CN111364071A - Lithium ion battery copper foil and preparation method thereof - Google Patents
Lithium ion battery copper foil and preparation method thereof Download PDFInfo
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- CN111364071A CN111364071A CN202010326375.2A CN202010326375A CN111364071A CN 111364071 A CN111364071 A CN 111364071A CN 202010326375 A CN202010326375 A CN 202010326375A CN 111364071 A CN111364071 A CN 111364071A
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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
- C25D1/00—Electroforming
- C25D1/04—Wires; Strips; Foils
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C63/00—Lining or sheathing, i.e. applying preformed layers or sheathings of plastics; Apparatus therefor
- B29C63/02—Lining or sheathing, i.e. applying preformed layers or sheathings of plastics; Apparatus therefor using sheet or web-like material
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C26/00—Coating not provided for in groups C23C2/00 - C23C24/00
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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
- C25D1/00—Electroforming
- C25D1/20—Separation of the formed objects from the electrodes with no destruction of said electrodes
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Abstract
The invention discloses a lithium ion battery copper foil and a preparation method thereof, wherein the lithium ion battery copper foil comprises a raw foil, a passivation layer and a silane layer, wherein the raw foil is a double-sided rough copper foil, the passivation layer is arranged on the surface of the raw foil, and the silane layer is arranged on the surface of the passivation layer; according to the invention, the passivation layer is arranged, so that the green foil is not oxidized and discolored due to direct contact with air, and meanwhile, the heat resistance of the green foil is also improved, and the arrangement of the silane layer can improve the oxidation resistance of the copper foil at normal temperature; on the other hand, when the copper foil is pressed into a plate at a high temperature, silane can enable the copper foil and the resin substrate to be better combined through coupling, the peeling strength is improved, the surface roughness of the copper foil can be greatly reduced through the organic composite auxiliary agent during preparation, and the copper foil has high tensile strength and high elongation.
Description
Technical Field
The invention relates to the technical field of lithium battery copper foils, in particular to a lithium ion battery copper foil and a preparation method thereof.
Background
The copper foil is one of key materials for producing the lithium ion battery, the copper foil is used as a carrier of a negative active substance and a collection and transmission body of negative electron current in the lithium battery, the quality of the copper foil directly influences the manufacturing process and the comprehensive performance of the lithium ion battery, and the good prospect of the lithium battery industry must also promote the development of the copper foil of the lithium battery towards the directions of high strength, few defects, low surface roughness, good ductility, thinner thickness and the like;
the copper foil prepared by simple chemical reaction during the production of the lithium battery copper foil has low tensile strength and elongation, and the process of antioxidant treatment on the surface of the lithium battery copper foil is single and cannot meet the production requirement, so the invention provides the lithium battery copper foil and the preparation method thereof to solve the problems in the prior art.
Disclosure of Invention
In order to solve the problems, the invention aims to provide a lithium ion battery copper foil and a preparation method thereof, the lithium ion battery copper foil and the preparation method thereof enable a raw foil not to be oxidized and discolored due to direct contact with air through the arrangement of a passivation layer, and simultaneously improve the heat resistance of the raw foil, and the arrangement of a silane layer can improve the oxidation resistance of the copper foil at normal temperature; on the other hand, when the copper foil is pressed into a plate at a high temperature, silane can enable the copper foil and the resin substrate to be better combined through coupling, the peeling strength is improved, the surface roughness of the copper foil can be greatly reduced through the organic composite auxiliary agent during preparation, and the copper foil has high tensile strength and high elongation.
In order to realize the purpose of the invention, the invention is realized by the following technical scheme: the lithium ion battery copper foil comprises a raw foil, a passivation layer and a silane layer, wherein the raw foil is a double-sided matte copper foil, the passivation layer is arranged on the surface of the raw foil, and the silane layer is arranged on the surface of the passivation layer.
The further improvement lies in that: the thickness of the raw foil is 6-18 mu m, the roughness value Rz of the double-sided surface is 1-2.5 mu m, the thickness of the passivation layer is 0.5-0.8 mu m, and the thickness of the silane layer is 0.3-0.6 mu m.
