JP5897430B2 - Aluminum alloy foil excellent in formability after lamination, manufacturing method thereof, and laminate foil using the aluminum alloy foil - Google Patents
Aluminum alloy foil excellent in formability after lamination, manufacturing method thereof, and laminate foil using the aluminum alloy foil Download PDFInfo
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- 239000011888 foil Substances 0.000 title claims description 67
- 229910000838 Al alloy Inorganic materials 0.000 title claims description 49
- 238000003475 lamination Methods 0.000 title claims description 12
- 238000004519 manufacturing process Methods 0.000 title claims description 12
- 238000005096 rolling process Methods 0.000 claims description 71
- 239000013078 crystal Substances 0.000 claims description 48
- 229910000765 intermetallic Inorganic materials 0.000 claims description 22
- 239000002245 particle Substances 0.000 claims description 13
- 238000004458 analytical method Methods 0.000 claims description 12
- 238000005097 cold rolling Methods 0.000 claims description 12
- 238000000137 annealing Methods 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 11
- 238000000265 homogenisation Methods 0.000 claims description 10
- 229910018084 Al-Fe Inorganic materials 0.000 claims description 7
- 229910018192 Al—Fe Inorganic materials 0.000 claims description 7
- 238000005098 hot rolling Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 238000011282 treatment Methods 0.000 claims description 7
- 229910052802 copper Inorganic materials 0.000 claims description 6
- 230000009467 reduction Effects 0.000 claims description 5
- 229910052725 zinc Inorganic materials 0.000 claims description 5
- 229910052749 magnesium Inorganic materials 0.000 claims description 4
- 229920005992 thermoplastic resin Polymers 0.000 claims description 3
- 239000000463 material Substances 0.000 description 35
- 238000012360 testing method Methods 0.000 description 34
- 238000000465 moulding Methods 0.000 description 11
- 229910045601 alloy Inorganic materials 0.000 description 8
- 239000000956 alloy Substances 0.000 description 8
- 238000001953 recrystallisation Methods 0.000 description 5
- 239000006104 solid solution Substances 0.000 description 5
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- 238000005461 lubrication Methods 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
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Description
本発明は、食品、医薬品、電子部品等に利用されるラミネート箔に用いられる、ラミネート後の成形性に優れたアルミニウム合金箔とその製造方法、および該アルミニウム合金箔を用いたラミネート箔に関する。 The present invention relates to an aluminum alloy foil excellent in formability after lamination used for a laminate foil used for foods, pharmaceuticals, electronic parts and the like, a method for producing the same, and a laminate foil using the aluminum alloy foil.
従来、成形加工用のアルミニウム合金として、１０００系アルミニウム合金、３０００系アルミニウム合金、５０００系アルミニウム合金、６０００系アルミニウム合金、８０００系アルミニウム合金が使用されてきた。その中でも、圧延性に優れた８０００系アルミニウム合金が成形加工用のアルミニウム合金箔用として広く用いられ、ＪＩＳ Ｈ４１６０にＡ８０７９合金やＡ８０２１合金、Ａｌ−Ｆｅ系のアルミニウム合金が規定されている。 Conventionally, 1000 series aluminum alloys, 3000 series aluminum alloys, 5000 series aluminum alloys, 6000 series aluminum alloys, and 8000 series aluminum alloys have been used as aluminum alloys for forming. Among them, an 8000 series aluminum alloy excellent in rollability is widely used for forming aluminum alloy foils, and A8079 alloy, A8021 alloy, and Al—Fe series aluminum alloy are defined in JIS H4160.
アルミニウム合金箔は、アルミニウム合金の鋳塊を均質化処理後、熱間圧延、冷間圧延を施すことにより製造され、必要に応じて冷間圧延途中の中間焼鈍や、冷間圧延後の最終焼鈍が行われる。このように作製されたアルミニウム合金箔は、例えば両面に熱可塑性樹脂をラミネートした状態で成形され、医薬品や電池のパッケージなど、包装材として用いられる。これら包装用ラミネート箔については、高成形性に対する要求が年々高まっており、難加工形状に成形されても破断やピンホールが発生しないことが求められている。 Aluminum alloy foil is manufactured by homogenizing an aluminum alloy ingot, then hot rolling and cold rolling, and if necessary, intermediate annealing during cold rolling or final annealing after cold rolling. Is done. The aluminum alloy foil produced in this manner is molded, for example, with a thermoplastic resin laminated on both sides, and is used as a packaging material for pharmaceuticals and battery packages. About these laminated foils for packaging, the request | requirement with respect to high moldability is increasing year by year, and it is calculated | required that a fracture | rupture and a pinhole do not generate | occur | produce even if it shape | molds in a difficult-to-process shape.
ラミネート箔の成形性を向上させるために、積層フィルムおよびアルミニウム合金箔の構成を検討し良好な冷間成形性を得るための条件が報告されているが、これらは最終製品としてのラミネート箔としての成形性を求めたものであり、ラミネート箔を構成するアルミニウム合金箔がラミネート後の成形性に与える影響については十分に検討されていない。 In order to improve the moldability of the laminate foil, the conditions for studying the composition of the laminated film and the aluminum alloy foil and obtaining good cold formability have been reported. The formability is required, and the influence of the aluminum alloy foil constituting the laminate foil on the formability after lamination has not been sufficiently studied.
また、製造工程により材料組織を調整して、成形加工性を向上させた８０００系合金も提案されている。例えば、固溶元素量を調整することにより箔圧延性を高め、ピンホールを少なくすること、金属間化合物粒子の分散状態を制御することにより、優れた成形加工性を達成できることなどが提案されているが、これらの提案は、主に箔圧延性の点から素箔の成形性向上を追及したものであり、ラミネート箔の状態でのプレス成形性を向上させるものではない。 In addition, an 8000 series alloy has been proposed in which the material structure is adjusted by the manufacturing process to improve the formability. For example, it has been proposed that by adjusting the amount of solid solution element, the foil rollability can be increased, pinholes can be reduced, and by controlling the dispersion state of intermetallic compound particles, excellent moldability can be achieved. However, these proposals are mainly aimed at improving the formability of the raw foil from the viewpoint of foil rollability, and do not improve the press formability in the state of the laminated foil.
