JP2629241B2 - Manufacturing method of electrode foil for aluminum electrolytic capacitor - Google Patents
Manufacturing method of electrode foil for aluminum electrolytic capacitorInfo
- Publication number
- JP2629241B2 JP2629241B2 JP3814188A JP3814188A JP2629241B2 JP 2629241 B2 JP2629241 B2 JP 2629241B2 JP 3814188 A JP3814188 A JP 3814188A JP 3814188 A JP3814188 A JP 3814188A JP 2629241 B2 JP2629241 B2 JP 2629241B2
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- Prior art keywords
- etching
- stage
- acid
- aqueous solution
- electrode foil
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Description
【発明の詳細な説明】 産業上の利用分野 本発明はアルミ電解コンデンサ用電極箔の製造方法に
関するものである。Description: TECHNICAL FIELD The present invention relates to a method for manufacturing an electrode foil for an aluminum electrolytic capacitor.
従来の技術 従来、アルミ電解コンデンサ用電極箔は、コンデンサ
の小形化，低価格化を図る為に、電極体となるアルミニ
ウム箔を電気化学的，あるいは化学的にエッチング処理
して表面積を拡大したものを使用している。2. Description of the Related Art Conventionally, electrode foils for aluminum electrolytic capacitors have been obtained by electrochemically or chemically etching an aluminum foil serving as an electrode body to increase the surface area in order to reduce the size and cost of the capacitor. You are using
発明が解決しようとする課題 このアルミニウム電極箔の表面積を拡大する為に種々
の方法が研究されているが、アルミニウム電極箔の機械
的強度を保持したまま表面積を拡大することは非常に困
難であった。すなわち、従来のエッチング技術では、一
般的に表面積を拡大するためにエッチング孔の密度を増
大させようとすると、同時にアルミニウム電極箔の表面
溶解も進行して期待出来る程表面積が増大しないばかり
か、アルミニウム電極箔の機械的強度も損なわれるとい
う問題があった。Problems to be Solved by the Invention Various methods have been studied to increase the surface area of this aluminum electrode foil, but it is very difficult to increase the surface area while maintaining the mechanical strength of the aluminum electrode foil. Was. That is, in the conventional etching technique, generally, when the density of the etching holes is increased in order to increase the surface area, the surface dissolution of the aluminum electrode foil also proceeds at the same time, and the surface area does not increase as much as expected. There was a problem that the mechanical strength of the electrode foil was also impaired.
本発明は上記の問題点を解決するもので、アルミニウ
ム電極箔の機械的強度を保持しつつ、エッチング孔の密
度を増大させ、表面積を拡大出来るアルミニウム電解コ
ンデンサ用電極箔の製造方法を提供するものである。The present invention solves the above problems, and provides a method for manufacturing an electrode foil for an aluminum electrolytic capacitor that can increase the density of etching holes and increase the surface area while maintaining the mechanical strength of the aluminum electrode foil. It is.
課題を解決するための手段 本発明はこのような従来の問題点を解決するものであ
り、塩化カリウム，塩化ナトリウム，塩化アンモニウム
のうち少なくとも１種0.1〜10％を含む水溶液中で直流
エッチングする第１段エッチング工程と、塩酸２〜15％
に硫酸，蓚酸，リン酸からなる多孔質皮膜生成酸のうち
少なくとも１種５〜35％を添加した水溶液中で直流エッ
チングする第２段エッチング工程と、塩酸２〜15％もし
くはそれに硫酸，蓚酸，リン酸からなる多孔質皮膜生成
酸のうち少なくとも１種を３％以下添加した水溶液中で
直流エッチングするか、または浸漬処理する第３段エッ
チング工程を有するものである。Means for Solving the Problems The present invention is to solve such a conventional problem and is directed to direct current etching in an aqueous solution containing 0.1 to 10% of at least one of potassium chloride, sodium chloride and ammonium chloride. One-step etching process and 2-15% hydrochloric acid
A second-stage etching step in which DC etching is performed in an aqueous solution in which at least one of a porous film-forming acid composed of sulfuric acid, oxalic acid, and phosphoric acid is added, and 2 to 15% of hydrochloric acid or sulfuric acid, oxalic acid, It has a third etching step in which DC etching or immersion treatment is performed in an aqueous solution to which at least one kind of a porous film-forming acid made of phosphoric acid is added at 3% or less.
