JPH04279017A - Manufacture of electrode foil for aluminum electrolytic capacitor - Google Patents
Manufacture of electrode foil for aluminum electrolytic capacitorInfo
- Publication number
- JPH04279017A JPH04279017A JP3067868A JP6786891A JPH04279017A JP H04279017 A JPH04279017 A JP H04279017A JP 3067868 A JP3067868 A JP 3067868A JP 6786891 A JP6786891 A JP 6786891A JP H04279017 A JPH04279017 A JP H04279017A
- Authority
- JP
- Japan
- Prior art keywords
- treatment
- foil
- hot water
- electrolytic capacitor
- aluminum 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.)
- Granted
Links
- 239000011888 foil Substances 0.000 title claims abstract description 42
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 19
- 239000003990 capacitor Substances 0.000 title claims abstract description 18
- 238000004519 manufacturing process Methods 0.000 title claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000000126 substance Substances 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- 230000036571 hydration Effects 0.000 claims abstract description 9
- 238000006703 hydration reaction Methods 0.000 claims abstract description 9
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims description 31
- 238000000034 method Methods 0.000 claims description 29
- 238000005530 etching Methods 0.000 abstract description 26
- 238000001035 drying Methods 0.000 abstract description 4
- 238000000354 decomposition reaction Methods 0.000 abstract 1
- 238000006298 dechlorination reaction Methods 0.000 description 13
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 7
- 229910001873 dinitrogen Inorganic materials 0.000 description 7
- 239000007864 aqueous solution Substances 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 6
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 239000003792 electrolyte Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 229910001882 dioxygen Inorganic materials 0.000 description 3
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 2
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- FLDCSPABIQBYKP-UHFFFAOYSA-N 5-chloro-1,2-dimethylbenzimidazole Chemical compound ClC1=CC=C2N(C)C(C)=NC2=C1 FLDCSPABIQBYKP-UHFFFAOYSA-N 0.000 description 1
- 239000001741 Ammonium adipate Substances 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 239000001361 adipic acid Substances 0.000 description 1
- 235000011037 adipic acid Nutrition 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 235000019293 ammonium adipate Nutrition 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
Abstract
Description
【０００１】0001
【産業上の利用分野】本発明はアルミニウム電解コンデ
ンサ用電極箔の製造方法に関し、さらに詳しく言えば、
エッチング箔に良質な酸化皮膜を形成し、コンデンサの
陽極箔の単位面積当りの静電容量を増加させるようにし
たもので、特に低圧用に好適なアルミニウム電解コンデ
ンサ用電極箔の製造方法に関するものである。[Field of Industrial Application] The present invention relates to a method for manufacturing electrode foil for aluminum electrolytic capacitors, and more specifically,
A high-quality oxide film is formed on the etched foil to increase the capacitance per unit area of the anode foil of the capacitor, and it relates to a method of manufacturing electrode foil for aluminum electrolytic capacitors, which is particularly suitable for low voltage applications. be.
【０００２】0002
【従来の技術】一般に、アルミニウム電解コンデンサは
、アルミニウム箔からなる陽極用電極箔と陰極用電極箔
とをセパレータを介して巻回してなるコンデンサ素子を
有し、同コンデンサ素子に電解液を含浸させ、外装ケー
ス内に封入した構造とされている。[Prior Art] Generally, an aluminum electrolytic capacitor has a capacitor element formed by winding an anode electrode foil and a cathode electrode foil made of aluminum foil with a separator in between, and the capacitor element is impregnated with an electrolyte. The structure is that it is enclosed within an outer case.
【０００３】ところで、陽極用電極箔はアルミニウム箔
の表面を粗面化して表面積を拡大するエッチング工程と
、同工程により得られたエッチング箔の表面に酸化皮膜
を形成する化成工程とを経て製造される。By the way, electrode foil for anodes is manufactured through an etching process in which the surface of the aluminum foil is roughened to increase its surface area, and a chemical conversion process in which an oxide film is formed on the surface of the etched foil obtained by the same process. Ru.
