WO2013157598A1 - 鋼箔及びその製造方法 - Google Patents
鋼箔及びその製造方法 Download PDFInfo
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- WO2013157598A1 WO2013157598A1 PCT/JP2013/061472 JP2013061472W WO2013157598A1 WO 2013157598 A1 WO2013157598 A1 WO 2013157598A1 JP 2013061472 W JP2013061472 W JP 2013061472W WO 2013157598 A1 WO2013157598 A1 WO 2013157598A1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/64—Carriers or collectors
- H01M4/66—Selection of materials
- H01M4/661—Metal or alloys, e.g. alloy coatings
- H01M4/662—Alloys
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B1/00—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
- B21B1/40—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling foils which present special problems, e.g. because of thinness
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/01—Layered products comprising a layer of metal all layers being exclusively metallic
- B32B15/013—Layered products comprising a layer of metal all layers being exclusively metallic one layer being formed of an iron alloy or steel, another layer being formed of a metal other than iron or aluminium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/01—Layered products comprising a layer of metal all layers being exclusively metallic
- B32B15/013—Layered products comprising a layer of metal all layers being exclusively metallic one layer being formed of an iron alloy or steel, another layer being formed of a metal other than iron or aluminium
- B32B15/015—Layered products comprising a layer of metal all layers being exclusively metallic one layer being formed of an iron alloy or steel, another layer being formed of a metal other than iron or aluminium the said other metal being copper or nickel or an alloy thereof
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/02—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
- C21D8/04—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips to produce plates or strips for deep-drawing
- C21D8/0421—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips to produce plates or strips for deep-drawing characterised by the working steps
- C21D8/0436—Cold rolling
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/02—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
- C21D8/04—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips to produce plates or strips for deep-drawing
- C21D8/0478—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips to produce plates or strips for deep-drawing involving a particular surface treatment
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/001—Ferrous alloys, e.g. steel alloys containing N
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/004—Very low carbon steels, i.e. having a carbon content of less than 0,01%
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/12—Ferrous alloys, e.g. steel alloys containing tungsten, tantalum, molybdenum, vanadium, or niobium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/14—Ferrous alloys, e.g. steel alloys containing titanium or zirconium
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/34—Pretreatment of metallic surfaces to be electroplated
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/34—Pretreatment of metallic surfaces to be electroplated
- C25D5/36—Pretreatment of metallic surfaces to be electroplated of iron or steel
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D7/00—Electroplating characterised by the article coated
- C25D7/06—Wires; Strips; Foils
- C25D7/0614—Strips or foils
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/64—Carriers or collectors
- H01M4/82—Multi-step processes for manufacturing carriers for lead-acid accumulators
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D2211/00—Microstructure comprising significant phases
- C21D2211/004—Dispersions; Precipitations
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D2251/00—Treating composite or clad material
- C21D2251/02—Clad material
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
- C21D9/46—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for sheet metals
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- 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 a steel foil that can be used for a negative electrode current collector foil of a non-aqueous electrolyte secondary battery represented by a lithium ion secondary battery, and a method for producing the same.
- Non-aqueous electrolyte secondary batteries represented by lithium ion secondary batteries have high energy density, and are therefore used as power sources for mobile communications or portable information terminals.
- the market is growing rapidly. Accordingly, in order to pursue further downsizing and weight reduction of the device, there is a demand for performance improvement for further downsizing and weight reduction of the battery occupying a large volume in the device.
- the negative electrode active material (hereinafter sometimes referred to as an active material) used in the secondary battery is mainly a graphite-based carbonaceous material.
- Graphite-based carbonaceous material is a key material that affects battery performance.
- the amount of lithium that can be reversibly inserted into and desorbed from the graphite-based carbonaceous material is limited to one lithium atom per six carbon atoms.
- the theoretical limit capacity of charge / discharge of the carbon material calculated from this limit value is 372 mAh / g in terms of electric capacity. Since the current secondary battery is used at a level close to this limit capacity, a dramatic improvement in performance cannot be expected in the future.
- the above-described high-capacity active material has a large volume fluctuation due to insertion and extraction of lithium compared to conventional graphite-based carbonaceous material. As a result, as the charge and discharge are repeated, the active material is pulverized or the active material is peeled off from the current collector. Thus, the active materials disclosed in Patent Documents 1 and 2 have a problem that good charge / discharge cycle characteristics cannot be obtained.
