JP4654637B2 - Manufacturing method of aluminum electrolytic capacitor - Google Patents
Manufacturing method of aluminum electrolytic capacitor Download PDFInfo
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- JP4654637B2 JP4654637B2 JP2004259222A JP2004259222A JP4654637B2 JP 4654637 B2 JP4654637 B2 JP 4654637B2 JP 2004259222 A JP2004259222 A JP 2004259222A JP 2004259222 A JP2004259222 A JP 2004259222A JP 4654637 B2 JP4654637 B2 JP 4654637B2
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- aluminum electrolytic
- electrolytic capacitor
- aluminum
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims description 57
- 229910052782 aluminium Inorganic materials 0.000 title claims description 56
- 239000003990 capacitor Substances 0.000 title claims description 52
- 238000004519 manufacturing process Methods 0.000 title claims description 8
- 239000011888 foil Substances 0.000 claims description 86
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 65
- 229910052799 carbon Inorganic materials 0.000 claims description 24
- 238000005530 etching Methods 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 17
- 238000007789 sealing Methods 0.000 claims description 12
- 229910052751 metal Inorganic materials 0.000 claims description 10
- 239000002184 metal Substances 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 14
- 239000002904 solvent Substances 0.000 description 14
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 12
- 239000003792 electrolyte Substances 0.000 description 12
- -1 inorganic acid salt Chemical class 0.000 description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 8
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 7
- 230000001965 increasing effect Effects 0.000 description 7
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- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 6
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- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 description 6
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- 239000004254 Ammonium phosphate Substances 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 2
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- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
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- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
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- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 2
- 229910000148 ammonium phosphate Inorganic materials 0.000 description 2
- 235000019289 ammonium phosphates Nutrition 0.000 description 2
- 150000003863 ammonium salts Chemical class 0.000 description 2
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 2
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 150000007522 mineralic acids Chemical class 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- BDJRBEYXGGNYIS-UHFFFAOYSA-N nonanedioic acid Chemical compound OC(=O)CCCCCCCC(O)=O BDJRBEYXGGNYIS-UHFFFAOYSA-N 0.000 description 2
- 239000004745 nonwoven fabric Substances 0.000 description 2
- 235000006408 oxalic acid Nutrition 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
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- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
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- CYSGHNMQYZDMIA-UHFFFAOYSA-N 1,3-Dimethyl-2-imidazolidinon Chemical compound CN1CCN(C)C1=O CYSGHNMQYZDMIA-UHFFFAOYSA-N 0.000 description 1
- RTBFRGCFXZNCOE-UHFFFAOYSA-N 1-methylsulfonylpiperidin-4-one Chemical compound CS(=O)(=O)N1CCC(=O)CC1 RTBFRGCFXZNCOE-UHFFFAOYSA-N 0.000 description 1
- BQNDPALRJDCXOY-UHFFFAOYSA-N 2,3-dibutylbutanedioic acid Chemical compound CCCCC(C(O)=O)C(C(O)=O)CCCC BQNDPALRJDCXOY-UHFFFAOYSA-N 0.000 description 1
- WKFQMDFSDQFAIC-UHFFFAOYSA-N 2,4-dimethylthiolane 1,1-dioxide Chemical compound CC1CC(C)S(=O)(=O)C1 WKFQMDFSDQFAIC-UHFFFAOYSA-N 0.000 description 1
- GFISDBXSWQMOND-UHFFFAOYSA-N 2,5-dimethoxyoxolane Chemical compound COC1CCC(OC)O1 GFISDBXSWQMOND-UHFFFAOYSA-N 0.000 description 1
- XWVFEDFALKHCLK-UHFFFAOYSA-N 2-methylnonanedioic acid Chemical compound OC(=O)C(C)CCCCCCC(O)=O XWVFEDFALKHCLK-UHFFFAOYSA-N 0.000 description 1
- BELGHMWMXFCZTP-UHFFFAOYSA-N 3-ethyl-1,3-oxazolidin-2-one Chemical compound CCN1CCOC1=O BELGHMWMXFCZTP-UHFFFAOYSA-N 0.000 description 1
- CMJLMPKFQPJDKP-UHFFFAOYSA-N 3-methylthiolane 1,1-dioxide Chemical compound CC1CCS(=O)(=O)C1 CMJLMPKFQPJDKP-UHFFFAOYSA-N 0.000 description 1
- OTLNPYWUJOZPPA-UHFFFAOYSA-N 4-nitrobenzoic acid Chemical compound OC(=O)C1=CC=C([N+]([O-])=O)C=C1 OTLNPYWUJOZPPA-UHFFFAOYSA-N 0.000 description 1
- ZKOGUIGAVNCCKH-UHFFFAOYSA-N 4-phenyl-1,3-dioxolan-2-one Chemical compound O1C(=O)OCC1C1=CC=CC=C1 ZKOGUIGAVNCCKH-UHFFFAOYSA-N 0.000 description 1
- FLDCSPABIQBYKP-UHFFFAOYSA-N 5-chloro-1,2-dimethylbenzimidazole Chemical compound ClC1=CC=C2N(C)C(C)=NC2=C1 FLDCSPABIQBYKP-UHFFFAOYSA-N 0.000 description 1
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- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 description 1
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- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 1
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- 150000001409 amidines Chemical class 0.000 description 1
- 235000019293 ammonium adipate Nutrition 0.000 description 1
- JFCQEDHGNNZCLN-UHFFFAOYSA-N anhydrous glutaric acid Natural products OC(=O)CCCC(O)=O JFCQEDHGNNZCLN-UHFFFAOYSA-N 0.000 description 1
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- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
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- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 description 1
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Description
本発明は各種電子機器に使用されるアルミ電解コンデンサ及びその製造方法に関するものである。 The present invention relates to an aluminum electrolytic capacitor used in various electronic devices and a method for manufacturing the same.
