WO2014192256A1 - 電池ケース用アルミニウム合金板及びその製造方法 - Google Patents

電池ケース用アルミニウム合金板及びその製造方法 Download PDF

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WO2014192256A1
WO2014192256A1 PCT/JP2014/002671 JP2014002671W WO2014192256A1 WO 2014192256 A1 WO2014192256 A1 WO 2014192256A1 JP 2014002671 W JP2014002671 W JP 2014002671W WO 2014192256 A1 WO2014192256 A1 WO 2014192256A1
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aluminum alloy
stage
hot
rolling
alloy plate
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PCT/JP2014/002671
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English (en)
French (fr)
Japanese (ja)
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広岳 大菅
賢 熱田
鈴木　義和
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株式会社Uacj
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Priority to JP2015519632A priority Critical patent/JP6006412B2/ja
Priority to CN201480029623.XA priority patent/CN105229186B/zh
Priority to KR1020157024790A priority patent/KR102198154B1/ko
Publication of WO2014192256A1 publication Critical patent/WO2014192256A1/ja

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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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21B—ROLLING OF METAL
    • B21B3/00—Rolling materials of special alloys so far as the composition of the alloy requires or permits special rolling methods or sequences ; Rolling of aluminium, copper, zinc or other non-ferrous metals
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
    • H01M50/10—Primary casings; Jackets or wrappings
    • H01M50/116—Primary casings; Jackets or wrappings characterised by the material
    • H01M50/117—Inorganic material
    • H01M50/119—Metals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
    • B22D11/16—Controlling or regulating processes or operations
    • B22D11/22—Controlling or regulating processes or operations for cooling cast stock or mould
    • 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
    • C22C21/12—Alloys based on aluminium with copper as the next major constituent
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
    • H01M50/10—Primary casings; Jackets or wrappings
    • H01M50/131—Primary casings; Jackets or wrappings characterised by physical properties, e.g. gas permeability, size or heat resistance
    • H01M50/133—Thickness
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
    • B22D11/04—Continuous casting of metals, i.e. casting in indefinite lengths into open-ended moulds
    • B22D11/049—Continuous casting of metals, i.e. casting in indefinite lengths into open-ended moulds for direct chill casting, e.g. electromagnetic casting
    • 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
    • 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

Definitions

  • the present invention relates to an aluminum alloy plate excellent in laser weldability, formability and corrosion resistance after long-term storage suitable as a battery case such as a lithium ion battery used in automobiles, mobile phones, digital cameras, notebook personal computers and the like.
  • the present invention relates to a method capable of producing this excellent aluminum alloy with a high yield.
  • the aluminum alloy plate obtained by this invention can also be utilized as a battery cover.
  • a can body is manufactured by deep drawing and ironing an aluminum plate or an aluminum alloy plate by pressing.
  • the lid is formed by punching or machining an aluminum plate or an aluminum alloy plate into a predetermined shape, and is provided with holes and depressions for attaching terminals, a liquid inlet, and the like.
  • the can body has a deep cylindrical shape, but the lid has a shape close to a flat plate.
  • the can and the lid are sealed by laser welding after enclosing an internal structure such as an electrode.
  • battery case materials are required to have good laser weldability as well as excellent formability.
  • batteries for automobiles and the like there are increasing cases where long-term durability is required for laser junctions.
  • the laser welding speed has been increased for efficient battery production, and the difficulty of laser welding has increased.
  • an aluminum alloy plate for a battery case that can provide a stable joint with less variation in the penetration depth and weld mark (bead) width even in high-speed laser welding.
  • weld cracking solidification cracking, hot cracking
  • JIS 8079 and JIS 8021 As an aluminum alloy plate excellent in laser weldability, an Al—Fe-based aluminum alloy plate represented by JIS 8079 and JIS 8021 has been proposed (Patent Documents 1 to 3).
  • Patent Documents 1 and 2 specify the content of Fe and the like
  • Patent Document 3 specifies the content of Fe and the like and the dispersion density of an intermetallic compound of 2 to 5 ⁇ m. It is known that the effect of the Fe content on laser weldability is large, and in particular, the presence of intermetallic compounds increases the laser absorption rate, so that deep penetration is likely to be obtained.
  • the battery case is formed by combining a plurality of processes consisting of drawing and ironing, but in recent years there has been a demand for more efficient battery production. Deep drawing and ironing of the case and punching of the battery lid are required. In addition, the machining speed has been increased. Due to high-speed molding or high-speed processing, the lubricity between the mold and the aluminum alloy plate decreases due to build-up due to adhesion of aluminum to the mold surface during molding or processing or seizure due to oxidation of the adhered aluminum. As a result, a streak pattern or a defect is likely to occur on the surface after molding, and a problem that it cannot be molded or processed into a predetermined shape is likely to occur. Therefore, an aluminum alloy plate excellent in formability, particularly surface quality after forming and forming stability is desired.
  • molded or processed materials may be stored for a long period of time, and those materials may be collectively laser welded. At this time, if corrosion occurs due to reaction with moisture in the atmosphere during long-term storage and oxides are formed, weld cracks and blowholes are generated due to the oxides during laser welding. Oxide formation can be prevented by controlling the atmosphere in the storage location of the material after molding or processing, but because of the high cost, an aluminum alloy plate with excellent corrosion resistance after long-term storage without controlling the atmosphere is desired. It is rare.
  • the present invention has been made against the background of the above circumstances, and has excellent laser weldability and formability by reliably and appropriately controlling the components of an aluminum alloy and the equivalent circle diameter and number density of an Al—Fe intermetallic compound. And it aims at provision of the aluminum alloy plate for battery cases which has corrosion resistance after long-term storage.
  • the aluminum alloy plate obtained in the present invention can also be used as a battery lid.
