CN101162650A - Flexible thin film type solid-state super capacitor and its manufacture process - Google Patents
Flexible thin film type solid-state super capacitor and its manufacture process Download PDFInfo
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- CN101162650A CN101162650A CN 200710035013 CN200710035013A CN101162650A CN 101162650 A CN101162650 A CN 101162650A CN 200710035013 CN200710035013 CN 200710035013 CN 200710035013 A CN200710035013 A CN 200710035013A CN 101162650 A CN101162650 A CN 101162650A
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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
- H01G11/22—Electrodes
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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
- 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
Abstract
The invention discloses a flexible film type solid state super capacitor and a method for manufacturing the same; the flexible film type solid state super capacitor comprises a positive electrode, a negative electrode, an outer electrode and an encapsulation film, wherein a flexibility solid state electrolyte membrane is arranged between the positive and the negative electrodes. The manufacturing method is as follows: the outer electrode pasting, the electrode pasting, the flexibility solid state electrolyte pasting, the electrode pasting, the outer electrode pasting and the encapsulation pasting are orderly and precisely coated on a basal body by the printing technique; by fitting the corresponding pressing, drying, cutting and packaging techniques, the flexible film type solid state super capacitor with electrode-membrane-electrode structure is finally formed. The flexible film type solid state super capacitor has the advantages of low product internal resistance and good power characteristic, and is suitable for the large scale production and particularly applied to flexible electric products such as electric papers, intelligent name cards and plastics electric products, etc.
Description
Technical field
The present invention relates to a kind of capacitor, particularly a kind of flexible thin film type solid-state super capacitor and manufacture method thereof.
Background technology
Capacitor is the indispensable important components and parts of electronics industry, and millifarad to farad level large value capacitor can be used for the energy storage device of circuit, but traditional electrolytic capacitor will accomplish that millifarad to farad level must have very big volume.
Ultracapacitor is a kind of novel energy-storing device that occurs in recent years, and its capacity can reach farad level even thousands of farad, than the big several magnitude of traditional electrical electrolysis condenser capacity.It has the advantage that conventional capacitor power density is big, the rechargeable battery energy density is high concurrently, but fast charging and discharging, and also the life-span is long.
Ultracapacitor can be divided into double electric layer capacitor and electrochemical capacitor two big classes.
The active carbon double electric layer capacitor is to be main electrode material with the active carbon, and its operation principle as shown in Figure 2.When metal electrode inserted in the electrolyte, net charge on the electrode surface and the charged ion in the solution formed electric double layer.Because have a barrier potential on the interface, two layer charges can not be crossed the border and neutralize each other, will form a plate condenser according to the capacitor principle.Because activated carbon surface is long-pending huge, and the electric double layer thickness that forms has only several dusts, tens little to hundreds of dusts more than general electrolytic capacitor oxide-film.Therefore, double electric layer capacitor can obtain the capacity of farad level.
The electric chemical super capacitor operation principle: with the ruthenium-oxide electrochemical capacitor is example, and electrode is ruthenium-oxide (RuO
x), electrolyte is sulfuric acid, and when metal oxide electrode charged (discharge) in electrolyte, hydrogen ion was adsorbed (desorb) and enters (leaving) oxide intracell, the generation redox reaction forms so-called Faraday pseudo-capacitance and carries out work, so be called electrochemical capacitor.Electrochemical capacitor can obtain the capacitance higher than double electric layer capacitor.
Just towards the development of weak point, little, light, thin direction, for adapting to this requirement, electronic devices and components are also to chip type, integrated, modularization development for electronic product at present.Though ultracapacitor has advantages such as capacity is big, power is high, the life-span is long, but because present ultracapacitor uses liquid solution to be electrolyte, reveal for preventing electrolyte, the encapsulation of device must be satisfied high requirement, make ultracapacitor be difficult to further reduced volume, therefore present ultracapacitor product structure has only convoluted (cylindric), button type (being similar to button cell), because the restriction of its contour structures also fails to obtain to use in products such as film-type electronic product, electronic card.
