JP3359408B2 - Manufacturing method of aluminum foil for electrode of electrolytic capacitor - Google Patents
Manufacturing method of aluminum foil for electrode of electrolytic capacitorInfo
- Publication number
- JP3359408B2 JP3359408B2 JP00526694A JP526694A JP3359408B2 JP 3359408 B2 JP3359408 B2 JP 3359408B2 JP 00526694 A JP00526694 A JP 00526694A JP 526694 A JP526694 A JP 526694A JP 3359408 B2 JP3359408 B2 JP 3359408B2
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- Prior art keywords
- rolling
- hot rolling
- temperature
- aluminum
- foil
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Description
【０００１】[0001]
【産業上の利用分野】この発明は、電解コンデンサ電極
用アルミニウム箔の製造方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing an aluminum foil for an electrode of an electrolytic capacitor.
【０００２】[0002]
【従来の技術及び解決しようとする課題】アルミニウム
電解コンデンサ用電極材として一般に用いられるＡｌ箔
には、その実効面積を拡大して単位面積当たりの静電容
量を増大するため、通常、電気化学的あるいは化学的エ
ッチング処理が施される。2. Description of the Related Art An aluminum foil generally used as an electrode material for an aluminum electrolytic capacitor generally has an electrochemical area in order to increase its effective area and increase the capacitance per unit area. Alternatively, a chemical etching process is performed.
【０００３】しかし、箔を単にエッチング処理するのみ
では十分な静電容量が得られない。このため、一般的に
は箔圧延後の最終焼鈍工程において、立方体方位を多く
有する集合組織にして箔のエッチング特性を向上させる
べく、４５０℃程度以上の高温加熱処理が施されている
が、立方体方位粒の占有率は製造条件によってバラツキ
が大きく、また非立方体方位粒の筋状分布や粗大化によ
って、部分的に低容量の領域ができるため、昨今の電解
コンデンサの小型化、高静電容量化の要求に対して十分
な満足を得るものではなかった。[0003] However, a sufficient capacitance cannot be obtained simply by etching the foil. For this reason, generally, in the final annealing step after the foil rolling, a high-temperature heat treatment of about 450 ° C. or higher is performed to improve the etching characteristics of the foil by forming a texture having many cube orientations. The occupancy of azimuthal grains varies greatly depending on manufacturing conditions, and a low-capacity region is partially formed due to the streak distribution and coarsening of non-cubic azimuthal grains. Was not satisfactory enough to meet the demands for chemical conversion.
【０００４】一般に、電解コンデンサ用Ａｌ箔はエッチ
ングピット密度を高くするために立方体方位粒の体積率
を上げる必要があるため、Ａｌ純度を上げる（特にＦｅ
量を少なくする）、中間焼鈍〜スキンパス圧下工程を導
入する等の方法が実施されている。In general, Al foil for electrolytic capacitors needs to increase the volume ratio of cubic grains in order to increase the etching pit density.
In other words, methods such as reducing the amount), and introducing a step of intermediate annealing to skin pass reduction are being carried out.
【０００５】しかしながら、これらの方法を用いても、
前述した立方体方位粒の占有率の製造条件バラツキ（以
下「（１００）面積率低下」と記す）や非立方体方位粒
の筋状分布（以下「筋状異方位」と記す）、非立方体方
位粒の粗大化（以下「異方位粗大粒」と記す）によっ
て、部分的に低容量の領域ができることを抑止すること
は難しかった。However, even if these methods are used,
Manufacturing condition variation of the occupancy of the cubic grain described above (hereinafter referred to as “(100) area ratio reduction”), streak distribution of non-cubic grain (hereinafter referred to as “streak different orientation”), non-cubic grain (Hereinafter referred to as "different orientation coarse grains"), it was difficult to suppress the formation of a partially low-capacity region.