一般的なアルミ電解コンデンサは、アルミニウム箔をエッチング処理によって実効表面積を拡大させた表面に陽極酸化により誘電体酸化皮膜を形成した陽極箔とアルミニウム箔をエッチング処理によって実効表面積を拡大させた陰極箔とをセパレータを介して巻回することによりコンデンサ素子を形成し、このコンデンサ素子に駆動用電解液を含浸させるとともに、このコンデンサ素子を金属ケース内に収納し、この金属ケースの開口部を封口体により封止した構成を有している。 A general aluminum electrolytic capacitor includes an anode foil in which a dielectric oxide film is formed by anodic oxidation on a surface of which an effective surface area is expanded by etching the aluminum foil, and a cathode foil in which the effective surface area is expanded by etching the aluminum foil. Is wound through a separator to form a capacitor element. The capacitor element is impregnated with a driving electrolyte, and the capacitor element is housed in a metal case. The opening of the metal case is sealed by a sealing body. It has a sealed configuration.
前記駆動用電解液としては、エチレングリコールまたはγ−ブチロラクトンを主溶媒とし、これに有機酸のアンモニウム塩などを加えたものが多く使用され、また、封口体としては、スチレンブタジエンゴム(SBR)、エチレンプロピレンゴム(EPM)、ブチルゴム(IIR)からなるものが多く使用されている。 As the driving electrolyte, a solution in which ethylene glycol or γ-butyrolactone is used as a main solvent and an ammonium salt of an organic acid is added to the main solvent is often used, and as a sealing body, styrene butadiene rubber (SBR), Many are made of ethylene propylene rubber (EPM) and butyl rubber (IIR).
近年、電子機器の小型化、デジタル化、高信頼性化に伴い、アルミ電解コンデンサに対するユーザーからのニーズも小型化が強く要望されており、そのためにはアルミ電解コンデンサに用いられる陽極箔及び陰極箔の単位面積当たりの静電容量を高めることが必要とされている。 In recent years, with the downsizing, digitization, and high reliability of electronic devices, there has been a strong demand for miniaturization of the needs for users of aluminum electrolytic capacitors. To that end, anode foil and cathode foil used for aluminum electrolytic capacitors It is necessary to increase the capacitance per unit area.
前記陽極箔及び陰極箔の実効表面積を拡大し単位面積当たりの静電容量を高めるには、一般的に硫酸、硝酸、燐酸、蓚酸などの皮膜を形成する酸を添加した塩酸水溶液中で化学的あるいは電気化学的にエッチング処理を行うことにより達成することができ、そのエッチング処理の電解液組成、電流密度などの条件を工夫・改善して、陽極箔及び陰極箔の静電容量や機械的強度などの特性の向上を図っている。 In order to increase the effective surface area of the anode foil and the cathode foil and increase the capacitance per unit area, it is generally chemically performed in an aqueous hydrochloric acid solution to which an acid forming a film such as sulfuric acid, nitric acid, phosphoric acid, and oxalic acid is added. Alternatively, it can be achieved by electrochemically performing etching treatment, and by devising and improving conditions such as the electrolyte composition and current density of the etching treatment, the capacitance and mechanical strength of the anode foil and cathode foil We are trying to improve the characteristics.
なお、この出願の発明に関する先行技術文献情報としては、例えば、特許文献1、2が知られている。
しかしながら前記従来のアルミ電解コンデンサにおいて、陽極箔及び陰極箔のエッチング処理による静電容量の拡大は、エッチング処理でできるピットをできるだけ分散性を高めることが必要であるが、エッチング処理の際ピット先端での液抵抗が大きくなるため効率よくエッチング処理を行うことが限界に近づきつつある。特に陰極箔は、そのアルミニウム箔の厚さが20〜50μmと薄く、エッチング処理による実効面積の拡大を向上させることが難しいとされている。 However, in the conventional aluminum electrolytic capacitor, the expansion of the electrostatic capacity by the etching process of the anode foil and the cathode foil needs to increase the dispersibility of the pits that can be formed by the etching process as much as possible. Since the liquid resistance increases, efficient etching is approaching its limit. In particular, the cathode foil has a thin aluminum foil thickness of 20 to 50 μm, and it is difficult to improve the expansion of the effective area by the etching process.
また、電荷引出しのために陰極箔にリード線を取り付けるが、このリード線と陰極箔の間に電位差が生じて電流が流れ腐食の原因となり、アルミ電解コンデンサの寿命特性に問題がある。 In addition, a lead wire is attached to the cathode foil for extracting the electric charge. However, a potential difference is generated between the lead wire and the cathode foil, current flows and causes corrosion, and there is a problem in the life characteristics of the aluminum electrolytic capacitor.
