JPH0760781B2 - Method for forming electrode foil for electrolytic capacitors - Google Patents
Method for forming electrode foil for electrolytic capacitorsInfo
- Publication number
- JPH0760781B2 JPH0760781B2 JP62008639A JP863987A JPH0760781B2 JP H0760781 B2 JPH0760781 B2 JP H0760781B2 JP 62008639 A JP62008639 A JP 62008639A JP 863987 A JP863987 A JP 863987A JP H0760781 B2 JPH0760781 B2 JP H0760781B2
- Authority
- JP
- Japan
- Prior art keywords
- chemical conversion
- formation
- electrode foil
- film
- electrolytic capacitors
- 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 - Lifetime
Links
- 239000011888 foil Substances 0.000 title claims description 26
- 239000003990 capacitor Substances 0.000 title claims description 13
- 238000000034 method Methods 0.000 title claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 33
- 239000000126 substance Substances 0.000 claims description 32
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 24
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 18
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 11
- 238000007598 dipping method Methods 0.000 claims description 6
- 230000015572 biosynthetic process Effects 0.000 description 16
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 15
- 229910052782 aluminium Inorganic materials 0.000 description 15
- 239000007864 aqueous solution Substances 0.000 description 8
- 238000007654 immersion Methods 0.000 description 6
- ILRRQNADMUWWFW-UHFFFAOYSA-K aluminium phosphate Chemical compound O1[Al]2OP1(=O)O2 ILRRQNADMUWWFW-UHFFFAOYSA-K 0.000 description 5
- 238000004090 dissolution Methods 0.000 description 5
- 239000011259 mixed solution Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 4
- 239000002244 precipitate 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
- 238000009835 boiling Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000007739 conversion coating Methods 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 238000007788 roughening Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
Landscapes
- Chemical Treatment Of Metals (AREA)
Description
【発明の詳細な説明】 ［発明の目的］ （産業上の利用分野） この発明は、電解コンデンサ用電極箔を化成する方法に
関する。DETAILED DESCRIPTION OF THE INVENTION Object of the Invention (Field of Industrial Application) The present invention relates to a method for forming an electrode foil for an electrolytic capacitor.
（従来の技術） 電解コンデンサ用電極箔、例えば、アルミ箔を粗面化す
るエッチング工程の後処理、又は化成工程の前処理とし
てアルミ箔に対する熱処理又は温純水への浸漬処理を行
い、化成皮膜厚/Vを小さくすることにより容量増加を図
っていた。しかしながら、このような方法で得られた化
成皮膜は結晶化し、そのとき生じるクラックやボイドに
よって電気的安定性、すなわち放置性、エージング時の
皮膜修復性及び漏れ電流の変化が大きいなどの問題点が
あった。このため化成工程中において、りん酸水溶液に
アルミ箔を浸漬処理して前記クラックやボイドの影響を
防止しているが完全に修復されず、特にコンデンサを無
負荷放置したときの漏れ電流の変化が大きく、また処理
中において生じる不溶性りん酸アルミニウムの浮遊物、
沈殿物がアルミ箔に付着して化成機の運転停止、掃除、
ローラ等の部品の交換を必要とする問題点があった。(Prior Art) Electrode capacitor electrode foil, for example, post-treatment of etching step for roughening aluminum foil, or heat treatment or dipping treatment in hot pure water for aluminum foil as pre-treatment of chemical conversion step The capacity was increased by reducing V. However, the chemical conversion film obtained by such a method is crystallized, and there are problems such as electrical stability due to cracks and voids generated at that time, that is, leaving property, film repairability during aging, and a large change in leakage current. there were. Therefore, during the chemical conversion process, the aluminum foil is immersed in a phosphoric acid aqueous solution to prevent the effects of the cracks and voids, but it is not completely repaired, and there is a change in the leakage current particularly when the capacitor is left unloaded. Large and insoluble aluminum phosphate suspensions that form during processing,
The deposit adheres to the aluminum foil, shuts down the chemical conversion machine, cleans it,
There is a problem that parts such as rollers need to be replaced.
