JP3450083B2 - Aluminum foil for electrode of electrolytic capacitor and method for producing the same - Google Patents
Aluminum foil for electrode of electrolytic capacitor and method for producing the sameInfo
- Publication number
- JP3450083B2 JP3450083B2 JP04487795A JP4487795A JP3450083B2 JP 3450083 B2 JP3450083 B2 JP 3450083B2 JP 04487795 A JP04487795 A JP 04487795A JP 4487795 A JP4487795 A JP 4487795A JP 3450083 B2 JP3450083 B2 JP 3450083B2
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- JP
- Japan
- Prior art keywords
- aluminum foil
- oxide film
- electrolytic capacitor
- thickness
- producing
- 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.)
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Description
【０００１】[0001]
【産業上の利用分野】電解コンデンサ、特に高圧コンデ
ンサの電極に用いられる電解コンデンサ電極用アルミニ
ウム箔およびその製造方法に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an electrolytic capacitor, particularly an aluminum foil for an electrolytic capacitor electrode used as an electrode of a high voltage capacitor, and a method for producing the same.
【０００２】[0002]
【従来の技術】一般に電解コンデンサ電極用アルミニウ
ム箔の製造には、純度９９．９％以上（例えば純度９
９．９６％以上）の純アルミニウムを常法により熱間、
冷間圧延して１００μｍ前後の厚さにし、これを最終焼
鈍した後、表面の粗面化処理、所定の化成処理（陽極酸
化）が行われる。上記した粗面化処理はアルミニウム箔
の表面積の拡大を目的としたものであり、一般に塩酸を
主体とした電解液の中で電気化学的に処理してキャピラ
リー状ピットを形成させる。この１つづつのピットは箔
面に垂直に伸びており、箔の表面積の増大をもたらし、
未処理のものに比べて数十倍の高い静電容量が得られ
る。この粗面化率（表面積拡大率）が大きい程、コンデ
ンサの電極に用いる際に使用する箔の量は少なくて済
み、小型化及び省資源に寄与することができる。このた
め、当業者においては、粗面化率に関連した電解エッチ
ングピットの形成と表面状況の関係について継続した研
究がなされており、粗面化率の高い箔を製造する技術の
開発が進められている。2. Description of the Related Art Generally, in manufacturing aluminum foil for electrolytic capacitor electrodes, a purity of 99.9% or more (for example, a purity of 9% or more) is used.
9.96% or more of pure aluminum is hot
After cold rolling to a thickness of about 100 μm and final annealing, surface roughening treatment and predetermined chemical conversion treatment (anodic oxidation) are performed. The above-described roughening treatment is intended to increase the surface area of the aluminum foil, and is generally electrochemically treated in an electrolytic solution mainly containing hydrochloric acid to form capillary pits. Each of these pits extends perpendicularly to the foil surface, increasing the surface area of the foil,
Capacitance several tens of times higher than that of untreated one can be obtained. The larger the surface roughening rate (surface area expansion rate), the smaller the amount of foil used when used for the electrodes of the capacitor, which can contribute to downsizing and resource saving. For this reason, those skilled in the art have continued research on the relationship between the formation of electrolytic etching pits related to the roughening rate and the surface condition, and the development of a technique for producing a foil with a high roughening rate has been advanced. ing.