この問題を解決するために、陰極箔の表面に2V程度の化成を行い流れる電流を少なくすることや、TiNなどを蒸着した箔を使用してリード線との電位差を小さくしている。 In order to solve this problem, formation of about 2 V is performed on the surface of the cathode foil to reduce the flowing current, or the potential difference from the lead wire is reduced by using a foil deposited with TiN or the like.
前記陰極箔の表面に化成を形成した場合、陰極箔の静電容量が低くなり、陽極箔の静電容量を十分に引き出すことができず、アルミ電解コンデンサの容量が小さくなる。また、TiNなどを蒸着した箔の場合、蒸着のプロセスが複雑であるため工業的に導入するのは困難という課題を有している。 When chemical conversion is formed on the surface of the cathode foil, the capacitance of the cathode foil is lowered, the capacitance of the anode foil cannot be sufficiently drawn, and the capacitance of the aluminum electrolytic capacitor is reduced. Further, in the case of a foil on which TiN or the like is vapor-deposited, there is a problem that it is difficult to introduce industrially because the vapor deposition process is complicated.
本発明は、前記従来の問題点を解決するもので、陰極箔の静電容量を向上させ、かつリード線と陰極箔間の電位差を小さくし、寿命特性に優れた高性能化、小型化のアルミ電解コンデンサを提供することを目的とするものである。 The present invention solves the above-mentioned conventional problems, and improves the capacitance of the cathode foil, reduces the potential difference between the lead wire and the cathode foil, and improves performance and size with excellent life characteristics. An object of the present invention is to provide an aluminum electrolytic capacitor.
前記目的を達成するために本発明は、前記アルミ電解コンデンサの製造方法は、アルミニウム箔をエッチング処理して誘電体酸化皮膜を形成した陽極箔を用意する工程と、アルミニウム箔の表面に比表面積が140〜400m 2 /gの活性炭を10〜77重量%を含む50〜360m 2 /gの比表面積を有する多孔質カーボン層を形成した陰極箔を用意する工程と、前記陽極箔と陰極箔とをセパレータを介して巻回してコンデンサ素子を形成し、このコンデンサ素子に駆動用電解液を含浸させる工程と、前記コンデンサ素子を金属ケースに収納して、この金属ケースの開口部を封口体で封止する工程を備えた製造方法とするものである。 In order to achieve the above object, the present invention provides a method for manufacturing an aluminum electrolytic capacitor comprising: preparing an anode foil in which an aluminum foil is etched to form a dielectric oxide film; and a specific surface area on the surface of the aluminum foil. preparing a cathode foil obtained by forming a porous carbon layer having a specific surface area of 50~360m 2 / g containing 10 to 77 wt% of activated charcoal 140~400m 2 / g, and the anode and cathode foils A capacitor element is formed by winding through a separator, the capacitor element is impregnated with a driving electrolyte, and the capacitor element is housed in a metal case, and the opening of the metal case is sealed with a sealing body It is set as the manufacturing method provided with the process to do.
本発明のアルミ電解コンデンサの製造方法において、アルミニウム箔の表面に比表面積が140〜400m 2 /gの活性炭を10〜77重量%を含む50〜360m 2 /gの比表面積を有する多孔質カーボン層を形成した陰極箔を用意する工程を有することにより、陰極箔の実効表面積を拡大することなく陰極箔の静電容量を高めることができ、かつリード線と陰極箔の電位差を小さくすることができるので、陰極箔に流れる電流が抑制されるため陰極箔の耐腐食性も向上し、高寿命化、小型化のアルミ電解コンデンサを得ることができるという効果を奏するものである。 In the method for producing an aluminum electrolytic capacitor of the present invention, a porous carbon layer having a specific surface area of 50 to 360 m 2 / g containing 10 to 77% by weight of activated carbon having a specific surface area of 140 to 400 m 2 / g on the surface of the aluminum foil. By having a step of preparing a cathode foil formed with a cathode foil, the capacitance of the cathode foil can be increased without increasing the effective surface area of the cathode foil, and the potential difference between the lead wire and the cathode foil can be reduced. Therefore, since the current flowing through the cathode foil is suppressed, the corrosion resistance of the cathode foil is improved, and an effect is obtained that a long-life and downsized aluminum electrolytic capacitor can be obtained.
以下、本発明の実施の形態について詳細に説明する。 Hereinafter, embodiments of the present invention will be described in detail.
