JP4653687B2 - Method for producing electrode foil for electrolytic capacitor - Google Patents
Method for producing electrode foil for electrolytic capacitor Download PDFInfo
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- JP4653687B2 JP4653687B2 JP2006099154A JP2006099154A JP4653687B2 JP 4653687 B2 JP4653687 B2 JP 4653687B2 JP 2006099154 A JP2006099154 A JP 2006099154A JP 2006099154 A JP2006099154 A JP 2006099154A JP 4653687 B2 JP4653687 B2 JP 4653687B2
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- 239000011888 foil Substances 0.000 title claims description 30
- 239000003990 capacitor Substances 0.000 title claims description 14
- 238000004519 manufacturing process Methods 0.000 title claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 22
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 16
- 229910052782 aluminium Inorganic materials 0.000 claims description 16
- 238000007743 anodising Methods 0.000 claims description 12
- WYXIGTJNYDDFFH-UHFFFAOYSA-Q triazanium;borate Chemical compound [NH4+].[NH4+].[NH4+].[O-]B([O-])[O-] WYXIGTJNYDDFFH-UHFFFAOYSA-Q 0.000 claims description 11
- 230000003647 oxidation Effects 0.000 claims description 9
- 238000007254 oxidation reaction Methods 0.000 claims description 9
- NGPGDYLVALNKEG-UHFFFAOYSA-N azanium;azane;2,3,4-trihydroxy-4-oxobutanoate Chemical compound [NH4+].[NH4+].[O-]C(=O)C(O)C(O)C([O-])=O NGPGDYLVALNKEG-UHFFFAOYSA-N 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 20
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 9
- 238000002048 anodisation reaction Methods 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 5
- 238000002425 crystallisation Methods 0.000 description 5
- 230000008025 crystallization Effects 0.000 description 5
- 230000006866 deterioration Effects 0.000 description 5
- 238000005530 etching Methods 0.000 description 5
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 4
- 239000004327 boric acid Substances 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- FLDCSPABIQBYKP-UHFFFAOYSA-N 5-chloro-1,2-dimethylbenzimidazole Chemical compound ClC1=CC=C2N(C)C(C)=NC2=C1 FLDCSPABIQBYKP-UHFFFAOYSA-N 0.000 description 3
- 239000001741 Ammonium adipate Substances 0.000 description 3
- 235000019293 ammonium adipate Nutrition 0.000 description 3
- 235000006408 oxalic acid Nutrition 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- WMYWOWFOOVUPFY-UHFFFAOYSA-L dihydroxy(dioxo)chromium;phosphoric acid Chemical compound OP(O)(O)=O.O[Cr](O)(=O)=O WMYWOWFOOVUPFY-UHFFFAOYSA-L 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
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Description
本発明は、電解コンデンサ用の電極箔の製造方法に関するものである。 The present invention relates to a method for producing an electrode foil for an electrolytic capacitor.
従来、電解コンデンサに使用される陽極箔はエッチング処理を施した高純度のアルミニウム箔をホウ酸アンモニウム水溶液中に浸漬し、陽極酸化することにより生成した結晶性の酸化皮膜を誘電体として利用している。
また、所定の電圧到達後、加熱処理や酸浸漬処理により陽極酸化皮膜中のボイドおよびクラックなどを露呈させ、更に再化成を繰り返すことにより陽極酸化皮膜を生成させている（非特許文献１参照）。
Conventionally, an anode foil used for an electrolytic capacitor is obtained by immersing a high-purity aluminum foil subjected to an etching treatment in an aqueous ammonium borate solution and anodizing the crystalline oxide film as a dielectric. Yes.
Moreover, after reaching a predetermined voltage, voids and cracks in the anodized film are exposed by heat treatment or acid dipping treatment, and further, re-forming is repeated to generate an anodized film (see Non-Patent Document 1). .
