CN114447340A - Anti-cracking copper foil and battery - Google Patents
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- CN114447340A CN114447340A CN202011228612.8A CN202011228612A CN114447340A CN 114447340 A CN114447340 A CN 114447340A CN 202011228612 A CN202011228612 A CN 202011228612A CN 114447340 A CN114447340 A CN 114447340A
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 137
- 239000011889 copper foil Substances 0.000 title claims abstract description 117
- 238000005336 cracking Methods 0.000 title abstract description 26
- 239000010949 copper Substances 0.000 claims abstract description 58
- 239000013078 crystal Substances 0.000 claims abstract description 49
- 229910052802 copper Inorganic materials 0.000 claims abstract description 20
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical group [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims description 12
- 229910001416 lithium ion Inorganic materials 0.000 claims description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 8
- 230000002035 prolonged effect Effects 0.000 abstract description 3
- 238000000137 annealing Methods 0.000 description 10
- 238000005452 bending Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
- 239000011149 active material Substances 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 238000012876 topography Methods 0.000 description 6
- 238000001035 drying Methods 0.000 description 5
- 239000012043 crude product Substances 0.000 description 4
- 238000001514 detection method Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 238000005498 polishing Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 239000007773 negative electrode material Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000012983 electrochemical energy storage Methods 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000011871 silicon-based negative electrode active material Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
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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
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
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- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Cell Electrode Carriers And Collectors (AREA)
Abstract
The application provides an anti-cracking copper foil and a battery, and belongs to the field of battery materials. In the crack-resistant copper foil, more than 99.8% of crystal domains are large-size crystal domains, the average diameter of the large-size crystal domains is 75-100 cm, and the index surface of the crystal domains is one of high crystal surface indexes except Cu (001), Cu (011) and Cu (111). The negative current collector of the battery is the anti-cracking copper foil. The crystal domain of the anti-cracking copper foil is mainly a large-size crystal domain required by a specific average diameter, and the crystal domain has a specific single crystal and a high-index surface, so that a copper material has good anti-cracking performance, the problem of damage of a negative current collector can be effectively solved, the service life of a battery can be effectively prolonged, the capacity of the battery can be effectively reduced, and the accident risk of the battery can be reduced.
Description
Technical Field
The application relates to the field of battery materials, in particular to a cracking-resistant copper foil and a battery.
Background
Driven by the development of electronic products, electric vehicles and renewable energy sources, electrochemical energy storage technology has not developed at a rate before. The lithium ion battery has the characteristics of light weight, high capacity, high energy density, long cycle life, high safety and the like, plays an important role in storing renewable electric energy, and is widely applied to electronic products such as mobile phones and computers, and the fields of electric automobiles, aerospace, large-scale energy storage and the like.
The negative electrode of the lithium ion battery comprises a negative electrode current collector and an active material, wherein the current negative electrode current collector is usually made of copper foil, and then the surface of the copper foil is coated with the active material such as carbon, graphite or silicon-based and the like to serve as the negative electrode of the battery. The copper foil as a negative electrode current collector can collect and output current generated from an active material in an electrochemical reaction, and the performance of the copper foil has a great influence on the internal resistance, capacity, cycle performance, safety, reliability, and the like of a battery.
At present, the copper foil mainly comprises two types of electrolytic copper foil and rolled copper foil, and the electrolytic copper foil is widely used as a negative current collector of the current commercial lithium ion battery due to the easy processing and lower cost of the thin copper foil. The elastic moduli of the electrolytic copper foil and rolled copper foil are reported to be about 70GPa and 50GPa, respectively. The electrolytic copper foil appears to be more brittle and more susceptible to bending and fracture; rolled copper foil is more resistant to bending, is more flexible, is less likely to crack and break when bent, and is more expensive. Therefore, in lithium battery products with low demand for flexibility, electrolytic copper foil is basically used instead of rolled copper foil.