また、結晶方位を制御することにより、ラミネート箔の成形性を向上させるための好適なＡｌ−Ｆｅ系アルミニウム合金箔が得られることも提案されているが、Ａｌ−Ｆｅ系合金において、ラミネート箔の成形性に重要な影響を及ぼす金属間化合物粒子についての検討が十分になされているとは言えず、ラミネート後における成形性は必ずしも十分ではない。 It has also been proposed to obtain a suitable Al-Fe-based aluminum alloy foil for improving the moldability of the laminate foil by controlling the crystal orientation. It cannot be said that the intermetallic compound particles that have an important influence on the moldability are sufficiently studied, and the moldability after lamination is not always sufficient.
本発明は、上記従来の問題点を解決するために、ラミネート箔にした状態で成形性向上を達成できるアルミニウム合金箔を得ることを目的として試験、検討を重ねた結果としてなされたものであり、その目的は、素箔の状態でも高い成形性を示すとともに、特にラミネート箔にした状態で最も良好な成形性を達成することができる、ラミネート後の成形性に優れたアルミニウム合金箔および該アルミニウム合金箔を用いたラミネート箔を提供することにある。 In order to solve the above-mentioned conventional problems, the present invention was made as a result of repeated testing and examination for the purpose of obtaining an aluminum alloy foil capable of achieving improvement in formability in a laminated foil state, The purpose of the aluminum alloy foil is excellent in formability after lamination, and can exhibit the best formability especially in a laminated foil state, while exhibiting high formability even in the state of a base foil and the aluminum alloy It is providing the laminated foil using foil.
上記の目的を達成するための請求項１によるラミネート後の成形性に優れたアルミニウム合金箔は、Ｆｅ：０．６〜１．６％（ｍａｓｓ％、以下同じ）、Ｓｉ：０．０２〜０．２％を含有し、Ｔｉ：０．０１〜０．１％、Ｂ：０．０１〜０．０５％の１種または２種を含有し、Ｍｎを０．１％以下、Ｍｇを０．１％以下、Ｃｕを０．１％以下、Ｚｎを０．２５％以下に制限し、残部Ａｌおよび不可避的不純物からなり、粒径（円相当径、以下同じ）１．０μｍ以上のＡｌ−Ｆｅ系金属間化合物の数密度が５００００個／ｍｍ２以下、電子後方散乱解析像法（ＥＢＳＰ）による結晶方位解析で５°以上の方位差を有する境界を結晶粒界と規定し、該結晶粒界に囲まれる結晶粒について、結晶粒径（円相当径、以下同じ）の平均値Ｄが１２μｍ以下であり、且つ、２０μｍを超える結晶粒径を有する結晶粒の面積率が３０％以下、２０℃における電気抵抗をＥ［ｎΩｍ］、Ｆｅ含有量をＣ［ｍａｓｓ％］としたとき、（Ｅ−２６．５）／Ｃの値が３．８以下であることを特徴とする。 The aluminum alloy foil excellent in formability after lamination according to claim 1 for achieving the above object is Fe: 0.6 to 1.6% (mass%, the same applies hereinafter), Si: 0.02 to 0 2%, Ti: 0.01% to 0.1%, B: 0.01% to 0.05%, or Mn is 0.1% or less, and Mg is 0.1% or less. 1% or less, Cu is limited to 0.1% or less, Zn is limited to 0.25% or less, the balance is Al and inevitable impurities, and the particle diameter (equivalent circle diameter, the same shall apply hereinafter) is 1.0 μm or more. A boundary having a misorientation of 5 ° or more in crystal orientation analysis by electron backscattering analysis image method (EBSP) is defined as a crystal grain boundary, wherein the number density of the intermetallic compound is 50000 / mm 2 or less, and the crystal grain boundary The average value D of the crystal grain size (equivalent circle diameter, the same shall apply hereinafter) is 12 μm or less for the crystal grains surrounded by When the area ratio of crystal grains having a crystal grain size exceeding 20 μm is 30% or less, the electrical resistance at 20 ° C. is E [nΩm], and the Fe content is C [mass%], (E− 26.5) The value of / C is 3.8 or less.
請求項２によるラミネート後の成形性に優れたアルミニウム合金箔の製造方法は、請求項１記載のアルミニウム合金箔を製造する方法であって、請求項１記載の組成を有するアルミニウム合金を溶解、鋳造し、得られた鋳塊を面削した後、５００〜６２０℃の温度で１時間以上保持する均質化処理を行い、続いて熱間粗圧延と熱間仕上圧延からなる熱間圧延を行い、熱間粗圧延は、熱間粗圧延中の温度範囲を３５０〜５５０℃とし、熱間粗圧延の圧延パス中、板厚が１５０ｍｍ未満となった圧延パス間で次の圧延まで３０秒以上保持する工程を１回以上行い、熱間粗圧延の最終パスの板厚減少率を４０％以上とし、熱間粗圧延後、熱間仕上圧延、冷間圧延を行い、最終焼鈍処理を施すことを特徴とする。 A method for producing an aluminum alloy foil having excellent formability after lamination according to claim 2 is a method for producing an aluminum alloy foil according to claim 1, wherein the aluminum alloy foil having the composition according to claim 1 is melted and cast. Then, after chamfering the obtained ingot, it is subjected to a homogenization treatment that is held at a temperature of 500 to 620 ° C. for 1 hour or more, followed by hot rolling consisting of hot rough rolling and hot finish rolling, In the hot rough rolling, the temperature range during hot rough rolling is set to 350 to 550 ° C., and during the hot rough rolling rolling pass, the sheet thickness is less than 150 mm, and is maintained for 30 seconds or more until the next rolling. The thickness reduction rate of the final pass of hot rough rolling should be 40% or more, and after hot rough rolling, hot finish rolling and cold rolling are performed, and the final annealing treatment is performed. Features.
請求項３によるラミネート箔は、請求項１に記載のアルミニウム合金箔の両面に熱可塑性樹脂からなる延伸フィルムをそれぞれ１層または２層以上張り合わせたことを特徴とする。 A laminate foil according to a third aspect is characterized in that one or more stretched films made of a thermoplastic resin are bonded to both surfaces of the aluminum alloy foil according to the first aspect.