People such as Joo-Hwan Sunga are the template electrode with the gold, by the synthetic preparation of electrochemistry polypyrrole (PPy) electrode, are using polyvinyl alcohol (PVA) and phosphoric acid (H
3PO
4) make gel electrolyte, the polypyrrole electrode is glued down and the formation flexible super capacitor this technology simple possible with this gel electrolyte, gold template electrode is reusable, but the polypyrrole electrode need be synthetic by electrolysis, and production efficiency is low, be not suitable for suitability for industrialized production, and the internal resistance height, power-performance is poor.
Summary of the invention
Require technical problem high, that volume is big, production efficiency is low for solving existing ultracapacitor encapsulation, the invention provides a kind of flexible thin film type solid-state super capacitor and manufacture method thereof.
The technical scheme that the present invention solves the problems of the technologies described above is: comprise positive and negative electrode, external electrode and encapsulating film, it is characterized in that: be provided with the flexible solid electrolyte membrance between positive and negative electrode.
In the above-mentioned flexible thin film type solid-state super capacitor, described positive and negative electrode consists of conducting polymer, active carbon, carbon black, metal oxide.
In the above-mentioned flexible thin film type solid-state super capacitor, described flexible solid electrolyte membrance is gel state electrolyte or solid electrolyte.
In the above-mentioned flexible thin film type solid-state super capacitor, described gel state electrolyte is made up of electrolytic salt, polymer, plasticizer, inorganic additive, and solid electrolyte is made up of polyoxyethylene or polyoxypropylene and electrolytic salt.
In the above-mentioned flexible thin film type solid-state super capacitor, described electrolytic salt is quaternary ammonium salt, ionic liquid or lithium salts.
In the above-mentioned flexible thin film type solid-state super capacitor, described quaternary ammonium salt is (C
2H
3)
1NBF
4Or CH
3(C
2H
5)
3NBF
1, ionic liquid is [EMIm] BF
4, [BMIm] BF
4, [BMIm] PF
6, [EMIm] NTf
2Or [BMPy] NTf
2, lithium salts is LiBF
4, LiPF6 or LiAsF6.
A kind of manufacture method of flexible thin film type solid-state super capacitor may further comprise the steps:
Prepare external electrode slurry, electrode slurry, flexible solid electrolyte slurry, packaging slurry respectively;
The external electrode slurry is printed on organic basement membrane, after the printing print film oven dry is obtained anodal outer electrode membrane;
Electrode slurry is printed on the outer electrode membrane of having dried, external electrode one end is exposed, all the other positions cover, and after the printing print film oven dry are obtained cathode film;
Electrolyte slurry is printed on the cathode film of having dried, makes dielectric film cover cathode film fully, and all slightly wideer than each limit of cathode film, after the printing print film oven dry is obtained solid electrolyte membrane;
Electrode slurry is printed on the solid electrolyte membrane of having dried, and printing area is identical with cathode film, and its position is just in time relative with cathode film, after the printing print film oven dry is obtained negative electrode film;
The external electrode slurry is printed on the negative electrode film of having dried, and its printing area and position are identical with anodal outer electrode membrane, after the printing print film oven dry are obtained the negative pole outer electrode membrane;
Packaging slurry is printed on the negative pole outer electrode membrane of having dried, the limit of drawing of anodal outer electrode membrane and negative pole outer electrode membrane is exposed, all the other places cover fully, after the printing print film oven dry are obtained encapsulating film.
External electrode, positive and negative electrode, electrolyte, the encapsulation of adopting technology of the present invention to produce all has flexible preferably, therefore can produce flexible device on the substrate with flexibility; Owing to adopt accurate printing technology to make, therefore can produce the film-type device again, and realize easily making in batches.To sum up, adopt the technology of the present invention can make the flexible thin film type ultracapacitor that thickness is 0.2～1.0mm in batches.
This flexible thin film type solid-state super capacitor is fit to large-scale production, and the product internal resistance is low, and power characteristic is good, is very suitable for the application of flexible electronic product (flexible electronic product), Electronic Paper for example, intelligent business card and plastic electronic product etc.
The present invention is further illustrated below in conjunction with the drawings and specific embodiments.
Description of drawings
Fig. 1 is a flexible thin film type solid-state super capacitor structure chart of the present invention.
Fig. 2 is an active carbon double electric layers supercapacitor fundamental diagram.
Fig. 3 is a flexible thin film type solid-state super capacitor manufacture process schematic diagram of the present invention.
