CN112927950A - Preparation method and application of biaxial tension flexible energy storage device - Google Patents
Preparation method and application of biaxial tension flexible energy storage device Download PDFInfo
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- CN112927950A CN112927950A CN202110097073.7A CN202110097073A CN112927950A CN 112927950 A CN112927950 A CN 112927950A CN 202110097073 A CN202110097073 A CN 202110097073A CN 112927950 A CN112927950 A CN 112927950A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
Abstract
The invention discloses a preparation method and application of a bidirectional stretching flexible energy storage device, wherein the preparation method comprises the following steps: designing a bidirectional stretching structure; preparing a flexible energy storage electrode, specifically comprising michael preparation, polypyrrole-coated bacterial cellulose preparation and electrode preparation; according to the assembly of the bidirectional stretching flexible energy storage device, the obtained interdigital electrodes are fixed on a polyimide-based bidirectional stretching substrate through double faced adhesive tapes, then the electrodes are connected with an integrated circuit through silver paste, free series-parallel connection is achieved according to actual use requirements, and corresponding solid gel electrolyte is dripped on the electrodes, so that the bidirectional stretching flexible energy storage device can be obtained. The invention can be reasonably reconstructed according to the requirements of actual devices, and can ensure excellent electrochemical performance, long-time circulation stability and reversible stretchability of the devices based on the reasonable design of the island bridge structure.
Description
Technical Field
The invention relates to the field of flexible energy storage devices, in particular to a preparation method and application of a bidirectional stretching flexible energy storage device.
Background
In recent years, with the rapid development of flexible and stretchable electronic devices and the configuration and use of intelligent applications, people's lives become more varied. Therefore, the micro power supply which can be compatible with bending deformation and can bear corresponding tensile deformation is urgently needed at present to perfect and strengthen the adaptability and operability of the whole intelligent system, so that the micro power supply can adapt to various environments and use situations while taking energy storage performance into consideration.
The design of two-way tensile structure combines flexible printed circuit preparation means to realize, through the design of two-way tensile structure, can carry out reasonable one-way and two-way deformation to portable little power according to the demand, carries out controllable deformation according to the concrete demand of use, realizes the flexibility and the deformation of little power, has improved the experience sense and the comfort of the person of wearing, is one of the necessary condition of flexible wearable equipment. And through the introduction of the flexible printed circuit technology, the integrated circuit can be stably deformed (stretched, bent and rotated), free series-parallel connection of single modules is realized through reasonable design of the circuit, and reasonable configuration of voltage or capacity can be carried out according to the requirements of equipment.
The micro super capacitor has the advantages of high charging speed, high power density and good cycle stability, particularly has extremely high safety due to the configuration of water-based electrode liquid, can realize in-plane integration with a wearable intelligent system, and is considered as one of the first technologies of the micro power source of the next-generation flexible wearable device. At present, the field of flexible energy storage devices is still in a development stage and faces the problems of low energy density, insufficient working voltage, poor stretching capacity, low cycling stability, poor integration capability with electrical appliances and the like. From the perspective of stretchable energy storage devices, existing stretchable structures typically employ a wave/corrugated electrode structure, in which two active thin film electrodes are stacked on a solid electrolyte that is conformal to each other, and attached to a pre-strained elastic substrate, and the extension of the wave/corrugated electrode when stretched can counteract the tensile stress, thereby achieving stretchability. Such an electrode structure has an inherent drawback: the electrochemical performance is rapidly degraded due to inevitable differences in physical and chemical properties between the active electrode and the elastic substrate, resulting in their poor interfacial adhesion under repeated deformation, strain mismatch and substrate delamination, and furthermore, the split-level electrode layout is not conducive to the integration of other microelectronic devices in planar circuits.
