JP2001172754A - Method of manufacturing for high purity aluminum foil for electrolytic capacitor - Google Patents
Method of manufacturing for high purity aluminum foil for electrolytic capacitorInfo
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- JP2001172754A JP2001172754A JP35406199A JP35406199A JP2001172754A JP 2001172754 A JP2001172754 A JP 2001172754A JP 35406199 A JP35406199 A JP 35406199A JP 35406199 A JP35406199 A JP 35406199A JP 2001172754 A JP2001172754 A JP 2001172754A
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- Prior art keywords
- aluminum foil
- cold
- electrolytic capacitor
- hot
- thickness
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Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、静電容量の高い電
解コンデンサ用電極箔を得ることのできる電解コンデン
サ用高純度アルミニウム箔の製造方法に関する。特に、
直流エッチング法で静電容量の高い電解コンデンサ高圧
用陽極箔を得ることのできる電解コンデンサ用高純度ア
ルミニウム箔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 a method for producing a high-purity aluminum foil for an electrolytic capacitor capable of obtaining an electrode foil for an electrolytic capacitor having a high capacitance. In particular,
The present invention relates to a method for producing a high-purity aluminum foil for an electrolytic capacitor, which can obtain a high-capacity anode foil for an electrolytic capacitor having a high capacitance by a DC etching method.
【０００２】[0002]
【従来の技術】従来より、電解コンデンサ用電極箔を製
造するためには、電解コンデンサ用アルミニウム箔にエ
ッチング処理を施し、箔表面に微細な孔を多数形成し
て、箔表面の表面積を拡大することが行なわれている。
特に、電解コンデンサ高圧用陽極箔を製造するには、電
解コンデンサ用高純度アルミニウム箔に直流エッチング
処理を施し、箔表面に多数の厚み方向に進行する微細な
孔（いわゆるトンネルピット）を形成して、箔表面の表
面積を拡大することが行なわれている。この表面積の拡
大は、電解コンデンサ高圧用陽極箔の静電容量を高める
ためには、最も有効な方法である。2. Description of the Related Art Conventionally, in order to manufacture an electrode foil for an electrolytic capacitor, an aluminum foil for an electrolytic capacitor is subjected to an etching treatment to form a large number of fine holes in the foil surface, thereby increasing the surface area of the foil surface. Things are going on.
In particular, in order to manufacture an anode foil for an electrolytic capacitor high voltage, a high-purity aluminum foil for an electrolytic capacitor is subjected to a DC etching treatment to form a number of fine holes (so-called tunnel pits) which progress in the thickness direction on the foil surface. It has been practiced to increase the surface area of the foil surface. This increase in surface area is the most effective method for increasing the capacitance of the anode foil for electrolytic capacitor high voltage.
【０００３】このようなトンネルピットは、電解コンデ
ンサ用高純度アルミニウム箔表面に生成している（１０
０）方位を持つ結晶粒を核として形成される。従って、
アルミニウム箔表面に高密度で多数の（１００）方位を
持つ結晶粒が生成しているほど、エッチングによる表面
積の拡大が図れるのである。なお、（１００）方位を持
つ結晶粒は、アルミニウム箔表面から裏面に貫通した状
態で存在する場合が多く、エッチング処理が施される
と、アルミニウム箔表面の（１００）方位を持つ結晶粒
の部位を核として、トンネルピットが形成されるのであ
る。[0003] Such tunnel pits are formed on the surface of a high-purity aluminum foil for electrolytic capacitors (10).
0) Crystals having orientations are formed as nuclei. Therefore,
The higher the density of crystal grains having a large number of (100) orientations on the surface of the aluminum foil, the greater the surface area can be increased by etching. The crystal grains having the (100) orientation are often present in a state penetrating from the front surface to the rear surface of the aluminum foil. Tunnel pits are formed around the nucleus.
【０００４】このため、従来より、アルミニウム箔に高
密度で多数の（１００）方位を持つ結晶粒を生成させる
方法として、以下のような方法が提案されている。即
ち、アルミニウム鋳塊に均質化処理及び熱間圧延を施し
た後、高冷間加工率で冷間圧延し、中間焼鈍を施した後
に、低冷間加工率の仕上冷間圧延を施し、そのあと最終
焼鈍を施して、電解コンデンサ用高純度アルミニウム箔
を得る方法が提案されている。この方法は、高冷間加工
率での冷間圧延後の中間焼鈍で、（１００）方位を持つ
結晶粒の核を生成させ、低冷間加工率での仕上冷間圧延
により、核成長の駆動力を大きくすれば、最終焼鈍によ
り、アルミニウム箔に多数の（１００）方位を持つ結集
粒を生成させうるとの知見に基づくものである。[0004] For this reason, the following methods have been conventionally proposed as a method for generating crystal grains having a large number of (100) orientations in an aluminum foil at high density. That is, after subjecting the aluminum ingot to homogenization and hot rolling, cold-rolling at a high cold-working rate, and performing intermediate annealing, then performing finish cold-rolling at a low cold-working rate. A method has been proposed in which a final annealing is performed to obtain a high-purity aluminum foil for an electrolytic capacitor. According to this method, nuclei of crystal grains having a (100) orientation are generated by intermediate annealing after cold rolling at a high cold working rate, and finish cold rolling at a low cold working rate is used to grow nuclei. It is based on the finding that if the driving force is increased, agglomerated grains having a large number of (100) orientations can be generated in the aluminum foil by final annealing.
