JP2010150637A - Aluminum alloy foil for lithium ion battery electrode charge collector - Google Patents
Aluminum alloy foil for lithium ion battery electrode charge collector Download PDFInfo
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- 239000011888 foil Substances 0.000 title claims abstract description 65
- 229910000838 Al alloy Inorganic materials 0.000 title claims abstract description 48
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000012535 impurity Substances 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims abstract description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 abstract description 13
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 12
- 238000010438 heat treatment Methods 0.000 abstract description 9
- 239000011149 active material Substances 0.000 abstract description 8
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 238000005096 rolling process Methods 0.000 abstract description 7
- 239000000203 mixture Substances 0.000 abstract description 6
- 230000006866 deterioration Effects 0.000 abstract description 4
- 238000001035 drying Methods 0.000 abstract description 4
- 230000001105 regulatory effect Effects 0.000 abstract description 4
- 229910052719 titanium Inorganic materials 0.000 abstract description 3
- 238000007599 discharging Methods 0.000 abstract description 2
- 229910052742 iron Inorganic materials 0.000 abstract description 2
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 21
- 238000000137 annealing Methods 0.000 description 15
- 238000005097 cold rolling Methods 0.000 description 15
- 238000005098 hot rolling Methods 0.000 description 12
- 239000000463 material Substances 0.000 description 10
- 239000003921 oil Substances 0.000 description 10
- 238000001556 precipitation Methods 0.000 description 8
- 239000010949 copper Substances 0.000 description 7
- 230000003746 surface roughness Effects 0.000 description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- 239000013078 crystal Substances 0.000 description 6
- 239000010936 titanium Substances 0.000 description 5
- 239000002131 composite material Substances 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 4
- 238000000265 homogenisation Methods 0.000 description 4
- 239000011572 manganese Substances 0.000 description 4
- 239000010731 rolling oil Substances 0.000 description 4
- 238000011282 treatment Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000011255 nonaqueous electrolyte Substances 0.000 description 3
- 239000007774 positive electrode material Substances 0.000 description 3
- 229910018084 Al-Fe Inorganic materials 0.000 description 2
- 229910018192 Al—Fe Inorganic materials 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 239000006258 conductive agent Substances 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 229910052733 gallium Inorganic materials 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 229910000765 intermetallic Inorganic materials 0.000 description 2
- 229910052745 lead Inorganic materials 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000007773 negative electrode material Substances 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910052718 tin Inorganic materials 0.000 description 2
- 229910052720 vanadium Inorganic materials 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910002551 Fe-Mn Inorganic materials 0.000 description 1
- 101000993059 Homo sapiens Hereditary hemochromatosis protein Proteins 0.000 description 1
- KLARSDUHONHPRF-UHFFFAOYSA-N [Li].[Mn] Chemical compound [Li].[Mn] KLARSDUHONHPRF-UHFFFAOYSA-N 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- CKFRRHLHAJZIIN-UHFFFAOYSA-N cobalt lithium Chemical compound [Li].[Co] CKFRRHLHAJZIIN-UHFFFAOYSA-N 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 238000009749 continuous casting Methods 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000002035 hexane extract Substances 0.000 description 1
- RSNHXDVSISOZOB-UHFFFAOYSA-N lithium nickel Chemical compound [Li].[Ni] RSNHXDVSISOZOB-UHFFFAOYSA-N 0.000 description 1
- SWAIALBIBWIKKQ-UHFFFAOYSA-N lithium titanium Chemical compound [Li].[Ti] SWAIALBIBWIKKQ-UHFFFAOYSA-N 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000002480 mineral oil Substances 0.000 description 1
- 235000010446 mineral oil Nutrition 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Cell Electrode Carriers And Collectors (AREA)
Abstract
Description
本発明は、リチウムイオン電池電極集電体用アルミニウム合金箔、詳しくは、非水電解質二次電池電極（正極）集電体用アルミニウム箔、より詳しくは、電極製造時の電極用活物質の塗布性に優れ、電極捲回時に破断し難く、電池となった後の充放電による電極の膨張収縮による電極劣化や破断に対しても優れたサイクル特性を有する非水電解質二次電池電極（正極）集電体用アルミニウム箔に関する。 The present invention relates to an aluminum alloy foil for a lithium ion battery electrode current collector, more specifically, an aluminum foil for a non-aqueous electrolyte secondary battery electrode (positive electrode) current collector, more specifically, application of an electrode active material during electrode production. Non-aqueous electrolyte secondary battery electrode (positive electrode) that has excellent cycle characteristics, is resistant to breakage when wound, and has excellent cycle characteristics against electrode deterioration and breakage due to expansion and contraction of the electrode due to charge and discharge after the battery is formed The present invention relates to an aluminum foil for a current collector.
