JP2012182263A - Electrode for electric double-layer capacitor and electric double-layer capacitor - Google Patents

Electrode for electric double-layer capacitor and electric double-layer capacitor Download PDF

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JP2012182263A
JP2012182263A JP2011043450A JP2011043450A JP2012182263A JP 2012182263 A JP2012182263 A JP 2012182263A JP 2011043450 A JP2011043450 A JP 2011043450A JP 2011043450 A JP2011043450 A JP 2011043450A JP 2012182263 A JP2012182263 A JP 2012182263A
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electric double
layer capacitor
electrode
polarizable electrode
moisture
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Toshihiro Nakabo
年宏 中坊
Yoshihisa Tanaka
義久 田中
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Nissin Electric Co Ltd
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Abstract

PROBLEM TO BE SOLVED: To provide a polarizable electrode that prevents moisture from entering into an electric double-layer capacitor, which has an adverse effect on the electric double-layer capacitor such as deterioration of long-term performance, and to provide the electric double-layer capacitor.SOLUTION: The polarizable electrode 24 of the electric double-layer capacitor has a moisture adsorbing layer 25 laminated on an upper layer of the polarizable electrode 24. A moisture adsorbing agent constituting the moisture adsorbing layer 25 is a moisture adsorbing material with a bore diameter of 0.4 nm or less and a particle diameter of 10 μm or less, and formed by subjecting the moisture adsorbing material to activation treatment at a temperature of 300°C or higher, then slurrying the material by using an organic solvent and an organic-solvent-based binder; and applying the slurry on the polarizable electrode 24 and drying the slurry.

Description

本発明は分極性電極を有する電気二重層キャパシタ用電極の構造とその電極を用いた電気二重層キャパシタに関する。   The present invention relates to an electrode structure for an electric double layer capacitor having a polarizable electrode and an electric double layer capacitor using the electrode.

電気二重層キャパシタで有機系の電解液を用いたものの代表的なものに筒型のセルがある。   A typical example of an electric double layer capacitor using an organic electrolyte is a cylindrical cell.

この筒型の代表的な構造を図２に示す。
正極となる複数枚のシート状の分極性電極１と負極となる複数枚のシート状の分極性電極２はセパレータ３を介在させた状態で、交互に積層され、電解液４を含浸させた状態で、筒形の金属製のケース５内に収容されている。
なお、分極性電極１、２は活性炭を主成分としたカーボンブラックの微粉やバインダを混合してシ−ト状に形成された活性炭シートをアルミ箔製の集電体に接着させて構成されている。 A typical structure of this cylindrical shape is shown in FIG.
A plurality of sheet-shaped polarizable electrodes 1 serving as positive electrodes and a plurality of sheet-shaped polarizable electrodes 2 serving as negative electrodes are alternately stacked with a separator 3 interposed therebetween and impregnated with an electrolytic solution 4 Thus, it is housed in a cylindrical metal case 5.
The polarizable electrodes 1 and 2 are formed by adhering an activated carbon sheet formed in a sheet shape by mixing carbon black fine powder or binder mainly composed of activated carbon to an aluminum foil current collector. Yes.

そして、前記各分極性電極１はリード線６に、各分極性電極２はリード線７にそれぞれ接続され、それらリード線６及び７が、合成樹脂製の端子台８に設けられた正極端子９及び負極端子１０にそれぞれ接続されている。
また、端子台８にはケース５内の内部圧力が増大すると開く圧力放出弁１２が取り付かられている。 Each polarizable electrode 1 is connected to a lead wire 6, each polarizable electrode 2 is connected to a lead wire 7, and the lead wires 6 and 7 are connected to a terminal block 8 made of synthetic resin. And the negative terminal 10 are respectively connected.
The terminal block 8 is provided with a pressure release valve 12 that opens when the internal pressure in the case 5 increases.