- an electrode for a lithium secondary battery formed by depositing an amorphous silicon thin film or a microcrystalline silicon thin film as an active material on a current collector such as a copper foil by a CVD method or a sputtering method is It has been found that good charge / discharge cycle characteristics are exhibited (see Patent Document 3). This is because the active material thin film is in close contact with the current collector.
- a conductive intermediate layer containing polyimide is disposed as a binder in a layer containing a silicon-based active material or between a layer containing a silicon-based active material and a metal foil current collector, and then the metal foil current collector
- a method for producing a current collector has been found in which a conductive intermediate layer is disposed thereon and sintered in a non-oxidizing atmosphere (see Patent Document 4).
- the conductive intermediate layer suppresses separation of the mixture layer from the current collector due to the expansion and contraction of the negative electrode active material accompanying the charge / discharge reaction, and therefore, between the mixture layer and the current collector. Increase adhesion.
- a higher-strength current collector that can withstand the stress generated by the volume expansion of the active material is required.
- One way to increase the tensile strength of the current collector is to increase the thickness of the current collector.
- simply increasing the thickness of the current collector cannot be expected to greatly improve the tensile strength of the current collector, but it also reduces the energy density of the battery due to the increase in the weight and volume of the battery. Occurs.
- Typical copper foils for the negative electrode current collector include those produced by rolling and those produced by an electrolytic method (electrolytic copper foil).
- electrolytic copper foil there is a limit to increasing the strength of the current collector using copper foil with electrolytic copper foil. Therefore, production of high-strength copper foil by a rolling method has been studied, and it has been proposed to use this rolled copper alloy foil as a negative electrode current collector (see Patent Document 5).
- the potential of the negative electrode when the lithium ion battery is operating normally is less than 2 V (relative to Li) and very low.
- the potential may be greater than 3V (vs. Li). At such a high potential, there is a problem that copper dissolves rapidly and causes deterioration of battery characteristics.
- copper is a metal having a large specific gravity (specific gravity: 8.9)
- specific gravity 8.9
- the weight ratio of the negative electrode current collector foil to the battery is relatively high, and energy per weight Impedes density improvement.
- copper foil is more expensive than Al foil used for the positive electrode.
- iron Since iron has a higher electrical resistance than copper, it tends to be questionable about its properties as a current collector. However, with recent improvements in battery structure and diversification of battery applications and required characteristics, electrical resistance has not necessarily become a problem.
- Patent Document 6 proposes to use an electrolytic iron foil having a thickness of 35 microns or less as a current collector for a negative electrode. From the viewpoint of rust prevention, it has also been proposed to use electrolytic iron foil plated with Ni.
- Ni plating on the electrolytic foil is a factor that increases the cost. Furthermore, unless the Ni plating is formed thick (1 ⁇ m or more), Fe elution during overdischarge is inevitable.
- Patent Document 7 proposes to use, as a negative electrode current collector, a metal foil obtained by forming iron sesquioxide on the surface of an iron foil or a nickel-plated iron foil.
- a metal foil obtained by forming iron sesquioxide on the surface of an iron foil or a nickel-plated iron foil.
- Fe elution during overdischarge is unavoidable, and side reactions at the negative electrode potential easily occur. As a result, the efficiency or life of the battery tends to be hindered.
- Patent Document 8 proposes a ferritic stainless steel foil current collector.
- ferritic stainless steel foil has a large electrical resistance, problems such as heat generation occur especially when the current collector becomes thinner. There is a problem that it becomes obvious. Further, ferritic stainless steel foil is not economical even when compared with copper foil.
- the demand for thinning is particularly strong, so in conventional high-strength steel, the strength and electrical resistance after thinning are reduced. It is difficult to balance.
- Patent Document 9 discloses a copper-coated steel foil for supporting a negative electrode active material of a lithium ion secondary battery, but the strength of the foil does not satisfy a necessary level, and the strength of the foil is increased. The knowledge about coexistence and electrical resistance is not disclosed. In this technique, since the surface layer is coated with copper that is softer and inferior in heat resistance than steel, the strength after heating tends to decrease. Further, since the surface layer is coated with copper, the overdischarge solubility is only the same as that of the copper foil, and a remarkable improvement effect or the like by the disclosed configuration is not recognized.
- An object of the present invention is to provide a steel foil for a negative electrode current collector that uses both a thin, strong, lightweight and economical steel foil, and which has both a strength and an electric resistance that are normally in a trade-off relationship.
- the gist of the present invention that achieves the above object is as follows.
