KR20170093401A - Washable and flexible textile fiber electrode and manufacturing method thereof - Google Patents
Washable and flexible textile fiber electrode and manufacturing method thereof Download PDFInfo
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- KR20170093401A KR20170093401A KR1020160014752A KR20160014752A KR20170093401A KR 20170093401 A KR20170093401 A KR 20170093401A KR 1020160014752 A KR1020160014752 A KR 1020160014752A KR 20160014752 A KR20160014752 A KR 20160014752A KR 20170093401 A KR20170093401 A KR 20170093401A
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- Prior art keywords
- fibers
- glue
- present
- fine particles
- fiber electrode
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- 239000010419 fine particle Substances 0.000 claims abstract description 47
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Images
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/40—Fibres
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
- H01G11/66—Current collectors
- H01G11/68—Current collectors characterised by their material
-
- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2505/00—Industrial
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The present invention relates to a flexible fiber electrode coated with a conductive layer containing polar carbon fine particles and glue on the surface of a two-dimensional organic fiber structure, and a super capacitor including the same.
Description
The present invention relates to a washable flexible fiber electrode and a method of manufacturing the same.
Wearable devices, which have been developed since the 1990s, have developed in the 2000s with full-fledged form, and the development speed is expected to accelerate with the high value-added trend in the IT field.
Currently, wearable devices refer to accessories that can be attached to the body, such as accessory smart watches or Google glasses. However, as the development of the technology progresses, it is expected that the wearable device will be developed as a clothing-type wearable device, that is, smart clothing integrated with clothes in an accessory type. It can easily give flexibility, can be easily processed and can be miniaturized, and it is possible to reduce the inconvenience to wear separately like an accessory type by giving a smart function to garments that are constantly worn by a person, Functions can be easily used and manifested.
In order to implement such a wearable smart device, a fiber type conductive fiber capable of serving as an electrode is required. Such conductive fibers must satisfy various requirements such as mechanical properties such as friction strength, bending strength, body suitability, and electronic properties as well as washing properties for use in a garment form.
Conductive fibers, which are currently being introduced, are mainly metal fibers and have excellent electrical conductivity. However, they are difficult to exhibit the inherent flexibility of fibers, and they are disadvantageous in terms of weight, which may cause problems in physical synthesis. In addition, even in the case of fibers coated with conductive polymers or metal fine particles, the electrical conductivity is lowered and the washing fastness is low, so that they are used only for limited use such as antistatic protection.
To improve this, Korean Patent Laid-Open Publication No. 10-2015-0041400 discloses a technique of incorporating a carbon nanomaterial having a higher-order structure by multiple hydrogen bonds into a polymer and melting or spinning it. However, in this case, there is a disadvantage that the process is complicated because it is necessary to induce the carbon nanomaterial or other conductive substance contained in the polymer to the fiber surface.
Similarly, there is a technique of mixing a conductive material and a carbon nanomaterial into a spinning solution, spinning the solution, and inducing a conductive material and a carbon nanomaterial to the surface of the fiber using the interaction between solvents used in the solidification process , Since it is necessary to use a specific solvent at the time of solidification, it is inevitably limited to solution spinning, and there is a disadvantage that it loads the environment due to the use of various solvents. It is also disadvantageous that it can not be introduced when the fiber material is a natural fiber rather than a polymer.
Although various attempts have been made to develop a fiber type electrode for manufacturing such a wearable device, development of a conductive fiber having all the required properties including both natural fibers and synthetic fibers is still a problem.
Disclosure of Invention Technical Problem [8] Accordingly, the present invention has been made keeping in mind the above problems occurring in the prior art, and it is an object of the present invention to provide a flexible fiber electrode capable of imparting conductivity regardless of natural fibers, synthetic fibers, and semi-synthetic fibers, And a method for producing the same.
One aspect of the present invention relates to a flexible fiber electrode coated with a conductive layer containing polar carbon fine particles and glue on the surface of a two-dimensional organic fiber structure.
Another aspect of the present invention relates to a method for producing a flexible fiber electrode comprising coating a two-dimensional organic fiber structure with a coating liquid containing polar carbon fine particles, glue, and a solvent and drying the same.
Another aspect of the present invention relates to a flexible supercapacitor including the flexible fiber electrode and the metal current collector formed on one surface of the flexible fiber electrode.