A preparation method of a lithium ion battery copper foil comprises the following steps:
the first step is as follows: putting a copper material raw material into a copper dissolving tank, adding pure water and sulfuric acid, introducing compressed air to carry out chemical combination reaction to generate a copper sulfate solution, repeatedly filtering the copper sulfate solution for many times, and then reintroducing the copper sulfate solution into the copper dissolving tank to carry out reaction, so as to reduce impurities in the copper sulfate solution;
the second step is that: pouring the prepared copper sulfate solution into an electrolytic bath, and adding an organic composite auxiliary agent for electrolysis;
the third step: continuously stripping the green foil from the cathode roller after the green foil deposited on the cathode roller of the electrolytic cell in the solution rotates out of the liquid level along with the roller, and generating the green foil through water washing, drying and coiling;
the fourth step: carrying out galvanizing treatment on the surface of the green foil, and carrying out surface passivation treatment by using chromate or chromate zincification salt solution to form a passivation layer;
the fifth step: and when the plate is pressed at a high temperature, the silane can enable the copper foil and the resin base material to be better combined through coupling, the peeling strength is improved, and the plate is dried at the temperature of 100-150 ℃.
And a sixth step: equally cutting and sampling finished products, respectively placing the samples in a 150 ℃ oven and a 180 ℃ oven, respectively drying for 30-60 min, visually checking whether the surfaces of the finished products are oxidized and discolored, covering a batch of the finished products which are not oxidized and discolored with an epoxy resin packaging film for storage, and isolating the finished products for rework if the oxidized and discolored products are generated.
The further improvement lies in that: the compressed air volume in the first step is 3.2m3/min，The reaction chemical formula is 2Cu +2H2SO4+ O2 ═ 2CuSO4+2H 2O.
The further improvement lies in that: the organic compound auxiliary agent in the second step is one of 5-20 g/L of polyethylene glycol, 500-1000 mg/L of sodium polydithio-dipropyl sulfonate, a mixture of 100-500 mg/L of thiourea and 30-70 mg/L of sodium methylthiocarbamyl propane sulfonate or polybrominated N-vinyl-N' -2-butylimidazole.
The further improvement lies in that: and in the fourth step, the surface of the green foil needs to stand for a period of time after being subjected to galvanizing treatment, the gray color of the surface of the green foil is converted into copper yellow, and the green foil is subjected to water washing, drying and water removal and then is subjected to silane layer spraying.
The invention has the beneficial effects that: according to the invention, the passivation layer is arranged, so that the green foil is not oxidized and discolored due to direct contact with air, and meanwhile, the heat resistance of the green foil is also improved, and the arrangement of the silane layer can improve the oxidation resistance of the copper foil at normal temperature; on the other hand, when the copper foil is pressed into a plate at a high temperature, silane can enable the copper foil and the resin substrate to be better combined through coupling, the peeling strength is improved, the surface roughness of the copper foil can be greatly reduced through the organic composite auxiliary agent during preparation, and the copper foil has high tensile strength and high elongation.
Drawings
FIG. 1 is a schematic view of a structural layer of the present invention.
FIG. 2 is a flow chart of the preparation method of the present invention.
Wherein: 1. raw foil; 2. a passivation layer; 3. a silane layer.
Detailed Description
In order to further understand the present invention, the following detailed description will be made with reference to the following examples, which are only used for explaining the present invention and are not to be construed as limiting the scope of the present invention.
Example 1
According to fig. 1 and 2, the embodiment provides a lithium ion battery copper foil and a preparation method thereof, and the lithium ion battery copper foil comprises a raw foil 1, a passivation layer 2 and a silane layer 3, wherein the raw foil 1 is a double-sided rough copper foil, the passivation layer 2 is arranged on the surface of the raw foil 1, and the silane layer 3 is arranged on the surface of the passivation layer 2.
The thickness of the green foil 1 is 6-18 mu m, the roughness value Rz of the double-sided surface is 1-2.5 mu m, the thickness of the passivation layer 2 is 0.5-0.8 mu m, and the thickness of the silane layer 3 is 0.3-0.6 mu m.