- the steel foil according to one embodiment of the present invention is, in mass%, C: 0.0001 to 0.02%, Si: 0.001 to 0.01%, Mn: 0.01 to 0.3% , P: 0.001 to 0.02%, S: 0.0001 to 0.01%, Al: 0.0005 to 0.1%, and N: 0.0001 to 0.004%,
- the steel foil described in the above (1) may further contain 0.1% or less of one or two of Ti and Nb by mass%.
- the steel foil according to (1) or (2) may further have a Ni plating layer or a Cr plating layer on the surface layer of the steel foil.
- the method for producing a steel foil according to another embodiment of the present invention is, in mass%, C: 0.0001 to 0.02%, Si: 0.001 to 0.01%, Mn: 0.01 to 0.3%, P: 0.001 to 0.02%, S: 0.0001 to 0.01%, Al: 0.0005 to 0.1%, and N: 0.0001 to 0.004% ,
- the steel sheet may further contain 0.1% or less of one or two of Ti and Nb by mass%.
- the method for manufacturing a steel foil according to (4) or (5) may further include a plating step of forming a Ni plating layer or a Cr plating layer on a surface layer of the steel foil after the foil rolling step. Good.
- the Ni plating layer may be a soft Ni plating layer.
- the method for manufacturing a steel foil according to (4) or (5) may further include a pre-rolling plating step of forming a Ni plating layer on a surface layer of the steel plate before the foil rolling step.
- the Ni plating layer may be a soft Ni plating layer.
- the rolled steel foil for a negative electrode current collector according to the present embodiment (hereinafter sometimes referred to as “steel foil according to the present embodiment”) has the following component composition (% is mass%) and has a thickness of 5 ⁇ m or more. It is characterized by being 15 ⁇ m or less and a tensile strength of more than 900 MPa and 1200 MPa or less.
- the manufacturing method of the steel foil which concerns on this embodiment performs cold rolling on the steel plate of the said component composition (mass%) with the cumulative rolling rate of 90% or more, thickness is 5 micrometers or more and 15 micrometers or less, and tensile strength. Is a steel foil of more than 900 MPa and not more than 1200 MPa.
- the steel foil according to this embodiment does not employ a strengthening mechanism such as solid solution strengthening, precipitation strengthening, or structure strengthening that is used in general high-strength steel materials.
- a strengthening mechanism such as solid solution strengthening, precipitation strengthening, or structure strengthening that is used in general high-strength steel materials.
- the content of elements that increase strength is suppressed to a level lower than that of conventional high-strength steel materials, and instead, strength is secured by using work hardening described later. This makes it possible to achieve both strength and electrical resistance.
- % means the mass%.
- C (C: 0.0001 to 0.02%) C is an element that increases the strength of the steel, but if contained excessively, the electrical resistance of the steel may deteriorate, so the upper limit of the C content is 0.02%.
- the lower limit of the C content is not particularly specified, but the limit in the current refining technology is about 0.0001%, so this was set as the lower limit.
- the C content is more preferably 0.001% to 0.01%.
- Si 0.001 to 0.01%
- Si is an element that increases the strength of steel, but if contained excessively, the electrical resistance of the steel may deteriorate, so the upper limit of Si content is 0.01%. If the Si content is less than 0.001%, the scouring cost increases, so the lower limit of the Si content is set to 0.001%.
- the Si content is more preferably 0.001% to 0.008%.
- Mn 0.01 to 0.3%) Mn is an element that increases the strength of steel, but if contained excessively, the electrical resistance of steel may deteriorate, so the upper limit of Mn content is set to 0.3%. If the Mn content is less than 0.01%, the refining cost becomes great, and the steel becomes too soft and rollability is lowered, which may lead to an increase in production cost. .01%.
- the Mn content is more preferably 0.05% to 0.2%.
- P is an element that increases the strength of the steel, but if contained excessively, the electrical resistance of the steel may deteriorate, so the upper limit of the P content is 0.02%. If the P content is less than 0.001%, the scouring cost may increase, so the lower limit of the P content is 0.001%.
- the P content is more preferably 0.001% to 0.01%.
- S is an element that lowers the hot workability and corrosion resistance of steel, the smaller the amount, the better. Furthermore, in the case of a thin steel foil such as the steel foil according to the present embodiment, if there is a large amount of S, the electrical resistance is deteriorated by inclusions due to the presence of S, or the strength of the steel is reduced. Therefore, the upper limit of the S content is 0.01%. If the S content is less than 0.0001%, the scouring cost may increase. Therefore, the lower limit of the S content is set to 0.0001%. The S content is more preferably 0.001% to 0.008%.