【０００５】具体的には種々の方法が開示されており、
例えば、特公平１−３３５４６号公報には、以下のよう
な方法が開示されている。即ち、厚さ４００ｍｍのアル
ミニウム鋳塊に、均質化処理を施し、次いで熱間圧延を
施して厚さ５ｍｍ（熱間加工率９８．８％）の熱間圧延
上がり板を得る。この熱間圧延上がり板を冷間圧延によ
り０．１４０ｍｍ（冷間加工率９７．２％）とした後、
２５０℃×１０時間の条件で中間焼鈍を施す。この後、
仕上冷間圧延を施して、厚さ０．１ｍｍ（冷間加工率２
８．６％）にした後、６００℃×４時間の条件で最終焼
鈍を施して、電解コンデンサ用高純度アルミニウム箔を
得る方法が開示されている。また、特公昭５４−１１２
４２号公報には、高冷間加工率で冷間圧延を終えた冷間
圧延材に、１８０〜３５０℃の温度で中間焼鈍を施した
後、冷間加工率５〜３５％の仕上冷間圧延を行い、３０
０〜６５０℃の温度で最終焼鈍を行う方法が開示されて
いる。Specifically, various methods have been disclosed.
For example, Japanese Patent Publication No. 33546/1990 discloses the following method. That is, a 400 mm-thick aluminum ingot is subjected to a homogenization treatment and then hot-rolled to obtain a hot-rolled finished plate having a thickness of 5 mm (hot-working rate of 98.8%). After the hot-rolled sheet is cold-rolled to 0.140 mm (cold working rate of 97.2%),
Intermediate annealing is performed at 250 ° C. × 10 hours. After this,
Finish cold rolling is performed to a thickness of 0.1 mm (cold working rate of 2
8.6%), followed by final annealing at 600 ° C. for 4 hours to obtain a high-purity aluminum foil for electrolytic capacitors. Also, Japanese Patent Publication No. 54-112
No. 42 discloses that a cold-rolled material that has been cold-rolled at a high cold-working rate is subjected to intermediate annealing at a temperature of 180 to 350 ° C., and then to a finish cold-working rate of 5 to 35%. Rolling, 30
A method for performing final annealing at a temperature of 0 to 650 ° C is disclosed.
【０００６】[0006]
【発明が解決しようとする課題】ところが、本発明者等
が種々実験を行なっていたところ、このような技術的常
識を覆す結果を得た。即ち、必ずしも冷間加工率が高く
なくても、熱間圧延における熱間加工率がある程度高け
れば、アルミニウム箔に多数の（１００）方位を持つ結
晶粒を十分に生成させうることが判明した。本発明者等
は、この知見に基づき、既に特願平１０−３６８７９１
号に係る発明を提案している。この発明は、純度９９．
９７％以上のアルミニウム鋳塊に、熱間加工率９９．３
〜９９．８％の条件で熱間圧延を施した後、冷間圧延，
中間焼鈍，仕上冷間圧延及び最終焼鈍を施すことを特徴
とする電解コンデンサ用高純度アルミニウム箔の製造方
法というものである。However, the inventors of the present invention have conducted various experiments, and have obtained a result that overturns such technical common sense. That is, it has been found that even if the cold working ratio is not necessarily high, if the hot working ratio in hot rolling is high to some extent, it is possible to sufficiently generate crystal grains having a large number of (100) orientations in the aluminum foil. Based on this finding, the present inventors have already filed Japanese Patent Application No. 10-368791.
The invention according to the above item is proposed. The present invention provides a purity of 99.
99.3% or more of aluminum ingot, hot working ratio 99.3
After performing hot rolling under the condition of ９９99.8%,
A method for producing a high-purity aluminum foil for an electrolytic capacitor, which comprises performing intermediate annealing, finish cold rolling, and final annealing.
【０００７】本発明者等は、上記した知見に基づき更に
研究を進めた結果、熱間圧延における熱間加工率及び冷
間圧延における冷間加工率の両者を一定の範囲内に調整
すると、中間焼鈍及びそれに続く仕上冷間圧延を施さな
くても、アルミニウム箔に多数の（１００）方位を持つ
結晶粒を十分に生成させうることが判明した。本発明
は、このような知見に基づいてなされたものであり、特
願平１０−３６８７９１号に係る発明で得られるアルミ
ニウム箔と同等のものを、他の方法で得られるようにし
たものである。As a result of further studies based on the above findings, the present inventors have found that when both the hot working ratio in hot rolling and the cold working ratio in cold rolling are adjusted within a certain range, the intermediate It has been found that the crystal grains having a large number of (100) orientations can be sufficiently generated in the aluminum foil without performing the annealing and the subsequent finish cold rolling. The present invention has been made based on such knowledge, and is intended to obtain, by another method, an aluminum foil equivalent to the aluminum foil obtained by the invention according to Japanese Patent Application No. 10-368791. .