  • the present inventors have rigorously adjusted the contents of Fe, Si, Cu, Ti, Mg, and Mn of the aluminum alloy, together with the manufacturing process, In particular, the inventors have found that the above-mentioned problems can be solved by strictly regulating the cooling rate during casting, and have completed the present invention.
  • Fe 0.8 to 2.0 mass%, Si: 0.03 to 0.20 mass%, Cu: 0 to 1.00 mass%, Ti: 0.004 to Containing 0.050 mass%, Mg: 0.02 mass% or less and Mn: 0.02 mass% or less, made of an aluminum alloy composed of the balance Al and unavoidable impurities, from the surface of the aluminum alloy plate having the final thickness
  • the average equivalent circle diameter of the Al—Fe-based intermetallic compound having an equivalent circle diameter of 1.0 to 16.0 ⁇ m in the metal structure up to a depth of at least 5 ⁇ m in the thickness direction is 1.3 to 1.9 ⁇ m, and circle variation coefficient of equivalent diameter is 0.55 or less, the Al-Fe-based average number density of 20 to 150 / in 2500 [mu] m 2, and the number density variation coefficient of 0.30 or more of intermetallic compounds
  • an aluminum alloy plate for a battery case characterized in that it.
  • the present invention provides a method for producing an aluminum alloy plate for a battery case according to claim 1, wherein the casting process is a casting process for casting the aluminum alloy; a chamfering process; and a casting process before or after the chamfering process.
  • the present invention does not include any one or both of the chamfering step and the surface treatment step.
  • the hot rolling process includes a heating and holding stage in which the ingot is heated and held before the hot rough rolling stage, and the homogenizing process or casting after the chamfering process The homogenization process after the process was replaced by the heating and holding stage.
  • the ingot is maintained at a temperature of 450 to 620 ° C. for 1 to 20 hours in the homogenization treatment step.
  • the hot finish in the hot rough rolling stage is 380 to 550 ° C. and the end temperature is 330 to 480 ° C. in the sixth aspect of the present invention.
  • the start temperature in the rolling stage was within the range of 20 ° C. and the end temperature of the hot rough rolling stage, and the end temperature was 250 to 370 ° C.
  • the present invention according to claim 7 is the cold rolling from the hot rolling step to the intermediate annealing step when an intermediate annealing step is provided in the middle of the cold rolling step according to any one of claims 2 to 6.
  • the rolling reduction in the process, and when the intermediate annealing stage is not provided in the middle of the cold rolling process, the rolling reduction in the cold rolling process from the hot rolling process to the final annealing stage is 50 to 85%. It was supposed to be.
  • the rolled material is 1-8 in a batch annealing furnace at a temperature of 350-450 ° C. in the final annealing stage and the intermediate annealing stage of the annealing process according to any one of claims 2-7. It was held for a period of time or in a continuous annealing furnace at a temperature of 400 to 550 ° C. for 0 to 30 seconds.
  • an aluminum alloy plate for a battery case having excellent laser weldability, formability, and corrosion resistance after long-term storage and a method capable of producing this excellent aluminum alloy with a high yield. be able to.
  • the aluminum alloy plate obtained in the present invention can also be used for a battery lid.
  • the present invention is described in detail below. 1. First, the component composition of the aluminum alloy plate for battery case according to the present invention and the reason for limitation will be described.
  • Fe 0.8 to 2.0 mass% Fe is an important component element that greatly affects laser weldability, formability, and corrosion resistance after long-term storage. Most of Fe is present in the matrix as Al—Fe intermetallic compounds. The presence of the Al—Fe-based intermetallic compound increases the laser absorptance, thereby achieving the effect of deepening the penetration during laser welding. In addition, the amount of Fe is caused by coarse grains because the recrystallization behavior in the subsequent processes after the casting process such as hot rolling and subsequent annealing changes depending on the dispersion state of the Al—Fe intermetallic compound. It greatly affects the occurrence of rough skin after molding. In addition, Al—Fe-based intermetallic compounds, particularly coarse Al—Fe-based intermetallic compounds, are the starting points of corrosion after long-term storage.
  • the Fe content is less than 0.8 mass% (hereinafter simply referred to as “%”), it may cause rough skin after forming due to coarsening of crystal grains. Furthermore, since the number density of the Al—Fe intermetallic compound having an equivalent circle diameter of 1.0 to 16.0 ⁇ m is sparse, the average value of the number density is small and the coefficient of variation is large, so that stable laser weldability is obtained. Absent. Further, the cleaning effect described later cannot be obtained, and the surface quality and molding stability after molding cannot be obtained.
  • the Fe content is set to 0.8 to 2.0%.
  • a preferable Fe content is 1.0 to 1.6%.
  • Si 0.03-0.20%
  • Si is an element that greatly affects laser weldability and formability.
  • the Si content is less than 0.03%, it is necessary to use a high purity aluminum ingot, which increases the cost.
  • it exceeds 0.20% the temperature difference between the liquidus and the solidus becomes large. By increasing this temperature difference, the amount of liquid phase remaining at the time of solidification immediately after laser welding is increased, and stress of solidification shrinkage is applied to the remaining portion of the liquid phase, so that welding cracks are likely to occur.
  • a coarse Al—Fe—Si based compound having an equivalent circle diameter exceeding 16.0 ⁇ m is crystallized, resulting in not only uneven penetration depth and bead width, but also a starting point of cracking during molding.
  • the Si content is set to 0.03 to 0.20%.
  • a preferable Si content is 0.04 to 0.15%.
