CN111755166B - Preparation of flexible patterned electrode and flexible electronic device - Google Patents
Preparation of flexible patterned electrode and flexible electronic device Download PDFInfo
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Abstract
The preparation method of the flexible electrode comprises the steps of forming a first polydimethylsiloxane layer on filter paper, conducting personalized patterned cutting on the filter paper with the first polydimethylsiloxane layer, mixing carbon nano tubes and absolute ethyl alcohol for ultrasonic dispersion, mixing the mixture with poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid to obtain a mixed solution, conducting suction filtration on the mixed solution on the filter paper which is subjected to personalized patterned cutting and is formed with the first polydimethylsiloxane layer, and forming an electrode layer; the carbon nano tube flexible patterned electrode prepared by utilizing the personalized PDMS template can be changed in shape at will, can be attached to any curved surface for use, and enlarges the application range.
Description
Technical Field
The invention relates to a patterned flexible electrode prepared by utilizing an individualized PDMS template, a preparation method thereof and flexible electronic equipment.
Background
In recent years, with the rise of flexible electronic devices, flexible electrodes have become a research focus, but the flexibility of the flexible electrodes and the pattern unicity thereof severely restrict the development of the flexible electronic devices. Among materials for flexible electrodes, carbon materials are the most widely used, because carbon materials have the advantages of good physical and chemical stability, mechanical properties, environmental friendliness and the like, and especially because of the ultrahigh specific surface area and good electrical conductivity, the carbon materials become the current research hotspot and are applied to the preparation process of most electrodes. In addition, carbon nanotubes have the advantage of lower cost than graphene in carbon materials, and thus carbon nanotubes are also considered as a preferred material for preparing flexible electrodes. However, the film prepared from the carbon nanotubes has low toughness, cannot be bent or folded to a large extent, and the electrode pattern prepared from the carbon nanotubes is single at present, so that the preparation of a complex pattern is difficult to realize, which has certain limitation in practical application, especially in the wearable field.
The current preparation methods of the flexible electrode material comprise the following steps:
1. chemical vapor deposition: chemical vapor deposition is a chemical technology for preparing materials such as inorganic films, is widely applied to preparing graphene films at present, and can also be used for depositing active substances on carbon fiber substrates by using the chemical vapor deposition technology for catalysis or energy storage and the like. And (3) placing the carbon fiber substrate in a chemical vapor deposition furnace, and introducing metal compound active substances into a deposition area to gasify dust at high temperature to obtain a metal compound composite fiber electrode layer with uniform deposition.
2. Electrostatic spraying method: electrostatic spraying is a method of spraying an active material onto the surface of a carbon fiber substrate using electrical action. Graphene oxide was obtained in the experiment by the hummer modified method, followed by two hours of sonication in deionized water, stirring the sonicated graphene oxide and absolute ethanol for 30 minutes, then electro-spraying the mixed solution onto the surface of the nickel layer at 18kV operating voltage at an injection rate of 0.5mm per minute, and furthermore, the temperature of the spray deposition process was 50 ℃, with the aim of rapid evaporation of the solvent (ethanol-water mixture), which helped to form a uniform graphene oxide electrode layer.
3. Spin coating method: firstly, uniformly stirring the prepared conductive material (silver nanowires, carbon nanotubes, graphene and the like), and then spin-coating on a flexible substrate by using a spin coater to form a flexible electrode layer. In the experiment, the obtained silver nanowire solution is spin-coated on a PET substrate at 1000 revolutions per minute for 20s to form an AgNW-PET flexible electrode, and then nodes crossed by the silver nanowires are welded together by using a welding method to promote the conductivity of the film.
4. Electrostatic spinning: the electrostatic spinning is to use a strong electric field to spray and spin the polymer solution through an injector. In particular syringe needles under the action of a strong electrostatic fieldThe droplets are changed from spherical to conical, i.e., forming a "taylor cone", and the fiber filaments are spread from the tip of the cone and then absorbed on a flat plate or a roller receiver covered with aluminum or tin foil. PVB/SnCl in the experiment2NWs was electrospun onto a PVB film spin-coated with hydrophobic material and then immersed in a silver nitrate solution to form a catalytic seed layer of silver. The sample was then rinsed and transferred to an electrodeposition solution to form a silver nanowire layer.