【０００８】[0008]
【課題を解決するための手段】即ち、本発明は、純度９
９．９７％以上のアルミニウム鋳塊に、均質化処理を施
した後、熱間加工率９９．２〜９９．８％の条件で熱間
圧延を施し、その後、冷間圧延途中に中間焼鈍を施すこ
となく、冷間加工率７５．０〜９７．０％の条件で冷間
圧延を施し、次いで最終焼鈍を施すことを特徴とする電
解コンデンサ用高純度アルミニウム箔の製造方法に関す
るものである。That is, the present invention provides a compound having a purity of 9%.
After applying a homogenization treatment to an aluminum ingot of 9.97% or more, hot rolling is performed under the conditions of a hot working rate of 99.2 to 99.8%, and then intermediate annealing is performed during cold rolling. The present invention relates to a method for producing a high-purity aluminum foil for an electrolytic capacitor, which comprises performing cold rolling under the condition of a cold working ratio of 75.0 to 97.0% without performing the same and then performing final annealing.
【０００９】まず、本発明で用いるアルミニウム鋳塊
は、純度が９９．９７％以上のものである。純度が９
９．９７％未満であると、本発明の方法を適用しても、
（１００）方位を持つ結晶粒を十分に生成させうること
が困難となる。また、本発明で用いるアルミニウム鋳塊
には、従来、電解コンデンサ用アルミニウム箔を製造す
る際に添加されているＦｅ，Ｓｉ，Ｃｕ等の元素が任意
量添加されていても良い。なお、（１００）方位を持つ
結晶粒の生成が十分であるか否かの判断基準は、一応、
アルミニウム箔表面において（１００）方位を持つ結晶
粒の占める面積割合（以下、「（１００）面占有率」と
言う。）が９０％以上であるか否かを目安としている
が、９５％以上であれば（１００）方位を持つ結晶粒の
生成が十分であると言える。First, the aluminum ingot used in the present invention has a purity of 99.97% or more. Purity 9
When it is less than 9.97%, even if the method of the present invention is applied,
It is difficult to sufficiently generate crystal grains having the (100) orientation. Further, the aluminum ingot used in the present invention may be added with an arbitrary amount of elements such as Fe, Si, and Cu which have been conventionally added when manufacturing an aluminum foil for an electrolytic capacitor. The criterion for determining whether the generation of crystal grains having the (100) orientation is sufficient is as follows.
It is based on whether or not the area ratio of crystal grains having the (100) orientation on the aluminum foil surface (hereinafter, referred to as “(100) plane occupancy”) is 90% or more. If so, it can be said that the generation of crystal grains having the (100) orientation is sufficient.
【００１０】アルミニウム鋳塊の厚さは任意であるが、
一般的に４００〜６００ｍｍの範囲である。これは、市
場に提供されるアルミニウム鋳塊の厚さが、この範囲の
ものが多いからである。Although the thickness of the aluminum ingot is arbitrary,
Generally, it is in the range of 400 to 600 mm. This is because the thickness of the aluminum ingot provided on the market is often in this range.
【００１１】このアルミニウム鋳塊には、従来公知の温
度条件及び時間で均質化処理が施され、続いて、従来公
知の温度条件で熱間圧延が施される。ただ、本発明にお
いては、この熱間圧延における熱間加工率を、従来公知
の条件よりも高くしているところに特徴がある。即ち、
従来公知の熱間加工率は、概ね９８％前後であったの
を、本発明においては、９９．２〜９９．８％にすると
ころに特徴がある。熱間加工率が９９．２％未満になる
と、得られるアルミニウム箔表面の（１００）面占有率
が低下する。また、熱間加工率が９９．８％を超えるよ
うにすることは、熱間圧延設備を極めて大きな馬力で作
動させなければならず、現実的ではない。なお、熱間加
工率とは、熱間圧延を行なう前のアルミニウム鋳塊の厚
さをｔ0とし、熱間圧延を終えた熱間圧延上がり板の厚
さをｔ1とした場合、〔（ｔ0−ｔ1）／ｔ0〕×１００で
算出されるものである。The aluminum ingot is subjected to a homogenizing treatment under a conventionally known temperature condition and time, and then subjected to hot rolling under a conventionally known temperature condition. However, the present invention is characterized in that the hot working ratio in the hot rolling is set higher than conventionally known conditions. That is,
In the present invention, the conventionally known hot working ratio is about 98%, but the present invention is characterized in that it is 99.2 to 99.8%. If the hot working ratio is less than 99.2%, the (100) plane occupation ratio of the obtained aluminum foil surface decreases. Further, making the hot working ratio exceed 99.8% is not realistic because the hot rolling equipment must be operated with extremely large horsepower. In the case with the hot processing rate, the thickness of the aluminum ingot prior to the hot rolling and t 0, the thickness of the hot-rolled sheet having been subjected to the hot rolling was set to t 1, [( t 0 −t 1 ) / t 0 ] × 100.
【００１２】一般の４００〜６００ｍｍ厚さのアルミニ
ウム鋳塊を用いた場合、熱間圧延によって、厚さ１．３
〜３．０ｍｍの熱間圧延上がり板を得るのが好ましい。
熱間圧延上がり板の厚さが３．０ｍｍを超えると、得ら
れるアルミニウム箔表面の（１００）面占有率が低下す
る傾向が生じる。また、熱間圧延上がり板の厚さを１．
３ｍｍ未満にすることは、現状の熱間圧延設備では現実
的ではない。When a general aluminum ingot having a thickness of 400 to 600 mm is used, a thickness of 1.3 is obtained by hot rolling.
