JPS6360524B2 - - Google Patents
Info
- Publication number
- JPS6360524B2 JPS6360524B2 JP56002412A JP241281A JPS6360524B2 JP S6360524 B2 JPS6360524 B2 JP S6360524B2 JP 56002412 A JP56002412 A JP 56002412A JP 241281 A JP241281 A JP 241281A JP S6360524 B2 JPS6360524 B2 JP S6360524B2
- Authority
- JP
- Japan
- Prior art keywords
- chemical
- aluminum foil
- chemical conversion
- foil
- phosphoric acid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
Links
- 239000000126 substance Substances 0.000 claims description 32
- 239000011888 foil Substances 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 17
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 12
- 229910052782 aluminium Inorganic materials 0.000 claims description 12
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 10
- WYXIGTJNYDDFFH-UHFFFAOYSA-Q triazanium;borate Chemical compound [NH4+].[NH4+].[NH4+].[O-]B([O-])[O-] WYXIGTJNYDDFFH-UHFFFAOYSA-Q 0.000 claims description 10
- 239000003990 capacitor Substances 0.000 claims description 6
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 230000005611 electricity Effects 0.000 claims description 3
- 238000000576 coating method Methods 0.000 description 10
- 230000015572 biosynthetic process Effects 0.000 description 8
- 239000011248 coating agent Substances 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 238000007739 conversion coating Methods 0.000 description 4
- 239000004254 Ammonium phosphate Substances 0.000 description 3
- 229910000148 ammonium phosphate Inorganic materials 0.000 description 3
- 235000019289 ammonium phosphates Nutrition 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000009835 boiling Methods 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 229910001593 boehmite Inorganic materials 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- -1 leakage current Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
Landscapes
- Electrochemical Coating By Surface Reaction (AREA)
Description
本発明は電解コンデンサ用アルミニウム箔の化
成方法に関するものである。
電解コンデンサ用アルミニウム箔はエツチング
工程で表面を粗面化させ、誘電体皮膜を付着せし
める化成工程へと移行される。この化成工程では
良質な誘電体皮膜を得るために様々な試みが実施
されている。その一例としてベーマイト皮膜と電
解皮膜の複合誘電体皮膜、焙焼皮膜と電解皮膜と
の複合誘電体皮膜、また２種以上の異つた化成液
を使用し化成を行い複合誘電体皮膜を作る等々の
方法がある。また皮膜の欠陥部修復あるいは漏れ
電流を減少せしめる工程として、中間焙焼あるい
は温水処理などによる中間処理によるデポライゼ
イシヨン（内部欠陥誘発）の処理を行つた後、再
化成による皮膜修復過程を経て製造される化成方
法がある。
しかしこれらの方法では漏れ電流、化成性など
において低下する要因があり、未だ充分満足でき
る段階には至つていない。
また一般にホウ酸アンモン系の化成皮膜は良質
なバリヤー型酸化皮膜を得るのに適しており、さ
らにかなり高い電圧まで安定した化成皮膜が得ら
れる特徴がある。従つて中高圧化成にはこのホウ
酸アンモン系の化成液はかなり一般に用いられて
いるのが現状である。
しかしこのホウ酸アンモン系化成液によつて得
られる化成皮膜は耐熱水性に対し著しく弱くなる
欠点を有しており、たとえば200Vまでホウ酸ア
ンモン系化成液によつて化成した箔を純水ボイル
処理を30〜60分行なうと、初期に耐圧が200Vあ
つたものが純水ボイル後ではわずかに５〜6Vま
でに低下してしまう。一方リン酸アンモン系で化
成した箔は同様の処理をしても、初期に200Vの
耐圧をもつたものなら195〜198Vまでにしか低下
しない。しかしリン酸アンモン系による化成は高
圧側においては著しく悪い特性を示し、ホウ酸ア
ンモン系の安定した皮膜と同様な皮膜を得るため
にはかなり困難な処理を行なわなければならない
欠点を有していた。
本発明は上述の欠点を解消し、漏れ電流、化成
性および損失などの電極箔の電気的特性を著しく
改善した電解コンデンサ用アルミニウム箔の化成
方法を提供しようとするものである。
すなわちアルミニウム箔をホウ酸アンモン系水
溶液に浸漬して化成処理する工程において、所定
の化成電圧に到達した後、該アルミニウム箔をリ
ン酸水溶液中に通電しないで、浸漬して引き上
げ、リン酸根が皮膜に付着したままの状態で、焙
焼処理する工程を含有したことを特徴とする電解
コンデンサ用アルミニウム箔の化成方法である。
以下、本発明をさらに詳述する。
上述のようにホウ酸アンモン系による化成皮膜
とリン酸アンモン系の化成皮膜のそれぞれの特質
を生かすことに着目し、本発明者は種々実験を繰
返した。
まずホウ酸アンモン系化成液による化成で設定
化成電圧まで到達した後、漏れ電流が順次減少し
てしぼれていく過程でのデボライゼイシヨンを誘
発する中間処理工程の直前にリン酸浸漬処理を行
ない、そのままリン酸根が皮膜に付着したままの
状態で中間焙焼処理を行なうと、該処理を行なわ
なかつたものと比べて化成箔の漏れ電流はかなり
減少しており、デポライゼイシヨンが充分行なわ
れたことにより、後の再化成工程による皮膜欠陥
修復もし易くなつたことが明らかになつた。また
併せて耐熱水性が向上し電解液とのなじみも改善
されていることが明らかになつた。
次にエツチングされた高純度アルミニウム箔を
用いて次の条件で電極箔を作成した。
実施例
ホウ酸アンモン系化成液による化成条件
化成液
組成：ホウ酸100ｇ／＋28％NH4OH
1.5c.c.／
比抵抗：300Ωcm（at85℃）
PH：6.8（at85℃）
液温：85℃
定電流化成：25ｍＡ／cm2
設定化成電圧：200V
上記条件により化成を行い、200V到達後15分
間化成する。
次いで、中間焙焼処理の前に75％リン酸３c.c.／
液（常温中）に通電しないで、３分間浸漬さ
せ、ただちに500℃で５分間中間焙焼を行い、そ
の後再びホウ酸アンモン系化成液によつて５分間
再化成し、化成を終了する。
結 果
上述の本発明の実施例および従来法による化成
箔を電解液中において、静電容量および箔損失を
測定し、また各々の化成箔を用いて定格160WV、
330μFの電解コンデンサを製作し、電気的特性を
測定した結果を表に示す。
The present invention relates to a method for forming aluminum foil for electrolytic capacitors. The surface of aluminum foil for electrolytic capacitors is roughened through an etching process, and then transferred to a chemical conversion process in which a dielectric film is attached. In this chemical formation process, various attempts have been made to obtain a high quality dielectric film. Examples include composite dielectric coatings of boehmite coating and electrolytic coating, composite dielectric coatings of roasted coating and electrolytic coating, and composite dielectric coatings made by chemical conversion using two or more different chemical solutions. There is a way. In addition, as a process for repairing defects in the coating or reducing leakage current, deporization (internal defect induction) is performed by intermediate processing such as intermediate roasting or hot