- Al 0.0005 to 0.1%)
- Al contains 0.0005% or more as a deoxidizing element of steel. If excessively contained, the electrical resistance deteriorates and the production cost may increase, so the upper limit of the Al content is 0.1%.
- the Al content is more preferably 0.01% to 0.05%.
- N 0.0001-0.004% Since N is an element that decreases the hot workability and workability of steel, the smaller the content, the better.
- the upper limit of the N content is 0.004%. If the N content is less than 0.0001%, the cost may increase, so the lower limit of the N content is 0.0001%.
- the N content is more preferably 0.001% to 0.003%.
- the balance of the components of the steel foil according to the present embodiment is Fe and impurities, but may further contain 0.1% or less of Ti and / or Nb.
- Ti and / or Nb can fix C and N in the steel as carbides and nitrides to improve the workability of the steel. However, when it adds excessively, the increase in manufacturing cost and the deterioration of electrical resistance may be caused.
- the preferred content ranges are Ti: 0.01 to 0.8%, Nb: 0.005 to 0.05%. More preferable content ranges are Ti: 0.01 to 0.1% and Nb: 0.005 to 0.04%.
- the steel foil according to the present embodiment may additionally contain B, Cu, Ni, Sn, Cr or the like as long as the characteristics of the steel foil according to the present embodiment are not impaired.
- the thickness of the steel foil according to this embodiment is 5 ⁇ m or more and 15 ⁇ m or less. This is because a thin current collector foil, that is, a thin steel foil is desired in reducing the size and weight of the battery. From the viewpoint of size reduction and weight reduction, the steel foil is preferably thinner, and there is no need to particularly limit the lower limit. However, when considering the uniformity of cost or thickness, 5 ⁇ m or more is preferable. In addition, when rolling the steel material which does not satisfy the component composition mentioned above and manufacturing steel foil, an electrical resistance may deteriorate notably in the area
- the tensile strength of the steel foil according to this embodiment is more than 900 MPa and not more than 1200 MPa.
- the tensile strength is a measured value at normal temperature.
- the tensile strength is 900 MPa or less, there is a possibility that the steel foil is deformed or the active material is peeled off due to the expansion and contraction of the active material accompanying charging and discharging. This tendency is remarkable when a high capacity negative electrode active material is applied to the steel foil.
- the steel foil according to the present embodiment has a certain degree of elongation, but even if it is not present (even if it is at an unmeasurable level), there is no problem in achieving the object of the present invention.
- the preferable elongation of the steel foil according to this embodiment is 0.1% or more.
- a current collector foil when a current collector foil is coated with an active material to produce an electrode, heat treatment at a maximum of about 400 ° C. may be performed.
- the steel foil according to the present embodiment has good heat resistance in addition to tensile strength, and even when subjected to a heat treatment of about 400 ° C., the strength hardly decreases, and even if the strength decreases, the maximum decrease in tensile strength is 10 %.
- the tensile strength reduction rate is a percentage of the tensile strength reduction amount with respect to the tensile strength before the heat treatment.
- the manufacturing method of the steel foil which concerns on this embodiment shown by FIG.1 and FIG.2 is as follows. First, a thin plate (steel plate) having a predetermined composition described above is manufactured according to a normal thin plate manufacturing method. Then, the above-mentioned thin plate is made into a steel foil of 5 ⁇ m or more and 15 ⁇ m or less by cold rolling (foil rolling) under large pressure. Utilizing work hardening caused by cold rolling under large pressure, a high strength of more than 900 MPa and 1200 MPa or less is achieved.
- the cumulative rolling rate during foil rolling is 90% or more.
- the cumulative rolling rate is a percentage of the cumulative reduction amount (the difference between the inlet plate thickness before the first pass and the outlet plate thickness after the final pass) with respect to the inlet plate thickness of the first rolling stand. If the cumulative rolling rate is less than 90%, sufficient foil strength is not exhibited.
- the cumulative rolling rate during foil rolling is preferably 95% or more.
- the upper limit of the cumulative rolling rate is not particularly limited. However, with normal rolling capacity, about 98% is the limit of the cumulative rolling rate that can be achieved.
- Cold rolling is performed by one or more passes, but if annealing is performed during rolling, the tensile strength may be insufficient. Therefore, it is preferable not to perform the annealing process during rolling. Since the steel foil according to the present embodiment has good rolling properties depending on its component composition, intermediate annealing is not necessary.
