WO2021253274A1 - 一种柔性图案化电极的制备和柔性电子设备 - Google Patents
一种柔性图案化电极的制备和柔性电子设备 Download PDFInfo
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- WO2021253274A1 WO2021253274A1 PCT/CN2020/096539 CN2020096539W WO2021253274A1 WO 2021253274 A1 WO2021253274 A1 WO 2021253274A1 CN 2020096539 W CN2020096539 W CN 2020096539W WO 2021253274 A1 WO2021253274 A1 WO 2021253274A1
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- 238000002360 preparation method Methods 0.000 title abstract description 14
- -1 polydimethylsiloxane Polymers 0.000 claims abstract description 117
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- 235000013870 dimethyl polysiloxane Nutrition 0.000 claims abstract description 79
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- 239000002041 carbon nanotube Substances 0.000 claims abstract description 56
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- 238000002156 mixing Methods 0.000 claims abstract description 20
- 229920000172 poly(styrenesulfonic acid) Polymers 0.000 claims abstract description 19
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- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 claims abstract description 7
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- YTPLMLYBLZKORZ-UHFFFAOYSA-N Thiophene Chemical compound C=1C=CSC=1 YTPLMLYBLZKORZ-UHFFFAOYSA-N 0.000 claims description 4
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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
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/044—Forming conductive coatings; Forming coatings having anti-static properties
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D165/00—Coating compositions based on macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain; Coating compositions based on derivatives of such polymers
-
- G—PHYSICS
- G09—EDUCATION; CRYPTOGRAPHY; DISPLAY; ADVERTISING; SEALS
- G09F—DISPLAYING; ADVERTISING; SIGNS; LABELS OR NAME-PLATES; SEALS
- G09F9/00—Indicating arrangements for variable information in which the information is built-up on a support by selection or combination of individual elements
- G09F9/30—Indicating arrangements for variable information in which the information is built-up on a support by selection or combination of individual elements in which the desired character or characters are formed by combining individual elements
-
- 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
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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
- H01B5/14—Non-insulated conductors or conductive bodies characterised by their form comprising conductive layers or films on insulating-supports
Definitions
- the invention relates to a patterned flexible electrode prepared by using a personalized PDMS template, a preparation method thereof, and a flexible electronic device.
- Chemical vapor deposition is a chemical technology for preparing inorganic films and other materials. It is currently widely used to prepare graphene films. Chemical vapor deposition technology can also be used to deposit active substances on carbon fiber substrates for catalysis or energy. Reserve etc.
- the carbon fiber substrate is placed in a chemical vapor deposition furnace, and high-temperature gasification dust of the metal compound active material is passed into the deposition area to obtain a uniformly deposited metal compound composite fiber electrode layer.
- Electrostatic spraying is a method of spraying the active material on the surface of the carbon brazing substrate by electric action.
- graphene oxide was obtained by hummer's improved method, and then sonicated in deionized water for two hours, the sonicated graphene oxide and absolute ethanol were stirred for 30 minutes, and then the mixed solution was placed under 18kV working voltage Electrospray onto the surface of the nickel layer at an injection rate of 0.5mm per minute.
- the temperature of the spray deposition process is 50°C. The purpose is to quickly evaporate the solvent (ethanol-water mixture), which helps to form a uniform graphene oxide Electrode layer.
- Electrospinning uses a strong electric field to spray polymer solution through a syringe. Specifically, under the action of a strong electrostatic field, the droplet at the needle of the syringe will change from a spherical shape to a conical shape to form a "Taylor cone", and extend from the tip of the cone to obtain fibrous filaments, which are then adsorbed on a flat plate covered with aluminum or tin foil. On the roller receiver.
- the PVB/SnCl 2 NWs in the experiment are electrospun onto a spin-coated hydrophobic PVB film, and then immersed in a silver nitrate solution to form a silver catalytic seed layer. The sample is then rinsed and transferred to an electrolytic deposition solution to form a layer of silver nanowires.
- a method for preparing a patterned flexible electrode using PDMS includes the following steps:
- the carbon nanotubes and absolute ethanol are mixed and ultrasonically dispersed, and then mixed with poly(3,4-ethylenedioxythiophene)-polystyrene sulfonic acid to obtain a mixed solution;
- a second polydimethylsiloxane layer is formed on the electrode layer and cured by heating to obtain a flexible electrode.
- the step of forming the first polydimethylsiloxane layer on the filter paper includes: coating a solution containing polydimethylsiloxane and a curing agent on the filter paper, and drying, The first polydimethylsiloxane layer is formed.
- the method for coating the solution containing polydimethylsiloxane and curing agent on the filter paper is spin coating, the spin coating speed is 400-700rpm, and the spin coating time is 8s-15s.