（発明が解決しようとする問題点） 従来の電解コンデンサ用電極箔の化成方法では、不溶性
りん酸アルミニウムの浮遊物や沈殿物によってアルミ箔
の溶解反応が著しく低下しコンデンサの電化的特性や運
転能率上の問題点を生じていた。(Problems to be Solved by the Invention) In the conventional method for forming electrode foils for electrolytic capacitors, the floating reaction or precipitation of insoluble aluminum phosphate significantly reduces the dissolution reaction of the aluminum foils, resulting in the electrical characteristics and operating efficiency of the capacitors. It caused the above problem.
この発明は上記の欠点を除去するもので、化成液におけ
る浮遊物や沈殿物の生成をなくし、アルミ箔の溶解反応
を低下させないで化成を行うことができる化成方法を提
供せんとするものである。This invention eliminates the above-mentioned drawbacks, and eliminates the formation of suspended solids and precipitates in the chemical conversion liquid, and provides a chemical conversion method capable of performing chemical conversion without lowering the dissolution reaction of aluminum foil. .
［発明の構成］ （問題点を解決するための手段） 本発明になる電解コンデンサ用電極箔の化成方法は、所
定の化成電圧上昇後に配置された化成槽の少なくとも１
槽が、りん酸及び硫酸をそれぞれ0.5重量％以上含み、
これの合計濃度Ａ（重量％）が１≦Ａ≦10で、液温度Ｔ
（℃）が65−5A≦Ｔ≦85−5Aである化成液を有し、この
化成液中に電極箔をｔ分間（ただしｔは、6/A≦ｔ≦30/
A）浸漬したのち、再化成することを特徴としたもので
ある。[Structure of the Invention] (Means for Solving the Problems) A method of forming an electrode foil for an electrolytic capacitor according to the present invention comprises at least one of the formation tanks arranged after a predetermined formation voltage rise.
The tank contains 0.5 wt% or more of phosphoric acid and sulfuric acid, respectively,
When the total concentration A (% by weight) of these is 1 ≦ A ≦ 10, the liquid temperature T
It has a chemical conversion liquid whose (° C) is 65-5A ≤ T ≤ 85-5A, and the electrode foil is kept in this chemical conversion liquid for t minutes (where t is 6 / A ≤ t ≤ 30 /
A) It is characterized by re-forming after immersion.
（作用） この発明によれば、所定の化成電圧に上昇した時点で電
極箔の表面に生成されているクラック、ボイドが本発明
たるりん酸及び硫酸の混合液中に浸漬されることによ
り、化成皮膜が表面から溶解するのでクラックやボイド
が化成液と接触できる状態となる。よって、前記クラッ
クやボイドの生成部分にも再化成による安定な皮膜を生
成できるものである。このようにしてできた皮膜中にり
ん酸イオンが取り込まれ、皮膜中にりん酸アルミニウム
の水に安定な化合物が生成される。また、りん酸、硫酸
の混合液中では硫酸イオンにより化成皮膜の溶解反応が
低下せずに続行され、さらに混合液の使用によって浮遊
物、沈殿物の生成も解消される作用がある。(Operation) According to the present invention, the formation of cracks and voids formed on the surface of the electrode foil at the time of rising to a predetermined formation voltage by immersing in the mixed solution of phosphoric acid and sulfuric acid of the present invention Since the film dissolves from the surface, cracks and voids can come into contact with the chemical conversion liquid. Therefore, it is possible to form a stable film by re-formation even in the portion where the cracks and voids are formed. Phosphate ions are incorporated into the film thus formed, and a water-stable compound of aluminum phosphate is formed in the film. Further, in the mixed solution of phosphoric acid and sulfuric acid, the dissolution reaction of the chemical conversion film is continued by the sulfate ion without lowering, and further, the use of the mixed solution has the effect of eliminating the formation of suspended solids and precipitates.