- the surface layer of the steel foil according to the present embodiment may be plated with Ni or Cr after foil rolling. Thereby, the metal elution property at the time of overdischarge can be improved. Depending on the type of plating, there is not only an improvement effect, but rather deterioration. In particular, Cu plating, Zn plating and the like cannot be used in the steel foil of the present invention. Further, the strength may decrease depending on the type of plating.
- a plating such as Ni or Cr
- pre-rolling plating it is possible to apply a plating such as Ni or Cr to the steel plate before foil rolling (pre-rolling plating), and to roll the steel plate (thin plate) having a plating layer on the surface layer under the above-mentioned conditions.
- careful attention is required for the selection of plating.
- the elongation of plating during foil rolling is smaller than the elongation of steel, defects such as cracks occur in the plating layer, and this defect may cause a decrease in foil strength.
- the foil strength may be significantly reduced when rolling is performed at a cumulative rolling rate of 90% or more. .
- the foil strength tends to decrease if the plating layer itself is too soft.
- the foil strength may still be adversely affected. If the elongation of the plating is smaller than the elongation of the steel foil, defects such as cracks may occur when the steel foil expands and contracts due to temperature changes. If the elongation of the plating is larger than the elongation of the steel foil, the foil strength tends to decrease.
- soft Ni plating is particularly suitable. Specifically, pure Ni plating containing no impurities other than those deposited on the steel plate is subjected to a heat treatment at 300 ° C. or higher, whereby the Ni plating in which the strain of the plating layer is released is referred to as soft Ni plating in this embodiment. To do.
- foil rolling of a steel sheet is performed in a state where plating other than Ni plating or Cr plating is adhered, the foil strength is lowered for the reasons described above, and the target performance of the present invention may not be obtained. Moreover, even when plating other than Ni plating or Cr plating is performed on the steel foil after foil rolling, the foil strength may be lowered due to the above-described reason.
- the preferable adhesion amount range of the Ni plating adhered on the steel foil according to the present embodiment is 1 g / m 2 or more.
- the more preferable adhesion amount of Ni plating is 5 g / m 2 or more and 20 g / m 2 or less.
- the preferable adhesion amount range of Cr plating adhered on the steel foil according to the present embodiment is 0.01 g / m 2 or more.
- the adhesion amount of Cr plating exceeds 0.5 g / m 2 , the crack of the plating layer on the steel foil increases, and the effect of improving the metal dissolution property is lost due to this crack, and the foil strength is reduced. There is. From the viewpoint of metal elution, a remarkable effect is observed with Cr plating with a smaller amount of deposition than with Ni plating.
- a more preferable adhesion amount of Cr plating is 0.1 g / m 2 or more and 0.3 g / m 2 or less.
- Example 1 Cold rolled steel sheets (annealed materials) having the component compositions shown in Table 1 were manufactured by a normal sheet manufacturing method, and then foil rolling was performed. Table 1 also shows the original thickness of the cold-rolled steel sheet, the cumulative rolling rate of foil rolling, and the thickness of the foil.
- Overdischarge solubility A tripolar beaker cell was assembled in a glove box in an argon atmosphere (dew point -60 ° C). A working electrode was obtained by tape-sealing the edge and back surface of each test material. Metal lithium was used as a counter electrode and a reference electrode.
- electrolytic solution a solution obtained by dissolving 1 mol / L LiPF 6 in a mixed solvent of ethylene carbonate and diethyl carbonate having a volume ratio of 1: 1 was used.
- the cell was held at 25 ° C., scanned from the immersion potential in a noble direction at 5 mV / sec, and a potential at which a current of 0.01 mA / cm 2 flowed was measured.
- the dissolution potential was expressed as a Li reference potential (V).
- Foil strength In parallel with the rolling direction, a 13B tensile test piece described in JIS Z 2201 was collected, and the tensile strength was determined according to JIS Z2241. The tensile strength of each of the steel foil as it was (the steel foil which was rolled only) and the steel foil after heating at 400 ° C. for 30 minutes was determined. The tensile strength after heating was determined as a reference value because the steel foil may be heated in the battery manufacturing process. However, since the value of the tensile strength required for the steel foil after heating differs depending on the battery, no pass / fail judgment was made regarding the tensile strength of the steel foil after heating.
- Volume resistivity was measured at 20 ° C. by the four probe method.
- a sample with an electrical resistance of less than 14 ⁇ cm is grade A
- a sample with an electrical resistance of 14 ⁇ cm to less than 16 ⁇ cm is Grade B
- a sample with an electrical resistance of 16 ⁇ cm to less than 20 ⁇ cm is Grade C
- a sample with an electrical resistance of 20 ⁇ cm or more is rated as Grade D Grade A and B samples were accepted.