図1は本発明の一実施の形態におけるアルミ電解コンデンサの部分切り欠き斜視図である。同図においてアルミニウム箔をエッチング処理により実効表面積を拡大した表面に陽極酸化により誘電体酸化皮膜を形成して引出し用の陽極リード15を接続した陽極箔11と、アルミニウム箔に活性炭を含む多孔質カーボン層を形成して引出し用の陰極リード16を接続した陰極箔12とをセパレータ13を介して巻回することによりコンデンサ素子19を構成し、このコンデンサ素子19に駆動用電解液14を含浸させて後、アルミニウムの金属ケース18内に挿入して金属ケース18の開口部を封口板17で封止されている。
FIG. 1 is a partially cutaway perspective view of an aluminum electrolytic capacitor according to an embodiment of the present invention. In the figure, an anode foil 11 in which a dielectric oxide film is formed by anodic oxidation on the surface of an aluminum foil which has been expanded by etching and an
前記陽極箔11は、その表面を実効表面積を拡大するためにエッチング処理を施す。このエッチング処理は硫酸、硝酸、燐酸、蓚酸などの皮膜を形成する酸を添加した塩酸水溶液中で化学的あるいは電気化学的(交流印加または直流印加)にエッチング処理を行う。この中で主に低圧用のアルミ電解コンデンサの陽極箔には交流印加のエッチング処理が用いられ、多数のエッチング槽で、液温度、周波数、時間を変化させてエッチング処理を行い、海綿状のピットを形成する。また、中高圧用に使用される陽極箔11のエッチング処理は、前段エッチング工程でトンネル状のピットを生成させ、後段エッチング工程で前記ピットをアルミ電解コンデンサの使用電圧に適した径まで拡大して形成する。 The anode foil 11 is subjected to an etching process in order to increase the effective surface area. This etching process is performed chemically or electrochemically (AC application or DC application) in an aqueous hydrochloric acid solution to which an acid that forms a film such as sulfuric acid, nitric acid, phosphoric acid, or oxalic acid is added. Among them, the AC foil is mainly used for the anode foil of low-voltage aluminum electrolytic capacitors. In many etching tanks, the etching temperature is changed by changing the liquid temperature, frequency, and time. Form. In addition, the etching process of the anode foil 11 used for medium and high pressures is performed by generating tunnel-like pits in the former etching process and expanding the pits to a diameter suitable for the working voltage of the aluminum electrolytic capacitor in the latter etching process. Form.
前記陰極箔12は、従来は陽極箔11と同様に実効表面積を拡大するためにエッチング処理を行っていたが、本発明の陰極箔12はアルミニウム箔の表面に50〜360m 2 /g以上の比表面積を有する多孔質カーボン層を被覆したものである。
The
この多孔質カーボン層は、少なくとも活性炭を含み、その活性炭を10〜77重量%を含むことにより、50〜360m2/gの比表面積を有する多孔質カーボン層を形成することができる。 The porous carbon layer contains at least activated carbon, and by containing 10 to 77 % by weight of the activated carbon, a porous carbon layer having a specific surface area of 50 to 360 m 2 / g can be formed.
また、前記陰極箔12は多孔質カーボン層を形成させる前のアルミニウム箔の表面または多孔質カーボン層の表面にリン酸皮膜を形成させることにより、アルミニウム箔の腐食を防止することができる。
The
この陰極箔12をアルミ電解コンデンサに用いることにより、耐腐食性に優れた高性能化、小型化のアルミ電解コンデンサを提供することができる。
By using this
前記駆動用電解液14は、極性溶媒と、無機酸、有機酸、無機酸塩、有機酸塩の1種以上を含む溶質とからなる。
The driving
前記極性溶媒としては,エチレングリコール、プロピレングリコール、1,4−ブタンジオール、グリセリン、ポリオキシアルキレンポリオール(分子量200以下のポリエチレンオキシド、ポリプロピレンオキシド、ポリオキシエチレン・オキシプロピレングリコールならびに、これら2種以上の併用)、フラン溶媒(2,5−ジメトキシテトラヒドロフラン等)、スルホラン溶媒(スルホラン、3−メチルスルホラン、2,4−ジメチルスルホラン等)、カーボネート溶媒(プロピレンカーボネート、エチレンカーボネート、ジエチルカーボネート、スチレンカーボネート、ジメチルカーボネート、またはメチルエチルカーボネート等)、ラクトン溶媒(γ−ブチロラクトン、γ−バレロラクトン、δ−バレロラクトン、3−メチル−1,3−オキサジリジン−2−オン、3−エチル−1,3−オキサゾリジン−2−オン等)、イミダゾリジノン溶媒(1,3−ジメチル−2−イミダゾリジノン等)、ピロリドン溶媒等が挙げられる。 Examples of the polar solvent include ethylene glycol, propylene glycol, 1,4-butanediol, glycerin, polyoxyalkylene polyol (polyethylene oxide having a molecular weight of 200 or less, polypropylene oxide, polyoxyethylene / oxypropylene glycol, and two or more kinds thereof. Combined use), furan solvent (2,5-dimethoxytetrahydrofuran, etc.), sulfolane solvent (sulfolane, 3-methylsulfolane, 2,4-dimethylsulfolane, etc.), carbonate solvent (propylene carbonate, ethylene carbonate, diethyl carbonate, styrene carbonate, dimethyl) Carbonate or methyl ethyl carbonate), lactone solvent (γ-butyrolactone, γ-valerolactone, δ-valerolactone, 3-methyl-1, - oxaziridine-2-one, 3-ethyl-1,3-oxazolidin-2-one, etc.), imidazolidinone solvent (1,3-dimethyl-2-imidazolidinone, etc.), pyrrolidone solvents.