前記分極性電極１，２等は、真空加熱乾燥機により乾燥された後、真空チャンバー内に収納され、そのチャンバー内が真空にされた後に高純度の窒素ガス雰囲気とされ、その中でケース１１内に組付けられ、更に電解液４が注入され、端子台８が取付けられるようになっている。なお、この場合、前記電解液４としては有機系電解液、例えば溶媒としてのプロピレンカーボネート（ＰＣ）に、電解質としてのテトラエチルアンモニウム・テトラフルオロボレート（Ｅｔ４ＮＢＦ４）を溶解したものが用いられる。 The polarizable electrodes 1, 2 and the like are dried by a vacuum heat dryer and then housed in a vacuum chamber. After the chamber is evacuated, a high-purity nitrogen gas atmosphere is formed. The terminal block 8 is attached by injecting the electrolytic solution 4 therein. In this case, as the electrolytic solution 4, an organic electrolytic solution, for example, a solution obtained by dissolving tetraethylammonium tetrafluoroborate (Et 4 NBF 4 ) as an electrolyte in propylene carbonate (PC) as a solvent is used.

上記分極性電極１，２の材質としては、粒径２０〜３０μｍの活性炭粉末に、粒径数μｍのメソカーボンを混合して、焼結成形したものが知られている（例えば特許文献１参照）。活性炭は、その表面に、０．１ｎｍ〜１００ｎｍと非常に小さい無数のポアと呼ぶ穴が存在するため、２０００〜３０００ｍ２／ｇもの広い表面積を有している。電気二重層キャパシタは、この膨大な比表面積を利用して、従来のコンデンサには見られない大きな静電容量を得ている。 As a material of the polarizable electrodes 1 and 2, a material obtained by mixing and molding a mesocarbon having a particle size of several μm with activated carbon powder having a particle size of 20 to 30 μm is known (for example, see Patent Document 1). ). Activated carbon has a surface area as wide as 2000 to 3000 m 2 / g because there are numerous pores called innumerable pores of 0.1 to 100 nm on the surface. The electric double layer capacitor utilizes this enormous specific surface area to obtain a large capacitance not found in conventional capacitors.

しかし、上記分極性電極１，２を構成する活性炭のポアは、環境中に存在する水蒸気やガスなども吸着してしまうことがあり、またそのような活性炭による吸着以外にも、いくつかの要因で電気二重層キャパシタ内に水（水蒸気）が供給されてしまう問題がある。この水の混入が、電気二重層キャパシタの寿命を著しく低下させる（劣化により静電容量が短期間で低下する）ことが、明らかとなっている。   However, the pores of the activated carbon constituting the polarizable electrodes 1 and 2 may adsorb water vapor and gas existing in the environment, and there are several factors other than the adsorption by the activated carbon. Thus, there is a problem that water (water vapor) is supplied into the electric double layer capacitor. It is clear that this mixing of water significantly reduces the life of the electric double layer capacitor (capacitance decreases in a short period due to deterioration).

以上のような活性炭の水分吸着等の問題を解決するため、特許文献２では吸着剤（モレキュラシ−ブ４A等）をセパレータやその他セル内の部品に混合することが開示されている。   In order to solve the problems such as moisture adsorption of activated carbon as described above, Patent Document 2 discloses mixing an adsorbent (such as molecular sieve 4A) with a separator or other components in the cell.

特開平０３−２０１５１６号公報Japanese Patent Laid-Open No. 03-201516 特開２００４−１９３２５１号公報JP 2004-193251 A

ところが、上記特許文献２において用いられる吸着剤によると、吸着剤の使用段階において、既に水分を吸着した状態にあり、水分吸着性能はあまり高くないと考えられる。さらに、吸着剤をセパレータや分極性電極内に混合する工程で、水を分散媒として用いているため、折角の吸着剤の吸着性能が著しく低下するという問題がある。   However, according to the adsorbent used in the above-mentioned Patent Document 2, it is considered that moisture is already adsorbed in the use stage of the adsorbent, and the moisture adsorption performance is not so high. Furthermore, since water is used as a dispersion medium in the step of mixing the adsorbent into the separator or polarizable electrode, there is a problem that the adsorption performance of the corner adsorbent is significantly reduced.