  • Cu 0 to 1.00%
  • Cu is an element that greatly affects laser weldability, formability, and corrosion resistance after long-term storage. Therefore, in order to obtain these effects, Cu may be selectively added. Most of the added Cu is dissolved in the matrix, and the thermal conductivity of the aluminum alloy can be reduced. Since the laser absorptance increases due to the decrease in thermal conductivity, the penetration of laser welding can be deepened even at a low output. As a result, the amount of energy input can be reduced, so that the manufacturing cost can be reduced. On the other hand, the addition of Cu increases the temperature difference between the liquidus and solidus, so if the Cu content exceeds 1.00%, weld cracks are likely to occur.
  • the Cu content when Cu content exceeds 1.00%, it will become a cause by which the corrosion resistance after long-term storage falls. If the Cu content is less than 0.05%, the above effect may not be sufficient. Therefore, the Cu content is preferably 0.05 to 1.00%, and preferably 0.20 to 0.80%. Is more preferable.
  • the Cu content is preferably 0.05 to 1.00%, and more preferably 0.20 to 0.80%.
  • Ti 0.004 to 0.050%
  • Ti is an element that greatly affects the solidification structure of the aluminum alloy. If the Ti content is less than 0.004%, the crystal grains of the ingot are not refined and become a coarse crystal grain structure, causing not only streak-like defects in the aluminum alloy plate but also the cause of rough skin after forming. It becomes. Moreover, since the effect of refining the solidified structure of the laser welded portion is reduced, it causes weld cracking. On the other hand, if the Ti content exceeds 0.050%, the effect of refining the solidification structure of the laser welded portion is saturated, so excessive addition causes an increase in cost.
  • the Ti content exceeds 0.050%, a Ti-based intermetallic compound is easily formed, and this intermetallic compound is distributed in a streak pattern on the rolled sheet, causing surface defects. Accordingly, the Ti content is set to 0.004 to 0.050%. A preferable Ti content is 0.007 to 0.030%.
  • Mg 0.02% or less Mg is an element that greatly improves strength and resistance to blistering, but remarkably deteriorates laser weldability. Specifically, since Mg has a low vapor pressure, it not only causes blowholes in the weld during laser welding, but also generates a weld crack in order to increase the temperature difference between the liquidus and solidus. Moreover, after long-term storage, an oxide is easily formed on the aluminum alloy plate surface, and blowholes and weld cracks are generated due to the oxide. By regulating the amount of Mg to 0.02% or less, characteristics as an aluminum alloy plate for battery cases are not impaired. When the amount of Mg exceeds 0.02%, laser weldability and corrosion resistance after long-term storage deteriorate.
  • the Mg content is restricted to 0.02% or less, preferably 0.01% or less.
  • the lower limit of the Mg content is not particularly specified and may be 0%, but if it is less than 0.001%, no particular improvement in the effect is obtained, and a high-purity aluminum material should be used. This increases the cost of raw materials. Therefore, the lower limit value of the Mg amount is preferably 0.001%.
  • Mn 0.02% or less
  • Mn is an element that greatly improves strength and blistering resistance, but is also an element that affects the equivalent circle diameter and number density of Al—Fe-based intermetallic compounds.
  • Mn the equivalent circle diameter of the Al—Fe-based intermetallic compound dispersed in the aluminum alloy plate increases, and the number density decreases.
  • a coarse Al—Mn intermetallic compound is formed.
  • the Mn content By regulating the Mn content to 0.02% or less, the characteristics as an aluminum alloy plate for battery cases will not be impaired. However, if the Mn content exceeds 0.02%, the laser weldability deteriorates and will be described later. As a result, the surface cleaning quality after molding is impaired.
  • the Mn content is restricted to 0.02% or less, preferably 0.01% or less.
  • the lower limit of the Mn content is not particularly specified and may be 0%, but if it is less than 0.001%, no particular improvement in the effect is obtained, and a high-purity aluminum material should be used. This increases the cost of raw materials. Therefore, the lower limit value of the Mn amount is preferably 0.001%.
  • a trace amount of at least one of B and C may be added in combination with Ti.
  • the total amount of both addition amounts is set to 0.0001 to 0.0020% in the case where either one is added instead. Is preferred.
  • the amount of these added is more preferably 0.0005 to 0.0015%. If the addition amount is less than 0.0001%, a sufficient effect of crystal grain refinement cannot be obtained. On the other hand, when the amount exceeds 0.0020%, not only the crystal grain refining effect is saturated, but also surface defects due to coarse aggregates of Ti—B compounds and Ti—C compounds are likely to occur.
  • the equivalent circle diameter and number density of the Al—Fe-based intermetallic compound greatly affect laser weldability, formability, and corrosion resistance after long-term storage.
  • An Al—Fe intermetallic compound is dispersed in the aluminum alloy.
  • an average circle of Al—Fe-based intermetallic compounds having a circle equivalent diameter of 1.0 to 16.0 ⁇ m in a metal structure from the surface of the aluminum alloy plate having the final thickness to a depth of at least 5 ⁇ m in the thickness direction.
  • the equivalent diameter is 1.3 to 1.9 ⁇ m
  • the coefficient of variation of the equivalent circle diameter is 0.55 or less
  • the average number density between the Al—Fe-based intermetallic compounds is 20 to 150/2500 ⁇ m 2 .
  • the coefficient of variation of the number density is 0.30 or less.
  • the Al—Fe intermetallic compound having the equivalent circle diameter as described above is dispersed at the number density as described above, thereby removing the adhesion of aluminum and aluminum oxide adhered to the mold during molding. Therefore, deterioration of the surface quality and molding stability after molding can be prevented.
  • Al-Fe-based intermetallic compound equivalent circle diameter A fine Al-Fe-based intermetallic compound having an equivalent-circle diameter of less than 1.0 ⁇ m has almost no influence on laser weldability and no cleaning effect. Therefore, in the present invention, those having this equivalent circle diameter are not intended. Further, when there is a coarse Al—Fe intermetallic compound having an equivalent circle diameter exceeding 16.0 ⁇ m, an increase in laser absorptance occurs locally. Then, not only is the penetration deeper in the local portion, but also defects such as welding defects due to non-uniform beads and spatters occur.