- the thickness of the first polydimethylsiloxane layer is 50-200 microns.
- the cutting method is laser cutting.
- the step of mixing carbon nanotubes and absolute ethanol to ultrasonically disperse, and then mixing with poly(3,4-ethylenedioxythiophene)-polystyrene sulfonic acid to obtain a mixed solution includes:
- the poly(3,4-ethylenedioxythiophene)-polystyrene sulfonic acid is mixed with the carbon nanotube dispersion liquid to obtain the mixed liquid.
- the step of dispersing the carbon nanotubes in the absolute ethanol to obtain a dispersion liquid of carbon nanotubes includes:
- the step of mixing the poly(3,4-ethylenedioxythiophene)-polystyrene sulfonic acid with the dispersion of carbon nanotubes includes: mixing the poly(3,4-ethylenedioxythiophene) Thiophene)-polystyrene sulfonic acid is mixed with the dispersion liquid of carbon nanotubes, and then ultrasonically dispersed.
- the ultrasonic dispersion step at 0°C is performed in an ice bath environment.
- the solid-to-liquid ratio of the carbon nanotubes to the absolute ethanol is 0.002-0.008:50-150ml; and/or, the poly(3,4-ethylenedioxythiophene)-poly
- the volume ratio of 3-8 ml of styrene sulfonic acid to the dispersion liquid of carbon nanotubes is 3-8 ml.
- the step of forming a second polydimethylsiloxane layer on the electrode layer includes: pouring a solution containing polydimethylsiloxane and a curing agent on the electrode layer superior.
- the step of preparing the solution containing polydimethylsiloxane and curing agent includes: mixing the polydimethylsiloxane and the curing agent, stirring and degassing, The solution containing polydimethylsiloxane and curing agent is obtained.
- the mass ratio of the polydimethylsiloxane and the curing agent is 8:1-10:1; and/or, the curing agent is polydimethylsiloxane curing Agent.
- the heating and curing step includes heating at 70-95° C. for 15-60 minutes.
- the carbon nanotubes are multi-walled carbon nanotubes.
- the present invention also provides a flexible electrode prepared by the method for preparing the flexible electrode.
- the present invention also provides a flexible electronic device including the flexible electrode.
- the flexible electronic device is a wearable electronic device.
- the flexible electronic device is a flexible display screen or an implantable medical device.
- a flexible electronic device is also provided.
- the method for preparing a flexible electrode is to form a first polydimethylsiloxane layer on a filter paper to form the filter paper with the first polydimethylsiloxane layer
- the carbon nanotubes and absolute ethanol are mixed and ultrasonically dispersed, and then mixed with poly(3,4-ethylenedioxythiophene)-polystyrene sulfonic acid to obtain a mixed solution.
- the flexible patterned carbon nanotube electrode prepared by the personalized PDMS template of the present invention can change its shape arbitrarily, and can be used in conjunction with any curved surface, which expands the scope of use.
- Fig. 1 is a preparation flow chart of a flexible electrode according to an embodiment.
- FIG. 2 is a schematic structural diagram of a filter paper formed with a first polydimethylsiloxane layer after personalized patterning and cutting according to an embodiment.
- FIG. 3 is a schematic diagram of the principle of preparing an electrode layer according to an embodiment.
- a method for preparing a flexible electrode includes the following steps:
- Step S110 forming a first polydimethylsiloxane layer on the filter paper.
- forming the first polydimethylsiloxane layer on the filter paper includes the following steps: coating a solution containing polydimethylsiloxane and a curing agent on the filter paper, and drying to form The first polydimethylsiloxane layer.
- the method for coating the solution containing polydimethylsiloxane and curing agent on the filter paper is spin coating, the spin coating speed is 400-700rpm, and the spin coating time is 8s-15s, The thickness of the first polydimethylsiloxane layer is 50-200 microns.
- Step S120 cutting the filter paper on which the first polydimethylsiloxane layer is formed in a personalized pattern.
- the cutting method is laser cutting.
- FIG. 2 is a schematic diagram of the filter paper formed with the first polydimethylsiloxane layer after being cut in a personalized pattern.
- Step S130 the carbon nanotubes and absolute ethanol are mixed and ultrasonically dispersed, and then mixed with poly(3,4-ethylenedioxythiophene)-polystyrene sulfonic acid to obtain a mixed solution.
- the step of mixing carbon nanotubes and absolute ethanol with ultrasonic dispersion, and then mixing with poly(3,4-ethylenedioxythiophene)-polystyrene sulfonic acid to obtain a mixed solution includes: Dispersing nanotubes in the absolute ethanol to obtain a dispersion of carbon nanotubes; and mixing the poly(3,4-ethylenedioxythiophene)-polystyrene sulfonic acid with the dispersion of carbon nanotubes , To obtain the mixed solution.