【０００４】上記エッチング工程において、アルミニウ
ム箔は塩化物を含む水溶液中でその表面が電気化学的に
溶解されて粗面化され、しかる後、硝酸、蓚酸、燐酸な
どにて脱塩素処理され、水洗後乾燥して巻き取られて次
の化成工程に移される。In the above etching process, the surface of the aluminum foil is electrochemically dissolved in an aqueous solution containing chloride to make it rough, and then dechlorinated with nitric acid, oxalic acid, phosphoric acid, etc., and washed with water. It is then dried, rolled up and transferred to the next chemical conversion step.
【０００５】[0005]
【発明が解決しようとする課題】陽極用電極箔の単位面
積当りの静電容量は、その値が大きい程、コンデンサ自
体を小型化することができるため、単位面積当りの静電
容量を増大させるための研究が種々行なわれている。[Problem to be solved by the invention] The larger the value of the capacitance per unit area of the electrode foil for the anode, the more compact the capacitor itself can be, which increases the capacitance per unit area. Various studies are being conducted for this purpose.
【０００６】その方法としては、おおよそ次の２法が知
られている。すなわち、第１の方法はエッチング箔の表
面積の拡大率を大きくする方法であり、第２の方法は化
成によりエッチング箔上にムラのない均一な酸化アルミ
ニウム（Ａｌ２Ｏ３）の皮膜を形成させる方法である。The following two methods are known as methods for this purpose. That is, the first method is a method of increasing the expansion rate of the surface area of the etching foil, and the second method is a method of forming an even and uniform aluminum oxide (Al2O3) film on the etching foil by chemical conversion. .
【０００７】ここで、後者である第２の方法をさらに展
開すると、同法は（ａ）酸化アルミニウムの皮膜を効率
よく化成させることを目的とする方法と、（ｂ）もっぱ
ら化成後の漏れ電流特性の向上を図ることを目的とする
方法とに分けられる。[0007] Here, the latter second method is further developed; (a) the method aims to efficiently chemically form the aluminum oxide film; and (b) the method focuses solely on leakage current after chemical formation. It can be divided into methods aimed at improving characteristics.
【０００８】上記（ａ）においては、１００Ｖ以下の低
圧用電極の場合、エッチングの後処理もしくは化成の前
処理として、４００〜６００℃の大気中で数分間熱処理
してエッチング箔上に酸化皮膜を形成する熱酸化を行な
ってから、本化成するようにしている。In the case of (a) above, in the case of a low voltage electrode of 100 V or less, as a post-etching treatment or a pre-treatment for chemical conversion, heat treatment is performed in the atmosphere at 400 to 600°C for several minutes to form an oxide film on the etching foil. After performing thermal oxidation to form the material, the main chemical formation is performed.
【０００９】これに対して、上記（ｂ）では例えば特開
昭６２−１７１８５号公報で説明されているように、エ
ッチング箔を燐酸を含む水溶液で処理し、次に高温にて
箔表面に熱酸化皮膜を形成した後、酸またはアルカリ溶
液にて処理し、その熱酸化皮膜の一部を残留させてから
化成するようにしている。On the other hand, in (b) above, the etching foil is treated with an aqueous solution containing phosphoric acid, and then the foil surface is heated at a high temperature, as described in JP-A No. 62-17185. After forming the oxide film, it is treated with an acid or alkaline solution to leave a portion of the thermal oxide film before chemical conversion.
【００１０】しかしながら、上記（ａ）（ｂ）の方法で
は、ともに単位面積当りの静電容量をアップさせること
、および化成電力の低減化が未だ不十分である。However, in both methods (a) and (b), it is still insufficient to increase the capacitance per unit area and to reduce the conversion power.
【００１１】また、酸化アルミニウムの皮膜を均一に形
成するための他の方法として、中高圧用箔については化
成前に熱水処理することが行なわれているが、水和処理
の皮膜は一般に厚いため、同方法を低圧用箔に適用して
も静電容量が増大しないばかりか、却って箔強度の低下
が起こり好ましい結果が得られない。[0011] Another method for uniformly forming an aluminum oxide film is to treat medium- and high-pressure foils with hot water before chemical formation, but the hydration-treated film is generally thicker. Therefore, even if the same method is applied to a low-voltage foil, not only will the capacitance not increase, but the strength of the foil will decrease, and favorable results will not be obtained.