In recent years, lithium ion batteries have been developed toward higher energy density and faster charging speed. However, the higher the energy, the greater the danger, which is shown in that the negative electrode current collector is easily damaged in use, so that more and more safety accidents are caused in recent years, and more pure electric vehicles are on fire and are recalled, and more frequent accidents such as swelling, firing and explosion of mobile phones occur.
Although the rolled copper foil with high cost and good toughness is adopted and the doping is carried out by adding Ag, Sn and the like into the copper, the problem caused by the damage of the negative current collector can be improved to a certain extent, but the problem of the damage of the negative current collector cannot be solved well, so that the problems of the reduction of the service life and the capacity of the battery and the reduction of the accident risk of the battery are still faced.
Disclosure of Invention
The application aims to provide an anti-cracking copper foil and a battery, which can effectively solve the problem of damage of a negative current collector, thereby effectively improving the problem of battery life and capacity reduction and reducing the risk of battery accidents.
Studies have shown that as lithium ion batteries move toward higher energy densities and faster charging speeds, the main cause of damage to their negative current collectors is: the mechanical stress caused by expansion and contraction of the active material of the negative electrode active material (particularly silicon-based negative electrode active material) in long-term charge and discharge can extrude the battery, so that the surface of the copper foil is easy to crack and break.
After cracks and fractures are generated on the surface of the copper foil, active materials and electrolyte can be filled into the cracks, so that effective connection between local active materials and a conductive network is lost, and the electrifying internal resistance is increased; meanwhile, the activity of the battery is also reduced or the battery cannot participate in charge-discharge reaction, so that the capacity of the lithium ion battery is reduced, and the cycle performance of the battery is greatly deteriorated.
With the increasing miniaturization and thinning of the current flexible electronic devices, high requirements are put forward in the aspects of flexibility or foldability, long service life and the like. Research shows that even if the rolled copper foil is bent with a certain curvature in a flexible lithium battery, the problem that the negative current collector cracks cannot be well avoided, and therefore the problem that the negative current collector is damaged cannot be effectively solved.
The embodiment of the application is realized as follows:
in a first aspect, the present invention provides a crack resistant copper foil, in which 99.8% or more of crystal domains are large-sized crystal domains, an average diameter of the large-sized crystal domains is 75 to 100cm, and an index plane of the crystal domains is one of high plane indices other than Cu (001), Cu (011), and Cu (111)).
In a second aspect, embodiments of the present application provide a battery, and a negative electrode current collector of the battery is a crack-resistant copper foil as provided in embodiments of the first aspect.
The anti-cracking copper foil provided by the embodiment of the application has the beneficial effects that:
the crystal domain of the anti-cracking copper foil is mainly a large-size crystal domain required by a specific average diameter, and the crystal domain has specific single crystal and high crystal face index, so that the copper material has good anti-cracking performance, the problem that a negative current collector is damaged can be effectively solved, the service life and the capacity of a battery can be effectively prolonged, and the accident risk of the battery can be reduced.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are required to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present application and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained from the drawings without inventive effort.
FIG. 1(a) is a schematic view showing cracks generated by bending a rolled copper foil;
FIG. 1(b) is a schematic view of cracks generated by bending a large-size domain single crystal copper foil;
FIG. 2 is a graph of the annealed surface topography of a crack resistant copper foil provided in accordance with an embodiment of the present application;
FIG. 3 is a surface topography map of a crack resistant copper foil after "annealing + electropolishing" as provided in an example of the present application;
FIG. 4 is a surface topography of a small domain multiple grain boundary rolled copper foil provided by a comparative example of the present application.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions of the embodiments of the present application will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are conventional products which are not indicated by manufacturers and are commercially available.
It should be noted that "and/or" in the present application, such as "feature 1 and/or feature 2" refers to "feature 1" alone, "feature 2" alone, and "feature 1" plus "feature 2" alone.
In addition, in the description of the present application, the meaning of "a plurality" of "one or more" means two or more unless otherwise specified; the range of "numerical value a to numerical value b" includes both values "a" and "b", and "unit of measure" in "numerical value a to numerical value b + unit of measure" represents both "unit of measure" of "numerical value a" and "numerical value b".