前記溶質は無機酸、有機酸、無機酸塩、有機酸塩の1種以上を含むものであるが、その中で好ましいものとしては、硼酸、リン酸、アゼライン酸、アジピン酸、グルタル酸、フタル酸、マレイン酸、安息香酸、5,6−デカンジカルボン酸、1,7−オクタンジカルボン酸、1,6−デカンジカルボン酸等の二塩基酸またはその塩が挙げられる。また、前記の塩としては、アンモニウム塩、アミン塩、四級アンモニウム塩、アミジン系塩等が使用できる。 The solute contains one or more of an inorganic acid, an organic acid, an inorganic acid salt, and an organic acid salt. Among them, preferred are boric acid, phosphoric acid, azelaic acid, adipic acid, glutaric acid, phthalic acid, Examples thereof include dibasic acids such as maleic acid, benzoic acid, 5,6-decanedicarboxylic acid, 1,7-octanedicarboxylic acid, 1,6-decanedicarboxylic acid, and salts thereof. Moreover, as said salt, ammonium salt, amine salt, quaternary ammonium salt, amidine type salt, etc. can be used.
前記セパレータ13はセルロース系繊維紙及びその混抄紙、積層紙などであり、セルロース系繊維紙としてはマニラ麻、クラフト、ヘンプ、エスパルト、コットンの少なくとも1種を含むものである。さらにはポリエチレンテレフタレート、ポリブチレンテレフタレート、ポリフェニレンサルファイド、ナイロン、芳香族ポリアミド、ポリイミド、ポリアミドイミド、ポリエーテルイミド、レーヨンなどの合成樹脂材料の不織布を用いることもできる。
The
これらは、繊維間隔が見掛け上緻密になり、かつ微細の貫通孔を多数有しているので、電解質の電導度を低下させることがないので、コンデンサとして抵抗損失を小さくすることができ、また、耐ショート性の向上を図ることができる。 Since the fiber spacing is apparently dense and has a large number of fine through-holes, the electrical conductivity of the electrolyte is not lowered, so that the resistance loss can be reduced as a capacitor, Short circuit resistance can be improved.
前記セパレータ13の秤量は1〜60g/m2の範囲のものを用いる。秤量の低いセパレータ13を用いた場合、ショートを引き起こし安定な特性を保つことができない、また、秤量が高くなりすぎると、等価直列抵抗が高くなる。
The
なお、前記セパレータ13は、セパレータ13の引っ張り強度を向上させる目的で紙力増強加工を施してもよい。この紙力増強加工を施すことにより、引っ張り強度が向上し、耐ショート性をさらに向上させることができる。
The
前記紙力増強加工は、セパレータ13に澱粉、植物性ガム、カルボキシアルキルセルロース、ポリオキシエチレンフタレートなどの水溶液を塗布もしくは含浸処理することにより行うことができる。
The paper strength enhancing process can be performed by applying or impregnating the
また、前記合成樹脂材料の不織布は、シート化の際に繊維間を接着するための接着剤を用いることなく熱接着法や機械的交絡法によりシート化することができる上、その融点も高いので、250℃を超えるハンダ付け実装条件下においても、樹脂の熱収縮によるセパレータ繊維の切断やESRの増大が生じにくく、ハンダ耐熱性に優れた低ESRなアルミ電解コンデンサを得ることができる。 In addition, since the nonwoven fabric of the synthetic resin material can be formed into a sheet by a thermal bonding method or a mechanical entanglement method without using an adhesive for bonding fibers during sheeting, its melting point is also high. Even under soldering mounting conditions exceeding 250 ° C., it is difficult for the separator fiber to be cut or ESR increased due to heat shrinkage of the resin, and a low ESR aluminum electrolytic capacitor having excellent solder heat resistance can be obtained.
前記封口板17は、エチレン−プロピレン−ジエン三元共重合体ゴム(EPDM)、ブタンゴム(IIR)、ウレタンゴム(U)、シリコーンゴム(Q)、クロロスルホン化ポリエチレンゴム(CSM)の少なくとも1種を主成分とするものであり、これに加硫剤、加硫助剤、補強材及び充填剤、劣化防止剤等を添加して混練し、その後成形して封口板17を得ることができる。
The
以下、具体的な実施例について説明をする。 Hereinafter, specific examples will be described.
(実施例1)
[陽極箔の作製]
厚さ100μm、純度99.98%のアルミニウム箔を用い、リン酸濃度が1.0wt%の90℃の水溶液に60秒間浸漬して前処理を行う。
Example 1
[Production of anode foil]
An aluminum foil having a thickness of 100 μm and a purity of 99.98% is used, and pretreatment is performed by dipping in a 90 ° C. aqueous solution having a phosphoric acid concentration of 1.0 wt% for 60 seconds.
次に、塩酸5wt%、塩化アルミニウム2wt%、硫酸0.1wt%、リン酸0.2wt%に調整した温度30℃の電解液に前記アルミニウム箔を浸漬し、交流電流を印加してエッチング処理を4段階に分けて行った。 Next, the aluminum foil is immersed in an electrolytic solution at a temperature of 30 ° C. adjusted to 5 wt% hydrochloric acid, 2 wt% aluminum chloride, 0.1 wt% sulfuric acid, and 0.2 wt% phosphoric acid, and an alternating current is applied to perform etching treatment. It was divided into four stages.
次に、硫酸10wt%の60℃の水溶液で100秒間の浸漬処理を行い、250℃で120秒間の熱処理を行って、陽極箔となるエッチング箔を作製した。 Next, an immersion treatment for 100 seconds was performed with an aqueous solution of 10 wt% sulfuric acid at 60 ° C., and a heat treatment was performed at 250 ° C. for 120 seconds to produce an etching foil serving as an anode foil.