従って、本発明は上記電気二重層キャパシタ内における水分による悪影響をさらになくすキャパシタ用電極及びそれを用いた電気二重層キャパシタを提供することを目的とする。   Accordingly, an object of the present invention is to provide an electrode for a capacitor that further eliminates the adverse effects of moisture in the electric double layer capacitor and an electric double layer capacitor using the same.

以上の課題に鑑み、本発明は、分極性電極を有する電気二重層キャパシタ用電極において、前記分極性電極の上層に水分吸着層を積層することを特徴としている。   In view of the above problems, the present invention is characterized in that, in an electrode for an electric double layer capacitor having a polarizable electrode, a moisture adsorption layer is laminated on the polarizable electrode.

また、より具体的には、前記分極性電極の上層に積層する水分吸着層を構成する水分吸着剤は、孔径0.4ｎｍ以下、粒径μｍ以下の水分吸着材料であり、該水分吸着材料を３００℃以上の温度で活性化処理した後、有機溶剤及び有機溶剤系バインダによりスラリーとし、該スラリーを前記分極性電極上に塗布、乾燥して形成されてなることを特徴としている。   More specifically, the moisture adsorbent constituting the moisture adsorption layer laminated on the polarizable electrode is a moisture adsorption material having a pore size of 0.4 nm or less and a particle size of μm or less. After the activation treatment at a temperature of not lower than ° C., a slurry is formed with an organic solvent and an organic solvent binder, and the slurry is formed on the polarizable electrode and dried.

また、以上の電気二重層キャパシタ用電極を用いた電気二重層キャパシタであることを特徴としている。   Further, the present invention is characterized by being an electric double layer capacitor using the above electrode for electric double layer capacitor.

なお、上記した水分吸着剤としては、モレキュラーシーブ（商品名）〔Ａ型ゼオライト〕等を採用することができる。   In addition, as the above-described moisture adsorbent, molecular sieve (trade name) [A-type zeolite] or the like can be employed.

本発明によると、水分吸着材料を活性化処理した後、有機溶剤及び有機溶剤系バインダによりスラリーとして、水分吸着剤を作製し、分極性電極上に塗布、乾燥するので、水との接触がほとんどなく、したがって、水分吸着能が高い状態を保持したまま分極性電極上に水分吸着層を積層できる。
また、分極性電極を構成する活性炭に水分（水蒸気）などが吸着することがないので、電気二重層キャパシタの寿命が著しく低下することを抑制することができる。 According to the present invention, after the moisture adsorbing material is activated, the moisture adsorbent is prepared as a slurry with an organic solvent and an organic solvent-based binder, applied onto the polarizable electrode, and dried, so that there is almost no contact with water. Therefore, a moisture adsorption layer can be laminated on the polarizable electrode while maintaining a high moisture adsorption capacity.
In addition, since moisture (water vapor) or the like is not adsorbed on the activated carbon constituting the polarizable electrode, it is possible to suppress the life of the electric double layer capacitor from being significantly reduced.

本発明に係る電気二重層キャパシタ用電極の概略図である。It is the schematic of the electrode for electric double layer capacitors which concerns on this invention. 従来の電気二重層キャパシタの概略図である。It is the schematic of the conventional electric double layer capacitor.

本発明の実施の形態について添付の図に基づいて説明する。
１．電気二重層キャパシタ用電極
図１は本発明に係る電気二重層キャパシタ用電極の概略図を示す。 Embodiments of the present invention will be described with reference to the accompanying drawings.
1. Electric Double Layer Capacitor Electrode FIG. 1 shows a schematic diagram of an electric double layer capacitor electrode according to the present invention.

