KR102398468B1 - Sheet electrode for electric double layer capacitor and manufacturing method thereof - Google Patents
Sheet electrode for electric double layer capacitor and manufacturing method thereof Download PDFInfo
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- KR102398468B1 KR102398468B1 KR1020150132899A KR20150132899A KR102398468B1 KR 102398468 B1 KR102398468 B1 KR 102398468B1 KR 1020150132899 A KR1020150132899 A KR 1020150132899A KR 20150132899 A KR20150132899 A KR 20150132899A KR 102398468 B1 KR102398468 B1 KR 102398468B1
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- 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
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
-
- 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
- H01G11/34—Carbon-based characterised by carbonisation or activation of carbon
-
- 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
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
본 발명은, 폴리머(Polymer), 활성탄(Active carbon), 도전재(Conductive material) 및 바인더(Binder)를 분산용매에 투입 및 혼합하여 전극 혼합물을 제조하는 단계와, 상기 전극 혼합물을 이용하여 시트를 제조하는 단계와, 상기 시트를 금속집전체에 적층한 후 열처리 압착하는 단계를 통해 제조되는 전기이중층 커패시터용 시트전극 제조방법에 있어서, 상기 폴리머는 수소결합이 형성된 관능기(Functional group)를 포함하는 폴리머이고, 상기 열처리 압착은 80 내지 200℃에서 이루어지되, 상기 열처리 압착에 의해 상기 폴리머에 포함된 상기 관능기의 수소결합(Hydrogen bond) 분해가 발생되고, 상기 관능기의 수소결합 분해를 통해 상기 금속집전체와 상기 시트가 접착되는 것을 기술적 요지로 한다. 이에 의해 전기이중층 커패시터용 시트전극 및 그 제조방법은 전극시트에 존재하는 폴리머(Polymer)의 카복실기(Carboxylic group) 또는 하이드록시기(Hydroxy group) 관능기 내의 수소결합이 끊어지면서 전극시트와 금속집전체가 직접적으로 결합되는 효과를 얻을 수 있다. 또한, 셀의 고온 및 고전압에서 부반응이 억제되며 우수한 전기적인 특성을 가질 수 있다.The present invention includes the steps of preparing an electrode mixture by adding and mixing a polymer, active carbon, a conductive material, and a binder in a dispersion solvent, and forming a sheet using the electrode mixture In the method for manufacturing a sheet electrode for an electric double layer capacitor manufactured through the manufacturing steps, laminating the sheet on a metal current collector and then heat-treating and compressing the sheet, the polymer comprises a functional group in which hydrogen bonds are formed. and the heat treatment compression is performed at 80 to 200° C., and hydrogen bond decomposition of the functional group included in the polymer is generated by the heat treatment compression, and the metal current collector through hydrogen bond decomposition of the functional group And it is a technical gist that the sheet is adhered. As a result, the sheet electrode for an electric double layer capacitor and a method for manufacturing the same are provided with the electrode sheet and the metal current collector as hydrogen bonds within the carboxylic group or hydroxyl group functional group of the polymer present in the electrode sheet are broken. can be directly combined. In addition, side reactions are suppressed at high temperature and high voltage of the cell, and excellent electrical properties may be obtained.
Description
본 발명은 전기이중층 커패시터용 시트전극 및 그 제조방법에 관한 것으로, 더욱 상세하게는 전극시트에 존재하는 폴리머(Polymer)의 카복실기(Carboxylic group) 또는 하이드록시기(Hydroxy group) 관능기 내의 수소결합이 끊어지면서 전극시트와 금속집전체가 직접적으로 결합되는 전기이중층 커패시터용 시트전극 및 그 제조방법에 관한 것이다.The present invention relates to a sheet electrode for an electric double layer capacitor and a method for manufacturing the same, and more particularly, hydrogen bonding in a carboxylic group or a hydroxyl group of a polymer present in the electrode sheet. It relates to a sheet electrode for an electric double layer capacitor in which an electrode sheet and a metal current collector are directly coupled while being cut off, and a method for manufacturing the same.
전기이중층 커패시터(Electric double layer capacitor, EDLC)는 탄소 재료로 이루어진 한 쌍의 분극성 전극 사이에 절연성이 우수한 격리막(Separator)이 배치되어 전극과 전해액 사이에 이중층을 형성하여 용량을 발현하는 에너지 저장 디바이스 중 하나이다. 이러한 전기이중층 커패시터는 에너지 저장 디바이스 중에서 에너지를 단시간에 입, 출력할 수 있어 정류회로, 잡음감쇠 및 전원용 펄스 발생 등에 응용되고 있다.An electric double layer capacitor (EDLC) is an energy storage device in which a separator with excellent insulation is disposed between a pair of polarizable electrodes made of a carbon material to form a double layer between the electrode and an electrolyte to express capacity. one of them Such an electric double layer capacitor can input and output energy in a short time among energy storage devices, and thus is applied to a rectifier circuit, noise attenuation, and power pulse generation.
최근에는 전자기기에 사용되고 있는 기존의 전기화학 커패시터에 비하여 비약적으로 용량이 증대된 전기이중층 커패시터가 개발되었으며, 고출력 펄스 파워 능력과 고용량 에너지 저장능력으로 인하여 전지와 더불어 소형 경량의 전기 화학적 에너지 저장장치, 대출력 펄스 파워 및 피크 파워의 부하 평준화용으로 응용을 추진하고 있다. 뿐만 아니라 여러 가지 에너지 저장장치 중 환경 친화적 재료의 사용, 장 수명 및 고충방전 효율 등으로 인하여 환경, 경제적인 측면에서 기술의 중요성이 부각되고 있는 전기이중층 커패시터의 활용으로서는 군사용, 우주항공용, 의료용, 전기자동차 등의 고부가 장비의 대출력 펄스 파워의 주전원 및 보조전원으로 사용될 것이 전망된다.In recent years, electric double layer capacitors have been developed, which have dramatically increased capacity compared to conventional electrochemical capacitors used in electronic devices. Applications are being promoted for load leveling of high power pulse power and peak power. In addition, among various energy storage devices, the use of eco-friendly materials, long lifespan, and high charging and discharging efficiency, etc. It is expected to be used as the main power and auxiliary power for high-output pulse power of high value-added equipment such as automobiles.
이러한 전기이중층 커패시터의 전극은 집전체에 부착되기 위해서 도 1에 도시된 종래기술 '대한민국특허청 공개특허 제10-2009-0103432호 전기 이중층 커패시터 및 그 제조 방법'과 같이 열가소성 수지(Thermoplastic) 또는 합성 수지(Synthetic resine)와, 그라파이트 (Graphite)또는 활성탄(Active carbon)과 같은 카본소재를 분산용매(Dispersion medium)인 D.I water에 분산시켜 도전성 접착제(Conducting adhesive)를 제조하고, 이를 알루미늄(Al), 구리(Cu) 등과 같은 금속 집전체(Current collector) 위에 도포한 후 도전성 접착제에 시트 전극을 부착하는 방식으로 시트 전극을 금속 집전체에 부착하였다.In order to be attached to the current collector, the electrode of the electric double layer capacitor is made of a thermoplastic resin or synthetic resin as in the prior art 'Korea Patent Office Publication No. 10-2009-0103432 Electric double layer capacitor and its manufacturing method' shown in FIG. 1 . (Synthetic resine) and a carbon material such as graphite or activated carbon are dispersed in D.I water, a dispersion medium, to prepare a conductive adhesive, which is then used for aluminum (Al), copper After coating on a metal current collector such as (Cu), the sheet electrode was attached to the metal current collector by attaching the sheet electrode to the conductive adhesive.