The preparation method of the copper foil of the lithium ion battery is characterized by comprising the following steps of:
the first step is as follows: putting a copper material raw material into a copper dissolving tank, adding pure water and sulfuric acid, introducing compressed air to carry out chemical combination reaction to generate a copper sulfate solution, repeatedly filtering the copper sulfate solution for many times, and then reintroducing the copper sulfate solution into the copper dissolving tank to carry out reaction, so as to reduce impurities in the copper sulfate solution;
the second step is that: pouring the prepared copper sulfate solution into an electrolytic bath, and adding an organic composite auxiliary agent for electrolysis;
the third step: continuously stripping the green foil 1 deposited on the cathode roller of the electrolytic cell in the solution after the green foil 1 rotates out of the liquid level along with the roller, and generating the green foil 1 through washing, drying and coiling;
the fourth step: carrying out galvanizing treatment on the surface of the green foil 1, and carrying out surface passivation treatment by using chromate or chromate zincification salt solution to form a passivation layer 2;
the fifth step: and a silane layer 3 is sprayed on the surface of the passivated raw foil 1 to improve the oxidation resistance of the copper foil at normal temperature, and when the copper foil is pressed into a plate at high temperature, silane can enable the copper foil and a resin substrate to be better combined through coupling, so that the peeling strength is improved, and the copper foil is dried at the temperature of 100-150 ℃.
And a sixth step: equally cutting and sampling finished products, respectively placing the samples in a 150 ℃ oven and a 180 ℃ oven, respectively drying for 30-60 min, visually checking whether the surfaces of the finished products are oxidized and discolored, covering a batch of the finished products which are not oxidized and discolored with an epoxy resin packaging film for storage, and isolating the finished products for rework if the oxidized and discolored products are generated.
The compressed air volume in the first step is 3.2m3And/min, the reaction chemical formula is 2Cu +2H2SO4+ O2 ═ 2CuSO4+2H 2O.
The organic composite auxiliary agents in the second step are 5-20 g/L of polyethylene glycol, 500-1000 mg/L of sodium polydithio-dipropyl sulfonate, 100-500 mg/L of thiourea and 30-70 mg/L of sodium methylthio-carbamoyl-propane sulfonate, and the raw foil with the surface roughness of less than 0.25 mu m, high tensile strength and strong elongation can be obtained.
And in the fourth step, the surface of the green foil 1 needs to stand for a period of time after being galvanized, the gray color of the surface of the green foil 1 is converted into copper yellow, and the green foil is sprayed with the silane layer 3 after being washed, dried and dehydrated.
Example 2
The embodiment provides a lithium ion battery copper foil and a preparation method thereof, and the lithium ion battery copper foil comprises a raw foil 1, a passivation layer 2 and a silane layer 3, wherein the raw foil 1 is a double-sided rough copper foil, the passivation layer 2 is arranged on the surface of the raw foil 1, and the silane layer 3 is arranged on the surface of the passivation layer 2.
The thickness of the green foil 1 is 6-18 mu m, the roughness value Rz of the double-sided surface is 1-2.5 mu m, the thickness of the passivation layer 2 is 0.5-0.8 mu m, and the thickness of the silane layer 3 is 0.3-0.6 mu m.
The preparation method of the copper foil of the lithium ion battery is characterized by comprising the following steps of:
the first step is as follows: putting a copper material raw material into a copper dissolving tank, adding pure water and sulfuric acid, introducing compressed air to carry out chemical combination reaction to generate a copper sulfate solution, repeatedly filtering the copper sulfate solution for many times, and then reintroducing the copper sulfate solution into the copper dissolving tank to carry out reaction, so as to reduce impurities in the copper sulfate solution;
the second step is that: pouring the prepared copper sulfate solution into an electrolytic bath, and adding an organic composite auxiliary agent for electrolysis;
the third step: continuously stripping the green foil 1 deposited on the cathode roller of the electrolytic cell in the solution after the green foil 1 rotates out of the liquid level along with the roller, and generating the green foil 1 through washing, drying and coiling;
the fourth step: carrying out galvanizing treatment on the surface of the green foil 1, and carrying out surface passivation treatment by using chromate or chromate and zinc salt solution to form a passivation layer 2;
the fifth step: and a silane layer 3 is sprayed on the surface of the passivated raw foil 1 to improve the oxidation resistance of the copper foil at normal temperature, and when the copper foil is pressed into a plate at high temperature, silane can enable the copper foil and a resin substrate to be better combined through coupling, so that the peeling strength is improved, and the copper foil is dried at the temperature of 100-150 ℃.