- the step of dispersing the carbon nanotubes in the absolute ethanol to obtain a dispersion liquid of the carbon nanotubes includes: mixing the carbon nanotubes with the absolute ethanol, and at 0°C Ultrasonic dispersion to obtain a mixture; centrifuge the mixture, take the supernatant to obtain the carbon nanotube dispersion; and/or, combine the poly(3,4-ethylenedioxythiophene)-polystyrene
- the step of mixing sulfonic acid with the dispersion of carbon nanotubes includes: mixing the poly(3,4-ethylenedioxythiophene)-polystyrene sulfonic acid with the dispersion of carbon nanotubes, and then performing ultrasound. dispersion.
- the step of ultrasonic dispersion at 0°C is carried out in an ice bath environment.
- the solid-to-liquid ratio of the carbon nanotubes to the absolute ethanol is 0.002-0.008:50-150ml; and/or, the poly(3,4-ethylenedioxythiophene)-poly
- the volume ratio of 3-8 ml of styrene sulfonic acid to the dispersion liquid of carbon nanotubes is 3-8 ml.
- Step S140 Suction and filter the mixed solution on the filter paper on which the first polydimethylsiloxane layer is formed after personalized patterning and cutting to form an electrode layer.
- FIG. 3 is a schematic diagram of the principle of preparing the electrode layer in this embodiment.
- Step S150 forming a second polydimethylsiloxane layer on the electrode layer, and curing it by heating to obtain a flexible electrode.
- the step of forming a second polydimethylsiloxane layer on the electrode layer includes: pouring a solution containing polydimethylsiloxane and a curing agent on the electrode layer superior.
- the preparation step of the solution containing polydimethylsiloxane and curing agent includes: mixing the polydimethylsiloxane and the curing agent, stirring and degassing, to obtain the polydimethylsiloxane containing A solution of dimethylsiloxane and curing agent.
- the mass ratio of the polydimethylsiloxane and the curing agent is 8:1-10:1; and/or, the curing agent is polydimethylsiloxane curing Agent.
- the heating and curing step includes heating at 70-95°C for 15-60 minutes.
- a first polydimethylsiloxane layer is formed on a filter paper, and the filter paper on which the first polydimethylsiloxane layer is formed is cut in a personalized pattern, and the carbon Nanotubes and anhydrous ethanol are mixed and ultrasonically dispersed, and then mixed with poly(3,4-ethylenedioxythiophene)-polystyrene sulfonic acid to obtain a mixed solution.
- the mixed solution is formed after personalized patterning and cutting.
- the carbon nanotube flexible patterned electrode prepared by using a personalized PDMS template in the present invention can change its shape arbitrarily, and can be used in conjunction with any curved surface, which expands the scope of use.
- the above preparation method is simple to operate, and at the same time, due to the biocompatibility, low cost, non-toxicity and other characteristics of PDMS itself, combined with a simple structure and an external circuit, the processing difficulty and preparation cost of the sensor are greatly reduced.
- the flexible electronic device can make it have higher sensitivity, higher precision, larger sensing range and longer service life.
- the preparation process of the tactile sensor in this implementation is as follows:
- the filter paper on which the first polydimethylsiloxane layer is formed is individually patterned and cut.
- the carbon nanotubes and the absolute ethanol are mixed at a solid-liquid ratio of 0.004g:80ml, and the carbon nanotubes and the absolute ethanol are mixed and heated at 0°C.
- Ultrasonic dispersion to obtain a mixture, centrifuge the mixture, take the supernatant to obtain the dispersion of the carbon nanotubes, and combine the poly(3,4-ethylenedioxythiophene)-polystyrene sulfonic acid with the
- the volume ratio of the dispersion liquid of the carbon nanotubes is 5 ml and mixed, and then ultrasonically dispersed to obtain the mixed liquid;
- the preparation process of the flexible electrode of this embodiment is roughly the same as that of Embodiment 1, except that the carbon nanotubes in step (2) of this embodiment are multi-walled carbon nanotubes.
- a Victor VC9806 digital multimeter was used to test the resistance values of the flexible electrodes of Examples 1 to 2 to obtain the corresponding conductivity of the flexible electrodes.
- the test data is greater than 50 times, and the arithmetic average is listed in the table below.
- the ESM303 mechanical testing machine of Mark-10 Corporation was used to test the bending and torsion properties of the flexible electrodes of Examples 1 to 2 to obtain the corresponding bending and torsion properties of the flexible electrodes.
- the maximum value of the test data is listed in the table below.
- the flexible electrode provided by the above-mentioned embodiment of the present invention has better electrical conductivity and bending performance and a larger torsion angle.
