JP3293241B2 - Aluminum foil material for electrodes of electrolytic capacitors with excellent surface area expansion effect - Google Patents
Aluminum foil material for electrodes of electrolytic capacitors with excellent surface area expansion effectInfo
- Publication number
- JP3293241B2 JP3293241B2 JP14145293A JP14145293A JP3293241B2 JP 3293241 B2 JP3293241 B2 JP 3293241B2 JP 14145293 A JP14145293 A JP 14145293A JP 14145293 A JP14145293 A JP 14145293A JP 3293241 B2 JP3293241 B2 JP 3293241B2
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- JP
- Japan
- Prior art keywords
- foil material
- content
- surface area
- diffusion
- weight
- Prior art date
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- Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)
Description
【０００１】[0001]
【産業上の利用分野】この発明は、エッチング処理で、
一段と大きい表面積の形成が可能な電解コンデンサの電
極用アルミニウム箔材に関するものである。This invention relates to an etching process,
The present invention relates to an aluminum foil material for an electrode of an electrolytic capacitor capable of forming a larger surface area.
【０００２】[0002]
【従来の技術】従来、一般に、電解コンデンサの電極と
して、純度：９９．９重量％以上のＡｌからなるアルミ
ニウム箔材が用いられており、また電極の表面積が大き
いほど高い静電容量が得られる、すなわち表面積と静電
容量とは比例することから、エッチング処理時により一
段と高い表面積を得る目的で、例えば特公昭６２−４２
３７０号公報や特開平１−１２８４１９号公報などに記
載されるように、箔材の表面部に、表面積拡大作用を有
するＰｂ，Ｂｉ，Ｉｎ、およびＳｎなどのうちの１種ま
たは２種以上を、０．００１〜０．２重量％（１０〜２
０００ppm ）の割合で含有する表面拡散層を形成してな
るアルミニウム箔材も提案されている。2. Description of the Related Art Conventionally, an aluminum foil material made of Al having a purity of 99.9% by weight or more is generally used as an electrode of an electrolytic capacitor, and a higher capacitance is obtained as the surface area of the electrode is larger. That is, since the surface area is proportional to the capacitance, for the purpose of obtaining a higher surface area during the etching process, for example, Japanese Patent Publication No. Sho 62-42
As described in JP-A-370 and JP-A-1-128419, one or two or more of Pb, Bi, In, Sn, and the like having a surface area increasing action are provided on the surface of the foil material. , 0.001-0.2% by weight (10-2
An aluminum foil material having a surface diffusion layer containing 2,000 ppm) is also proposed.
【０００３】[0003]
【発明が解決しようとする課題】一方、近年の電解コン
デンサの小型化および高性能化に対する要求は強く、こ
れに伴ない、電極には一段の表面積拡大化が望まれてい
るが、上記の従来アルミニウム箔材では、上記の要求を
満足するに足る十分な表面積をエッチング処理で形成す
ることができず、また他方で上記の表面積拡大作用成分
の箔材表面部における含有量を多くして、より一層の表
面積拡大化をはかる試みもなされたが、これらの成分が
多くなると、エッチングが過度に進行し、全面腐食型と
なってしまい、表面積の望む拡大がはかれないのが現状
である。On the other hand, in recent years, there has been a strong demand for downsizing and high performance of electrolytic capacitors, and accordingly, it has been desired to further increase the surface area of the electrodes. In an aluminum foil material, a sufficient surface area that satisfies the above-mentioned requirements cannot be formed by etching, and on the other hand, the content of the above-mentioned surface area increasing action component in the foil material surface portion is increased, so that Attempts have been made to further increase the surface area, but when these components are increased, the etching proceeds excessively and the entire surface becomes corrosive, and the desired surface area cannot be increased at present.