  • a coarse Al—Fe-based intermetallic compound having an equivalent circle diameter of more than 16.0 ⁇ m becomes a starting point of corrosion and causes a failure that becomes a starting point of cracking in forming.
  • a coarse Al—Fe intermetallic compound having an equivalent circle diameter exceeding 16.0 ⁇ m which causes the above-described obstacles, is not formed. Therefore, in the present invention, a coarse Al—Fe intermetallic compound having an equivalent circle diameter exceeding 16.0 ⁇ m is not considered.
  • the equivalent circle diameter and number density of the Al—Fe intermetallic compound are targeted for the Al—Fe intermetallic compound having an equivalent circle diameter of 1.0 to 16.0 ⁇ m.
  • each Al—Fe-based intermetallic compound having an equivalent circle diameter of 1.0 to 16.0 ⁇ m is small, so that a cleaning effect is obtained.
  • the surface quality and molding stability after molding deteriorate.
  • the effect of increasing the laser absorption rate is small, the effect of deepening the penetration during laser welding is reduced, and a stable penetration depth cannot be obtained.
  • the average equivalent circle diameter exceeds 1.9 ⁇ m, the number density of the Al—Fe-based intermetallic compound becomes small and the distribution of the Al—Fe-based intermetallic compound becomes sparse, so that the beat width and the penetration depth are small.
  • the average equivalent circle diameter of the Al—Fe-based intermetallic compound having an equivalent circle diameter of 1.0 to 16.0 ⁇ m is set to 1.3 to 1.9 ⁇ m.
  • a preferable average equivalent circle diameter is 1.4 to 1.8 ⁇ m.
  • the average equivalent circle diameter means an arithmetic average value of equivalent circle diameters.
  • the variation coefficient of the equivalent circle diameter is a parameter indicating the relative variation of the equivalent circle diameter of the Al—Fe-based intermetallic compound having an equivalent circle diameter of 1.0 to 16.0 ⁇ m.
  • this coefficient of variation exceeds 0.55, the variation in the equivalent circle diameter of the Al—Fe-based intermetallic compound is large, and the relative variation in the equivalent circle diameter is also increased, and the beat width and the penetration depth are stabilized. Laser weldability cannot be obtained.
  • the variation coefficient of the equivalent circle diameter is 0.55 or less, the relative variation in the size of the Al—Fe-based intermetallic compound is small and excellent in uniformity. Absent. Therefore, the variation coefficient of the equivalent circle diameter is 0.55 or less.
  • a preferable variation coefficient is 0.50 or less.
  • the lower limit of the coefficient of variation is not particularly limited, but is naturally determined by the aluminum alloy composition used in the present invention and the method of manufacturing the aluminum alloy material. In the present invention, 0.30 is the lower limit.
  • the average number density of the Al—Fe-based intermetallic compound having a circle-equivalent diameter of 1.0 to 16.0 ⁇ m is set to 20 to 150 pieces / 2500 ⁇ m 2 .
  • a preferable average number density is 30 to 130 / 2,500 ⁇ m 2 .
  • the coefficient of variation of number density When the coefficient of variation of the number density exceeds 0.30, the relative dispersion of the Al—Fe intermetallic compound distribution is large and the distribution becomes non-uniform, and laser weldability with stable beat width and penetration depth is obtained. I can't.
  • the variation coefficient of the number density is 0.30 or less, the relative variation in the distribution of the Al—Fe-based intermetallic compound is small and the uniformity is excellent, so that there is no trouble as in the case of exceeding 0.30.
  • the variation coefficient of the number density is 0.30 or less.
  • a preferable coefficient of variation is 0.25 or less.
  • the lower limit of the coefficient of variation is not particularly limited, but is naturally determined by the aluminum alloy composition used in the present invention and the method of manufacturing the aluminum alloy material. In the present invention, 0.10 is the lower limit value.
  • the above-mentioned coefficient of variation of equivalent circle diameter and number density is also called a relative standard deviation, and is defined as a standard deviation / arithmetic mean value in statistics, and is a parameter indicating the degree of relative variation.
  • the average equivalent circle diameter between Al—Fe-based intermetallic compounds having an equivalent circle diameter of 1.0 to 16.0 ⁇ m is 1.3 to 1.9 ⁇ m, and the variation coefficient of the equivalent circle diameter is 0.
  • the aluminum alloy sheet having an average number density between the Al—Fe intermetallic compounds of 20 to 150/2500 ⁇ m 2 and a coefficient of variation of the number density of 0.30 or less Al-Fe-based intermetallic compound dispersed in the material has an appropriate range of equivalent circle diameter and number density, and since the relative variation in the equivalent circle diameter and number density is small and excellent in uniformity, Laser weldability, formability, and corrosion resistance after long-term storage are achieved.
  • the equivalent circle diameter and the number density of the above-mentioned intermetallic compound in the metal structure from the aluminum alloy plate surface of the final plate thickness it is necessary to satisfy the circle equivalent diameter and the number density of the above-mentioned intermetallic compound in the metal structure from the aluminum alloy plate surface of the final plate thickness to a depth of at least 5 ⁇ m in the plate thickness direction.
  • the influence of the above-mentioned laser weldability, cleaning effect, and corrosion resistance due to the equivalent circle diameter and number density of the intermetallic compound on the plate It is smaller than the region up to a depth of 5 ⁇ m in the thickness direction. Therefore, in the region having a depth exceeding 5 ⁇ m, the equivalent circle diameter and the number density are not particularly limited.