しかしながら、近年、電子機器の高性能化、長寿命化が進み、電解コンデンサにも高い信頼性が求められている。それに伴い電解コンデンサ用電極箔においても、耐充放電や耐リプル特性に優れた非晶質皮膜の形成が求められている。 However, in recent years, electronic devices have been improved in performance and life, and electrolytic capacitors are also required to have high reliability. Accordingly, formation of an amorphous film excellent in charge / discharge resistance and ripple resistance is also demanded in electrode foils for electrolytic capacitors.
このような非晶質皮膜の電解コンデンサ用電極箔を製造するにあたって、従来は、エッチングされたアルミニウム箔をシュウ酸や硫酸等の酸性水溶液中で陽極酸化してポーラス型皮膜を形成し、その後、ホウ酸アンモニウム、アジピン酸アンモニウム等の中性水溶液中で陽極酸化を行い、バリアー型皮膜を形成している（特許文献１参照）。
従来、中高圧の電圧領域での非晶質皮膜の製造方法は、シュウ酸や硫酸等の水溶液中でポーラス型皮膜を形成する工程と、その後、ホウ酸アンモニウム、アジピン酸アンモニウム等の水溶液中でバリアー型皮膜を形成する工程とからなっている。ここで、ポーラス型皮膜を形成せず、ホウ酸アンモニウムやアジピン酸アンモニウム等の水溶液中で中高圧の電圧領域まで陽極酸化を行うと、ボイドやクラックを多く有する結晶性の酸化皮膜が形成される。
よって、バリアー型皮膜形成前にポーラス型皮膜を形成することが必要であり、この形成方法により、結晶化が抑制され、非晶質皮膜の形成が可能となる。
Conventionally, a method for producing an amorphous film in a medium to high voltage range includes a step of forming a porous film in an aqueous solution of oxalic acid or sulfuric acid, and then an aqueous solution of ammonium borate, ammonium adipate, or the like. And a step of forming a barrier-type film. Here, when a anodic oxidation is performed up to a medium to high voltage region in an aqueous solution such as ammonium borate or ammonium adipate without forming a porous film, a crystalline oxide film having many voids and cracks is formed. .
Therefore, it is necessary to form a porous-type film before forming the barrier-type film, and this formation method suppresses crystallization and enables formation of an amorphous film.
ここに、本発明者は、シュウ酸や硫酸等の酸性水溶液中での陽極酸化により形成したポーラス型皮膜を利用した従来の非晶質皮膜製造方法とは異なる方法で非晶質皮膜を形成しようとするものである。 Here, the present inventor intends to form an amorphous film by a method different from a conventional amorphous film manufacturing method using a porous film formed by anodic oxidation in an acidic aqueous solution such as oxalic acid or sulfuric acid. It is what.
すなわち、本発明の課題は、中性水溶液中での陽極酸化を利用して、バリアー型皮膜のみで非晶質皮膜を形成可能にした中高圧電解コンデンサ用電極箔の製造方法を提供することにある。 That is, an object of the present invention is to provide a method for producing an electrode foil for medium- and high-voltage electrolytic capacitors that enables an amorphous film to be formed only by a barrier-type film using anodization in a neutral aqueous solution. is there.
上記課題を解決するために、本発明に係る電解コンデンサ用電極箔の製造方法では、アルミニウム箔を酒石酸アンモニウム水溶液中で陽極酸化し、皮膜を形成する第１の陽極酸化工程と、前記第１の陽極酸化工程の後、当該第１の陽極酸化より高い電圧までホウ酸アンモニウム水溶液中で陽極酸化し、皮膜を形成する第２の陽極酸化工程とを有することを特徴とする。 In order to solve the above-mentioned problems, in the method for producing an electrode foil for an electrolytic capacitor according to the present invention, a first anodizing step in which an aluminum foil is anodized in an aqueous solution of ammonium tartrate to form a film; After the anodizing step, the second anodizing step of forming a film by anodizing in an aqueous ammonium borate solution to a voltage higher than that of the first anodizing.
