CN111768895A - Air-permeable transparent flexible fiber-based surface electrode and preparation method thereof - Google Patents
Air-permeable transparent flexible fiber-based surface electrode and preparation method thereof Download PDFInfo
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
- D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0076—Electro-spinning characterised by the electro-spinning apparatus characterised by the collecting device, e.g. drum, wheel, endless belt, plate or grid
- D01D5/0084—Coating by electro-spinning, i.e. the electro-spun fibres are not removed from the collecting device but remain integral with it, e.g. coating of prostheses
Abstract
The invention discloses a breathable transparent flexible fiber-based surface skin electrode and a preparation method thereof. The motor comprises a transparent flexible nanofiber support and a transparent conductive nano three-dimensional network arranged above the transparent flexible nanofiber support in a filtering mode. The preparation method comprises the following steps: dissolving a high molecular polymer in an organic solvent to obtain a uniform polymer solution; mounting a polyethylene terephthalate plate on a fiber receiver for receiving a fiber support; installing an injector containing a polymer spinning solution in an electrostatic spinning device to spin into a nanofiber bracket; and adding the conductive nano material into a dispersion solvent to obtain a dispersion liquid, and compounding the dispersion liquid and the polymer nano fiber support to obtain the transparent flexible fiber-based surface electrode. The air-permeable transparent flexible fiber-based skin electrode prepared by the invention has good conductivity and transparency, can realize seamless joint of the skin electrode and human skin, and avoids the damage to the skin caused by air impermeability in the long-time real-time wearing process.
Description
Technical Field
The invention relates to a breathable transparent flexible fiber-based surface skin electrode and a preparation method thereof, belonging to the technical field of novel flexible electrodes.
Background
With the development of science and technology, wearable electronic devices are also gradually popularized in the lives of people. Among them, electrodes are essential parts of electronic devices, but most of the electronic devices at present use metal electrodes, and these hard electrodes make it difficult to make wearable electronic devices flexible and lightweight. In addition, in various wearable flexible electronic sensors, a flexible transparent electrode is an essential element, and the opaque property of the common metal electrode makes it difficult to apply the flexible electronic sensor to the novel flexible electronic devices.
At present, a plurality of wearable flexible sensors need to be attached to the skin of a human body in a seamless and smooth mode, and the high-fidelity sensing of various human body physiological signals can be guaranteed. Therefore, more and more researchers are working on developing a skin electrode having good conductivity and high transparency. Many skin electrodes are usually a composite of metal and plastic, and such skin electrodes have the problems of air impermeability in addition to wearing difficulty, causing skin inflammation, itching and the like after being worn on the skin for a long time, and being not good for skin health. Therefore, a low-cost, simple and efficient preparation method is needed to be developed to realize the preparation and development of the breathable transparent flexible fiber-based surface electrode.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the problem that the existing wearable flexible sensor is not breathable in the long-time wearing process and can bring harm to the skin is solved.
In order to solve the problems, the invention provides a breathable transparent flexible fiber-based surface skin electrode which is characterized by comprising a transparent flexible nanofiber support and a transparent conductive nano three-dimensional network arranged above the transparent flexible nanofiber support in a filtering mode, wherein the transparent flexible nanofiber support is obtained by an electrostatic spinning technology.
Preferably, the thickness of the transparent flexible nanofiber scaffold is 0.1-1 μm; the thickness of the transparent conductive nano three-dimensional network is 0.1-1 μm.
The invention also provides a preparation method of the air-permeable transparent flexible fiber-based skin electrode, which is characterized by comprising the following steps of:
the first step is as follows: dissolving a high molecular polymer for preparing a transparent flexible nanofiber scaffold in an organic solvent to obtain a uniform polymer solution; then, carrying out ultrasonic treatment to eliminate bubbles in the polymer solution for later use;
the second step is that: adding the obtained polymer solution into a spinning injector; cutting a polyethylene terephthalate (PET) plate into a required electrode shape by a laser cutting machine, and installing the PET plate on a fiber receiver for receiving a fiber support; installing an injector containing a polymer spinning solution in an electrostatic spinning device, and setting spinning processing technological parameters to spin a nanofiber bracket;
the third step: adding a conductive nano material for preparing a transparent conductive nano three-dimensional network into a dispersion solvent, performing ultrasonic dispersion to obtain uniform dispersion liquid, and compounding the dispersion liquid with a polymer nanofiber support through a suction filtration device or a filtering device to obtain the transparent flexible electrode.