  • the Al—Fe-based intermetallic compound refers to an intermetallic compound such as Al 3 Fe, Al 6 Fe, Al m Fe, ⁇ -AlFeSi, and ⁇ -AlFeSi. Note that the equivalent circle diameter and number density of the Al—Fe intermetallic compound in the metal structure were measured from an arbitrary surface of the aluminum alloy material to a depth of 5 ⁇ m in the thickness direction using a scanning electron microscope. A (COMP image) is taken, and the obtained micrograph is analyzed by image analysis.
  • a method for producing an aluminum alloy plate for a battery case according to the present invention is the method for producing an aluminum alloy plate for a battery case according to claim 1, wherein a casting step of casting the aluminum alloy; a chamfering step; A homogenization process for homogenizing the ingot before or after the process; a hot rolling process comprising a hot rough rolling stage and a hot finish rolling stage; a cold rolling process; an annealing process; A surface treatment step before or after at least one of the treatment step, the hot rolling step, the cold rolling step, and the annealing step, and the annealing step, and the annealing step includes an intermediate annealing step and a cold step in the middle of the cold rolling step.
  • the cooling rate at the time of solidification at the ingot thickness position corresponding to the surface of the aluminum alloy sheet having the final thickness is 2 to 20 ° C./second Also features It is.
  • the hot rolling process includes a heating and holding stage in which the ingot is heated and held before the hot rough rolling stage, and the homogenizing process after the chamfering process or the homogenizing process after the casting process is performed in the heating and holding stage. May be substituted.
  • the molten aluminum alloy adjusted to the above component composition range is appropriately subjected to molten metal treatment such as degassing and filtration, and then cast according to a conventional method such as DC casting.
  • FIG. 1 shows a conceptual diagram of the DC casting method and a graph showing a change in cooling rate during solidification.
  • the molten metal poured into the mold comes into contact with the water-cooled mold wall and is rapidly cooled.
  • the ingot surface layer produced by solidification shrinks, and a gap is formed between the ingot surface and the mold. Since the heat transfer resistance of the gap is much larger than that of the mold or spray water, the amount of heat diffused from the ingot to the outside decreases, and the cooling rate during solidification also decreases accordingly.
  • the cooling rate during solidification increases rapidly.
  • a fine micro-solidified structure called a chill layer is generated in a region where the mold wall that has been cooled with water is brought into contact with the mold wall and rapidly cooled. Moreover, in the region where the cooling rate during solidification decreases due to the formation of voids between the ingot surface and the mold, a coarse micro solidified structure called a coarse cell layer is generated. When the ingot descends and the ingot surface comes into contact with the spray water, a fine micro solidified structure called a fine cell layer is generated in a region where the cooling rate during solidification increases rapidly.
  • the present inventors set the appropriate value for the equivalent circle diameter and number density of the Al—Fe intermetallic compound.
  • an aluminum alloy plate excellent in uniformity can be obtained by reducing these variations.
  • the cooling rate at the time of solidification decreases to less than 2 ° C./second
  • the variation coefficient of the equivalent diameter is increased, and the average number density of the Al—Fe intermetallic compound is small and the variation coefficient of the number density is large.
  • the cooling rate during solidification at the ingot thickness position corresponding to the surface of the aluminum alloy plate having the final thickness is set to 2 to 20 ° C./second.
  • a preferable cooling rate during solidification is 3 to 10 ° C./second.
  • the cooling rate during solidification can be adjusted by controlling the casting speed, mold material, cooling conditions, molten metal temperature, and the like. Specifically, there is a region where the cooling rate at the time of solidification is reduced due to the formation of a gap between the ingot surface and the mold. The amount of decrease in the cooling rate is reduced, and further, the cooling rate during solidification in the entire casting region including this region is changed.
  • the ingot after the casting process may be chamfered according to the state and shape of the ingot surface and the distribution of the cooling rate during solidification in the ingot. If the ingot surface has a undulating shape, or if the ingot surface has oxide or dirt formed or adhered in the casting process, the final plate will be subjected to hot rolling or cold rolling. In order to cause streaky patterns and wrinkles, chamfering is performed. The amount of chamfering is determined such that the cooling rate during solidification at the ingot thickness position corresponding to the final plate surface is 2 to 20 ° C./second as described above.
  • the final plate Chamfering is performed so that the cooling rate during solidification at the ingot thickness position corresponding to the surface is 2 to 20 ° C./second.
  • the chamfering amount may be determined in consideration of the surface removal amount.
  • the surface treatment process Chemical and electrical for the purpose of removing dirt and oxide film on the ingot surface before and after at least one of the homogenization process, hot rolling process, cold rolling process and annealing process after the casting process. You may provide the surface treatment process which removes the material surface chemically or mechanically. In the surface treatment process, part of the surface of the aluminum alloy plate is removed, so the surface removal amount is determined so that the cooling rate during solidification at the ingot thickness position corresponding to the final plate surface is 2 to 20 ° C / sec. There is a need to.
  • the surface treatment step may be provided before or after any step of the homogenization treatment step, the hot rolling step, the cold rolling step, and the annealing step. Further, the surface treatment step may be provided once or a plurality of times.
  • the ingot thickness position corresponding to the surface thickness of the aluminum alloy plate of the final plate thickness is estimated from the ingot thickness after casting, the chamfering amount in the chamfering process, the surface removal amount in the surface treatment process, and the plate thickness in the surface treatment process. Is possible. For example, as shown in FIG. 2, when the ingot after casting is subjected to a chamfering process, and a surface treatment process is provided once during the homogenization treatment process, hot rolling process, cold rolling process, and annealing process.
  • the ingot thickness position corresponding to the surface of the aluminum alloy plate having the final thickness is expressed by the following equation.