The flexible fiber electrode according to the present invention can impart both electrical conductivity to the two-dimensional organic fiber structure irrespective of the natural fiber, the synthetic fiber and the semisynthetic fiber by coating the conductive layer containing the polar carbon fine particles and the glue on the surface thereof , It is possible to have electrical conductivity through the coating layer formed on the surface while making use of flexibility that is the main characteristic of the fiber. Further, by adding glue, it is possible to improve the washing fastness of the coating layer while being human-friendly, and thus the durability of the coating layer having electric conductivity can be improved.
The fiber electrode according to the present invention can be widely applied to a flexible device requiring flexibility as well as a sensor, an energy generation and storage device that can detect various changes in the body by applying to the clothing through the above-described characteristics.
1 shows a method of manufacturing a flexible fiber electrode according to an embodiment of the present invention.
Fig. 2 is a scanning electron microscope (SEM) image of the conductive layer formed on the flexible fiber electrode prepared in Example 1. Fig.
3 and 4 are X-ray photoelectron spectroscopy spectra of a flexible fiber electrode manufactured according to Example 1 of the present invention.
FIG. 5 is a graph showing changes in sheet resistance according to the number of times of washing of the fiber electrode manufactured according to Example 1. FIG.
FIG. 6 (a) is a graph showing the concentration of the coating liquid and the coating layer formation amount used in Examples 1 to 7, (b) showing the cyclic voltage-current curves of Examples 1 to 7, and (c) To 7, and d represents the charging / discharging stability of Examples 1 to 7.
FIG. 7A shows the cyclic voltage-current curve of Example 8, c shows the area capacity according to the scanning speed, d shows the constant current charge / discharge curve with time, The impedance spectroscopy curve, and f is the charge / discharge stability measurement.
Hereinafter, the flexible fiber electrode according to the present invention and its manufacturing method will be described in more detail with reference to the drawings and specific examples. It should be understood, however, that the drawings or specific examples are only for the purpose of describing the present invention in detail, and the present invention is not limited thereto.
Unless otherwise defined, all technical and scientific terms have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
In addition, the following drawings are provided by way of example so that those skilled in the art can fully understand the spirit of the present invention. Therefore, the present invention is not limited to the following drawings, but may be embodied in other forms, and the drawings presented below may be exaggerated in order to clarify the spirit of the present invention. Also, throughout the specification, like reference numerals designate like elements.
Also, the singular forms as used in the specification and the appended claims are intended to include the plural forms as well, unless the context clearly indicates otherwise.
In describing the components of the present invention, terms such as first, second, A, B, (a), and (b) may be used. These terms are intended to distinguish the constituent elements from other constituent elements, and the terms do not limit the nature, order or order of the constituent elements. When a component is described as being "connected", "coupled", or "connected" to another component, the component may be directly connected to or connected to the other component, It should be understood that an element may be "connected," "coupled," or "connected."
The term " fiber " used in the present invention includes a staple, a filament, and a combination thereof, each of which is a linear, long and bendable material regardless of the material.
The term 'fibrous structure' used in the present invention is a material having a two-dimensional shape produced by processing the fiber, and examples of the fibrous structure include a fabric, a knitted fabric, and a nonwoven fabric.
As used herein, the term " pores " refers to pores, depressions, or tunnel shapes formed on the surface of one strand of the fiber and may be present or connected independently of each other.
The term "surface" used in the present invention refers to the outer surface of a fiber constituting the fibrous structure, and may include the inner surface of the pore when the fiber has pores.
DISCLOSURE OF THE INVENTION It is an object of the present invention to provide a method for manufacturing a wearable device, in which a fiber electrode used in a wearable device has poor mechanical properties, electronic characteristics, Layer, it has been found that the washing fastness can be dramatically increased and at the same time excellent electrical and electronic characteristics can be exhibited. The process is simple and the electric conductivity can be imparted regardless of the material and the manufacturing method of the fiber base material such as the natural fiber and the artificial fiber.
That is, the flexible fiber electrode according to the present invention may be one in which a conductive layer containing polar carbon fine particles and glue is coated on the surface of the two-dimensional organic fiber structure.
In the present invention, the organic fiber structure can be used without limitation as long as it can form a fibrous structure such as a fabric, a knitted fabric, a felt, and a nonwoven fabric. Examples of the organic fiber structure include natural fibers such as cotton fibers, hemp fibers, silk fibers and fibrillated fibers, semisynthetic fibers such as rayon fibers, polyolefin fibers such as polyethylene fibers and polypropylene fibers, polyamide fibers, polyacrylic fibers, And polyurethane fibers, and it is preferable to use a cotton fiber, a polyamide fiber, a polyurethane fiber, or the like.