water treatment, and then the coating is repaired by re-formation. There is a chemical method by which it is manufactured. However, these methods have factors that reduce leakage current, chemical formability, etc., and have not yet reached a fully satisfactory stage. In addition, ammonium borate-based chemical conversion coatings are generally suitable for obtaining high-quality barrier-type oxide coatings, and are also characterized by being able to provide stable chemical conversion coatings up to considerably high voltages. Therefore, at present, ammonium borate-based chemical liquids are quite commonly used in medium and high pressure chemical conversion. However, the chemical conversion film obtained with this ammonium borate-based chemical solution has the disadvantage of being extremely weak in hot water resistance. If this is done for 30 to 60 minutes, the initial breakdown voltage of 200V will drop to only 5 to 6V after boiling with pure water. On the other hand, even if foils chemically treated with ammonium phosphate are treated in the same way, if they initially had a withstand voltage of 200V, the voltage would only drop to 195-198V. However, chemical conversion using ammonium phosphate had extremely poor properties on the high pressure side, and had the disadvantage of requiring considerably difficult treatment in order to obtain a stable film similar to that of ammonium borate. . The present invention aims to eliminate the above-mentioned drawbacks and provide a method for forming an aluminum foil for an electrolytic capacitor, which significantly improves the electrical properties of the electrode foil, such as leakage current, chemical formability, and loss. That is, in the process of immersing aluminum foil in an ammonium borate aqueous solution for chemical conversion treatment, after reaching a predetermined chemical conversion voltage, the aluminum foil is immersed and pulled up in the phosphoric acid aqueous solution without applying electricity, and the phosphoric acid groups form a film. This is a method for chemically converting aluminum foil for electrolytic capacitors, characterized by including a step of roasting the aluminum foil while it remains attached to the aluminum foil. The present invention will be explained in further detail below. As mentioned above, the present inventors focused on taking advantage of the respective characteristics of ammonium borate-based chemical conversion coatings and ammonium phosphate-based chemical conversion coatings, and repeated various experiments. First, after reaching the set chemical formation voltage by chemical formation using an ammonium borate chemical liquid, phosphoric acid immersion treatment is performed immediately before the intermediate treatment process that induces devolization in the process where the leakage current gradually decreases and dries up. If the intermediate roasting treatment is performed while the phosphate radicals remain attached to the film, the leakage current of the chemically converted foil is considerably reduced compared to that without the treatment, indicating that sufficient deporization has occurred. It has become clear that this makes it easier to repair film defects in the subsequent re-forming process. It was also revealed that the hot water resistance was improved and the compatibility with the electrolyte was also improved. Next, an electrode foil was prepared using the etched high-purity aluminum foil under the following conditions. Example Chemical formation conditions using ammonium borate chemical liquid Composition of chemical liquid: 100 g of boric acid / +28% NH 4 OH 1.5 cc / Specific resistance: 300 Ωcm (at 85°C) PH: 6.8 (at 85°C) Liquid temperature: 85°C Constant current chemical formation : 25mA/cm 2 Setting chemical formation voltage: 200V Chemical formation is performed under the above conditions, and after reaching 200V, chemical formation is performed for 15 minutes. Then 3 c.c./75% phosphoric acid before intermediate roasting treatment
The product is immersed in the liquid (at room temperature) for 3 minutes without electricity, then immediately subjected to intermediate roasting at 500°C for 5 minutes, and then reconstituted with ammonium borate chemical solution for 5 minutes to complete the chemical conversion. Results The capacitance and foil loss of the chemically formed foils according to the embodiments of the present invention and the conventional method described above were measured in an electrolytic solution, and each chemically formed foil was used to measure the rated 160WV,
A 330μF electrolytic capacitor was manufactured and the electrical characteristics were measured.The results are shown in the table.