- Table 1 shows the tensile strength and electrical resistance.
- Table 1 shows the tensile strength and electrical resistance.
- the overdischarge solubility since all the examples were better than the Cu foil and there was no great difference between the levels, it was not shown in Table 1 (the test was conducted for the Cu foil of 3.4 V). (Examples and comparative examples are 3.5 to 3.6 V).
- both tensile strength and electrical resistance which are likely to be in a trade-off relationship, can be achieved. What deviates from the scope of the present invention cannot achieve both tensile strength and electrical resistance.
- Examples 22 to 25 and Comparative Example 10 Various platings were formed on the steel foil produced in Example 1 by electroplating.
- the Ni plating conditions are as follows. Using a bath composed of Ni sulfate: 320 g / l, Ni chloride: 70 g / l, boric acid: 40 g / l, various deposition amounts of Ni were plated at a bath temperature of 65 ° C. and a current density of 20 A / dm 2 . .
- the Cr plating conditions are as follows. Using a bath composed of chromic anhydride: 150 g / l and sulfuric acid: 1.5 g / l, various deposits of Cr were plated at a bath temperature of 50 ° C. and a current density of 50 A / dm 2 .
- the Zn plating conditions are as follows. Zn was plated at a bath temperature of 60 ° C. and a current density of 50 A / dm 2 using a bath composed of Zn sulfate: 250 g / l, sulfuric acid: 15 g / l, sodium sulfate: 50 g / l.
- Example 12 For the steel foil produced in Example 19, 1 g / m in a plating bath consisting of copper pyrophosphate: 80 g / l, potassium pyrophosphate: 300 g / l, aqueous ammonia: 3 ml / l in advance. 2 Cu strike plating, and then using a bath composed of copper sulfate: 210 g / l, sulfuric acid: 45 g / l, and a 20 g / m 2 Cu plating at a liquid temperature of 40 ° C. and a current density of 10 A / dm 2 . went.
- a plating bath consisting of copper pyrophosphate: 80 g / l, potassium pyrophosphate: 300 g / l, aqueous ammonia: 3 ml / l in advance. 2 Cu strike plating, and then using a bath composed of copper sulfate: 210 g / l, sulfuric acid: 45
- the evaluation method is the same as the previous example.
- overdischarge solubility could be improved from the Cu level (3.4 V) by plating with Ni or Cr.
- the Zn-plated one was worse in overdischarge solubility than Cu.
- Those subjected to Cu plating had the same level of overdischarge solubility as Cu, and no improvement effect was found.
- the tensile strength after heating of the steel foil plated with Zn decreased. This is because Zn forms a brittle Zn—Fe intermetallic compound layer by heating, and the breakage of this layer causes the steel foil to break. Those plated with Cu also had a reduced tensile strength. This is because Cu, which is extremely soft compared to steel, is present in the surface layer. Since Cu was further softened by heating, the tensile strength of the steel foil further decreased after heating.
- Examples 30 to 33 and Comparative Examples 13 to 14 Various types of plating were formed on the cold-rolled steel sheet (annealed material, 0.3 mm) used in Example 1.
- the Ni plating treatment was performed under the same conditions as in the previous example.
- the plating conditions for Ni—P are as follows.
- the evaluation method is the same as the previous example.
- the overdischarge solubility could be improved from the Cu level (3.4 V). Further, there was no decrease in tensile strength due to plating with Ni. However, as shown in the comparative example, the tensile strength was significantly reduced in the case where Ni—P was plated.
- Ni—P is amorphous and very hard when plated (when only plating is performed). Further, when heated, Ni—P becomes harder due to precipitation of the Ni 3 P compound. When rolling with a high cumulative rolling rate was performed with such a layer in the surface layer, cracks occurred frequently in the plating layer, and these cracks reached the steel foil of the base material, resulting in a decrease in tensile strength.
- a thin, strong, lightweight and economical steel foil can be obtained.