作 用 この様な本発明の構成によれば、第１段エッチングに
塩化カリウム，塩化ナトリウム，塩化アンモニウムの中
性塩のうち少なくとも１種類を含む水溶液を用いている
ため、アルミニウム箔表面の化学的に活性な部分、すな
わち表面酸化皮膜に多数存在する欠陥部等からまずエッ
チング孔が発生する。続いて行なう第２段エッチングで
は塩酸に硫酸，蓚酸，リン酸からなる多孔質皮膜生成酸
のうち少なくとも１種類を添加した水溶液を用いている
ため、第１段エッチングではエッチング孔が発生しなか
った比較的欠点部の少ない表面にまず多孔質皮膜が生成
し、その孔の部分を塩素イオンが侵食して、更に多数の
エッチング孔が発生する。According to the configuration of the present invention, since the aqueous solution containing at least one of potassium chloride, sodium chloride, and neutral salt of ammonium chloride is used for the first-stage etching, chemical etching of the aluminum foil surface is prevented. First, an etching hole is generated from an active portion, that is, a defect portion or the like present in a large number of surface oxide films. In the subsequent second-stage etching, an aqueous solution in which at least one of a porous film-forming acid composed of sulfuric acid, oxalic acid and phosphoric acid was added to hydrochloric acid was used, so that no etching holes were generated in the first-stage etching. First, a porous film is formed on the surface having relatively few defects, and the pores are eroded by chlorine ions, so that more etching holes are generated.
そして、第３段エッチングでは塩酸または塩酸に硫
酸，蓚酸，リン酸からなる多孔質皮膜生成酸のうち少な
くとも１種類を添加した水溶液中で比較的低電流密度で
エッチングするか、または侵漬処理をるため、第１段お
よび第２段エッチングで発生したエッチング孔が効果的
に拡大される。In the third-stage etching, etching is performed at a relatively low current density in an aqueous solution in which at least one of a porous film-forming acid composed of sulfuric acid, oxalic acid, and phosphoric acid is added to hydrochloric acid or hydrochloric acid, or immersion treatment is performed. Therefore, the etching holes generated in the first and second etching steps are effectively enlarged.
そのため、表面溶解が少なく機械的強度を保持したま
ま、高密度で充分な太さの径をもったエッチング孔を均
一な分布で発生させることが出来る。Therefore, it is possible to generate etching holes having a high density and a sufficiently large diameter in a uniform distribution while maintaining the mechanical strength with little surface dissolution.
実施例 以下に本発明の第１段エッチング工程、第２段エッチ
ング工程、第３段エッチング工程につき、それぞれ具体
的にエッチング条件を説明する。EXAMPLES Hereinafter, the etching conditions of the first-stage etching process, the second-stage etching process, and the third-stage etching process of the present invention will be specifically described.
第１段エッチング工程 エッチング孔を高密度かつ均一に生成させるために塩
化カリウム，塩化ナトリウム，塩化アンモニウムのうち
の少なくとも１種類を含む水溶液を用いた直流エッチン
グが必要である。First-stage etching step DC etching using an aqueous solution containing at least one of potassium chloride, sodium chloride and ammonium chloride is necessary in order to form etching holes with high density and uniformity.
前述のいずれの中性塩の水溶液の場合でも、その濃度
が0.1％未満ではエッチグ効果が小さく、10％を超える
と表面の全面溶解が起こる。従って0.1〜10％の範囲内
で、特に１〜５％が好ましい。この様な好適範囲内で
は、表面溶解をほとんど起こすことなく高密度かつ均一
なエッチング孔を発生させることが出来る。In the case of any of the above neutral salt aqueous solutions, if the concentration is less than 0.1%, the etching effect is small, and if it exceeds 10%, the entire surface is dissolved. Therefore, within the range of 0.1 to 10%, particularly preferably 1 to 5%. Within such a preferable range, a high-density and uniform etching hole can be generated with almost no surface melting.
エッチング液温も重要な影響を及ぼし、50℃未満では
エッチング効果が小さく、10℃を超えると表面の全面溶
解が起こる。従って50〜100℃の範囲内で特に70〜90％
が好ましい。The temperature of the etching solution also has an important effect. If the temperature is lower than 50 ° C., the etching effect is small, and if it exceeds 10 ° C., the entire surface of the surface is dissolved. Therefore, especially in the range of 50-100 ° C, 70-90%
Is preferred.
また、電流密度は5A/dm2未満ではエッチング効果が小
さく、70A/dm2を超えると表面の全面溶解が起こる。従
って５〜70A/dm2の範囲内特に８〜30OA/dm2が好まし
い。When the current density is less than 5 A / dm 2 , the etching effect is small, and when the current density exceeds 70 A / dm 2 , the entire surface is dissolved. Thus the range of 5~70A / dm 2, especially 8~30OA / dm 2 is preferred.