하지만 이와 같이 도전성 페이스트를 이용하여 금속 집전체와 시트 전극을 부착한 전극의 경우 전기이중층 커패시터 셀에 온도 또는 높은 전압이 인가되게 되면 시트 전극과 도전성 페이스트가 부착된 면에서 수지의 분해 반응이 일어나 셀에 크랙이 발생하는 등 문제가 발생한다. However, in the case of an electrode to which a metal current collector and a sheet electrode are attached using a conductive paste as described above, when a temperature or high voltage is applied to the electric double layer capacitor cell, a decomposition reaction of the resin occurs on the surface to which the sheet electrode and the conductive paste are attached. There are problems such as cracks in the
따라서 본 발명의 목적은, 전극시트에 존재하는 폴리머(Polymer)의 카복실 기(Carboxylic group) 또는 하이드록시기(Hydroxy group) 관능기 내의 수소결합이 끊어지면서 전극시트와 금속집전체가 직접적으로 결합되는 전기이중층 커패시터용 시트전극 및 그 제조방법을 제공하는 것이다.Therefore, it is an object of the present invention, the electrode sheet and the metal current collector are directly coupled while the hydrogen bond in the carboxylic group or the hydroxyl group functional group of the polymer present in the electrode sheet is broken. To provide a sheet electrode for a double-layer capacitor and a method for manufacturing the same.
또한, 셀의 고온 및 고전압에서 부반응이 억제되며 우수한 전기적인 특성을 갖는 전기이중층 커패시터용 시트전극 및 그 제조방법을 제공하는 것이다.Another object of the present invention is to provide a sheet electrode for an electric double layer capacitor having excellent electrical properties and suppressing side reactions at high temperature and high voltage of the cell, and a method for manufacturing the same.
상기한 목적은, 폴리머(Polymer), 활성탄(Active carbon), 도전재(Conductive material) 및 바인더(Binder)를 분산용매에 투입 및 혼합하여 전극 혼합물을 제조하는 단계와, 상기 전극 혼합물을 이용하여 시트를 제조하는 단계와, 상기 시트를 금속집전체에 적층한 후 열처리 압착하는 단계를 통해 제조되는 전기이중층 커패시터용 시트전극 제조방법에 있어서, 상기 폴리머는 수소결합이 형성된 관능기(Functional group)를 포함하는 폴리머이고, 상기 열처리 압착은 80 내지 200℃에서 이루어지되, 상기 열처리 압착에 의해 상기 폴리머에 포함된 상기 관능기의 수소결합(Hydrogen bond) 분해가 발생되고, 상기 관능기의 수소결합 분해를 통해 상기 금속집전체와 상기 시트가 접착되는 것을 특징으로 하는 전기이중층 커패시터용 시트전극 제조방법에 의해 달성된다. The above object is to prepare an electrode mixture by adding and mixing a polymer, active carbon, a conductive material, and a binder in a dispersion solvent, and a sheet using the electrode mixture In the method for manufacturing a sheet electrode for an electric double layer capacitor manufactured through the steps of manufacturing a manufacturing method, laminating the sheet on a metal current collector and then heat-treating and compressing the sheet, the polymer includes a functional group in which hydrogen bonds are formed. It is a polymer, and the heat treatment compression is performed at 80 to 200° C., but hydrogen bond decomposition of the functional group included in the polymer occurs by the heat treatment compression, and the hydrogen bond decomposition of the functional group through the hydrogen bond decomposition of the metal collection It is achieved by a method for manufacturing a sheet electrode for an electric double layer capacitor, characterized in that the whole and the sheet are adhered.
여기서, 상기 관능기(Functional group)는, 카복실기(Carboxylic group) 또는 하이드록시기(Hydroxy group)로 이루어진 군 및 이의 혼합물 군에서 선택된 1종이며, 상기 관능기를 포함하는 폴리머(Polymer)는, 폴리아크릴산(Polyacrylic acid), 폴리올레산(Polyoleic acid), 폴리비닐알콜(Polyvinyl alcohol), 폴리비닐아세테이트(Polyvinyl acetate), 폴리에틸렌옥사이드(Polyethylene oxide), 폴리프로필렌옥사이드(Polypropylene oixde), 폴리에틸렌글리콜(Polyethylene glycol), 폴리프로필렌글리콜(Polypropylene glycol), 디에틸아미노아세테이트(Diethylamino acetate), 폴리비닐피롤리돈(Polyvinyl pyrrolidone), 메틸셀룰로스(Methylcellulose), 에틸셀룰로스(Ethylcellulose), 히드록시메틸셀룰로스(Hydroxymethylcellulose), 히드록시에틸셀룰로스(Hydroxyethylcellulose), 히드록시에틸메틸셀룰로스(Hydroxyethylcellulose), 히드록시프로필셀룰로스(Hydroxypropylcellulose), 폴리옥시에틸렌(Polyoxyethylene), 폴리옥시에틸렌-폴리옥시프로필렌 공중합체(Polyoxyethylene-polyoxypropylene resin), 폴리비닐알콜-폴리에틸렌글리콜 공중합체(Polyvinyl alcohol-polyethylene glycol resin), 비닐피롤리돈-비닐아세테이드 공중합체(Vinylpyrrolidone-vinyl acetate resin), 스티렌말레익인컴언하이드라이드코폴리머(Styrene-maleic income anhydride copolymer)로 이루어진 군 및 이의 혼합물 군에서 선택된 1종인 것이 바람직하다.Here, the functional group is one selected from the group consisting of a carboxylic group or a hydroxyl group and mixtures thereof, and a polymer including the functional group is polyacrylic acid (Polyacrylic acid), polyoleic acid (Polyoleic acid), polyvinyl alcohol, polyvinyl acetate (Polyvinyl acetate), polyethylene oxide (Polyethylene oxide), polypropylene oxide (Polypropylene oixde), polyethylene glycol (Polyethylene glycol), Polypropylene glycol, diethylamino acetate, polyvinyl pyrrolidone, methylcellulose, ethylcellulose, hydroxymethylcellulose, hydroxyethyl Cellulose (Hydroxyethylcellulose), hydroxyethylmethylcellulose (Hydroxyethylcellulose), hydroxypropylcellulose (Hydroxypropylcellulose), polyoxyethylene (Polyoxyethylene), polyoxyethylene-polyoxypropylene copolymer (Polyoxyethylene-polyoxypropylene resin), polyvinyl alcohol-polyethylene Glycol copolymer (Polyvinyl alcohol-polyethylene glycol resin), vinylpyrrolidone-vinyl acetate resin (Vinylpyrrolidone-vinyl acetate resin), Styrene-maleic income anhydride copolymer (Styrene-maleic income anhydride copolymer) It is preferable that it is one selected from the group and mixtures thereof.