And a sixth step: equally cutting and sampling finished products, respectively placing the samples in a 150 ℃ oven and a 180 ℃ oven, respectively drying for 30-60 min, visually checking whether the surfaces of the finished products are oxidized and discolored, covering a batch of the finished products which are not oxidized and discolored with an epoxy resin packaging film for storage, and isolating the finished products for rework if the oxidized and discolored products are generated.
The compressed air volume in the first step is 3.2m3And/min, the reaction chemical formula is 2Cu +2H2SO4+ O2 ═ 2CuSO4+2H 2O.
The organic composite auxiliary agent in the second step is polybrominated N-vinyl-N' -2-butylimidazole, and raw foil with fine grains, brightness and smoothness can be obtained.
And in the fourth step, the surface of the green foil 1 needs to stand for a period of time after being galvanized, the gray color of the surface of the green foil 1 is converted into copper yellow, and the green foil is sprayed with the silane layer 3 after being washed, dried and dehydrated.
Example 3
The embodiment provides a lithium ion battery copper foil and a preparation method thereof, and the lithium ion battery copper foil comprises a raw foil 1, a passivation layer 2 and a silane layer 3, wherein the raw foil 1 is a double-sided rough copper foil, the passivation layer 2 is arranged on the surface of the raw foil 1, and the silane layer 3 is arranged on the surface of the passivation layer 2.
The thickness of the green foil 1 is 6-18 mu m, the roughness value Rz of the double-sided surface is 1-2.5 mu m, the thickness of the passivation layer 2 is 0.5-0.8 mu m, and the thickness of the silane layer 3 is 0.3-0.6 mu m.
The preparation method of the copper foil of the lithium ion battery is characterized by comprising the following steps of:
the first step is as follows: putting a copper material raw material into a copper dissolving tank, adding pure water and sulfuric acid, introducing compressed air to carry out chemical combination reaction to generate a copper sulfate solution, repeatedly filtering the copper sulfate solution for many times, and then reintroducing the copper sulfate solution into the copper dissolving tank to carry out reaction, so as to reduce impurities in the copper sulfate solution;
the second step is that: pouring the prepared copper sulfate solution into an electrolytic bath, and adding an organic composite auxiliary agent for electrolysis;
the third step: continuously stripping the green foil 1 deposited on the cathode roller of the electrolytic cell in the solution after the green foil 1 rotates out of the liquid level along with the roller, and generating the green foil 1 through washing, drying and coiling;
the fourth step: carrying out galvanizing treatment on the surface of the green foil 1, and carrying out surface passivation treatment by using chromate or chromate zincification salt solution to form a passivation layer 2;
the fifth step: and a silane layer 3 is sprayed on the surface of the passivated raw foil 1 to improve the oxidation resistance of the copper foil at normal temperature, and when the copper foil is pressed into a plate at high temperature, silane can enable the copper foil and a resin substrate to be better combined through coupling, so that the peeling strength is improved, and the copper foil is dried at the temperature of 100-150 ℃.
And a sixth step: equally cutting and sampling finished products, respectively placing the samples in a 150 ℃ oven and a 180 ℃ oven, respectively drying for 30-60 min, visually checking whether the surfaces of the finished products are oxidized and discolored, covering a batch of the finished products which are not oxidized and discolored with an epoxy resin packaging film for storage, and isolating the finished products for rework if the oxidized and discolored products are generated.
The compressed air volume in the first step is 3.2m3And/min, the reaction chemical formula is 2Cu +2H2SO4+ O2 ═ 2CuSO4+2H 2O.
The organic composite auxiliary agent in the second step is phthalocyanine dye, which can play a role in reducing current during electrolysis, and can simultaneously refine crystal grains of the green foil and improve the performance of the green foil.
And in the fourth step, the surface of the green foil 1 needs to stand for a period of time after being galvanized, the gray color of the surface of the green foil 1 is converted into copper yellow, and the green foil is sprayed with the silane layer 3 after being washed, dried and dehydrated.