Disclosure of Invention
The invention aims to provide a preparation method and application of a biaxial stretching flexible energy storage device, which can be reasonably reconstructed according to the requirements of actual devices, and can ensure excellent electrochemical performance, long-term cycling stability and reversible stretchability of the device based on the reasonable design of an island bridge structure.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of a bidirectional stretching flexible energy storage device comprises the following steps:
(1) design of biaxial stretching structure
The biaxial stretching structure is designed by Auto CAD software, the island bridge structure and the snake-shaped interconnection structure are used as basic structures to form the biaxial stretching structure, the biaxial stretching structure is finally obtained by a flexible circuit printing manufacturing process, the design value of the biaxial stretching structure is 3.5-4.5cm, the uniaxial stretching rate is 57.1-100%, the biaxial stretching rate is 104-300%, and finally the biaxial stretching structure is converted into a PCB file to manufacture a mature commercial polyimide flexible circuit according to the designed CAD drawing;
(2) preparation of flexible energy storage electrode
Preparation of michael: dissolving 0.5-1.5g of lithium fluoride in 5-30mL of hydrochloric acid to form an etching solution, then adding 0.1-0.3g of aluminum titanium carbonate, reacting at 30-50 ℃ for 12-60 hours, washing the obtained centrifugal product with deionized water, putting 0.05-0.2g of centrifugal product Ti3C2Tx powder into 30-80mL of deionized water, and then carrying out ultrasonic treatment on the mixture in an ice bath for 0.5-2 hours to obtain a michaene nanosheet, namely an MXene nanosheet;
preparing polypyrrole-coated bacterial cellulose: adding 1-3mL of pyrrole monomer into 3-9mL of absolute ethyl alcohol, adding the mixture into 30-80mL of bacterial cellulose solution with the concentration of 1.5 mg/mL < -1 > under the condition of stirring in an ice-water bath, slowly adding 30-100mL of hydrochloric acid solution containing 0.5-1g of ferric chloride hexahydrate into the mixed solution, reacting for 10 hours, and filtering the mixed reaction solution in vacuum to obtain 1D conductive polypyrrole-coated bacterial cellulose fibers with a core-shell structure, namely one-dimensional conductive BC @ PPy fibers;
preparing an electrode: taking a colloidal solution of an MXene nanosheet and the obtained one-dimensional conductive BC @ PPy fiber suspension, wherein the volume of the one-dimensional conductive BC @ PPy fiber suspension is 10-50mL, obtaining an MXene/BC @ PPy mixed film on a cellulose ester film by following a vacuum filtration step, wherein the weight content of 1D conductive BC @ PPy fibers inserted into a sheet layer is different from 0-51.6%, drying for 2 hours, separating from a filter membrane to finally obtain the MXene/BC @ PPy mixed film, and finally, manufacturing an interdigital electrode with a designed size based on the MXene/PPy @ BC mixed film by using a laser cutting machine;
(3) assembly of biaxially oriented flexible energy storage device
The obtained interdigital electrode is fixed on a polyimide-based bidirectional stretching substrate through double-sided adhesive tape, then the electrode is connected with an integrated circuit through silver paste, free series-parallel connection is achieved according to actual use requirements, and corresponding solid gel electrolyte is dripped on the electrode, so that the bidirectional stretching flexible energy storage device can be obtained.
Preferably, in the step (1), the serpentine interconnection structure in the island bridge structure is designed according to different stretching requirements.
Preferably, in the step (1), the design value of the stretching structure is 4.5cm, the uniaxial stretching rate is 100%, and the biaxial stretching rate is 300%.
Preferably, in the step (2), the MXene nanosheets obtained by the ice bath are stored in a refrigerated manner before being used.
Preferably, in the step (2), the synthesized one-dimensional conductive BC @ PPy fiber with the core-shell structure needs to be re-dispersed in deionized water to wait for further electrode synthesis.
Preferably, in the step (2), the thickness of the prepared interdigital electrode is 10-60 um.
Preferably, the preparation method is applied to the bidirectional stretching flexible energy storage device, and the bidirectional stretching flexible energy storage device is used for in-plane device integration.
Compared with the prior art, the invention has the beneficial effects that:
1) the bidirectional stretching structure designed by the invention can be reasonably reconstructed according to the requirements of actual devices, and the reasonable design based on the island bridge structure can ensure the excellent electrochemical performance, long-term circulation stability and reversible stretchability of the devices;
2) the invention introduces the electrode film of 'electron/ion double transmission channels', provides higher working voltage and energy density, and is beneficial to improving the applicability and stability of the stretchable energy storage device;
3) the invention adopts an accurate and feasible manufacturing method of the flexible printed circuit, so that the integrated circuit can be stably deformed (stretched, bent and rotated), free series-parallel connection of single modules is realized through reasonable design of the circuit, and reasonable configuration of voltage or capacity can be carried out according to the requirements of equipment.