【０００６】この発明は、かかる技術的背景に鑑みてな
されたものであって、（１００）面積率低下、筋状異方
位、異方位粗大粒の発生を抑制して、小型化、高静電容
量化を図り得る電解コンデンサ電極用アルミニウム箔の
製造方法の提供を目的とする。The present invention has been made in view of the above technical background, and is intended to reduce the (100) area ratio, to suppress generation of streak-like misorientations and coarse grains of different orientations, and to reduce the size and increase the static electricity. An object of the present invention is to provide a method for producing an aluminum foil for an electrolytic capacitor electrode which can achieve a large capacity.
【０００７】[0007]
【課題を解決するための手段】上記目的を達成するため
に、発明者は鋭意研究の結果、箔製造工程における熱間
圧延途中パスの温度履歴とパススケジュールを制御する
ことで、結晶粒を微細均一にし、上記不具合を解消し得
ることを見出し、この発明を完成し得たものである。Means for Solving the Problems In order to achieve the above object, the present inventors have made intensive studies and as a result, controlled the temperature history and the pass schedule of the hot rolling pass in the foil manufacturing process to reduce the crystal grain size. It has been found that the invention can be made uniform and the above-mentioned problems can be solved, and the present invention has been completed.
【０００８】即ち、この発明は、アルミニウム純度９
９．９％以上のアルミニウム鋳塊に均熱加熱、面削を実
施した後、４７０〜５８０℃の温度、２４〜３時間の保
持時間で前加熱する工程と、前加熱後直ちに熱間圧延を
開始し、板厚１００〜２０ｍｍになった時点で冷却速度
０．５℃／ｓｅｃ以上の冷却速度で３８０〜４５０℃の
温度まで冷却し、その後の１パスを２５％以上の圧下率
で圧延する工程と、その後、引き続いて板厚３〜５０ｍ
ｍまで熱間圧延する工程とを実施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を要旨
とする。[0008] That is, the present invention provides an aluminum purity of 9
A step of preheating at a temperature of 470 to 580 ° C. and a holding time of 24 to 3 hours after performing soaking heating and face milling on an aluminum ingot of 9.9% or more, and hot rolling immediately after the preheating. It starts and when the thickness of the plate becomes 100 to 20 mm, it is cooled to a temperature of 380 to 450 ° C. at a cooling rate of 0.5 ° C./sec or more, and the subsequent one pass is rolled at a rolling reduction of 25% or more. Process, and then, subsequently, a thickness of 3 to 50 m
and a step of hot-rolling to an aluminum foil for an electrolytic capacitor electrode.
【０００９】この発明に用いるアルミニウム鋳塊のアル
ミニウム純度に９９．９％以上を必要とするのは、９
９．９％未満の純度では、箔のエッチング時にエッチン
グピットの成長が多くの不純物の存在によって阻害さ
れ、本発明に係る製造工程を実施してもなお均一な深い
トンネル状のエッチングピットを形成できず、従って静
電容量の高いアルミニウム箔を得ることができないから
である。好ましくはアルミニウム純度を９９．９８％以
上とするのが良い。[0009] The reason why the aluminum ingot used in the present invention requires aluminum purity of 99.9% or more is 99.9%.
At a purity of less than 9.9%, the growth of etching pits during the etching of the foil is hindered by the presence of many impurities, and uniform deep tunnel-shaped etching pits can still be formed even when the manufacturing process according to the present invention is performed. Therefore, an aluminum foil having a high capacitance cannot be obtained. Preferably, the aluminum purity is 99.98% or more.
【００１０】アルミニウム箔は一般的には、アルミニウ
ム鋳塊に均熱加熱、面削、熱間圧延、冷間圧延、箔圧延
を実施することにより製造される。均熱加熱、面削は常
法により行えば良い。[0010] Aluminum foil is generally produced by subjecting an aluminum ingot to soaking heating, facing, hot rolling, cold rolling and foil rolling. The soaking and heating may be carried out by conventional methods.