  • X (t ⁇ t) ⁇ (T ⁇ s) / t
  • X the ingot thickness position (mm) from the center position of the ingot plate thickness corresponding to the aluminum alloy plate surface of the final plate thickness
  • T In the ingot, the distance from the center position of the ingot plate thickness to the surface (mm)
  • ⁇ s the amount of single-sided chamfering in the chamfering step (mm)
  • ⁇ t the amount of single-sided surface removal in the surface treatment step (mm)
  • t Distance (mm) from the center position of the ingot plate thickness to the plate material surface in the surface treatment step.
  • DELTA DELTA
  • Manufacturing processes other than the casting process, the chamfering process, and the surface treatment process are not particularly limited. However, the following manufacturing process is used to improve the formability, blister resistance, and surface quality of the final plate. It is preferable from the point.
  • Homogenization treatment step A homogenization treatment step is provided in which the ingot is homogenized at a temperature of 450 to 620 ° C. for a holding time of 1 to 20 hours.
  • the temperature of the homogenization treatment is less than 450 ° C. or the holding time of the homogenization treatment is less than 1 hour, the homogenization effect is small, and the hot rough rolling step and the hot finish rolling step, which will be described later, and the intermediate annealing step and the final annealing step are performed.
  • the recrystallized grains become coarse. Due to such coarse recrystallized grains, rough skin tends to occur after molding.
  • the homogenization treatment conditions are preferably a temperature of 450 to 620 ° C. and a holding time of 1 to 20 hours, and more preferably a temperature of 480 to 600 ° C. and a holding time of 3 to 15 hours.
  • Hot rolling process is composed of a hot rough rolling stage and a hot finish rolling stage. However, a hot holding stage may be provided before the hot rough rolling stage.
  • Heating and holding stage When a heating and holding stage is provided before the hot rough rolling stage of the hot rolling process, the ingot before rolling is heated at a predetermined temperature for a predetermined time in this stage.
  • a heating and holding stage is provided before the hot rough rolling stage of the hot rolling process, the ingot before rolling is heated at a predetermined temperature for a predetermined time in this stage.
  • a homogenization effect is also provided with a heating effect before hot rolling.
  • the heating and holding stage By substituting the homogenization process step by the heating and holding stage, not only the same effect as the homogenization process can be obtained, but also compared with the case where the homogenization process step is provided before and after the chamfering process, This is advantageous in terms of the number of manufacturing processes and cost reduction.
  • the heating and holding stage is performed under conditions that do not perform the homogenization process and the effect of the homogenization process is not obtained, the subsequent hot rough rolling stage and hot finish rolling stage, and intermediate annealing are performed. In the stage and the final annealing stage, the recrystallized grains are coarsened, and rough skin after molding is likely to occur.
  • the holding temperature is 450 to 620 ° C. and the holding time is 1 to 20 hours.
  • the holding temperature is less than 450 ° C. or the holding time is less than 1 hour, the homogenization effect is small, and the recrystallized grains become coarse in the hot rough rolling stage and the hot finish rolling stage, and in the intermediate annealing stage and the final annealing stage, Rough skin is likely to occur after molding.
  • holding temperature exceeds 620 degreeC, a part of ingot will melt
  • the holding time and holding temperature in the heating and holding stage are not limited as described above, and the ingot is held under normal conditions, for example, at a temperature of 380 to 560 ° C. for 1 to 10 hours. You may make it do.
  • the hot rough rolling start temperature is less than 380 ° C., a uniform recrystallized structure after completion of hot rough rolling cannot be obtained, which may cause rough skin after forming.
  • the hot rough rolling start temperature exceeds 550 ° C., the recrystallized grains after completion of the hot rough rolling may be coarsened and cause rough skin after forming.
  • generated on the roll surface at the time of rolling is transcribe
  • the hot rough rolling start temperature is preferably 380 to 550 ° C.
  • the hot rough rolling finish temperature is preferably set to 330 to 480 ° C.
  • Hot finish rolling stage The hot finish rolling method includes a tandem method in which a plurality of rolling mills are combined and a reverse method in which hot rolling is performed with a single rolling mill.
  • Hot finish rolling refers to rolling in which a plurality of rolling mills are combined in the case of the tandem method, and from rolling immediately before winding to the final rolling in the case of the reverse method.
  • the plate thickness at which hot finish rolling is started is about 15 to 40 mm.
  • the temperature difference between the hot rough rolling finish temperature and the hot finish rolling start temperature is set to 20 ° C. or less. If the temperature difference is within 20 ° C., the moldability is not impaired. In general, the hot finish rolling start temperature is lower than the hot rough rolling end temperature.
  • the hot finish rolling finish temperature is preferably 250 to 370 ° C.
  • the reduction ratio in the cold rolling process after the hot rolling process is the cold rolling from the hot rolling process to the intermediate annealing stage when an intermediate annealing stage is provided in the middle of the cold rolling process.
  • the rolling reduction in the process is shown, and when the intermediate annealing stage is not provided, the rolling reduction in the cold rolling process from the hot rolling process to the final annealing stage is shown.
  • Annealing process and further cold rolling process (final cold rolling process) Depending on the tempering of the final aluminum alloy sheet, it may be subjected to the final annealing step after the cold rolling step without providing an intermediate annealing step, or after being subjected to the intermediate annealing step in the middle of the cold rolling step, As a further cold rolling process, a final cold rolling process according to a conventional method may be applied.
  • the conditions for the final annealing stage and the intermediate annealing stage are not particularly limited, and may be performed according to a conventional method.
  • the holding time is 1 to 8 hours at a temperature of 350 to 450 ° C., and when using a continuous annealing furnace, the holding time is 0 to 30 seconds at a temperature of 400 to 550 ° C. (Here, the holding time of 0 second means that the cooling is performed immediately after reaching the predetermined temperature).