Although the flexible electrode and the flexible electrode material can be prepared by the methods and have good conductivity, the prepared electrode has a single pattern, and other patterns cannot be well prepared according to requirements, so that the problems of cost rise in other aspects, limited application range and the like can be caused in practical application.
Disclosure of Invention
In view of the above, it is desirable to provide a flexible electrode capable of manufacturing complex patterns and bending and folding to a large extent and a method for manufacturing the same.
A method for preparing a patterned flexible electrode by using PDMS comprises the following steps:
forming a first polydimethylsiloxane layer on the filter paper;
performing personalized patterned cutting on the filter paper with the first polydimethylsiloxane layer;
mixing the carbon nano tube and absolute ethyl alcohol, performing ultrasonic dispersion, and mixing with poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid to obtain a mixed solution;
performing suction filtration on the mixed solution on the filter paper which is subjected to personalized patterned cutting and is provided with the first polydimethylsiloxane layer to form an electrode layer; and
and forming a second polydimethylsiloxane layer on the electrode layer, and heating and curing to obtain the flexible electrode.
In some of these embodiments, the step of forming a first polydimethylsiloxane layer on the filter paper comprises: and coating a solution containing polydimethylsiloxane and a curing agent on filter paper, and drying to form the first polydimethylsiloxane layer.
In some of the examples, the method for coating the solution containing polydimethylsiloxane and the curing agent on the filter paper is spin coating, the spin coating speed is 400-700rpm, the spin coating time is 8s-15s, and the thickness of the first polydimethylsiloxane layer is 50-200 microns.
In some of these embodiments, the method of cutting is laser cutting.
In some embodiments, the step of mixing the carbon nanotubes and absolute ethyl alcohol for ultrasonic dispersion, and then mixing the mixture with poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid to obtain a mixed solution comprises:
dispersing the carbon nano tube in absolute ethyl alcohol to obtain dispersion liquid of the carbon nano tube; and
and mixing the poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid with the dispersion liquid of the carbon nano tube to obtain the mixed liquid.
In some embodiments, the step of dispersing the carbon nanotubes in the absolute ethanol to obtain the dispersion of carbon nanotubes comprises:
mixing the carbon nano tube with the absolute ethyl alcohol and performing ultrasonic dispersion at 0 ℃ to obtain a mixture;
centrifuging the mixture, and taking supernatant to obtain dispersion liquid of the carbon nano tube;
and/or the step of mixing the poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid with the dispersion of carbon nanotubes comprises: mixing the poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid with the dispersion liquid of the carbon nanotubes, and then performing ultrasonic dispersion.
In some of these embodiments, the step of ultrasonically dispersing at 0 ℃ is performed in an ice bath environment.
In some embodiments, the solid-to-liquid ratio of the carbon nanotubes to the absolute ethyl alcohol is 0.002-0.008:50-150 ml; and/or the volume ratio of 3-8ml of poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid to the dispersion liquid of the carbon nano tube is 3-8 ml.
In some of these embodiments, the step of forming a second polydimethylsiloxane layer over the electrode layer comprises: a solution containing polydimethylsiloxane and a curing agent was poured onto the electrode layer.
In some of these embodiments, the step of preparing the solution comprising polydimethylsiloxane and the curing agent comprises: and mixing the polydimethylsiloxane and the curing agent, and stirring and degassing to obtain the solution containing the polydimethylsiloxane and the curing agent.
In some of these embodiments, the mass ratio of the polydimethylsiloxane to the curing agent is from 8:1 to 10: 1; and/or the curing agent is a polydimethylsiloxane curing agent.
In some of these embodiments, the step of heat curing comprises: heating at 70-95 deg.C for 15-60 min.
In some of these embodiments, the carbon nanotubes are multi-walled carbon nanotubes.
In addition, the invention also provides the flexible electrode prepared by the preparation method of the flexible electrode.
In addition, the invention also provides a flexible electronic device comprising the flexible electrode.
In some of these embodiments, the flexible electronic device is a wearable electronic device.
In some of these embodiments, the flexible electronic device is a flexible display screen or an implantable medical device.
In addition, a flexible electronic device is also provided.
