JPH043409A - Method of etching aluminum foil for electrolytic capacitor - Google Patents
Method of etching aluminum foil for electrolytic capacitorInfo
- Publication number
- JPH043409A JPH043409A JP10461290A JP10461290A JPH043409A JP H043409 A JPH043409 A JP H043409A JP 10461290 A JP10461290 A JP 10461290A JP 10461290 A JP10461290 A JP 10461290A JP H043409 A JPH043409 A JP H043409A
- Authority
- JP
- Japan
- Prior art keywords
- etching
- aluminum foil
- etching step
- etching process
- electrolytic
- 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.)
- Pending
Links
- 238000005530 etching Methods 0.000 title claims abstract description 66
- 238000000034 method Methods 0.000 title claims abstract description 30
- 239000011888 foil Substances 0.000 title claims abstract description 27
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 26
- 239000003990 capacitor Substances 0.000 title claims description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 17
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- -1 chlorine ions Chemical class 0.000 claims abstract description 8
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract description 5
- 239000002253 acid Substances 0.000 claims abstract description 5
- 238000003486 chemical etching Methods 0.000 claims abstract description 4
- 229910002651 NO3 Inorganic materials 0.000 claims abstract description 3
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 3
- 239000000460 chlorine Substances 0.000 claims abstract description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 17
- 239000008151 electrolyte solution Substances 0.000 claims description 11
- 238000004140 cleaning Methods 0.000 claims description 7
- 235000006408 oxalic acid Nutrition 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 2
- 239000000243 solution Substances 0.000 claims 2
- 239000003792 electrolyte Substances 0.000 abstract description 11
- 230000015572 biosynthetic process Effects 0.000 abstract description 5
- 239000007788 liquid Substances 0.000 abstract description 4
- 238000005406 washing Methods 0.000 abstract description 3
- 239000003930 superacid Substances 0.000 abstract 2
- 239000011248 coating agent Substances 0.000 abstract 1
- 238000000576 coating method Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
- 230000036571 hydration Effects 0.000 description 3
- 238000006703 hydration reaction Methods 0.000 description 3
- 238000007654 immersion Methods 0.000 description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
Landscapes
- Fixed Capacitors And Capacitor Manufacturing Machines (AREA)
- ing And Chemical Polishing (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は電解コンデンサ用アルミニウム箔のエツチング
方法に関し、さらに詳しく言えば、中高圧用のアルミニ
ウム電解コンデンサ用電極箔のエツチング方法に関する
ものである。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a method of etching aluminum foil for electrolytic capacitors, and more specifically, to a method of etching electrode foils for medium-high voltage aluminum electrolytic capacitors.
この種の電極箔には、電極体となるアルミニウム箔を電
気的もしくは化学的にエツチング処理して実効表面積を
拡大したものが使用される。This type of electrode foil uses an aluminum foil serving as an electrode body that has been electrically or chemically etched to enlarge its effective surface area.
拡面率を上げる方法は種々提案されているが、−船釣に
は、アルミニウム箔を硫酸、蓚酸、燐酸などの皮膜を形
成する酸を添加した塩化物水溶液中で電気的エツチング
を行ない、ピットを多数形成する前段エツチングと、塩
素イオン、硝酸イオンの少なくとも１種以上を含む水溶
液中で電気的もしくは化学的エツチングを行ない、ピッ
トの内壁に沿ってアルミニウムを溶解し、ピット径を目
的の太さにする後段エツチングとを組合せて行なうよう
にしている。Various methods have been proposed to increase the area expansion ratio, but for boat fishing, aluminum foil is electrically etched in a chloride aqueous solution to which a film-forming acid such as sulfuric acid, oxalic acid, or phosphoric acid is added to form a pit. A pre-etching process is performed to form a large number of pits, and electrical or chemical etching is performed in an aqueous solution containing at least one of chlorine ions and nitrate ions to dissolve aluminum along the inner wall of the pit and reduce the pit diameter to the desired thickness. This is done in combination with subsequent etching.
