WO2014002997A1 - Feuille de cuivre électrolytique, son procédé de fabrication, électrode négative pour batterie secondaire au lithium-ion et batterie secondaire au lithium-ion - Google Patents

Feuille de cuivre électrolytique, son procédé de fabrication, électrode négative pour batterie secondaire au lithium-ion et batterie secondaire au lithium-ion Download PDF

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Publication number
WO2014002997A1
WO2014002997A1 PCT/JP2013/067380 JP2013067380W WO2014002997A1 WO 2014002997 A1 WO2014002997 A1 WO 2014002997A1 JP 2013067380 W JP2013067380 W JP 2013067380W WO 2014002997 A1 WO2014002997 A1 WO 2014002997A1
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Prior art keywords
copper foil
electrolytic copper
secondary battery
ion secondary
electrolytic
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PCT/JP2013/067380
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English (en)
Japanese (ja)
Inventor
季実子 藤澤
昭頼 橘
健作 篠崎
鈴木　昭利
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古河電気工業株式会社
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Priority to JP2013541901A priority Critical patent/JP5503814B1/ja
Publication of WO2014002997A1 publication Critical patent/WO2014002997A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C9/00—Alloys based on copper
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D1/00—Electroforming
    • C25D1/04—Wires; Strips; Foils
    • 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
    • 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
    • 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 electrolytic copper foil having high strength and high conductivity, a method for producing the same, a negative electrode using the electrolytic copper foil, and a lithium ion secondary battery incorporating the negative electrode.
  • a lithium (Li) ion secondary battery includes, for example, a positive electrode, a negative electrode having a negative electrode active material layer formed on the surface of a negative electrode current collector, and a non-aqueous electrolyte. Is used.
  • the negative electrode of the lithium ion secondary battery is formed, for example, by applying carbon particles as a negative electrode active material layer on the surface of a negative electrode current collector made of a copper foil having smooth surfaces, drying, and pressing.
  • a so-called “untreated electrolytic copper foil” manufactured by electrolysis is subjected to a rust prevention treatment.
  • a negative electrode active material for a lithium ion secondary battery development of a next-generation negative electrode active material having a charge / discharge capacity that greatly exceeds the theoretical capacity of a carbon material is underway.
  • a material containing a metal that can be alloyed with lithium such as silicon (Si) or tin (Sn) is expected.
  • Patent Documents 1 to 11 describe an electrolytic copper foil used for a negative electrode current collector of a lithium ion secondary battery.
  • an object of the present invention is to provide an electrolytic copper foil having high strength and high conductivity.
  • Another object of the present invention is to provide a negative electrode using the electrolytic copper foil of the present invention having high strength (tensile strength) and high conductivity as a current collector, and a lithium ion secondary battery incorporating the negative electrode.
  • the electrolytic copper foil of this invention can be preferably used also as a copper foil for circuit boards as uses other than the collector for batteries, for example.
  • the electrolytic copper foil of the present invention has an average number of intersection points of an arbitrary line segment having a length of 500 nm and a twin plane which is a (111) ⁇ 3 grain boundary in a transmission electron microscope (TEM) observation image. It is.
  • the average number of intersections between an arbitrary line segment having a length of 500 nm and a twin plane which is a (111) ⁇ 3 grain boundary in a transmission electron microscope (TEM) observation image is larger.
  • a preferred range is 10 to 36.
  • the method for producing an electrolytic copper foil of the present invention includes an electrolytic solution containing copper and sulfuric acid, containing 20 to 50 ppm of chlorine, 1 to 10 ppm of a thiourea compound, and 1 to 20 ppm of a water-soluble polymer compound as additives.
  • the average number of intersections between an arbitrary line segment having a length of 500 nm and a twin plane which is a (111) ⁇ 3 grain boundary is 5 to 40 in a transmission electron microscope (TEM) observation image after electrolytic treatment with a plating solution.
  • the electrolytic copper foil production method is for producing an electrolytic copper foil of 10 to 36.
  • the electrolytic copper foil which raised tensile strength and electrical conductivity can be provided.
  • the electrolytic copper foil of the present invention with increased tensile strength and conductivity as a current collector it is possible to provide a lithium ion secondary battery with increased battery capacity and improved charge / discharge characteristics of the secondary battery. .
  • FIG. 1 is a TEM image according to the example.