次に、前記エッチング箔を15%アジピン酸アンモニウム水溶液中にて19Vの直流電圧を印加して化成処理を行い、陽極箔を得た。 Next, the etching foil was subjected to a chemical conversion treatment by applying a DC voltage of 19 V in a 15% ammonium adipate aqueous solution to obtain an anode foil.
[陰極箔の作製]
平均粒径5μmの活性炭粉末(BET比表面積:140m2/g)と導電性付与剤として平均粒径0.05μmのカーボンブラックとポリテトラフルオロエチレン(以下、PTFEと略す)とを10:2:1の重量比に混合して分散した水溶性バインダー溶液を混練機で十分に混練した後、水の分散溶媒を少しずつ加えてさらに混練してペーストを作製する。
[Preparation of cathode foil]
Activated carbon powder (BET specific surface area: 140 m 2 / g) having an average particle diameter of 5 μm, carbon black having an average particle diameter of 0.05 μm and polytetrafluoroethylene (hereinafter abbreviated as PTFE) as a conductivity imparting agent are 10: 2: A water-soluble binder solution mixed and dispersed at a weight ratio of 1 is sufficiently kneaded with a kneader, and then a water dispersion solvent is added little by little to further knead to prepare a paste.
次に、厚さ30μm、純度99.9%のアルミニウム箔の一方の表面に前記ペーストを厚さが10μmになるように塗布し、150℃で乾燥して多孔質カーボン層を形成した陰極箔を得た。 Next, a cathode foil having a porous carbon layer formed by applying the paste to a thickness of 10 μm on one surface of an aluminum foil having a thickness of 30 μm and a purity of 99.9% and drying at 150 ° C. Obtained.
なお、前記多孔質カーボン層における活性炭の含有量は77重量%で、比表面積は140m2/gであった。 The activated carbon content in the porous carbon layer was 77% by weight, and the specific surface area was 140 m 2 / g.
[駆動用電解液]
駆動用電解液の組成を下記に示す(以下、駆動用電解液Aとする)。
[Drive electrolyte]
The composition of the driving electrolyte is shown below (hereinafter referred to as driving electrolyte A).
エチレングリコール :85重量%
リン酸 :2重量%
1,6−デカンジカルボン酸:12重量%
p−ニトロ安息香酸 :1重量%
[アルミ電解コンデンサの作製]
前記陽極箔と前記陰極箔とをマニラ紙のセパレータを介して巻回することによりコンデンサ素子を形成し、このコンデンサ素子に前記駆動用電解液Aを含浸させて金属ケースに収納し、この金属ケースの開口部に樹脂加硫ブチルゴム封口板(ブチルゴムポリマー30部、カーボン20部、無機充填剤50部から構成、封口板硬度:70IRHD[国際ゴム硬さ単位])で封入した後、カーリング処理により開口部を封止してアルミ電解コンデンサを作製した(サイズ:直径10mm×高さ16mm 定格400WV 6.8μF)。
Ethylene glycol: 85% by weight
Phosphoric acid: 2% by weight
1,6-decanedicarboxylic acid: 12% by weight
p-Nitrobenzoic acid: 1% by weight
[Production of aluminum electrolytic capacitors]
A capacitor element is formed by winding the anode foil and the cathode foil through a separator made of Manila paper. The capacitor element is impregnated with the driving electrolyte A and stored in a metal case. After sealing with a resin vulcanized butyl rubber sealing plate (30 parts butyl rubber polymer, 20 parts carbon, 50 parts inorganic filler, sealing board hardness: 70 IRHD [international rubber hardness unit]), it is opened by curling treatment. The part was sealed to produce an aluminum electrolytic capacitor (size: diameter 10 mm ×
(実施例2)
前記実施例1において、多孔質カーボン層の活性炭を平均粒径5μmの活性炭粉末(BET比表面積:220m2/g)のものを用いて形成した以外は前記実施例1と同様にしてアルミ電解コンデンサを作製した。
(Example 2)
An aluminum electrolytic capacitor was prepared in the same manner as in Example 1 except that the activated carbon of the porous carbon layer was formed using activated carbon powder having an average particle size of 5 μm (BET specific surface area: 220 m 2 / g). Was made.
なお、前記多孔質カーボン層の比表面積は210m2/gであった。 The specific surface area of the porous carbon layer was 210 m 2 / g.
(実施例3)
前記実施例1において、多孔質カーボン層の活性炭を平均粒径5μmの活性炭粉末(BET比表面積:400m2/g)のものを用いて形成した以外は前記実施例1と同様にしてアルミ電解コンデンサを作製した。
(Example 3)
Aluminum electrolytic capacitor in the same manner as in Example 1 except that the activated carbon of the porous carbon layer in Example 1 was formed using activated carbon powder having an average particle size of 5 μm (BET specific surface area: 400 m 2 / g). Was made.
なお、前記多孔質カーボン層の比表面積は360m2/gであった。 The specific surface area of the porous carbon layer was 360 m 2 / g.