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Abstract
Description
本願は、2012年4月19日に日本にて出願された特願2012-095840号に基づき優先権を主張し、その内容をここに援用する。
Si:0.001~0.01%、
Mn:0.01~0.3%、
P:0.001~0.02%、
S:0.0001~0.01%、
Al:0.0005~0.1%、
N:0.0001~0.004%、及び、
残部Fe及び不純物。
Cは、鋼の強度を高める元素であるが、過剰に含有させると鋼の電気抵抗が悪化する場合があるので、C含有量の上限を0.02%とする。C含有量の下限は、特に規定されないが、現行の精錬技術における限界が0.0001%程度であるので、これを下限とした。C含有量は、より好ましくは0.001%~0.01%である。
Siは、鋼の強度を高める元素であるが、過剰に含有させると鋼の電気抵抗が悪化する場合があるので、Si含有量の上限を0.01%とする。Si含有量を0.001%未満にすると、精練コストが多大となるので、Si含有量の下限は0.001%とする。Si含有量は、より好ましくは0.001%~0.008%である。
Mnは、鋼の強度を高める元素であるが、過剰に含有させると鋼の電気抵抗が悪化する場合があるので、Mn含有量の上限を0.3%とする。Mn含有量を0.01%未満にすると、精練コストが多大となるとともに、鋼が軟質化しすぎて圧延性が低下し、製造コストの増大を招く場合があるので、Mn含有量の下限は0.01%とする。Mn含有量は、より好ましくは0.05%~0.2%である。
Pは、鋼の強度を高める元素であるが、過剰に含有させると鋼の電気抵抗が悪化する場合があるので、P含有量の上限を0.02%とする。P含有量を0.001%未満にすると、精練コストが多大となる場合があるので、P含有量の下限は0.001%とする。P含有量は、より好ましくは0.001%~0.01%である。
Sは、鋼の熱間加工性及び耐食性を低下させる元素であるから、少ないほど好ましい。さらに、本実施形態に係る鋼箔のような薄い鋼箔の場合、Sが多いと、Sの存在に起因する介在物によって電気抵抗が悪化したり、また、鋼の強度が低下したりする場合があるので、S含有量の上限は0.01%とする。S含有量を0.0001%未満にすると、精練コストが多大となる場合があるので、S含有量の下限は0.0001%とする。S含有量は、より好ましくは0.001%~0.008%である。
Alは、鋼の脱酸元素として0.0005%以上を含有させる。過剰に含有させると、電気抵抗が悪化し、また、製造コストの増大を招く場合があるので、Al含有量の上限は0.1%とする。Al含有量は、より好ましくは0.01%~0.05%である。
Nは、鋼の熱間加工性及び加工性を低下させる元素であるから、少ないほど好ましく、N含有量の上限は0.004%とする。N含有量を0.0001%未満にすると、コストが多大となる場合があるので、N含有量の下限は0.0001%とする。N含有量は、より好ましくは0.001%~0.003%である。
本実施形態に係る鋼箔の成分の残部は,Fe及び不純物であるが、さらにTi及び/又はNbを0.1%以下含有することができる。Ti及び/又はNbは、鋼中のC及びNを炭化物及び窒化物として固定して、鋼の加工性を向上させることができる。ただし、過剰に添加すると、製造コストの増大、及び電気抵抗の悪化を招く場合がある。好ましい含有量範囲は、Ti:0.01~0.8%、Nb:0.005~0.05%である。さらに好ましい含有量範囲は、Ti:0.01~0.1%、Nb:0.005~0.04%である。
なお、めっきの伸びが鋼箔の伸びに比較して小さい、又は大きい場合、このめっきが箔圧延後に施された場合であっても、やはり箔強度に悪影響を及ぼす場合がある。めっきの伸びが鋼箔の伸びに比較して小さいと、鋼箔が温度変化によって伸縮した場合に、クラックなどの欠陥が発生する可能性がある。めっきの伸びが鋼箔の伸びに比較して大きいと、やはり箔強度が低下しやすい。
通常の薄板製造方法で、表1に示す成分組成の冷延鋼板(焼鈍材)を製造し、次いで、箔圧延を行った。冷延鋼板の元厚さ、箔圧延の累積圧延率、及び、箔の厚さも、表1に示す。
過放電溶解性:アルゴン雰囲気(露点-60℃)のグローブボックス内にて、三極式ビーカーセルを組み立てた。各供試材のエッジと裏面とをテープシールしたものを作用極とした。対極及び参照極としては金属リチウムを用いた。電解液としては、1mol/LのLiPF6を、体積比で1:1のエチレンカーボネートとジエチルカーボネートとの混合溶媒に溶解させたものを用いた。
実施例1で製造した鋼箔に対して、各種のめっきを電気めっき法で形成した。Niめっき条件は、次の通りである。硫酸Ni:320g/l、塩化Ni:70g/l、ほう酸:40g/lからなる浴を用い、浴温度:65℃、電流密度:20A/dm2にて、種々の付着量のNiをめっきした。