The following provides a detailed description of the crack resistant copper foil and the battery according to the examples of the present application.
In a first aspect, an embodiment of the present invention provides a crack-resistant copper foil, in which at least 99.8% of domains are large-sized domains, and an average diameter of the large-sized domains is 75 to 100 cm. The index plane of the domain is one of high plane indices other than Cu (001), Cu (011), and Cu (111), that is, the domain is a single crystal and a high index plane.
Research shows that when the copper foil material is applied as a negative electrode current collector, when a battery is extruded by mechanical stress caused by long-term charge and discharge of a negative electrode active material, the copper foil is easy to crack at a crystal boundary, so that the surface of the copper foil is easy to crack and fracture. In the current electrolytic copper foil and rolled copper foil, because of small crystal domain size, a large number of crystal boundaries (the number of the crystal boundaries is usually more than 10000/cm) are arranged in the copper foil material2) And the copper foil can not well prevent cracking, so that the problem that the negative current collector is damaged can not be solved well. Furthermore, when the copper foil is a single-crystal high-index surface copper foil, the copper foil has higher anti-cracking performance.
It has also been found that different lattice orientations in the copper foil have different crack resistance properties.
The crystal domain of the anti-cracking copper foil is mainly a large-size crystal domain required by a specific average diameter, and the crystal domain has a specific high crystal face index, so that the copper material has good performance of resisting cracks, the problem of damage of a negative current collector can be effectively solved, the service life and the capacity of a battery can be effectively prolonged, and the risk of battery accidents can be reduced.
As shown in FIGS. 1(a) and 1(b), the cracks generated under the same bending stress condition for different types of copper samples in FIGS. 1(a) and 1(b) are compared. FIG. 1(a) shows that a rolled copper foil has a large number of cracks after being bent; FIG. 1(b) shows that the large-size domain single crystal copper has very few cracks after bending.
As an example, the average diameter of the large-sized domains may be selected according to the performance requirements of a particular application scenario, such as, but not limited to, any one of 75cm, 80cm, 85cm, 90cm, 95cm, and 100cm, or a range between any two.
Considering that the distribution density of the copper crystal boundary has important influence on the cracking resistance of the copper foil, the proper number of the copper crystal boundaries in unit area can effectively regulate and control the cracking resistance of the copper foil. In some exemplary embodiments, in the case of satisfying the above-mentioned requirement of the average diameter of the large-sized domains, the number of copper grain boundaries is also required to be 8/cm or less2Further, the number of the copper grain boundaries is, for example, not more than 5/cm2。
It is understood that in the embodiments of the present application, the specific condition that the crystal domain is a single crystal and the high index face may be selected as needed, for example, but not limited to, the index face of the crystal domain is one of Cu (100), Cu (110), Cu (112), Cu (113), Cu (122), Cu (123), Cu (133), Cu (211), Cu (223), Cu (233), and Cu (355).
Considering that the copper foil has different crack prevention properties in different lattice orientations or crystal plane indexes, the index plane of the crystal domain is one of Cu (100), Cu (110), and Cu (211), as an example.
The thickness of the copper foil which is mainly used as a negative electrode current collector of the battery at present has several specifications such as 4.5 microns, 6 microns, 9 microns and the like, so that the thickness of the copper foil which is resistant to cracking can be specifically controlled to better meet the thickness requirement used in the battery.
As an example, the crack resistant copper foil has a thickness of 2-18 μm, such as, but not limited to, any one or a range between any two of 2 μm, 4.5 μm, 6 μm, 9 μm, 12 μm, 15 μm, and 18 μm.
Considering the tensile strength and the elongation of the copper foil as the main mechanical properties of the copper foil, the tensile strength and the elongation are favorably controlled under certain standards under the standards of specific domain size requirements, lattice orientation requirements and the like of the copper foil, and further, the copper foil is favorably prevented from being damaged in use.