【００１２】0012
【課題を解決するための手段】本発明は上記従来の欠点
を解消するためになされたもので、その構成上の特徴は
、アルミニウム箔の表面を粗面化し、脱塩素処理を行な
ったエッチング箔を、乾燥せずにそのままもしくは乾燥
させた後に、温水中に浸漬して水和処理を行ない、次に
予備加熱処理を行ない、引き続き熱処理して水和アルミ
ナを熱分解させた後、上記エッチング箔の表面に酸化皮
膜を形成する化成処理を行なうことにある。[Means for Solving the Problems] The present invention has been made to eliminate the above-mentioned conventional drawbacks, and its structural features include an etched foil in which the surface of aluminum foil is roughened and dechlorinated. The above-mentioned etched foil is processed as it is without drying or after drying, immersed in hot water to perform hydration treatment, then preheated, and then heat treated to thermally decompose the hydrated alumina. The purpose is to perform a chemical conversion treatment to form an oxide film on the surface of the material.
【００１３】この場合、上記水和処理における温水温度
は４０〜９８℃、好ましくは６０〜９０℃であり、かつ
、その処理時間は０．３〜３０分、好ましくは０．５〜
５分である。[0013] In this case, the hot water temperature in the above hydration treatment is 40 to 98°C, preferably 60 to 90°C, and the treatment time is 0.3 to 30 minutes, preferably 0.5 to 98°C.
It's 5 minutes.
【００１４】また、上記予備加熱処理の加熱温度は５０
〜２５０℃、好ましくは８０〜２３０℃であり、かつ、
その処理時間は０．３〜５分、好ましくは０．５〜３分
である。[0014] Furthermore, the heating temperature in the preheating treatment is 50°C.
-250°C, preferably 80-230°C, and
The treatment time is 0.3 to 5 minutes, preferably 0.5 to 3 minutes.
【００１５】さらに、上記熱処理の温度は２３０〜５５
０℃、好ましくは３５０〜５００℃であり、かつ、その
処理時間は０．０３〜２０時間、好ましくは０．５〜１
５時間である。Furthermore, the temperature of the heat treatment is 230 to 55
0°C, preferably 350-500°C, and the treatment time is 0.03-20 hours, preferably 0.5-1
It is 5 hours.
【００１６】[0016]
【作用】温水中に浸漬させる水和処理により、アルミニ
ウム表面に水和アルミナ（水酸化アルミニウム）が形成
される。次の予備加熱乾燥処理により吸着水が除去され
るとともに、その後の熱処理により水酸化アルミニウム
が熱分解され、表面に良質の酸化アルミニウムを有する
エッチング箔が得られる。[Operation] Hydrated alumina (aluminum hydroxide) is formed on the aluminum surface by hydration treatment by immersion in hot water. The adsorbed water is removed by the next preliminary heating and drying treatment, and the aluminum hydroxide is thermally decomposed by the subsequent heat treatment, resulting in an etched foil having high quality aluminum oxide on the surface.
【００１７】そして、以後の通常の化成処理により、良
質な皮膜を有する複合酸化皮膜が形成される。[0017] A complex oxide film having a good quality film is then formed by the subsequent ordinary chemical conversion treatment.
【００１８】このように本発明によれば、予めエッチン
グ箔表面に良質な酸化アルミニウムが形成されているた
め、化成皮膜形成時の電力消費が低減される。As described above, according to the present invention, since high-quality aluminum oxide is previously formed on the surface of the etching foil, power consumption during formation of the chemical conversion film is reduced.
【００１９】また、薄くて耐電圧を有する緻密な複合酸
化皮膜が形成されるため、単位面積当りの静電容量が増
大するとともに、コンデンサの駆動用電解液との反応が
非常に少なくなり、特に漏れ電流の安定したコンデンサ
が得られる。In addition, since a thin and dense composite oxide film with withstand voltage is formed, the capacitance per unit area increases and the reaction with the driving electrolyte of the capacitor is extremely reduced. A capacitor with stable leakage current can be obtained.