Compared with the prior art, the preparation method of the flexible electrode provided by the invention has the advantages that a first polydimethylsiloxane layer is formed on filter paper, the filter paper with the first polydimethylsiloxane layer is subjected to personalized patterned cutting, the carbon nano tubes and absolute ethyl alcohol are mixed and ultrasonically dispersed, then the mixture is mixed with poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid to obtain a mixed solution, and the mixed solution is subjected to suction filtration on the filter paper with the first polydimethylsiloxane layer formed after the personalized patterned cutting to form an electrode layer; the carbon nano tube flexible patterned electrode prepared by utilizing the personalized PDMS template can be changed in shape at will, can be attached to any curved surface for use, and enlarges the application range.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments of the present invention or in the description of the prior art will be briefly described below, and it is obvious that the drawings described below are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
Fig. 1 is a flow chart illustrating a process for manufacturing a flexible electrode according to an embodiment.
Fig. 2 is a schematic structural diagram of a filter paper with a first polydimethylsiloxane layer formed after personalized pattern cutting according to an embodiment.
FIG. 3 is a schematic diagram illustrating the principle of preparing an electrode layer according to an embodiment.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the drawings are illustrative and intended to be illustrative of the invention and are not to be construed as limiting the invention.
In the description of the present invention, it is to be understood that the terms "upper", "lower", "horizontal", "inside", "outside", and the like, indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, are only for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present invention.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments.
As shown in fig. 1, a method for manufacturing a flexible electrode according to an embodiment of the present invention includes the following steps:
step S110: a first polydimethylsiloxane layer was formed on the filter paper.
In one embodiment, forming the first polydimethylsiloxane layer on the filter paper comprises the following steps: and coating a solution containing polydimethylsiloxane and a curing agent on filter paper, and drying to form the first polydimethylsiloxane layer.
In one embodiment, the method for applying the solution containing polydimethylsiloxane and the curing agent on the filter paper is spin coating, the spin coating speed is 400-700rpm, the spin coating time is 8s-15s, and the thickness of the first polydimethylsiloxane layer is 50-200 microns.
Step S120: and performing personalized patterned cutting on the filter paper with the first polydimethylsiloxane layer.
Specifically, the cutting method is laser cutting.
Fig. 2 is a schematic structural diagram of the filter paper with the first polydimethylsiloxane layer formed after the personalized patterning cutting.
Step S130: mixing the carbon nano tube and absolute ethyl alcohol, performing ultrasonic dispersion, and mixing with poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid to obtain a mixed solution.
In one embodiment, the step of mixing the carbon nanotubes and absolute ethyl alcohol for ultrasonic dispersion, and then mixing the mixture with poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid to obtain a mixed solution comprises the following steps: dispersing the carbon nano tube in the absolute ethyl alcohol to obtain a dispersion liquid of the carbon nano tube; and mixing the poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid with the dispersion liquid of the carbon nano tube to obtain the mixed liquid.
Specifically, the step of dispersing the carbon nanotubes in the absolute ethyl alcohol to obtain a dispersion liquid of the carbon nanotubes includes: mixing the carbon nano tube with the absolute ethyl alcohol, and performing ultrasonic dispersion at 0 ℃ to obtain a mixture; centrifuging the mixture, and taking supernatant to obtain dispersion liquid of the carbon nano tube; and/or the step of mixing the poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid with the dispersion of carbon nanotubes comprises: mixing the poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid with the dispersion liquid of the carbon nanotubes, and then performing ultrasonic dispersion.
Further, the step of ultrasonic dispersion at 0 ℃ is carried out in an ice bath environment.
In one embodiment, the solid-to-liquid ratio of the carbon nanotubes to the absolute ethyl alcohol is 0.002-0.008:50-150 ml; and/or the volume ratio of 3-8ml of poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid to the dispersion liquid of the carbon nano tube is 3-8 ml.
Step S140: and performing suction filtration on the mixed solution on the filter paper which is subjected to personalized patterned cutting and is provided with the first polydimethylsiloxane layer to form an electrode layer. Fig. 3 is a schematic diagram illustrating a principle of preparing an electrode layer according to the present embodiment.
Step S150: and forming a second polydimethylsiloxane layer on the electrode layer, and heating and curing to obtain the flexible electrode.
In some of these embodiments, the step of forming a second polydimethylsiloxane layer over the electrode layer comprises: a solution containing polydimethylsiloxane and a curing agent was poured onto the electrode layer.
Wherein the preparation of the solution containing polydimethylsiloxane and the curing agent comprises the following steps: and mixing the polydimethylsiloxane and the curing agent, and stirring and degassing to obtain the solution containing the polydimethylsiloxane and the curing agent.