(実施例4)
前記実施例1において、活性炭とカーボンブラック及びポリエステル樹脂の重量比を7:5:1にし、また、有機分散溶媒を用いた以外は前記実施例1と同様にしてアルミ電解コンデンサを作製した。
Example 4
In Example 1, an aluminum electrolytic capacitor was produced in the same manner as in Example 1 except that the weight ratio of activated carbon to carbon black and polyester resin was 7: 5: 1 and an organic dispersion solvent was used.
なお、前記多孔質カーボン層における活性炭の含有量は54重量%で、比表面積は110m2/gであった。 The activated carbon content in the porous carbon layer was 54% by weight, and the specific surface area was 110 m 2 / g.
(実施例5)
前記実施例1において、活性炭とカーボンブラック及びポリエステル樹脂の重量比を4:8:1にし、また、有機分散溶媒を用いた以外は前記実施例1と同様にしてアルミ電解コンデンサを作製した。
(Example 5)
In Example 1, an aluminum electrolytic capacitor was produced in the same manner as in Example 1 except that the weight ratio of activated carbon, carbon black, and polyester resin was 4: 8: 1 and an organic dispersion solvent was used.
なお、前記多孔質カーボン層における活性炭の含有量は30重量%で、比表面積は65m2/gであった。 The activated carbon content in the porous carbon layer was 30% by weight and the specific surface area was 65 m 2 / g.
(実施例6)
前記実施例1において、活性炭とカーボンブラック及びポリエステル樹脂の重量比を1.3:10.7:1にし、また、有機分散溶媒を用いた以外は前記実施例1と同様にしてアルミ電解コンデンサを作製した。
(Example 6)
In Example 1, the weight ratio of activated carbon to carbon black and polyester resin was 1.3: 10.7: 1, and an aluminum electrolytic capacitor was prepared in the same manner as in Example 1 except that an organic dispersion solvent was used. Produced.
なお、前記多孔質カーボン層における活性炭の含有量は10重量%で、比表面積は50m2/gであった。 The content of activated carbon in the porous carbon layer was 10% by weight, and the specific surface area was 50 m 2 / g.
(実施例7)
前記実施例1において、陰極箔に用いるアルミニウム箔を2%リン酸アンモニウム水溶液に浸漬して、その表面にリン酸皮膜を形成したものを用いた以外は前記実施例1と同様にしてアルミ電解コンデンサを作製した。
(Example 7)
An aluminum electrolytic capacitor in the same manner as in Example 1 except that the aluminum foil used for the cathode foil was immersed in a 2% aqueous ammonium phosphate solution and a phosphate film was formed on the surface. Was made.
(実施例8)
前記実施例1において、陰極箔に用いるアルミニウム箔を10%塩酸水溶液でその表面を粗面化し、その後、2%リン酸アンモニウム水溶液に浸漬して、その表面にリン酸皮膜を形成したものを用いた以外は前記実施例1と同様にしてアルミ電解コンデンサを作製した。
(Example 8)
In Example 1, the aluminum foil used for the cathode foil was roughened with a 10% aqueous hydrochloric acid solution and then immersed in a 2% aqueous ammonium phosphate solution to form a phosphate film on the surface. An aluminum electrolytic capacitor was produced in the same manner as in Example 1 except that.
(実施例9)
前記実施例1において、駆動用電解液として下記に示す組成(以下、駆動用電解液Bとする)のものを用いた以外は前記実施例1と同様にしてアルミ電解コンデンサを作製した(サイズ:直径10mm×高さ16mm 定格16WV 330μF)。
Example 9
In Example 1, an aluminum electrolytic capacitor was produced in the same manner as in Example 1 except that the driving electrolyte solution having the following composition (hereinafter referred to as driving electrolyte solution B) was used (size: 10 mm diameter x 16 mm height, rated 16 WV 330 μF).
γブチルラクトン:43重量%
スルホラン :40重量%
フタル酸 :5重量%
トリエチルアミン:12重量%
(比較例1)
前記実施例1において、陰極箔としてアルミニウム箔を10%塩酸水溶液でその表面を粗面化し、その後、350℃で1分間熱処理したものを用いた以外は前記実施例1と同様にしてアルミ電解コンデンサを作製した。
γ-butyl lactone: 43% by weight
Sulfolane: 40% by weight
Phthalic acid: 5% by weight
Triethylamine: 12% by weight
(Comparative Example 1)
An aluminum electrolytic capacitor was prepared in the same manner as in Example 1 except that the surface of the aluminum foil as a cathode foil was roughened with a 10% hydrochloric acid aqueous solution and then heat-treated at 350 ° C. for 1 minute. Was made.
(比較例2)
前記比較例1において、駆動用電解液として駆動用電解液Bを用いた以外は前記比較例1と同様にしてアルミ電解コンデンサを作製した。
(Comparative Example 2)
An aluminum electrolytic capacitor was produced in the same manner as in Comparative Example 1 except that the driving electrolytic solution B was used as the driving electrolytic solution in Comparative Example 1.
前記実施例1〜9と比較例1及び2のアルミ電解コンデンサについて、その初期特性(容量、tanδ、漏れ電流(LC))及び105℃中での高温負荷試験を行った。その結果を(表1)に示す。 The aluminum electrolytic capacitors of Examples 1 to 9 and Comparative Examples 1 and 2 were subjected to initial characteristics (capacity, tan δ, leakage current (LC)) and a high temperature load test at 105 ° C. The results are shown in (Table 1).