It is preferable to obtain a hot-rolled finished plate of up to 3.0 mm.
When the thickness of the hot-rolled sheet exceeds 3.0 mm, the occupancy of the (100) plane of the surface of the obtained aluminum foil tends to decrease. Further, the thickness of the hot-rolled finished plate is set to 1.
Making it less than 3 mm is not realistic with current hot rolling equipment.
【００１３】熱間圧延を終えた熱間圧延上がり板には、
冷間圧延が施される。この冷間圧延における冷間加工率
は、７５．０〜９７．０％とする。冷間加工率が９７．
０％を超えると、熱間圧延時に生成した（１００）方位
を持つ結晶粒の核が崩れて、（１００）面占有率が低下
する。また、冷間加工率を７５．０％未満とすると、一
般に市場に提供されている電解コンデンサ用電極箔の厚
さとならないので、現実的ではない。具体的には、熱間
圧延上がり板の厚さを１．３〜３．０ｍｍとした場合、
これに冷間圧延を施して、厚さ０．０９〜０．３０ｍｍ
の冷間圧延上がりアルミニウム箔を得るのが好ましい。
なお、冷間圧延における冷間加工率とは、冷間圧延が施
される前の熱間圧延上がり板の厚さをｔ1とし、冷間圧
延上がりアルミニウム箔の厚さをｔ2とした場合、
〔（ｔ1−ｔ2）／ｔ1〕×１００で算出されるものであ
る。また、本発明の範囲外ではあるが、将来、熱間圧延
設備の改良によって、熱間圧延上がり板の厚さを１．３
ｍｍ未満の厚さとすることができれば、冷間加工率を７
５．０％未満、例えば１０％前後にすることも可能と考
えられる。何故なら、冷間加工率は、熱間圧延時に生成
した（１００）方位を持つ結晶粒の核に駆動力を与え、
成長させることのできる程度であれば良いからである。[0013] The hot-rolled finished plate after hot rolling is:
Cold rolling is performed. The cold working rate in this cold rolling is 75.0 to 97.0%. Cold working rate is 97.
If it exceeds 0%, the nuclei of the crystal grains having the (100) orientation generated during hot rolling collapse, and the (100) plane occupancy decreases. On the other hand, if the cold working ratio is less than 75.0%, the thickness of the electrode foil for an electrolytic capacitor generally provided on the market does not become the thickness, which is not practical. Specifically, when the thickness of the hot-rolled finished sheet is set to 1.3 to 3.0 mm,
This is subjected to cold rolling to a thickness of 0.09 to 0.30 mm
It is preferable to obtain an aluminum foil after cold rolling.
Note that the cold working ratio in the cold rolling, the thickness of the hot-rolled plate before the cold rolling is performed as t 1, when the thickness of the cold-rolled aluminum foil was t 2 ,
It is calculated by [(t 1 −t 2 ) / t 1 ] × 100. Further, although it is outside the scope of the present invention, in the future, the thickness of the hot-rolled finished sheet will be reduced to 1.3 by improving hot rolling equipment.
If the thickness can be reduced to less than 7 mm, the cold working rate can be reduced to 7
It is thought that it can be less than 5.0%, for example, around 10%. This is because the cold working rate gives a driving force to the nuclei of the (100) crystal grains generated during hot rolling,
This is because it is only necessary to be able to grow.
【００１４】冷間圧延の後、中間焼鈍及びそれに続く仕
上冷間圧延を施すことなく、冷間圧延上がりアルミニウ
ム箔に最終焼鈍が施される。最終焼鈍の温度条件は、従
来採用されている条件で良い。具体的には、５３０〜５
８０℃であるのが好ましい。また、最終焼鈍の時間も、
従来採用されている時間で良く、具体的には３〜１０時
間程度である。この最終焼鈍によって、（１００）方位
を持つ結晶粒がアルミニウム箔に高密度に生成するので
ある。After cold rolling, final annealing is performed on the cold-rolled aluminum foil without performing intermediate annealing and subsequent finish cold rolling. The temperature conditions for the final annealing may be those conventionally employed. Specifically, 530-5
Preferably it is 80 ° C. Also, the time of final annealing,
The time conventionally used may be sufficient, and specifically, about 3 to 10 hours. By this final annealing, crystal grains having the (100) orientation are formed at a high density in the aluminum foil.
【００１５】更に、最終焼鈍の昇温速度を５０〜５００
℃／ｈとするのが好ましい。最終焼鈍時に、この範囲内
の昇温速度を採用すると、得られる電解コンデンサ用高
純度アルミニウム箔表面の（１００）面占有率をより高
めることができ、例えば、９７．０％以上にしやすくな
る。昇温速度が５０℃／ｈ未満であると、（１００）面
占有率が若干低下し、９５．０〜９７．０％程度になり
やすい。また、昇温速度が５００℃／ｈを超えると、
（１００）方位以外の異方位を持つ粗大な結晶粒が成長
する恐れがあり、（１００）面占有率が低下する傾向が
生じる。Further, the rate of temperature rise in the final annealing is 50 to 500.