本発明では、ホウ酸アンモニウム水溶液中で陽極酸化する前に、酒石酸アンモニウム水溶液中で陽極酸化を行うため、酒石酸アンモニウム水溶液による酸化皮膜を形成後、ホウ酸アンモニウム水溶液中で陽極酸化を行う際の結晶化を抑制でき、非晶質皮膜の形成が可能となる。 In the present invention, since anodization is performed in an ammonium tartrate aqueous solution before anodization in the ammonium borate aqueous solution, after forming an oxide film with the ammonium tartrate aqueous solution, crystals when anodizing in the ammonium borate aqueous solution are performed. The formation of an amorphous film is possible.
本発明は、前記アルミニウム箔として、表面がエッチングにより粗面化されたものに適用できる他、表面がエッチングにより粗面化されていないものにも適用できる。 The present invention can be applied not only to the aluminum foil whose surface is roughened by etching, but also to the aluminum foil whose surface is not roughened by etching.
本発明において、前記第１の陽極酸化工程の前に、前記アルミニウム箔表面上に形成されている自然酸化皮膜を除去することが好ましい。
アルミニウムは酸素との化学親和性が強く、箔表面は自然酸化皮膜に覆われている。自然酸化皮膜は結晶化の核となるため、この皮膜を除去することにより、さらに結晶化を抑制することができる。
In the present invention, it is preferable to remove the natural oxide film formed on the surface of the aluminum foil before the first anodic oxidation step.
Aluminum has a strong chemical affinity with oxygen, and the foil surface is covered with a natural oxide film. Since the natural oxide film becomes the nucleus of crystallization, crystallization can be further suppressed by removing this film.
本発明では、ホウ酸アンモニウム水溶液中で陽極酸化する前に、酒石酸アンモニウム水溶液中で陽極酸化を行うため、酒石酸アンモニウム水溶液による酸化皮膜を形成後、ホウ酸アンモニウム水溶液中で陽極酸化を行う際の結晶化を抑制でき、非晶質皮膜の形成が可能となる。
また、アルミニウム箔表面に形成されている自然酸化皮膜は、結晶化の核となるため、この皮膜を除去した後、陽極酸化を行えば、さらに結晶化を抑制することができる。
上記の非晶質皮膜を形成したアルミニウム箔を電極箔に用いた電解コンデンサでは、漏れ電流の低減を図ることができる。
In the present invention, since anodization is performed in an aqueous solution of ammonium tartrate before anodization in an aqueous solution of ammonium borate, an oxide film is formed using the aqueous solution of ammonium tartrate, and then crystals are formed when anodization is performed in the aqueous solution of ammonium borate. The formation of an amorphous film is possible.
Moreover, since the natural oxide film formed on the surface of the aluminum foil serves as a nucleus for crystallization, crystallization can be further suppressed by performing anodic oxidation after removing this film.
In the electrolytic capacitor using the aluminum foil having the above amorphous film as the electrode foil, the leakage current can be reduced.
以下、実施例に基づいて本発明をより具体的に説明する。 Hereinafter, based on an Example, this invention is demonstrated more concretely.
［実施例１］
エッチングされたアルミニウム箔を９０℃のリン酸−クロム酸混合溶液中に浸漬し、表面上の自然酸化皮膜を溶解除去する（皮膜除去工程）。
[Example 1]
The etched aluminum foil is immersed in a phosphoric acid-chromic acid mixed solution at 90 ° C., and the natural oxide film on the surface is dissolved and removed (film removal step).
次に、３ｇ／Ｌ酒石酸アンモニウム水溶液中（液温２５℃）に自然酸化皮膜を除去したアルミニウムエッチング箔を浸漬し、電流密度５０ｍＡ／ｃｍ2の直流電流で電圧３００Ｖまで陽極酸化を行い、３００Ｖ到達後、定電圧で５分間保持することにより皮膜を生成する（第１の陽極酸化工程）。 Next, an aluminum etching foil from which a natural oxide film was removed was immersed in a 3 g / L ammonium tartrate aqueous solution (liquid temperature: 25 ° C.), and anodized to a voltage of 300 V with a direct current of 50 mA / cm 2 in current density, reaching 300 V. Thereafter, the film is formed by holding at a constant voltage for 5 minutes (first anodic oxidation step).