【００１１】また、結晶粒微細化のためには、熱間圧延
の開始温度は再結晶温度以上でできるだけ低いことが望
ましい。しかし、開始温度が４７０℃未満ではＡｌ−Ｆ
ｅ、あるいはＡｌ−Ｆｅ−Ｓｉの微細析出物がマトリッ
クス内に析出し、最終焼鈍後もこの微細析出物が再固溶
することなく残るため、エッチング時に局部溶解を起こ
し高静電容量を得ることができない。一方、開始温度が
５８０℃を越えると熱間圧延初期の再結晶粒径が粗大化
するため、後述する条件によっても熱間圧延上がりの結
晶粒を微細化できず、高（１００）面積率を得ることが
できない。従って、熱間圧延の開始温度を４７０〜５８
０℃とし、このために熱間圧延に際しての前加熱を４７
０〜５８０℃の温度、２４〜３時間の保持時間で行う。
好ましくは、５００〜５５０℃×１２〜５時間である。Further, in order to refine the crystal grains, it is desirable that the starting temperature of the hot rolling be as low as possible above the recrystallization temperature. However, if the starting temperature is lower than 470 ° C., Al—F
e, or a fine precipitate of Al-Fe-Si precipitates in the matrix, and remains after the final annealing without re-dissolving, resulting in local dissolution during etching to obtain a high capacitance. Can not. On the other hand, if the starting temperature exceeds 580 ° C., the recrystallized grain size in the early stage of hot rolling becomes coarse, so that the crystal grains after hot rolling cannot be refined even under the conditions described later, and the high (100) area ratio increases. I can't get it. Therefore, the starting temperature of hot rolling is set to 470-58.
0 ° C., so that the pre-heating during hot rolling was 47 ° C.
The reaction is performed at a temperature of 0 to 580 ° C. and a holding time of 24 to 3 hours.
Preferably, it is 500-550 degreeC x 12-5 hours.
【００１２】次に、熱間圧延により板厚が１００〜２０
ｍｍになった時点で冷却による温度制御を行う。板厚が
１００ｍｍを越えると熱間圧延開始からのパス回数が少
なく（１パス圧下率は、再結晶を促進するためにあまり
低くできない）、再結晶が繰り返し起こらないため、高
（１００）面積率を得ることができない。一方、板厚が
２０ｍｍ未満では、その後の温間加工度を大きくとれな
いため、結晶粗大の原因となる。従って、冷却時の板厚
は１００〜２０ｍｍとする。好ましくは８０〜３０ｍｍ
である。Next, the sheet thickness is 100 to 20 by hot rolling.
When the pressure reaches mm, temperature control by cooling is performed. When the sheet thickness exceeds 100 mm, the number of passes from the start of hot rolling is small (the rolling reduction in one pass cannot be too low to promote recrystallization), and recrystallization does not occur repeatedly. Can not get. On the other hand, if the plate thickness is less than 20 mm, the subsequent degree of warm working cannot be increased, which causes crystal coarsening. Therefore, the plate thickness at the time of cooling is set to 100 to 20 mm. Preferably 80 to 30 mm
It is.
【００１３】冷却は水冷により冷却速度０．５℃／ｓｅ
ｃ以上の冷却速度で３８０〜４５０℃の温度まで行う。
冷却後の温度が３８０℃未満ではその後の１パスで再結
晶が進行せず前パスの再結晶粒がそのまま圧延されるた
め、結晶粒径が粗大となり、高（１００）面積率を得る
ことができない。また、冷却後の温度が４５０℃を越え
ると、その後の１パスでの再結晶における再結晶粒が大
きくなり、熱間圧延上がりの結晶粒を微細化できず、や
はり高（１００）面積率を得ることができない。従っ
て、水冷後の温度は３８０〜４５０℃とする。好ましく
は４００〜４５０℃である。また、冷却速度が０．５℃
／ｓｅｃ以上に規定されるのは、結晶粒成長を押さえる
ためであり、好ましくは１℃／ｓｅｃ以上である。The cooling rate is 0.5 ° C./sec by water cooling.