【表】
※は純水ボイル１時間後の耐圧を示す。
以上ように本発明法によつて化成した箔は耐熱
水性においても電解液のなじみにもすぐれてお
り、また製品化した場合においても静電容量、損
失（tanδ）、漏れ電流共に従来法と比較して著し
く改善されていることが確認され、品質改善に大
きく寄与し、工業的ならびに実用的な価値の大な
るものがある。[Table] * indicates the pressure resistance after 1 hour of pure water boiling.
As mentioned above, the foil chemically formed by the method of the present invention has excellent hot water resistance and electrolyte compatibility, and when commercialized, the capacitance, loss (tan δ), and leakage current are compared with the conventional method. It has been confirmed that the process has been significantly improved, making a significant contribution to quality improvement, and having great industrial and practical value.
Claims (1)
浸漬して化成処理する工程において、所定の化成
電圧に到達した後、該アルミニウム箔をリン酸水
溶液中に通電しないで浸漬して引き上げ、リン酸
根が皮膜に付着したままの状態で、焙焼処理する
工程を含有したことを特徴とする電解コンデンサ
用アルミニウム箔の化成方法。1 In the process of immersing aluminum foil in an ammonium borate aqueous solution for chemical conversion treatment, after reaching a predetermined chemical conversion voltage, the aluminum foil is immersed in a phosphoric acid aqueous solution without electricity and pulled up, so that the phosphoric acid groups form a film. 1. A method for forming aluminum foil for electrolytic capacitors, comprising a step of roasting the foil while it is still attached.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP241281A JPS57115815A (en) | 1981-01-09 | 1981-01-09 | Method of compounding aluminum foil for electrolytic condenser |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP241281A JPS57115815A (en) | 1981-01-09 | 1981-01-09 | Method of compounding aluminum foil for electrolytic condenser |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS57115815A JPS57115815A (en) | 1982-07-19 |
| JPS6360524B2 true JPS6360524B2 (en) | 1988-11-24 |
Family
ID=11528525
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP241281A Granted JPS57115815A (en) | 1981-01-09 | 1981-01-09 | Method of compounding aluminum foil for electrolytic condenser |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS57115815A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02274451A (en) * | 1989-04-14 | 1990-11-08 | Tsudakoma Corp | Pallet exchange system of machine tool and connector used therein |
| CN110073037A (en) * | 2016-12-16 | 2019-07-30 | 株式会社Uacj | The manufacturing method and manufacturing device of electrolytic aluminum foil |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4470885A (en) * | 1983-02-07 | 1984-09-11 | Sprague Electric Company | Process for treating aluminum electrolytic capacitor foil |
| JPS6043812A (en) * | 1983-08-19 | 1985-03-08 | 松下電器産業株式会社 | Method of compounding aluminum electrolytic condenser electrode foil |
| US4537665A (en) * | 1984-09-04 | 1985-08-27 | Sprague Electric Company | Production of aluminum foil capacitor electrodes |
| US4582574A (en) * | 1985-08-15 | 1986-04-15 | Sprague Electric Company | Preparation of capacitor electrodes |
| JPS63146424A (en) * | 1986-12-10 | 1988-06-18 | 松下電器産業株式会社 | Manufacture of electrode foil for aluminum electrolytic capacitor |
| CN107287638A (en) * | 2017-07-11 | 2017-10-24 | 新疆金泰新材料技术有限公司 | Formation method of electrode foil resistant to large ripple current |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5245547A (en) * | 1975-10-08 | 1977-04-11 | Elna Co Ltd | Process for anodizing aluminum for electrolytic condenser |
-
1981
- 1981-01-09 JP JP241281A patent/JPS57115815A/en active Granted
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5245547A (en) * | 1975-10-08 | 1977-04-11 | Elna Co Ltd | Process for anodizing aluminum for electrolytic condenser |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02274451A (en) * | 1989-04-14 | 1990-11-08 | Tsudakoma Corp | Pallet exchange system of machine tool and connector used therein |
| CN110073037A (en) * | 2016-12-16 | 2019-07-30 | 株式会社Uacj | The manufacturing method and manufacturing device of electrolytic aluminum foil |
| CN110073037B (en) * | 2016-12-16 | 2021-04-30 | 株式会社Uacj | Method and apparatus for manufacturing electrolytic aluminum foil |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS57115815A (en) | 1982-07-19 |
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