リチウムイオン二次電池の形状としては円筒型と角型があり、いずれも正極と負極がセパレータを介して捲回された極板群からなり、これを電池ケース内へ挿入し、非水電解質を注入して、封口した構造となっている。 There are two types of lithium ion secondary batteries: a cylindrical type and a square type, both of which consist of an electrode plate group in which a positive electrode and a negative electrode are wound with a separator interposed therebetween. Injected and sealed structure.
正極活物質としては、リチウムコバルト複合酸化物、リチウムニッケル複合酸化物、リチウムマンガン複合酸化物、リチウムチタン複合酸化物若しくは、前記正極活物質を数種組み合わせた混合品が用いられ、負極活物質としてはコークスや黒鉛等のリチウムイオンを吸脱着できる炭素材料が用いられている。 As the positive electrode active material, a lithium cobalt composite oxide, a lithium nickel composite oxide, a lithium manganese composite oxide, a lithium titanium composite oxide, or a mixed product obtained by combining several kinds of the positive electrode active materials is used. Carbon materials that can adsorb and desorb lithium ions such as coke and graphite are used.
これらの正極活物質または負極活物質は、バインダーと、必要に応じてアセチレンブラックや黒鉛などの導電剤および溶媒を加えて撹拌・混合し、練合物になったものをアルミニウムや銅などの金属箔からなる集電体へ塗布し、乾燥後、圧延を行ない、圧延中もしくは圧延前後で熱処理を行い結着力を向上させ、所定寸法に裁断することでシート状に成形し、リチウムイオン二次電池の電極とする（特許文献１参照）。 These positive electrode active materials or negative electrode active materials are prepared by adding a binder and, if necessary, a conductive agent and a solvent such as acetylene black and graphite, stirring and mixing them, and forming a kneaded material such as aluminum or copper. Lithium ion secondary battery is applied to a current collector made of foil, dried, rolled, heat treated during or before and after rolling to improve the binding force, and cut into a predetermined size to form a sheet. (Refer to Patent Document 1).
正極集電体用アルミニウム箔に関しては、１回以上の充電を行った後の巻回方向における破断までの伸び率が３％以上のアルミニウム箔を用いることにより、負極活物質の膨張収縮の繰り返しにより充放電サイクル中に正極が劣化したり破断することを防止し、サイクル特性を向上させることが提案されている（特許文献２参照）。
しかしながら、伸び率が３％以上のアルミニウム箔を用いる場合には、活物質塗布、乾燥後の圧延に耐える引張強さが必要となり、また前記伸び率を確保するために、箔の厚みを厚くしなければならず、電池の容量が低下してしまうという問題がある。 However, when an aluminum foil having an elongation of 3% or more is used, it is necessary to have a tensile strength that can withstand rolling after applying an active material and drying, and in order to ensure the elongation, the thickness of the foil is increased. There is a problem that the capacity of the battery is reduced.
本発明は、上記の問題を解消するためになされたものであり、その目的は、電極製造時における活物質の塗布、乾燥、圧延時には十分な引張強さを有し、その後２００℃以下の比較的低い温度で熱処理することにより、セパレータを介して正極と負極の巻回時、さらに電極として電池に組込まれた時には、十分な延びを有し、電池として充放電を繰り返した場合においても、正極が劣化したり破断することを防止でき、電池のサイクル寿命を十分なものとすることを可能とするリチウムイオン電池電極集電体用アルミニウム箔を提供することにある。 The present invention has been made to solve the above-mentioned problems, and its purpose is to have a sufficient tensile strength at the time of application, drying and rolling of an active material during electrode production, and thereafter a comparison of 200 ° C. or lower. When the positive electrode and the negative electrode are wound through the separator and further incorporated into the battery as an electrode, the positive electrode has a sufficient extension and is repeatedly charged and discharged as a battery. It is an object of the present invention to provide an aluminum foil for a lithium ion battery electrode current collector that can prevent deterioration and breakage of the battery and can make the cycle life of the battery sufficient.
上記の目的を達成するための請求項１によるリチウムイオン電池電極集電体用アルミニウム合金箔は、Ｆｅ：０．８〜２．０％、Ｔｉ：０．０２％以下を含有し、不純物としてのＳｉを０．１５％以下、Ｃｕを０．０５％以下に規制し、残部Ａｌおよびその他の不可避不純物からなるアルミニウム合金箔であって、引張強度が１６０ＭＰａ以上で、ダブルブリッジ法により液体窒素中で測定した電気抵抗が０．５５μΩｃｍ以下であることを特徴とする。 An aluminum alloy foil for a lithium ion battery electrode current collector according to claim 1 for achieving the above object contains Fe: 0.8 to 2.0%, Ti: 0.02% or less, It is an aluminum alloy foil comprising Si and 0.15% or less, Cu and 0.05% or less, the balance Al and other inevitable impurities, the tensile strength is 160 MPa or more, in liquid nitrogen by the double bridge method The measured electric resistance is 0.55 μΩcm or less.