  • FIG. 2 is an explanatory diagram showing the intersection of the line segment and the (111) ⁇ 3 grain boundary by drawing a line segment on the TEM image according to the example.
  • the electrolytic copper foil of the present embodiment is a copper foil suitable as a negative electrode current collector of a lithium ion secondary battery.
  • the crystal structure of the cross section that is, an observation image with a transmission electron microscope (TEM) ⁇ hereinafter simply referred to as “TEM image”.
  • TEM image The average number of intersections between an arbitrary line segment having a length of 500 nm and a twin plane that is a (111) ⁇ 3 grain boundary is 5 to 40, more preferably 10 to 36. is there.
  • the average number of intersections between an arbitrary line segment having a length of 500 nm and a twin plane which is a (111) ⁇ 3 grain boundary is first shown in a TEM image as shown in FIG. An arbitrary line segment having a length of 500 nm is entered, and the number of intersections with the twin plane which is the (111) ⁇ 3 grain boundary is obtained. Next, three similar lines are drawn while rotating by 60 ° around the midpoint of the line segment, and the number of intersections between each line segment and the twin plane is obtained. This is a value obtained by averaging the number of intersections.
  • a large number of (111) ⁇ 3 grain boundaries are introduced into a metal structure having many nano-sized crystal grains, and the average number of intersections between an arbitrary line segment having a length of 500 nm and a twin plane that is a (111) ⁇ 3 grain boundary
  • the ratio By setting the ratio to 5 to 40, it is possible to set the conductivity suitable for use for a secondary battery while improving the tensile strength, which is a typical index of mechanical strength.
  • the average particle diameter of the copper particles constituting the electrolytic copper foil is 5 to 200 nm.
  • An average particle size of less than 5 nm is not preferable because the conductivity is low.
  • it exceeds 200 nm the tensile strength decreases, which is not preferable.
  • the electrolytic copper foil of the present embodiment preferably has a tensile strength of 500 to 900 MPa.
  • the tensile strength is 500 to 900 MPa, it can be preferably used as a battery structural member and other electronic device material even when it is thinned.
  • the tensile strength is less than 500 MPa, the strength of the structural member is insufficient, and when it exceeds 900 MPa, defects such as cracks are likely to occur during processing.
  • the electrolytic copper foil of the present embodiment has a tensile strength of more preferably 600 to 800 MPa. When the pressure is 600 to 800 MPa, the durability is further enhanced and the battery capacity can be further increased.
  • the electrolytic copper foil of this embodiment preferably has a conductivity of 60% IACS or higher.
  • the conductivity By setting the conductivity to 60% IACS or more, it is possible to suppress heat generated when used as an electronic device while having sufficient conductivity.
  • the electrical conductivity is 60% IACS or less, heat is generated due to electric resistance, or when used as a current collector for a lithium ion secondary battery, problems such as a decrease in output voltage due to IR drop occur.
  • the electrolytic copper foil of the present embodiment has a conductivity of 70% IACS or more more preferably. When it is at least 70% IACS, the charge / discharge characteristics are further enhanced when used as a lithium ion secondary battery.
  • the average number of intersections between an arbitrary line segment having a length of 500 nm and a twin plane which is a (111) ⁇ 3 grain boundary is 5 to 40, so that the above preferable tensile Strength and appropriate electrical conductivity can be realized.
  • strength high electrical conductivity electrolytic copper foil of this embodiment is provided with the antirust process layer on the surface.
  • the antirust treatment layer is, for example, a chromate treatment layer, or a Ni or Ni alloy plating layer, a Co or Co alloy plating layer, a Zn or Zn alloy plating layer, a Sn or Sn alloy plating layer, or the above various plating layers.
  • It is an inorganic rust prevention treatment such as one provided with a chromate treatment layer, or an organic rust prevention treatment layer such as benzotriazole.
  • a silane coupling agent treatment layer or the like may be formed.
  • the inorganic rust prevention treatment, organic rust prevention treatment, and silane coupling agent treatment increase the adhesion strength with the active material when used as a lithium ion secondary battery, and also prevent the charge / discharge cycle efficiency of the battery from decreasing. Fulfill.
  • the high-strength, high-conductivity electrolytic copper foil of the present embodiment is subjected to a roughening treatment on the surface on which the active material layer of the electrolytic copper foil is provided, and a rust-proofing treatment layer is provided on the surface subjected to the roughening treatment. Is provided.