【０００４】[0004]
【課題を解決するための手段】そこで、本発明者等は、
上述のような観点から、エッチング処理で一段と大きい
表面積拡大化が可能な電解コンデンサの電極用アルミニ
ウム箔材を開発すべく研究を行なった結果、箔材中心部
を実質的に９９．９重量％以上の純度を有するＡｌで構
成して、電極に要求される強度と電気的特性を確保した
状態で、箔材表面部に、Ｐｂ，Ｂｉ，Ｉｎ、およびＳｎ
のうちの１種または２種以上（以下、これらを総称して
第１拡散成分という）と、Ｆｅ，Ｎｉ，Ｃｏ，Ｃｒ，Ｍ
ｎ、およびＺｒのうちの１種または２種以上（以下、こ
れらを総称して第２拡散成分という）とを、それぞれ箔
材最表面部における含有量が、第１拡散成分で０．２５
〜３重量％、第２拡散成分で０．００１〜１重量％とな
る割合で共存含有させると共に、これら成分の含有量が
表面から０．５〜２０μｍの範囲内の所定深さ位置まで
減少する濃度勾配層を形成したアルミニウム箔材におい
ては、これにエッチング処理を施すと、箔材最表面部に
おける相対的に高含有量の第１拡散成分と第２拡散成分
との共存、並びに箔材表面部の濃度勾配によって、箔材
表面には深く微細なピットが高い密度で均一に形成され
るようになり、この結果表面積の著しい拡大がもたらさ
れるという研究結果を得たのである。Means for Solving the Problems Accordingly, the present inventors have
From the above-mentioned viewpoints, as a result of conducting research to develop an aluminum foil material for an electrode of an electrolytic capacitor capable of further increasing the surface area by etching, the center of the foil material was substantially 99.9% by weight or more. Pb, Bi, In, and Sn are formed on the surface of the foil material while the strength and electrical characteristics required for the electrode are ensured.
And one or more of these (hereinafter, collectively referred to as a first diffusion component), Fe, Ni, Co, Cr, M
One or more of n and Zr (hereinafter, these are collectively referred to as a second diffusion component) have a content in the outermost surface of the foil material of the first diffusion component of 0.25, respectively.
To 3% by weight and 0.001 to 1% by weight of the second diffusion component, and the content of these components decreases from the surface to a predetermined depth within a range of 0.5 to 20 μm. When an aluminum foil material having a concentration gradient layer formed thereon is subjected to an etching treatment, a relatively high content of the first diffusion component and the second diffusion component having a relatively high content at the outermost surface of the foil material, According to the research results, the concentration gradient of the portion allows the deep and fine pits to be uniformly formed at a high density on the foil material surface, resulting in a remarkable increase in the surface area.
【０００５】この発明は、上記の研究結果にもとづいて
なされたものであって、箔材最表面部における第１拡散
成分の含有量が０．２５〜３重量％、同じく第２拡散成
分の含有量が０．００１〜１重量％にして、箔材表面部
には、前記最表面部における第１および第２拡散成分の
含有量が表面から０．５〜２０μｍの範囲内の所定深さ
位置まで減少する濃度勾配を有し、かつ箔材中心部が実
質的に純度：９９．９重量％以上のＡｌからなる、エッ
チング処理ですぐれた表面積拡大効果を発揮する電解コ
ンデンサの電極用アルミニウム箔材に特徴を有するもの
である。The present invention has been made based on the above research results, wherein the content of the first diffusing component in the outermost surface of the foil material is 0.25 to 3% by weight, and the content of the second diffusing component is the same. The amount is set to 0.001 to 1% by weight, and at the surface of the foil material, the first and second diffusion components in the outermost surface are located at a predetermined depth within a range of 0.5 to 20 μm from the surface. Aluminum foil material for electrodes of electrolytic capacitors that has a concentration gradient that decreases to a minimum and that the center of the foil material is substantially composed of Al having a purity of 99.9% by weight or more, and exhibits an excellent surface area expansion effect by etching. It is characterized by the following.