In the present invention, the organic fiber structure may have a porous structure. In this case, the porous structure means pores, and the pores may mean pores formed on the surface of the fiber strands of the organic fiber structure. As a result, the polar carbon fine particles contained in the conductive layer naturally permeate into the pores and are fixed, so that the polar carbon fine particles can be prevented from being desorbed. At the same time, as the surface area of the electrode increases and the area of the electrochemical reaction increases, And as a result, the efficiency of the fiber electrode can be increased.
In the present invention, the organic fiber structure may have a porosity of 10 to 95% by volume. If the porosity is less than 10% by volume, the efficiency of the fiber electrode may be reduced due to insufficient penetration of the polar carbon particles into the organic fibers. If the porosity is more than 95% by volume, the organic fiber structure or the fiber electrode The mechanical properties of the polymer can be greatly reduced.
In the present invention, the organic fiber may include a functional group capable of hydrogen bonding. This is to further increase the bonding force between the conductive layer and the organic fibers by mutual hydrogen bonding with the polar carbon fine particles contained in the conductive layer and the other functional groups contained in the glue.
In the present invention, the functional group includes those having strong electronegativity, such as nitrogen (N) and oxygen (O), to induce hydrogen bonding between adjacent functional groups. The functional group according to the present invention includes the polar carbon Fine particles, an organic fiber structure, and any one or more selected from a carboxyl group, a carbonyl group, a hydroxyl group, a urethane group, an amide group, an amine group and a urea group, . ≪ / RTI >
In the present invention, the functional group may be contained in the fiber molecule itself depending on the material of the organic fiber structure, and may be introduced through surface treatment, post-processing, graft polymerization or the like. In the case of the former, natural fibers such as cotton fiber, hemp fiber, wool fiber, and silk fiber, semisynthetic fiber or polyurethane, etc. In addition, surface modification by weight reduction, refining, electron beam, copolymerization with the monomer having the functional group, Functional groups can be introduced through graft polymerization or the like.
In the present invention, the conductive layer may include polar carbon fine particles and glue.
In the present invention, the polar carbon fine particles may be a two-dimensional or three-dimensional carbon material having various functional groups on its surface and capable of hydrogen bonding with a functional group such as a carboxyl group, a carbonyl group, a hydroxyl group, a urethane group, an amide group, It means a three-dimensional carbon structure.
In the present invention, the polar carbon fine particles may be subjected to various methods commonly used in the art for introducing functional groups onto the surface of a general carbon structure. Examples include thermal oxidation, chemical oxidation, oxygen plasma treatment, and ozone treatment. In addition, one or more derivatives may be reacted to introduce a functional group.
In the present invention, the functional groups that can be introduced into the polar carbon fine particles include, but are not limited to, a carboxyl group, a carbonyl group, a hydroxyl group, a urethane group, an amide group, an amine group and a urea group. It may be different.
In the present invention, the carbon structure may be a single-walled carbon structure such as graphene, carbon nanotube, or fullerene; Or a multilayer structure such as graphite, carbon black, acetylene black, ketjen black, denka black, thermal black, channel black, furnace black, lamp black, summer black and super-P such as graphite, soft graphite, graphite and artificial graphite Or a mixture thereof.
In the present invention, the polar carbon fine particles may have an average particle diameter of 5 to 1,000 nm, preferably 10 to 500 nm, and most preferably 10 to 50 nm. In this range, it is possible to effectively penetrate and adhere to the pores formed in the organic fiber structure. In addition, as described later, it is preferable that the polar carbon fine particles are easily dispersed during the production of the coating liquid.
In the present invention, the polar carbon fine particles may have a zeta potential of -10 to -70 mV. The zeta potential represents the surface potential of the polar carbon microparticles and is a factor that can determine the degree of bonding between the polar carbon fine particles and the glue and the organic fiber structure, dispersion in the coating liquid, coagulation, stability, and control of the function.
In the present invention, when the zeta potential of the carbon microparticles is more than -10 mV, the interfacial bonding strength between the polar carbon fine particles and the glue and the organic fiber structure is decreased, resulting in poor washing fastness of the conductive layer. The formation of the conductive layer may become difficult.