【００２０】[0020]
【実施例】以下、本発明の実施例およびそれと比較する
上での比較例について説明する。
《実施例１》
（Ａ）エッチング工程；純度９９．９％、厚み９０μｍ
のアルミニウム箔を塩酸９％、燐酸０．５％および硝酸
０．５％の水溶液からなる温度３０℃のエッチング液中
に浸漬し、正弦波交流電流で電流密度０．３Ａ／平方ｃ
ｍ、電気量１２０Ｃ／平方ｃｍのエッチングを行なった
。
（Ｂ）脱塩素処理；５％硝酸水溶液（液温４０℃）中に
１分間浸漬した。
（Ｃ）温水処理；４０℃の温水中に３０分間浸漬した。
（Ｄ）予備加熱処理；５０℃の大気中に５分間放置した
。
（Ｅ）熱処理；５２０℃の窒素ガス中で２時間熱処理し
た。
《実施例２》
（Ａ）エッチング工程；実施例１に同じ。
（Ｂ）脱塩素処理；実施例１に同じ。
（Ｃ）温水処理；５０℃の温水中に１５分間浸漬した。
（Ｄ）予備加熱処理；１５０℃の大気中に３分間放置し
た。
（Ｅ）熱処理；２５０℃の窒素ガス中で２０時間熱処理
した。
《実施例３》
（Ａ）エッチング工程；実施例１に同じ。
（Ｂ）脱塩素処理；実施例１に同じ。
（Ｃ）温水処理；６０℃の温水中に７分間浸漬した。
（Ｄ）予備加熱処理；１５０℃の大気中に２分間放置し
た。
（Ｅ）熱処理；５００℃の大気中で４時間熱処理した。
《実施例４》
（Ａ）エッチング工程；実施例１に同じ。
（Ｂ）脱塩素処理；実施例１に同じ。
（Ｃ）温水処理；７０℃の温水中に３分間浸漬した。
（Ｄ）予備加熱処理；２００℃の大気中に２分間放置し
た。
（Ｅ）熱処理；３５０℃の水素ガスと窒素ガスの混合ガ
ス中で１５時間熱処理した。
《実施例５》
（Ａ）エッチング工程；実施例１に同じ。
（Ｂ）脱塩素処理；実施例１に同じ。
（Ｃ）温水処理；８０℃の温水中に２分間浸漬した。
（Ｄ）予備加熱処理；２００℃の大気中に１分間放置し
た。
（Ｅ）熱処理；５００℃の窒素ガスと酸素ガスの混合ガ
ス中で４時間熱処理した。
《実施例６》
（Ａ）エッチング工程；実施例１に同じ。
（Ｂ）脱塩素処理；実施例１に同じ。
（Ｃ）温水処理；８０℃の温水中に２分間浸漬した。
（Ｄ）予備加熱処理；２００℃の大気中に１分間放置し
た。
（Ｅ）熱処理；５００℃の窒素ガスと酸素ガスの混合ガ
ス中で０．５時間熱処理した。
《実施例７》
（Ａ）エッチング工程；実施例１に同じ。
（Ｂ）脱塩素処理；実施例１に同じ。
（Ｃ）温水処理；８０℃の温水中に２分間浸漬した。
（Ｄ）予備加熱処理；２００℃の大気中に１分間放置し
た。
（Ｅ）熱処理；５００℃の窒素ガスと酸素ガスの混合ガ
ス中で０．０３時間熱処理した。
《実施例８》
（Ａ）エッチング工程；実施例１に同じ。
（Ｂ）脱塩素処理；実施例１に同じ。
（Ｃ）温水処理；９０℃の温水中に１分間浸漬した。
（Ｄ）予備加熱処理；２５０℃の大気中に１分間放置し
た。
（Ｅ）熱処理；４００℃のアルゴンガス中で１２時間熱
処理した。
《実施例９》
（Ａ）エッチング工程；実施例１に同じ。
（Ｂ）脱塩素処理；実施例１に同じ。
（Ｃ）温水処理；９８℃の温水中に０．５分間浸漬した
。
（Ｄ）予備加熱処理；２５０℃の大気中に０．５分間放
置した。
（Ｅ）熱処理；４００℃の大気中で１２時間熱処理した
。
〈比較例１〉
（Ａ）エッチング工程；実施例１に同じ。
（Ｂ）脱塩素処理；実施例１に同じ。
（Ｃ）温水処理；９８℃の温水中に２分間浸漬した。
（Ｄ）予備加熱処理；なし。
（Ｅ）熱処理；なし。
〈比較例２〉
（Ａ）エッチング工程；実施例１に同じ。
（Ｂ）脱塩素処理；実施例１に同じ。
（Ｃ）温水処理；なし。
（Ｄ）予備加熱処理；なし。
（Ｅ）熱処理；なし。
〈比較例３〉
（Ａ）エッチング工程；実施例１に同じ。
（Ｂ）脱塩素処理；実施例１に同じ。
（Ｃ）温水処理；なし。
（Ｄ）予備加熱処理；なし。
（Ｅ）熱処理；５００℃の窒素ガス中で４時間熱処理し
た。
〈比較例４〉
（Ａ）エッチング工程；実施例１に同じ。
（Ｂ）脱塩素処理；実施例１に同じ。
（Ｃ）燐酸処理；０．１％燐酸水溶液（液温４０℃）に
１分間浸漬した。
（Ｄ）熱処理；５００℃の大気中で１分間熱処理した。
（Ｅ）溶解処理；５％クエン酸水溶液（液温４０℃）に
２分間浸漬した。EXAMPLES Examples of the present invention and comparative examples for comparison therewith will be described below. <<Example 1>> (A) Etching process; purity 99.9%, thickness 90 μm
aluminum foil was immersed in an etching solution of 9% hydrochloric acid, 0.5% phosphoric acid, and 0.5% nitric acid at a temperature of 30°C, and the current density was 0.3 A/sq.c. using a sinusoidal alternating current.