Embodiment
The structure of flexible thin film type solid-state super capacitor of the present invention as shown in Figure 1, by positive and negative two electrodes (3,5), two interelectrode flexible solid electrolyte membrances 4, external electrode 2,6 and flexible package film 1.
Embodiment 1:
(1) electrode slurry preparation: 80g active carbon, 10g carbon black, 10g Kynoar (PVDF) were stirred mixed 3 hours with 500g and N methyl pyrrolidone.
(2) electrolyte slurry preparation: 100g pva powder (PVA) is mixed with the 800g deionized water, be heated to 95 ℃ and stirred 2 hours, add the 1g SiO of granularity＜5 μ m again
2Micro mist, 15g tetraethylammonium tetrafluoroborate stir and mixed in 10 hours.
(3) external electrode slurry preparation: 10g pva powder (PVA) is mixed with the 100g deionized water, be heated to 90 ℃ and stirred 1 hour, add again, stirred 2 hours with 20g nickel powder (200 order) and 10g silver powder (200 order).
(4) packaging slurry preparation: 50g Kynoar (PVDF) is gone to mix 3 hours from Yu Shui with 500g.
(5) be ready for the printing stencil that prints outer electrode membrane, electrode film, dielectric film, encapsulating film in advance.
(6) print anodal outer electrode membrane: the external electrode slurry is printed on the thick silicone rubber-based membranes of 0.1mm, printing area: 4.0 * 2.0mm, thickness: 30～100 μ m, shown in the first step of Fig. 3.After the printing print film drying in 60 ℃～120 ℃ baking oven was obtained anodal outer electrode membrane in 30 minutes.
(7) printing cathode film: electrode slurry is printed on the outer electrode membrane of having dried, printing area: 2.0 * 2.0mm, thickness: 30～100 μ m, make external electrode one end expose 2.0mm, all the other positions cover, shown in second step of Fig. 3.After the printing print film drying in 60 ℃～120 ℃ baking oven was obtained cathode film in 30 minutes.
(8) printing solid electrolyte membrane: electrolyte slurry is printed on the cathode film of having dried, printing area: 3.0 * 3.0mm, thickness: 30～100 μ m make dielectric film cover cathode film fully, and than all wide 0.5mm in each limit of cathode film, shown in the 3rd step of Fig. 3.After the printing drying in the baking oven of 60 ℃～120 ℃ of print film was obtained solid electrolyte membrane in 30 minutes.
(9) printing negative electrode film: electrode slurry is printed on the solid electrolyte membrane of having dried, printing area: 2.0 * 2.0mm, thickness: 30～100 μ m, each limit that makes negative electrode film is all than the narrow 0.5mm of dielectric film, be that negative electrode film is just in time relative with cathode film, shown in the 4th step of Fig. 3.After the printing drying in the baking oven of 60 ℃～120 ℃ of print film was obtained negative electrode film in 30 minutes.
(10) printing negative pole outer electrode membrane: the external electrode slurry is printed on the negative electrode film of having dried, printing area: 4.0 * 2.0mm, thickness: 50～100 μ m make a length of side of negative pole outer electrode membrane go out negative pole 2.0mm, all the other places just in time cover, shown in the 5th step of Fig. 3.After the printing drying in the baking oven of 60 ℃～120 ℃ of print film was obtained the negative pole outer electrode membrane in 30 minutes.
(11) printing encapsulating film: packaging slurry is printed on the negative pole outer electrode membrane of having dried, printing area: 4.0 * 4.0mm, thickness: 50～100 μ m make the outside limit of anodal outer electrode membrane and negative pole outer electrode membrane respectively expose 1.0mm, all the other places cover fully, shown in the 6th step of Fig. 3.After the printing drying in the baking oven of 60 ℃～120 ℃ of print film was obtained encapsulating film in 30 minutes.
Embodiment 2:
(1) electrode slurry preparation: 60g active carbon, 25g manganese dioxide, 5g carbon black, 10g Kynoar (PVDF) were stirred mixed 3 hours with 500g N methyl pyrrolidone.
(2) electrolyte slurry preparation: 100g pva powder (PVA) is mixed with the 800g deionized water, be heated to 95 ℃ of stirrings 2 hours, add granularity＜1g SiO2 micro mist of 5 μ m, 15g tetraethylammonium tetrafluoroborate again, stir and mixed in 10 hours.