【０００３】その中でも特に精力的に行われたきたこと
は最終焼鈍条件の調整である。種々の試みの中から、焼
鈍雰囲気を非酸化性雰囲気（真空またはアルゴン、窒素
等の不活性ガス中）で行うの好ましいことがわかり、現
状では一般的にこの方法が行われている。この場合真空
度では１×１０-2ｐａ以下、また不活性ガス雰囲気とし
ては１ｐｐｍ以下の酸素濃度で行われているのが通常で
ある。このような雰囲気にて焼鈍された箔は、例えば酸
化性雰囲気（１％Ｏ2分圧）で焼鈍された場合に比べ粗
面化率では格段の進歩をしている。上記方法で焼鈍を行
えば酸化皮膜の成長が抑えられ、後の粗面化処理で良好
な粗面化率が得られる。その一方で、酸化皮膜の厚さが
薄すぎると、粗面化処理の際に、全面腐食が生じ、表面
積拡大効果が大幅に低下することも知られている。この
ような観点から、非酸化性雰囲気での焼鈍による酸化皮
膜の厚さは、５０Å程度が望ましいとされている。Among them, what has been done particularly vigorously is the adjustment of the final annealing conditions. From various attempts, it has been found preferable to carry out the annealing atmosphere in a non-oxidizing atmosphere (vacuum or an inert gas such as argon or nitrogen), and at present, this method is generally carried out. In this case, the degree of vacuum is usually 1 × 10 −2 pa or less, and the inert gas atmosphere is usually 1 ppm or less in oxygen concentration. The foil annealed in such an atmosphere has made remarkable progress in the roughening rate as compared with the case of being annealed in an oxidizing atmosphere (1% O 2 partial pressure). If the annealing is performed by the above method, the growth of the oxide film is suppressed, and a good surface roughening rate can be obtained by the subsequent surface roughening treatment. On the other hand, it is also known that if the thickness of the oxide film is too thin, general corrosion will occur during the roughening treatment and the surface area enlarging effect will be greatly reduced. From such a viewpoint, it is said that the thickness of the oxide film formed by annealing in a non-oxidizing atmosphere is preferably about 50Å.
【０００４】[0004]
【発明が解決しようとする問題点】ところで、近年コン
デンサの小型化の要求は益々強くなっており、さらにア
ルミニウム箔の粗面化率を高めることが要望されてい
る。しかし、上記従来技術により製造された製品は、通
常コイルに巻かれた状態で焼鈍されており、そのコイル
の巾方向で粗面化率が異なったり、長さ方向で異なった
りするという問題があり、また特に大きな問題は、コイ
ル全体が、必要な粗面化率に達しないことがしばしば発
生し、十分な静電容量が得られないということである。
本発明は、上記事情を背景としてなされたものであり、
粗面化率が高く、静電容量の大きな電解コンデンサが得
られる電解コンデンサ電極用アルミニウム箔およびその
製造方法を提供するものである。By the way, in recent years, there has been an increasing demand for miniaturization of capacitors, and it has been demanded to further increase the surface roughening rate of aluminum foil. However, the products manufactured by the above-mentioned conventional technique are usually annealed in a state of being wound on a coil, and there is a problem that the surface roughening rate differs in the width direction of the coil or the length direction differs. Also, a particularly big problem is that the entire coil often does not reach the required roughening rate, and sufficient capacitance cannot be obtained.
The present invention has been made in the background of the above circumstances,
The present invention provides an aluminum foil for an electrolytic capacitor electrode, which can obtain an electrolytic capacitor having a high surface roughening rate and a large electrostatic capacity, and a method for producing the same.
【０００５】[0005]
【問題を解決するための手段】上記課題を解決するため
本発明の電解コンデンサ電極用アルミニウム箔は、粗面
化処理前の表面に形成されている酸化皮膜の厚みが３０
〜５０Åであり、かつこの酸化皮膜の結晶化率が１％以
下であることを特徴とする。また、本発明の電解コンデ
ンサ電極用アルミニウム箔の製造方法は、粗面化処理前
に、純アルミニウム箔を還元性ガス雰囲気中で最終焼鈍
することを特徴とする。In order to solve the above problems, in the aluminum foil for electrolytic capacitor electrodes of the present invention, the thickness of the oxide film formed on the surface before roughening treatment is 30.
The crystallization rate of the oxide film is 1% or less. The method for producing an aluminum foil for electrolytic capacitor electrodes of the present invention is characterized in that the pure aluminum foil is finally annealed in a reducing gas atmosphere before the surface roughening treatment.