本発明の電気二重層キャパシタ用電極２１はアルミ箔製の集電体２２上にスラリー状の活性炭を塗布した活性炭層２３からなる分極性電極２４の活性炭層２３上に塗布した水分吸着剤を主成分とする水分吸着層２５から構成されている。   The electrode 21 for an electric double layer capacitor of the present invention is mainly composed of a moisture adsorbent coated on the activated carbon layer 23 of the polarizable electrode 24 composed of the activated carbon layer 23 coated with slurry activated carbon on a current collector 22 made of aluminum foil. It is composed of a moisture adsorption layer 25 as a component.

前記水分吸着剤は孔径0.4ｎｍ以下、粒径１０μｍ以下の水分吸着材料であり、例えばモレキュラーシーブ（Ａ型ゼオライト）である。   The moisture adsorbent is a moisture adsorbing material having a pore size of 0.4 nm or less and a particle size of 10 μm or less, such as molecular sieve (A-type zeolite).

前記電気二重層キャパシタ用電極２１の作製方法としては、水分吸着材料を３００℃以上の温度で活性化処理した後、有機溶剤及び有機溶剤系バインダによりスラリーとし、該スラリーを前記分極性電極２４上に塗布、乾燥して作製する。   As a method for producing the electric double layer capacitor electrode 21, after the moisture adsorbing material is activated at a temperature of 300 ° C. or higher, it is made into a slurry with an organic solvent and an organic solvent binder, and the slurry is formed on the polarizable electrode 24. It is prepared by coating and drying.

なお、乾燥の過程で、有機溶剤系バインダに対して貧溶媒であるアルコール（プロパノールやブタノール）等に浸漬し、水分吸着層を多孔質にしてもよい。   In the course of drying, the moisture adsorbing layer may be made porous by immersing it in alcohol (propanol or butanol) which is a poor solvent with respect to the organic solvent binder.

以下、水分吸着層を有する場合と有しない場合の電気二重層キャパシタ電極およびそれを用いた電気二重層キャパシタの作製方法及び性能試験結果について説明する。   Hereinafter, an electric double layer capacitor electrode with and without a moisture adsorption layer, an electric double layer capacitor manufacturing method using the electrode, and a performance test result will be described.

（実施例１）
（１）分極性電極の作製
ヤシガラ活性炭１００重量部、アセチレンブラック５重量部、カルボキシメチルセルロース及びスチレンブタジエンゴムのそれぞれ３重量部を適量の蒸留水で分散混合した分散液の3種類を混合したスラリーを、電解エッチングを施したアルミ箔集電体２２上に塗布乾燥し、厚さ50μｍの分極性電極２４を作製した。 Example 1
(1) Production of polarizable electrode A slurry prepared by mixing three kinds of dispersions in which 100 parts by weight of coconut husk activated carbon, 5 parts by weight of acetylene black, 3 parts by weight of carboxymethyl cellulose and styrene butadiene rubber were dispersed and mixed with an appropriate amount of distilled water. The aluminum foil current collector 22 subjected to electrolytic etching was applied and dried to prepare a polarizable electrode 24 having a thickness of 50 μm.

（２）水分吸着層の形成
粉末状（粒径１０μｍ以下）のモレキュラーシーブ３Ａを３００℃にて8時間熱処理し、窒素雰囲気下で冷却した後、ｎ-メチルピロドロン（ＮＭＰ）にポリビニリデンフルオイド（ＰＶＤＦ）を溶解させた溶液と混合し、有機溶剤系のスラリーを作製した後、前記分極性電極２４上に塗布し、厚み３０μｍの水分吸着層２５を形成した。 (2) Formation of moisture adsorption layer The molecular sieve 3A in powder form (particle size of 10 μm or less) was heat-treated at 300 ° C. for 8 hours, cooled in a nitrogen atmosphere, and then into polyvinylideneful in n-methylpyrodrone (NMP). After mixing with a solution in which Euid (PVDF) was dissolved to prepare an organic solvent-based slurry, the slurry was applied on the polarizable electrode 24 to form a moisture adsorption layer 25 having a thickness of 30 μm.