In some of these embodiments, the mass ratio of the polydimethylsiloxane to the curing agent is from 8:1 to 10: 1; and/or the curing agent is a polydimethylsiloxane curing agent.
The step of heat curing comprises: heating at 70-95 deg.C for 15-60 min.
According to the preparation method of the flexible electrode, a first polydimethylsiloxane layer is formed on filter paper, the filter paper with the first polydimethylsiloxane layer is subjected to personalized patterned cutting, carbon nanotubes and absolute ethyl alcohol are mixed and subjected to ultrasonic dispersion, then the mixture is mixed with poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid to obtain a mixed solution, and the mixed solution is subjected to suction filtration on the filter paper with the first polydimethylsiloxane layer formed after the personalized patterned cutting to form an electrode layer; the carbon nano tube flexible patterned electrode prepared by utilizing the personalized PDMS template can be changed in shape at will, can be attached to any curved surface for use, and enlarges the application range.
The preparation method is simple to operate, and meanwhile, due to the characteristics of biocompatibility, low cost, no toxicity and the like of PDMS, the processing difficulty and the preparation cost of the sensor are greatly reduced by matching with a simple structure and an external circuit.
The flexible electrode prepared by the method for preparing a flexible electrode according to an embodiment and a flexible electronic device including the flexible electrode are wearable electronic devices, flexible display screens or implantable medical devices. The flexible electronic equipment has the advantages that by adopting the flexible electrode, the flexible electronic equipment has higher sensitivity, higher precision, larger sensing range and longer service life.
The following are specific examples:
example 1
The tactile sensor of the present embodiment is prepared as follows:
(1) the solution containing polydimethylsiloxane and the curing agent was spin-coated on filter paper at 400rpm and dried to form the first polydimethylsiloxane layer.
(2) And performing personalized patterned cutting on the filter paper with the first polydimethylsiloxane layer.
(3) Under an ice-bath environment, mixing the carbon nano tube with the absolute ethyl alcohol according to a solid-liquid ratio of 0.004 g: 80ml, mixing the carbon nano tube with the absolute ethyl alcohol, performing ultrasonic dispersion at 0 ℃ to obtain a mixture, centrifuging the mixture, taking supernatant to obtain dispersion liquid of the carbon nano tube, mixing the poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid with the volume ratio of the dispersion liquid of the carbon nano tube being 5ml, and performing ultrasonic dispersion to obtain the mixed solution;
(4) carrying out laser cutting on the filter paper with the first polydimethylsiloxane layer, placing the mixed solution on the first polydimethylsiloxane layer, and carrying out suction filtration to form an electrode layer;
(5) mixing the polydimethylsiloxane and the curing agent, and stirring and degassing to obtain the solution containing the polydimethylsiloxane and the curing agent, wherein the mass ratio of the polydimethylsiloxane to the curing agent is 5: 0.5; and the curing agent is polydimethylsiloxane curing agent, and a solution containing polydimethylsiloxane and the curing agent is poured on the electrode layer, heated at 90 ℃ for 20 minutes and heated and cured to obtain the flexible electrode.
Example 2
The process for preparing the flexible electrode of this embodiment is substantially the same as that of embodiment 1, except that the carbon nanotubes of step (2) of this embodiment are multi-walled carbon nanotubes.
And (3) testing:
the resistance values of the flexible electrodes of examples 1-2 were tested using a Victor instrument (Victor) VC9806 digital multimeter to obtain the conductivity of the corresponding flexible electrode. The test data were greater than 50 times and the arithmetic mean values are listed in the table below. The bending and torsion properties of the flexible electrodes of examples 1-2 were tested using a mechanical testing machine of ESM303 of Mark-10 Corporation to obtain the bending and torsion properties of the corresponding flexible electrodes. The test data are shown in the following table with the maximum values.
TABLE 1
Resistance value | Bending properties | Angle of torsion | |
Example 1 | 20.13 | 90° | 90° |
Example 2 | 22.06 | 90° | 90° |
As can be seen from table 1, the flexible electrode provided in the above embodiment of the present invention has better conductivity and bending performance and a larger torsion angle.
The foregoing is considered as illustrative only of the preferred embodiments of the invention, and is presented merely for purposes of illustration and description of the principles of the invention and is not intended to limit the scope of the invention in any way. Any modifications, equivalents and improvements made within the spirit and principles of the invention and other embodiments of the invention without the creative effort of those skilled in the art are included in the protection scope of the invention based on the explanation here.