本発明によれば、特にラミネート箔にした状態で最も良好な成形性を達成することができる、ラミネート後の成形性に優れたアルミニウム合金箔とその製造方法、および該アルミニウム合金箔を用いたラミネート箔が提供される。 ADVANTAGE OF THE INVENTION According to this invention, the aluminum alloy foil excellent in the moldability after lamination which can achieve the best moldability especially in the state made into the laminate foil, its manufacturing method, and the laminate using this aluminum alloy foil A foil is provided.
本発明のアルミニウム合金箔の合金成分の意義および限定理由について説明する。
Ｆｅ：
Ｆｅは本合金系における主要な合金元素であり、金属間化合物として存在して、再結晶時の核生成を促し、結晶粒を微細にするよう機能する。Ｆｅの好ましい含有量は０．６〜１．６％の範囲であり、０．６％未満では、結晶粒を微細にするための金属間化合物が少なくなって微細粒が得られず、１．６％を超えると、過多に形成した金属間化合物がピンホールや成形加工中のラミネート剥離の起点となる。Ｆｅのより好ましい含有範囲は０．７５〜１．５５％、さらに好ましい含有範囲は０．９〜１．５％である。
The significance and reasons for limitation of the alloy components of the aluminum alloy foil of the present invention will be described.
Fe:
Fe is a main alloy element in the present alloy system, and exists as an intermetallic compound, which promotes nucleation during recrystallization and functions to make crystal grains fine. The preferable content of Fe is in the range of 0.6 to 1.6%. If it is less than 0.6%, the amount of intermetallic compounds for making the crystal grains finer becomes small and fine grains cannot be obtained. If it exceeds 6%, the excessively formed intermetallic compound becomes the starting point of delamination during pinholes or molding. A more preferable content range of Fe is 0.75 to 1.55%, and a more preferable content range is 0.9 to 1.5%.
Ｓｉ：
ＳｉはＦｅと共に金属間化合物を形成するが、Ｍｎが含有された場合、金属間化合物粒子の粒径が小さくなって結晶粒の発達を阻害し、混粒組織の形成を促すので、好ましいＳｉ含有量の上限は０．２％以下とする。Ｓｉ量に特に下限は定めないが、Ｓｉ量が少なくなると、高純度地金を使用することとなり、地金コストが高くなるため、通常は０．０２％以上とするのが好ましい。
Si:
Si forms an intermetallic compound with Fe. However, when Mn is contained, the grain size of the intermetallic compound particles is reduced to inhibit the development of crystal grains and promote the formation of a mixed grain structure. The upper limit of the amount is 0.2% or less. There is no particular lower limit to the amount of Si, but if the amount of Si decreases, high-purity bullion will be used and the bullion cost will increase, so it is usually preferably 0.02% or more.
本発明において、Ｍｎ、Ｍｇ、ＣｕおよびＺｎは強度を向上させ、成形時の局部変形を抑制し、ラミネート後の成形性改善に寄与するが、これらの元素は以下の理由によりその含有量を制限することが必要であり、必ずしも含有させる必要はない。 In the present invention, Mn, Mg, Cu and Zn improve strength, suppress local deformation during molding, and contribute to improvement of moldability after lamination. However, the content of these elements is limited for the following reasons. It is necessary to do, and it is not always necessary to contain.
Ｍｎは、ＦｅおよびＳｉと共に金属間化合物を形成するが、Ｍｎが含有された金属間化合物粒子はサイズが小さいため、結晶粒の発達を阻害して混粒組織の形成を促す。そのためＭｎの含有量は０．１％以下とするのが好ましい。Ｍｇ、ＣｕおよびＺｎは、アルミニウム合金箔に固溶して、最終焼鈍における再結晶を遅延させ、最終箔において粗大な結晶粒を生じさせ、成形性を低下させる原因となるため、これらの元素の含有量は、Ｍｇ：０．１％以下、Ｃｕ：０．１％以下、Ｚｎ：０．２５％以下とするのが好ましい。 Mn forms an intermetallic compound together with Fe and Si. However, since the intermetallic compound particle containing Mn is small in size, it inhibits the development of crystal grains and promotes the formation of a mixed grain structure. Therefore, the Mn content is preferably 0.1% or less. Since Mg, Cu and Zn are dissolved in the aluminum alloy foil, the recrystallization in the final annealing is delayed, and coarse crystal grains are formed in the final foil. The contents are preferably Mg: 0.1% or less, Cu: 0.1% or less, and Zn: 0.25% or less.
ＴｉおよびＢは鋳造組織を微細化して、鋳造時に生成する晶出物の分散形態および結晶粒組織を均一にするよう機能する。好ましい含有量は、それぞれＴｉ：０．０１〜０．１％、Ｂ：０．０１〜０．０５％の範囲であり、この上限を超えて含有されると、粗大な金属間化合物が生成し、ピンホールや成形加工中のラミネート剥離が発生する。 Ti and B function to refine the cast structure to make the dispersion form and crystal grain structure of the crystallized product generated during casting uniform. Preferable contents are in the ranges of Ti: 0.01 to 0.1% and B: 0.01 to 0.05%, respectively, and if it exceeds this upper limit, a coarse intermetallic compound is generated. , Delamination during pinholes and molding occurs.