In some possible embodiments, the crack resistant copper foil has a tensile strength of 155MPa or greater and an elongation of 2.9% or greater.
Considering that the copper purity and impurity content in the copper foil have certain influence on the mechanical property and electrical property of the copper foil, the mechanical property and electrical property requirements of the copper foil can be favorably ensured by improving the copper purity and reducing the impurities in the copper to a specific standard.
In some possible embodiments, the purity of the copper in the crack resistant copper foil is > 99.98%.
In some possible embodiments, the oxygen content in the crack resistant copper foil is < 10 ppm.
Considering that the anti-cracking copper foil is applied to a battery as a negative current collector, the conductivity performance is an important parameter for meeting the electrochemical performance requirement of the battery.
As an example, the electrical conductivity properties of the crack resistant copper foil are 103% IACS or greater. (internal connecting wrapper standard), such as but not limited to 103% IACS, 104% IACS, or 105% IACS. Wherein the conductivity of the standard annealed pure copper is 100% IACS.
The anti-cracking copper foil provided by the embodiment of the application has better anti-cracking performance, tensile strength, elongation, conductivity and other performances, and can be better applied to a current collector, for example, as a negative current collector of a battery.
As an example, the crack-resistant copper foil is annealed from an original small-crystal-domain copper foil, and then subjected to an electropolishing process and a drying process in this order under specific conditions. Specifically, the method comprises the following steps: the volume fraction of the polishing solution is 3: 1, respectively adopting a copper foil crude product and a copper plate as a positive electrode and a negative electrode, performing electropolishing treatment for 30-200 seconds under the condition that the current density is 4A/dm2, wherein the voltage is 2V; and then drying in a vacuum drying oven at the temperature of 50 ℃ for 10min to obtain the anti-cracking copper foil. The processing mode enables the anti-cracking copper foil to have better surface performance and can be better applied as a negative current collector.
In a second aspect, embodiments of the present application provide a battery, and a negative electrode current collector of the battery is a crack-resistant copper foil as provided in embodiments of the first aspect.
The lithium ion battery has the characteristics of light weight, high capacity, high energy density, long cycle life, high safety and the like.
As one example, the battery is a lithium ion battery.
Research shows that the anti-cracking copper foil provided by the embodiment of the first aspect of the application can better meet high performance requirements in the aspects of flexibility or folding, long service life and the like when being used as a negative electrode current collector of a flexible lithium ion battery.
Furthermore, the battery is a flexible lithium ion battery.
It is understood that in the embodiments of the present application, the battery may be of a kind well known in the art. The basic structure of the cell may also be one known in the art, which differs from the current cell structure in that the negative current collector is replaced by a copper foil resistant to cracking as provided in the embodiments of the first aspect of the present application.
The features and properties of the present application are described in further detail below with reference to examples.
In the present application, the crack resistant copper foils of the examples were prepared as follows.
The preparation process of the anti-cracking copper foil comprises the following steps:
s1, placing the original small crystal domain copper foil into annealing equipment, and introducing N2And an inert gas atmosphere such as Ar or He.
S2, when the annealing temperature of the copper foil is reached, introducing H2Or a reducing gas such as CO, to start the annealing process.
And S3, after the annealing is finished, continuously introducing inert gas and cooling to room temperature to obtain the copper foil with the large-size crystal domain.
And S4, carrying out XRD ray analysis and detection on the large-size domain copper foil, screening out a single crystal product with the highest specific peak intensity ratio, and ensuring that the number of copper crystal boundaries in unit area of the product is a specific number to obtain a copper foil crude product.
And S5, sequentially carrying out electropolishing treatment and drying treatment on the copper foil crude product by using polishing liquid. Wherein, the volume fraction of the polishing solution is 3: 1, the positive electrode and the negative electrode are respectively a copper foil crude product and a copper plate, the voltage is 2V, and the electropolishing treatment is carried out for 30-200 seconds under the condition that the current density is 4A/dm 2. And then drying in a vacuum drying oven at the temperature of 50 ℃ for 10min to obtain the anti-cracking copper foil.