請求項２によるリチウムイオン電池電極集電体用アルミニウム合金箔は、請求項１または２において、前記アルミニウム合金箔が、さらにＭｎ：０．０５％以下を含有することを特徴とする。 The aluminum alloy foil for a lithium ion battery electrode current collector according to claim 2 is characterized in that, in claim 1 or 2, the aluminum alloy foil further contains Mn: 0.05% or less.
請求項３によるリチウムイオン電池電極集電体用アルミニウム合金箔は、請求項１〜３のいずれかにおいて、厚さが１０〜３０μｍであることを特徴とする。 The aluminum alloy foil for a lithium ion battery electrode current collector according to claim 3 is characterized in that in any one of claims 1 to 3, the thickness is 10 to 30 μm.
本発明によれば、電極製造時の電極用活物質の塗布性に優れ、電極製造の塗布、乾燥、圧延時には十分な引張強さを有し、その後２００℃以下の比較的低い温度で熱処理することにより、セパレータを介して正極と負極の巻回時、さらに電極として電池に組込まれた時には、十分な延びを有し、破断し難く、電池として充放電を繰り返した場合においても、電極の膨張収縮による電極劣化や破断を防止することができ、電池のサイクル寿命を十分なものとすることができるリチウムイオン電池電極集電体用アルミニウム合金箔が提供される。 According to the present invention, it is excellent in the application property of the electrode active material at the time of electrode production, has sufficient tensile strength at the time of application, drying and rolling of electrode production, and then heat-treated at a relatively low temperature of 200 ° C. or less. Thus, when the positive electrode and the negative electrode are wound through the separator, and further assembled into the battery as an electrode, the electrode has sufficient extension, is not easily broken, and the electrode expands even when charging and discharging are repeated as the battery. Provided is an aluminum alloy foil for a lithium ion battery electrode current collector, which can prevent electrode deterioration and breakage due to shrinkage and can make the cycle life of the battery sufficient.
本発明によるリチウムイオン電池電極集電体用アルミニウム合金箔を用いることにより、製造歩留りが向上し、十分なサイクル寿命を有する非水電解質二次電池を製造することができる。 By using the aluminum alloy foil for a lithium ion battery electrode current collector according to the present invention, the production yield is improved and a nonaqueous electrolyte secondary battery having a sufficient cycle life can be produced.
本発明のアルミニウム合金箔における合金成分の意義および限定理由について説明する。
Ｆｅは強度向上のために機能する。Ｆｅの好ましい含有量は０．８〜２．０％の範囲であり、０．８％未満では十分な引張強さが確保できなくなり、２．０％を超えて含有されると、Ａｌ成分との間で局部電池が形成されて腐食反応が進み耐食性が低下する。Ｆｅのより好ましい含有量は１．２〜１．７％、さらに好ましい含有量は１．４〜１．６％の範囲である。
The significance and reasons for limitation of the alloy components in the aluminum alloy foil of the present invention will be described.
Fe functions to improve strength. The preferable content of Fe is in the range of 0.8 to 2.0%, and if it is less than 0.8%, sufficient tensile strength cannot be ensured. A local battery is formed between them, and the corrosion reaction proceeds and the corrosion resistance decreases. A more preferable content of Fe is 1.2 to 1.7%, and a more preferable content is 1.4 to 1.6%.
Ｔｉはアルミニウム合金箔の結晶粒を微細化する。Ｔｉの好ましい含有量は０．０２％以下の範囲であり、０．０２％を超えて含有すると、アルミニウム合金箔のピンホールの原因となることがある。ＢはＴｉと共に添加して同様の効果を得ることができる。アルミニウム合金箔中のＢの含有量は、同様の理由で、０．０１重量％以下とするのが好ましい。 Ti refines the crystal grains of the aluminum alloy foil. The preferable content of Ti is in the range of 0.02% or less, and if it exceeds 0.02%, it may cause pinholes in the aluminum alloy foil. B can be added together with Ti to obtain the same effect. For the same reason, the content of B in the aluminum alloy foil is preferably 0.01% by weight or less.
Ｓｉは不純物として含有するが、Ｓｉ含有量が多いと、Ｓｉを含む化合物や単体Ｓｉが析出して再結晶が促進され過ぎ、結晶粒径が粗大となってピンホールの発生が多くなるとともに、Ａｌ成分との間で局部電池を形成して腐食反応が進み耐食性が低下するため、０．１５％以下に規制するのが好ましい。より好ましくは０．０８％以下とする。 Although Si is contained as an impurity, if the Si content is large, a compound containing Si or simple substance Si is precipitated and recrystallization is promoted too much, and the crystal grain size becomes coarse and the generation of pinholes increases. Since a local battery is formed with the Al component and the corrosion reaction proceeds and the corrosion resistance is lowered, the content is preferably regulated to 0.15% or less. More preferably, it is 0.08% or less.