  • the rolling reduction in the final cold rolling process after the intermediate annealing stage is preferably 20 to 60%.
  • the leveler correction process after the final cold rolling process or the final annealing stage, the leveler correction process, the above-mentioned surface treatment process, the degreasing process using an organic solvent or hot water, and a coating that applies oil so as not to cause scratches when the aluminum alloy plates are stacked.
  • An oil process or the like may be provided.
  • the ingot is heated and held. After heating and holding to a predetermined temperature, it is preferable to cool to the starting temperature of hot rough rolling and then go to the hot rough rolling stage.
  • the start temperature and end temperature of the hot rough rolling stage and the hot finish rolling stage can be adjusted to appropriate temperatures.
  • the temperature difference is small, the ingot is hot-rolled immediately after the heating and holding stage without passing through the cooling stage.
  • Invention Examples 1 to 16 and Comparative Examples 17 to 27 Using an aluminum alloy having the composition shown in Table 1, an ingot having a thickness of 550 mm was cast by a semi-continuous casting method. In addition, about less than 0.01% of component, it was set as 0.00%. The obtained ingot was subjected to a chamfering process as shown in Table 2, and then subjected to a homogenization treatment process at a temperature of 540 ° C. and a holding time of 4 hours. The ingot was then cooled once to room temperature. Immediately after the cooled ingot is heated and held at a temperature of 460 ° C. for 4 hours (not a substitute for the homogenization step), hot rough rolling with a start temperature of 430 ° C.
  • the rolled plate was then subjected to a hot finish rolling step with an end temperature of 270 ° C. to obtain a hot rolled plate having a thickness of 3 mm.
  • the obtained hot-rolled sheet was subjected to a cold rolling process, and the surface treatment shown in Table 2 was performed. Thereafter, the cold-rolled sheet was subjected to final annealing at a temperature of 390 ° C. and a holding time of 3 hours using a batch annealing furnace to obtain an aluminum alloy sheet having a final thickness of 0.8 mm.
  • Example 1 of the present invention the hot-rolled sheet after the hot finish rolling stage is subjected to the surface treatment process, and in Examples 9 and 13 of the present invention, the cold-rolled sheet obtained during the cold rolling process is subjected to the surface treatment process. It was.
  • the hot-rolled sheet was subjected to a cold rolling process to a thickness of 0.81 mm, and then the cold-rolled sheet was subjected to a final annealing step, which was then subjected to a surface treatment process. It was.
  • DAS measurement In the ingot after the casting process, the cooling rate at the time of solidification at the ingot thickness position corresponding to the surface of the aluminum alloy plate having the final thickness was obtained.
  • a slice plate having a thickness of 20 mm was cut from the ingot after the casting process along a plane perpendicular to the casting direction.
  • one cut surface of the slice plate was polished, and the polished observation surface was subjected to electrolytic treatment with Barker's solution.
  • DAS of the observation surface was measured using the optical microscope.
  • X shown in Table 2 is the ingot thickness position corresponding to the surface of the aluminum alloy plate having the final thickness.
  • the cooling rate at the time of casting shown in Table 2 was computed from the said relational expression 1 using DAS in the position X.
  • the surface of the obtained aluminum alloy plate was polished by about 2 to 3 ⁇ m from the final plate surface in the plate thickness direction according to a conventional method.
  • the equivalent circle diameter and number density of the Al—Fe intermetallic compound dispersed on the polished aluminum alloy plate surface were measured. Specifically, the presence or absence of an Al—Fe intermetallic compound having an equivalent circle diameter exceeding 16 ⁇ m, the equivalent circle diameter of an Al—Fe based intermetallic compound having an equivalent circle diameter of 1.0 to 16.0 ⁇ m, and Number density was measured. Note that it is necessary to observe an Al—Fe-based intermetallic compound having an equivalent circle diameter of 1.0 ⁇ m or more, for example, at a magnification of 500 times or more.
  • the average equivalent circle diameter of the Al—Fe-based intermetallic compound was obtained by taking a reflected electron composition image (COMP image) with a scanning electron microscope at an acceleration voltage of 15 kV and an observation visual field area of 250,000 ⁇ m 2. Obtained by image analysis. At an acceleration voltage of 15 kV, the penetration depth of the electron beam in aluminum is about 2 to 3 ⁇ m, and the COMP image obtained by observation includes information up to a depth of 2 to 3 ⁇ m in the plate thickness direction.
  • the average equivalent circle diameter (arithmetic mean) and standard deviation were determined from the equivalent circle diameters of all Al—Fe-based intermetallic compounds having an equivalent circle diameter of 1.0 to 16.0 ⁇ m observed in the measurement visual field. . Further, the coefficient of variation of the equivalent circle diameter was calculated by dividing the standard deviation of the equivalent circle diameter by the average equivalent circle diameter. The results are shown in Table 3.
  • the number density of the Al—Fe-based intermetallic compound having an equivalent circle diameter of 1.0 to 16.0 ⁇ m is obtained by dividing the observation field of 250,000 ⁇ m 2 into 100 narrow fields of 50 ⁇ m ⁇ 50 ⁇ m.
  • the total number of the intermetallic compounds present in the visual field (2500 ⁇ m 2 ) was measured.
  • the arithmetic average value of the measured number of each narrow visual field was calculated
  • the number density variation coefficient was calculated by obtaining the standard deviation of the number density from the number density of each narrow field of view and dividing this by the average number density. The results are shown in Table 3.
  • the equivalent circle diameter and number density of the intermetallic compound were measured for the non-polished surface, the surface polished 2 to 3 ⁇ m from the above surface, and the surface polished 4 to 5 ⁇ m from the surface as described above using the same sample. It was confirmed that almost the same data was obtained in all cases.