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Abstract
Description
电阻值 | 弯曲性能 | 扭转角度 | |
实施例1 | 20.13 | 90° | 90° |
实施例2 | 22.06 | 90° | 90° |
Claims (17)
- 一种利用个性化PDMS模板制备图案化柔性电极的方法,其特征在于,包括如下步骤:在滤纸上形成第一聚二甲基硅氧烷层;将形成有所述第一聚二甲基硅氧烷层的所述滤纸进行个性化图案化切割;将碳纳米管和无水乙醇混合超声分散,再与聚(3,4-乙烯二氧噻吩)-聚苯乙烯磺酸混合得到混合液;将所述混合液于个性化图案化切割后的形成有所述第一聚二甲基硅氧烷层的所述滤纸上进行抽滤,形成电极层;及在所述电极层上形成第二聚二甲基硅氧烷层,经加热固化,得到柔性电极。
- 如权利要求1所述的柔性电极的制备方法,其特征在于,所述在滤纸上形成第一聚二甲基硅氧烷层的步骤包括:将含有聚二甲基硅氧烷和固化剂的溶液涂敷在滤纸上,经干燥,形成所述第一聚二甲基硅氧烷层。
- 如权利要求2所述的柔性电极的制备方法,其特征在于,所述将含有聚二甲基硅氧烷和固化剂的溶液涂敷在滤纸上的方法为旋涂,旋涂速度是400-700rpm,旋涂时间是8s-15s,所述第一聚二甲基硅氧烷层的厚度50-200微米。
- 如权利要求1所述的柔性电极的制备方法,其特征在于,所述切割的方法为激光切割。
- 如权利要求1所述的柔性电极的制备方法,其特征在于,所述将碳纳米管和无水乙醇混合超声分散,再与聚(3,4-乙烯二氧噻吩)-聚苯乙烯磺酸混合得到混合液的步骤包括:将所述碳纳米管分散在无水乙醇中,得到碳纳米管的分散液;及将所述聚(3,4-乙烯二氧噻吩)-聚苯乙烯磺酸与所述碳纳米管的分散液混合,得到所述混合液。
- 如权利要求5所述的柔性电极的制备方法,其特征在于,所述将所述碳纳米管分散在所述无水乙醇中,得到碳纳米管的分散液的步骤包括:将所述碳纳米管与所述无水乙醇混合并在0℃下超声分散,得到混合物;将所述混合物离心处理,取上清液,得到所述碳纳米管的分散液;及/或,将所述聚(3,4-乙烯二氧噻吩)-聚苯乙烯磺酸与所述碳纳米管的分散液混合的步骤包括:将所述聚(3,4-乙烯二氧噻吩)-聚苯乙烯磺酸与所述碳纳米管的分散液混合,然后进行超声分散。
- 如权利要求6所述的柔性电极的制备方法,其特征在于,所述在0℃下超声分散的步骤是在冰浴环境下进行的。
- 如权利要求5-7任一项所述的柔性电极的制备方法,其特征在于,所述碳纳米管与所述无水乙醇的固液比为0.002-0.008:50-150ml;及/或,所述聚(3,4-乙烯二氧噻吩)-聚苯乙烯磺酸3-8ml与所述碳纳米管的分散液的体积比为3-8ml。
- 如权利要求1所述的柔性电极的制备方法,其特征在于,所述在所述电极层上形成第二聚二甲基硅氧烷层的步骤包括:将含有聚二甲基硅氧烷和固化剂的溶液倒在所述电极层上。
- 如权利要求2或9所述的柔性电极的制备方法,其特征在于,所述含有聚二甲基硅氧烷和固化剂的溶液的制备步骤包括:将所述聚二甲基硅氧烷和所述固化剂混合,经搅拌和脱气,得到所述含有聚二甲基硅氧烷和固化剂的溶液。
- 如权利要求10所述的柔性电极的制备方法,其特征在于,所述聚二甲基硅氧烷和所述固化剂的质量比为8:1—10:1;及/或,所述固化剂为聚二甲基硅氧 烷固化剂。
- 如权利要求1所述的柔性电极的制备方法,其特征在于,所述加热固化的步骤包括:在70-95℃下加热15-60分钟。
- 如权利要求1所述的柔性电极的制备方法,其特征在于,所述碳纳米管为多壁碳纳米管。
- 一种由权利要求1-13任一项所述的柔性电极的制备方法制备得到的柔性电极。
- 一种柔性电子设备,其特征在于,包括权利要求13所述的柔性电极。
- 如权利要求15所述的柔性电子设备,其特征在于,所述柔性电子设备为可穿戴式电子设备。
- 如权利要求16所述的柔性电子设备,其特征在于,所述柔性电子设备为柔性显示屏或植入式医疗器械。
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