Preferably, the polymer in the first step is any one or a mixture of more than one of polyvinylidene fluoride, polyacrylonitrile, polylactic acid, chitosan, polyvinyl alcohol, polyethylene glycol, polytrifluoroethylene, polystyrene, polyimide, polyvinylidene fluoride-hexafluoropropylene, ethyl cellulose, polyvinylidene fluoride-trifluoroethylene, polyethersulfone, polyetherimide, polyurethane and polyvinylidene fluoride-trichloro vinyl ether; the solvent is one or more of hexafluoroisopropanol, tetrahydrofuran, N-dimethylacetamide, acetone, ethanol, N-dimethylformamide, acetic acid, ultrapure water, formic acid, trifluoroacetic acid, trichloromethane and isopropanol dichloromethane; the mass concentration of the obtained polymer solution is 10-50%.
Preferably, the dissolving condition in the first step is 30-100 ℃, and the stirring is carried out for 0.5-12 hours; the technological parameters of the ultrasonic treatment are as follows: the ultrasonic power is 10-90W, and the ultrasonic time is 2-120 min.
Preferably, the process parameters of the laser cutting machine in the second step are as follows: the speed is 10-80 mm/s, and the power is 30-95%; the spinning processing parameters are as follows: the voltage is 7-50 kV, the receiving distance is 5-30 cm, the perfusion speed is 0.1-6 mL/h, the temperature is 10-35 ℃, and the relative humidity is 10-90%.
Preferably, the conductive nanomaterial used for preparing the transparent conductive network in the third step is at least one conductive nanomaterial selected from silver nanowires, copper nanowires, reduced graphene oxide and carbon nanotubes; the mass concentration of the conductive nano material in the dispersion liquid is 0.0001-5%.
Preferably, the process parameters of the ultrasound in the third step are as follows: the ultrasonic power is 10-90W, and the ultrasonic time is 2-120 min.
Preferably, the suction filtration device in the third step is a vacuum suction filtration device.
Preferably, the transparent flexible fiber-based epidermal electrode prepared in the third step is directly attached to the skin by van der waals force.
The invention develops and prepares the air-permeable fiber-based flexible epidermal electrode with good conductivity and transparency by combining the high conductivity of the conductive nano material and the flexibility of the nano fiber through the electrostatic spinning technology and the filtering technology, can realize the seamless joint use of the epidermal electrode and the skin of a human body,
compared with the prior art, the invention has the beneficial effects that:
1. the prepared air-permeable transparent flexible fiber-based surface electrode is different from the traditional hard metal electrode, the surface electrode has good transparency and flexibility, and the fiber-based electrode has high transparency and high conductivity, thereby laying a foundation for widening the application of wearable electronic devices in the field of flexible display. In addition, the ultra-light and ultra-thin characteristics of the electrode promote the development of electronic devices towards flexibility and light weight.
2. The prepared epidermal electrode has good air permeability, and when the electronic device is worn for a long time in real time, the electronic device is not breathable, so that skin itch, red swelling and inflammation are caused, and the skin health of a human body is not facilitated. The prepared electronic skin has good air permeability, and various skin problems caused by the problem of air impermeability when the wearable electronic device is in contact with the skin of a human body are avoided.
3. The invention combines the electrostatic spinning technology and the filtering technology, so that the surface electrode is obtained by compounding the nano conductive network and the transparent nano fiber, and the method avoids the methods of magnetron sputtering, vapor deposition and the like which have relatively complex using process and high cost. In addition, the prepared epidermal electrode does not need additional adhesive tape or punching fixation, and is directly attached to the skin in a seamless and tight manner by virtue of Van der Waals force, so that the sensing precision is greatly improved.
Drawings
FIG. 1 is a schematic diagram of the preparation of the breathable transparent flexible fiber-based skin electrode prepared in examples 1-3, wherein 1 is a nano conductive material dispersion, 2 is a PET framework, and 3 is an electrospun nanofiber scaffold;
FIG. 2 is a photograph of a real object of the breathable transparent flexible fiber-based skin electrode prepared in example 1;
FIG. 3 is a view showing the application of the breathable transparent flexible fiber-based skin electrode manufactured in example 1 to form a conductive path on the skin;
fig. 4 is a scanning electron microscope picture of the air-permeable transparent flexible fiber-based skin electrode prepared in example 2.
