KR101812376B1 - Sealing Material, Flexible Thin-film type Super-Capacitor Device Manufacturing Method having the same and Super-Capacitor Device thereof - Google Patents
Sealing Material, Flexible Thin-film type Super-Capacitor Device Manufacturing Method having the same and Super-Capacitor Device thereof Download PDFInfo
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- KR101812376B1 KR101812376B1 KR1020140131302A KR20140131302A KR101812376B1 KR 101812376 B1 KR101812376 B1 KR 101812376B1 KR 1020140131302 A KR1020140131302 A KR 1020140131302A KR 20140131302 A KR20140131302 A KR 20140131302A KR 101812376 B1 KR101812376 B1 KR 101812376B1
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- 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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The present invention relates to a method of manufacturing a flexible thin film type supercapacitor element and a super capacitor element therefor, wherein the flexible thin film type supercapacitor element comprises: a flexible base film; A separation membrane interposed between the base films; An active material formed around the base film; And a thermally adhesive film sealable inside the base film so as to maintain airtightness by confining an electrolyte provided between the active materials, wherein the electrolyte comprises KOH with high corrosiveness, and the thermally adhesive film comprises a plastic paraffin film .
Thus, it is possible to easily and conveniently confine an electrolyte which is very thin, flexible, economical, mass-producible, and corrosive, while maintaining high electrical conductivity and high adhesion.
Description
The present invention relates to a sealing material, a method of manufacturing a flexible thin film type supercapacitor device and a supercapacitor device therefor, and more particularly, to a flexible film having a flexible film formed on a base film, A method of manufacturing a flexible thin film type supercapacitor device using the same, and a super capacitor device therefor.
Generally, like the electrodes of the capacitor, the electrodes such as the secondary battery and the electrochemical capacitor are largely composed of an active material for generating an electrochemical reaction and a current collector for transferring electrons generated from the active material to an external circuit. It is preferable that the current collector has a high electrical conductivity with a minimum resistance so that the flow of electrons supplied from the active material is not disturbed. In addition, since the electrons move through the interface between the active material and the active material, it is required to have a wide contact area as much as possible, and the contacted active material is not easily peeled off. Thus, mechanical and electrical characteristics are maintained even under repeated charging and discharging conditions for a long time It is desirable to have a long lifetime.
Electrodes of currently used secondary batteries and electrochemical capacitors are generally formed by applying a slurry containing an active material, a conductive material, a binder, or a binder to an aluminum foil current-etched electrochemically, Lt; / RTI >
In addition, in recent years, electronic devices that are folded or worn have appeared, and in particular, there is a growing need for a flexible capacitor device.
Prior art related to this technique is disclosed in Japanese Patent Application Laid-Open No. 2000-357631 (2000.12.26), Japanese Patent Application Laid-Open No. 2010-098109 (2010.04.30).
However, in this method, cavities may be formed because the inside of pits formed by etching are not completely filled, and electrode resistance is increased due to the bonding agent used. As time elapses, And there is a concern that the flexibility is lacking.
SUMMARY OF THE INVENTION Accordingly, it is an object of the present invention to provide a sealing material, a flexible thin film type supercapacitor device, and a supercapacitor device therefor, which are designed to solve the problems of the prior art, and which are very thin and flexible while maintaining high electrical conductivity and high- will be.
It is another object of the present invention to provide a sealing material which is economical and mass-producible, a method of manufacturing a flexible thin film type supercapacitor element by the method, and a super capacitor element therefor.
An object of the present invention is to provide a capacitor element comprising: a flexible base film; A separation membrane interposed between the base films; Wherein the graphene oxide slurry is heated and irradiated with light and then heat-treated to form the active material, wherein the active material is formed on the base film. Device.
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In addition, the base film may be formed of a material containing at least one of polyphenylene sulfide (PPS), polypropylene (PP), polyethylene phthalate (PET), polycarbonate (PC), polyethylene naphthalate (PEN), polyethylene terephthalate It is preferred that the film comprises one of a film on which a metal is deposited.
The base film is preferably surface-treated.
The collector may further include a collector formed on the base film between the base film and the separator, wherein the collector includes a metal plated after the surface of the base film is treated.
The metal may include one of nickel, platinum, silver, gold, copper, aluminum, palladium and iridium. .
The electrolyte may further include an electrolyte to permeate the active material, and the electrolyte may include an aqueous electrolyte or a non-aqueous (organic, ionic liquid) electrolyte, and the electrolyte may include any one of a liquid, a gel, .
The current collector may be formed by a method of depositing a metal or carbon-containing conductor by one or more of plating, vacuum deposition, screen printing, and stamping, or by forming a metal foil or conductive composite It is preferable to include the conductive film made.