次に、３０ｇ／Ｌのホウ酸に０．５ｍｌ／Ｌのアンモニア水を添加した水溶液中（液温２５℃）に、上記の第１の陽極酸化工程を施したアルミニウムエッチング箔を浸漬し、電流密度２０ｍＡ／ｃｍ2の直流電流で電圧６００Ｖまで陽極酸化を行い、６００Ｖ到達後、定電圧で３０分間保持する（第２の陽極酸化工程）。
次に、加熱処理や酸浸漬処理により酸化皮膜中のボイド、クラックを露呈させ、上記ホウ酸アンモニウム水溶液中で再化成を数回行い、電極箔試料を作製した。
Next, the aluminum etching foil subjected to the first anodic oxidation step is immersed in an aqueous solution (liquid temperature 25 ° C.) obtained by adding 0.5 ml / L ammonia water to 30 g / L boric acid, Anodization is performed up to a voltage of 600 V with a direct current of density 20 mA / cm 2 , and after reaching 600 V, a constant voltage is maintained for 30 minutes (second anodization step).
Next, voids and cracks in the oxide film were exposed by heat treatment or acid immersion treatment, and re-chemical conversion was performed several times in the aqueous ammonium borate solution to prepare an electrode foil sample.
［実施例２］
上記の皮膜除去を行わなかった以外は、実施例１と同様にして、電極箔試料を作製した。
[Example 2]
An electrode foil sample was prepared in the same manner as in Example 1 except that the above film removal was not performed.
（比較例）
実施例１と同様に皮膜除去を行ったが、酒石酸アンモニウム水溶液による第１の陽極酸化は行わず、ホウ酸にアンモニア水を添加した水溶液による、第２の陽極酸化を実施例１と同様に行って、電極箔試料を作製した。
(Comparative example)
The film was removed in the same manner as in Example 1, but the first anodic oxidation with an aqueous ammonium tartrate solution was not performed, and the second anodic oxidation with an aqueous solution in which ammonia water was added to boric acid was performed in the same manner as in Example 1. Thus, an electrode foil sample was prepared.
上記した本発明の実施例１、２、比較例の電極箔試料について、７０ｇ／Ｌのホウ酸水溶液中で５０Ｖ刻みに印加電圧を上昇させて各電圧における１８０秒後の漏れ電流値を測定した結果を図１に示す。 For the electrode foil samples of Examples 1 and 2 and Comparative Example of the present invention described above, the applied voltage was increased in increments of 50 V in a 70 g / L boric acid aqueous solution, and the leakage current value after 180 seconds at each voltage was measured. The results are shown in FIG.
また、上記の電極箔試料の耐電圧を測定後、沸騰した１０ｍｌ／Ｌの硫酸中に１５分間浸漬した後、水洗・乾燥し、その後、７０ｇ／Ｌのホウ酸水溶液中に浸漬し、電流密度１０ｍＡ／ｃｍ２の直流電流を印加し、６０秒後の電圧値を測定した。次に、以下の式
硫酸ボイル劣化率（％）＝｛（耐電圧−６０秒後の電圧値）／耐電圧｝×１００
から皮膜の劣化率（％）を求めた。その結果を表１に示す。
In addition, after measuring the withstand voltage of the electrode foil sample, it was immersed in boiling 10 ml / L sulfuric acid for 15 minutes, washed and dried, and then immersed in a 70 g / L boric acid aqueous solution. A direct current of 10 mA / cm 2 was applied, and the voltage value after 60 seconds was measured. Next, the following formula: sulfuric acid boil sulfate deterioration rate (%) = {(withstand voltage−voltage value after 60 seconds) / withstand voltage} × 100
From this, the deterioration rate (%) of the film was determined. The results are shown in Table 1.