  • the maximum bead width wmax, the minimum bead width wmin, the maximum penetration depth dmax and the minimum penetration depth dmin are measured, and wmax / wave, wmin / wave, dmax / dave, and dmin / dave are all 0.90 to 1.10.
  • the ones in the range are the best ( ⁇ mark), 0.85 or more and less than 0.90, or the ones in the range from 1.10 to 1.15 are excellent ( ⁇ mark), 0.80 or more and less than 0.85 Those in the range of more than 1.15 and less than or equal to 1.20 were judged as good ( ⁇ mark), and those in the range of less than 0.8 or more than 1.2 were judged as bad (x mark).
  • Table 3 The results are shown in Table 3.
  • the aluminum alloy plate sample (short side: 60 mm, long side: 100 mm, thickness: 0.8 mm) was held in a humid atmosphere of 50 ° C. and 95% humidity for 100 hours. Next, the long sides of these samples were butted together and a laser welding test was performed over a total length of 100 mm. Prior to the holding in the above-mentioned wet atmosphere, the butt surfaces were subjected to planar processing using a milling machine. Welding was performed at a welding speed of 5 m / min.
  • the condensing diameter was 0.1 mm ⁇ , the output was adjusted so that the average penetration depth was 70% with respect to the thickness of 0.6 mm of the rolled material, and laser welding was performed under continuous wave (CW, Continuous Wave) conditions. No termination processing was performed to reduce the output stepwise at the termination section.
  • the appearance observation and cross-sectional observation of the bead were performed similarly to the soundness of the laser welded portion described above. In both appearance observation and cross-sectional observation, weld cracks, bead defects and blowholes were not generated well (circle mark), weld cracks, bead defects and blowholes were generated Was determined to be defective (x). The results are shown in Table 3.
  • the aluminum alloy plate was subjected to multi-stage molding, specifically, three-stage drawing test and ten-stage iron molding to form a square battery case 1 shown in FIG.
  • This battery case 1 has a width of 30 mm, a height of 8 mm, a depth of 45 mm (not shown), an average plate thickness of 0.62 mm on the side surface, an average plate thickness of 0.51 mm on the top and bottom surfaces, and an angle R of 1.5 mm.
  • the above-described rectangular battery case 1 was molded by performing the ironing process in seven stages instead of ten stages.
  • the average equivalent circle diameter between Al—Fe-based intermetallic compounds having an equivalent circle diameter of 1.0 to 16.0 ⁇ m is 1.3 to 1.9 ⁇ m, and the equivalent circle diameter varies.
  • Invention Examples 3, 5 to 12 had high tensile strength.
  • Comparative Example 17 since the Fe content was large, a coarse Al—Fe intermetallic compound exceeding the equivalent circle diameter of 16.0 ⁇ m was formed. As a result, the laser absorptance locally increased, the penetration depth and the bead width became non-uniform, and the stability of laser welding deteriorated. In addition, cracking occurred as a starting point during molding, and cracking occurred during molding, resulting in deterioration of moldability. Furthermore, after long-term storage, corrosion started from coarse Al—Fe-based intermetallic compounds, resulting in weld cracking and blowholes during laser welding, and the corrosion resistance after long-term storage deteriorated.
  • the amount of Ti is small, the crystal grain of the ingot is not refined and becomes a coarse grain structure, not only does the aluminum alloy plate have streak-like defects, but it also causes rough skin after forming, and the formability is low. It got worse.
  • Comparative Example 20 since the amount of Ti is large, a Ti-based intermetallic compound is formed, and this intermetallic compound is distributed in a streak pattern on the rolled plate, causing surface defects, causing cracks during molding, and during molding Cracks occurred and formability deteriorated.
  • Comparative Example 24 since the cooling rate at the time of solidification at the ingot thickness position corresponding to the aluminum alloy plate surface of the final plate thickness was small, the average value and variation coefficient of the equivalent circle diameter of the Al—Fe-based intermetallic compound were large. Furthermore, the average value of the number density was small and the coefficient of variation of the number density was large. As a result, the stability of laser weldability, formability, and corrosion resistance after long-term storage deteriorated.
  • Comparative Example 25 since the cooling rate at the time of solidification at the ingot thickness position corresponding to the surface of the aluminum alloy plate having the final plate thickness was large, the average equivalent circle diameter of the Al—Fe-based intermetallic compound was small and the average number density was Became larger. As a result, the stability of laser weldability deteriorated, the cleaning effect could not be obtained, the surface quality after molding and the molding stability were inferior, and the moldability deteriorated.
  • Comparative Example 26 since the cooling rate at the time of solidification at the ingot thickness position corresponding to the surface of the aluminum alloy plate having the final plate thickness was small, the average value and variation coefficient of the equivalent circle diameter of the Al—Fe-based intermetallic compound were large. Furthermore, the average value of the number density was small, and the coefficient of variation of the number density was large. As a result, the stability of laser weldability, formability, and corrosion resistance after long-term storage deteriorated.
  • Comparative Example 27 since the cooling rate at the time of solidification at the ingot thickness position corresponding to the surface of the aluminum alloy plate having the final plate thickness was large, the average equivalent circle diameter of the Al—Fe-based intermetallic compound was small, and the average number density was Became larger. As a result, the stability of laser weldability deteriorated, the cleaning effect could not be obtained, the surface quality after molding and the molding stability were inferior, and the moldability deteriorated.
  • an aluminum alloy plate for a battery case that is excellent in laser weldability, formability, and corrosion resistance after long-term storage. Moreover, according to the manufacturing method of the aluminum alloy plate for battery cases which concerns on this invention, the said aluminum alloy plate for battery cases can be obtained reliably and stably with a sufficient yield.
  • the aluminum alloy plate for a battery case exhibits excellent characteristics as a battery lid.

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