The adhesive film may further include a heat adhesive film that surrounds the base film and includes an adhesive bonding the heat adhesive films to one another. The adhesive may be formed of an acrylate, a silicone, an epoxy, It is preferable to include one of them.
In addition, the separator preferably includes one of polyethylene (PE), polypropylene (PP), nonwoven fabric, and electrolyte-integrated separator.
On the other hand, an object of the present invention is to provide a base film having flexibility; A separation membrane interposed between the base films; An electrode electrically connected to the active material formed around the base film; And a thermally adhesive film sealable between the electrodes so as to seal the electrolyte provided between the active materials so as to maintain airtightness, wherein the electrolyte comprises KOH having high corrosiveness, and the thermal adhesive film Wherein the paraffin film comprises a plastic paraffin film and a polyolefin film, the paraffin film being capable of contacting with the electrolyte to prevent the electrolyte from flowing out, and the polyolefin film is bonded to the outside of the paraffin film to maintain the adhesion between the electrodes And is coupled between the electrodes.
Further, it is preferable to further include a reinforcing member which is bonded to the rear side of the heat adhesive film and thermally adhered to each other.
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The method of bonding the heat adhesive film and the reinforcing material is preferably selected from one or more of adhesive application method, heat bonding method, heat fusion method, and welding method.
On the other hand, an object of the present invention is to provide a method of manufacturing a capacitor device, which comprises: providing a base film having flexibility; Forming an active material on the upper side of the base film; Coupling the base film containing the active material to each other with the separator interposed therebetween so that the active materials face each other; Wherein the active material is formed using graphene oxide and the graphene oxide slurry is heated and irradiated with heat to form the active material.
In addition, the base film may be formed of a material containing at least one of polyphenylene sulfide (PPS), polypropylene (PP), polyethylene phthalate (PET), polycarbonate (PC), polyethylene naphthalate (PEN), polyethylene terephthalate And a film on which a metal is deposited, wherein the base film is preferably surface-treated.
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And forming a current collector formed on the base film between the base film and the separator, wherein the current collector is formed by plating, and the method for plating includes electroless plating or electroplating , The plating solution is one selected from the group consisting of Ni, Pt, Ag, Au, Cu, Al, Pd, .
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In addition, in the step of forming the current collector, the base film may include polyphenylene sulfide (PPS), and the surface to be plated of the base film may be roughened and sensitized, It is preferable that the base film is put into a plating solution to perform plating on the surface of the base film.
Further, in the step of forming the current collector, the base film includes polypropylene (PP), and the surface to be plated of the base film is etched, the fine particles of the catalyst are attached to the base surface and activated, .
Further, it is preferable that the method further comprises vacuum-impregnating the base film so that the electrolyte penetrates the
On the other hand, an object of the present invention is to provide a method of manufacturing a capacitor element, comprising: providing a base film having flexibility; Forming a current collector on the upper side of the base film; Forming an active material on the current collector with graphene oxide; Coupling the current collector and the base film including the active material to each other with the separator interposed therebetween so that the active materials face each other; And bonding the heat adhesive film to seal the periphery of the base film so as to maintain the airtightness of the electrolyte provided between the active materials.
Further, it is preferable to further include a reinforcing member which is bonded to the rear side of the heat adhesive film and thermally adhered to each other.
In addition, it is preferable that the electrolyte includes a strong corrosive substance, and the thermal adhesive film preferably includes a plastic paraffin film and a polyolefin film.
The method of bonding the heat adhesive film and the reinforcing material is preferably selected from one or more of adhesive application method, heat bonding method, heat fusion method, and welding method.
On the other hand, an object of the present invention is to provide a method of manufacturing a semiconductor device, comprising: providing a base film having flexibility; Forming a current collector on the upper side of the base film; Forming an active material on the current collector by graphene oxide and an electrode electrically connected to the active material; Coupling the current collector and the base film including the active material to each other with the separator interposed therebetween so that the active materials face each other; And bonding the heat-sealable film around the base film or between the electrodes so as to seal the electrolyte provided between the active materials, wherein the electrolyte includes KOH having high corrosiveness, and the heat adhesive Wherein the film comprises a plastic paraffin film and a polyolefin film, wherein the paraffin film is contactably engaged with the electrolyte to block the outflow of the electrolyte, and wherein the polyolefin film is bonded to the outer side of the paraffin film, And a capacitor element forming step of forming a capacitor element.
According to the present invention, there is provided a sealing material which is very thin and flexible, has a low energy consumption, is economical and can be mass-produced while maintaining high electrical conductivity and high bondability, and a method of manufacturing a flexible thin film type supercapacitor device A super capacitor device can be provided.