(3) external electrode slurry preparation: with 10g Kynoar powder (PVDF) and 100gN methyl pyrrolidone, be heated to 60 ℃ and stirred 1 hour, add again, stirred 2 hours with 20g nickel powder (200 order) and 10 silver powder (200 order).
(4) packaging slurry preparation: 50g Kynoar (PVDF) was mixed 3 hours with the 500g deionized water and stirring.
(5) adopt printing technology successively external electrode slurry, electrode slurry, flexible solid electrolyte slurry, electrode slurry, external electrode slurry, packaging slurry accurately to be applied on organic basement membrane (any of PVDF, PVC, polyurethane, silicon rubber, natural rubber) by the processing step of embodiment 1, cooperate corresponding compacting, oven dry, cutting, technology of the package, finally form the flexible thin film type solid-state super capacitor of electrode/membrane/electrode structure.
Embodiment 3:
(1) electrode slurry preparation: 85g polypyrrole (PPy), 5g carbon black, 10g Kynoar (PVDF) were stirred mixed 3 hours with 500g and N methyl pyrrolidone.
(2) electrolyte slurry preparation: (VDF-HFP) mixes with 800gNMP with the 100g copolymer p, stirs 2 hours, adds 30ml dibutyl phthalate (DBP), stirs 1 hour, adds 0.3g Al again
2O
3(average grain diameter＜60nm), 15g tetraethylammonium tetrafluoroborate stir and mixed in 1 hour nanometer powder.
(3) external electrode slurry preparation: with 10g Kynoar powder (PVDF) and 100gN methyl pyrrolidone, be heated to 60 ℃ and stirred 1 hour, add again, stirred 2 hours with 20g nickel powder (200 days) and 10 silver powder (200 order).
(4) packaging slurry preparation: 50g Kynoar (PVDF) was mixed 3 hours with the 500g deionized water and stirring.
(5) adopt printing technology successively external electrode slurry, electrode slurry, flexible solid electrolyte slurry, electrode slurry, external electrode slurry, packaging slurry accurately to be applied on the matrix (any of PVDF, PVC, polyurethane, silicon rubber, natural rubber) by the processing step of embodiment 1, cooperate corresponding compacting, oven dry, cutting, technology of the package, finally form the flexible thin film type solid-state super capacitor of electrode/membrane/electrode structure.
Embodiment 4:
(1) electrode slurry preparation: 85g polyaniline (PANI), 5g carbon black, 10g Kynoar (PVDF) were stirred mixed 3 hours with 500g and N methyl pyrrolidone.
(2) electrolyte slurry preparation: (VDF-HFP) mixes with 800gNMP with the 100g copolymer p, stirs 2 hours, adds 30ml dibutyl phthalate (DBP), stirs 1 hour, adds 0.3g Al again
2O
3(average grain diameter＜60nm), 15g trimethyl-ethyl ammonium tetrafluoroborate stir and mixed in 1 hour nanometer powder.
(3) external electrode slurry preparation: with 10g Kynoar powder (PVDF) and 100gN methyl pyrrolidone, be heated to 60 ℃ and stirred 1 hour, add again, stirred 2 hours with 20g nickel powder (200 order) and 10 silver powder (200 order).
(4) packaging slurry preparation: 50g Kynoar (PVDF) was mixed 3 hours with the 500g deionized water and stirring.
(5) adopt printing technology successively external electrode slurry, electrode slurry, flexible solid electrolyte slurry, electrode slurry, external electrode slurry, packaging slurry accurately to be applied on the matrix (any of PVDF, PVC, polyurethane, silicon rubber, natural rubber) by the processing step of embodiment 1, cooperate corresponding compacting, oven dry, cutting, technology of the package, finally form the flexible thin film type solid-state super capacitor of electrode/membrane/electrode structure.
The ultracapacitor performance of making gained in the foregoing description is as shown in table 1.