（実施例） エッチング済みの電解コンデンサ用アルミ箔を70V化成
する場合の実施例について述べる。エッチング済みアル
ミ箔をアジピン酸アンモニウム50g/1水溶液（60℃）中
で化成し70Vに上昇後、りん酸３重量％及び硫酸３重量
％の混合水溶液（液温度60℃）中に２分間の浸漬を行
い、その後前記と同じ濃度、温度、電圧からなる定電圧
化成を20分間行った後、450℃中で１分間の熱処理を行
った。このようにして浸漬処理を行ったアルミ箔を、前
記と同じアジピン酸アンモニウム50g/1水溶液（60℃）
からなる化成液中に５分間浸漬して再化成を行った。こ
の得られた化成済みアルミ箔を0.5dm2のサイズに打ち抜
き、98℃以上の純水中に１時間煮沸した後、化成電圧到
達時間は50秒で、静電容量値は630μF/dm2であった。こ
の試料の化成電圧到達時間は、初期の状態（すなわち再
化成後、煮沸していない状態。50秒で化成電圧まで到
達）と変わらない。なお、前記の煮沸は、得られた化成
箔を試験して、試料間の特性の差異を明確に出現させる
ために行う強制劣化の手段である。(Example) An example of forming an etched aluminum foil for electrolytic capacitors at 70 V will be described. After etching the etched aluminum foil in ammonium adipate 50g / 1 aqueous solution (60 ° C) and raising it to 70V, soak it in a mixed aqueous solution (liquid temperature 60 ° C) of phosphoric acid 3% by weight and sulfuric acid 3% by weight for 2 minutes. After that, a constant voltage chemical conversion consisting of the same concentration, temperature, and voltage as described above was performed for 20 minutes, and then heat treatment was performed at 450 ° C. for 1 minute. The aluminum foil thus dipped was treated with the same ammonium adipate 50 g / 1 aqueous solution (60 ° C) as above.
It was re-formed by immersing it in a chemical conversion solution consisting of 5 minutes. Punching the obtained chemical conversion already aluminum foil to the size of 0.5 dm 2, after boiling for 1 hour in pure water above 98 ° C., the formation voltage arrival time is 50 seconds, the electrostatic capacitance value is 630μF / dm 2 there were. The time required to reach the formation voltage of this sample is the same as that in the initial state (that is, the state in which the material has not been boiled after re-formation and reached the formation voltage in 50 seconds). The above boiling is a means of forced deterioration, which is carried out in order to test the obtained formed foil and to clearly show the difference in the characteristics between the samples.
以上の実施例を工程順に示すと次のようになる。The above embodiment will be described below in order of process.
化成（70Vまで上昇させる）→浸漬処理（りん酸＋
硫酸混合液に浸漬）→定電圧化成（の化成と同じ液
濃度、温度、電圧）→熱処理→再化成 これに対し、エッチング済みアルミ箔をアジピン酸アン
モニウム50g/1水溶液（60℃）中で化成し70Vに上昇後、
浸漬処理をりん酸３重量％水溶液（液温度60℃）を用い
て行った後、本発明と同じ条件で定電圧化成、熱処理、
再化成及び煮沸を施した従来例の化成電圧到達時間は10
分で、静電容量値は620μF/dm2であった（下表の従来例
１参照）。Chemical conversion (up to 70V) → Immersion treatment (phosphoric acid +
Dipping in sulfuric acid mixture) → Constant voltage formation (same concentration, temperature and voltage as formation) → heat treatment → re-formation In contrast, etched aluminum foil is formed in ammonium adipate 50g / 1 aqueous solution (60 ℃) After rising to 70V,
After the dipping treatment was carried out using a phosphoric acid 3% by weight aqueous solution (liquid temperature 60 ° C.), constant voltage formation, heat treatment, and
The time required to reach the formation voltage of the conventional example after re-formation and boiling was 10
In minutes, the capacitance value was 620 μF / dm 2 (see Conventional Example 1 in the table below).
また、りん酸水溶液への浸漬処理を行わない場合は、化
成電圧まで到達せず、かつ容量値は600μF/dm2であった
（下表の従来例２参照）。When the dipping treatment in the phosphoric acid aqueous solution was not carried out, the formation voltage was not reached and the capacitance value was 600 μF / dm 2 (see Conventional Example 2 in the table below).