実施例9で製造した鋼箔に対して、先の例と同様の手法で各種のめっき処理を行った。
(比較例12)実施例19で製造した鋼箔に対して、予め、ピロリン酸銅:80g/l、ピロリン酸カリウム:300g/l、アンモニア水:3ml/lからなるめっき浴にて1g/m2のCuストライクめっきを行い、次いで、硫酸銅:210g/l、硫酸:45g/lからなる浴を用い、液温:40℃、電流密度10A/dm2にて20g/m2のCuめっきを行った。
実施例1で用いた冷延鋼板(焼鈍材、0.3mm)に対して、各種のめっきを形成した。Niめっき処理は、先の例と同条件で行った。Ni-Pのめっき条件は、次の通りである。
2 めっき工程
3 圧延前めっき工程
Claims (9)
- 質量%で、
C:0.0001~0.02%、
Si:0.001~0.01%、
Mn:0.01~0.3%、
P:0.001~0.02%、
S:0.0001~0.01%、
Al:0.0005~0.1%、及び、
N:0.0001~0.004%、を含み、
残部:Fe及び不純物からなる鋼箔であって、
厚さが5μm以上15μm以下、且つ引張強度が900MPa超1200MPa以下であることを特徴とする鋼箔。 - 前記鋼箔が、さらに、質量%で、Ti及びNbの1種又は2種をそれぞれ0.1%以下含有することを特徴とする請求項1に記載の鋼箔。
- 前記鋼箔の表層に、Niめっき層又はCrめっき層を有することを特徴とする請求項1又は2に記載の鋼箔。
- 質量%で、
C:0.0001~0.02%、
Si:0.001~0.01%、
Mn:0.01~0.3%、
P:0.001~0.02%、
S:0.0001~0.01%、
Al:0.0005~0.1%、及び、
N:0.0001~0.004%、を含み、
残部:Fe及び不純物からなる鋼板に、90%以上98%以下の累積圧延率で冷間圧延を施し、厚さが5μm以上15μm以下、且つ引張強度が900MPa超1200MPa以下の鋼箔とする箔圧延工程
を含むことを特徴とする鋼箔の製造方法。 - 前記鋼板が、さらに、質量%で、Ti及びNbの1種又は2種を0.1%以下含有することを特徴とする請求項4に記載の鋼箔の製造方法。
- 前記箔圧延工程後に、前記鋼箔の表層に、Niめっき層又はCrめっき層を形成するめっき工程をさらに含むことを特徴とする請求項4又は5に記載の鋼箔の製造方法。
- 前記Niめっき層が軟質Niめっき層であることを特徴とする請求項6に記載の鋼箔の製造方法。
- 前記箔圧延工程前に、前記鋼板の表層にNiめっき層を形成する圧延前めっき工程をさらに含むことを特徴とする請求項4又は5に記載の鋼箔の製造方法。
- 前記Niめっき層が軟質Niめっき層であることを特徴とする請求項8に記載の鋼箔の製造方法。
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WO2021200506A1 (ja) * | 2020-03-31 | 2021-10-07 | 日鉄ケミカル&マテリアル株式会社 | ニッケル水素二次電池集電体用Niめっき鋼箔、ニッケル水素二次電池集電体、及びニッケル水素二次電池 |
JP7474096B2 (ja) | 2020-03-31 | 2024-04-24 | 日鉄ケミカル&マテリアル株式会社 | ニッケル水素二次電池集電体用Niめっき鋼箔、ニッケル水素二次電池集電体、及びニッケル水素二次電池 |
JP7475931B2 (ja) | 2020-03-31 | 2024-04-30 | 日鉄ケミカル&マテリアル株式会社 | ニッケル水素二次電池集電体用Niめっき鋼箔、ニッケル水素二次電池集電体、及びニッケル水素二次電池 |
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Also Published As
Publication number | Publication date |
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CN103857818A (zh) | 2014-06-11 |
KR20140068114A (ko) | 2014-06-05 |
CN103857818B (zh) | 2016-03-23 |
US20150037684A1 (en) | 2015-02-05 |
EP2743365B1 (en) | 2020-09-16 |
JP6124801B2 (ja) | 2017-05-10 |
KR101599166B1 (ko) | 2016-03-02 |
JPWO2013157598A1 (ja) | 2015-12-21 |
US9997786B2 (en) | 2018-06-12 |
EP2743365A4 (en) | 2015-12-09 |
EP2743365A1 (en) | 2014-06-18 |
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