【０００６】なお、この発明のアルミニウム箔材は、上
記第１拡散成分：１．５〜２０ppmを含有し、残りがＡ
ｌと不可避不純物からなるＡｌ合金箔素材を用意し、こ
のＡｌ合金箔素材の表面に、イオンプレーティング法な
どによって上記第２拡散成分の薄膜を所定の厚さで形成
するか、あるいは上記第２拡散成分のアセチルアセト
ン、ステアリン酸、およびナフテン酸塩などのうちの１
種または２種以上を通常０．１〜０．５重量％程度含有
するＩＰＡ溶液またはミネラルスピリット溶液を所定の
厚さで塗布し、この状態のＡｌ合金箔素材に、非酸化性
雰囲気中、５００〜６００℃の温度に加熱保持の条件で
加熱処理を施すことによって製造するのが望ましく、上
記加熱処理によって、Ａｌ合金箔素材中に均等に含有す
る上記第１拡散成分が箔材表面部に拡散移動して、箔材
中心部が９９．９重量％以上の純度をもったＡｌとな
り、一方箔材表面部には第１拡散成分の含有量が最表面
部ほど高くなる濃度勾配層が形成され、さらにＡｌ合金
箔素材表面上に存在する第２拡散成分も表面から素材内
部に拡散して、前記第２拡散成分の含有量が最表面部ほ
ど高くなる濃度勾配層が形成されるようになるものであ
り、また、箔材最表面部における第１および第２拡散成
分の含有量、並びに濃度勾配層の深さは、主としてＡｌ
合金箔素材中の第１拡散成分の含有量、加熱温度、およ
び加熱時間を適宜調整することにより制御することがで
きる。The aluminum foil material of the present invention contains the first diffusion component: 1.5 to 20 ppm, and the balance is A
1 and an unavoidable impurity, an Al alloy foil material is prepared, and a thin film of the second diffusion component is formed on the surface of the Al alloy foil material by an ion plating method or the like to a predetermined thickness. One of the diffusion components acetylacetone, stearic acid, naphthenate, etc.
An IPA solution or a mineral spirit solution generally containing about 0.1 to 0.5% by weight of a seed or two or more kinds is applied to a predetermined thickness, and the Al alloy foil material in this state is placed in a non-oxidizing atmosphere in a non-oxidizing atmosphere. It is desirable to manufacture by performing a heat treatment under the condition of heating and holding at a temperature of up to 600 ° C., and the first diffusion component uniformly contained in the Al alloy foil material is diffused to the surface of the foil material by the heat treatment. By moving, the central portion of the foil material becomes Al having a purity of 99.9% by weight or more, while a concentration gradient layer in which the content of the first diffusion component is higher at the outermost surface portion is formed on the surface portion of the foil material. Further, the second diffusion component existing on the surface of the Al alloy foil material also diffuses from the surface into the inside of the material, so that a concentration gradient layer in which the content of the second diffusion component becomes higher toward the outermost surface is formed. And the top of the foil material Content of the first and second diffuse component in section, and the depth of the concentration gradient layer is mainly Al
It can be controlled by appropriately adjusting the content of the first diffusion component in the alloy foil material, the heating temperature, and the heating time.
【０００７】この発明のアルミニウム箔材において、第
１および第２拡散成分の箔材最表面部における含有量お
よび表面部における濃度勾配層深さ、さらに箔材中心部
のＡｌ純度を上記の通りに限定した理由を以下に説明す
る。すなわち、これらの第１および第２拡散成分の含有
量、濃度勾配層深さ、およびＡｌ純度は上記の通りＡｌ
合金箔素材中の第１拡散成分の含有量および加熱処理条
件によって所定の値に制御されるものであるが、箔材最
表面部の第１拡散成分の含有量が０．２５重量％未満の
場合、箔材表面部に形成されるこれの濃度勾配層の深さ
を０．５μｍ以上にすることが困難となり、この場合
や、同じく第２拡散成分の含有量が０．００１重量％未
満の場合には、エッチング処理で著しい表面積拡大効果
が得られる微細にして深いピットの高密度での形成が困
難になり、一方第１および第２拡散成分の箔材最表面部
の含有量がそれぞれ３重量％および１重量％を越えると
腐食減量が多くなりすぎ、箔材強度が低下するようにな
ることから、第１および第２拡散成分の含有量をそれぞ
れ０．２５〜３重量％および０．００１〜１重量％と定
めた。In the aluminum foil material of the present invention, the contents of the first and second diffusion components at the outermost surface of the foil material, the depth of the concentration gradient layer at the surface portion, and the Al purity at the center of the foil material are as described above. The reason for the limitation will be described below. That is, the content of these first and second diffusion components, the depth of the concentration gradient layer, and the Al purity are as described above.