In the present invention, the polar carbon fine particles may have a total content of heteroatoms such as oxygen and nitrogen in the total element composition of 10 to 35 atomic%, more preferably 20 to 30 atomic%. When the above-mentioned range is satisfied, a functional group is formed on the surface of the carbon fine particles to form a hydrogen bond with the glue and the organic fiber structure, and as a result, the fastness of the conductive layer can be increased.
In the present invention, the polar carbon fine particles may preferably be brown or soft. Songbang means soot generated when burning pine trees. Flexible means soot generated when burning vegetable oil such as soybean oil, rapeseed oil, camellia oil, or animal oil. When soot is produced, Hydrogen, nitrogen, sulfur, oxygen and the like are contained in addition to carbon to form a functional group capable of hydrogen bonding. Through this, the affinity with the solvent during the preparation of the coating liquid becomes high, and the hydrogen bonding with the glue and the organic fiber structure can be effectively performed.
In more detail, when a coating liquid in a sol state is applied to an organic fiber structure having porosity and subjected to a semi-aqueous treatment, the coating liquid permeates through pores distributed in the organic fiber structure. Then, the solvent in the coating solution evaporates and the gelation of the coating solution progresses as the temperature decreases. At this time, a glue form in which the glue component encapsulates the polar carbon particles and solidifies, and the glue component cures while forming the crosslinks in the upper and lower sides. Since the cured glue component forms a hydrogen bond with the polar carbon fine particles and the organic fiber structure, the physical bonding and the chemical bonding are simultaneously performed, thereby preventing the polar carbon fine particles from being separated from the organic fiber structure.
In the present invention, glue is a kind of animal natural adhesive which has been used for many years as a preservative, a coating agent, and a fixing agent in various fields such as painting, woods, crafts and the like. It is mixed with polar carbon fine particles, . Also, since the polymer has a hydroxyl group rich in the molecule, hydrogen bonding with the polar carbon fine particles and the organic fiber structure can be achieved, thereby increasing washing fastness.
In the present invention, glue is not limited to any kind as long as it is used in the art as a coating agent, a fixing agent, and the like. Examples of the glue include a glue, a glue, a deer glue, a glue glue, a glue glue, a glue glue, Is preferable not only because it has strong adhesion to the organic fiber structure and the polar carbon fine particles at a low concentration but also because of its high flexibility.
In the present invention, glue may be an animal protein as a main component. Animal protein is the main protein that constitutes connective tissue of animal, and it may be widely distributed in animal dermis, bones, tendons and the like.
Examples of the animal protein in the present invention include collagen, gelatin, casein and polydodamine. The animal protein may further include proteins such as fibroin, elastin, keratin, albumin, globulin, and mucin.
In the present invention, the flexible fiber electrode has excellent adhesive strength between the organic fiber structure and the conductive layer, so that physical and electrochemical properties can be maintained even after washing.
As shown in FIG. 5, in the case of the organic fiber structure in which the conductive layer is not coated, the resistance reaches infinity due to no conductivity, whereas the flexible fiber electrode according to the present invention has a resistance of 0.5 Ω / , And it can be seen that the resistance value does not significantly increase even after washing 10 times.
Specifically, the flexible fiber electrode according to an example of the present invention may satisfy the following relational expression (1).
[Relation 1]
R A × 2 ≥ R B
(Where R A is the resistance value (Ω / □) of the flexible fiber electrode before washing, and R B is the resistance value (Ω / □) of the flexible fiber electrode after 10 washing cycles).
This has the advantage that the wearable device can be manufactured because the electrochemical properties are maintained even after washing because the adhesive strength is improved by coating the conductive layer using glue together with the polar carbon fine particles.
Hereinafter, the present invention will be described in more detail with reference to the production method.
The method for producing a flexible fiber electrode according to the present invention may include coating a two-dimensional organic fiber structure with a coating liquid containing polar carbon fine particles, glue and a solvent and drying the same.
In the present invention, the organic fiber structure, the polar carbon fine particles and the glue are the same as those described above, and a duplicate description will be omitted.
In the present invention, the solvent can be used without limitation, as long as it can effectively dissolve a solute having a functional group on its surface, such as glue and polar carbon fine particles.
Examples of the polar protic solvent include alcohols such as methanol, ethanol, propanol, butanol, etc., and organic solvents such as acetic acid and the like. The polar protic solvent may be, for example, water, polar protic solvent or mixed solvent thereof. And organic acids. However, the present invention is not limited thereto, and the present invention is not limited thereto, as long as it is a substance that can be mixed with the glue and the polar carbon fine particles to increase the dispersibility.