Fig. 5 is a picture of a real object of the breathable transparent flexible fiber-based skin electrode manufactured in example 2.
Fig. 6 is a scanning electron microscope picture of the air-permeable transparent flexible fiber-based skin electrode prepared in example 3.
Fig. 7 is a photograph of a real object of the breathable transparent flexible fiber-based skin electrode manufactured in example 3.
Detailed Description
In order to make the invention more comprehensible, preferred embodiments are described in detail below with reference to the accompanying drawings.
Example 1
The transparent flexible fiber-based surface skin electrode with the air permeability comprises a transparent flexible nanofiber support and a high-conductivity nano three-dimensional network arranged above the transparent flexible nanofiber support in a filtering mode, wherein the transparent flexible nanofiber support is obtained through an electrostatic spinning technology. The preparation method of the air-permeable transparent flexible fiber-based skin electrode comprises the following steps:
the first step is as follows: 10g of polyvinylidene fluoride (molecular weight is 320000) is added into 40g N, N-dimethylformamide solvent, and the mixture is heated and stirred for 3 hours in a water bath kettle at 60 ℃ to obtain the polyvinylidene fluoride electrostatic spinning solution with the uniform mass fraction of 20 wt%. The polymer solution was further sonicated for 30 minutes to remove air bubbles.
The second step is that: extracting 10mL of the polyvinylidene fluoride electrostatic spinning solution with the mass fraction of 20 wt% and adding the extracted solution into a spinning injector; cutting a polyethylene terephthalate (PET) plate into a shape of 1.5 multiplied by 2cm2 by a laser cutting machine, and mounting the PET plate on a fiber receiver for receiving a fiber support; and (3) installing an injector containing polyvinylidene fluoride electrostatic spinning solution in an electrostatic spinning device for spinning. The spinning parameters are as follows: voltage 25kV, receiving distance 20cm, perfusion speed 1.5mL/h, temperature 25 ℃, relative humidity 45%. The thickness of the electrospun fiber scaffold prepared was (1 μm).
The third step: then 10mg/mL of the silver nanowire dispersion was subjected to ultrasonic dispersion at room temperature (25 ℃) for 2 minutes at 300W to form a uniform stable dispersion system. And compounding the electrode with a polyvinylidene fluoride electrostatic spinning bracket in a suction filtration mode to obtain the transparent electrode.
The fourth step: the prepared air-permeable transparent flexible fiber-based epidermal electrode is directly attached to the skin by virtue of Van der Waals force, and a test is carried out.
The breathable transparent flexible fiber-based skin electrode manufactured as described above is shown in fig. 1 and 2. The resistance of the breathable transparent flexible fiber-based skin electrode was 10.765 Ω, indicating that the electrode had good electrical conductivity. Fig. 3 is an application of the prepared breathable transparent flexible fiber-based skin electrode to form a conductive path on the skin.
Example 2
The transparent flexible fiber-based surface skin electrode with the air permeability comprises a transparent flexible nanofiber support and a high-conductivity nano three-dimensional network arranged above the transparent flexible nanofiber support in a filtering mode, wherein the transparent flexible nanofiber support is obtained through an electrostatic spinning technology. The preparation method of the air-permeable transparent flexible fiber-based skin electrode comprises the following steps:
the first step is as follows: 3g of polyacrylonitrile (molecular weight 150000) was added to a 17g N, N-dimethylformamide solvent, and stirred at room temperature for 5 hours to obtain a uniform polyacrylonitrile electrospinning solution with a mass fraction of 15 wt%. The polymer solution was further sonicated for 30 minutes to remove air bubbles.
The second step is that: extracting 10mL of the polyacrylonitrile electrostatic spinning solution with the mass fraction of 15 wt% and adding the polyacrylonitrile electrostatic spinning solution into a spinning injector; cutting a polyethylene terephthalate (PET) plate into a shape of 1.5 multiplied by 2cm2 by a laser cutting machine, and mounting the PET plate on a fiber receiver for receiving a fiber support; and (3) installing the injector containing the polyacrylonitrile electrostatic spinning solution in an electrostatic spinning device for spinning. The spinning parameters are as follows: voltage 15kV, receiving distance 15cm, perfusion speed 2mL/h, temperature 25 ℃, relative humidity 40%. The thickness of the electrospun fiber scaffold prepared was (0.7 μm).