상기 도전재(Conductive material)는, 그라파이트(Graphite), 그래핀(Graphene), 소프트카본(Soft carbon), 하드카본(Hard carbon), 카본블랙(Carbon black), 탄소나노튜브(Carbon nano tube, CNT), 탄소나노섬유(Carbon nano fiber, CNF), 변형탄소(Modified carbon), 탄소복합소재(Carbon composite), 아세틸렌블랙(Acetylene black), 케천블랙(Ketjen black), 구리(Cu), 니켈(Ni), 알루미늄(Al) 또는 은(Ag)으로 이루어진 군 및 이의 혼합물 군에서 선택된 1종이며, 상기 바인더는, 폴리테트라플루오로에틸렌(Polytetrafluoroethylene), 카복시메틸셀룰로스(Carboxymethylcellulose), 폴리비닐알콜(Polyvinyl alcohol), 폴리비닐리덴플로라이드(Polyvinylidene fluoride), 폴리비닐피롤리돈(Polyvinylpyrrolidone), 메틸셀룰로오스(Methylcellulose), 에틸렌-염화비닐 공중합수지(Polyethylene-vinyl chloride resin), 염화비닐리덴 라텍스(Vinylidene chloride latex), 초산비닐수지(Polyvinyl acetate resin), 폴리비닐부티랄(Polyvinyl butyral), 비스페놀계 에폭시수지(Bisphenol A epoxy resin), 스티렌-부타디엔고무(Styrene butadiene rubber), 부타디엔고무(Butadiene rubber), 이소프렌고무(Isoprene rubber), 니트릴-부타디엔고무(Nitrilebutadiene rubber), 우레탄고무(Uretane rubber), 실리콘고무(Silicon rubber), 아크릴고무(acrylic rubber)로 이루어진 군 및 이의 혼합물 군에서 선택된 1종인 것이 바람직하며, 상기 분산용매는, 물, 증류수, 메탄올(Methanol), 에탄올(Ethanol), 프로판올(Propanol), 이소프로판올(Isopropanol), 부탄올(Butanol)로 이루어진 군 및 이의 혼합물 군에서 선택된 1종인 것이 바람직하다.The conductive material is, graphite, graphene, soft carbon, hard carbon, carbon black, carbon nanotube (CNT) ), Carbon nano fiber (CNF), Modified carbon, Carbon composite, Acetylene black, Ketjen black, Copper (Cu), Nickel (Ni) ), one selected from the group consisting of aluminum (Al) or silver (Ag) and mixtures thereof, and the binder is polytetrafluoroethylene, carboxymethylcellulose, polyvinyl alcohol ), polyvinylidene fluoride, polyvinylpyrrolidone, methylcellulose, polyethylene-vinyl chloride resin, vinylidene chloride latex , Polyvinyl acetate resin, Polyvinyl butyral, Bisphenol A epoxy resin, Styrene butadiene rubber, Butadiene rubber, isoprene rubber ( Isoprene rubber), nitrile-butadiene rubber, urethane rubber, silicone rubber, acrylic rubber, and mixtures thereof are preferably selected from the group consisting of, and the dispersion The solvent is water, distilled water, methanol (Methan ol), ethanol (Ethanol), propanol (Propanol), isopropanol (Isopropanol), butanol (Butanol) is preferably one selected from the group consisting of and mixtures thereof.
또한, 상기 전극 혼합물을 이용하여 시트를 제조하는 단계는, 상기 전극 혼합물 내의 분산용매를 증발하는 단계를 더 포함하는 데, 상기 분산용매를 증발하는 단계는 상기 분산용매 전량을 증발시키며, 상기 분산용매를 증발하는 단계 이후에, 분산용매가 증발된 상기 전극 혼합물에 상기 전극 혼합물 100중량부 대비 0.1 내지 2중량부의 분산용매를 추가하여 상기 전극 혼합물을 반죽하는 단계를 더 포함하는 것이 바람직하다.In addition, the manufacturing of the sheet using the electrode mixture further includes evaporating the dispersion solvent in the electrode mixture, wherein the evaporating the dispersion solvent evaporates the entire amount of the dispersion solvent, and the dispersion solvent After the step of evaporating, it is preferable to further include kneading the electrode mixture by adding 0.1 to 2 parts by weight of a dispersion solvent based on 100 parts by weight of the electrode mixture to the electrode mixture in which the dispersion solvent is evaporated.
상기 전극 혼합물을 이용하여 시트를 제조하는 단계 및 상기 압착하는 단계는, 각각의 단계가 상기 전극 혼합물을 가압(Pressurization), 압연(Rolling), 압출(Extrusion) 중 어느 하나의 방법을 이용하여 시트 형상으로 제조하는 것이 바람직하다.In the step of manufacturing a sheet using the electrode mixture and the pressing step, each step is a sheet shape using any one method of pressurization, rolling, and extrusion of the electrode mixture. It is preferable to manufacture with
상기 금속집전체는 표면이 에칭(Etching)된 것을 특징으로 하며, 상기 급속 집전체는, 구리(Cu), 알루미늄(Al), 백금(Pt), 금(Au), 니켈(Ni), 티타늄(Ti), 철(Fe), 몰리브덴(Mo)으로 이루어진 군 및 이의 혼합물 군에서 선택된 1종인 것이 바람직하다.The metal current collector is characterized in that the surface is etched, and the rapid current collector is copper (Cu), aluminum (Al), platinum (Pt), gold (Au), nickel (Ni), titanium ( Ti), iron (Fe), and preferably one selected from the group consisting of molybdenum (Mo) and mixtures thereof.
상기한 또 다른 목적은, 폴리머, 활성탄, 도전재 및 바인더를 갖는 전극시트와, 상기 전극시트와 열처리 압착되는 금속집전체를 포함하는전기이중층 커패시터용 시트전극에 있어서, 수소결합이 형성된 관능기(Functional group)를 포함하는 상기 폴리머는 80 내지 200℃에서 상기 시트의 압착 열처리에 의한 상기 관능기의 수소결합 분해가 발생하며, 상기 관능기의 수소결합 분해를 통해 상기 금속집전체와 상기 시트가 접착되는 것을 특징으로 하는 전기이중층 커패시터용 시트전극에 의해 달성된다.Another object is, in the sheet electrode for an electric double layer capacitor comprising an electrode sheet having a polymer, activated carbon, a conductive material and a binder, and a metal current collector that is heat-treated and compressed with the electrode sheet, a functional group in which hydrogen bonds are formed (Functional) group), hydrogen bond decomposition of the functional group occurs by compression heat treatment of the sheet at 80 to 200° C., and the metal current collector and the sheet are adhered through hydrogen bond decomposition of the functional group This is achieved by a sheet electrode for an electric double layer capacitor.
상술한 본 발명의 구성에 따르면 전기이중층 커패시터용 시트전극 및 그 제조방법은 전극시트에 존재하는 폴리머(Polymer)의 카복실기(Carboxylic group) 또는 하이드록시기(Hydroxy group) 관능기 내의 수소결합이 끊어지면서 전극시트와 금속집전체가 직접적으로 결합되는 효과를 얻을 수 있다.According to the above-described configuration of the present invention, a sheet electrode for an electric double layer capacitor and a method for manufacturing the same are performed while a hydrogen bond in a carboxylic group or a hydroxyl group functional group of a polymer present in the electrode sheet is broken. It is possible to obtain the effect that the electrode sheet and the metal current collector are directly coupled.
또한, 셀의 고온 및 고전압에서 부반응이 억제되며 우수한 전기적인 특성을 가질 수 있다.In addition, side reactions are suppressed at high temperature and high voltage of the cell, and excellent electrical properties may be obtained.
도 1은 종래기술에 따른 전기이중층 커패시터용 시트전극 제조방법의 개념도이고,
도 2는 본 발명의 실시예에 따른 전기이중층 커패시터용 시트전극의 순서도이고,
도 3은 본 발명의 실시예에 따른 전기이중층 커패시터용 시트전극의 개념도이고,
도 4는 시트전극의 단위면적당 전류에 따른 용량유지율을 나타낸 그래프이다.1 is a conceptual diagram of a method for manufacturing a sheet electrode for an electric double layer capacitor according to the prior art;
2 is a flowchart of a sheet electrode for an electric double layer capacitor according to an embodiment of the present invention;
3 is a conceptual diagram of a sheet electrode for an electric double layer capacitor according to an embodiment of the present invention;
4 is a graph showing the capacity retention rate according to the current per unit area of the sheet electrode.