本発明のアルミニウム合金箔における材料組織の限定理由について説明する。本発明においては、粒径１．０μｍ以上のＡｌ−Ｆｅ系金属間化合物の数密度が５００００個／ｍｍ２以下、電子後方散乱解析像法（ＥＢＳＰ）による結晶方位解析で５°以上の方位差を有する境界を結晶粒界と規定し、該結晶粒界に囲まれる結晶粒について、結晶粒径の平均値Ｄが１２μｍ以下であり、且つ、２０μｍを超える結晶粒径を有する結晶粒の面積率が３０％以下、２０℃における電気抵抗をＥ［ｎΩｍ］、Ｆｅ含有量をＣ［ｍａｓｓ％］としたとき、（Ｅ−２６．５）／Ｃの値が３．８以下であることを特徴とする。 The reason for limiting the material structure in the aluminum alloy foil of the present invention will be described. In the present invention, the number density of Al—Fe intermetallic compounds having a particle size of 1.0 μm or more is 50000 pieces / mm 2 or less, and the orientation difference is 5 ° or more by crystal orientation analysis by electron backscatter analysis image method (EBSP). Is defined as a crystal grain boundary, and the crystal grains surrounded by the crystal grain boundary have an average crystal grain size D of 12 μm or less and an area ratio of crystal grains having a crystal grain size exceeding 20 μm Is 30% or less, the electrical resistance at 20 ° C. is E [nΩm], and the Fe content is C [mass%], the value of (E-26.5) / C is 3.8 or less. And
粒径１．０μｍ以上の粗大なＡｌ−Ｆｅ系金属間化合物粒子は、再結晶時の核生成を促し、結晶粒を微細にする働きがあるが、過多に存在すると、圧延時のピンホール発生や成形加工中のラミネート剥離の原因となるので、粒径が１．０μｍ以上のＡｌ−Ｆｅ系金属間化合物粒子の数密度は５００００個／ｍｍ２以下とするのが好ましい。 Coarse Al-Fe intermetallic compound particles with a particle size of 1.0 μm or more promote nucleation during recrystallization and make the crystal grains finer. However, if excessively present, pinholes are generated during rolling. Or the number density of Al—Fe-based intermetallic compound particles having a particle size of 1.0 μm or more is preferably 50,000 / mm 2 or less.
結晶粒が粗大であると、成形加工中に微視的な肌荒れが発生し、破断の起点となる。本発明においては、電界放射型電子銃をそなえた走査型電子顕微鏡を用いて、電子後方散乱解析像法（ＥＢＳＰ）による結晶方位解析で５°以上の方位差を有する境界を結晶粒界と規定し、該結晶粒界に囲まれる結晶粒について、結晶粒径の平均値Ｄが１２μｍ以下であることが望ましい。 If the crystal grains are coarse, microscopic rough skin is generated during the forming process, which becomes the starting point of fracture. In the present invention, using a scanning electron microscope equipped with a field emission electron gun, a boundary having an orientation difference of 5 ° or more in crystal orientation analysis by electron backscattering analysis image method (EBSP) is defined as a grain boundary. And about the crystal grain enclosed by this crystal grain boundary, it is desirable that the average value D of a crystal grain diameter is 12 micrometers or less.
また、結晶粒の平均粒径が小さくても、粗大な結晶粒が混在する組織（混粒組織）である場合、粗大な結晶粒に変形が集中し、破断の起点になる。したがって、上記の方位差５°以上で規定される粒界に囲まれる結晶粒径２０μｍ以上の結晶粒の面積率が３０％以下であることが好ましい。 In addition, even if the average grain size of the crystal grains is small, when the structure is a mixture of coarse crystal grains (mixed grain structure), deformation concentrates on the coarse crystal grains and becomes the starting point of fracture. Therefore, it is preferable that the area ratio of crystal grains having a crystal grain size of 20 μm or more surrounded by the grain boundaries defined by the orientation difference of 5 ° or more is 30% or less.
Ｆｅは金属間化合物として存在したとき結晶粒の微細化をもたらすが、固溶状態では成形加工中の加工硬化を促し、ネッキングによる破断を引き起こす。したがって、添加したＦｅ量に対し、固溶Ｆｅ原子が少ないほうがよく、２０℃における電気抵抗をＥ［ｎΩｍ］、Ｆｅ添加量をＣ［ｍａｓｓ％］としたとき、（Ｅ−２６．５）／Ｃの値が３．８以下であることが好ましい。 When Fe is present as an intermetallic compound, crystal grains are refined, but in a solid solution state, work hardening during forming is promoted, and fracture due to necking is caused. Therefore, it is better that the number of dissolved Fe atoms is less than the amount of Fe added. When the electrical resistance at 20 ° C. is E [nΩm] and the amount of Fe added is C [mass%], (E-26.5) / The value of C is preferably 3.8 or less.
次いで、本発明のアルミニウム合金箔の製造方法について説明すると、前記の組成を有するアルミニウム合金を溶解し、例えばＤＣ鋳造によって造塊する。得られた鋳塊を面削した後、鋳塊の溶質原子の成分偏析を取り除き、晶出物を球状化させるとともに、Ｆｅ含有金属間化合物粒子を粗大化させるため、均質化処理を行う。 Next, the manufacturing method of the aluminum alloy foil of the present invention will be described. The aluminum alloy having the above composition is melted and ingoted by DC casting, for example. After chamfering the obtained ingot, homogenization is performed in order to remove component segregation of solute atoms in the ingot, spheroidize the crystallized product, and coarsen the Fe-containing intermetallic compound particles.
均質化処理の好ましい温度は５００〜６２０℃であり、好ましい保持時間は１時間以上である。均質化処理温度が５００℃未満では、固溶元素の析出が不十分となり、成形性が低下し易い。６２０℃を超えると、鋳塊表層に膨れや部分的な溶融が発生して微小欠陥となり、成形加工中の破断の起点となる。また、均質化処理時間が１時間未満では、固溶元素の析出が不十分となり、成形性が低下し易い。加熱時間の上限は特に定めないが、生産効率の点から、通常は２４時間程度である。 The preferable temperature of the homogenization treatment is 500 to 620 ° C., and the preferable holding time is 1 hour or more. If the homogenization temperature is less than 500 ° C., precipitation of solid solution elements becomes insufficient, and the moldability tends to be lowered. When it exceeds 620 ° C., swelling or partial melting occurs in the ingot surface layer, resulting in a minute defect, which becomes a starting point of breakage during forming. Moreover, if the homogenization treatment time is less than 1 hour, the precipitation of the solid solution element becomes insufficient and the moldability tends to be lowered. The upper limit of the heating time is not particularly defined, but is usually about 24 hours from the viewpoint of production efficiency.