工業的に連続エツチングを行なうと、前段エツチングの
電解液中に含まれている皮膜形成用の硫酸、蓚酸がアル
ミニウム箔に付着して後段エツチングの電解液中に持ち
込まれ、その量が増加していく。When continuous etching is carried out industrially, the sulfuric acid and oxalic acid for film formation contained in the electrolyte of the first stage etching adhere to the aluminum foil and are brought into the electrolyte of the second stage etching, increasing their amount. go.
後段エツチングの電解液中にこれらの酸が所定量以上存
在すると、アルミニウム箔に前段エツチングで形成され
たピットが太くなりにくくなり、大幅な拡面率の低下を
もたらすことになる。If these acids are present in a predetermined amount or more in the electrolyte for the second stage etching, the pits formed in the first stage etching on the aluminum foil will be difficult to thicken, resulting in a significant reduction in the area enlargement ratio.
このため、従来では定期的に電解液を更新したり、特殊
な処理設備を設置してこれらのイオンを除去するように
しているが、コストアップの問題が生ずる。また、電解
液を更新する際には、その都度ラインを止める必要があ
るため、生産性にも悪影響をおよぼすことになる。For this reason, conventional methods have been to periodically renew the electrolyte or install special processing equipment to remove these ions, but this poses the problem of increased costs. Furthermore, since it is necessary to stop the line each time the electrolyte is replaced, productivity is also adversely affected.
本発明は上記従来の課題を解決するためになされたもの
で、その特徴とするところは、３Ｎまたは４Ｎのアルミ
ニウム箔を硫酸、蓚酸、燐酸などの皮膜を形成する酸を
添加した塩化物水溶液の電解液中において電気的にエツ
チングして多数のピットを形成する第１のエツチング工
程と、同工程で形成されたビット径を目的とする太さに
するため、塩素イオン、硝酸イオンの少なくとも１種以
上を含む電解液中において電気的もしくは化学的なエツ
チングを行なう第２のエツチング工程とを有する電解コ
ンデンサ用アルミニウム箔のエツチング方法において、
第１のエツチング工程と第２のエツチング工程との間に
、同第１のエツチング工程にてエツチングされたアルミ
ニウム箔の洗浄工程を介在させることにある。The present invention was made to solve the above-mentioned conventional problems, and its characteristics are that 3N or 4N aluminum foil is treated with a chloride aqueous solution to which a film-forming acid such as sulfuric acid, oxalic acid, or phosphoric acid is added. A first etching step in which a large number of pits are formed by electrically etching in an electrolytic solution, and at least one type of chlorine ion or nitrate ion is used to make the bits formed in the same step have the desired diameter. A method for etching an aluminum foil for an electrolytic capacitor, which comprises a second etching step of performing electrical or chemical etching in an electrolytic solution containing the above,
The object of the present invention is to interpose a cleaning step for the aluminum foil etched in the first etching step between the first etching step and the second etching step.
この場合、洗浄工程の洗浄液としては、水もしくは第２
のエツチング工程の電解液と同一の電解液が用いられる
。水を使用する場合には、アルミニウム箔表面への水和
皮膜の形成が少ない短時間、例えば加温せずに３０秒間
以下で洗浄するのが好ましい、なお、第２のエツチング
工程の電解液中に持ち込まれる第１のエツチング工程の
硫酸イオン、蓚酸イオン、燐酸イオンの混入濃度はそれ
ぞれ３００ｐｐｍ以下、好ましくは１００ｐＰ園以下、
特に好ましくは３０ｐＰ−以下とされる。In this case, water or secondary
The same electrolytic solution as that used in the etching process is used. When using water, it is preferable to wash for a short time, such as 30 seconds or less without heating, to minimize the formation of a hydration film on the surface of the aluminum foil. The mixed concentration of sulfate ions, oxalate ions, and phosphate ions in the first etching step is each 300 ppm or less, preferably 100 ppm or less,
Particularly preferably, it is 30 pP- or less.