第２段エッチング工程 表面溶解を抑制しながら、更にエッチング孔を発生，
増加させる為に、塩酸に硫酸，蓚酸，リン酸からなる多
孔質皮膜生成酸のうち少なくとも１種類を添加した水溶
液を用いた直流エッチングが必要である。塩酸濃度は２
％未満であるとエッチング効果が小さく、15％を超える
と表面の全面溶解が起こる。従って２〜15％の範囲内
で、特に３〜８％が好ましい。多孔質皮膜を生成し得る
酸の添加量については、硫酸，蓚酸，リン酸のいずれの
場合も５％未満であると多孔質皮膜の生成が不充分であ
り、35％を超えると皮膜生成反応よりむしろ溶解反応が
強くなって表面の全面溶解が起こる。Second etching step Generates more etching holes while suppressing surface dissolution,
To increase the amount, direct current etching using an aqueous solution obtained by adding at least one of a porous film-forming acid composed of sulfuric acid, oxalic acid, and phosphoric acid to hydrochloric acid is required. Hydrochloric acid concentration is 2
%, The etching effect is small, and if it exceeds 15%, the entire surface is dissolved. Therefore, within the range of 2 to 15%, particularly 3 to 8% is preferable. Regarding the amount of acid that can form the porous film, if the amount of sulfuric acid, oxalic acid, or phosphoric acid is less than 5%, the formation of the porous film is insufficient. Rather, the dissolution reaction becomes stronger and the entire surface is dissolved.
従って５〜35％の範囲内で、特に15〜25％が好まし
い。この様な好適範囲内では高密度かつ均一な孔を持つ
多孔質皮膜がアルミ箔表面に生成し、その孔の部分を塩
素イオンが侵食してエッチング孔が形成されるが、一方
孔以外の部分は皮膜で覆われているから表面溶解が抑制
され、結果的に第１段エッチングで出来たエッチング孔
を破壊することなしに新たな均一なエッチング孔を発生
させせることが出来る。Therefore, within the range of 5 to 35%, particularly 15 to 25% is preferable. Within such a preferred range, a porous film having high density and uniform pores is formed on the aluminum foil surface, and the pores are eroded by chlorine ions to form etching holes. Since the surface is covered with the film, surface dissolution is suppressed, and as a result, a new uniform etching hole can be generated without destroying the etching hole formed by the first-stage etching.
第１段エッチングと同様の理由から、液温は50〜100
℃の範囲が良く、特に70〜90℃が好ましい。また電流密
度についても、第１段エッチングと同様、５〜70A/dm2
の範囲が良いが、特に10〜40A/dm2が好ましい。For the same reason as the first stage etching, the liquid temperature is 50-100
The temperature range is good, and 70 to 90 ° C is particularly preferable. The current density was 5 to 70 A / dm 2 , as in the first stage etching.
Is good, but 10 to 40 A / dm 2 is particularly preferable.
第３段エッチング工程 第１段および第２段エッチングで発生したエッチング
孔を効果的に拡大するために、塩酸のみかまたは塩酸に
硫酸，蓚酸，リン酸からなる多孔質皮膜生成酸のうち少
なくとも１種類を少量添加した水溶液中で直流エッチン
グするか、または浸漬処理をすることが必要である。塩
酸濃度は２％未満であるとエッチング効果が小さく、15
％を超えると表面の全面溶解が起こる。Third-stage etching step In order to effectively enlarge the etching holes generated in the first-stage and second-stage etching, at least one of hydrochloric acid alone and a porous film-forming acid composed of sulfuric acid, oxalic acid and phosphoric acid is added to hydrochloric acid. It is necessary to perform direct current etching or immersion treatment in an aqueous solution to which a small amount of a type is added. If the hydrochloric acid concentration is less than 2%, the etching effect is small, and
%, The entire surface is dissolved.
従って２〜15％の範囲内で、特に３〜８％が好まし
い。多孔質皮膜を生成し得る酸の添加については、無く
ても良いが、添加する場合は、硫酸，蓚酸，リン酸のい
ずれの場合も３％を超えると皮膜生成反応により溶解反
応がおさえられ、エッチング効果が小さくなる。Therefore, within the range of 2 to 15%, particularly 3 to 8% is preferable. The addition of an acid capable of forming a porous film may be omitted. However, in the case of adding sulfuric acid, oxalic acid, or phosphoric acid, if it exceeds 3%, the dissolution reaction is suppressed by the film forming reaction, The etching effect is reduced.