Also, it is possible to provide a sealing material capable of effectively and stably holding the material contained therein, and a method of manufacturing a flexible thin film type supercapacitor device and a supercapacitor device therefor.
FIGS. 1A and 1B are views for explaining a manufacturing process according to an embodiment of the present invention and another embodiment;
Figures 2a and 2b are tables and photographs showing chemical stability test results according to various embodiments of the base film,
2C is a photograph showing the result of the chemical stability test when the base film is PP,
FIG. 3 is a photograph of a tackiness test of a collector formed by plating when the base film is PPS,
FIGS. 4A and 4B are a schematic explanatory view for explaining a process of preprocessing and forming a current collector when the base film is PP, a photograph of a tackiness test of a plated collector,
5 is a schematic view for explaining a process of forming an active material,
6 is a graph showing electrochemical characteristics according to an embodiment of the present invention,
FIGS. 7A and 7B are graphs showing electrochemical characteristics according to another embodiment of the present invention,
8 to 13 are graphs showing electrochemical characteristics according to still another embodiment of the present invention,
14A and 14B are an exploded perspective view and a sectional view for explaining an embodiment of a sealing material constituting a capacitor element,
15 is a table comparing types and characteristics of thermal adhesives,
16A and 16C are an exploded perspective view and a sectional view showing another embodiment of the thermal adhesive,
17A and 17B are an exploded perspective view and a cross-sectional view respectively showing still another embodiment.
A method of manufacturing a flexible thin film type super capacitor device according to an embodiment of the present invention and a super capacitor device therefor will be described in detail with reference to FIGS. 1A to 17B.
FIGS. 1A and 1B are views for explaining a manufacturing process according to an embodiment of the present invention and FIGS. 2A and 2B are tables and photographs showing the results of the chemical stability test according to various embodiments of the base film FIG. 2C is a photograph showing the result of the chemical stability test when the base film is PP, FIG. 3 is a photograph of the adhesion test of the current collector formed by plating when the base film is PPS, FIGS. FIG. 5 is a schematic view for explaining the process of forming the active material, FIG. 6 is a schematic view for explaining the process of forming the active material, FIG. FIGS. 7A and 7B are graphs showing electrochemical characteristics according to another embodiment of the present invention, and FIGS. 7A and 7B are graphs showing electrochemical characteristics according to an embodiment of the present invention. FIGS. 8 to 13 are graphs showing electrochemical characteristics according to other embodiments of the present invention. FIGS. 14A and 14B are exploded perspective views for explaining an embodiment of a sealing material constituting a capacitor element, and FIGS. 16A and 16C are an exploded perspective view and a cross-sectional view showing another embodiment of the thermal adhesive, and Figs. 17A and 17B are views showing still another embodiment, respectively. Fig. An exploded perspective view and a cross-sectional view.
A method of manufacturing a flexible thin film supercapacitor element 100 (hereinafter, referred to as a capacitor element) according to an embodiment of the present invention includes a step S110 of providing a
Here, 'capacitor' in the capacitor element means a lithium-ion capacitor (LiC), an electric double-layer capacitor (EDLC), a pseudocapacitor, a hybrid capacitor, a general electrolytic capacitor, and a common capacitor.
Hereinafter, the contents related to each step will be described in detail.
First, a
In order to select the
As one example of the
PPS and PET films were selectively stable only in sulfuric acid. Fig. 2b shows the results of chemical stability test at room temperature (25 ° C) and 70 ° C As a result, the PPS film has the best chemical stability and it is also preferable to use PC, PEN and PET film when sulfuric acid is used as the electrolyte.
However, the PPS film having the best performance has a disadvantage in low cost mass production because the unit price of the product is rather high. In consideration of this, PP film was selected as a material that can be applied to mass production and satisfying price and performance among films capable of replacing PPS film. PP film is more easily coated with electroless nickel plating film than PPS film There is an advantage that it can be formed. FIG. 2c shows the state of the PP film after the chemical stability test at 6M KOH at 25 ° C and 70 ° C, indicating that the PP film after the chemical stability test is stable.
The surface of the
≪ Example 1 >
When the
≪ Example 2 >
When the
Hereinafter, the process according to the present invention will be described through various examples.
≪ Example 3 >
The process S120 of forming the
For example, the
The components of the electroless nickel plating solution contained 25 g / l of nickel sulfate (NiSO4), 50 g / l of disodium hydrogenphosphate (Na2HPO4), 25 g / l of sodium hypophosphite (NaH2PO2) and ammonium hydroxide (NH4OH) The
<Example 4>
Palladium fine particles were attached to the surface of the
This process is schematically shown in Fig. 4A.