In the present application, the performance parameters of the copper foils in the examples and comparative examples were measured as follows.
(1) Detecting the number of crystal boundaries: and observing by a metallographic microscope, and randomly taking the number of the grain boundaries within the range of 250 x 400 mm.
(2) Detection of average diameter of large domains: and (5) observing by a metallographic microscope, randomly taking the maximum distance between the grain boundary and the grain boundary of 10 crystal domains within the range of 250 x 400mm, and counting the average value.
(3) And (3) detecting the tensile strength: the test was carried out using a tensile tester.
(4) And (3) detecting the elongation: the test was carried out using a tensile tester.
(5) Conductivity detection: GB-T351.
(6) And (3) detecting the purity and the oxygen content of copper: GB/T5121.
In the present application, the performance parameters of the copper foils in the respective examples and comparative examples are shown in table 1. Wherein the copper foils in "comparative examples 1 and 2" were rolled copper foils of original small-domain polycrystallization before annealing; examples 1 and 2, crack resistant copper foils for annealed large size domain single crystals; fig. 2 is a surface topography diagram of a crack-resistant copper foil obtained by finishing the manufacturing process after only performing the annealing of step S4 according to the embodiment of the present application; fig. 3 is a surface topography diagram of a crack-resistant copper foil obtained by performing the electropolishing and drying process of step S5 after annealing the crack-resistant copper foil provided in the example of the present application in step S4; FIG. 4 is a surface topography of a small domain multiple grain boundary rolled copper foil provided by a comparative example of the present application.
As can be seen from fig. 2 and 3, the copper foil after annealing is subjected to electropolishing treatment, so that the copper foil has a smoother surface and better surface properties.
TABLE 1 copper foil Performance parameters
As can be seen from table 1, the crack-resistant copper foils provided in examples 1 and 2 of the present application have significantly improved elongation compared to the original small-grained rolled copper foils before annealing in comparative examples 1 and 2, and can maximally prevent the generation of cracks under the bending stress test, and can be better applied to batteries and used as a negative current collector copper foil material. The crack resistant copper foils provided in examples 1 and 2 of the present application have better crack resistance under the condition of the average diameter of the specific large domains and the number of grain boundaries than the crack resistant copper foil provided in comparative example 3.
The embodiments described above are some, but not all embodiments of the present application. The detailed description of the embodiments of the present application is not intended to limit the scope of the claimed application, but is merely representative of selected embodiments of the application. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
Claims (9)
1. A crack-resistant copper foil, characterized in that, in the crack-resistant copper foil, 99.8% or more of crystal domains are large-size crystal domains, the average diameter of the large-size crystal domains is 75-100 cm, and the index surface of the crystal domains is one of high crystal surface indexes except Cu (001), Cu (011) and Cu (111).
2. The crack resistant copper foil of claim 1, wherein the number of copper grain boundaries in the crack resistant copper foil is 8/cm or less2。
3. The crack resistant copper foil of claim 1, wherein the index plane of the domains is one of Cu (100), Cu (110), Cu (112), Cu (113), Cu (122), Cu (123), Cu (133), Cu (211), Cu (223), Cu (233), and Cu (355).
4. The crack-resistant copper foil according to any one of claims 1 to 3, wherein the crack-resistant copper foil has a thickness of 2 to 18 μm.
5. The crack resistant copper foil of any one of claims 1-3, wherein the crack resistant copper foil has a Cu purity of > 99.98% and an oxygen content of < 10 ppm.
6. The crack-resistant copper foil according to any one of claims 1 to 3, wherein the crack-resistant copper foil has an electrical conductivity of not less than 103% IACS.
7. A battery, characterized in that the negative electrode current collector of the battery is the crack-resistant copper foil according to any one of claims 1 to 6.
8. The battery of claim 7, wherein the battery is a lithium ion battery.
9. The battery of claim 8, wherein the battery is a flexible lithium ion battery.
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