C / h is preferred. At the time of the final annealing, if the heating rate within this range is adopted, the (100) plane occupancy of the surface of the high-purity aluminum foil for an electrolytic capacitor to be obtained can be further increased, for example, to 97.0% or more. If the rate of temperature rise is less than 50 ° C./h, the (100) plane occupancy slightly decreases and tends to be about 95.0 to 97.0%. Also, if the heating rate exceeds 500 ° C./h,
Coarse crystal grains having a different orientation other than the (100) orientation may grow, and the (100) plane occupancy tends to decrease.
【００１６】以上のようにして得られた、電解コンデン
サ用高純度アルミニウム箔には、従来公知のエッチング
処理が施され、電解コンデンサ用電極箔として用いられ
る。特に、直流エッチング処理を施し、電解コンデンサ
高圧用陽極箔として好適に用いられる。なお、最終的に
得られる電解コンデンサ用高純度アルミニウム箔の厚さ
は、一般的に、９０〜３００μｍ程度である。The high-purity aluminum foil for an electrolytic capacitor obtained as described above is subjected to a conventionally known etching treatment and used as an electrode foil for an electrolytic capacitor. In particular, it is subjected to a DC etching treatment, and is suitably used as an anode foil for a high voltage electrolytic capacitor. In addition, the thickness of the high-purity aluminum foil for an electrolytic capacitor finally obtained is generally about 90 to 300 μm.
【００１７】[0017]
【実施例】以下、実施例に基づいて本発明を説明する
が、本発明は実施例に限定されるものではない。本発明
は、熱間圧延における熱間加工率及び冷間圧延における
冷間加工率の両者を一定の範囲内に調整すると、従来の
技術的常識に反して、中間焼鈍及びそれに続く仕上冷間
圧延を施さなくても、（１００）面占有率の高いアルミ
ニウム箔が得られるとの知見に基づいてなされたもので
あるとして、解釈されるべきである。Hereinafter, the present invention will be described based on examples, but the present invention is not limited to the examples. When the present invention adjusts both the hot working ratio in the hot rolling and the cold working ratio in the cold rolling within a certain range, contrary to the conventional technical knowledge, the intermediate annealing and the subsequent finish cold rolling Should be interpreted as having been made based on the finding that an aluminum foil having a high (100) plane occupancy ratio can be obtained without performing the above.
【００１８】実施例１ Ｆｅ：１０ｐｐｍ，Ｓｉ：１２ｐｐｍ，Ｃｕ：５０ｐｐ
ｍ，Ｐｂ：０．５ｐｐｍ及びその他の不可避不純物を含
む９９．９９％純度のアルミニウム鋳塊（厚さ５００ｍ
ｍ，巾１０５０ｍｍ，長さ３０００ｍｍ）に、６００℃
にて５時間の均質化処理を施した後、熱間圧延を繰り返
し施して、熱間加工率が９９．６％となるようにし、厚
さ２．０ｍｍの熱間圧延上がり板を得た。この熱間圧延
上がり板に、冷間圧延を繰り返し施して、冷間加工率が
９４．７％となるようにし、厚さ０．１０６ｍｍの冷間
圧延上がりアルミニウム箔を得た。その後、この冷間圧
延上がりアルミニウム箔に、昇温速度を１００℃／ｈと
し、温度５５０℃で５時間の条件で最終焼鈍を施し、電
解コンデンサ用高純度アルミニウム箔を得た。Example 1 Fe: 10 ppm, Si: 12 ppm, Cu: 50 pp
m, Pb: 99.99% pure aluminum ingot containing 0.5 ppm and other unavoidable impurities (thickness: 500 m
m, width 1050mm, length 3000mm) and 600 ℃
After performing a homogenization treatment for 5 hours, hot rolling was repeatedly performed so that the hot working ratio was 99.6%, and a hot-rolled finished plate having a thickness of 2.0 mm was obtained. The hot-rolled finished sheet was repeatedly subjected to cold rolling so that the cold-working rate became 94.7%, and a cold-rolled aluminum foil having a thickness of 0.106 mm was obtained. Thereafter, the cold-rolled aluminum foil was subjected to final annealing at a temperature rising rate of 100 ° C./h at a temperature of 550 ° C. for 5 hours to obtain a high-purity aluminum foil for an electrolytic capacitor.
【００１９】この電解コンデンサ用高純度アルミニウム
箔表面の（１００）面占有率を測定するために、箔表面
を化学エッチングして結晶粒を現出させ、顕微鏡写真を
撮影した。この顕微鏡写真に基づいて、一定面積に占め
る（１００）方位を持つ結晶粒の面積を測定することに
よって、アルミニウム箔表面の（１００）面占有率を求
め、その結果を表１に示した。In order to measure the (100) plane occupancy of the surface of the high-purity aluminum foil for an electrolytic capacitor, the foil surface was chemically etched to reveal crystal grains, and a micrograph was taken. Based on this micrograph, the area of the crystal grains having the (100) orientation occupying a certain area was measured to determine the (100) plane occupancy of the aluminum foil surface, and the results are shown in Table 1.