Drawings
Fig. 1 is a PCB engineering design drawing of a biaxial stretching structure in embodiment 1 of the present invention;
fig. 2 is a schematic structural diagram of a biaxially oriented flexible energy storage device in example 1 of the present invention, wherein 1, solid gel electrolyte, 2, interdigital electrodes, 3, polyimide-based biaxially oriented substrate, 4, and double-sided adhesive tape;
FIG. 3 is a graph showing the cycle stability and charge/discharge curves of a single device in example 1 of the present invention;
FIG. 4 is an impedance curve of a single device and a bidirectional tensile flexible energy storage device in example 1 of the invention;
FIG. 5 is a current-voltage characteristic curve of a single device and a bidirectional tensile flexible energy storage device in example 1 of the invention;
fig. 6 is a photograph showing the uniaxial tension and the biaxial tension of the biaxial tension flexible energy storage device in application example 1 of the invention;
fig. 7 is a photograph showing the uniaxial tension and the biaxial tension of the biaxial tension flexible energy storage device in application example 1 of the invention in example 2;
fig. 8 is a photograph showing the uniaxial tension and the biaxial tension of the biaxial tension flexible energy storage device in application example 1 of the invention 3;
fig. 9 is a dimensional diagram of three examples of a biaxially oriented flexible energy storage device in application example 1 of the present invention;
fig. 10 is a display picture of the biaxially oriented flexible energy storage device of application example 2 in combination with a watch.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in 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 protection scope of the present invention.
Example 1
A preparation method of a bidirectional stretching flexible energy storage device comprises the following steps:
(1) design of biaxial stretching structure
The bidirectional stretching structure is designed through Auto CAD software, the island bridge structure and the snake-shaped interconnection structure are used as basic structures to form the bidirectional stretching structure, the bidirectional stretching structure is finally obtained through a flexible circuit printing manufacturing process, and the circuit and the flexible stretchable substrate can be combined through the adoption of a flexible circuit printing technology, so that the integration of an electrode circuit can be realized. Through the change to snakelike interconnect structure parameter, can adapt to the demand of actual tensile strain, tensile structure design numerical value is 3.5, and the unidirectional stretching rate 100%, the bidirectional stretching rate 300%, according to the CAD drawing of designing at last, convert into the PCB file and carry out ripe commercial polyimide flexible circuit preparation, PCB engineering design drawing is as shown in FIG. 1.
(2) Preparation of flexible energy storage electrode
MXene (Michelene) preparation: 1g of lithium fluoride was dissolved in 15mL of hydrochloric acid to form an etching solution, and then 0.2g of titanium aluminum carbonate was added. After 48 hours of reaction at 40 ℃, the resulting centrifuged product was washed with deionized water (DI), and 0.15g of centrifuged product Ti3C2Tx (titanium carbide) powder was put into 50mL of deionized water. And then, treating the mixture in an ice bath by ultrasonic waves for 1 hour to obtain MXene nanosheets, wherein the MXene nanosheets obtained in the ice bath need to be refrigerated and stored before being used.
Preparation of BC @ PPy (polypyrrole coated bacterial cellulose): 2mL of pyrrole monomer was added to 6mL of absolute ethanol, and the mixture was added to 50mL of a 1.5 mg/mL-1 BC solution (bacterial cellulose solution) with stirring in an ice-water bath. Then, 50mL of a hydrochloric acid solution containing 0.75g of ferric chloride hexahydrate was slowly added to the above mixed solution. After 10 hours of reaction, the reaction solution was mixed by vacuum filtration to obtain a 1D (one-dimensional) conductive BC @ PPy fiber with a core-shell structure, and the synthesized one-dimensional conductive BC @ PPy fiber with a core-shell structure was re-dispersed in deionized water to wait for further electrode synthesis.