（３）電気二重層キャパシタセルの作製
前記分極性電極２４上に前記水分吸着層２５を積層した電気二重層キャパシタ用電極２１を２枚対抗させ、市販のセルロース製セパレータを挟んで積層し、引き出し用の外部電極を取り付けた後、アルミラミネートパックし、電解液としてトリエチルメチルアンモニウムテトラフルオロボートをプロピレンカーボネート溶媒に溶解させたもの（ＴＥＭＡ・ＢＦ４／ＰＣ）を注液し、封止して電気二重層キャパシタセルを製作した。 (3) Production of an electric double layer capacitor cell Two electric double layer capacitor electrodes 21 each having the moisture adsorbing layer 25 laminated on the polarizable electrode 24 are opposed to each other, laminated with a commercially available cellulose separator interposed therebetween, and drawn. After mounting the external electrode, aluminum laminate pack was prepared, and an electrolyte solution prepared by dissolving triethylmethylammonium tetrafluoroboat in propylene carbonate solvent (TEMA / BF4 / PC) was injected, sealed, and sealed. A multilayer capacitor cell was manufactured.

（比較例１）
実施例１と同様な方法で分極性電極２４を作製した後、水分吸着層２５を形成しないで、電気二重層キャパシタ用電極とし、電気キャパシタセルを作製した。 (Comparative Example 1)
After the polarizable electrode 24 was produced by the same method as in Example 1, an electric capacitor cell was produced without forming the moisture adsorption layer 25 as an electrode for an electric double layer capacitor.

（比較例２）
（１）分極性電極の作製
ヤシガラ活性炭１００重量部、アセチレンブラック５重量部、あらかじめ３００℃にて8時間熱処理した粉末状（粒径１０μｍ以下）のモレキュラーシーブ３Ａ重量部、カルボキシメチルセルロース及びスチレンブタジエンゴムをそれぞれ４重量部を適量の蒸留水で分散混合した分散液の４種を混合したスラリーを、電解エッチングを施したアルミ箔上に塗布乾燥し、厚さ50μｍの分極性電極２４を作製した。 (Comparative Example 2)
(1) Production of polarizable electrode 100 parts by weight of coconut husk activated carbon, 5 parts by weight of acetylene black, 3A parts by weight of molecular sieve in a powder form (particle size of 10 μm or less) previously heat-treated at 300 ° C. for 8 hours, carboxymethylcellulose and styrene butadiene rubber A slurry obtained by mixing 4 types of each of the dispersions obtained by dispersing and mixing 4 parts by weight with an appropriate amount of distilled water was applied onto an aluminum foil subjected to electrolytic etching and dried to prepare a polarizable electrode 24 having a thickness of 50 μm.

（２）電気二重層キャパシタセルの作製
前記分極性電極２４を用い、実施例１と同様の方法で電気二重層キャパシタセルを作製した。 (2) Production of Electric Double Layer Capacitor Cell Using the polarizable electrode 24, an electric double layer capacitor cell was produced in the same manner as in Example 1.

以上の実施例１及び比較例１及び２の電気二重層キャパシタセルについて６０℃、２．５Ｖにて１０００時間課電した後の静電容量の変化を調べ初期値に対する低下率を調べた。その結果を以下に示す。   With respect to the electric double layer capacitor cells of Example 1 and Comparative Examples 1 and 2 described above, the change in capacitance after applying 1000 hours at 60 ° C. and 2.5 V was examined, and the rate of decrease relative to the initial value was examined. The results are shown below.


低下率
実施例１ ３％
比較例１ １０％
比較例２ ６％
Decrease rate Example 1 3%
Comparative Example 1 10%
Comparative Example 2 6%

以上の結果、本発明の水分吸着層２５を積層した分極性電極を用いた電気二重層キャパシタセルの静電容量の劣化率が低いことわかる。   From the above results, it can be seen that the rate of deterioration of the capacitance of the electric double layer capacitor cell using the polarizable electrode in which the moisture adsorption layer 25 of the present invention is laminated is low.

長期性能低下を抑えることのできる電気二重層キャパシタとして利用できる。   It can be used as an electric double layer capacitor that can suppress long-term performance degradation.