The third step: then, the 0.02 wt% carbon nanotube dispersion was subjected to ultrasonic dispersion at room temperature (25 ℃ C.) under 300W for 10 minutes to form a uniform stable dispersion system. And the transparent electrode is obtained by compounding the carbon fiber with a polyacrylonitrile electrostatic spinning bracket in a filtering mode.
The fourth step: the prepared air-permeable transparent flexible fiber-based epidermal electrode is directly attached to the skin by virtue of Van der Waals force, and a test is carried out.
The air-permeable transparent flexible fiber-based skin electrode prepared as described above is shown in fig. 1, 4 and 5, and it can be seen that the prepared electrode has better transparency. The resistance of the breathable transparent flexible fiber-based skin electrode was 10.585 Ω, indicating that the electrode had good electrical conductivity. Fig. 3 is an application of the prepared breathable transparent flexible fiber-based skin electrode to form a conductive path on the skin.
Example 3
The transparent flexible fiber-based surface skin electrode with the air permeability comprises a transparent flexible nanofiber support and a high-conductivity nano three-dimensional network arranged above the transparent flexible nanofiber support in a filtering mode, wherein the transparent flexible nanofiber support is obtained through an electrostatic spinning technology. The preparation method of the air-permeable transparent flexible fiber-based skin electrode comprises the following steps:
the first step is as follows: 10g of polyurethane (molecular weight: 350000) was added to 40g N, N-dimethylformamide solvent, and stirred at room temperature for 3 hours to obtain a uniform polyurethane electrospinning solution with a mass fraction of 20 wt%. And then ultrasonic treatment is carried out for 30 minutes to remove air bubbles in the polyurethane electrostatic spinning solution.
The second step is that: extracting 10mL of the obtained polyurethane electrostatic spinning solution with the mass fraction of 20 wt% and adding the extracted solution into a spinning injector; cutting a polyethylene terephthalate (PET) plate into a shape of 1.5 multiplied by 2cm2 by a laser cutting machine, and mounting the PET plate on a fiber receiver for receiving a fiber support; the syringe containing the polyurethane electrospinning solution was set in an electrospinning device to carry out spinning. The spinning parameters are as follows: voltage 30kV, receiving distance 20cm, perfusion speed 1mL/h, temperature 25 ℃, relative humidity 70%. The thickness of the electrospun fiber scaffold prepared was (1 μm).
The third step: . Then, 0.02 wt% of the reduced graphene oxide dispersion was subjected to ultrasonic dispersion at room temperature (25 ℃) for 5 minutes at 300W to form a uniform and stable dispersion system. And compounding the electrode with a polyurethane electrostatic spinning bracket in a filtering mode to obtain the transparent electrode.
The fourth step: the prepared air-permeable transparent flexible fiber-based epidermal electrode is directly attached to the skin by virtue of Van der Waals force, and a test is carried out.
The air-permeable transparent flexible fiber-based skin electrode prepared as described above is shown in fig. 1, 6 and 7, and it can be seen that the prepared electrode has better transparency. The resistance of the breathable transparent flexible fiber-based skin electrode was 10.617 Ω, indicating that the electrode had good electrical conductivity.
Claims (10)
1. The air-permeable transparent flexible fiber-based surface skin electrode is characterized by comprising a transparent flexible nanofiber support and a transparent conductive nano three-dimensional network arranged above the transparent flexible nanofiber support in a filtering mode, wherein the transparent flexible nanofiber support is obtained through an electrostatic spinning technology.
2. The breathable transparent flexible fiber-based skin electrode according to claim 1, wherein the transparent flexible nanofiber scaffold has a thickness of 0.1-1 μm; the thickness of the transparent conductive nano three-dimensional network is 0.1-1 μm.