이하 도면을 참조하여 본 발명의 실시예에 따른 전기이중층 커패시터용 시트전극 및 그 제조방법을 상세히 설명한다.Hereinafter, a sheet electrode for an electric double layer capacitor and a manufacturing method thereof according to an embodiment of the present invention will be described in detail with reference to the drawings.
도 2에 도시된 바와 같이 먼저, 전극 혼합물을 제조한다(S1).As shown in FIG. 2, first, an electrode mixture is prepared (S1).
전극 혼합물은 용량 발현을 위한 활성탄(Active carbon), 시트의 도전성을 증가시키기 위한 도전재(Conductive material), 전극 혼합물을 통해 시트를 제조할 때 시트 형상을 유지하기 위한 바인더(Binder) 및 수소결합이 형성된 관능기(Functional group)를 포함하는 폴리머(Polymer)를 분산용매에 투입하여 혼합한다. 이러한 전극 혼합물은 서로 균일하게 혼합되도록 1 내지 3시간 동안 충분히 교반한다.The electrode mixture has activated carbon for capacity expression, a conductive material for increasing the conductivity of the sheet, a binder for maintaining the sheet shape when manufacturing a sheet through the electrode mixture, and hydrogen bonding. A polymer including the formed functional group is added to a dispersion solvent and mixed. These electrode mixtures are sufficiently stirred for 1 to 3 hours so that they are uniformly mixed with each other.
여기서, 폴리머의 수소결합(Hydrogen bond)이 형성된 관능기는 카복실기(Carboxylic group) 또는 하이드록시기(Hydroxy group)로 이루어진 군 및 이의 혼합물 군에서 선택된 1종인 것이 바람직하며, 관능기의 수소결합 분해는 주로 폴리머의 말단에서 일어나기 때문에 말단에 관능기를 포함하는 폴리머를 사용하는 것이 바람직하다.Here, the functional group in which a hydrogen bond of the polymer is formed is preferably one selected from the group consisting of a carboxylic group or a hydroxyl group and a mixture thereof, and the hydrogen bond decomposition of the functional group is mainly Since it occurs at the end of the polymer, it is preferable to use a polymer having a functional group at the end.
이와 같이 관능기를 포함하는 폴리머는, 폴리아크릴산(Polyacrylic acid), 폴리올레산(Polyoleic acid), 폴리비닐알콜(Polyvinyl alcohol), 폴리비닐아세테이트(Polyvinyl acetate), 폴리에틸렌옥사이드(Polyethylene oxide), 폴리프로필렌옥사이드(Polypropylene oixde), 폴리에틸렌글리콜(Polyethylene glycol), 폴리프로필렌글리콜(Polypropylene glycol), 디에틸아미노아세테이트(Diethylamino acetate), 폴리비닐피롤리돈(Polyvinyl pyrrolidone), 메틸셀룰로스(Methylcellulose), 에틸셀룰로스(Ethylcellulose), 히드록시메틸셀룰로스(Hydroxymethylcellulose), 히드록시에틸셀룰로스(Hydroxyethylcellulose), 히드록시에틸메틸셀룰로스(Hydroxyethylcellulose), 히드록시프로필셀룰로스(Hydroxypropylcellulose), 폴리옥시에틸렌(Polyoxyethylene), 폴리옥시에틸렌-폴리옥시프로필렌 공중합체(Polyoxyethylene-polyoxypropylene resin), 폴리비닐알콜-폴리에틸렌글리콜 공중합체(Polyvinyl alcohol-polyethylene glycol resin), 비닐피롤리돈-비닐아세테이드 공중합체(Vinylpyrrolidone-vinyl acetate resin), 스티렌말레익인컴언하이드라이드코폴리머(Styrene-maleic income anhydride polymer)로 이루어진 군 및 이의 혼합물 군에서 선택된 1종인 것을 사용한다.As such, the polymer including a functional group is polyacrylic acid, polyoleic acid, polyvinyl alcohol, polyvinyl acetate, polyethylene oxide, polypropylene oxide ( Polypropylene oixde), polyethylene glycol, polypropylene glycol, diethylamino acetate, polyvinyl pyrrolidone, methylcellulose, ethylcellulose, Hydroxymethylcellulose, hydroxyethylcellulose, hydroxyethylmethylcellulose, hydroxypropylcellulose, polyoxyethylene, polyoxyethylene-polyoxypropylene copolymer ( Polyoxyethylene-polyoxypropylene resin), Polyvinyl alcohol-polyethylene glycol resin, Vinylpyrrolidone-vinyl acetate resin, Styrene maleic incomanhydride One selected from the group consisting of a styrene-maleic income anhydride polymer and a mixture thereof is used.
또한, 도전재는 그라파이트(Graphite), 그래핀(Graphene), 소프트카본(Soft carbon), 하드카본(Hard carbon), 카본블랙(Carbon black), 탄소나노튜브(Carbon nano tube, CNT), 탄소나노섬유(Carbon nano fiber, CNF), 변형탄소(Modified carbon), 탄소복합소재(Carbon composite), 아세틸렌블랙(Acetylene black), 케천블랙(Ketjen black), 구리(Cu), 니켈(Ni), 알루미늄(Al) 또는 은(Ag)으로 이루어진 군 및 이의 혼합물 군에서 선택된 1종인 것이 바람직하며, 바인더는 폴리테트라플루오로에틸렌(Polytetrafluoroethylene), 카복시메틸셀룰로스(Carboxymethylcellulose), 폴리비닐알콜(Polyvinyl alcohol), 폴리비닐리덴플로라이드(Polyvinylidene fluoride), 폴리비닐피롤리돈(Polyvinylpyrrolidone), 메틸셀룰로오스(Methylcellulose), 에틸렌-염화비닐 공중합수지(Polyethylene-vinyl chloride resin), 염화비닐리덴 라텍스(Vinylidene chloride latex), 초산비닐수지(Polyvinyl acetate resin), 폴리비닐부티랄(Polyvinyl butyral), 비스페놀계 에폭시수지(Bisphenol A epoxy resin), 스티렌-부타디엔고무(Styrene butadiene rubber), 부타디엔고무(Butadiene rubber), 이소프렌고무(Isoprene rubber), 니트릴-부타디엔고무(Nitrilebutadiene rubber), 우레탄고무(Uretane rubber), 실리콘고무(Silicon rubber), 아크릴고무(acrylic rubber)로 이루어진 군 및 이의 혼합물 군에서 선택된 1종인 것이 바람직하다.In addition, the conductive material is graphite, graphene, soft carbon, hard carbon, carbon black, carbon nanotube (CNT), carbon nanofiber (Carbon nano fiber, CNF), Modified carbon, Carbon composite, Acetylene black, Ketjen black, Copper (Cu), Nickel (Ni), Aluminum (Al) ) or silver (Ag) and preferably one selected from the group consisting of and mixtures thereof, and the binder is polytetrafluoroethylene, carboxymethylcellulose, polyvinyl alcohol, polyvinylidene Polyvinylidene fluoride, Polyvinylpyrrolidone, Methylcellulose, Polyethylene-vinyl chloride resin, Vinylidene chloride latex, Vinyl acetate resin ( Polyvinyl acetate resin), Polyvinyl butyral, Bisphenol A epoxy resin, Styrene butadiene rubber, Butadiene rubber, Isoprene rubber, Nitrile -Butadiene rubber (Nitrilebutadiene rubber), urethane rubber (Uretane rubber), silicone rubber (Silicon rubber), it is preferably one selected from the group consisting of acrylic rubber (acrylic rubber) and mixtures thereof.