従って０〜３％の範囲内で、特に0.01〜0.5％が好ま
しい。Therefore, within the range of 0 to 3%, particularly 0.01 to 0.5% is preferable.
この様な好適範囲内では第１段および第２段エッチン
グで発生したエッチング孔の破壊や、無駄な表面の溶解
をほとんど起こすことなく、効果的にエッチング孔を拡
大することが出来る。Within such a preferred range, the etching holes can be effectively enlarged without destruction of the etching holes generated by the first and second etching steps and almost no unnecessary dissolution of the surface.
エッチング液温については、第１段および第２段エッ
チングと同様の理由から、50〜100℃の範囲が良く、特
に70〜90℃が好ましい。また、電流については印加しな
くても良いが、生産性を上げるため印加する場合、15A/
dm2以上にするとエッチング孔の拡大よりも表面溶解が
激しくなる。The etching solution temperature is preferably in the range of 50 to 100 ° C., particularly preferably 70 to 90 ° C., for the same reason as in the first and second stage etching. Also, it is not necessary to apply the current, but if it is applied to increase the productivity, 15 A /
When dm 2 or more, the surface dissolution becomes more intense than the enlargement of the etching hole.
従って、０〜15A/dm2の範囲内で特に０〜10A/dm2が好
ましい。Thus, in particular 0~10A / dm 2 is preferred in the range of 0~15A / dm 2.
以下、比較例とともに本発明の具体的な実施例を示
す。ただし、試料のアルミニウム箔は純度99.99％，厚
さ100μｍの焼鈍したものを用いた。Hereinafter, specific examples of the present invention will be described together with comparative examples. However, the annealed aluminum foil having a purity of 99.99% and a thickness of 100 μm was used as a sample.
（比較例−１） 第１段エッチグを塩酸５％に硫酸25％を添加した液温
80℃の水溶液で電流密度30A/dm2の直流電流を120秒印加
して行なった後、第２段エッチングを塩酸７％に蓚酸0.
1％を添加した液温80℃の水溶液に300秒浸漬して行っ
た。(Comparative Example-1) Liquid temperature of first-stage etching obtained by adding 25% of sulfuric acid to 5% of hydrochloric acid
After applying a direct current with a current density of 30 A / dm 2 for 120 seconds in an aqueous solution at 80 ° C., the second stage etching was performed using 7% hydrochloric acid and 0.1% oxalic acid.
The sample was immersed in an aqueous solution at a liquid temperature of 80 ° C. to which 1% was added for 300 seconds.
（比較例−２） 第１段エッチングを塩化ナトリウム４％，液温80℃の
水溶液で電流密度15A/dm2の直流電流を240秒印加して行
った後、第２段エッチングを塩酸７％に蓚酸0.1％を添
加した液温80℃の水溶液に300秒浸漬して行った。(Comparative Example - 2) Sodium chloride 4% first stage etching, after carried out by applying a direct current of a current density of 15A / dm 2 240 sec with an aqueous solution of a liquid temperature 80 ° C., the second stage etching hydrochloric 7% The sample was immersed in an aqueous solution at a liquid temperature of 80 ° C. to which 0.1% of oxalic acid was added for 300 seconds.
（実施例） 第１段エッチングを塩化ナトリウム４％，液温80℃の
水溶液で電流密度15A/dm2の直流電流を180秒印加して行
った後、第２段エッチングを塩酸５％に硫酸25％を添加
した液温80℃の水溶液で、電流密度30A/dm2の直流電流
を100秒印加して行い、第３段エッチングを塩酸７％に
蓚酸0.1％を添加した液温80℃の水溶液に180秒浸漬して
行った。(Example) The first-stage etching was performed by applying a direct current having a current density of 15 A / dm 2 for 180 seconds with an aqueous solution of 4% sodium chloride and a liquid temperature of 80 ° C., and then the second-stage etching was performed using 5% hydrochloric acid and sulfuric acid. A DC current having a current density of 30 A / dm 2 was applied for 100 seconds with an aqueous solution at a liquid temperature of 80 ° C. to which 25% was added, and the third stage etching was performed at a liquid temperature of 80 ° C. by adding 7% of hydrochloric acid and 0.1% of oxalic acid. This was performed by immersing in an aqueous solution for 180 seconds.