Here, although the
≪ Example 5 >
In the above-described embodiments, nickel is included as an example of the metal forming the
≪ Example 6 >
It is preferable to form the
That is, graphene oxide is prepared using a Hummer's method, and a graphene oxide solution such as an ink is prepared. For example, a graphene oxide solution is formed on a current collector having a diameter of 2.54 cm After a proper amount is dropped, graphene oxide is deposited on the gold collector surface by hydrothermal evaporation from a hot plate at 90 ° C. Next, the graphene oxide is reduced using light including a camera flash, and the remaining moisture is removed by putting it in an oven at about 200 ° C., and an additional thermal reduction process is performed to form an active material composed of graphene on the current collector 130 (S140). FIG. 5 is a simplified illustration of such an embodiment.
The detailed process of this embodiment is described in the 'Grain-based thin film supercapacitor electrode device using oxidized graphene directly using solution and method of manufacturing the same' filed by the present applicant, and a detailed description thereof will be omitted below.
However, the graphene structure deposited through the hydrothermal evaporation deposition can be induced to form a layer while maintaining the state of mutual bonding without being destroyed or damaged, so that the binding of the active material and the reliability of the product can be improved.
The electrode thus prepared (hereafter, the electrode means a state in which the
On the other hand, unlike the present embodiment, the active material that can be applied to the present invention includes organic and inorganic electrode active materials capable of constituting a known supercapacitor electrode including carbon, for example, a carbon material, a carbon hybrid material, a metal oxide, , Sulfides, conductive polymers, and the like.
≪ Example 7 >
The
In the cyclic voltammogram of FIG. 7A, the quadrangular shape, which is a typical form of the electric double layer, is maintained up to 30 mV / s. The specific capacity obtained at 5 mV / s is 143.5 F / The equivalent series resistance value (ESR) obtained from the AC-impedance measurement is 1.16 Ω.
≪ Example 8 >
1A is a plan view of a
That is, a thermal adhesive (not shown) containing epoxy is applied to the periphery of the
FIG. 8 shows the electrochemical characteristics of the
≪ Example 9 >
The
≪ Example 10 >
In this embodiment, 95 wt% of graphene powder (Skyspring nanomaterials, inc.), 2.5 wt% of styrene-butadiene rubber (SBR) as a binder, 2.5 wt% of carboxymethyl cellulose (CMC) Is deposited on the
≪ Example 11 >
In the case of this embodiment, a solution obtained by mixing 95 wt% of graphene powder (Skyspring nanomaterials, inc.) And 5.0 wt% of polystyrene with a binder is applied to the nickel foil collector 130 ). FIG. 11 shows a result of a three electrode test in which a
≪ Example 12 >
1A and 1B schematically illustrate the fabrication process of a
The adhesive, which is an adhesive material used for bonding the device, preferably includes one of acrylate, silicone, epoxy and thermal adhesive.
FIG. 12 shows the electrochemical characteristics of the
On the other hand, in order to form the device, one or a plurality of methods are preferably selected from a bonding method using an adhesive, a thermal bonding method, a heat welding method, and other welding methods.
In the present embodiment, mainly a plastic paraffin film and a polyolefin film are thermally bonded in parallel and PP films are thermally fused to each other.
Here, an adhesion method capable of stably holding all types of electrolytic solution is preferable. For example, in the case of a lithium battery using an organic electrolyte, if it is assembled using an aluminum pouch, there is no great corrosivity and there is not much trouble in adhesion. However, in the present invention, there is almost no method of stably holding the electrolyte when a corrosive electrolyte such as 6M KOH is used. However, in the present invention, a paraffin film having high hydrophobicity is thermally adhered to the outer surface of the inner electrolyte (Waterproof), and an adhesive force between the
This method can be applied not only to the capacitor element but also to the case where the other acid / base must be trapped.
On the other hand, the electrolytes applicable to the present invention include aqueous and non-aqueous (organic, ionic liquid) electrolytes, and the shape of the electrolyte may include liquid, gel, solid type and the like.
On the other hand, the separator that can be applied in the present invention includes a separator made of polyethylene and polypropylene series, nonwoven fabric, and electrolyte.
≪ Example 12 >
13 shows the electrochemical characteristics of the
Therefore, according to the present invention, it is possible to provide a simple process which is very thin and flexible while maintaining high electrical conductivity and high bondability, and which does not require an electrochemical etching process even in the manufacturing process, and shortens the heating time in a hydrocarbon atmosphere, And a supercapacitor element according to the method can be provided.