In the present invention, the coating liquid may contain 50 to 200 parts by weight of polar carbon fine particles and 0.1 to 10 parts by weight of glue per 100 parts by weight of solvent, more preferably 80 to 150 parts by weight of polar carbon fine particles per 100 parts by weight of solvent , And 1 to 5 parts by weight of glue.
In one example of the present invention, the coating solution is expanded to the maximum when the glue is first put into water and left for about one day. Next, the glue-containing dispersion is stirred at 50 to 80 ° C in a bath to prepare a glue solution. Next, when the glue solution is prepared, the glue solution is gradually poured into the polar carbon fine particles and mixed. A solvent, a glue solution or polar carbon fine particles may be further added while checking the viscosity of the coating liquid while mixing.
In the present invention, the optimum pH range of the coating solution is not limited, but if the acid or alkali is too acidic, the coating solution may be weakly acidic to weakly alkaline, more preferably neutral. That is, the pH is preferably 5 to 9, more preferably 6 to 7 at an appropriate pH.
When the coating solution is completed, the coating solution is coated on the organic fiber structure. In this case, the coating method is not limited to the present invention but may be carried out by immersing the organic fiber structure in the coating solution, leaving the coating solution in the spray device, and spraying the organic fiber structure onto the organic fiber structure. In addition, the coating step is not limited in the number of times, and can be repeated two or more times as necessary. At this time, although the upper limit of the number of times is not particularly limited, the upper limit may be set to 100 times or less in consideration of the efficiency of the process.
Next, the organic fiber structure coated with the coating liquid may be dried to produce a flexible fiber electrode that can be washed. The gelation of the glue component proceeds through the evaporation of the solvent and the physical and chemical bonding of the coating solution and the organic fiber structure can be achieved by the adhesion mode in which the glue component surrounds the polar carbon fine particles and solidifies. In addition, when washing is performed before drying, it is preferable to evaporate the solvent through the drying step since the amount of the coating layer may be increased.
The drying may be performed at a temperature of 20 to 90 DEG C in order to prevent evaporation of the solvent and deterioration of the glue component. It is more preferable to carry out the drying step at a temperature of 50 to 80 캜. The drying time is not particularly limited, but drying is preferably performed for a time sufficient for the solvent to evaporate, and it is preferable to proceed for about 30 minutes to about 2 hours for a specific example.
Still another aspect of the present invention relates to a flexible supercapacitor including a flexible fiber electrode and a metal current collector formed on one surface of the flexible fiber electrode.
Specifically, the metal current collector according to the present invention may be one formed on one side of the flexible fiber electrode, and the flexible supercapacitor may include a laminated structure in which a metal current collector is laminated on one side of the flexible fiber electrode.
In the present invention, the flexible fiber electrode is the same as that described above, and a duplicate description will be omitted.
The metal current collector according to the present invention can collect electrons generated by the electrochemical reaction in the flexible fiber electrode or supply electrons necessary for the electrochemical reaction.
The metal current collector according to the present invention is not particularly limited in its shape, but may be a metal particle, a metal fiber, a metal coated organic fiber, a mixed fiber mixed with metal, or a mixture thereof to secure excellent flexibility have. As a specific example, metal particles may be formed, or the metal particles may be melted or grown to form short fibers or long fibers. This can be freely selected depending on the type of the organic fiber structure and the use of the organic fiber electrode, and the present invention is not limited thereto. In the present invention, when the metal collector is in the form of fibers, the fineness of the metal fibers is not particularly limited.
In another embodiment of the conductive metal current collector, the metal may be formed into a short fiber or a long fiber, and then may be combined with an organic fiber such as general synthetic fiber or natural fiber to produce a single fiber having a large fineness. In this case, general synthetic fibers or natural fibers to be woven with the metal fibers may be ordinary fibers used in fabrics, knitted fabrics and nonwoven fabrics in the art, and they may be the same or different materials as the organic fiber structures.
In the case where the metal current collector is composed of the metal fibers and the organic fibers, the metal fibers may be introduced in an amount of 0.1 to 100 parts by weight based on 100 parts by weight of the organic fibers. However, the present invention is not limited thereto, Anticipated physical properties, and other reasons.