続いて熱間圧延を行う。熱間圧延は、リバース圧延の熱間粗圧延と、熱間粗圧延に引続き連続して３スタンドあるいは４スタンドにより一方向に圧延してコイルアップする熱間仕上圧延の組み合わせにより行う。熱間粗圧延においては、複数パスの熱間粗圧延を行って厚さ２０〜４０ｍｍとする。熱間粗圧延中の温度範囲は３５０〜５５０℃とするのが好ましい。３５０℃未満では熱間粗圧延中の回復および再結晶が不十分となり、５５０℃を超えると熱間粗圧延中に粗大な再結晶粒が形成し、いずれも最終箔における混粒組織の原因となる。 Subsequently, hot rolling is performed. Hot rolling is performed by a combination of hot rough rolling of reverse rolling and hot finish rolling that is rolled up in one direction by three or four stands and coiled up following the hot rough rolling. In hot rough rolling, hot rough rolling is performed in multiple passes to a thickness of 20 to 40 mm. The temperature range during hot rough rolling is preferably 350 to 550 ° C. If it is less than 350 ° C., recovery and recrystallization during hot rough rolling are insufficient, and if it exceeds 550 ° C., coarse recrystallized grains are formed during hot rough rolling, both of which are the cause of the mixed grain structure in the final foil. Become.
また、熱間粗圧延においては、板厚が１５０ｍｍ未満となった圧延パス間で、次の圧延を開始するまで３０秒以上保持する工程、すなわち次の圧延を開始するまで圧延材を３０秒以上待機させる工程を圧延中に１回以上含むことが好ましい。板厚が１５０ｍｍ以上の圧延パス間で３０秒以上保持する工程を行っても、内部まで均一な組織とならず、３０秒以上保持することにより逆に混粒組織が生じ易くなる。圧延パス間で３０秒以上保持する工程を１回も含まず、連続して複数パスの熱間粗圧延を終了した場合には、熱間粗圧延中の回復が不十分となり易く、最終箔に混粒組織が生じ易くなる。熱間粗圧延の最終パスの好ましい板厚減少率（加工度）は４０％以上である。板厚減少率が４０％未満では、加工組織の発達が不十分となり、最終箔の混粒組織の原因となる。 Further, in the hot rough rolling, the step of holding for 30 seconds or more until the next rolling is started between rolling passes where the plate thickness is less than 150 mm, that is, the rolling material is kept for 30 seconds or more until the next rolling is started. It is preferable that the step of waiting is included once or more during rolling. Even if a step of holding for 30 seconds or more between rolling passes having a plate thickness of 150 mm or more is performed, a uniform structure is not formed to the inside, and a mixed grain structure is easily generated by holding for 30 seconds or more. If the hot rough rolling of a plurality of passes is completed continuously without including a process of holding for 30 seconds or more between rolling passes, recovery during hot rough rolling tends to be insufficient, and the final foil A mixed grain structure is likely to occur. A preferable sheet thickness reduction rate (working degree) of the final pass of hot rough rolling is 40% or more. If the sheet thickness reduction rate is less than 40%, the development of the processed structure becomes insufficient, which causes the mixed grain structure of the final foil.
熱間粗圧延を終了後、出側温度を２００〜３８０℃とする熱間仕上圧延を行って厚さ１．６〜４．０ｍｍとし、続いて複数パスの冷間圧延により厚さ１０〜８０μｍとする。この場合、熱間仕上圧延後から冷間圧延のパス間に２５０〜４００℃で１時間以上の焼鈍を行ってもよい。所定の箔厚まで冷間圧延した後、２５０〜４００℃で１時間以上の最終焼鈍を行うことにより、本発明のアルミニウム合金箔が得られる。 After finishing the hot rough rolling, hot finish rolling is performed at a delivery temperature of 200 to 380 ° C. to a thickness of 1.6 to 4.0 mm, followed by cold rolling of multiple passes to a thickness of 10 to 80 μm. And In this case, after hot finish rolling, annealing may be performed at 250 to 400 ° C. for 1 hour or more between cold rolling passes. After cold rolling to a predetermined foil thickness, the aluminum alloy foil of the present invention is obtained by performing final annealing at 250 to 400 ° C. for 1 hour or more.
以下、本発明の実施例を比較例と対比して説明し、その効果を実証する。なお、これらの実施例は、本発明の好ましい一実施形態を説明するためのものであり、本発明はこれらに限定されない。 Examples of the present invention will be described below in comparison with comparative examples to demonstrate the effects. In addition, these Examples are for describing preferable one Embodiment of this invention, and this invention is not limited to these.
実施例１
表１に示す組成を有するアルミニウム合金（Ａ１〜Ａ１３）を常法により溶解し、半連続鋳造により造塊して、得られた鋳塊について、空気炉中で５５０℃で１０ｈの均質化処理を行った。その後、４７０℃より熱間粗圧延を開始し、圧延途中、板厚が１２０ｍｍとなった圧延パス間で３０秒以上保持する工程を１回行い、熱間粗圧延の最終パスの板厚減少率を５０％とし、終了温度が３５０〜４５０℃となるパススケジュールで熱間粗圧延を行った。
Example 1
Aluminum alloys (A1 to A13) having the composition shown in Table 1 are melted by a conventional method, ingot-formed by semi-continuous casting, and the obtained ingot is homogenized at 550 ° C. for 10 hours in an air furnace. went. Thereafter, hot rough rolling was started at 470 ° C., and during the rolling, the process of holding for 30 seconds or more between rolling passes where the plate thickness became 120 mm was performed once, and the plate thickness reduction rate of the final pass of hot rough rolling The hot rough rolling was performed with a pass schedule in which the end temperature was 350 to 450 ° C.
熱間粗圧延後、出側温度２１０〜２５０℃となるよう熱間仕上圧延を行い、２．５ｍｍの板材とした。次いで、冷間圧延により厚さ４０μｍの箔とし、３５０℃で１２ｈの最終焼鈍を行った。得られたアルミニウム合金箔を試験材（試験材１〜１３）として、以下に示す方法により特性を評価した。結果を表１に示す。 After the hot rough rolling, hot finish rolling was performed so that the outlet temperature was 210 to 250 ° C. to obtain a 2.5 mm plate. Next, a foil having a thickness of 40 μm was formed by cold rolling, and final annealing was performed at 350 ° C. for 12 hours. Using the obtained aluminum alloy foil as a test material (test materials 1 to 13), the characteristics were evaluated by the following methods. The results are shown in Table 1.