【０００６】本発明に用いられるアルミニウム箔には純
度９９．９％以上、さらに９９．９６％以上のものが望
ましい。そして、このアルミニウム箔の製造では、鋳
造、圧延は通常のアルミ箔と同様な工程で作ることがで
き、最終厚み（０．１ｍｍ前後）に至るまでの製造方法
は特に限定されるものではない。最終焼鈍では、還元性
ガスとして単独ガスを用いることができるが、混合ガス
を用いることもでき、例えば、２〜１００容量％（さら
には２０容量％以上）の水素ガスと、残部が不活性ガス
からなる混合ガスを用いるのが望ましい。また、その他
の還元性ガスとしては、ＣＯや炭化水素等があり、この
単独ガスまたは混合ガスを用いることができる。上記最
終焼鈍は、５００〜６００℃の温度で、１〜２４時間保
持して行うのが望ましい。The aluminum foil used in the present invention preferably has a purity of 99.9% or more, more preferably 99.96% or more. Then, in the production of this aluminum foil, casting and rolling can be performed in the same steps as those of ordinary aluminum foil, and the production method up to the final thickness (about 0.1 mm) is not particularly limited. In the final annealing, a single gas can be used as the reducing gas, but a mixed gas can also be used. For example, 2 to 100% by volume (further 20% by volume or more) hydrogen gas and the balance inert gas. It is desirable to use a mixed gas consisting of Further, other reducing gases include CO and hydrocarbons, and these single gases or mixed gases can be used. The final annealing is preferably carried out at a temperature of 500 to 600 ° C. for 1 to 24 hours.
【０００７】[0007]
【作用】すなわち、本発明のアルミニウム箔によれば、
適度な厚さを有し、しかも結晶化率を抑えた酸化皮膜を
有しており、粗面化処理に際して高密度で均一なキャピ
ラリー状ピットが形成され、高い粗面化率が得られる。
ここで、表面に形成された酸化皮膜の厚みを、３０〜５
０Å（オンク゛ストローム）としたのは、３０Å未満では粗面化
処理の場合に、全面溶解が起り、キャピラリーピットの
長さが短くなる結果、静電容量が低下するためであり、
また５０Åを越えた場合、耐食性が優れ、結果としてキ
ャピラリー状ピットの発生が少なくなるためであり、高
密度で深いキャピラリー状ピットを形成するため酸化皮
膜の厚みを上記範囲に限定した。このアルミニウム箔は
第２の発明によって得ることができる。In other words, according to the aluminum foil of the present invention,
Since it has an oxide film having an appropriate thickness and a suppressed crystallization rate, high-density and uniform capillary pits are formed during the surface roughening treatment, and a high surface roughening rate is obtained.
Here, the thickness of the oxide film formed on the surface is 30 to 5
The reason for setting 0 Å (angstrom) is that when the surface roughness is less than 30 Å, the entire surface is melted in the case of the roughening treatment and the length of the capillary pit is shortened, resulting in a decrease in capacitance.
Further, when it exceeds 50 Å, the corrosion resistance is excellent, and as a result, the generation of capillary pits is reduced, and the thickness of the oxide film is limited to the above range in order to form high density and deep capillary pits. This aluminum foil can be obtained by the second invention.
【０００８】また、従来のように真空下または不活性ガ
ス雰囲気下で焼鈍をしても、上記と同程度の厚さの酸化
皮膜を得ることは可能である。しかし、この方法で焼鈍
されたアルミニウム箔は、酸化皮膜の結晶化率（酸化皮
膜中の結晶質皮膜の占有割合）が数％であり、粗面化処
理の際に不均一なピットが形成される原因となってい
る。この結晶化率を抑えることによって均一なピットの
形成が可能になる。すなわち、ほぼ完全な非晶質酸化膜
の構造の酸化皮膜は、表面電位は、場所的に均一と考え
られるため、電解条件に対応したエッチングピットが形
成される。さらに結晶化の部分が少ないため、化学腐食
量も少なくなり、孔食性に富み、均一で深いピットが高
密度で形成されることになる。そのためには、結晶化率
を１％以下にする必要があり、さらには０．５％以下に
抑制するのが望ましい。 上記した高密度で均一なピッ
トが形成されることにより、このアルミニウム箔を用い
た電解コンデンサは大きな静電容量を得ることができ
る。Further, even if annealing is performed in a vacuum or in an inert gas atmosphere as in the prior art, it is possible to obtain an oxide film having a thickness similar to the above. However, the aluminum foil annealed by this method has a crystallization rate of the oxide film (occupation ratio of the crystalline film in the oxide film) of several%, and uneven pits are formed during the roughening treatment. Is a cause. By suppressing this crystallization rate, it is possible to form uniform pits. That is, since the surface potential of an oxide film having an almost completely amorphous oxide film structure is considered to be uniform locally, etching pits corresponding to electrolytic conditions are formed. Furthermore, since the crystallized portion is small, the amount of chemical corrosion is small, rich in pitting corrosion, and uniform and deep pits are formed at high density. For that purpose, the crystallization rate needs to be 1% or less, and more preferably 0.5% or less. By forming the high-density and uniform pits, the electrolytic capacitor using this aluminum foil can obtain a large capacitance.