【００２０】実施例２ 熱間圧延上がり板の厚さを３．０ｍｍとし、冷間圧延上
がりアルミニウム箔の厚さを０．３０ｍｍとする他は、
実施例１と同様の方法により、電解コンデンサ用高純度
アルミニウム箔を得た。Example 2 Except that the thickness of the hot-rolled sheet was 3.0 mm and the thickness of the cold-rolled aluminum foil was 0.30 mm,
A high-purity aluminum foil for an electrolytic capacitor was obtained in the same manner as in Example 1.
【００２１】実施例３ 冷間圧延上がりアルミニウム箔の厚さを０．０９ｍｍと
する他は、実施例２と同様の方法により、電解コンデン
サ用高純度アルミニウム箔を得た。Example 3 A high-purity aluminum foil for an electrolytic capacitor was obtained in the same manner as in Example 2 except that the thickness of the cold-rolled aluminum foil was changed to 0.09 mm.
【００２２】実施例４ 熱間圧延上がり板の厚さを１．３ｍｍとする他は、実施
例２と同様の方法により、電解コンデンサ用高純度アル
ミニウム箔を得た。Example 4 A high-purity aluminum foil for an electrolytic capacitor was obtained in the same manner as in Example 2 except that the thickness of the hot-rolled finished plate was 1.3 mm.
【００２３】実施例５ 冷間圧延上がりアルミニウム箔の厚さを０．０９ｍｍと
する他は、実施例４と同様の方法により、電解コンデン
サ用高純度アルミニウム箔を得た。Example 5 A high-purity aluminum foil for an electrolytic capacitor was obtained in the same manner as in Example 4, except that the thickness of the cold-rolled aluminum foil was 0.09 mm.
【００２４】実施例６ 最終焼鈍の昇温速度を５０℃／ｈとする他は、実施例１
と同様の方法により、電解コンデンサ用高純度アルミニ
ウム箔を得た。Example 6 Example 1 was repeated except that the heating rate of the final annealing was set to 50 ° C./h.
A high-purity aluminum foil for electrolytic capacitors was obtained in the same manner as described above.
【００２５】実施例７ 最終焼鈍の昇温速度を５００℃／ｈとする他は、実施例
１と同様の方法により、電解コンデンサ用高純度アルミ
ニウム箔を得た。Example 7 A high-purity aluminum foil for an electrolytic capacitor was obtained in the same manner as in Example 1, except that the rate of temperature rise in the final annealing was 500 ° C./h.
【００２６】実施例８ 最終焼鈍の昇温速度を２０℃／ｈとする他は、実施例１
と同様の方法により、電解コンデンサ用高純度アルミニ
ウム箔を得た。Example 8 Example 1 was repeated except that the heating rate of the final annealing was set at 20 ° C./h.
A high-purity aluminum foil for electrolytic capacitors was obtained in the same manner as described above.
【００２７】実施例９ 鋳塊厚さを６００ｍｍ、熱間圧延上がり板の厚さを３．
０ｍｍ、冷間圧延上がりアルミニウム箔の厚さを０．１
０６ｍｍとする他は、実施例１と同様の方法により、電
解コンデンサ用高純度アルミニウム箔を得た。Example 9 The thickness of the ingot was 600 mm, and the thickness of the hot-rolled sheet was 3.
0 mm, cold-rolled aluminum foil thickness of 0.1
A high-purity aluminum foil for an electrolytic capacitor was obtained in the same manner as in Example 1 except that the thickness was set to 06 mm.
【００２８】実施例１０ 鋳塊厚さを４００ｍｍ、熱間圧延上がり板の厚さを３．
０ｍｍ、冷間圧延上がりアルミニウム箔の厚さを０．１
０６ｍｍとする他は、実施例１と同様の方法により、電
解コンデンサ用高純度アルミニウム箔を得た。Example 10 The thickness of the ingot was 400 mm, and the thickness of the hot-rolled sheet was 3.
0 mm, cold-rolled aluminum foil thickness of 0.1
A high-purity aluminum foil for an electrolytic capacitor was obtained in the same manner as in Example 1 except that the thickness was set to 06 mm.
【００２９】実施例１１ Ｆｅ，Ｓｉ，Ｃｕ，Ｐｂ及びその他の不可避不純物を含
む９９．９７％純度のアルミニウム鋳塊を用い、最終焼
鈍の昇温速度を５０℃／ｈとする他は、実施例１と同様
の方法により、電解コンデンサ用高純度アルミニウム箔
を得た。Example 11 An aluminum ingot having a purity of 99.97% containing Fe, Si, Cu, Pb and other unavoidable impurities was used, and the heating rate of the final annealing was set at 50 ° C./h. In the same manner as in Example 1, a high-purity aluminum foil for an electrolytic capacitor was obtained.
【００３０】比較例１ Ｆｅ，Ｓｉ，Ｃｕ，Ｐｂ及びその他の不可避不純物を含
む９９．９２％純度のアルミニウム鋳塊を用いる他は、
実施例１と同様の方法により、電解コンデンサ用高純度
アルミニウム箔を得た。Comparative Example 1 An aluminum ingot of 99.92% purity containing Fe, Si, Cu, Pb and other unavoidable impurities was used.
A high-purity aluminum foil for an electrolytic capacitor was obtained in the same manner as in Example 1.
【００３１】比較例２ 熱間圧延上がり板の厚さを５．０ｍｍとする他は、実施
例２と同様の方法により、電解コンデンサ用高純度アル
ミニウム箔を得た。Comparative Example 2 A high-purity aluminum foil for an electrolytic capacitor was obtained in the same manner as in Example 2 except that the thickness of the hot-rolled finished plate was 5.0 mm.