Ａｌ−Ｆｅ系金属間化合物の数密度（個／ｍｍ２）：試験材をペーパーおよびバフ研磨により鏡面仕上した後、電界放射型電子銃を備えた走査型電子顕微鏡により、加速電圧１０ｋＶにて１０００倍にて観察した写真を画像解析して測定した。解析には１０視野以上の写真を用い、画像解析した総面積は６×１０４μｍ２以上である。 Number density of Al—Fe-based intermetallic compound (pieces / mm 2 ): After the test material was mirror-finished by paper and buffing, it was 1000 at an acceleration voltage of 10 kV using a scanning electron microscope equipped with a field emission electron gun. The photograph observed at a magnification was subjected to image analysis and measured. For the analysis, photographs with 10 or more fields of view are used, and the total area of the image analysis is 6 × 10 4 μm 2 or more.
（Ｅ−２６．５）／Ｃ値の測定：試験材について、ＪＩＳ Ｈ０５０５に基づき、２０℃にて電気抵抗を測定し、（Ｅ−２６．５）／Ｃ値を算出した。 Measurement of (E-26.5) / C value: For the test material, the electrical resistance was measured at 20 ° C. based on JIS H0505, and (E-26.5) / C value was calculated.
結晶粒径：試験材について、ペーパーおよびバフ研磨により鏡面仕上した後、電界放射型電子銃を備えた走査型電子顕微鏡により、加速電圧１０ｋＶ、測定ステップサイズ０．１μｍにて、電子後方散乱解析像法（ＥＢＳＰ）による結晶方位解析を行い、解析結果より、５°以上の方位差を有する境界を結晶粒界と規定し、該結晶粒界に囲まれる結晶粒について結晶粒径を求め、平均値Ｄを算出した。また、円相当径が２０μｍを超える結晶粒の面積率を測定した。 Crystal grain size: The test material was mirror-finished by paper and buffing, and then an electron backscattering analysis image at an acceleration voltage of 10 kV and a measurement step size of 0.1 μm using a scanning electron microscope equipped with a field emission electron gun. The crystal orientation analysis by the method (EBSP) is performed, and the boundary having an orientation difference of 5 ° or more is defined as the crystal grain boundary based on the analysis result, the crystal grain size is obtained for the crystal grain surrounded by the crystal grain boundary, and the average value D was calculated. Further, the area ratio of crystal grains having an equivalent circle diameter exceeding 20 μm was measured.
成形性：試験材の両面にラミネート加工を施し、ナイロン２５μｍ／アルミニウム合金箔４０μｍ／ポリプロピレン５０μｍのラミネート箔を作製した。このラミネート箔のナイロン側を外面として、図１に示す形状のポンチ（幅５０ｍｍ×奥行き３０ｍｍ、Ｒ１．０ｍｍ）を用いて成形深さ５．０ｍｍのプレス成形を行い、成形可否により成形性を評価した。なお、プレスは成形速度を１０００ｍｍ／ｍｉｎとして無潤滑で行い、１条件につきｎ＝１０の試験を行って、全数が不具合無く成形できたものを合格（○）と評価し、破断を生じたものを不合格（×）と評価した。 Formability: Lamination was performed on both sides of the test material to prepare a laminate foil of nylon 25 μm / aluminum alloy foil 40 μm / polypropylene 50 μm. With the nylon side of this laminated foil as the outer surface, press forming with a forming depth of 5.0 mm is performed using a punch (width 50 mm × depth 30 mm, R 1.0 mm) shown in FIG. did. The press was made without lubrication at a molding speed of 1000 mm / min, and the test was performed with n = 10 per condition. Was evaluated as rejected (x).
比較例１
表２に示す組成を有するアルミニウム合金（Ａ１４〜Ａ２２）を常法により溶解し、実施例１と同様に造塊、均質化処理、熱間圧延、冷間圧延、最終焼鈍を行ってアルミニウム合金箔を作製し、これを試験材（試験材１４〜２２）として、実施例１と同じ方法により特性を評価した。結果を表２に示す。なお、表２において、本発明の条件を外れたものには下線を付した。
Comparative Example 1
Aluminum alloys (A14 to A22) having the compositions shown in Table 2 were melted by a conventional method, and ingot forming, homogenization treatment, hot rolling, cold rolling, and final annealing were performed in the same manner as in Example 1 to produce an aluminum alloy foil. Was used as a test material (test materials 14 to 22), and the characteristics were evaluated by the same method as in Example 1. The results are shown in Table 2. In Table 2, those outside the conditions of the present invention are underlined.
表１にみられるように、本発明に従う試験材１〜１３はいずれも、ラミネート箔として良好な成形性を示した。 As can be seen from Table 1, all of the test materials 1 to 13 according to the present invention exhibited good moldability as a laminate foil.
これに対して、表２に示すように、試験材１４はＦｅ含有量が少ないため、結晶粒が粗大となり成形時に破断が生じた。試験材１５はＦｅ含有量が多いため、１μｍ以上の金属間化合物粒子が増加し成形時に破断が生じた。試験材１６はＳｉ含有量が多いため、微細な金属間化合物が形成し、混粒組織となって成形時に破断が生じた。試験材１７はＭｎの含有量が多いため、微細な金属間化合物が形成し、混粒組織となって成形時に破断が生じた。 On the other hand, as shown in Table 2, since the test material 14 had a small Fe content, the crystal grains became coarse and fracture occurred during molding. Since the test material 15 had a large Fe content, intermetallic compound particles of 1 μm or more increased and fracture occurred during molding. Since the test material 16 had a large Si content, a fine intermetallic compound was formed, resulting in a mixed grain structure and fracture during molding. Since the test material 17 had a high Mn content, a fine intermetallic compound was formed, resulting in a mixed grain structure and fracture during molding.