Etching was performed with an electric charge of 120 C/cm2. (B) Dechlorination treatment; immersed in 5% nitric acid aqueous solution (liquid temperature 40°C) for 1 minute. (C) Hot water treatment; immersed in 40°C hot water for 30 minutes. (D) Preheating treatment; left in the atmosphere at 50°C for 5 minutes. (E) Heat treatment: Heat treatment was performed in nitrogen gas at 520° C. for 2 hours. <<Example 2>> (A) Etching process; same as Example 1. (B) Dechlorination treatment; same as Example 1. (C) Hot water treatment: Immersed in hot water at 50°C for 15 minutes. (D) Preheating treatment; left in the atmosphere at 150°C for 3 minutes. (E) Heat treatment: Heat treatment was performed in nitrogen gas at 250° C. for 20 hours. <<Example 3>> (A) Etching process; same as Example 1. (B) Dechlorination treatment; same as Example 1. (C) Hot water treatment; immersed in hot water at 60°C for 7 minutes. (D) Preheating treatment; left in the atmosphere at 150°C for 2 minutes. (E) Heat treatment: Heat treatment was performed in the atmosphere at 500°C for 4 hours. <<Example 4>> (A) Etching process; same as Example 1. (B) Dechlorination treatment; same as Example 1. (C) Hot water treatment: Immersed in hot water at 70°C for 3 minutes. (D) Preheating treatment; left in the atmosphere at 200°C for 2 minutes. (E) Heat treatment: Heat treatment was performed for 15 hours in a mixed gas of hydrogen gas and nitrogen gas at 350°C. <<Example 5>> (A) Etching process; same as Example 1. (B) Dechlorination treatment; same as Example 1. (C) Hot water treatment; immersed in 80°C hot water for 2 minutes. (D) Preheating treatment; left in the atmosphere at 200° C. for 1 minute. (E) Heat treatment: Heat treatment was performed for 4 hours in a mixed gas of nitrogen gas and oxygen gas at 500°C. <<Example 6>> (A) Etching process; same as Example 1. (B) Dechlorination treatment; same as Example 1. (C) Hot water treatment; immersed in 80°C hot water for 2 minutes. (D) Preheating treatment; left in the atmosphere at 200° C. for 1 minute. (E) Heat treatment: Heat treatment was performed for 0.5 hours in a mixed gas of nitrogen gas and oxygen gas at 500°C. <<Example 7>> (A) Etching process; same as Example 1. (B) Dechlorination treatment; same as Example 1. (C) Hot water treatment; immersed in 80°C hot water for 2 minutes. (D) Preheating treatment; left in the atmosphere at 200° C. for 1 minute. (E) Heat treatment: Heat treatment was performed for 0.03 hours in a mixed gas of nitrogen gas and oxygen gas at 500°C. <<Example 8>> (A) Etching process; same as Example 1. (B) Dechlorination treatment; same as Example 1. (C) Hot water treatment: Immersed in 90°C hot water for 1 minute. (D) Preheating treatment; left in the atmosphere at 250°C for 1 minute. (E) Heat treatment: Heat treatment was performed in argon gas