特開平１−２１２４２６号公報によれば、第１のエツチ
ング工程と第２のエツチング工程との間に、中間処理と
してＨ，Ｏによる浸漬処理を行なってアルミニウム箔表
面に水和皮膜を形成することが提案されているが、本発
明によると、そのような水和皮膜の形成を抑止しつつ、
硫酸根、蓚酸機、燐酸根などの第２のエツチング工程へ
の持ち込みが防止される。According to JP-A-1-212426, between the first etching step and the second etching step, immersion treatment with H and O is performed as an intermediate treatment to form a hydration film on the surface of the aluminum foil. However, according to the present invention, while suppressing the formation of such a hydration film,
Sulfuric acid radicals, oxalic acid radicals, phosphoric acid radicals, etc. are prevented from being brought into the second etching process.
以下、本発明の実施例を比較例とともに説明する。なお
試料としては、厚み１００μｍ、純度４Ｎのアルミニウ
ム箔を使用している。Examples of the present invention will be described below along with comparative examples. Note that an aluminum foil with a thickness of 100 μm and a purity of 4N is used as the sample.
〈比較例１〉
第１のエッチング工程；塩酸５ｗｔ％、硫酸３（ｈｔ％
、液温８０℃の電解液中において、電流密度３００＋ｓ
Ａ／ｃｄの直流電流を６０秒間通電した。<Comparative Example 1> First etching step; Hydrochloric acid 5 wt%, sulfuric acid 3 (ht%
, in an electrolytic solution with a liquid temperature of 80°C, a current density of 300+s
A direct current of A/cd was applied for 60 seconds.
第２のエッチング工程；塩酸８ｗｔ％で液温８５℃の電
解液中において、電流密度１００＋＊Ａ／ａ＃の直流電
流を６分間通電した。Second etching step: A direct current with a current density of 100+*A/a# was applied for 6 minutes in an electrolytic solution containing 8 wt% hydrochloric acid and a liquid temperature of 85°C.
この場合、第１のエツチング工程後、特にアルミニウム
箔を洗浄することなく、第２のエツチング工程を実施し
た。第２のエツチング工程における電解液中の硫酸濃度
は２５０ｐｐ＋ｍであった６〈比較例２〉
第１のエッチング工程；比較例１と同じ。In this case, after the first etching step, the second etching step was carried out without particularly cleaning the aluminum foil. The sulfuric acid concentration in the electrolyte in the second etching step was 250 pp+m. 6 Comparative Example 2 First etching step; same as Comparative Example 1.
第２のエッチング工程；硝酸１０ｗｔ％で液温８５℃の
電解液中において、電流密度２００ｍＡ／ｃｄの直流電
流を３分間通電した。Second etching step: A direct current with a current density of 200 mA/cd was applied for 3 minutes in an electrolytic solution containing 10 wt% nitric acid and a liquid temperature of 85°C.
この場合も比較例１と同様に、第１のエッチング工程後
、特にアルミニウム箔を洗浄することなく、第２のエツ
チング工程を実施した。In this case, as in Comparative Example 1, after the first etching step, the second etching step was carried out without particularly cleaning the aluminum foil.
（実施例１）
第１のエツチング工程および第２のエツチング工程は比
較例１と同じであるが、その工程の間に、水温２０℃の
水シヤワーによる水洗工程を２０秒間実施した。第２の
エツチング工程の電解液中の硫酸根は１５ｐｐ−であっ
た。(Example 1) The first etching step and the second etching step were the same as in Comparative Example 1, but between the steps, a rinsing step using a water shower at a water temperature of 20° C. was performed for 20 seconds. The sulfate group in the electrolyte in the second etching step was 15 pp-.