上記３例のエッチング箔をホウ酸系水溶液で370V化成
した後の静電容量と折曲げ強度（1.0R,200g荷重，折曲
げ角90゜により１往復で１回とする）を測定した結果を
表−１に示す。The capacitance and bending strength (1.0 R, 200 g load, bending angle 90 °, one reciprocation is assumed to be one time) after forming the etching foils of the above three examples with a boric acid-based aqueous solution at 370 V were measured. It is shown in Table 1.
発明の効果 以上の説明から明らかな様に、本発明により、静電容
量が大きく、かつ機械的強度にも優れたアルミ電解コン
デンサ用電極箔を得ることが出来る。 Effect of the Invention As is clear from the above description, the present invention can provide an electrode foil for an aluminum electrolytic capacitor having a large capacitance and excellent mechanical strength.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 島谷 涼一 大阪府門真市大字門真1006番地 松下電 器産業株式会社内 (72)発明者 神崎 信義 大阪府門真市大字門真1006番地 松下電 器産業株式会社内 (56)参考文献 特開 昭60−169130（ＪＰ，Ａ) 特開 平１−212423（ＪＰ，Ａ) ──────────────────────────────────────────────────の Continuing on the front page (72) Inventor Ryoichi Shimatani 1006 Kazuma Kadoma, Osaka Prefecture Inside Matsushita Electric Industrial Co., Ltd. (72) Inventor Nobuyoshi Kanzaki 1006 Okadoma Kadoma, Kadoma City, Osaka Matsushita Electric Industrial Co., Ltd. In-company (56) References JP-A-60-169130 (JP, A) JP-A-1-212423 (JP, A)
Claims (3)
の３段階に分けて行うものとし、第１段エッチングとし
て塩化カリウム，塩化ナトリウム，塩化アンモニウムの
うち少なくとも１種0.1〜10％を含む水溶液中で直流エ
ッチングし、第２段エッチングとして塩酸２〜15％に硫
酸，蓚酸，リン酸からなる多孔質皮膜生成酸のうち少な
くとも１種５〜35％を添加した水溶液中で直流エッチン
グし、第３段エッチングとして塩酸２〜15％もしくはそ
れに硫酸，蓚酸，リン酸からなる多孔質皮膜生成酸のう
ち少なくとも１種を３％以下添加した水溶液中で直流エ
ッチングするか、または浸漬処理をすることを特徴とす
るアルミ電解コンデンサ用電極箔の製造方法。An etching process is performed in three stages, a first stage, a second stage, and a third stage. At least one of potassium chloride, sodium chloride and ammonium chloride is used in the first stage etching. % In an aqueous solution containing 2% to 15% of a porous film-forming acid consisting of sulfuric acid, oxalic acid, and phosphoric acid added to 2 to 15% of hydrochloric acid as a second stage etching. Etching, as a third stage etching, DC etching in an aqueous solution containing 2 to 15% of hydrochloric acid or 3% or less of at least one of a porous film-forming acid composed of sulfuric acid, oxalic acid and phosphoric acid, or immersion treatment A method for producing an electrode foil for an aluminum electrolytic capacitor, comprising:
請求項１記載のアルミ電解コンデンサ用電極箔の製造方
法。2. The method according to claim 1, wherein the temperature of the etching solution is 50 to 100 ° C.
いては５〜70A/dm2であり、第３段エッチングについて
は０〜15A/dm2である請求項１記載のアルミ電解コンデ
ンサ用電極箔の製造方法。3. The current density is the first stage and the second stage etching is 5~70A / dm 2, for aluminum electrolytic capacitors according to claim 1, wherein the 0~15A / dm 2 for the third stage etching Manufacturing method of electrode foil.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3814188A JP2629241B2 (en) | 1988-02-19 | 1988-02-19 | Manufacturing method of electrode foil for aluminum electrolytic capacitor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3814188A JP2629241B2 (en) | 1988-02-19 | 1988-02-19 | Manufacturing method of electrode foil for aluminum electrolytic capacitor |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH01212428A JPH01212428A (en) | 1989-08-25 |
| JP2629241B2 true JP2629241B2 (en) | 1997-07-09 |
Family
ID=12517138
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP3814188A Expired - Lifetime JP2629241B2 (en) | 1988-02-19 | 1988-02-19 | Manufacturing method of electrode foil for aluminum electrolytic capacitor |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2629241B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105097286B (en) * | 2015-09-01 | 2017-10-31 | 广西贺州市桂东电子科技有限责任公司 | A kind of caustic solution of super-pressure energy storage material |
-
1988
- 1988-02-19 JP JP3814188A patent/JP2629241B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH01212428A (en) | 1989-08-25 |
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