10-22 |
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