분산용매는 수계 관능기인 카복실기 또는 하이드록시기를 포함하는 폴리머가 용이하게 분산되도록 물, 증류수, 메탄올(Methanol), 에탄올(Ethanol), 프로판올(Propanol), 이소프로판올(Isopropanol), 부탄올(Butanol)로 이루어진 군 및 이의 혼합물 군에서 선택된 1종인 것을 사용한다.The dispersion solvent consists of water, distilled water, methanol, ethanol, propanol, isopropanol, and butanol so that a polymer containing a carboxyl group or a hydroxyl group, which is a water-based functional group, is easily dispersed. One selected from the group and mixtures thereof is used.
전극 혼합물을 이용하여 시트를 제조한다(S2).A sheet is prepared using the electrode mixture (S2).
분산용매를 포함하는 전극 혼합물을 이용하여 시트를 제조하기 위해 전극 혼합물 내의 분산용매를 전량 증발시킨다. 그 후 전극 혼합물에 전극 혼합물 100중량부 대비 0.1 내지 2중량부의 분산용매를 추가하여 반죽 상태로 만든다. 이러한 반죽상태의 전극 혼합물을 골고루 반죽한다. 경우에 따라서 전극 혼합물의 분산용매를 전량을 증발시키기 않고 반죽 상태로 일부만 남도록 조절하여 증발시킨 뒤 바로 반죽을 실시할 수도 있다.In order to prepare a sheet using the electrode mixture including the dispersion solvent, the entire amount of the dispersion solvent in the electrode mixture is evaporated. Thereafter, 0.1 to 2 parts by weight of a dispersion solvent based on 100 parts by weight of the electrode mixture is added to the electrode mixture to make a dough. The electrode mixture in this kneaded state is evenly kneaded. In some cases, kneading may be performed immediately after evaporating the dispersion solvent of the electrode mixture by adjusting it so that only a part remains in a kneaded state without evaporating the entire amount.
이와 같이 반죽된 전극 혼합물 반죽은 가압(Pressurization), 압연(Rolling), 압출(Extrusion) 중 어느 하나의 방법을 이용하여 두께를 감소시켜 시트 형상으로 제조한다. 제조된 시트는 절단을 통해 원하는 크기 및 넓이를 얻을 수 있다.The electrode mixture kneaded in this way is manufactured in a sheet shape by reducing the thickness by using any one method of Pressurization, Rolling, and Extrusion. The manufactured sheet can be cut to obtain a desired size and width.
시트를 금속집전체에 적층한 후 열처리 압착한다(S3).After the sheet is laminated on the metal current collector, heat treatment is pressed (S3).
도 3에 도시된 바와 같이 S2 단계를 통해 제조된 시트를 금속집전체에 적층한 후 80 내지 120℃에서 압착 열처리한다. 수소결합인 O-H 결합이 형성된 상태에서 시트에 열처리를 하게 되면, 시트에 포함된 폴리머의 원자간 결합 중에 비교적 약한 결합에 속하는 O-H 결합이 끊어지게 되어 산소(O)와 수소(H)로 분해된다. 여기서 H는 일부 분산용매가 잔존하는 상태에서 분산용매 내의 O와 결합하거나, 공기 중에 있던 O와 결합하여 H2O 즉 물을 형성하게 된다. 수소결합 분해에 의해 형성된 소량의 물은 고체상태의 시트에 존재하는 폴리머와 닿게 되면 폴리머의 표면이 일부 녹게 된다. 이로 인해 폴리머는 점성이 있는 상태로 존재하게 되고, 이러한 폴리머에서 물이 증발하게 되면 다시 고체 상태로 되면서 말단에 H가 존재하지 않은 상태에서 옆에 존재하는 분자들과 더욱 강하게 결합을 하게 된다. 이로 인해 열처리 이전에는 개별적으로 고체 상태로 존재하던 폴리머가 주위의 분자들끼리 강하게 결합하면서 접착제 역할을 하게 되고, 이러한 폴리머가 굳어지면서 더욱 단단한 폴리머의 결합이 형성된다.As shown in FIG. 3 , the sheet prepared in step S2 is laminated on a metal current collector and then compressed and heat treated at 80 to 120° C. If the sheet is heat-treated while the OH bond, which is a hydrogen bond, is formed, the OH bond belonging to a relatively weak bond among the interatomic bonds of the polymer contained in the sheet is broken and decomposed into oxygen (O) and hydrogen (H). Here, H combines with O in the dispersion solvent in a state where some dispersion solvent remains, or combines with O in the air to form H 2 O, that is, water. When a small amount of water formed by hydrogen bond decomposition comes into contact with the polymer present in the solid sheet, the surface of the polymer is partially melted. Due to this, the polymer exists in a viscous state, and when water evaporates from the polymer, it becomes a solid state again and bonds more strongly with neighboring molecules in the absence of H at the end. Due to this, the polymer, which existed in a solid state individually before heat treatment, strongly bonds with surrounding molecules to act as an adhesive, and as the polymer hardens, a stronger polymer bond is formed.
이때 폴리머를 포함하는 시트 내의 폴리머끼리도 단단하게 결합되지만, 폴리머와 접촉하고 있던 금속기판 표면의 분자들과 폴리머도 함께 결합하여 단단하게 고정된다. 즉 이를 통해 폴리머가 존재하는 시트와, 시트와 접촉된 금속기판이 폴리머의 접착제 역할로 인해 서로 견고하게 고정된다. 이와 같은 반응은 폴리머의 단부에 수소결합이 형성된 관능기가 존재하며, 관능기의 수소결합이 분해됨에 의해 별도의 접착제를 이용하지 않고 시트와 금속기판이 서로 접착될 수 있다.At this time, the polymers in the sheet containing the polymer are also firmly bonded, but the molecules on the surface of the metal substrate in contact with the polymer and the polymer are also firmly fixed by bonding together. That is, through this, the sheet in which the polymer exists and the metal substrate in contact with the sheet are firmly fixed to each other due to the role of the polymer as an adhesive. In this reaction, a functional group in which a hydrogen bond is formed is present at the end of the polymer, and the sheet and the metal substrate can be adhered to each other without using a separate adhesive because the hydrogen bond of the functional group is decomposed.
이 상태에서 압력이 가해지면 시트와 금속집전체는 서로 접착되는데, 접착제 역할을 하는 폴리머의 말단에 수소결합이 형성된 관능기가 많을수록 접착력이 강해진다.In this state, when pressure is applied, the sheet and the metal current collector are adhered to each other, and the more functional groups in which hydrogen bonds are formed at the end of the polymer serving as an adhesive, the stronger the adhesive force.
시트와 금속집전체 간의 압착은 시트를 제조할 때와 마찬가지로 가압(Pressurization), 압연(Rolling), 압출(Extrusion) 중 어느 하나의 방법을 이용하는 것이 바람직하다.Compression between the sheet and the metal current collector is preferably performed using any one of Pressurization, Rolling, and Extrusion, as in manufacturing the sheet.