Ｃｕは強度を向上させる元素であるが、Ｃｕ含有量が多いと、固溶Ｃｕ量が多くなり、固溶できなくなったＡｌ−Ｆｅ化合物が冷間圧延工程において急激に析出し、結果として、アルミニウム合金箔の平均結晶粒径が大きくなって、アルミニウム合金箔のピンホール数が多くなるため、０．０５％以下に規制するのが好ましい。より好ましくは０．０１％以下とする。 Cu is an element that improves the strength. However, when the Cu content is large, the amount of solid solution Cu increases, and the Al-Fe compound that cannot be solid solution precipitates rapidly in the cold rolling process. Since the average crystal grain size of the alloy foil is increased and the number of pinholes in the aluminum alloy foil is increased, it is preferably regulated to 0.05% or less. More preferably, the content is 0.01% or less.
Ｍｎは強度を向上させるよう機能するが、０．０５％を超えて含有すると粗大なＡｌ−Ｆｅ−Ｍｎ系の金属間化合物が形成しやすくなり、ピンホールが発生し易くなるので、Ｍｎの好ましい含有量は０．０１％以下とする。 Mn functions to improve strength, but if it exceeds 0.05%, a coarse Al—Fe—Mn intermetallic compound is likely to be formed, and pinholes are likely to be generated. The content is 0.01% or less.
アルミニウム合金箔には、Ｆｅ、Ｔｉ、Ｂ、Ｓｉ、Ｃｕ、Ｍｎ及びＡｌの他に、Ｍｇ、Ｚｎ、Ｇａ、Ｎｉ、Ｃｒ、Ｓｎ、Ｐｂ、Ｖなどの不可避不純物が含有されている。Ｚｎ、Ｇａ、Ｎｉ、Ｃｒ、Ｓｎ、Ｐｂ、Ｖの含有は、それぞれ０．０２％以下とするのが好ましく、さらに好ましくは、それぞれ０．０１％以下とする。また、Ｍｇについては、含有量が多くなると、Ｍｇがアルミニウム素地とアルミニウム酸化皮膜との界面に濃縮してＭｇＯ層が形成され、このＭｇＯ層がウィークバウンダリーレイヤーとなってアルミニウム合金箔との接着性を低下させるため、０．００５％以下に限定するのが好ましい。より好ましくは０．００３％以下とする。 In addition to Fe, Ti, B, Si, Cu, Mn, and Al, the aluminum alloy foil contains inevitable impurities such as Mg, Zn, Ga, Ni, Cr, Sn, Pb, and V. The contents of Zn, Ga, Ni, Cr, Sn, Pb, and V are each preferably 0.02% or less, and more preferably 0.01% or less. As for Mg, when the content increases, Mg concentrates at the interface between the aluminum base and the aluminum oxide film to form an MgO layer. This MgO layer becomes a weak boundary layer and adheres to the aluminum alloy foil. In order to reduce the property, the content is preferably limited to 0.005% or less. More preferably, it is 0.003% or less.
本発明のアルミニウム合金箔は、電気抵抗を０．５５μΩｃｍ以下とする必要がある。これは、アルミニウム合金箔中に微細な多数のＡｌ−Ｆｅ系金属間化合物を分散させ、結晶粒の微細化や強度を向上させるとともに、２００℃以下の比較的低い温度での熱処理によって３％以上の大きな伸びを得るためである。さらに大きな伸びを得るためには、電気抵抗を０．５０μΩｃｍ以下とするのがより好ましい。 The aluminum alloy foil of the present invention needs to have an electric resistance of 0.55 μΩcm or less. This is because a large number of fine Al—Fe intermetallic compounds are dispersed in the aluminum alloy foil to improve crystal grain refinement and strength, and at least 3% by heat treatment at a relatively low temperature of 200 ° C. or less. This is to obtain a large growth. In order to obtain a larger elongation, the electric resistance is more preferably 0.50 μΩcm or less.
電気抵抗の測定は，箔厚×３ｍｍ幅×２３０ｍｍ長さに成形して試料を作製し、マイクロメーターで厚みを測定し、四端子をスポット溶接後、ダブルブリッジ法を用いて液体窒素中で試料抵抗を測定した後に、比抵抗（電気抵抗）を計算することにより行う。 The electrical resistance is measured by forming a foil thickness x 3 mm width x 230 mm length, preparing a sample, measuring the thickness with a micrometer, spot welding the four terminals, and then using the double bridge method in liquid nitrogen After measuring the resistance, the specific resistance (electrical resistance) is calculated.