at 400° C. for 12 hours. <<Example 9>> (A) Etching process; same as Example 1. (B) Dechlorination treatment; same as Example 1. (C) Hot water treatment: immersed in 98°C hot water for 0.5 minutes. (D) Preheating treatment; left in the atmosphere at 250°C for 0.5 minutes. (E) Heat treatment: Heat treatment was performed in the atmosphere at 400°C for 12 hours. <Comparative Example 1> (A) Etching step; same as Example 1. (B) Dechlorination treatment; same as Example 1. (C) Hot water treatment: Immersed in 98°C hot water for 2 minutes. (D) Preheating treatment: None. (E) Heat treatment: None. <Comparative Example 2> (A) Etching step; same as Example 1. (B) Dechlorination treatment; same as Example 1. (C) Hot water treatment; none. (D) Preheating treatment: None. (E) Heat treatment: None. <Comparative Example 3> (A) Etching step; same as Example 1. (B) Dechlorination treatment; same as Example 1. (C) Hot water treatment; none. (D) Preheating treatment: None. (E) Heat treatment: Heat treatment was performed in nitrogen gas at 500° C. for 4 hours. <Comparative Example 4> (A) Etching step; same as Example 1. (B) Dechlorination treatment; same as Example 1. (C) Phosphoric acid treatment: Immersed in 0.1% phosphoric acid aqueous solution (liquid temperature 40°C) for 1 minute. (D) Heat treatment: Heat treatment was performed in the air at 500° C. for 1 minute. (E) Dissolution treatment: Immersed in 5% citric acid aqueous solution (liquid temperature 40°C) for 2 minutes.
【００２１】上記実施例１〜９および比較例１〜４で得
られた各エッチング箔を５％アジピン酸水溶液（液温８
５℃）中で３５Ｖの化成電圧を印加して化成を行ない、
それらの単位面積当りの静電容量（μＦ／平方ｃｍ）と
、化成に要した電気量（クーロン／平方ｃｍ）を測定し
た結果を表１に示す。Each of the etched foils obtained in Examples 1 to 9 and Comparative Examples 1 to 4 above was treated with a 5% adipic acid aqueous solution (liquid temperature: 8
5°C) by applying a formation voltage of 35V,
Table 1 shows the results of measuring the capacitance per unit area (μF/cm2) and the amount of electricity required for chemical formation (coulombs/cm2).
【００２２】次に、これらの各エッチング箔を陽極箔に
用い、セパレータを介して陰極箔とともに巻回した後、
電解液を含浸させ外装ケース内に封入して、定格２５Ｖ
・１０００μＦのアルミニウム電解コンデンサを製作し
た。なお、電解液にはアジピン酸アンモニウム１０％、
水１０％、そしてエチレングリコール８０％のものを用
いた。Next, each of these etched foils was used as an anode foil, and after being wound together with a cathode foil through a separator,
Impregnated with electrolyte and sealed inside the outer case, rated at 25V
・Manufactured a 1000μF aluminum electrolytic capacitor. In addition, the electrolyte contains 10% ammonium adipate,
10% water and 80% ethylene glycol were used.