  • the electrolytic copper foil of the present embodiment is, for example, an insoluble anode made of titanium coated with a white metal element or an oxide element thereof using a sulfuric acid-copper sulfate aqueous solution as an electrolytic solution, and a titanium cathode provided facing the anode. While supplying the electrolytic solution between the drum and rotating the cathode drum at a constant speed, a direct current is passed between the two electrodes to deposit copper on the surface of the cathode drum, and the deposited copper is removed from the surface of the cathode drum. It is manufactured by a method of peeling and continuously winding.
  • the electrolytic copper foil of the present embodiment can be produced, for example, by performing electrolytic treatment in a sulfuric acid-copper sulfate electrolytic plating solution.
  • the current density during the electrolytic treatment is preferably 30 to 70 A / dm 2 .
  • the copper concentration of the sulfuric acid-copper sulfate electroplating solution is, for example, in the range of 40 to 120 g / L, and preferably in the range of 60 to 100 g / L.
  • the sulfuric acid concentration in the sulfuric acid-copper sulfate electroplating solution is, for example, in the range of 40 to 60 g / L.
  • This sulfuric acid concentration is an important condition, and if it is less than this range, the conductivity of the plating solution will be lowered, so that the uniform electrodeposition of the copper foil will be reduced, and N (nitrogen) and S ( This is not preferable because the effect of the sulfur-containing additive is hardly exhibited, and the strength of the copper foil is reduced and the crystal orientation is randomized.
  • the chlorine concentration of the sulfuric acid-copper sulfate electroplating solution for example, a range of 20 to 50 ppm is used. Moreover, both the organic additives A and B shown below are used.
  • the organic additive A is an organic compound containing at least one N (nitrogen) atom and S (sulfur) atom in one molecule. By adding an appropriate amount of at least one organic additive A, a large number of (111) ⁇ 3 grain boundaries can be introduced into the metal structure of the produced electrolytic copper foil.
  • the organic additive A is desirably a thiourea compound, and more desirably a thiourea compound having 3 or more carbon atoms. Examples of the organic additive A include thiourea (CH 4 N 2 S), N, N′-dimethylthiourea (C 3 H 8 N 2 S), N, N′-diethylthiourea (C 5 H 12 N 2 S).
  • thiourea (C 5 H 12 N 2 S ), tetramethyl thiourea (C 5 H 12 N 2 S ), thiosemicarbazide Sid (CH 5 N 3 S), N- allyl thiourea (C 4 H 8 N 2 S ), ethylene thiourea (C 3 H 6 N 2 S) is a water-soluble thiourea or a thiourea compound such as a thiourea derivative.
  • the additive A added to the electrolytic plating solution one or more selected from these thiourea compounds are used.
  • Organic additives B include, for example, glue, gelatin, polyethylene glycol, polypropylene glycol, starch, high molecular polysaccharides such as cellulose water-soluble polymers (carboxyl methyl cellulose, hydroxyethyl cellulose, etc.), polyethylene imine, polyamine polymers, poly Water-soluble polymer compounds such as acrylamide.
  • additive B to be added to the electroplating solution one or more selected from these water-soluble polymer compounds are used.
  • organic additive B in addition to organic additive A a large number of (111) ⁇ 3 grain boundaries can be introduced into the metal structure of the produced electrolytic copper foil.
  • a TEM image is obtained by performing electrolytic treatment with an electrolytic plating solution containing copper and sulfuric acid, containing 20 to 50 ppm of chlorine, 1 to 10 ppm of a thiourea compound, and 1 to 20 ppm of a water-soluble polymer compound.
  • an electrolytic copper foil having an average number of intersection points between an arbitrary line segment having a length of 500 nm and a twin plane which is a (111) ⁇ 3 grain boundary can be produced.
  • the heat resistance can be further improved by adding a transition metal element to the sulfuric acid-copper sulfate electroplating solution.
  • the metal element to be added is preferably an element in which an oxide is stable in a sulfuric acid aqueous solution, and more preferably an element capable of stably taking a trivalent or higher polyvalent oxide.
  • the average number of intersections between an arbitrary line segment having a length of 500 nm and a twin plane which is a (111) ⁇ 3 grain boundary in a TEM image is 5 to 40.
  • the surface on the side where the electrolytic copper foil is in contact with the surface of the cathode drum at the time of manufacture is referred to as the S surface (glossy surface), and the opposite surface is referred to as the M surface (matt surface).
  • the produced electrolytic copper foil for example, chromate treatment, Ni or Ni alloy plating, Co or Co alloy plating, Zn or Zn alloy plating, Sn or Sn alloy plating, or the above various types
  • An inorganic rust prevention treatment such as a chromate treatment on the plating layer, or an organic rust prevention treatment such as benzotriazole.
  • the silane coupling agent process etc. are given, for example, and it uses as an electrolytic copper foil for lithium ion secondary battery negative electrode collectors.
  • the inorganic rust prevention treatment, organic rust prevention treatment, and silane coupling agent treatment increase the adhesion strength with the active material and prevent the charge / discharge cycle efficiency of the battery from being lowered.