Further, in one example of the present invention, the flexible fiber electrode and the metal current collector may have a woven shape. That is, the organic fiber and the fiber-like metal current collector before the flexible fiber electrode is coated with the coating solution may be woven to form the mixed structure having the metal current collector and the organic fiber in the form of a single fabric. Thereafter, the mixed structure is coated with a coating liquid so that the organic fiber electrode and the metal current collector can be woven together to form a single structure. In this case, since the electrode and the current collector are woven together to form a single fabric, there is an advantage that a binder or the like for binding the electrode and the current collector to each other may not be used, and the electrode and the current collector are woven together closely It is possible to further improve the electrochemical performance.
In the present invention, the metal component contained in the metal current collector can be used without limitation as long as it is a component used as a current collector in the art. Examples of the metal component are selected from gold, platinum, silver, copper, aluminum, magnesium, molybdenum, tungsten, zinc, cobalt, cadmium, nickel, ruthenium, iron, lithium, tin, platinum, palladium, selenium, tantalum and lead , And preferably, gold, silver, platinum, copper, aluminum, or the like is used in view of electric conductivity.
According to the present invention, a flexible fiber electrode comprising a fibrous substrate containing polar carbon fine particles in the void and a conductive metal current collector in physical contact with the substrate is manufactured through the above-described method, The contact area with the polar carbon fine particles can be increased, and at the same time, the fiber electrode having excellent electrical characteristics can be manufactured by a simple method without limiting the material of the fibers having the polar carbon fine particles inside the voids. Also, by adding glue to the coating layer, it is possible to improve the washing fastness of the coating layer while improving the durability of the coating layer having electric conductivity.
The laminated structure according to the present invention may have various structures depending on the shape of the metal current collector. For example, when the metal current collector is in the form of metal particles, metal particles may be attached to the surface of the organic fiber structure.
Hereinafter, a flexible fiber electrode according to the present invention and a method for producing the same will be described in more detail with reference to Examples and Comparative Examples. However, the following examples and comparative examples are merely examples for explaining the present invention in more detail, and the present invention is not limited by the following examples and comparative examples.
The physical properties of the specimens prepared through Examples and Comparative Examples were measured as follows.
(Amount of carbon fine particles coated)
After the weight of the specimen was measured before coating, the weight of the specimen after coating and drying of the coating solution was measured and the difference between them was calculated.
(Washing fastness)
A specimen of 10 cm long and 10 cm long was placed in a washing bag and then placed in a washing machine (SEW-G120, Samsung Electronics). Separately, 10 grams of laundry detergent (Power Green Double Action, Oxygen) was separately supplied to the same specimen and washing machine, and they were washed 2, 4, 6, 8, and 10 times for 90 minutes each.
(Electrical property)
All measurements were made using an electrochemical analyzer (CHI 600E, CH Instrument) and pre-injected 5 times at a scanning rate of 5 mV / s before measurement.
① cyclic voltammetry (cyclic voltammetry)
CV data at a scanning rate of 5, 10, 25, 50, 100, 200, 500, and 1,000 mV / s were measured in a voltage range of 0 to 1 V, respectively.
② constant current charge-discharge (galvanostatic charge-discharge)
2, 5, 10, 15 and 20 mA in the voltage range of 0 to 1 V, respectively.
(3) Electrical impedance spectroscopy
Data were measured while changing the frequency of the 10 mV voltage from 10 mHz to 100 kHz.
(Material property)
The surface morphology of the specimens was measured using a scanning electron microscope (FE-SEM, JSM-700F, JEOL) and the chemical composition of the specimens was measured using an energy dispersive X-ray spectroscope (EDX, JSM-700F, JEOL).
The specimen components were measured under the conditions of spot size 0.5 μm using an optoelectronic spectrometer (XPS, Multilab 2000, Thermo) and the degree of crystallization of the specimen was measured using an X-ray diffractometer (Empyrean, PANalytical).
TEM images were taken using a high-resolution transmission electron microscope (JEM-ARM200F, JEOL). The electrical surface resistance was measured using a four-point probe auto-resistivity measuring system (DHY-ARS-200, Dasol Eng ).
(Example)
First, a hybrid fabric (Sanisilver ⓡ , Less EMF Inc.) composed of a silver layer and a cotton layer was prepared. (Conductive layer thickness: 0.28 Ω / sq or less, hybrid fabric thickness: 330 탆) Then, the hybrid fabric was cut into a rectangle having a size of 4 cm x 6 cm, immersed for 1 minute in an ink (Ganhyun, Buyoung Co.) with a coating solution, taken out, put on a sponge, and naturally dried. The dried hybrid fabric was immersed again in water and dried three times to prepare a specimen having a silver current collector on the organic fiber electrode.