【００２３】このようにして製作した各コンデンサにつ
いて、８５℃の高温貯蔵試験を１０００時間行なった後
に漏れ電流（μＡ）を測定した。その結果を表１に併せ
て示す。For each of the capacitors thus manufactured, a high temperature storage test at 85° C. was conducted for 1000 hours, and then the leakage current (μA) was measured. The results are also shown in Table 1.
【００２４】[0024]
【表１】[Table 1]
【００２５】[0025]
【発明の効果】以上説明したように、本発明によれば、
従来に比べて静電容量が約６〜２３％高められる。また
、化成電力が低減できるとともに、漏れ電流が少なく、
しかもその特性の安定した電極箔が製造される。[Effects of the Invention] As explained above, according to the present invention,
The capacitance is increased by about 6 to 23% compared to the conventional one. In addition, the chemical power consumption can be reduced, and leakage current is small.
Moreover, an electrode foil with stable characteristics can be manufactured.
【００２６】したがって、アルミニウム電解コンデンサ
の小型化およびコストダウン、さらには長寿命化に寄与
するところ大である。[0026] Therefore, it greatly contributes to miniaturization and cost reduction of aluminum electrolytic capacitors, as well as to longer life.
Claims (4)
処理を行なったエッチング箔を、温水中に浸漬して水和
処理を行ない、次に予備加熱処理を行ない、引き続き熱
処理して水和アルミナを熱分解させた後、上記エッチン
グ箔の表面に酸化皮膜を形成する化成処理を行なうこと
を特徴とするアルミニウム電解コンデンサ用電極箔の製
造方法。Claim 1: Etched aluminum foil whose surface has been roughened and dechlorinated is immersed in hot water for hydration treatment, then preheated, and then heat treated for hydration. A method for manufacturing an electrode foil for an aluminum electrolytic capacitor, comprising thermally decomposing alumina and then performing a chemical conversion treatment to form an oxide film on the surface of the etched foil.
８℃であり、かつ、その処理時間は０．３〜３０分であ
る請求項１に記載のアルミニウム電解コンデンサ用電極
箔の製造方法。[Claim 2] The hot water temperature in the hydration treatment is 40 to 9
The method for manufacturing an electrode foil for an aluminum electrolytic capacitor according to claim 1, wherein the temperature is 8°C and the treatment time is 0.3 to 30 minutes.
０℃であり、かつ、その処理時間は０．３〜５分である
請求項１に記載のアルミニウム電解コンデンサ用電極箔
の製造方法。[Claim 3] The heating temperature of the preheating treatment is 50 to 25%.
2. The method for producing an electrode foil for an aluminum electrolytic capacitor according to claim 1, wherein the temperature is 0° C. and the treatment time is 0.3 to 5 minutes.