Claims (15)
1. A method for preparing a patterned flexible electrode by utilizing a personalized PDMS template is characterized by comprising the following steps:
forming a first polydimethylsiloxane layer on the filter paper;
performing personalized patterned cutting on the filter paper with the first polydimethylsiloxane layer;
mixing the carbon nano tube and absolute ethyl alcohol, performing ultrasonic dispersion, and mixing with poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid to obtain a mixed solution;
performing suction filtration on the mixed solution on the filter paper which is subjected to personalized patterned cutting and is provided with the first polydimethylsiloxane layer to form an electrode layer; and
forming a second polydimethylsiloxane layer on the electrode layer, and heating and curing to obtain a flexible electrode;
the step of mixing the carbon nano tube and absolute ethyl alcohol for ultrasonic dispersion, and then mixing the carbon nano tube and absolute ethyl alcohol with poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid to obtain a mixed solution comprises the following steps:
dispersing the carbon nano tube in absolute ethyl alcohol to obtain dispersion liquid of the carbon nano tube; and
mixing the poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid with the dispersion liquid of the carbon nano tube to obtain the mixed liquid;
the step of dispersing the carbon nanotubes in the absolute ethyl alcohol to obtain the dispersion liquid of the carbon nanotubes comprises:
mixing the carbon nano tube with the absolute ethyl alcohol and performing ultrasonic dispersion at 0 ℃ to obtain a mixture;
centrifuging the mixture, and taking supernatant to obtain dispersion liquid of the carbon nano tube;
and/or the step of mixing the poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid with the dispersion of carbon nanotubes comprises: mixing the poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid with the dispersion liquid of the carbon nanotubes, and then performing ultrasonic dispersion.
2. The method of preparing a patterned flexible electrode using a personalized PDMS template of claim 1, wherein the step of forming a first polydimethylsiloxane layer on the filter paper comprises: and coating a solution containing polydimethylsiloxane and a curing agent on filter paper, and drying to form the first polydimethylsiloxane layer.
3. The method of claim 2, wherein the solution containing polydimethylsiloxane and curing agent is applied on the filter paper by spin coating at 400-700rpm for 8-15 s, and the thickness of the first polydimethylsiloxane layer is 50-200 μm.
4. The method of fabricating a patterned flexible electrode using a personalized PDMS template of claim 1, wherein the cutting method is laser cutting.
5. The method of preparing a patterned flexible electrode using a personalized PDMS template according to claim 4, wherein the step of ultrasonically dispersing at 0 ℃ is performed in an ice bath environment.
6. The method of any of claims 3-5, wherein the solid to liquid ratio of the carbon nanotubes to the absolute ethanol is 0.002-0.008:50-150 ml; and/or the volume ratio of 3-8ml of poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid to the dispersion liquid of the carbon nano tube is 3-8 ml.
7. The method of preparing a patterned flexible electrode using a personalized PDMS template of claim 1, wherein the step of forming a second polydimethylsiloxane layer on the electrode layer comprises: a solution containing polydimethylsiloxane and a curing agent was poured onto the electrode layer.
8. The method of preparing a patterned flexible electrode using a personalized PDMS template according to claim 2 or 7, wherein the step of preparing the solution containing polydimethylsiloxane and curing agent comprises: and mixing the polydimethylsiloxane and the curing agent, and stirring and degassing to obtain the solution containing the polydimethylsiloxane and the curing agent.
9. The method of preparing a patterned flexible electrode using a personalized PDMS template according to claim 8, wherein the mass ratio of the polydimethylsiloxane to the curing agent is 8:1 to 10: 1; and/or the curing agent is a polydimethylsiloxane curing agent.
10. The method of preparing a patterned flexible electrode using a personalized PDMS template of claim 1, wherein the step of heat curing comprises: heating at 70-95 deg.C for 15-60 min.
11. The method of claim 1, wherein the carbon nanotubes are multi-walled carbon nanotubes.
12. A flexible electrode prepared by the method of preparing a patterned flexible electrode using a personalized PDMS template according to any one of claims 1 to 11.
13. A flexible electronic device comprising the flexible electrode of claim 12.
14. The flexible electronic device of claim 13, wherein the flexible electronic device is a wearable electronic device.
15. The flexible electronic device of claim 14, wherein the flexible electronic device is a flexible display screen or an implantable medical device.
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