本発明のアルミニウム合金箔はまた、引張強度を１６０ＭＰａ以上とする必要がある。これは、アルミニウム合金箔に活物質を塗布、乾燥した後、活物質の密度向上と集電体への密着などを目的とするロールプレスによる圧着工程において、箔の塑性変形により活物質の剥離などが生じるのを防止するためである。 The aluminum alloy foil of the present invention also needs to have a tensile strength of 160 MPa or more. This is because the active material is applied to the aluminum alloy foil and dried, and then the active material is peeled off by plastic deformation of the foil in a press-bonding process with a roll press for the purpose of improving the density of the active material and adhering to the current collector. This is to prevent the occurrence of.
また、上記アルミニウム合金箔においては、その厚さは通常１０〜３０μｍである。リチウムイオン電池電極集電体用としては、厚さ１０〜１５μｍとするのがより好ましい。 Moreover, in the said aluminum alloy foil, the thickness is 10-30 micrometers normally. For a lithium ion battery electrode current collector, the thickness is more preferably 10 to 15 μm.
アルミニウム合金箔の表面粗度Ｒａは、０．０８〜０．３０μｍとするのが好ましい。表面粗度Ｒａが大きいと、アルミニウム合金箔にピンホールが生じ易くなり、また、又、表面粗度Ｒａが小さいと、活物質、バインダー、導電剤および溶媒などの練合物の密着性が低下する。アルミニウム合金箔の表面粗度Ｒａは、０．１２〜０．２５μｍがさらに好ましい。 The surface roughness Ra of the aluminum alloy foil is preferably 0.08 to 0.30 μm. If the surface roughness Ra is large, pinholes are likely to occur in the aluminum alloy foil, and if the surface roughness Ra is small, the adhesion of the kneaded material such as the active material, binder, conductive agent and solvent decreases. To do. The surface roughness Ra of the aluminum alloy foil is more preferably 0.12 to 0.25 μm.
表面粗度Ｒａは、ＪＩＳ Ｂ０６０１−２００１に準拠して測定されたものであり、具体的には、アルミニウム合金箔の幅方向の表面粗度Ｒａは、アルミニウム合金箔の表面において、幅方向に任意５点の表面粗度Ｒａを測定し、その平均値をいう。 The surface roughness Ra is measured in accordance with JIS B0601-2001. Specifically, the surface roughness Ra in the width direction of the aluminum alloy foil is arbitrary in the width direction on the surface of the aluminum alloy foil. The surface roughness Ra of 5 points is measured and the average value is referred to.
また、アルミニウム合金箔表面における圧延油などの油分の除去が不十分であると、上記練合物の密着性が低下するのばかりでなく、電池として充放電を繰り返した場合、活物質層（電極合剤層）と終電体との密着性が低下するので、残留油分量は１４０μｇ／ｍ２以下とするのが好ましい。 In addition, if the removal of oil such as rolling oil on the aluminum alloy foil surface is insufficient, not only the adhesion of the kneaded material is lowered, but also when the battery is repeatedly charged and discharged, the active material layer (electrode Since the adhesion between the mixture layer) and the final electrode is reduced, the residual oil content is preferably 140 μg / m 2 or less.
本発明のアルミニウム合金箔は、所定の組成を有するアルミニウム合金の鋳塊に均質化処理、熱間圧延、冷間圧延、必要に応じて最終焼鈍を施すことにより製造されるが、通常、冷間圧延後のアルミニウム合金箔表面には圧延油が残存し、鉱油、脂肪酸、エステルなどの圧延油成分が検出される。箔表面における圧延油の残存状態は、アルミニウム表面の外層部に位置する付着油と、その内層部に位置しアルミニウム素地との結合力がきわめて高い吸着油とに分類できる。付着油はヘキサンに溶解する油成分であり、吸着油は箔表面の油分をヘキサンで抽出しても残存する油分として定義付けできる。 The aluminum alloy foil of the present invention is produced by subjecting an ingot of aluminum alloy having a predetermined composition to homogenization treatment, hot rolling, cold rolling, and final annealing as necessary. Rolling oil remains on the surface of the aluminum alloy foil after rolling, and rolling oil components such as mineral oil, fatty acid, and ester are detected. The remaining state of the rolling oil on the foil surface can be classified into adhering oil located in the outer layer portion of the aluminum surface and adsorbed oil located in the inner layer portion and having a very high bonding force with the aluminum substrate. Adhering oil is an oil component that dissolves in hexane, and adsorbed oil can be defined as oil that remains even if the oil on the foil surface is extracted with hexane.