3. The method for preparing a gas-permeable transparent flexible fiber-based skin electrode according to claim 1 or 2, comprising the steps of:
the first step is as follows: dissolving a high molecular polymer for preparing a transparent flexible nanofiber scaffold in an organic solvent to obtain a uniform polymer solution; then, carrying out ultrasonic treatment to eliminate bubbles in the polymer solution for later use;
the second step is that: adding the obtained polymer solution into a spinning injector; cutting a polyethylene terephthalate plate into a required electrode shape by a laser cutting machine, and installing the polyethylene terephthalate plate on a fiber receiver for receiving a fiber support; installing an injector containing a polymer spinning solution in an electrostatic spinning device, and setting spinning processing technological parameters to spin a nanofiber bracket;
the third step: adding a conductive nano material for preparing a transparent conductive nano three-dimensional network into a dispersion solvent, performing ultrasonic dispersion to obtain uniform dispersion liquid, and compounding the dispersion liquid with a polymer nanofiber support through a suction filtration device or a filtering device to obtain the transparent flexible fiber-based surface electrode.
4. The method for preparing the air-permeable transparent flexible fiber-based skin electrode according to claim 3, wherein the polymer in the first step is one or a mixture of more than one of polyvinylidene fluoride, polyacrylonitrile, polylactic acid, chitosan, polyvinyl alcohol, polyethylene glycol, polytrifluoroethylene, polystyrene, polyimide, polyvinylidene fluoride-hexafluoropropylene, ethyl cellulose, polyvinylidene fluoride-trifluoroethylene, polyethersulfone, polyetherimide, polyurethane and polyvinylidene fluoride-trichlorovinylether; the solvent is one or more of hexafluoroisopropanol, tetrahydrofuran, N-dimethylacetamide, acetone, ethanol, N-dimethylformamide, acetic acid, ultrapure water, formic acid, trifluoroacetic acid, trichloromethane and isopropanol dichloromethane; the mass concentration of the obtained polymer solution is 10-50%.
5. The method for preparing the breathable transparent flexible fiber-based skin electrode according to claim 3, wherein the dissolving conditions in the first step are 30-100 ℃ and stirring is carried out for 0.5-12 h; the technological parameters of the ultrasonic treatment are as follows: the ultrasonic power is 10-90W, and the ultrasonic time is 2-120 min.
6. The method for preparing the breathable transparent flexible fiber-based skin electrode according to claim 3, wherein the process parameters of the laser cutting machine in the second step are as follows: the speed is 10-80 mm/s, and the power is 30-95%; the spinning processing parameters are as follows: the voltage is 7-50 kV, the receiving distance is 5-30 cm, the perfusion speed is 0.1-6 mL/h, the temperature is 10-35 ℃, and the relative humidity is 10-90%.
7. The method for preparing the breathable transparent flexible fiber-based skin electrode according to claim 3, wherein the conductive nanomaterial used for preparing the transparent conductive network in the third step is at least one conductive nanomaterial selected from silver nanowires, copper nanowires, reduced graphene oxide, and carbon nanotubes; the mass concentration of the conductive nano material in the dispersion liquid is 0.0001-5%.
8. The method for preparing the breathable transparent flexible fiber-based skin electrode according to claim 3, wherein the process parameters of the ultrasound in the third step are as follows: the ultrasonic power is 10-90W, and the ultrasonic time is 2-120 min.
9. The method for manufacturing the breathable transparent flexible fiber-based skin electrode according to claim 3, wherein the suction filtration device in the third step is a vacuum suction filtration device.
10. The method for manufacturing a breathable transparent flexible fiber-based epidermal electrode of claim 3, wherein the transparent flexible fiber-based epidermal electrode manufactured in the third step is directly attached to the skin by van der Waals' force.
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| CN114059233A (en) * | 2021-11-17 | 2022-02-18 | 东华大学 | Transparent nanofiber membrane, preparation method thereof and application of transparent nanofiber membrane to transparent mask |
| CN114470335A (en) * | 2020-10-26 | 2022-05-13 | 天津理工大学 | Preparation method of safe, nontoxic and environment-friendly intelligent bionic skin |
| CN114618006A (en) * | 2022-04-11 | 2022-06-14 | 北京服装学院 | Intelligent wound dressing, preparation method and application thereof, and flexible sensor |
| CN114753061A (en) * | 2022-04-01 | 2022-07-15 | 苏州大学 | Preparation method of transparent polyurethane film based on ionic liquid group |
| CN114934327A (en) * | 2022-05-16 | 2022-08-23 | 电子科技大学长三角研究院(湖州) | Preparation method of millimeter-diameter fibrous aerogel electrode fully infiltrated by gel electrolyte |
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Application publication date: 20201013 |