It is controlled to a predetermined value by the content of the first diffusion component in the alloy foil material and the heat treatment conditions, but the content of the first diffusion component at the outermost surface of the foil material is less than 0.25% by weight. In this case, it is difficult to make the depth of the concentration gradient layer formed on the surface of the foil material 0.5 μm or more. In this case, the content of the second diffusion component is also less than 0.001% by weight. In this case, it is difficult to form fine and deep pits at a high density so that a remarkable surface area enlargement effect can be obtained by the etching process, while the content of the first and second diffusion components in the outermost surface of the foil material is 3% respectively. If it exceeds 1% by weight, the weight loss due to corrosion becomes too large, and the strength of the foil material decreases. Therefore, the contents of the first and second diffusion components are 0.25 to 3% by weight and 0. 001 to 1% by weight.
【０００８】また、上記濃度勾配層は、最表面部におけ
る第１および第２拡散成分の高含有と相まって、深く細
かいピットを高密度で形成するのに不可欠であるが、そ
の深さが０．５μｍ未満では腐食が全面腐食型になって
しまい、所望のすぐれた表面積拡大効果が得られず、一
方その深さが２０μｍを越えると、箔材の強度が低下す
るようになることから、濃度勾配層深さを０．５〜２０
μｍと定めた。さらに、箔材中心部のＡｌ純度が９９．
９重量％未満では、電解コンデンサの電極に要求される
強度および電気的特性を保持することができなくなるこ
とから、その純度を９９．９重量％以上と定めた。The concentration gradient layer is indispensable for forming deep and fine pits at high density in combination with the high content of the first and second diffusion components in the outermost surface portion. If the thickness is less than 5 μm, the corrosion becomes a general corrosion type, and the desired excellent surface area enlarging effect cannot be obtained. On the other hand, if the depth exceeds 20 μm, the strength of the foil material is reduced. 0.5 to 20 layer depth
μm. Furthermore, the purity of Al at the center of the foil material is 99.
If the content is less than 9% by weight, the strength and electrical characteristics required for the electrodes of the electrolytic capacitor cannot be maintained, so the purity is determined to be 99.9% by weight or more.
【０００９】[0009]
【実施例】つぎに、この発明のアルミニウム箔材を実施
例により具体的に説明する。通常の低周波誘導溶解炉に
て、原料として用いた純度：９９．９９重量％の純Ａ
ｌ：５kgをそれぞれ溶解し、これに表１に示される量の
第１拡散成分を含有させ、半連続鋳造法にて断面形状：
４０mm×１８０mm、長さ：２５０mmの鋳塊とし、この鋳
塊に、両面をそれぞれ０．５mmの厚さ面削した状態で、
５２０℃の熱間圧延開始温度にて熱間圧延を施して、厚
さ：６mmの熱延板とし、これに通常の条件で、必要に応
じて中間焼鈍を加えながら冷間圧延を施して同じく表１
に示される厚さのＡｌ合金箔素材Ａ〜Ｏを形成し、つい
で前記Ａｌ合金箔素材Ａ〜ＯのうちのＫ〜Ｏを除くＡ〜
ＪのＡｌ合金箔素材のそれぞれの表面に表２に示される
組合せで、イオンプレーティング法を用い、通常の条件
で第２拡散成分薄膜をそれぞれ形成し、つぎにこの結果
の表面に第２拡散成分薄膜を有するＡｌ合金箔素材Ａ〜
Ｊおよび上記の第２拡散成分薄膜の形成がないＡｌ合金
箔素材Ｋ〜Ｏのそれぞれに、同じく表２に示される条件
で加熱処理を施すことにより本発明箔材１〜１０および
従来箔材１〜５をそれぞれ製造した。EXAMPLES Next, the aluminum foil material of the present invention will be specifically described with reference to examples. Purity used as a raw material in a normal low-frequency induction melting furnace: purity 99.99% by weight pure A
l: 5 kg each was dissolved, and the first diffusion component in the amount shown in Table 1 was added thereto.