図１に示すように、本発明の実施例１では、比較例より漏れ電流が低減している。また、表１に示すように、実施例１は比較例より硫酸ボイル劣化率が低減している。
結晶性酸化皮膜は、皮膜の結晶化に伴い、結晶部の周りにボイド（欠陥）を有しており、硫酸によって皮膜が溶解しやすい構造となっている。一方、非晶質皮膜は、結晶部がなく均一な皮膜であり、硫酸によって皮膜が溶解しにくい構造となっている。
従って、硫酸ボイル劣化率が高い（皮膜の溶解量が多い）程、皮膜中の結晶性酸化皮膜の割合が高く、また、硫酸ボイル劣化率が低い（皮膜の溶解が少ない）程、皮膜中の結晶性酸化皮膜の割合が低い。すなわち、非晶質皮膜の割合が高く、コンデンサでの耐充放電特性やリプル特性に優れている。
よって、実施例１、２は比較例より非晶質皮膜の割合が高く、耐充放電特性やリプル特性に優れているといえる。
As shown in FIG. 1, in Example 1 of the present invention, the leakage current is reduced as compared with the comparative example. Moreover, as shown in Table 1, Example 1 has a lower sulfuric acid boil deterioration rate than the comparative example.
The crystalline oxide film has voids (defects) around the crystal part as the film crystallizes, and has a structure in which the film is easily dissolved by sulfuric acid. On the other hand, the amorphous film is a uniform film having no crystal part and has a structure in which the film is difficult to dissolve by sulfuric acid.
Therefore, the higher the sulfuric acid boil deterioration rate (the more the film dissolves), the higher the ratio of the crystalline oxide film in the film, and the lower the sulfuric acid boil deterioration rate (the less the film dissolves), Low percentage of crystalline oxide film. That is, the ratio of the amorphous film is high, and the capacitor is excellent in charge / discharge resistance characteristics and ripple characteristics.
Accordingly, it can be said that Examples 1 and 2 have a higher proportion of the amorphous film than the comparative example, and are excellent in charge / discharge resistance characteristics and ripple characteristics.
Claims (2)
前記第１の陽極酸化工程の後、当該第１の陽極酸化より高い電圧までホウ酸アンモニウム水溶液中で陽極酸化し、皮膜を形成する第２の陽極酸化工程とを有することを特徴とする電解コンデンサ用電極箔の製造方法。 A first anodizing step in which an aluminum foil is anodized in an aqueous ammonium tartrate solution to form a film;
An electrolytic capacitor comprising: a second anodizing step for anodizing in an aqueous solution of ammonium borate to a voltage higher than that of the first anodizing step to form a film after the first anodizing step. Of manufacturing electrode foil for use.
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| JP5144206B2 (en) * | 2007-10-19 | 2013-02-13 | 三菱アルミニウム株式会社 | Method for producing surface-treated aluminum material |
| JP5352204B2 (en) * | 2008-11-25 | 2013-11-27 | 三菱アルミニウム株式会社 | Surface-treated aluminum material for vacuum equipment |
| CN106463266A (en) * | 2014-05-01 | 2017-02-22 | 昭和电工株式会社 | Method for manufacturing tungsten-based capacitor element |
| CN107354498B (en) * | 2017-07-18 | 2019-04-30 | 丰宾电子（深圳）有限公司 | A kind of manufacturing method of the electrode foil for aluminum electrolytic capacitors of high pressure high capacity |
| JPWO2021192607A1 (en) * | 2020-03-27 | 2021-09-30 | ||
| CN113436891A (en) * | 2021-06-15 | 2021-09-24 | 桂林理工大学 | Method for inducing medium-high voltage anode foil to uniformly corrode and form pores by adopting nano pits after anodic oxidation |
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| JPH02267915A (en) * | 1989-04-07 | 1990-11-01 | Hitachi Aic Inc | Manufacture of solid-state electrolytic capacitor |
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| JP2000252169A (en) * | 1999-02-26 | 2000-09-14 | Hitachi Aic Inc | Manufacture of solid electrolytic capacitor |
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