Table 1
| Electrode material | Membrane materials for electrolyte | Product size/mm | Capacity/mF | Internal resistance/Ω | Leakage current/μ A | |
| Embodiment 1 | Active carbon+carbon black | Polyvinyl alcohol+Et 4NBF 4 | 2×2× 0.3 | 2.2± 20％ | 51.5 ±15 ％ | 0.10± 20％ |
| Embodiment 2 | Active carbon+manganese dioxide+carbon black | Polyvinyl alcohol+Et 4NBF 4 | 5×4× 0.4 | 2.9± 20％ | 58.8 ±15 ％ | 0.20± 20％ |
| Embodiment 3 | Polypyrrole+carbon black | P(VDF-HFP) +Et 4NBF 4 | 5×4× 0.4 | 3.5± 20％ | 46.4 ±15 ％ | 0.20± 20％ |
| Embodiment 4 | Polyaniline+carbon black | P(VDF-HFP) +Me 3Et NBF 4 | 5×4× 0.4 | 3.8± 20％ | 43.6 ±15 ％ | 0.15± 20％ |
As can be seen from Table 2, can produce the flexible thin film type solid ultracapacitor of function admirable by the present invention.
Above-mentioned only is several example of the present invention, does not illustrate that the present invention only limits to the described content of following example, and the technical staff in the industry all belongs to content of the present invention according to the product of claim item of the present invention manufacturing.
Claims (10)
1. a flexible thin film type solid-state super capacitor comprises positive and negative electrode, external electrode and encapsulating film, it is characterized in that: be provided with the flexible solid electrolyte membrance between positive and negative electrode.
2. flexible thin film type solid-state super capacitor according to claim 1 is characterized in that: described positive and negative electrode consists of conducting polymer, active carbon, carbon black, metal oxide.
3. flexible thin film type solid-state super capacitor according to claim 1 is characterized in that: described flexible solid electrolyte membrance is gel state electrolyte or solid electrolyte.
4. flexible thin film type solid-state super capacitor according to claim 3, it is characterized in that: described gel state electrolyte is made up of electrolytic salt, polymer, plasticizer, inorganic additive, and solid electrolyte is made up of polyoxyethylene or polyoxypropylene and electrolytic salt.
5. flexible thin film type solid-state super capacitor according to claim 4 is characterized in that: described electrolytic salt is quaternary ammonium salt, ionic liquid or lithium salts.
6. flexible thin film type solid-state super capacitor according to claim 5 is characterized in that: described quaternary ammonium salt is (C
2H
5)
4NBF
4Or CH
3(C
2H
5)
3NBF
4, ionic liquid is [EMIm] BF
4, [BMIm] BF
4, [BMIm] PF
6, [EMIm] NTf
2Or [BMPy] NTf
2, lithium salts is LiBF
4, LiPF6 or LiAsF6.
7. the manufacture method of a flexible thin film type solid-state super capacitor may further comprise the steps:
Prepare external electrode slurry, electrode slurry, flexible solid electrolyte slurry, packaging slurry respectively;
The external electrode slurry is printed on organic basement membrane, after the printing print film oven dry is obtained anodal outer electrode membrane;
Electrode slurry is printed on the outer electrode membrane of having dried, external electrode one end is exposed, all the other positions cover, and after the printing print film oven dry are obtained cathode film;
Electrolyte slurry is printed on the cathode film of having dried, makes dielectric film cover cathode film fully, and all slightly wideer than each limit of cathode film, after the printing print film oven dry is obtained solid electrolyte membrane;
Electrode slurry is printed on the solid electrolyte membrane of having dried, and printing area is identical with cathode film, and its position is just in time relative with cathode film, after the printing print film oven dry is obtained negative electrode film;
The external electrode slurry is printed on the negative electrode film of having dried, and its printing area and position are identical with anodal outer electrode membrane, after the printing print film oven dry are obtained the negative pole outer electrode membrane;
Packaging slurry is printed on the negative pole outer electrode membrane of having dried, the limit of drawing of anodal outer electrode membrane and negative pole outer electrode membrane is exposed, all the other places cover fully, after the printing print film oven dry are obtained encapsulating film.
8. the manufacture method of flexible thin film type solid-state super capacitor according to claim 7, described flexible solid electrolyte slurry is gel state electrolyte or solid electrolyte.
9. the manufacture method of flexible thin film type solid-state super capacitor according to claim 7, described positive and negative electrode slurry consists of conducting polymer, active carbon, carbon black, metal oxide.
10. the manufacture method of flexible thin film type solid-state super capacitor according to claim 7, organic basement membrane be PVDF, PVC, polyurethane, silicon rubber, natural rubber any.
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