금속집전체는 구리(Cu), 알루미늄(Al), 백금(Pt), 금(Au), 니켈(Ni), 티타늄(Ti), 철(Fe), 몰리브덴(Mo)으로 이루어진 군 및 이의 혼합물 군에서 선택된 1종인 것이 바람직하다. 또한 금속집전체는 표면이 에칭(Etching)된 것을 사용하는 것이 바람직하다. 표면이 에칭되지 않고 균일한 금속집전체를 사용할 경우 시트와의 접착력이 상대적으로 약해진다. 따라서 표면이 균일하지 않도록 에칭시켜 시트의 접착력을 증가시키는 것이 바람직하다.The metal current collector is a group consisting of copper (Cu), aluminum (Al), platinum (Pt), gold (Au), nickel (Ni), titanium (Ti), iron (Fe), molybdenum (Mo), and mixtures thereof It is preferable that it is one selected from. In addition, it is preferable to use a metal current collector whose surface is etched. If the surface is not etched and a uniform metal current collector is used, the adhesion to the sheet is relatively weak. Therefore, it is preferable to increase the adhesion of the sheet by etching so that the surface is not uniform.
이와 같은 방법을 통해 제조되는 전기이중층 커패시터용 시트전극은 다음과 같은 실시예를 통해 그 효과를 확인할 수 있다.The effect of the sheet electrode for an electric double layer capacitor manufactured through this method can be confirmed through the following examples.
<비교예><Comparative example>
이소프로판올(Isopropanol) 100ml에 이소프로판올 100중량부에 대해 활성탄 85중량부, 도전재 10중량부, 바인더 5중량부를 넣고 2000rpm으로 2시간 동안 교반한다. 여기서 도전재는 카본블랙(Carbon black), 바인더는 폴리테트라플루오로에틸렌(PTFE)을 사용하였다. 이렇게 제조된 혼합물을 건조하여 이소프로판올을 전부 건조시킨 후 남은 혼합물을 이소프로판올 1ml 정도의 소량을 추가하여 반죽한다. 반죽이 끝난 후 cold roll press를 이용하여 롤 간격을 감소시키면서 압연 과정을 반복하여 150㎛ 두께의 시트를 제조하였다. 이렇게 제조되어진 시트를 금속 집전체인 에칭 알루미늄에 접착하기 위하여 도전성 페이스트(Conducting paste)를 5㎛로 도포한 뒤 시트를 표면에 부착하고, 120℃의 hot roll press기를 통해 가압하여 시트전극을 제조하였다.In 100 ml of isopropanol, 85 parts by weight of activated carbon, 10 parts by weight of a conductive material, and 5 parts by weight of a binder based on 100 parts by weight of isopropanol, and stirring at 2000 rpm for 2 hours. Here, carbon black was used as the conductive material, and polytetrafluoroethylene (PTFE) was used as the binder. The mixture thus prepared is dried to dry all isopropanol, and the remaining mixture is kneaded by adding a small amount of about 1 ml of isopropanol. After kneading, the rolling process was repeated while reducing the roll gap using a cold roll press to manufacture a 150 μm thick sheet. In order to adhere the thus-prepared sheet to the etched aluminum, which is a metal current collector, a conductive paste was applied at a thickness of 5 μm, the sheet was attached to the surface, and the sheet was pressed through a hot roll press at 120° C. to prepare a sheet electrode. .
<실시예 1><Example 1>
분산용매인 이소프로판올 100ml에 이소프로판올 100중량부에 대해 활성탄 85중량부, 도전재 10중량부, 바인더 4중량부, 관능기를 포함하는 폴리머 1중량부를 넣고 2000rpm으로 2시간 교반하였다. 여기서 도전재는 카본블랙, 바인더는 PTFE, 관능기를 포함하는 폴리머는 폴리아크릴산(PAA)을 사용하였다.In 100 ml of isopropanol, a dispersion solvent, 85 parts by weight of activated carbon, 10 parts by weight of a conductive material, 4 parts by weight of a binder, and 1 part by weight of a polymer including a functional group with respect to 100 parts by weight of isopropanol were added and stirred at 2000 rpm for 2 hours. Here, carbon black was used as a conductive material, PTFE as a binder, and polyacrylic acid (PAA) as a polymer containing a functional group.
이렇게 제조되어진 전극혼합물을 건조하여 분산용매를 전부 건조시킨 후, 남은 전극혼합물에 이소프로판올 1ml를 추가하여 반죽한다. 반죽이 끝난 후 비교예와 동일하게 cold roll press를 이용하여 롤 간격을 감소시키면서 압연 과정을 반복하여 150㎛ 두께의 시트를 제조하였다. 이렇게 제조되어진 시트를 금속 집전체인 에칭 알루미늄에 접착하기 위하여 120℃의 hot roll press기를 통해 가압하여 시트전극을 제조하였다.After drying the thus-prepared electrode mixture to dry all of the dispersion solvent, 1 ml of isopropanol is added to the remaining electrode mixture and kneaded. After the kneading was completed, the rolling process was repeated while reducing the roll interval using a cold roll press in the same manner as in Comparative Example to prepare a sheet having a thickness of 150 μm. In order to adhere the thus-prepared sheet to the etched aluminum, which is a metal current collector, it was pressed through a hot roll press at 120° C. to prepare a sheet electrode.
<실시예 2><Example 2>
분산용매인 이소프로판올 100ml에 이소프로판올 100중량부에 대해 활성탄 85중량부, 도전재 10중량부, 바인더 4중량부, 관능기를 포함하는 폴리머 1중량부를 넣고 2000rpm으로 2시간 교반하였다. 여기서 도전재는 카본블랙, 바인더는 PTFE, 관능기를 포함하는 폴리머는 폴리비닐알콜(PVA)을 사용하였다.In 100 ml of isopropanol, a dispersion solvent, 85 parts by weight of activated carbon, 10 parts by weight of a conductive material, 4 parts by weight of a binder, and 1 part by weight of a polymer including a functional group with respect to 100 parts by weight of isopropanol were added and stirred at 2000 rpm for 2 hours. Here, carbon black was used as a conductive material, PTFE as a binder, and polyvinyl alcohol (PVA) as a polymer containing a functional group.
이렇게 제조되어진 전극혼합물을 건조하여 분산용매를 전부 건조시킨 후, 남은 전극혼합물에 이소프로판올 1ml를 추가하여 반죽한다. 반죽이 끝난 후 비교예와 동일하게 cold roll press를 이용하여 롤 간격을 감소시키면서 압연 과정을 반복하여 150㎛ 두께의 시트를 제조하였다. 이렇게 제조되어진 시트를 금속 집전체인 에칭 알루미늄에 접착하기 위하여 120℃의 hot roll press기를 통해 가압하여 시트전극을 제조하였다.After drying the thus-prepared electrode mixture to dry all of the dispersion solvent, 1 ml of isopropanol is added to the remaining electrode mixture and kneaded. After the kneading was completed, the rolling process was repeated while reducing the roll interval using a cold roll press in the same manner as in Comparative Example to prepare a sheet having a thickness of 150 μm. In order to adhere the thus-prepared sheet to the etched aluminum, which is a metal current collector, it was pressed through a hot roll press at 120° C. to prepare a sheet electrode.
<셀 제조><Cell Manufacturing>
제조되어진 각각의 시트전극의 크기를 2×2㎠으로 재단하고, 전극이 코팅되지 않은 에칭 알루미늄 집전체의 한쪽 끝 면은 길이방향으로 길게 재단하여 단자로서 활용하였다.The size of each prepared sheet electrode was cut to 2×2 cm 2 , and one end surface of the etched aluminum current collector on which the electrode was not coated was cut lengthwise in the longitudinal direction to be used as a terminal.