【００３２】比較例３ 冷間圧延上がりアルミニウム箔の厚さを０．０７ｍｍと
する他は、実施例２と同様の方法により、電解コンデン
サ用高純度アルミニウム箔を得た。Comparative Example 3 A high-purity aluminum foil for an electrolytic capacitor was obtained in the same manner as in Example 2 except that the thickness of the cold-rolled aluminum foil was changed to 0.07 mm.
【００３３】なお、実施例２〜１１及び比較例１〜３の
各々においても、熱間加工率及び冷間加工率を、表１に
示しておいた。また、各々の例においても、実施例１と
同様にして、アルミニウム箔表面の（１００）面占有率
を測定し、その結果を表１に示しておいた。In each of Examples 2 to 11 and Comparative Examples 1 to 3, the hot working ratio and the cold working ratio are shown in Table 1. Also in each example, the (100) plane occupancy of the aluminum foil surface was measured in the same manner as in Example 1, and the results are shown in Table 1.
【００３４】[0034]
【表１】 [Table 1]
【００３５】表１の結果から明らかなように、実施例に
係る方法で得られた電解コンデンサ用高純度アルミニウ
ム箔は、比較例に係る方法で得られた電解コンデンサ用
高純度アルミニウム箔に比べて、その表面における（１
００）面占有率が高く、エッチング処理したとき、表面
積をより拡大することができ、高静電容量の電解コンデ
ンサ用電極箔が得られることが分かる。As is clear from the results in Table 1, the high-purity aluminum foil for an electrolytic capacitor obtained by the method according to the example is higher than the high-purity aluminum foil for an electrolytic capacitor obtained by the method according to the comparative example. , On its surface (1
00) It can be seen that the surface occupancy is high, the surface area can be further increased when the etching treatment is performed, and an electrode foil for an electrolytic capacitor having a high capacitance can be obtained.
【００３６】[0036]
【作用】本発明において、熱間圧延における熱間加工率
をある程度高くし、その後、適切な冷間加工率で冷間圧
延を行うと、中間焼鈍を省略しても、得られるアルミニ
ウム箔表面における（１００）面占有率が高くなる理由
は定かではない。しかしながら、上記実施例及び比較例
に見られるように、現実に、熱間加工率を一定の範囲で
高くし、且つ、冷間加工率を一定の範囲で行えば、中間
焼鈍を省略しても、アルミニウム箔表面における（１０
０）面占有率が高くなっている。In the present invention, if the hot working ratio in hot rolling is increased to some extent and then cold rolling is performed at an appropriate cold working ratio, even if the intermediate annealing is omitted, the surface of the obtained aluminum foil can be obtained. It is not clear why the (100) plane occupancy increases. However, as can be seen in the above Examples and Comparative Examples, actually, if the hot working ratio is increased in a certain range, and if the cold working ratio is performed in a certain range, the intermediate annealing can be omitted. , On the aluminum foil surface (10
0) The surface occupancy is high.
【００３７】[0037]
【発明の効果】従って、本発明に係る方法を採用すれ
ば、表面における（１００）面占有率の高い電解コンデ
ンサ用高純度アルミニウム箔を得ることができ、エッチ
ングによる表面積の拡大を図ることができ、高静電容量
を持つ電解コンデンサ用電極箔が得られるという効果を
奏する。特に、直流エッチングにより、トンネルピット
を多数且つ高密度に形成させることができ、高静電容量
を持つ電解コンデンサ高圧用陽極箔が得られるという効
果を奏する。Therefore, by employing the method according to the present invention, it is possible to obtain a high-purity aluminum foil for an electrolytic capacitor having a high (100) plane occupancy on the surface, and to increase the surface area by etching. This has the effect that an electrode foil for an electrolytic capacitor having a high capacitance can be obtained. In particular, a large number and high density of tunnel pits can be formed by DC etching, and an effect is obtained that an anode foil for electrolytic capacitor high voltage having high capacitance can be obtained.
【００３８】また、本発明に係る方法を採用すれば、中
間焼鈍及びそれに続く仕上冷間圧延を省略することがで
き、エッチング性の良好な電解コンデンサ用高純度アル
ミニウム箔の製造を合理化しうるという効果をも奏す
る。Further, if the method according to the present invention is adopted, the intermediate annealing and the subsequent finish cold rolling can be omitted, and the production of high-purity aluminum foil for electrolytic capacitors with good etching properties can be rationalized. It also has an effect.
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.7 識別記号 ＦＩ テーマコート゛(参考） Ｃ２２Ｆ 1/00 ６８０ Ｃ２２Ｆ 1/00 ６８６Ｚ ６８６ ６９１Ａ ６９１ ６９１Ｂ ６９４Ａ ６９４ Ｈ０１Ｇ 9/04 ３３７ ──────────────────────────────────────────────────続 き Continued on the front page (51) Int.Cl. 7 Identification symbol FI Theme coat ゛ (Reference) C22F 1/00 680 C22F 1/00 686Z 686 691A 691 691B 694A 694 H01G 9/04 337
Claims (3)
塊に、均質化処理を施した後、熱間加工率９９．２〜９
９．８％の条件で熱間圧延を施し、その後、冷間圧延途
中に中間焼鈍を施すことなく、冷間加工率７５．０〜９
７．０％の条件で冷間圧延を施し、次いで最終焼鈍を施
すことを特徴とする電解コンデンサ用高純度アルミニウ
ム箔の製造方法。An aluminum ingot having a purity of 99.97% or more is subjected to a homogenization treatment, and then a hot working ratio of 99.2 to 9 is obtained.