（実施例２）
第１のエツチング工程および第２のエツチング工程は比
較例２と同じであるが、その工程の間に、水温２５℃の
水に浸漬する水洗工程を１５秒間実施した。第２のエツ
チング工程の電解液中の硫酸根は１０ｐｐｍ＋であった
。(Example 2) The first etching step and the second etching step were the same as in Comparative Example 2, but between the steps, a rinsing step of immersion in water at a water temperature of 25° C. was performed for 15 seconds. The sulfate group in the electrolyte in the second etching step was 10 ppm+.
上記比較例１，２および実施例１，２にて得られたエツ
チド箔を３５０ｖで化成してそれらの各静電容量を測定
した結果を次の表に示す。The etched foils obtained in Comparative Examples 1 and 2 and Examples 1 and 2 were chemically converted at 350 V and their respective capacitances were measured. The results are shown in the following table.
（表）
工程と第２のエツチング工程の間に水洗（洗浄）処理を
行なうことにより、静電容量が増大することが認められ
た。(Table) It was found that the capacitance increased by performing water washing (washing) treatment between the step and the second etching step.
以上説明したように、本発明によれば、第１のエツチン
グ工程と第２のエツチング工程との間に、同第１のエツ
チング工程にてエツチングされたアルミニウム箔の洗浄
工程を介在させ、硫酸根、蓚酸機、燐酸根などの第２の
エツチング工程への持ち込みを防止するようにしたこと
により、静電容量の増大を図ることができ、特に工業的
に連続エツチングを行なう場合に有効である。As explained above, according to the present invention, a cleaning process of the aluminum foil etched in the first etching process is interposed between the first etching process and the second etching process, and the sulfuric acid radical is removed. By preventing contaminants such as oxalic acid, phosphoric acid, etc. from being carried into the second etching step, the capacitance can be increased, which is particularly effective when continuous etching is carried out industrially.
特許出願人 エルナー株式会社Patent applicant: Elna Co., Ltd.
Claims (3)
形成する酸を添加した塩化物水溶液の電解液中において
電気的にエッチングして多数のピットを形成する第１の
エッチング工程と、同工程で形成されたピット径を目的
とする太さにするため、塩素イオン、硝酸イオンの少な
くとも１種以上を含む電解液中において電気的もしくは
化学的なエッチングを行なう第２のエッチング工程とを
有する電解コンデンサ用アルミニウム箔のエッチング方
法において、上記第１のエッチング工程と上記第２のエ
ッチング工程との間に、同第１のエッチング工程にてエ
ッチングされたアルミニウム箔の洗浄工程を介在させる
ことを特徴とする電解コンデンサ用アルミニウム箔のエ
ッチング方法。(1) A first etching process in which a large number of pits are formed by electrically etching aluminum foil in an electrolytic solution of an aqueous chloride solution containing a film-forming acid such as sulfuric acid, oxalic acid, or phosphoric acid; In order to make the diameter of the pit formed in the desired thickness, an electrolytic method comprising a second etching step of performing electrical or chemical etching in an electrolytic solution containing at least one of chlorine ions and nitrate ions. The method for etching aluminum foil for a capacitor is characterized in that a step of cleaning the aluminum foil etched in the first etching step is interposed between the first etching step and the second etching step. Etching method for aluminum foil for electrolytic capacitors.
２のエッチング工程の電解液と同一の電解液が用いられ
る請求項１に記載の電解コンデンサ用アルミニウム箔の
エッチング方法。(2) The method of etching aluminum foil for an electrolytic capacitor according to claim 1, wherein water or the same electrolytic solution as the electrolytic solution used in the second etching step is used as the cleaning solution in the cleaning step.