전극, 분리막(celgard 3501) 및 3면이 밀폐된 라미네이트 폴리머 파우치 필름을 이용하여 활성탄소전극-분리막-활성탄소전극의 순서로 겹쳐 쌓은 후 폴리머 파우치에 집어 넣고, 진공 감압 및 가압이 가능한 전해액 주입기에서 1.0M TEABF4가 용해되어 있는 폴리카보네이트(PC)계 공용매 전해액을 함침하고 진공 실링(Sealing)하여 셀을 제조하였다.Using an electrode, a separator (celgard 3501) and a laminated polymer pouch film sealed on three sides, stack the activated carbon electrode-separator-activated carbon electrode in the order, put it in the polymer pouch, and in an electrolyte injector that can vacuum depressurize and pressurize A cell was prepared by impregnating a polycarbonate (PC)-based cosolvent electrolyte in which 1.0M TEABF4 was dissolved and vacuum sealing.
<용량유지율><Capacity maintenance rate>
율특성은 충방전 시험기(MACCOR, 모델명 Series 4000)에서 정전류법으로 충전과 방전을 행하였다. 구동전압은 0 내지 2.5V에서, 인가 전류밀도는 0.1 내지 100mA/㎠의 조건으로 3cycle씩 측정하였다. 수퍼커패시터의 정전용량은 3번째의 정전류 방전에서의 시간-전압 곡선에서 아래의 식에 의해 계산하였다.For rate characteristics, charging and discharging were performed using a constant current method in a charge/discharge tester (MACCOR, model name Series 4000). The driving voltage was 0 to 2.5V, and the applied current density was measured for 3 cycles at a condition of 0.1 to 100mA/cm 2 . The capacitance of the supercapacitor was calculated by the following equation from the time-voltage curve in the third constant current discharge.
C(정전용량, F) = dt·I/dvC (capacitance, F) = dt I/dv
이와 같은 실험을 통해 얻어진 값은 다음과 같은 도 4에서 확인할 수 있다. 도 4는 3cycle 마다 단위면적당 전류를 상승시켜 용량유지율을 파악한 것을 나타낸 그래프이다. 단위면적당 전류를 0.1mA/㎠ 에서 100mA/㎠까지 3cycle씩 측정한 것으로 관능기를 포함하는 폴리머를 혼합하지 않은 비교예는 단위면적당 전류가 증가할 수록 용량유지율 감소 폭이 크며, 실시예 1 및 2는 비교예에 비해 감소 폭이 작은 것을 확인할 수 있다. 최종적으로 100mA/㎠에서 비교예의 용량유지율은 72.9% 이지만 실시예1 및 2는 각각 89.4% 및 84.7%로 비교예보다 용량유지율이 우수한 것을 확인할 수 있다. 즉 전기이중층 커패시터 셀로써 출력특성이 우수하다는 것을 증명할 수 있다.The value obtained through such an experiment can be confirmed in FIG. 4 as follows. 4 is a graph showing that the capacity retention rate is grasped by increasing the current per unit area every 3 cycles. The current per unit area was measured by 3 cycles from 0.1 mA/cm 2 to 100 mA/cm 2 , and in Comparative Examples without mixing a polymer including a functional group, the decrease in capacity retention rate increased as the current per unit area increased, Examples 1 and 2 It can be seen that the reduction width is smaller than that of the comparative example. Finally, at 100 mA/cm 2 , the capacity retention rate of the comparative example was 72.9%, but Examples 1 and 2 were 89.4% and 84.7%, respectively, confirming that the capacity retention rate was superior to that of the comparative example. That is, it can be proved that the output characteristics are excellent as an electric double layer capacitor cell.
종래의 시트전극은 금속집전체와 전극이 페이스트에 의해 접착되어 있기 때문에 셀에 온도 또는 높은 전압이 인가되게 되면 도 4와 같이 페이스트 영역에서 분해 반응과 크랙이 발생하게 된다. 하지만 본 발명에 따른 전기이중층 커패시터용 시트전극은 시트에 존재하는 폴리머(Polymer)의 카복실기(Carboxylic group) 또는 하이드록시기(Hydroxy group) 관능기 내의 수소결합이 끊어지면서 전극시트와 금속집전체가 직접적으로 결합되는 효과를 얻을 수 있다. 또한, 셀의 고온 및 고전압에서 크랙(Crack) 등과 같은 부반응이 억제되며 우수한 전기적인 특성을 가질 수 있다.In the conventional sheet electrode, since the metal current collector and the electrode are bonded by the paste, when a temperature or a high voltage is applied to the cell, a decomposition reaction and cracks occur in the paste region as shown in FIG. 4 . However, in the sheet electrode for an electric double layer capacitor according to the present invention, as the hydrogen bond in the carboxylic group or hydroxyl group functional group of the polymer present in the sheet is broken, the electrode sheet and the metal current collector are directly connected to each other. combined effect can be obtained. In addition, side reactions such as cracks are suppressed at high temperature and high voltage of the cell, and excellent electrical properties may be obtained.
Claims (12)
분산용매에 활성탄(Active carbon), 도전재(Conductive material), 폴리머(Polymer) 및 바인더(Binder)를 투입 및 혼합하여 전극 혼합물을 제조하는 단계;
상기 전극 혼합물을 이용하여 시트를 제조하는 단계; 및
상기 시트를 금속집전체에 적층한 후 열처리 압착하는 단계;를 포함하고,
상기 전극 혼합물을 제조하는 단계에 있어서, 상기 분산용매, 활성탄(Active carbon), 도전재(Conductive material), 바인더(Binder) 및 폴리머(Polymer)의 비율은 100 : 85 : 10 : 4 : 1 중량비 비율로 포함되어 1~3시간 혼합되며,
상기 폴리머는 카복실기 또는 하이드록시기를 갖는 폴리아크릴산(PAA)으로 수소결합에 의하여 상기 금속집전체와 상기 시트가 도전성 접착제 없이 온도 80~120℃ 열압착에 의하여 부착됨에 따라 전류밀도 100mA/㎠에서 용량유지율이 89.4%를 갖는 것을 특징으로 하는 전기이중층 커패시터용 시트전극 제조방법.A method for manufacturing a sheet electrode for an electric double layer capacitor, the method comprising:
preparing an electrode mixture by adding and mixing active carbon, a conductive material, a polymer, and a binder in a dispersion solvent;
manufacturing a sheet using the electrode mixture; and
Including; laminating the sheet on a metal current collector and then heat-treating and compressing the sheet;
In the step of preparing the electrode mixture, the ratio of the dispersion solvent, active carbon, conductive material, binder, and polymer is 100: 85: 10: 4: 1 by weight ratio is included and mixed for 1 to 3 hours,
The polymer is polyacrylic acid (PAA) having a carboxyl group or a hydroxyl group. As the metal current collector and the sheet are attached by thermocompression bonding at a temperature of 80 to 120° C. without a conductive adhesive by hydrogen bonding, the capacity at a current density of 100 mA/cm 2 A method for manufacturing a sheet electrode for an electric double layer capacitor, characterized in that the retention rate is 89.4%.