吸着油の抽出方法は、以下のようにして行う。
箔表面積約４００ｃｍ２をヘキサン（５０００倍濃縮検定品）８０ｍｌ中に浸漬し、２０分間超音波洗浄を実施する。ヘキサン抽出後の箔を蒸留水９０ｍｌ、ヘキサン３０ｍｌおよび６Ｎ塩酸(ヘキサン洗浄塩酸)３０ｍｌを加え、アルミの分解反応がおさまるまで放置し、さらに６Ｎ塩酸１０ｍｌを加え、箔の表面が完全に分解するまで放置する。次に、蒸留水４０ｍｌを加え、ガラス製のスポイトでヘキサン抽出液を、１００ｍｌビーカーに移し入れ、抽出液が約２０ｍｌになるまで加熱蒸発させ、さらに室温で約５ｍｌまで蒸発させる。その後、吸引デシケーターで減圧濃縮し、ヘキサンを完全に蒸発させ、箔表面吸着物質を得る。これをヘキサン１００μｌで溶解し、その４μｌをガスクロマトグラフに注入する。ガスクロマトグラフ分析条件は以下のとおりである。
装置：島津製 ＧＣ−１４Ｂ
カラム：Ｇカラム Ｇ−２０５ ４０ｍ
カラム温度：７０℃→２７０℃ １０℃／ｍｉｎ １０ｍｉｎ保持
検出器：ＦＩＤ
検出器温度：３２０℃
注入口温度：３２０℃
キャリヤガス：Ｎ２ ３０ｍｌ／ｍｉｎ
ＲＡＮＧＥ：１０１ ＡＴＴ５
The extraction method of adsorbed oil is performed as follows.
A surface area of about 400 cm 2 of foil is immersed in 80 ml of hexane (5000-fold concentrated assay product) and subjected to ultrasonic cleaning for 20 minutes. Add 90 ml of distilled water, 30 ml of hexane and 30 ml of 6N hydrochloric acid (hexane-washed hydrochloric acid) to the foil after extraction with hexane, and let stand until the decomposition reaction of aluminum stops, and then add 10 ml of 6N hydrochloric acid until the foil surface is completely decomposed. put. Next, 40 ml of distilled water is added, and the hexane extract is transferred to a 100 ml beaker with a glass dropper, heated and evaporated until the extract reaches about 20 ml, and further evaporated to about 5 ml at room temperature. Then, it concentrate | evaporates under reduced pressure with a suction desiccator, hexane is evaporated completely, and foil surface adsorption | suction substance is obtained. This is dissolved in 100 μl of hexane, and 4 μl thereof is injected into a gas chromatograph. Gas chromatographic analysis conditions are as follows.
Equipment: GC-14B made by Shimadzu
Column: G column G-205 40m
Column temperature: 70 ° C. → 270 ° C. 10 ° C./min 10 min holding Detector: FID
Detector temperature: 320 ° C
Inlet temperature: 320 ° C
Carrier gas: N2 30ml / min
RANGE: 101 ATT5
つぎに、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。
前記組成を有するアルミニウム合金を溶解し、公知の半連続鋳造法により造塊する。アルミニウム合金箔の電気抵抗を０．５５μΩｃｍ以下とし、強度を確保するために、得られた鋳塊を均質化処理し、固溶している合金元素を微細に析出させる。均質化処理は４６０〜５２０℃の温度で８〜２０時間保持するのが好ましい。４６０℃より低い温度または８ｈｒより短い時間では均質化処理が不十分となり、５２０℃を超えると十分な析出得られない。また、２０ｈｒを越えて均質化処理をしてもその効果は変らない。
Below, the manufacturing method of the aluminum alloy foil of this invention is demonstrated.
An aluminum alloy having the above composition is melted and ingot-formed by a known semi-continuous casting method. In order to set the electric resistance of the aluminum alloy foil to 0.55 μΩcm or less and ensure the strength, the obtained ingot is homogenized to finely precipitate the dissolved alloy elements. The homogenization treatment is preferably held at a temperature of 460 to 520 ° C. for 8 to 20 hours. If the temperature is lower than 460 ° C. or shorter than 8 hours, the homogenization treatment is insufficient, and if it exceeds 520 ° C., sufficient precipitation cannot be obtained. Moreover, the effect does not change even if the homogenization treatment is performed over 20 hours.
続いて、熱間圧延を行う。熱間圧延は、熱間加工中にさらにＦｅの微細析出を促進させ、アルミニウム合金箔の電気抵抗を０．５５μΩｃｍ以下とし、さらに強度と低温熱処理後の十分な伸びを確保するために、４００〜４５０℃で開始し、２００〜２５０℃で終了するのが好ましい。熱間圧延後、コイルとて巻き取る。 Subsequently, hot rolling is performed. The hot rolling further promotes fine precipitation of Fe during hot working, makes the electric resistance of the aluminum alloy foil 0.55 μΩcm or less, and further ensures strength and sufficient elongation after low-temperature heat treatment. It is preferred to start at 450 ° C and end at 200-250 ° C. After hot rolling, it is wound up as a coil.