【０００９】また、本発明の製造方法によれば、従来の
ように非酸化性雰囲気で焼鈍する場合に比べて若干、酸
化皮膜の厚みが薄くなり、エッチング性が向上する。従
来法では、酸化皮膜が薄くなると、良好なピットが形成
されないという現象が生じたが、本発明法では、より薄
い皮膜においても良好なピットが形成されている。これ
は本発明法では、酸化皮膜が従来法に比べてより均一な
厚さを有しており、厚さのばらつきが多い従来法に比
べ、より薄い皮膜においても全面腐食が生じにくいため
と考えられる。さらに、非常に重要なことは、通常の非
酸化性雰囲気では酸化皮膜の結晶化が不均一に数％以上
生じる所、本発明の還元性ガス雰囲気焼鈍では、結晶化
率は均一に１％以下に抑えられることである。この結晶
化率によって上記したように、粗面化処理の際には高密
度で均一なピットが形成され、高い粗面化率が得られ
る。Further, according to the manufacturing method of the present invention, the thickness of the oxide film is slightly thinner than that in the conventional case of annealing in a non-oxidizing atmosphere, and the etching property is improved. In the conventional method, the phenomenon that good pits are not formed when the oxide film becomes thin occurs, but in the method of the present invention, good pits are formed even in a thinner film. This is considered to be because in the method of the present invention, the oxide film has a more uniform thickness as compared with the conventional method, and general corrosion is less likely to occur even in a thinner film as compared with the conventional method in which there are many variations in thickness. To be Furthermore, it is very important that the crystallization of the oxide film is unevenly produced by several percent or more in the usual non-oxidizing atmosphere. In the reducing gas atmosphere annealing of the present invention, the crystallization rate is uniformly 1% or less. Is to be suppressed to. As described above, due to this crystallization rate, high density and uniform pits are formed during the surface roughening treatment, and a high surface roughening rate is obtained.
【００１０】焼鈍雰囲気に関しては、例えば、水素ガス
と不活性ガスとの混合ガスを使用する場合、水素ガスを
２容量％以上とするのが望ましく、さらには２０容量％
以上とするのが望ましく、これによりエッチングピット
がより均一、かつ高密度に形成される。また使用するＨ
2ガス、Ａｒガス、Ｎ2ガス等は水分、酸素を極力含んで
いない方がよく、露点−３０℃以下が好ましい。上記し
た還元性ガスは、酸化皮膜を均一に薄くし、結晶化率を
低く抑えるとともに、還元性ガス、例えば水素ガスが酸
化皮膜及びアルミニウムの表面層に導入され、それが、
酸化皮膜の化学的活性化につながり、エッチングピット
の起点が多くなると考えられる。Regarding the annealing atmosphere, for example, when a mixed gas of hydrogen gas and an inert gas is used, it is desirable that the hydrogen gas content be 2% by volume or more, and further 20% by volume.
It is desirable that the above be set, and as a result, etching pits can be formed more uniformly and with high density. Also used H
It is preferable that the 2 gas, Ar gas, N 2 gas, etc. do not contain water and oxygen as much as possible, and the dew point is preferably -30 ° C or lower. The reducing gas described above uniformly thins the oxide film and suppresses the crystallization rate, and a reducing gas, for example, hydrogen gas, is introduced into the oxide film and the surface layer of aluminum, which is
It is thought that this leads to chemical activation of the oxide film and that the starting points of etching pits increase.