  • a roughening process is performed to the electrolytic copper foil surface, for example.
  • a plating method, an etching method, or the like can be suitably employed.
  • the plating method is a method of roughening the surface by forming a thin film layer having irregularities on the surface of the untreated electrolytic copper foil.
  • an electrolytic plating method and an electroless plating method can be employed.
  • a method of forming a plating film mainly composed of copper such as copper or copper alloy on the surface of the untreated electrolytic copper foil is preferable.
  • a roughening method by plating generally used for copper foil for printed circuits disclosed in Patent Document 7 is preferably used. That is, after forming a granular copper plating layer by so-called “bake plating”, “cover plating” is performed on this granular copper plating layer so as not to impair the uneven shape, thereby substantially smoothing.
  • a method by physical etching or chemical etching is suitable.
  • physical etching there is a method of etching by sandblasting or the like, and for chemical etching, many liquids containing an inorganic or organic acid, an oxidizing agent, and an additive have been proposed.
  • Patent Literature 8 discloses a corrosion inhibitor such as an inorganic acid + hydrogen peroxide + triazole + a surfactant.
  • Patent Document 9 discloses a liquid containing inorganic acid + peroxide + azole + halide.
  • (111) ⁇ 3 so that the average number of intersections between an arbitrary line segment having a length of 500 nm in a TEM image and a twin plane that is a (111) ⁇ 3 grain boundary is 5 to 40.
  • an electrolytic copper foil with improved tensile strength and electrical conductivity can be obtained.
  • durability is improved, battery capacity is increased, and charging / discharging is performed.
  • a lithium ion secondary battery with improved characteristics can be manufactured.
  • the observation of the metal structure when obtaining the number of intersections between an arbitrary line segment having a length of 500 nm in the TEM image and the twin plane which is the (111) ⁇ 3 grain boundary is performed by a transmission electron microscope (TEM). It carried out in.
  • a TEM image is shown in FIG.
  • the number of intersections with the (111) ⁇ 3 grain boundary is an arbitrary line segment having a length of 500 nm on the structure to be observed, and the twin plane that is the (111) ⁇ 3 grain boundary. Find the number of intersections with.
  • the average crystal grain size can be measured by, for example, an intercept method. In the intercept method, an arbitrary line segment is drawn on the structure to be observed, and the average crystal grain size is obtained from the length of the line segment and the number of crystal grains intersecting with the line segment.
  • the tensile strength is a value measured by a method defined in the IPC standard (IPC-TM-650).
  • the conductivity is calculated from the specific resistance obtained based on the IPC standard (IPC-TM-650).
  • Comparative Examples 1 to 3 an untreated copper foil having a thickness of 20 ⁇ m was produced from an electrolytic solution having the composition shown in Table 1.
  • 2M-5S is 2-mercapto-5-benzimidazolesulfonic acid
  • SPS is bis (3-sulfopropyl) disulfide
  • DDAC diallyldimethylammonium chloride.
  • the presence or absence of the (111) ⁇ 3 grain boundary and the number of intersections were determined by observing the metal structure with a transmission electron microscope with an observation field of 100 to 360,000 times.
  • the (111) ⁇ 3 grain boundary was defined as a continuous and linear line of 10 nm or more in the metal structure observation.
  • the “number of intersection points” is an arbitrary line segment having a length of 500 nm on the structure to be observed, and the number of intersection points with the twin plane which is the (111) ⁇ 3 grain boundary.
  • a similar line is drawn while rotating by 60 ° around the midpoint of the line segment, the number of intersections between each line segment and the twin plane is obtained, and the twin plane intersecting each line is determined. The number of intersections was averaged to obtain the “number of intersections”.
  • the conductivity is a value calculated from the specific resistance obtained based on the IPC standard (IPC-TM-650). In the comprehensive evaluation, “Good” indicates that both the tensile strength and the electrical conductivity are good, “Fair” indicates that the tensile strength and electrical conductivity are good, and “Poor” indicates that one of them is defective.
  • Examples 1 to 11 in which the average number of intersection points between an arbitrary line segment having a length of 500 nm in a TEM image and a twin plane which is a (111) ⁇ 3 grain boundary are 5 to 40 are as follows: Both tensile strength and electrical conductivity were good. On the other hand, in Comparative Examples 1 to 3, either the tensile strength or the conductivity was poor.
  • the electrolytic copper foil of the present invention can be preferably used for applications other than lithium ion secondary batteries, for example, as a copper foil for circuit boards and electronic device materials.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Mechanical Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Cell Electrode Carriers And Collectors (AREA)