Preparing an electrode: taking a colloidal solution of MXene nanosheets and the obtained one-dimensional conductive BC @ PPy fiber suspension, the volume of the one-dimensional conductive BC @ PPy fiber suspension was 50mL to prepare a mixed suspension. Following the vacuum filtration step, an MXene/BC @ PPy mixed film was obtained on the cellulose ester film with a weight content of 51.6% of the 1D conductive BC @ PPy fibers inserted into the sheet layer. After drying for 2 hours, MXene/BC @ PPy mixed film was finally obtained by simple separation from the filter. Finally, by using a laser cutting machine, the interdigital electrode 2 with designed size based on the MXene/PPy @ BC mixed film can be manufactured.
(3) Assembly of biaxially oriented flexible energy storage device
Fixing the obtained interdigital electrode 2 on a polyimide-based biaxial tension substrate 3 through a double-sided adhesive tape 4; and the electrodes are connected with the integrated circuit through silver paste, free series-parallel connection can be realized according to actual use requirements, and corresponding solid gel electrolyte 1 is dripped on the electrodes to obtain the flexible energy storage device with bidirectional stretching.
As can be seen from fig. 3, 4 and 5, based on the excellent electrochemical performance of a single device and based on the design of the bidirectional stretching flexible energy storage device, the serial test conforms to the law, has good electrochemical performance, and can be applied to actual production and life.
Application example 1
An integration of a biaxial stretching flexible energy storage device is shown in figures 6, 7 and 8, the preparation of a single device is the same as that of the embodiment 1, and the size is shown in figure 9; the difference lies in that different island bridge structure designs are carried out according to different environmental requirements, and different stretching ratios are obtained.
The step (1) is the same as the preparation method of the embodiment 1, and a bidirectional stretchable structure is designed; the difference is that the designed stretch length differs according to specific requirements.
Step (2) was performed in the same manner as in example 1 to prepare a plurality of energy storage electrodes.
And (3) placing the four pairs of energy storage electrodes on a substrate with a flexible circuit at the bottom, connecting the energy storage electrodes in series and in parallel freely by using silver paste according to the requirement, and finally dropwise adding solid electrolyte to successfully prepare and package the bidirectional stretching flexible energy storage device.
The integration of the bidirectional stretching flexible energy storage device can be connected in series and parallel at will according to actual needs, thereby realizing the multiplication of voltage and current and meeting the actual needs.
Application example 2
Integration of a flat biaxial tension flexible energy storage device with an electronic device, see fig. 10, preparation of a single flexible electrode is the same as in example 1; the multiple electrode integration is the same as application example 2; the difference is that the flexible device is integrated with other electronic devices.
The step (1) is the same as the preparation method of the embodiment 1, and a bidirectional stretchable structure is designed; the difference is that the designed stretch length differs according to specific requirements.
Step (2) was performed in the same manner as in example 1 to prepare a plurality of energy storage electrodes.
And (3) placing the four pairs of energy storage electrodes on a substrate with a flexible circuit at the bottom, connecting the energy storage electrodes and a chronometer in series by using silver paste, and finally, dropwise adding solid electrolyte to successfully prepare and package the bidirectional stretching flexible energy storage device, so that one chronometer can be driven.
The integration of the bidirectional stretching flexible energy storage device prepared by the method and the dial can be successfully driven and normally timed.
The foregoing is merely exemplary and illustrative of the present invention and various modifications, additions and substitutions may be made by those skilled in the art to the specific embodiments described without departing from the scope of the present invention as defined in the accompanying claims.