【００１１】[0011]
【実施例】以下に、本発明の一実施例を説明する。常法
で作られた純度９９．９９％の純アルミニウムを常法に
より溶解、圧延し、０．１ｍｍ厚のロール上がりの硬質
アルミニウム箔を得た。このアルミニウム箔を５５０℃
×４ｈｒで最終焼鈍するに際し、その雰囲気を発明法で
は還元性雰囲気、比較法では真空雰囲気または中性雰囲
気とし、還元性雰囲気では、水素ガスの導入量を変えて
それぞれ焼鈍を行った。EXAMPLE An example of the present invention will be described below. Pure aluminum having a purity of 99.99% produced by an ordinary method was melted and rolled by an ordinary method to obtain a rolled-up hard aluminum foil having a thickness of 0.1 mm. 550 ℃ this aluminum foil
At the time of final annealing at × 4 hr, the atmosphere was a reducing atmosphere in the invention method, a vacuum atmosphere or a neutral atmosphere in the comparative method, and annealing was performed in the reducing atmosphere while changing the introduction amount of hydrogen gas.
【００１２】得られたアルミニウム箔には、引き続き、
以下の条件で粗面化処理および化成処理を行った後、静
電容量を測定した。
１．粗面化処理条件
（１）第１段エッチング条件（電解エッチング）
電解液 温度 電流密度 時間
HCl 1モル/l
H2SO4 3モル/l ７５℃ ０．８Ａ／ｃｍ2 ４０秒
AlCl3,6H2O 60g/l
（２）第２段エッチング条件（化学エッチング）
Ｈ2Ｏ：ＨＮＯ3（1:1） ７５℃ ３００秒
２．化成条件（２７０Ｖ） 温度 電流密度 到達電圧
硼酸 １００ｇ／ｌ ８５℃ ０．１Ａ／ｃｍ2 ２７０Ｖ
硼酸アンモン １ｇ／ｌThe obtained aluminum foil was continuously
After performing the roughening treatment and the chemical conversion treatment under the following conditions, the capacitance was measured. 1. Roughening treatment condition (1) the first step etching conditions (electrolytic etching) electrolyte temperature current density time HCl 1 mol / l H 2 SO 4 3 mol / l 75 ℃ 0.8A / cm 2 40 sec AlCl 3, 6H 2 O 60g / l (2) Second stage etching conditions (chemical etching) H 2 O: HNO 3 (1: 1) 75 ° C 300 seconds 2. Chemical conversion conditions (270 V) Temperature Current density Ultimate voltage Boric acid 100 g / l 85 ° C. 0.1 A / cm 2 270 V Ammonium borate 1 g / l
【００１３】さらに、得られた試料について、ブロム−
メタノール液でＡｌを溶かし、シャーレ上に浮上した酸
化皮膜を透過型電子顕微鏡で観察し、暗視野像の撮影を
行って結晶化の面積率を計算した。また、島津製作所の
光電子分光装置（ＥＳＣＡ）を用い、次式により酸化皮
膜厚を測定した。
酸化皮膜厚み（Å）＝２３．７ｌｎ（１÷ＩＭ／ＩＴ）
ＩＭ：金属Ａｌのピークの積分強度
ＩＴ：金属、及酸化Ａｌのピークの積分強度
上記した、各測定結果は表１にまとめて示した。Further, regarding the obtained sample, bromine-
Al was dissolved in a methanol solution, and the oxide film floating on the petri dish was observed with a transmission electron microscope, and a dark field image was taken to calculate the area ratio of crystallization. Further, the oxide film thickness was measured by the following equation using a photoelectron spectrometer (ESCA) manufactured by Shimadzu Corporation. Oxide film thickness (Å) = 23.7 ln (1 ÷ IM / IT) IM: integrated intensity of peak of metal Al IT: integrated intensity of peak of metal and oxidized Al The above measurement results are summarized in Table 1. Indicated.
【００１４】[0014]
【表１】 [Table 1]
【００１５】表から明らかなように、本発明法によって
最終焼鈍したアルミニウム箔（発明材）は、適度な厚さ
を有し、かつ低い結晶化率を示しており、測定された静
電容量も優れた値を示していた。これに対し、比較法に
より得られたアルミニウム箔（比較材）は、結晶化率が
高く、静電容量は発明材に比べて劣っていた。As is apparent from the table, the aluminum foil (invention material) finally annealed by the method of the present invention has an appropriate thickness and exhibits a low crystallization rate, and the measured capacitance is also It showed an excellent value. On the other hand, the aluminum foil (comparative material) obtained by the comparison method had a high crystallization rate and was inferior in electrostatic capacity to the invention material.