１、２ 分極性電極
３ セパレータ
４ 電解液
５ ケース
６、７ リード線
８ 端子台
９ 正極端子
１０ 負極端子
１１ ガスケット
１２ 圧力放出弁
２１ 電気二重層キャパシタ電極
２２ 集電体
２３ 活性炭層
２４ 分極性電極
２５ 水分吸着層 1, 2 Polarized electrode 3 Separator 4 Electrolyte 5 Case 6, 7 Lead wire 8 Terminal block 9 Positive terminal 10 Negative terminal 11 Gasket 12 Pressure release valve 21 Electric double layer capacitor electrode 22 Current collector 23 Activated carbon layer 24 Polarized electrode 25 Moisture adsorption layer

Claims (3)

分極性電極を有する電気二重層キャパシタ用電極において、前記分極性電極の上層に水分吸着層を積層することを特徴とする電気二重層キャパシタ用電極。   An electrode for an electric double layer capacitor having a polarizable electrode, wherein a moisture adsorption layer is laminated on the polarizable electrode. 前記水分吸着層を構成する水分吸着剤は、孔径0.4ｎｍ以下、粒径１０μｍ以下の水分吸着材料であり、該水分吸着材料を３００℃以上の温度で活性化処理した後、有機溶剤及び有機溶剤系バインダによりスラリーとし、該スラリーを前記分極性電極上に塗布、乾燥して形成してなる請求項１に記載のキャパシタ用電極。   The moisture adsorbent constituting the moisture adsorption layer is a moisture adsorption material having a pore diameter of 0.4 nm or less and a particle diameter of 10 μm or less. After the moisture adsorption material is activated at a temperature of 300 ° C. or more, an organic solvent and an organic solvent are used. The capacitor electrode according to claim 1, wherein the capacitor electrode is formed by forming a slurry with a system binder and applying the slurry onto the polarizable electrode and drying. 請求項１及び２に記載のキャパシタ用電極を用いた電気二重層キャパシタ。
An electric double layer capacitor using the capacitor electrode according to claim 1.
JP2011043450A 2011-03-01 2011-03-01 Electrode for electric double-layer capacitor and electric double-layer capacitor Withdrawn JP2012182263A (en)

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WO2015026881A1 (en) * 2013-08-22 2015-02-26 Corning Incorporated Carbon-based electrodes containing molecular sieve
JP2016103402A (en) * 2014-11-28 2016-06-02 株式会社豊田自動織機 Electrode manufacturing method
CN105684114A (en) * 2013-08-30 2016-06-15 康宁股份有限公司 Low resistance ultracapacitor electrode and manufacturing method thereof
KR20200053180A (en) 2018-11-08 2020-05-18 한국전기연구원 Electrode for super capacitor comprising conductor layer including additive preventing corrosion, manufacturing method for the same and supercapacitor using the same

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2014143226A (en) * 2013-01-22 2014-08-07 Murata Mfg Co Ltd Flush ssd
WO2014163856A3 (en) * 2013-03-12 2015-01-08 Cooper Technologies Company Electrochemical energy storage device with molecular seive storage cell
WO2015026881A1 (en) * 2013-08-22 2015-02-26 Corning Incorporated Carbon-based electrodes containing molecular sieve
CN105900199A (en) * 2013-08-22 2016-08-24 康宁股份有限公司 Carbon-based electrodes containing molecular sieve
JP2016534565A (en) * 2013-08-22 2016-11-04 コーニング インコーポレイテッド Carbon-based electrode containing molecular sieve
CN105684114A (en) * 2013-08-30 2016-06-15 康宁股份有限公司 Low resistance ultracapacitor electrode and manufacturing method thereof
JP2016103402A (en) * 2014-11-28 2016-06-02 株式会社豊田自動織機 Electrode manufacturing method
KR20200053180A (en) 2018-11-08 2020-05-18 한국전기연구원 Electrode for super capacitor comprising conductor layer including additive preventing corrosion, manufacturing method for the same and supercapacitor using the same

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