According to the lithium ion battery copper foil and the preparation method, the passivation layer 2 is arranged, so that the green foil 1 is not oxidized and discolored due to direct contact with air, the heat resistance of the green foil 1 is improved, and the silane layer 3 can improve the oxidation resistance of the copper foil at normal temperature; on the other hand, when the high-temperature press plate is used, the silane layer 3 can enable the copper foil and the resin substrate to be better combined through coupling, the peeling strength is improved, the surface roughness of the copper foil can be greatly reduced through the organic composite auxiliary agent during preparation, and the copper foil has high tensile strength and high elongation.
The foregoing illustrates and describes the principles, general features, and advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (6)
1. A lithium ion battery copper foil is characterized in that: the production method comprises a raw foil (1), a passivation layer (2) and a silane layer (3), wherein the raw foil (1) is a double-sided rough copper foil, the passivation layer (2) is arranged on the surface of the raw foil (1), and the silane layer (3) is arranged on the surface of the passivation layer (2).
2. The lithium ion battery copper foil according to claim 1, wherein: the thickness of the raw foil (1) is 6-18 mu m, the roughness value Rz of the double-sided surface is 1-2.5 mu m, the thickness of the passivation layer (2) is 0.5-0.8 mu m, and the thickness of the silane layer (3) is 0.3-0.6 mu m.
3. The method for preparing the copper foil of the lithium ion battery according to claim 1, which is characterized by comprising the following steps of:
the first step is as follows: putting a copper material raw material into a copper dissolving tank, adding pure water and sulfuric acid, introducing compressed air to carry out chemical combination reaction to generate a copper sulfate solution, repeatedly filtering the copper sulfate solution for many times, and then reintroducing the copper sulfate solution into the copper dissolving tank to carry out reaction, so as to reduce impurities in the copper sulfate solution;
the second step is that: pouring the prepared copper sulfate solution into an electrolytic bath, and adding an organic composite auxiliary agent for electrolysis;
the third step: continuously stripping the raw foil (1) deposited on a cathode roller of an electrolytic cell in the solution from the liquid surface along with the roller, washing with water, drying, and coiling to generate the raw foil (1);
the fourth step: carrying out galvanizing treatment on the surface of the green foil (1), and carrying out surface passivation treatment by using chromate or chromate zinc-adding salt solution to form a passivation layer (2);
the fifth step: and spraying a silane layer (3) on the surface of the passivated raw foil (1) to improve the oxidation resistance of the copper foil at normal temperature, enabling the copper foil and the resin substrate to be better combined through coupling by silane when the copper foil is pressed into a plate at high temperature, improving the peel strength, and drying at the temperature of 100-150 ℃.
And a sixth step: equally cutting and sampling finished products, respectively placing the samples in a 150 ℃ oven and a 180 ℃ oven, respectively drying for 30-60 min, visually checking whether the surfaces of the finished products are oxidized and discolored, covering a batch of the finished products which are not oxidized and discolored with an epoxy resin packaging film for storage, and isolating the finished products for rework if the oxidized and discolored products are generated.
4. The method for preparing the copper foil of the lithium ion battery according to claim 3, wherein the method comprises the following steps: the compressed air volume in the first step is 3.2m3And/min, the reaction chemical formula is 2Cu +2H2SO4+ O2 ═ 2CuSO4+2H 2O.
5. The method for preparing the copper foil of the lithium ion battery according to claim 3, wherein the method comprises the following steps: the organic composite auxiliary agent in the second step is one of 5-20 g/L of polyethylene glycol, 500-1000 mg/L of sodium polydithio-dipropyl sulfonate, a mixture of 100-500 mg/L of thiourea and 30-70 mg/L of sodium methylthiocarbamyl propane sulfonate or polybrominated N-vinyl-N' -2-butylimidazole or phthalocyanine dye.
6. The method for preparing the copper foil of the lithium ion battery according to claim 3, wherein the method comprises the following steps: and in the fourth step, the surface of the green foil (1) needs to stand for a period of time after being galvanized, the gray color on the surface of the green foil (1) is converted into copper yellow, and the green foil is washed with water, dried and dehydrated and then sprayed with the silane layer (3).
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