Claims (7)
1. A preparation method of a bidirectional stretching flexible energy storage device is characterized by comprising the following steps:
(1) design of biaxial stretching structure
The biaxial stretching structure is designed by Auto CAD software, the island bridge structure and the snake-shaped interconnection structure are used as basic structures to form the biaxial stretching structure, the biaxial stretching structure is finally obtained by a flexible circuit printing manufacturing process, the design value of the biaxial stretching structure is 3.5-4.5cm, the uniaxial stretching rate is 57.1-100%, the biaxial stretching rate is 104-300%, and finally the biaxial stretching structure is converted into a PCB file to manufacture a mature commercial polyimide flexible circuit according to the designed CAD drawing;
(2) preparation of flexible energy storage electrode
Preparation of michael: dissolving 0.5-1.5g of lithium fluoride in 5-30mL of hydrochloric acid to form an etching solution, then adding 0.1-0.3g of aluminum titanium carbonate, reacting at 30-50 ℃ for 12-60 hours, washing the obtained centrifugal product with deionized water, putting 0.05-0.2g of centrifugal product Ti3C2Tx powder into 30-80mL of deionized water, and then carrying out ultrasonic treatment on the mixture in an ice bath for 0.5-2 hours to obtain a michaene nanosheet, namely an MXene nanosheet;
preparing polypyrrole-coated bacterial cellulose: adding 1-3mL pyrrole monomer into 3-9mL absolute ethyl alcohol, adding the mixture into 30-80mL with the concentration of 1.5 mg/mL under the condition of stirring in ice-water bath-1Then slowly adding 30-100mL hydrochloric acid solution containing 0.5-1g ferric chloride hexahydrate into the mixed solution, reacting for 10 hours, and filtering the mixed reaction solution in vacuum to obtain 1D conductive polypyrrole-coated bacterial cellulose fibers with a core-shell structure, namely one-dimensional conductive BC @ PPy fibers;
preparing an electrode: taking a colloidal solution of an MXene nanosheet and the obtained one-dimensional conductive BC @ PPy fiber suspension, wherein the volume of the one-dimensional conductive BC @ PPy fiber suspension is 10-50mL, obtaining an MXene/BC @ PPy mixed film on a cellulose ester film by following a vacuum filtration step, wherein the weight content of 1D conductive BC @ PPy fibers inserted into a sheet layer is different from 0-51.6%, drying for 2 hours, separating from a filter membrane to finally obtain the MXene/BC @ PPy mixed film, and finally, manufacturing an interdigital electrode with a designed size based on the MXene/PPy @ BC mixed film by using a laser cutting machine;
(3) assembly of biaxially oriented flexible energy storage device
The obtained interdigital electrode is fixed on a polyimide-based bidirectional stretching substrate through double-sided adhesive tape, then the electrode is connected with an integrated circuit through silver paste, free series-parallel connection is achieved according to actual use requirements, and corresponding solid gel electrolyte is dripped on the electrode, so that the bidirectional stretching flexible energy storage device can be obtained.
2. The method for preparing the biaxially oriented flexible energy storage device according to claim 1, wherein the method comprises the following steps: in the step (1), the serpentine interconnection structure in the island bridge structure is designed according to different stretching requirements.
3. The method for preparing the biaxially oriented flexible energy storage device according to claim 1, wherein the method comprises the following steps: in the step (1), the design value of the stretching structure is 4.5cm, the unidirectional stretching rate is 100%, and the bidirectional stretching rate is 300%.
4. The method for preparing the biaxially oriented flexible energy storage device according to claim 1, wherein the method comprises the following steps: in the step (2), the MXene nanosheets obtained by ice bath need to be refrigerated and stored before being used.
5. The method for preparing the biaxially oriented flexible energy storage device according to claim 1, wherein the method comprises the following steps: in the step (2), the synthesized one-dimensional conductive BC @ PPy fiber with the core-shell structure needs to be re-dispersed in deionized water to wait for further electrode synthesis.
6. The method for preparing the biaxially oriented flexible energy storage device according to claim 1, wherein the method comprises the following steps: in the step (2), the thickness of the prepared interdigital electrode is 10-60 um.
7. Use of a biaxially oriented flexible energy storage device prepared by the process according to any one of claims 1 to 6, wherein: the bidirectional stretching flexible energy storage device is used for in-plane device integration.
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Cited By (2)
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| CN114645450A (en) * | 2022-04-28 | 2022-06-21 | 广东精英纺织服饰科技有限公司 | Dyeing and finishing process of energy-saving environment-friendly flame-retardant fabric |
| CN114645450B (en) * | 2022-04-28 | 2024-05-14 | 汕头市鼎泰丰实业有限公司 | Dyeing and finishing process of energy-saving environment-friendly flame-retardant fabric |
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Application publication date: 20210608 |