また、熱間圧延後、加工度４０〜６０％の冷間圧延を行って析出サイトとなる加工歪を導入したのち第１回目の中間焼鈍を行い、その後冷間圧延し第２回目の中間焼鈍を施して、さらに冷間圧延するのが望ましく、中間焼鈍条件は、第１回目、第２回目ともに、３００〜４００℃で１〜５時間とするのが好ましい。 In addition, after hot rolling, cold rolling at a working degree of 40 to 60% is performed to introduce a working strain that becomes a precipitation site, and then the first intermediate annealing is performed, and then cold rolling is performed and the second intermediate annealing is performed. The intermediate annealing conditions are preferably 300 to 400 ° C. for 1 to 5 hours in both the first and second rounds.
熱間圧延後の熱延コイルにおいては、析出、組織ともに不均一で、そのまま冷間圧延を行うと、不均一な析出が生じ易く、また組織の均一化も得られ難いため、そのまま冷間圧延を継続した場合には、不均一組織部においてピンホールが生じ易くなる。 In hot-rolled coils after hot rolling, both precipitation and structure are non-uniform. If cold rolling is performed as it is, non-uniform precipitation is likely to occur and it is difficult to obtain uniform structure. When this is continued, pinholes are likely to occur in the non-uniform tissue portion.
本発明においては、熱間圧延後、加工度４０〜６０％の冷間圧延を行い、その後中間焼鈍を行う。熱間圧延後できるだけ早く冷間圧延し、中間焼鈍を行うのが好ましい。熱間圧延後６０％を越える冷間圧延を施して中間焼鈍すると、形成された不均一な冷間圧延組織が均一化し難い。熱間圧延後、加工度４０〜６０％の冷間圧延を行い、その後第１回目の中間焼鈍を施して冷間圧延を行い、第２回目の中間焼鈍を施して、さらに冷間圧延、箔圧延することによって、析出量が多く、加工により転位が均一に導入されているため析出形態も微細且つ均一となる。 In the present invention, after hot rolling, cold rolling with a work degree of 40 to 60% is performed, and then intermediate annealing is performed. It is preferable to cold-roll as soon as possible after hot rolling and to perform intermediate annealing. When cold rolling exceeding 60% is performed after hot rolling and intermediate annealing is performed, the formed non-uniform cold rolling structure is difficult to homogenize. After the hot rolling, cold rolling with a work degree of 40 to 60% is performed, then the first intermediate annealing is performed to perform cold rolling, the second intermediate annealing is performed, and further cold rolling and foil are performed. By rolling, the amount of precipitation is large, and dislocations are introduced uniformly by processing, so that the precipitation form becomes fine and uniform.
上記の工程を経たアルミニウム合金箔の引張強さは１６０ＭＰａ以上となり、さらに、１７０℃で５分間の低温熱処理を行うことにより、厚さ１５μｍ程度の箔であっても３％以上の大きな伸びを得ることができる。 The tensile strength of the aluminum alloy foil that has undergone the above steps is 160 MPa or more. Further, by performing a low-temperature heat treatment at 170 ° C. for 5 minutes, a large elongation of 3% or more is obtained even for a foil having a thickness of about 15 μm. be able to.
以下、本発明の実施例を比較例と対比して説明し、本発明の効果を実証する。これらの実施例は本発明の一実施態様を示すものであり、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 of the present invention. These examples show one embodiment of the present invention, and the present invention is not limited thereto.
実施例１、比較例１
表１に示すＡ〜Ｋの組成を有するアルミニウム合金を溶製し、ＤＣ鋳造法により鋳造速度４０ｍｍ／分で厚さ５００ｍｍのスラブを造塊した。得られたスラブを４８０℃で１２時間均質化処理した後、開始温度４００℃、終了温度２５０℃の熱間圧延を行い、厚さ４ｍｍの板を得た。
Example 1 and Comparative Example 1
Aluminum alloys having compositions A to K shown in Table 1 were melted, and a slab having a thickness of 500 mm was ingoted at a casting speed of 40 mm / min by a DC casting method. The obtained slab was homogenized at 480 ° C. for 12 hours, and then hot rolled at a start temperature of 400 ° C. and an end temperature of 250 ° C. to obtain a plate having a thickness of 4 mm.
続いて、上記熱間圧延板に冷間圧延を複数回繰り返し施して、厚さ１５μｍのアルミニウム合金箔を得た。なお、冷間圧延の途中で、板厚が２ｍｍのときに、３００℃で２時間の第一回目の中間焼鈍を行い、板厚が０．５ｍｍのときに、３００℃で２時間の第二回目の中間焼鈍を実施した。 Subsequently, cold rolling was repeated a plurality of times on the hot rolled sheet to obtain an aluminum alloy foil having a thickness of 15 μm. During the cold rolling, when the plate thickness is 2 mm, the first intermediate annealing is performed at 300 ° C. for 2 hours, and when the plate thickness is 0.5 mm, the second annealing is performed at 300 ° C. for 2 hours. A second intermediate annealing was performed.