Abstract

L'invention concerne une feuille de cuivre électrolytique présentant une résistance à la traction et une conductivité électrique supérieures, et son procédé de fabrication. L'invention concerne également une batterie secondaire au lithium-ion utilisant une électrode négative qui fait appel à la feuille de cuivre électrolytique précédemment mentionnée comme collecteur. Dans une image par microscopie électronique en transmission (MET) de cette feuille de cuivre électrolytique, le nombre moyen d'intersections entre un segment de droite arbitraire de 500 nm de long et des plans doubles qui sont des joints de grain (111) Σ3, est compris entre 5 et 40, inclus. La batterie secondaire au lithium-ion précédemment mentionnée fait appel à une électrode négative qui utilise ladite feuille de cuivre électrolytique comme collecteur.
PCT/JP2013/067380 2012-06-27 2013-06-25 Feuille de cuivre électrolytique, son procédé de fabrication, électrode négative pour batterie secondaire au lithium-ion et batterie secondaire au lithium-ion WO2014002997A1 (fr)

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JP2013541901A JP5503814B1 (ja) 2012-06-27 2013-06-25 電解銅箔とその製造方法、リチウムイオン二次電池の負極電極、およびリチウムイオン二次電池

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JP2012-144609 2012-06-27
JP2012144609 2012-06-27

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Publication number Priority date Publication date Assignee Title
JP7085394B2 (ja) * 2018-04-13 2022-06-16 東洋鋼鈑株式会社 積層電解箔
CN110592621B (zh) * 2019-09-03 2021-08-03 南京理工大学 采用高频脉冲制备纳米孪晶铜层的方法

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001011685A (ja) * 1999-06-30 2001-01-16 Mitsui Mining & Smelting Co Ltd 電解銅箔およびその製造方法
JP2001123289A (ja) * 1999-10-27 2001-05-08 Dowa Mining Co Ltd 電解銅箔およびその製造方法
JP2001181886A (ja) * 1999-12-28 2001-07-03 Mitsui Mining & Smelting Co Ltd 電解銅箔
JP2002053993A (ja) * 2000-08-04 2002-02-19 Mitsui Mining & Smelting Co Ltd 電解銅箔およびその製造方法
JP2009299100A (ja) * 2008-06-10 2009-12-24 Mitsui Mining & Smelting Co Ltd 電解銅箔及びその電解銅箔の製造方法

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001011685A (ja) * 1999-06-30 2001-01-16 Mitsui Mining & Smelting Co Ltd 電解銅箔およびその製造方法
JP2001123289A (ja) * 1999-10-27 2001-05-08 Dowa Mining Co Ltd 電解銅箔およびその製造方法
JP2001181886A (ja) * 1999-12-28 2001-07-03 Mitsui Mining & Smelting Co Ltd 電解銅箔
JP2002053993A (ja) * 2000-08-04 2002-02-19 Mitsui Mining & Smelting Co Ltd 電解銅箔およびその製造方法
JP2009299100A (ja) * 2008-06-10 2009-12-24 Mitsui Mining & Smelting Co Ltd 電解銅箔及びその電解銅箔の製造方法

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