【００１６】[0016]
【発明の効果】以上説明したように、本発明の電解コン
デンサ電極用アルミニウム箔によれば、粗面化処理前の
表面に形成されている酸化皮膜の厚みが３０〜５０Åで
あり、かつ酸化皮膜の結晶化率が１％以下であるので、
粗面化処理の際に高い粗面化率でピットが均一高密度に
形成され、大きな静電容量の電解コンデンサを得ること
ができる。As described above, according to the aluminum foil for electrolytic capacitor electrodes of the present invention, the thickness of the oxide film formed on the surface before the roughening treatment is 30 to 50Å, and the oxide film is also formed. Since the crystallization rate of is less than 1%,
During the surface roughening treatment, pits are uniformly formed with a high surface roughening rate and a high electrostatic capacitance can be obtained.
【００１７】また本発明の電解コンデンサ電極用アルミ
ニウム箔の製造方法によれば、粗面化処理前に、純アル
ミニウム箔を還元性ガス雰囲気中で最終焼鈍するので、
結晶化率が低く、均一な厚さの薄膜酸化皮膜が得られ、
上記のように大きな静電容量の電解コンデンサが得られ
る。According to the method for producing an aluminum foil for electrolytic capacitor electrodes of the present invention, since the pure aluminum foil is finally annealed in a reducing gas atmosphere before the surface roughening treatment,
The crystallization rate is low and a thin oxide film with a uniform thickness can be obtained.
As described above, an electrolytic capacitor having a large capacitance can be obtained.
───────────────────────────────────────────────────── フロントページの続き (58)調査した分野(Int.Cl.7，ＤＢ名) H01G 9/04 304 H01G 9/055 C22F 1/04 ─────────────────────────────────────────────────── ─── Continuation of the front page (58) Fields surveyed (Int.Cl. 7 , DB name) H01G 9/04 304 H01G 9/055 C22F 1/04
Claims (2)
化皮膜の厚みが３０〜５０Åであり、かつ、この酸化皮
膜の結晶化率が１％以下であることを特徴とする電解コ
ンデンサ電極用アルミニウム箔1. An electrolytic capacitor, wherein an oxide film formed on the surface before roughening treatment has a thickness of 30 to 50 Å, and a crystallization rate of the oxide film is 1% or less. Aluminum foil for electrodes
元性ガス雰囲気中で最終焼鈍することを特徴とする電解
コンデンサ電極用アルミニウム箔の製造方法2. A method for producing an aluminum foil for an electrolytic capacitor electrode, which comprises subjecting a pure aluminum foil to final annealing in a reducing gas atmosphere before roughening treatment.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP04487795A JP3450083B2 (en) | 1995-02-09 | 1995-02-09 | Aluminum foil for electrode of electrolytic capacitor and method for producing the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP04487795A JP3450083B2 (en) | 1995-02-09 | 1995-02-09 | Aluminum foil for electrode of electrolytic capacitor and method for producing the same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH08222488A JPH08222488A (en) | 1996-08-30 |
| JP3450083B2 true JP3450083B2 (en) | 2003-09-22 |
Family
ID=12703730
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP04487795A Expired - Lifetime JP3450083B2 (en) | 1995-02-09 | 1995-02-09 | Aluminum foil for electrode of electrolytic capacitor and method for producing the same |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3450083B2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4493721B2 (en) * | 2009-02-03 | 2010-06-30 | 昭和電工株式会社 | Aluminum material for electrolytic capacitor electrode and electrolytic capacitor |
| CN104711663B (en) * | 2013-12-15 | 2017-05-31 | 江苏荣生电子有限公司 | It is a kind of to use seven grades of middle-high voltage electrode foil manufacture methods of different hair engaging aperture conditions |
-
1995
- 1995-02-09 JP JP04487795A patent/JP3450083B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH08222488A (en) | 1996-08-30 |
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