Hot rolling is performed under the condition of 9.8%, and thereafter, the cold working rate is 75.0 to 9 without performing intermediate annealing during cold rolling.
A method for producing a high-purity aluminum foil for electrolytic capacitors, wherein cold rolling is performed under the condition of 7.0%, and then final annealing is performed.
００ｍｍのアルミニウム鋳塊に、均質化処理を施した
後、熱間圧延を施して、厚さ１．３〜３．０ｍｍの熱間
圧延上がり板を得、次いで該熱間圧延上がり板に、途中
に中間焼鈍を施すことなく冷間圧延を施して、厚さ０．
０９〜０．３０ｍｍの冷間圧延上がりアルミニウム箔を
得た後、最終焼鈍を施すことを特徴とする電解コンデン
サ用高純度アルミニウム箔の製造方法。2. A thickness of 400 to 6 with a purity of 99.97% or more.
The aluminum ingot of 00 mm is subjected to a homogenization treatment and then subjected to hot rolling to obtain a hot-rolled sheet having a thickness of 1.3 to 3.0 mm. Cold-rolled without intermediate annealing to a thickness of 0.1 mm.
A method for producing a high-purity aluminum foil for an electrolytic capacitor, comprising subjecting a cold-rolled aluminum foil of 09 to 0.30 mm to final annealing.
であり、その昇温速度を５０〜５００℃／ｈとする請求
項１又は２記載の電解コンデンサ用高純度アルミニウム
箔の製造方法。3. The final annealing temperature condition is 530 to 580 ° C.
The method for producing a high-purity aluminum foil for an electrolytic capacitor according to claim 1 or 2, wherein the heating rate is 50 to 500 ° C / h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP35406199A JP4060501B2 (en) | 1999-12-14 | 1999-12-14 | Method for producing high-purity aluminum foil for electrolytic capacitors |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP35406199A JP4060501B2 (en) | 1999-12-14 | 1999-12-14 | Method for producing high-purity aluminum foil for electrolytic capacitors |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2001172754A true JP2001172754A (en) | 2001-06-26 |
| JP4060501B2 JP4060501B2 (en) | 2008-03-12 |
Family
ID=18435041
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP35406199A Expired - Fee Related JP4060501B2 (en) | 1999-12-14 | 1999-12-14 | Method for producing high-purity aluminum foil for electrolytic capacitors |
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| Country | Link |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008153347A (en) * | 2006-12-15 | 2008-07-03 | Mitsubishi Alum Co Ltd | Aluminum foil for electrolytic capacitor and its manufacturing method |
| CN100441714C (en) * | 2003-03-07 | 2008-12-10 | 东洋铝株式会社 | Aluminium foil for electrolytic capacitor, and producing method thereof |
| JP2009062594A (en) * | 2007-09-07 | 2009-03-26 | Sumitomo Light Metal Ind Ltd | Aluminum foil material |
| JP2009062595A (en) * | 2007-09-07 | 2009-03-26 | Sumitomo Light Metal Ind Ltd | Aluminum foil material |
| JP2009120963A (en) * | 2002-08-21 | 2009-06-04 | Showa Denko Kk | Manufacturing method of aluminum material for electrolytic capacitor electrode |
| CN114669622A (en) * | 2022-03-22 | 2022-06-28 | 浙江永杰铝业有限公司 | Preparation method of battery aluminum foil and battery aluminum foil |
-
1999
- 1999-12-14 JP JP35406199A patent/JP4060501B2/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009120963A (en) * | 2002-08-21 | 2009-06-04 | Showa Denko Kk | Manufacturing method of aluminum material for electrolytic capacitor electrode |
| CN100441714C (en) * | 2003-03-07 | 2008-12-10 | 东洋铝株式会社 | Aluminium foil for electrolytic capacitor, and producing method thereof |
| JP2008153347A (en) * | 2006-12-15 | 2008-07-03 | Mitsubishi Alum Co Ltd | Aluminum foil for electrolytic capacitor and its manufacturing method |
| JP2009062594A (en) * | 2007-09-07 | 2009-03-26 | Sumitomo Light Metal Ind Ltd | Aluminum foil material |
| JP2009062595A (en) * | 2007-09-07 | 2009-03-26 | Sumitomo Light Metal Ind Ltd | Aluminum foil material |
| CN114669622A (en) * | 2022-03-22 | 2022-06-28 | 浙江永杰铝业有限公司 | Preparation method of battery aluminum foil and battery aluminum foil |
| CN114669622B (en) * | 2022-03-22 | 2023-09-29 | 浙江永杰铝业有限公司 | Preparation method of battery aluminum foil and battery aluminum foil |
Also Published As
| Publication number | Publication date |
|---|---|
| JP4060501B2 (en) | 2008-03-12 |
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