C. to a temperature of 380-450 ° C. at a cooling rate of c or more.
If the temperature after cooling is lower than 380 ° C., recrystallization does not proceed in one subsequent pass and recrystallized grains in the previous pass are rolled as they are, so that the crystal grain size becomes coarse and a high (100) area ratio can be obtained. Can not. On the other hand, if the temperature after cooling exceeds 450 ° C., the recrystallized grains in the subsequent recrystallization in one pass become large, and the crystal grains after hot rolling cannot be refined. I can't get it. Therefore, the temperature after water cooling is 380 to 450 ° C. Preferably it is 400-450 degreeC. The cooling rate is 0.5 ° C
/ Sec or more is for suppressing the growth of crystal grains, and is preferably 1 ° C / sec or more.
【００１４】水冷直後の１パス目の圧下率は、再結晶を
起こさせる必要性から、２５％以上好ましくは３５％以
上とする。[0014] The rolling reduction in the first pass immediately after water cooling is set to 25% or more, preferably 35% or more because of the necessity of causing recrystallization.
【００１５】その後引き続いて熱間圧延を行うが、熱間
圧延上がりの板厚が５０ｍｍを越えると、冷間圧延に非
常に多くの時間を要し、工業的に不利である。一方３ｍ
ｍ未満ではその後の冷間加工度が低すぎて、十分な圧延
集合組織が発達せず高（１００）面積率を得ることがで
きない。従って、熱間圧延上がりの板厚は３〜５０ｍｍ
とする。好ましくは５〜２０ｍｍである。Thereafter, hot rolling is performed. If the thickness of the hot-rolled sheet exceeds 50 mm, much time is required for cold rolling, which is industrially disadvantageous. 3m
If it is less than m, the subsequent cold work degree is too low, and a sufficient rolling texture is not developed, so that a high (100) area ratio cannot be obtained. Therefore, the thickness after hot rolling is 3 to 50 mm.
And Preferably it is 5 to 20 mm.
【００１６】このような熱間圧延工程を経ることによ
り、熱間圧延上がりにおける再結晶粒の圧延方向と直交
する方向の幅を５００μｍ以下とすることができ、最終
（１００）面積率が高く、筋状異方位分布、異方位粗大
粒がなく、全域にわたって高静電容量の箔を得ることが
できる。Through such a hot rolling step, the width of the recrystallized grains in the direction perpendicular to the rolling direction after hot rolling can be made 500 μm or less, and the final (100) area ratio is high. It is possible to obtain a foil having a high capacitance over the entire area without any streak-like hetero-orientation distribution and hetero-orientation coarse grains.
【００１７】熱間圧延終了後、箔圧延を含む冷間圧延を
行い、必要に応じて冷間圧延途中に中間焼鈍を行い、さ
らに最終焼鈍を実施する。これらの冷間圧延、中間焼
鈍、最終焼鈍は常法の条件により行えば良い。After the completion of the hot rolling, cold rolling including foil rolling is performed, and if necessary, intermediate annealing is performed during the cold rolling, and final annealing is further performed. These cold rolling, intermediate annealing, and final annealing may be performed under ordinary conditions.
【００１８】[0018]
【作用】箔製造工程における熱間圧延途中パスの温度履
歴とパススケジュールを制御することにより、結晶粒が
微細均一となり、（１００）面積率低下、筋状異方位、
異方位粗大粒の発生が抑制される。By controlling the temperature history and the pass schedule of the hot rolling pass during the foil manufacturing process, the crystal grains become fine and uniform, the (100) area ratio decreases, streak-like misorientation,
Generation of coarse grains in different directions is suppressed.
【００１９】[0019]
【実施例】表１に示す各種組成のアルミニウム鋳塊に、
均熱加熱、面削を施した後、前加熱を５５０℃の温度、
１２時間の保持時間で実施した。EXAMPLE An aluminum ingot of various compositions shown in Table 1 was used.
After uniform heating and facing, preheating is performed at 550 ° C.
Performed with a 12 hour hold time.