以上のことから、本発明になる化成方法では、耐水性が
大幅に向上し、また浸漬処理中におけるりん酸アルミニ
ウムの沈殿物の発生がなく、作業性、外観不良も減少し
た。From the above, in the chemical conversion method according to the present invention, the water resistance was significantly improved, the precipitation of aluminum phosphate was not generated during the dipping treatment, and the workability and the appearance defect were also reduced.
この発明により得られたアルミ箔を使用して作製した定
格50V−1000μＦの電解コンデンサについて、85℃中に
無負荷放置した場合の漏れ電流の変化を第１図に示す
が、1000時間まで変化が少なく、従来のりん酸水溶液へ
の浸漬処理を行ったもの、及び浸漬を行わなかったもの
に比し大幅に改善される。Fig. 1 shows the change in leakage current of an electrolytic capacitor with a rating of 50V-1000µF produced using the aluminum foil obtained according to the present invention when left unloaded at 85 ° C. A small amount, which is significantly improved as compared with those obtained by conventional immersion treatment in a phosphoric acid aqueous solution and those not subjected to immersion treatment.
上記の実施例について化成皮膜の変化を第２図に示す。
すなわち、第２図（Ａ）に示すごとく、化成電圧まで上
昇した時点で、アルミ箔１の表面に生成された化成皮膜
２中には、すでにクラック３やボイド４が発生してお
り、これがりん酸及び硫酸の混合液中に浸漬されると、
第２図（Ｂ）のごとく化成皮膜２が表面から溶解し、化
成皮膜２の厚さが薄くなるので、クラック３やボイド４
が化成液と接触可能な状態となり、これを再度化成を行
うことによってこれらの部分に電気的に安定な皮膜５が
生成されるのである。このとき化成皮膜２中にりん酸イ
オンが取り込まれ、皮膜２中にりん酸アルミニウムの水
に安定な化合物ができ、第２図（Ｃ）のごときさらに安
定な皮膜５となるのである。この現象は、りん酸・硫酸
混合液中では、2Al3+＋3SO4 2-Al2（SO4）３と解離状態
となり、SO4 2-により溶解反応が低下せずに続行され
る。またりん酸・硫酸混合液を用いることによりAl3+へ
の解離定数が大きくなり、溶液中への浮遊物、沈殿物の
生成も解消されることになる。なお、各種処理条件を設
定し実験した結果を下表に示す。FIG. 2 shows the changes in the chemical conversion coating for the above examples.
That is, as shown in FIG. 2 (A), cracks 3 and voids 4 have already been generated in the chemical conversion film 2 formed on the surface of the aluminum foil 1 at the time when the chemical conversion voltage is increased, and these are phosphorus. When immersed in a mixture of acid and sulfuric acid,
As shown in FIG. 2 (B), the chemical conversion film 2 is melted from the surface, and the thickness of the chemical conversion film 2 is reduced.
Is brought into contact with the chemical conversion liquid, and by conducting chemical conversion again, an electrically stable film 5 is formed on these portions. At this time, phosphate ions are taken into the chemical conversion film 2 to form a water-stable compound of aluminum phosphate in the film 2, and the film 5 becomes more stable as shown in FIG. 2 (C). This phenomenon is dissociated with 2Al 3+ + 3SO 4 2- Al 2 (SO 4 ) 3 in the phosphoric acid / sulfuric acid mixed solution, and the dissolution reaction is continued without being reduced by SO 4 2− . In addition, the use of the phosphoric acid / sulfuric acid mixed solution increases the dissociation constant into Al 3+ and eliminates the formation of suspended solids and precipitates in the solution. The table below shows the results of experiments conducted under various treatment conditions.