得られたアルミニウム合金箔について、引張強度、電気抵抗を測定した、さらに１７０℃で５分間の低温熱処理を行った後、引張強度、伸びを測定した。測定結果を表２に示す。なお、表１、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。 The obtained aluminum alloy foil was measured for tensile strength and electrical resistance, and further subjected to low-temperature heat treatment at 170 ° C. for 5 minutes, and then measured for tensile strength and elongation. The measurement results are shown in Table 2. In Tables 1 and 2, those outside the conditions of the present invention are underlined.
表２に示すように、本発明に従う試験材１〜５はいずれも、電気抵抗値が０．５５μΩｃｍ以下であり、１６０ＭＰａ以上の引張強度を有し、１７０℃で５分間の低温熱処理後の伸びが３％以上で、リチウムイオン電池電極用アルミニウム合金箔として優れた特性をそなえていた。 As shown in Table 2, each of the test materials 1 to 5 according to the present invention has an electrical resistance value of 0.55 μΩcm or less, a tensile strength of 160 MPa or more, and elongation after low-temperature heat treatment at 170 ° C. for 5 minutes. 3% or more, it had excellent characteristics as an aluminum alloy foil for lithium ion battery electrodes.
これに対して、試験材６は、Ｆｅ含有量が少ないため強度が劣り、試験材７は、Ｆｅ含有量が多いため箔圧延性が低下し、ピンホールが増加した。試験材８は、Ｓｉ量が多いため結晶粒が粗大となってピンホールの発生が多くなった。 On the other hand, the test material 6 had a low strength because the Fe content was small, and the test material 7 had a high Fe content, resulting in a decrease in foil rollability and an increase in pinholes. Since the test material 8 had a large amount of Si, the crystal grains were coarse and the occurrence of pinholes increased.
試験材９は、Ｍｎ量が多いためピンホールの発生が多くなった。試験材１０は、Ｃｕ量が多いため結晶粒が粗大となってピンホールの発生が多く、また電気抵抗値が増大し、低温熱処理後の伸びが不十分となった。 Since the test material 9 had a large amount of Mn, the occurrence of pinholes increased. Since the test material 10 had a large amount of Cu, the crystal grains were coarse and many pinholes were generated, the electrical resistance value increased, and the elongation after the low-temperature heat treatment was insufficient.
比較例２
実施例１で造塊した表１のＡの組成を有するアルミニウム合金のスラブを、４８０℃で１２時間均質化処理した後、開始温度４８０℃、終了温度２８０℃の熱間圧延を行い、厚さ４ｍｍの板を得た。
Comparative Example 2
The aluminum alloy slab formed in Example 1 and having the composition of A in Table 1 was homogenized at 480 ° C. for 12 hours, and then hot-rolled at a start temperature of 480 ° C. and an end temperature of 280 ° C. to obtain a thickness A 4 mm plate was obtained.
続いて、上記熱間圧延に冷間圧延を複数回繰り返し施して、厚さ１５μｍのアルミニウム合金箔を得た。なお、前記冷間圧延処の途中で、板厚が２ｍｍのときに、３００℃で２時間の第一回目の中間焼鈍を行い、板厚が０．５ｍｍのときに、３００℃で２時間の第二回目の中間焼鈍を実施した。 Subsequently, the hot rolling was repeatedly subjected to cold rolling a plurality of times to obtain an aluminum alloy foil having a thickness of 15 μm. In the middle of the cold rolling process, when the plate thickness is 2 mm, the first intermediate annealing is performed at 300 ° C. for 2 hours, and when the plate thickness is 0.5 mm, the first annealing is performed at 300 ° C. for 2 hours. A second intermediate annealing was performed.
得られたアルミニウム合金箔について、実施例１と同様に、引張強度、電気抵抗を測定した、さらに１７０℃で５分間の低温熱処理をなった後の引張強度、伸びを測定した。測定結果を表３に示す。表３において、本発明の条件を外れたものには下線を付した。 The obtained aluminum alloy foil was measured for tensile strength and electrical resistance in the same manner as in Example 1, and further measured for tensile strength and elongation after low-temperature heat treatment at 170 ° C. for 5 minutes. Table 3 shows the measurement results. In Table 3, those outside the conditions of the present invention are underlined.
表３に示すように、試験材１１は、熱間圧延の開始温度および終了温度が高いため、Ｆｅの微細析出が不十分となって、電気抵抗が０．５５μΩｃｍを越え、強度と低温熱処理後の十分な伸びを確保することができなかった。 As shown in Table 3, since the test material 11 has a high hot rolling start temperature and end temperature, Fe fine precipitation is insufficient, electric resistance exceeds 0.55 μΩcm, strength and after low temperature heat treatment It was not possible to secure sufficient elongation.
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