≪ Example 13 >
In this embodiment, any one of a paraffin film and a polyolefin film is used as a thermal adhesive material. In this embodiment, not only an electrolyte but also an acidic or alkali-resistant material, The sealing
First, as shown in FIGS. 14A and 14B, the sealing
Assuming that the sealing
Although the paraffin, polyolefin, or ethylene vinyl acetate (EVA) used as the
The sealing means, which is a sealing method for sealing the
FIG. 15 is a table showing the results of testing the suitability of the sealing portion when the receiving material, which is a substance to be sealed after heat-sealing using a variety of thermal adhesives (491) by thermal sealing, is 'KOH' Respectively. It can be confirmed in FIG. 15 that paraffin, polyolefin, or ethylene vinyl acetate (EVA) material is used as the
On the other hand, in the sealing
The present embodiment is applicable not only to the above-described capacitor element but also to a case of sealing / sealing various materials capable of sealing the received and received materials therein.
In the prior art, a method of confining 'KOH' used as an electrolyte other than a battery of various sizes including a conventional AA type battery was not found, so that 'KOH' could not be used in the thin plate capacitor element of the present invention. That is, in the prior art, no consideration is given to the thermal adhesive as described above.
However, according to the present invention, it is possible to solve the problems that can not be solved by the sealing materials (400, 500) of the present invention by referring to the various graphs and tables attached heretofore and it is possible to stably and efficiently It can be confined.
≪ Example 14 >
The sealing
17B with respect to the sealing
That is, a sealing portion 793a1 is disposed inside the sealing
With this embodiment, it is possible to provide a sealing
While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is evident that many alternatives, modifications and variations will be apparent to those skilled in the art without departing from the scope and spirit of the invention. will be. The scope of the invention will be determined by the appended claims and their equivalents.
100: capacitor element 110: base film
130: current collector 150: active material
170: separator 191: thermal adhesive film
191a: Auxiliary thermal adhesive 193: Stiffener
Claims (31)
An electrode formed on the base film and including a current collector formed on an upper side thereof and having a region protruding from the external power source so as to be connected to an external power source;
A separator interposed between the base films to separate the active material;
And a thermally adhesive film sealingly sealing the sealing portion between the inner periphery of the base film and the extending region of the electrode so as to confine the electrolyte provided between the active materials,
Wherein the electrolyte comprises KOH which is highly corrosive,
Wherein the thermally adhesive film comprises a plastic paraffin film and a polyolefin film, wherein the paraffin film is contactably engaged with the electrolyte to block the external flow of the electrolyte, and the polyolefin film is bonded to the outside of the paraffin film, And between the extended regions of the electrode to maintain an adhesive force between the extended regions.
And a stiffener joined to the rear of the thermal adhesive film and thermally adhered to each other.
Wherein the thermal adhesive film further comprises an ethylene-vinyl acetate (EVA) film.
Wherein the heat adhesive film and the reinforcing material are adhered to each other by one or a plurality of methods selected from an adhesive application method, a thermal adhesion method, a heat fusion method and a welding method.
Forming a current collector on the upper side of the base film;
Providing an electrode including an active material formed of graphene oxide in the current collector and the current collector and electrically connected to the current collector and having a region protruding and extending to be connected to an external power source;
Coupling the current collector and the base film including the active material to each other with the separator interposed therebetween so that the active materials face each other;
And sealingly bonding the heat adhesive film between the extending region of the electrode and the base film to confine the electrolyte provided between the active materials so as to maintain the airtightness,
Wherein the electrolyte comprises KOH which is highly corrosive, the thermal adhesive film comprises a plastic paraffin film and a polyolefin film,
Wherein the paraffin film is bonded to the electrolyte to prevent external leakage of the electrolyte, and the polyolefin film is bonded to the outside of the paraffin film to maintain an adhesive strength.
And a stiffener joined to the rear of the thermal adhesive film and thermally adhered to each other.
Wherein the thermal adhesive film comprises an ethylene-vinyl acetate (EVA) film.
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US14/602,443 US9520243B2 (en) | 2014-02-17 | 2015-01-22 | Method of manufacturing flexible thin-film typer super-capacitor device using a hot-melt adhesive film, and super-capacitor device manufactured by the method |
US15/158,764 US9842706B2 (en) | 2014-02-17 | 2016-05-19 | Sealing material used as a flexible thin-film type super-capacitor device |
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KR102447851B1 (en) * | 2021-06-24 | 2022-09-27 | 나노캡 주식회사 | Ultra-thin electric double layer capacitor of high voltage using gel electrolyte and method for manufacturing the same |
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