酸イオン、蓚酸イオン、燐酸イオン混入濃度がそれぞれ
１００ｐｐｍ以下である請求項１に記載の電解コンデン
サ用アルミニウム箔のエッチング方法。(3) The method for etching aluminum foil for an electrolytic capacitor according to claim 1, wherein the concentration of sulfate ions, oxalate ions, and phosphate ions in the electrolytic solution used in the second etching step is each 100 ppm or less.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10461290A JPH043409A (en) | 1990-04-20 | 1990-04-20 | Method of etching aluminum foil for electrolytic capacitor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10461290A JPH043409A (en) | 1990-04-20 | 1990-04-20 | Method of etching aluminum foil for electrolytic capacitor |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH043409A true JPH043409A (en) | 1992-01-08 |
Family
ID=14385263
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP10461290A Pending JPH043409A (en) | 1990-04-20 | 1990-04-20 | Method of etching aluminum foil for electrolytic capacitor |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH043409A (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005290491A (en) * | 2004-03-31 | 2005-10-20 | Nippon Chemicon Corp | Aluminum anode foil for electrolytic capacitor |
| US7132383B2 (en) | 2000-09-12 | 2006-11-07 | Toyo Boseki Kabushiki Kaisha | Polymerization catalyst for polyester, polyester produced with the same, and process for producing polyester |
| US7144614B2 (en) | 2001-02-23 | 2006-12-05 | Toyo Boseki Kabushiki Kaisha | Polyester polymerization catalyst, polyester produced by using the same, and process for producing polyester |
| US7208565B1 (en) | 1999-08-24 | 2007-04-24 | Toyo Boseki Kabushiki Kaisha | Polymerization catalyst for polyesters, polyester produced with the same, and process for production of polyester |
| JP2007227770A (en) * | 2006-02-24 | 2007-09-06 | Nichicon Corp | Manufacturing method of anode foil for electrolytic capacitor |
| CN100360714C (en) * | 2005-09-21 | 2008-01-09 | 中国海洋大学 | Chemical Etching Solutions for Aluminum and Aluminum Alloys |
| US7501373B1 (en) * | 1998-10-23 | 2009-03-10 | Toyo Boseki Kabushiki Kaisha | Polymerization catalyst for polyester production, polyester, and process for producing polyester |
| US9888157B2 (en) | 2012-07-31 | 2018-02-06 | Sony Corporation | Lens mounting mechanism, lens mounting method, and image pickup device |
-
1990
- 1990-04-20 JP JP10461290A patent/JPH043409A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7501373B1 (en) * | 1998-10-23 | 2009-03-10 | Toyo Boseki Kabushiki Kaisha | Polymerization catalyst for polyester production, polyester, and process for producing polyester |
| US7208565B1 (en) | 1999-08-24 | 2007-04-24 | Toyo Boseki Kabushiki Kaisha | Polymerization catalyst for polyesters, polyester produced with the same, and process for production of polyester |
| US7132383B2 (en) | 2000-09-12 | 2006-11-07 | Toyo Boseki Kabushiki Kaisha | Polymerization catalyst for polyester, polyester produced with the same, and process for producing polyester |
| US7144614B2 (en) | 2001-02-23 | 2006-12-05 | Toyo Boseki Kabushiki Kaisha | Polyester polymerization catalyst, polyester produced by using the same, and process for producing polyester |
| JP2005290491A (en) * | 2004-03-31 | 2005-10-20 | Nippon Chemicon Corp | Aluminum anode foil for electrolytic capacitor |
| CN100360714C (en) * | 2005-09-21 | 2008-01-09 | 中国海洋大学 | Chemical Etching Solutions for Aluminum and Aluminum Alloys |
| JP2007227770A (en) * | 2006-02-24 | 2007-09-06 | Nichicon Corp | Manufacturing method of anode foil for electrolytic capacitor |
| US9888157B2 (en) | 2012-07-31 | 2018-02-06 | Sony Corporation | Lens mounting mechanism, lens mounting method, and image pickup device |
| US10298821B2 (en) | 2012-07-31 | 2019-05-21 | Sony Corporation | Lens mounting mechanism, lens mounting method, and image pickup device |
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