Next, a paper filter separator was inserted between two specimens manufactured by the above method in a cell puncher having a diameter of 14 mm, and a 5M lithium chloride electrolyte was added thereto.
(Comparative Example 1)
The same procedure as in the previous example was carried out except that, in the formation of the coating layer, the carbon nanotubes instead of the inks were mixed in water at a ratio of 1.2 mg / ml and dispersed in an ultrasonic disperser for 30 minutes.
2 showing the formation of the conductive layer of the organic fiber electrode manufactured through the above example, it can be seen that the coating solution is naturally coated on both the silver current collector layer and the pure cotton layer. When the degree of coating of the carbon fine particles was confirmed, the coating amount of the carbon fine particles in Comparative Example 1, which had little polarity on the surface, was 5.5 mg /
As shown in Table 1 and FIG. 5, where the washing fastness was measured, it was found that even though the washing was repeated in both the silver blend layer and the cotton layer, the surface resistance hardly increased to 1? / Sq or less have. It can be seen that the separation of the coating layer hardly occurs even under repeated washing conditions and rough conditions including detergent.
(Examples 2 to 7)
An aqueous supercapacitor was prepared in the same manner as in Example 1, except that the concentration of the coating liquid was adjusted as shown in Table 2 below. The measured cyclic voltammetry curves (CV), areal capacitance according to the scanning speed and charge / discharge stability of each water-based supercapacitor were measured and shown in FIG. 6. (Example 1) The coating liquid concentration was set at 100% as a standard.)
As shown in FIG. 6 (b), when the conductive layer is not formed at all (0%), a CV curve similar to that of a general capacitor is shown. However, this is due to the redox reaction between the silver component and impurities contained in the current collector layer .
Also, as the conductive layer formation amount increases, the shape of the CV curve gradually changes to a rectangular shape, which means that the electrical properties gradually improve as the amount of conductive layer formation increases.
It can be seen from FIG. 6C that the area capacity according to the scanning speed is measured, the area capacity increases dramatically compared with the case where the conductive layer is not formed at the scanning speed of 5 mV / s (4.8 mF / cm 2) In particular, the area capacity of 52 mF / cm < 2 > This means that as the concentration of the conductive layer increases, the amount of polar nanoparticles increases together with the electrochemical properties of the organic fiber electrode.
6, where the charge / discharge stability was measured, the capacitor of Example 1 showed the highest stability when the charge and discharge cycles were repeated 10,000 times at 1,000 mV / s, and the concentration of the coating solution increased by 100% or more The more stable the stability is.
(Example 8)
1 g of polyvinyl alcohol (weight average molecular weight: 93,500, Sigma) was charged into a 5M lithium chloride electrolyte, which was then heated and stirred at a temperature of 90 DEG C for 30 minutes to prepare a gel-like electrolytic solution. Next, several drops of the electrolytic solution were dropped on the organic fiber electrode of the specimen prepared in Example 5, and left for about 1 hour, so that the electrolyte solution completely permeated the organic fiber electrode. Then, a paper filter separator was superimposed between the two electrodes to produce a symmetrical supercapacitor.
7B, which shows the CV curve according to the change of the scanning speed, it can be seen that the shape of the curve changes to a rectangle as the scanning speed increases, and the curve c of FIG. 7 It can be seen that the area capacity gradually decreases as the scanning speed increases.
7D, which shows a constant current charge / discharge curve with time, it can be seen that the shape of the graph is almost triangular as compared with the case where no conductive layer is formed (no ink). In addition, it can be confirmed that an electrical double layer is reliably formed.
7, which is an electrical impedance spectroscopy curve, shows a quasi-vertical Nyquist plot in the low frequency region. It can be seen that the supercapacitor according to the present invention has nearly ideal capacitance characteristics. In addition, the absence of a semicircular graph in the high frequency region indicates that the supercapacitor according to the present invention has excellent ion conductivity.
7, which shows the charge / discharge stability, it can be seen that the electric capacity is reduced by only 5% even when the charge / discharge cycle is repeated 30,000 times at a scanning speed of 1,000 mV / s. It can be seen that the super capacitor including the organic fiber electrode according to the present invention has excellent energy capacity and output capacity, and has excellent battery lifetime characteristics because chemical change hardly occurs despite repeated charge and discharge.