40mm x 180mm, length: 250mm ingot, with both sides of this ingot having a 0.5mm thick face cut,
Hot rolling is performed at a hot rolling start temperature of 520 ° C. to form a hot-rolled sheet having a thickness of 6 mm, which is subjected to cold rolling under ordinary conditions while adding intermediate annealing as necessary. Table 1
To form the Al alloy foil materials A to O having the thickness shown in FIG.
A second diffusion component thin film is formed on each surface of the Al alloy foil material of J in accordance with the combination shown in Table 2 by ion plating under normal conditions, and then the second diffusion component thin film is formed on the resulting surface. Al alloy foil material A with component thin film
J and the Al alloy foil materials KO having no second diffusion component thin film formed thereon are subjected to a heat treatment under the same conditions as shown in Table 2 to obtain the foil materials 1 to 10 of the present invention and the conventional foil material 1. To 5 were each manufactured.
【００１０】この結果得られた本発明箔材１〜１０およ
び従来箔材１〜５について、最表面部、すなわち表面か
ら深さ：０．０５μｍの位置の第１拡散成分の含有量お
よび中心部のＡｌ純度を測定し、さらに本発明箔材１〜
１０については、最表面部の第２拡散成分の含有量を測
定すると共に、前記最表面部から第１および第２拡散成
分の含有量がそれぞれ減少して、第１拡散成分について
は箔材中心部と同じ含有量となり、また第２拡散成分に
ついては実質的に含有しない状態となる表面からの深さ
位置、すなわち表面濃度勾配層の平均層厚、並びに前記
表面濃度勾配層の中間点の第１および第２拡散成分の含
有量を測定し、これらの測定結果を表３，４に示した。
また、表３，４には、水：１ｌに対し塩酸：１モルと硫
酸：３モルの割合で加えた８０℃の混酸水溶液中に浸漬
し、電流密度：０．６Ａ／cm2 、時間：４０秒の条件で
エッチング処理を行ない、かつ化成電圧：２５０Ｖで静
電容量を測定した結果も示した。Regarding the foil materials 1 to 10 of the present invention and the conventional foil materials 1 to 5 obtained as a result, the content and the center of the first diffusion component at the outermost surface, that is, at a depth of 0.05 μm from the surface. Was measured, and the foil materials 1 to 5 of the present invention were further measured.
For 10, the content of the second diffusion component in the outermost surface was measured, and the content of the first and second diffusion components decreased from the outermost surface, respectively. Part, and the depth position from the surface at which the second diffusion component is not substantially contained, that is, the average thickness of the surface concentration gradient layer, and the middle position of the surface concentration gradient layer. The contents of the first and second diffusion components were measured, and the measurement results are shown in Tables 3 and 4.
Tables 3 and 4 show that the sample was immersed in a mixed acid aqueous solution at 80 ° C. added at a ratio of 1 mol of hydrochloric acid and 3 mol of sulfuric acid to 1 liter of water, current density: 0.6 A / cm 2 , time: The results obtained by performing the etching treatment under the condition of 40 seconds and measuring the capacitance at a formation voltage of 250 V are also shown.
【００１１】[0011]
【表１】 [Table 1]
【００１２】[0012]
【表２】 [Table 2]
【００１３】[0013]
【表３】 [Table 3]
【００１４】[0014]
【表４】 [Table 4]
【００１５】[0015]
【発明の効果】表１〜４に示される結果から、本発明箔
材１〜１０は、いずれも最表面部における第１拡散成分
の高含有および第２拡散成分の共存含有、並びに表面部
に形成された第１および第２拡散成分の濃度勾配層によ
って、従来箔材１〜５に比して大きな静電容量を示し、
エッチング処理による表面積拡大率がきわめて高いこと
が明らかである。上述のように、この発明のアルミニウ
ム箔材は、エッチング処理で高い表面積拡大率を示すの
で、これを電解コンデンサの電極として用いた場合に、
これの小形化および高性能化に大いに寄与するものであ
る。From the results shown in Tables 1 to 4, all of the foil materials 1 to 10 of the present invention have a high content of the first diffusion component and a coexistence content of the second diffusion component in the outermost surface, and Due to the formed concentration gradient layers of the first and second diffusion components, a large capacitance is shown as compared with the conventional foil materials 1 to 5,
It is clear that the surface area expansion rate by the etching process is extremely high. As described above, since the aluminum foil material of the present invention shows a high surface area expansion rate by etching, when this is used as an electrode of an electrolytic capacitor,
This greatly contributes to downsizing and high performance.