り、かつ、その処理時間は０．０３〜２０時間である請
求項１に記載のアルミニウム電解コンデンサ用電極箔の
製造方法。4. The method of manufacturing an electrode foil for an aluminum electrolytic capacitor according to claim 1, wherein the temperature of the heat treatment is 230 to 550° C., and the treatment time is 0.03 to 20 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3067868A JPH07114178B2 (en) | 1991-03-07 | 1991-03-07 | Method for manufacturing electrode foil for aluminum electrolytic capacitor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3067868A JPH07114178B2 (en) | 1991-03-07 | 1991-03-07 | Method for manufacturing electrode foil for aluminum electrolytic capacitor |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH04279017A true JPH04279017A (en) | 1992-10-05 |
| JPH07114178B2 JPH07114178B2 (en) | 1995-12-06 |
Family
ID=13357338
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP3067868A Expired - Fee Related JPH07114178B2 (en) | 1991-03-07 | 1991-03-07 | Method for manufacturing electrode foil for aluminum electrolytic capacitor |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH07114178B2 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005347681A (en) * | 2004-06-07 | 2005-12-15 | Nichicon Corp | Method of manufacturing anode foil for aluminum electrolytic capacitor |
| JP2006108395A (en) * | 2004-10-06 | 2006-04-20 | Nichicon Corp | Manufacturing method for electrode foil for aluminum electrolytic capacitor |
| JP2021027120A (en) * | 2019-08-02 | 2021-02-22 | ニチコン株式会社 | Method for manufacturing electrode foil for aluminum electrolytic capacitor |
-
1991
- 1991-03-07 JP JP3067868A patent/JPH07114178B2/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005347681A (en) * | 2004-06-07 | 2005-12-15 | Nichicon Corp | Method of manufacturing anode foil for aluminum electrolytic capacitor |
| JP2006108395A (en) * | 2004-10-06 | 2006-04-20 | Nichicon Corp | Manufacturing method for electrode foil for aluminum electrolytic capacitor |
| JP4576192B2 (en) * | 2004-10-06 | 2010-11-04 | ニチコン株式会社 | Method for producing electrode foil for aluminum electrolytic capacitor |
| JP2021027120A (en) * | 2019-08-02 | 2021-02-22 | ニチコン株式会社 | Method for manufacturing electrode foil for aluminum electrolytic capacitor |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH07114178B2 (en) | 1995-12-06 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP2663541B2 (en) | Method for producing electrode foil for aluminum electrolytic capacitor | |
| JPH04279017A (en) | Manufacture of electrode foil for aluminum electrolytic capacitor | |
| JP3853432B2 (en) | Method for producing electrode foil for aluminum electrolytic capacitor | |
| JPH10135080A (en) | Solid-state electrolytic capacitor and its manufacture | |
| JP3478039B2 (en) | Method of forming electrode foil for aluminum electrolytic capacitor | |
| JP4811939B2 (en) | Formation method of electrode foil for electrolytic capacitor | |
| JPH04280413A (en) | Manufacture of electrode foil for aluminum electrolytic capacitor | |
| JPH04279018A (en) | Manufacture of electrode foil for aluminum electrolytic capacitor | |
| JP3480311B2 (en) | Method for producing electrode foil for aluminum electrolytic capacitor | |
| JPH09167720A (en) | Aluminum solid electrolyte capacitor electrode manufacturing method | |
| JP3407470B2 (en) | Method for producing electrode foil for aluminum electrolytic capacitor | |
| JPH08296088A (en) | Production of electrode foil for aluminum electrolytic capacitor | |
| JPH0777180B2 (en) | Method for manufacturing solid electrolytic capacitor | |
| JPH0566005B2 (en) | ||
| JP3460418B2 (en) | Manufacturing method of electrode foil for aluminum electrolytic capacitor | |
| JPH10112423A (en) | Formation method for anodic foil for aluminum electrolytic capacitor | |
| JP3309177B2 (en) | Surface enlargement treatment method for electrode foil for aluminum electrolytic capacitor | |
| JPH07272985A (en) | Manufacturing method for anode foil for aluminum electrolytic capacitor | |
| JP2008112877A (en) | Manufacturing method of electrode foil for electrolytic capacitor | |
| JPH0722078B2 (en) | Manufacturing method of solid electrolytic capacitor | |
| JPH0661104A (en) | Treatment method of electrode material for capacitor | |
| JPS6053453B2 (en) | Aluminum chemical conversion method | |
| JPH0566004B2 (en) | ||
| JPH01287918A (en) | Manufacture of electrode foil for aluminum electrolytic capacitor | |
| JPH01287916A (en) | Manufacture of electrode foil for aluminum electrolytic capacitor |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A01 | Written decision to grant a patent or to grant a registration (utility model) |
Free format text: JAPANESE INTERMEDIATE CODE: A01 Effective date: 19960806 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20081206 Year of fee payment: 13 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20081206 Year of fee payment: 13 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20091206 Year of fee payment: 14 |
|
| LAPS | Cancellation because of no payment of annual fees |