なお、浸漬処理条件において、合計濃度が１重量％未
満、浸漬時間が6/A未満、液温度が65−5A未満では、化
成皮膜の溶解が少なく、したがってクラックやボイドま
で溶解が達しないので耐水性が低い。また、これと逆の
場合は、化成皮膜の溶解が進み過ぎ、再化成により生成
される皮膜の占める割合が増加し、その皮膜は結晶化し
ないため静電容量が減少する結果となる。 Under the immersion treatment conditions, if the total concentration is less than 1% by weight, the immersion time is less than 6 / A, and the liquid temperature is less than 65-5A, the chemical conversion film does not dissolve so much that cracks and voids do not reach the water resistance. It is not very popular. On the other hand, in the opposite case, dissolution of the chemical conversion film proceeds too much, the ratio of the film formed by re-chemical conversion increases, and the film does not crystallize, resulting in a decrease in capacitance.
［発明の効果］ この発明になる電解コンデンサ用電極箔の化成方法によ
れば、電解コンデンサの漏れ電流特性及び耐水性の改善
と浮遊物、沈殿物の生成が解消できるのである。[Effect of the Invention] According to the method of forming an electrode foil for an electrolytic capacitor according to the present invention, it is possible to improve the leakage current characteristics and water resistance of the electrolytic capacitor and eliminate the formation of suspended matters and precipitates.
第１図は本発明の実施例により得られたアルミ箔を使用
した電解コンデンサの漏れ電流特性を示す曲線図、第２
図は本発明になる化成皮膜の変化を示す断面図である。 １……アルミ箔 ２……化成皮膜 ３……クラック ４……ボイド ５……安定な皮膜FIG. 1 is a curve diagram showing a leakage current characteristic of an electrolytic capacitor using an aluminum foil obtained according to an embodiment of the present invention.
The figure is a cross-sectional view showing changes in the chemical conversion coating according to the present invention. 1 ... Aluminum foil 2 ... Chemical coating 3 ... Crack 4 ... Void 5 ... Stable coating
Claims (1)
の少なくとも１槽において、りん酸及び硫酸をそれぞれ
0.5重量％以上含み、これの合計濃度Ａ（重量％）が１
≦Ａ≦10であり、液温度Ｔ（℃）が65−5A≦Ｔ≦85−5A
である化成液に、電極箔をｔ分間（ただしｔは、6/A≦
ｔ≦30/A）浸漬したのち、再化成することを特徴とする
電解コンデンサ用電極箔の化成方法。1. Phosphoric acid and sulfuric acid are respectively contained in at least one of the chemical conversion tanks arranged after a predetermined increase in chemical conversion voltage.
Contain 0.5% by weight or more, and the total concentration A (% by weight) is 1
≦ A ≦ 10 and liquid temperature T (° C) is 65-5A ≦ T ≦ 85-5A
The electrode foil is added to the chemical liquid for t minutes (where t is 6 / A ≦
t ≦ 30 / A) A method for forming an electrode foil for electrolytic capacitors, which comprises dipping and then re-forming.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62008639A JPH0760781B2 (en) | 1987-01-17 | 1987-01-17 | Method for forming electrode foil for electrolytic capacitors |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62008639A JPH0760781B2 (en) | 1987-01-17 | 1987-01-17 | Method for forming electrode foil for electrolytic capacitors |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63176480A JPS63176480A (en) | 1988-07-20 |
| JPH0760781B2 true JPH0760781B2 (en) | 1995-06-28 |
Family
ID=11698521
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62008639A Expired - Lifetime JPH0760781B2 (en) | 1987-01-17 | 1987-01-17 | Method for forming electrode foil for electrolytic capacitors |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0760781B2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2621079B2 (en) * | 1988-01-25 | 1997-06-18 | マルコン電子株式会社 | Method of forming electrode foil for aluminum electrolytic capacitor |
| WO2025047740A1 (en) * | 2023-08-29 | 2025-03-06 | 日本ケミコン株式会社 | Positive electrode body of solid electrolytic capacitor, solid electrolytic capacitor, method for manufacturing positive electrode body of solid electrolytic capacitor, and method for manufacturing solid electrolytic capacitor |
-
1987
- 1987-01-17 JP JP62008639A patent/JPH0760781B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPS63176480A (en) | 1988-07-20 |
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