フロントページの続き (56)参考文献 特開 平３−257913（ＪＰ，Ａ) 特開 昭56−142623（ＪＰ，Ａ) 特開 平４−213810（ＪＰ，Ａ) 特開 平４−120234（ＪＰ，Ａ) 特開 昭60−101917（ＪＰ，Ａ) 特公 昭54−2376（ＪＰ，Ｂ１) (58)調査した分野(Int.Cl.7，ＤＢ名) H01G 9/00 - 9/28 C22C 21/00 Continuation of the front page (56) References JP-A-3-257913 (JP, A) JP-A-56-142623 (JP, A) JP-A-4-213810 (JP, A) JP-A-4-120234 (JP) JP-A-60-101917 (JP, A) JP-B-54-2376 (JP, B1) (58) Fields investigated (Int. Cl. 7 , DB name) H01G 9/00-9/28 C22C 21/00
Claims (1)
ｎ、およびＳｎのうちの１種または２種以上からなる第
１拡散成分の含有量が０．２５〜３重量％、同じくＦ
ｅ，Ｎｉ，Ｃｏ，Ｃｒ，Ｍｎ、およびＺｒのうちの１種
または２種以上からなる第２拡散成分の含有量が０．０
０１〜１重量％にして、箔材表面部には、前記最表面部
における第１および第２拡散成分の含有量が表面から
０．５〜２０μｍの範囲内の所定の深さ位置まで減少す
る濃度勾配層を有し、かつ箔材中心部が実質的に純度：
９９．９重量％以上のＡｌからなることを特徴とする表
面積拡大効果のすぐれた電解コンデンサの電極用アルミ
ニウム箔材。1. Pb, Bi, I at the outermost surface of a foil material
n, and the content of the first diffusion component composed of one or more of Sn is 0.25 to 3% by weight.
e, Ni, Co, Cr, Mn, and Zr, when the content of the second diffusion component composed of one or more of them is 0.0
On the other hand, the content of the first and second diffusion components in the outermost surface portion is reduced to a predetermined depth position within a range of 0.5 to 20 μm from the surface at the surface portion of the foil material. Having a concentration gradient layer and a substantially central purity of the foil material:
An aluminum foil material for an electrode of an electrolytic capacitor having an excellent surface area increasing effect, comprising at least 99.9% by weight of Al.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP14145293A JP3293241B2 (en) | 1993-05-20 | 1993-05-20 | Aluminum foil material for electrodes of electrolytic capacitors with excellent surface area expansion effect |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP14145293A JP3293241B2 (en) | 1993-05-20 | 1993-05-20 | Aluminum foil material for electrodes of electrolytic capacitors with excellent surface area expansion effect |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH06333786A JPH06333786A (en) | 1994-12-02 |
| JP3293241B2 true JP3293241B2 (en) | 2002-06-17 |
Family
ID=15292244
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP14145293A Expired - Fee Related JP3293241B2 (en) | 1993-05-20 | 1993-05-20 | Aluminum foil material for electrodes of electrolytic capacitors with excellent surface area expansion effect |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3293241B2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002118035A (en) * | 2000-07-31 | 2002-04-19 | Showa Denko Kk | Electrolytic capacitor electrode aluminum foil |
| US8749954B2 (en) | 2009-10-30 | 2014-06-10 | Panasonic Corporation | Electrode foil and capacitor using same |
-
1993
- 1993-05-20 JP JP14145293A patent/JP3293241B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH06333786A (en) | 1994-12-02 |
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