【００２０】その後直ちに熱間圧延を開始したのち、表
１に示す板厚になった時点で、冷却した。冷却速度、冷
却後の温度は表１に示すとおりとした。Immediately after the hot rolling was started, when the sheet thickness shown in Table 1 was reached, the sheet was cooled. The cooling rate and the temperature after cooling were as shown in Table 1.
【００２１】そして、直後の１パスを表１に示す圧下率
で圧延した後、引き続いて板厚５ｍｍまで熱間圧延し
た。Then, one pass immediately after the above was rolled at a rolling reduction shown in Table 1, and subsequently hot-rolled to a thickness of 5 mm.
【００２２】熱間圧延終了後、冷間圧延、中間焼鈍、冷
間圧延を実施し、最終厚さμｍの箔としたのち、最終焼
鈍を実施した。なお、試料Ａ、Ｂの箔については、中間
焼鈍を２５０℃×５時間、最終焼鈍を５００℃×５時間
の条件で行った。また、試料Ｃ〜Ｇの箔については、中
間焼鈍を２７０℃×５時間、最終焼鈍を５５０℃×５時
間の条件で行った。After the completion of the hot rolling, cold rolling, intermediate annealing, and cold rolling were performed to obtain a foil having a final thickness of μm, and then final annealing was performed. The foils of Samples A and B were subjected to intermediate annealing at 250 ° C. for 5 hours and final annealing at 500 ° C. for 5 hours. The foils of samples C to G were subjected to intermediate annealing at 270 ° C. × 5 hours and final annealing at 550 ° C. × 5 hours.
【００２３】[0023]
【表１】 そして、得られた各アルミニウム箔の立方体方位の占有
率、及び筋状異方位、異方位粗大粒の有無を調べた。そ
の結果を表２に示す。[Table 1] Then, the occupancy of the obtained aluminum foil in the cubic orientation, and the presence or absence of streak different orientations and different orientation coarse grains were examined. Table 2 shows the results.
【００２４】次に、以下の条件でエッチングを実施した
のち、得られたアルミニウム箔に５％ホウ酸浴中で２５
０Ｖの化成処理を行って、静電容量を測定した。その結
果を、試料Ｂの静電容量を１００％としたときの相対比
較にて、表２に示す。Next, after etching was carried out under the following conditions, the obtained aluminum foil was placed in a 5% boric acid bath for 25 minutes.
A chemical conversion treatment of 0 V was performed, and the capacitance was measured. The results are shown in Table 2 as a relative comparison when the capacitance of Sample B is set to 100%.
【００２５】［エッチング条件］ 前処理：なし 一次エッチング 液組成：５％ＨＣｌ＋２０％Ｈ2 ＳＯ
4 、液温：８０℃、電流密度：直流２０Ａ／ｄｍ2 、時
間：８０〜１８０秒 二次エッチング 液組成：５％ＨＣｌ＋０．１％Ｈ2 Ｃ
2 Ｏ4 、液温：８０℃、 電流密度：
直流５Ａ／ｄｍ2 、時間：１０分[Etching conditions] Pre-treatment: none Primary etching solution composition: 5% HCl + 20% H 2 SO
4. Liquid temperature: 80 ° C., current density: DC 20 A / dm 2 , time: 80 to 180 seconds Secondary etching liquid composition: 5% HCl + 0.1% H 2 C
2 O 4 , liquid temperature: 80 ° C, current density:
DC 5A / dm 2 , time: 10 minutes
【表２】 上記表２の結果からわかるように、本発明によって製造
した実施品は、比較品に較べて、立方体方位占有率が大
きく、筋状異方位、異方位粗大粒が存在せず、また静電
容量も大きいことを確認し得た。[Table 2] As can be seen from the results in Table 2 above, the embodiment product manufactured according to the present invention has a larger cubic orientation occupancy, has no streak-like misorientation and different-orientation coarse grains as compared with the comparative product, and has a capacitance. Was also large.