(表1)から明らかなように、実施例1〜9のアルミ電解コンデンサは初期特性及び105℃中での高温負荷試験において各比較例のアルミ電解コンデンサに比べて優れている。この(表1)の実施例1〜3では陰極箔の多孔質カーボン層の表面積を変化させたものであるが、多孔質カーボン層の表面積が大きくなると容量は高くなり、tanδ及びLCも高くなるが比較例1よりは低い。 As is clear from Table 1, the aluminum electrolytic capacitors of Examples 1 to 9 are superior to the aluminum electrolytic capacitors of the comparative examples in the initial characteristics and the high temperature load test at 105 ° C. In Examples 1 to 3 of this (Table 1), the surface area of the porous carbon layer of the cathode foil was changed, but as the surface area of the porous carbon layer increased, the capacity increased and tan δ and LC also increased. Is lower than Comparative Example 1.
また、多孔質カーボン層の活性炭を10重量%以上にすることにより、比較例1に比べて容量が高く、tanδ及びLCも低い。 Further, by making the activated carbon of the porous carbon layer 10% by weight or more, the capacity is higher than that of Comparative Example 1, and tan δ and LC are also low.
この活性炭の比表面積が大きいと、多孔質カーボン層の活性炭量を少なくすることができるが、活性炭量を10重量%未満にすると容量の高いものが得られない。 If the specific surface area of the activated carbon is large, the amount of activated carbon in the porous carbon layer can be reduced, but if the amount of activated carbon is less than 10% by weight, a high capacity cannot be obtained.
さらに、駆動用電解液をエチレングリコールの溶媒からγ−ブチルラクトンの溶媒に変えても各比較例に比べてコンデンサ特性が優れる。 Further, even if the driving electrolyte is changed from the solvent of ethylene glycol to the solvent of γ-butyllactone, the capacitor characteristics are excellent as compared with the comparative examples.
本発明のアルミ電解コンデンサは、陰極箔の表面に比表面積が50m2/g以上の多孔質カーボン層を被覆することにより、陰極箔の実効表面積を拡大することなく陰極箔の静電容量を高めることができ、かつリード線と陰極箔の電位差を小さくすることができるので、陰極箔に流れる電流が抑制されるため陰極箔の耐腐食性も向上し、高寿命化、小型化のアルミ電解コンデンサを得ることができる。 The aluminum electrolytic capacitor of the present invention increases the capacitance of the cathode foil without enlarging the effective surface area of the cathode foil by coating the surface of the cathode foil with a porous carbon layer having a specific surface area of 50 m 2 / g or more. And the potential difference between the lead wire and the cathode foil can be reduced, so that the current flowing through the cathode foil is suppressed, so that the corrosion resistance of the cathode foil is improved, and the lifetime and size of the aluminum electrolytic capacitor are reduced. Can be obtained.
11 陽極箔
12 陰極箔
13 セパレータ
14 駆動用電解液
15 陽極リード
16 陰極リード
17 封口板
18 金属ケース
19 コンデンサ素子
DESCRIPTION OF SYMBOLS 11
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JP4862602B2 (en) * | 2006-10-13 | 2012-01-25 | パナソニック株式会社 | Aluminum electrolytic capacitor |
KR101932966B1 (en) * | 2016-11-30 | 2018-12-27 | 삼신디바이스 주식회사 | Super capacitor and method for manufacturing the same |
WO2019240041A1 (en) | 2018-06-11 | 2019-12-19 | 日本ケミコン株式会社 | Electrode body, electrolytic capacitor provided with electrode body, and method for producing electrode body |
WO2020059609A1 (en) | 2018-09-21 | 2020-03-26 | 日本ケミコン株式会社 | Electrode body, electrolytic capacitor including electrode body, and method of manufacturing electrode body |
JP7358804B2 (en) * | 2019-07-04 | 2023-10-11 | 日本ケミコン株式会社 | Electrode body, electrolytic capacitor including the electrode body, and method for manufacturing the electrode body |
JP2022039636A (en) * | 2020-08-28 | 2022-03-10 | 日本ケミコン株式会社 | Electrolytic capacitor and manufacturing method thereof |
JP2022121196A (en) * | 2021-02-08 | 2022-08-19 | 日本ケミコン株式会社 | Electrolytic capacitor |
WO2022172720A1 (en) | 2021-02-09 | 2022-08-18 | 日本ケミコン株式会社 | Capacitor |
WO2023132212A1 (en) | 2022-01-06 | 2023-07-13 | 日本ケミコン株式会社 | Capacitor and method for manufacturing same |
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JPH11288849A (en) * | 1998-01-23 | 1999-10-19 | Matsushita Electric Ind Co Ltd | Electrode-metal material, capacitor using material thereof and manufacture thereof |
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JPS5226466A (en) * | 1975-08-25 | 1977-02-28 | Hitachi Condenser | Electrolytic capacitor |
JPH11288849A (en) * | 1998-01-23 | 1999-10-19 | Matsushita Electric Ind Co Ltd | Electrode-metal material, capacitor using material thereof and manufacture thereof |
JP2004186579A (en) * | 2002-12-05 | 2004-07-02 | Nippon Chemicon Corp | Electrolytic capacitor |
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