상기 도전재(Conductive material)는,
그라파이트(Graphite), 그래핀(Graphene), 소프트카본(Soft carbon), 하드카본(Hard carbon), 카본블랙(Carbon black), 탄소나노튜브(Carbon nano tube, CNT), 탄소나노섬유(Carbon nano fiber, CNF), 변형탄소(Modified carbon), 탄소복합소재(Carbon composite), 아세틸렌블랙(Acetylene black), 케천블랙(Ketjen black), 구리(Cu), 니켈(Ni), 알루미늄(Al) 또는 은(Ag)으로 이루어진 군 및 이의 혼합물 군에서 선택된 1종인 것을 특징으로 하는 전기이중층 커패시터용 시트전극 제조방법.The method of claim 1,
The conductive material is
Graphite, graphene, soft carbon, hard carbon, carbon black, carbon nano tube (CNT), carbon nano fiber , CNF), modified carbon, carbon composite, acetylene black, Ketjen black, copper (Cu), nickel (Ni), aluminum (Al) or silver ( A method for manufacturing a sheet electrode for an electric double layer capacitor, characterized in that it is one selected from the group consisting of Ag) and mixtures thereof.
상기 바인더는,
폴리테트라플루오로에틸렌(Polytetrafluoroethylene), 카복시메틸셀룰로스(Carboxymethylcellulose), 폴리비닐알콜(Polyvinyl alcohol), 폴리비닐리덴플로라이드(Polyvinylidene fluoride), 폴리비닐피롤리돈(Polyvinylpyrrolidone), 메틸셀룰로오스(Methylcellulose), 에틸렌-염화비닐 공중합수지(Polyethylene-vinyl chloride resin), 염화비닐리덴 라텍스(Vinylidene chloride latex), 초산비닐수지(Polyvinyl acetate resin), 폴리비닐부티랄(Polyvinyl butyral), 비스페놀계 에폭시수지(Bisphenol A epoxy resin), 스티렌-부타디엔고무(Styrene butadiene rubber), 부타디엔고무(Butadiene rubber), 이소프렌고무(Isoprene rubber), 니트릴-부타디엔고무(Nitrilebutadiene rubber), 우레탄고무(Uretane rubber), 실리콘고무(Silicon rubber), 아크릴고무(acrylic rubber)로 이루어진 군 및 이의 혼합물 군에서 선택된 1종인 것을 특징으로 하는 전기이중층 커패시터용 시트전극 제조방법.The method of claim 1,
The binder is
Polytetrafluoroethylene, carboxymethylcellulose, polyvinyl alcohol, polyvinylidene fluoride, polyvinylpyrrolidone, methylcellulose, ethylene -Polyethylene-vinyl chloride resin, vinylidene chloride latex, polyvinyl acetate resin, polyvinyl butyral, bisphenol A epoxy resin ), styrene-butadiene rubber, butadiene rubber, isoprene rubber, nitrile-butadiene rubber, urethane rubber, silicone rubber, acrylic A method for manufacturing a sheet electrode for an electric double layer capacitor, characterized in that it is one selected from the group consisting of acrylic rubber and mixtures thereof.
상기 분산용매는,
물, 증류수, 메탄올(Methanol), 에탄올(Ethanol), 프로판올(Propanol), 이소프로판올(Isopropanol), 부탄올(Butanol)로 이루어진 군 및 이의 혼합물 군에서 선택된 1종인 것을 특징으로 하는 전기이중층 커패시터용 시트전극 제조방법.The method of claim 1,
The dispersion solvent is
Manufacturing a sheet electrode for an electric double layer capacitor, characterized in that it is one selected from the group consisting of water, distilled water, methanol, ethanol, propanol, isopropanol, butanol, and mixtures thereof Way.
상기 전극 혼합물을 이용하여 시트를 제조하는 단계는,
상기 전극 혼합물 내의 분산용매를 증발하는 단계를 더 포함하는 것을 특징으로 하는 전기이중층 커패시터용 시트전극 제조방법.The method of claim 1,
The step of preparing a sheet using the electrode mixture,
The method for manufacturing a sheet electrode for an electric double layer capacitor, characterized in that it further comprises the step of evaporating the dispersion solvent in the electrode mixture.
상기 분산용매를 증발하는 단계는 상기 분산용매 전량을 증발시키며,
상기 분산용매를 증발하는 단계 이후에, 분산용매가 증발된 상기 전극 혼합물에 상기 전극 혼합물 100중량부 대비 0.1 내지 2중량부의 분산용매를 추가하여 상기 전극 혼합물을 반죽하는 단계를 더 포함하는 것을 특징으로 하는 전기이중층 커패시터용 시트전극 제조방법.8. The method of claim 7,
The step of evaporating the dispersion solvent evaporates the entire amount of the dispersion solvent,
After evaporating the dispersion solvent, adding 0.1 to 2 parts by weight of a dispersion solvent based on 100 parts by weight of the electrode mixture to the electrode mixture in which the dispersion solvent is evaporated, further comprising the step of kneading the electrode mixture A method for manufacturing a sheet electrode for an electric double layer capacitor.
상기 전극 혼합물을 이용하여 시트를 제조하는 단계 및 상기 압착하는 단계는,
각각의 단계가 상기 전극 혼합물을 가압(Pressurization), 압연(Rolling), 압출(Extrusion) 중 어느 하나의 방법을 이용하여 시트 형상으로 제조하는 것을 특징으로 하는 전기이중층 커패시터용 시트전극 제조방법.The method of claim 1,
The step of manufacturing a sheet using the electrode mixture and the pressing step,
Each step is a method of manufacturing a sheet electrode for an electric double-layer capacitor, characterized in that the electrode mixture is manufactured in a sheet shape using any one method of pressurization, rolling, and extrusion.
상기 금속집전체는 표면이 에칭(Etching)된 것을 특징으로 하는 전기이중층 커패시터용 시트전극 제조방법.The method of claim 1,
The method for manufacturing a sheet electrode for an electric double layer capacitor, characterized in that the surface of the metal current collector is etched.
상기 금속집전체는 구리(Cu), 알루미늄(Al), 백금(Pt), 금(Au), 니켈(Ni), 티타늄(Ti), 철(Fe), 몰리브덴(Mo)으로 이루어진 군 및 이의 혼합물 군에서 선택된 1종인 것을 특징으로 하는 전기이중층 커패시터용 시트전극 제조방법.The method of claim 1,
The metal current collector is a group consisting of copper (Cu), aluminum (Al), platinum (Pt), gold (Au), nickel (Ni), titanium (Ti), iron (Fe), molybdenum (Mo), and mixtures thereof A method for manufacturing a sheet electrode for an electric double layer capacitor, characterized in that it is one selected from the group.
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| JPH03165458A (en) * | 1989-11-24 | 1991-07-17 | Yuasa Battery Co Ltd | Positive electrode for battery |
| KR100542804B1 (en) * | 2003-05-26 | 2006-01-20 | 한국전기연구원 | Method for manufacturing electrode of high generating power type electric double layer capacitor |
| KR100581230B1 (en) * | 2003-12-12 | 2006-06-19 | (주)에스와이하이테크 | Electric Double Layer Capacitor and manufacturing method of sheet type electrode for EDLC |
| KR101198297B1 (en) * | 2011-04-12 | 2012-11-07 | 한국전기연구원 | Sheet Electrode Of Carbon-PolyTetraFluoroEthylene-Hydrophilic Binder For Electric Double Layer Capacitor And Manufacturing Method thereof |
| KR20130104013A (en) * | 2012-03-12 | 2013-09-25 | 한국세라믹기술원 | Electrode material containing mixture of substituted polyacrylates as binder and lithium secondary battery using the same |
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- 2015-09-21 KR KR1020150132899A patent/KR102398468B1/en active IP Right Grant
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