【００２６】[0026]
【発明の効果】この発明は上述の次第で、箔製造工程に
おける熱間圧延途中パスの温度履歴とパススケジュール
を所定状態に制御するものであるから、結晶粒を微細均
一にでき、（１００）面積率低下、筋状異方位、異方位
粗大粒の発生を抑制し得て、エッチング適性に優れたも
のとなしえ、静電容量の大きなアルミニウム箔を提供す
ることができる。As described above, according to the present invention, the temperature history and the pass schedule of the hot rolling pass in the foil manufacturing process are controlled to a predetermined state, so that the crystal grains can be made fine and uniform. It is possible to suppress the reduction of the area ratio, the generation of streak-like different orientations, and the generation of coarse grains in different orientations, thereby achieving excellent etching suitability and providing an aluminum foil having a large capacitance.
フロントページの続き (72)発明者 明城 信彦 堺市海山町６丁224番地 昭和アルミニ ウム株式会社内 (72)発明者 御所名 健二 堺市海山町６丁224番地 昭和アルミニ ウム株式会社内 (56)参考文献 特開 平４−89118（ＪＰ，Ａ) 特開 昭62−193238（ＪＰ，Ａ) 特開 平１−276612（ＪＰ，Ａ) (58)調査した分野(Int.Cl.7，ＤＢ名) H01G 9/055 Continued on the front page (72) Inventor Nobuhiko Meijo 6,224 Kaiyama-cho, Sakai City Inside Showa Aluminum Co., Ltd. (72) Inventor Kenji 6,224 Kaiyama-cho Sakai City Inside Showa Aluminum Co., Ltd. (56 References JP-A-4-89118 (JP, A) JP-A-62-193238 (JP, A) JP-A-1-276612 (JP, A) (58) Fields investigated (Int. Cl. 7 , DB (Name) H01G 9/055
Claims (1)
ミニウム鋳塊に均熱加熱、面削を実施した後、４７０〜
５８０℃の温度、２４〜３時間の保持時間で前加熱する
工程と、 前加熱後直ちに熱間圧延を開始し、板厚１００〜２０ｍ
ｍになった時点で冷却速度０．５℃／ｓｅｃ以上の冷却
速度で３８０〜４５０℃の温度まで冷却し、その後の１
パスを２５％以上の圧下率で圧延する工程と、 その後、引き続いて板厚３〜５０ｍｍまで熱間圧延する
工程とを実施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。An ingot of aluminum having an aluminum purity of 99.9% or more is subjected to soaking and heating, and is subjected to face milling.
A step of preheating at a temperature of 580 ° C. and a holding time of 24 to 3 hours; and immediately after the preheating, hot rolling is started and the sheet thickness is 100 to 20 m.
m, at a cooling rate of 0.5 ° C./sec or more to a temperature of 380-450 ° C.
A method for producing an aluminum foil for an electrolytic capacitor electrode, comprising: a step of rolling a pass at a rolling reduction of 25% or more; and a step of subsequently hot rolling to a thickness of 3 to 50 mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP00526694A JP3359408B2 (en) | 1994-01-21 | 1994-01-21 | Manufacturing method of aluminum foil for electrode of electrolytic capacitor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP00526694A JP3359408B2 (en) | 1994-01-21 | 1994-01-21 | Manufacturing method of aluminum foil for electrode of electrolytic capacitor |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH07211591A JPH07211591A (en) | 1995-08-11 |
| JP3359408B2 true JP3359408B2 (en) | 2002-12-24 |
Family
ID=11606432
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP00526694A Expired - Lifetime JP3359408B2 (en) | 1994-01-21 | 1994-01-21 | Manufacturing method of aluminum foil for electrode of electrolytic capacitor |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3359408B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000269092A (en) * | 1999-03-18 | 2000-09-29 | Kobe Steel Ltd | Aluminum foil for electrolytic capacitor having superior ability to etch, and its manufacture |
-
1994
- 1994-01-21 JP JP00526694A patent/JP3359408B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH07211591A (en) | 1995-08-11 |
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