試験材１８、試験材１９および試験材２０は、それぞれＭｇ、ＣｕおよびＺｎの固溶量が増し、熱延中の回復および再結晶を阻害し、混粒組織となって成形時に破断が生じた。試験材２１および試験材２２は、それぞれＴｉおよびＢの含有量が多いため、粗大な金属間化合物が形成し成形時に破断が生じた。 The test material 18, the test material 19 and the test material 20 increased in solid solution amounts of Mg, Cu and Zn, respectively, inhibited recovery and recrystallization during hot rolling, became a mixed grain structure, and fractured during molding. . Since the test material 21 and the test material 22 each had a large content of Ti and B, a coarse intermetallic compound was formed, and fracture occurred during molding.
実施例２
表１の合金Ａ３を常法により溶解し、半連続鋳造により造塊して、得られた鋳塊について、表３に示す製造条件で熱間粗圧延まで実施した後、出側温度２１０〜２５０℃となるよう厚さ２．５ｍｍまで熱間仕上圧延を行い、次いで、冷間圧延により厚さ４０μｍのアルミニウム合金箔とし、３５０℃で１２ｈの最終焼鈍を行った。なお、表３において、熱間粗圧延における圧延パス間の保持については、板厚が１２０ｍｍとなった圧延パス間で４０秒保持したものは（注１）、板厚が１２０ｍｍとなった圧延パス間で６０秒保持したものは（注２）、板厚が１２０ｍｍおよび１００ｍｍとなった圧延パス間でそれぞれ４０秒保持したものは（注３）で示した。得られたアルミニウム合金箔を試験材（試験材２３〜２８）として、実施例１と同様の方法で特性を評価した。評価結果を表３に示す。
Example 2
The alloy A3 in Table 1 was melted by a conventional method, ingot-formed by semi-continuous casting, and the resulting ingot was subjected to hot rough rolling under the production conditions shown in Table 3, and then the outlet temperature 210-250 Hot finish rolling was carried out to a thickness of 2.5 mm so as to be at 0 ° C., and then an aluminum alloy foil having a thickness of 40 μm was formed by cold rolling, followed by a final annealing at 350 ° C. for 12 hours. In Table 3, with regard to holding between rolling passes in hot rough rolling, the holding pass for 40 seconds between the rolling passes with a plate thickness of 120 mm (Note 1) is the rolling pass with a plate thickness of 120 mm. Those held for 60 seconds between (Note 2), and those held for 40 seconds between the rolling passes with the plate thickness of 120 mm and 100 mm are shown as (Note 3). Using the obtained aluminum alloy foil as a test material (test materials 23 to 28), the characteristics were evaluated in the same manner as in Example 1. The evaluation results are shown in Table 3.
比較例２
表１の合金Ａ３を常法により溶解し、半連続鋳造により造塊して、得られた鋳塊について、表４に示す製造条件で熱間粗圧延まで実施した後、出側温度２１０〜２５０℃となるよう厚さ２．５ｍｍまで熱間仕上圧延を行い、次いで、冷間圧延により厚さ４０μｍのアルミニウム合金箔とし、３５０℃で１２ｈの最終焼鈍を行った。得られたアルミニウム合金箔を試験材（試験材２９〜３６）として、実施例１と同様の方法で特性を評価した。評価結果を表４に示す。試験材３６については、熱間粗圧延において、板厚が２００ｍｍとなった圧延パス間で４０秒保持した（注４）。なお、表４において、本発明の条件を外れたものには下線を付した。
Comparative Example 2
The alloy A3 in Table 1 was melted by a conventional method, ingot-formed by semi-continuous casting, and the obtained ingot was subjected to hot rough rolling under the production conditions shown in Table 4, and then the outlet temperature 210-250 Hot finish rolling was carried out to a thickness of 2.5 mm so as to be at 0 ° C., and then an aluminum alloy foil having a thickness of 40 μm was formed by cold rolling, followed by a final annealing at 350 ° C. for 12 hours. Using the obtained aluminum alloy foil as a test material (test materials 29 to 36), the characteristics were evaluated in the same manner as in Example 1. The evaluation results are shown in Table 4. The test material 36 was held for 40 seconds between rolling passes with a plate thickness of 200 mm in hot rough rolling (Note 4). In Table 4, those outside the conditions of the present invention are underlined.
表３にみられるように、本発明に従う試験材２３〜２８はいずれも、ラミネート箔として良好な成形性を示した。 As can be seen in Table 3, all of the test materials 23 to 28 according to the present invention exhibited good moldability as a laminate foil.
これに対して、表４に示すように、試験材２９は均質化処理温度が低く、したがって析出が十分に進行せず、（Ｅ−２６．５）／Ｃの値が本発明の範囲外となり、成形性が低下した。試験材３０は均質化処理温度が高く、鋳塊表層にフクレを生じ、その結果、箔圧延時に箔切れを起こした。試験材３１は均質化処理時間が短く、析出が十分に進行せず、（Ｅ−２６．５）／Ｃの値が本発明の範囲外となり、成形性が低下した。 On the other hand, as shown in Table 4, the test material 29 has a low homogenization temperature, and therefore precipitation does not proceed sufficiently, and the value of (E-26.5) / C is outside the scope of the present invention. As a result, moldability decreased. The test material 30 had a high homogenization temperature, and blisters were generated on the ingot surface layer. As a result, foil breakage occurred during foil rolling. The test material 31 had a short homogenization time, precipitation did not proceed sufficiently, the value of (E-26.5) / C was outside the range of the present invention, and the moldability was reduced.
試験材３２は熱間粗圧延の温度が低く混粒組織となり、成形性が低下した。試験材３３は熱間粗圧延の温度が高く混粒組織となり、成形性が低下した。試験材３４は熱間粗圧延中の圧延パス間に３０秒以上保持する工程を含まないため混粒組織となり、成形性が低下した。試験材３５は熱間粗圧延の最終パスの加工度が低く混粒組織となり、成形性が低下した。試験材３６は、熱間粗圧延において、内部まで均一な加工組織となっていない板厚２００ｍｍの段階の圧延パス間で保持を行ったため混粒組織となり、成形性が低下した。 The test material 32 had a low temperature of hot rough rolling and had a mixed grain structure, and the formability decreased. The test material 33 had a high hot rough rolling temperature and a mixed grain structure, and the formability decreased. Since the test material 34 does not include the step of holding for 30 seconds or more between rolling passes during hot rough rolling, it became a mixed grain structure, and the formability deteriorated. The test material 35 had a low degree of processing in the final pass of the hot rough rolling and had a mixed grain structure, and the formability decreased. In the hot rough rolling, the test material 36 was held between rolling passes at a stage with a plate thickness of 200 mm, which was not a uniform processed structure up to the inside, so that it became a mixed grain structure, and the formability deteriorated.