Claims (12)
Wherein the organic fiber structure comprises any one or two or more selected from cotton fibers, hemp fibers, silk fibers, flax fibers, rayon fibers, polyolefin fibers, polyamide fibers, polyacrylic fibers, polyester fibers and polyurethane fibers.
Wherein the organic fiber structure has a functional group capable of hydrogen bonding and a porosity of 10 to 95% by volume.
Wherein the polar carbon fine particles have a zeta potential in a range of -10 to -70 mV and include a flexible fiber electrode comprising at least one polar group selected from a carboxyl group, a carbonyl group, a hydroxyl group, a urethane group, an amide group, .
Wherein the glue comprises at least one protein component selected from collagen, gelatin, casein and polydodamine.
Wherein the flexible fiber electrode satisfies the following relational expression (1).
[Relation 1]
R A × 2 ≥ R B
(Where R A is the resistance value (Ω / □) of the flexible fiber electrode before washing, and R B is the resistance value (Ω / □) of the flexible fiber electrode after 10 washing cycles).
Wherein the solvent comprises water, a polar protic solvent or a mixed solvent thereof.
Wherein the coating liquid comprises 50 to 200 parts by weight of polar carbon fine particles and 0.1 to 10 parts by weight of glue per 100 parts by weight of solvent.
Wherein the drying is performed at a temperature of 20 to 90 캜.
Wherein the metal current collector comprises metal particles, metal fibers, organic fibers coated with a metal, mixed fibers obtained by mixing metals, or a mixture thereof.
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| CN108232027A (en) * | 2017-12-27 | 2018-06-29 | 青岛海信电器股份有限公司 | Patterned flex electrode and preparation method, flexible display apparatus |
| EP3482819A1 (en) * | 2017-11-13 | 2019-05-15 | Korea Advanced Institute Of Science And Technology | Apparatus for generating electrical energy based on hydrophilic fiber membrane and method of fabricating same |
| KR20200021219A (en) * | 2018-08-20 | 2020-02-28 | 한국과학기술원 | Hydroscopic material incorporated carbon layer coated hydrophilic fiber membrane based self-powered electrical energy generator and manufacturing method thereof |
| CN111121870A (en) * | 2019-12-25 | 2020-05-08 | 陕西科技大学 | Bionic multifunctional flexible sensor based on collagen aggregate and preparation method thereof |
| KR20230066892A (en) * | 2021-11-08 | 2023-05-16 | 한국과학기술원 | Energy generator added by asymmetrically coated two dimensional hygroscopic nanoclay and manufacturing method for the energy generator |
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| JP2009212131A (en) * | 2008-02-29 | 2009-09-17 | Nippon Zeon Co Ltd | Collector for hybrid capacitor and electrode sheet for hybrid capacitor using the same |
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| EP3482819A1 (en) * | 2017-11-13 | 2019-05-15 | Korea Advanced Institute Of Science And Technology | Apparatus for generating electrical energy based on hydrophilic fiber membrane and method of fabricating same |
| US11404222B2 (en) | 2017-11-13 | 2022-08-02 | Korea Advanced Institute Of Science And Technology | Apparatus for generating electrical energy based on hydrophilic fiber membrane and method of fabricating same |
| CN108232027A (en) * | 2017-12-27 | 2018-06-29 | 青岛海信电器股份有限公司 | Patterned flex electrode and preparation method, flexible display apparatus |
| CN108232027B (en) * | 2017-12-27 | 2020-03-06 | 青岛海信电器股份有限公司 | Graphical flexible electrode, preparation method and flexible display device |
| KR20200021219A (en) * | 2018-08-20 | 2020-02-28 | 한국과학기술원 | Hydroscopic material incorporated carbon layer coated hydrophilic fiber membrane based self-powered electrical energy generator and manufacturing method thereof |
| CN111121870A (en) * | 2019-12-25 | 2020-05-08 | 陕西科技大学 | Bionic multifunctional flexible sensor based on collagen aggregate and preparation method thereof |
| KR20230066892A (en) * | 2021-11-08 | 2023-05-16 | 한국과학기술원 | Energy generator added by asymmetrically coated two dimensional hygroscopic nanoclay and manufacturing method for the energy generator |
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| KR101827321B1 (en) | 2018-02-09 |
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