Claims (3)
Priority Applications (5)
| Application Number | Priority Date | Filing Date | Title |
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| JP2012189605A JP5897430B2 (en) | 2012-08-30 | 2012-08-30 | Aluminum alloy foil excellent in formability after lamination, manufacturing method thereof, and laminate foil using the aluminum alloy foil |
| PCT/JP2013/067384 WO2014034240A1 (en) | 2012-08-30 | 2013-06-25 | Aluminum alloy foil with excellent formability after laminating, process for producing same, and laminated foil obtained using said aluminum alloy foil |
| KR1020157005129A KR20150046067A (en) | 2012-08-30 | 2013-06-25 | Aluminum alloy foil with excellent formability after laminating, process for producing same, and laminated foil obtained using said aluminum alloy foil |
| CN201380041988.XA CN104641011B (en) | 2012-08-30 | 2013-06-25 | The alloy foil having excellent formability and its manufacture method after lamination and the laminating foil using the alloy foil |
| TW102123762A TWI558551B (en) | 2012-08-30 | 2013-07-03 | An aluminum alloy foil having good formability after molding, a method of manufacturing the same, and a laminated foil using the aluminum alloy foil |
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| JP2012189605A JP5897430B2 (en) | 2012-08-30 | 2012-08-30 | Aluminum alloy foil excellent in formability after lamination, manufacturing method thereof, and laminate foil using the aluminum alloy foil |
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| JP6396067B2 (en) * | 2014-04-10 | 2018-09-26 | 株式会社Uacj | Aluminum alloy plate for bus bar and manufacturing method thereof |
| JP6496490B2 (en) * | 2014-04-16 | 2019-04-03 | 三菱アルミニウム株式会社 | Aluminum alloy soft foil and manufacturing method thereof |
| WO2015182624A1 (en) * | 2014-05-26 | 2015-12-03 | 古河電気工業株式会社 | Aluminum alloy conductor wire, aluminum alloy twisted wire, sheathed electrical cable, wire harness, and method for manufacturing aluminum alloy conductor wire |
| US10553327B2 (en) | 2014-05-26 | 2020-02-04 | Furukawa Electric Co., Ltd. | Aluminum alloy conductor wire, aluminum alloy stranded wire, coated wire, wire harness and method of manufacturing aluminum alloy conductor wire |
| BR112017000317B1 (en) * | 2014-07-09 | 2022-03-29 | Hydro Aluminium Rolled Products Gmbh | Method to produce an aluminum-plastic composite construction part and aluminum alloy |
| CN106191544B (en) * | 2016-08-10 | 2018-08-28 | 河南明泰铝业股份有限公司 | A kind of lithium battery 8021 Soft Roll aluminium foils and its production method |
| JP6792463B2 (en) * | 2017-01-19 | 2020-11-25 | 株式会社神戸製鋼所 | Aluminum alloy soft foil for molding |
| JP6461248B2 (en) | 2017-07-06 | 2019-01-30 | 三菱アルミニウム株式会社 | Aluminum alloy foil and method for producing aluminum alloy foil |
| JP6461249B2 (en) | 2017-07-06 | 2019-01-30 | 三菱アルミニウム株式会社 | Aluminum alloy foil and method for producing aluminum alloy foil |
| JP6754025B1 (en) * | 2018-12-26 | 2020-09-09 | 三菱アルミニウム株式会社 | Manufacturing method of aluminum alloy foil and aluminum alloy foil |
| WO2020189674A1 (en) | 2019-03-18 | 2020-09-24 | 東洋アルミニウム株式会社 | Aluminum alloy foil, laminate, method for manufacturing aluminum alloy foil, and method for manufacturing laminate |
| CN110867534A (en) * | 2019-10-09 | 2020-03-06 | 浙江华正能源材料有限公司 | Aluminum-plastic composite film |
| US20230022746A1 (en) * | 2019-12-25 | 2023-01-26 | Ma Aluminum Corporation | Aluminum alloy foil |
| CN215955369U (en) | 2020-06-09 | 2022-03-04 | 株式会社Lg化学 | Pouch film, pouch-type battery case, and pouch-type secondary battery |
| JPWO2022030620A1 (en) * | 2020-08-06 | 2022-02-10 | ||
| CN112251652B (en) * | 2020-10-22 | 2022-05-06 | 厦门厦顺铝箔有限公司 | Production method of aluminum foil for high-elongation lithium ion battery |
| EP4269639A4 (en) | 2020-12-25 | 2024-02-14 | Ma Aluminum Corp | Aluminum alloy foil |
| WO2022224615A1 (en) | 2021-04-22 | 2022-10-27 | Ｍａアルミニウム株式会社 | Aluminum alloy foil |
| CN113927973A (en) * | 2021-09-30 | 2022-01-14 | 江西睿捷新材料科技有限公司 | External packing material for high-depth-of-penetration battery device |
| CN114164361B (en) * | 2021-12-09 | 2022-10-25 | 厦门厦顺铝箔有限公司 | Production process of aluminum foil for high-ductility high-deep-drawing power aluminum plastic film |
| TWI830452B (en) | 2022-10-21 | 2024-01-21 | 財團法人工業技術研究院 | Aluminum alloy material, aluminum alloy object and method for manufacturing the same |
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| JPH0787928B2 (en) * | 1987-07-03 | 1995-09-27 | 古河電気工業株式会社 | Method for manufacturing aluminum foil |
| JP2686093B2 (en) * | 1988-05-06 | 1997-12-08 | 株式会社神戸製鋼所 | Aluminum alloy foil excellent in formability and method for producing the same |
| JP4015518B2 (en) * | 2002-05-07 | 2007-11-28 | 日本製箔株式会社 | Aluminum alloy foil, method for producing the same, and aluminum laminate |
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