CN115287715A - Production process of double-optical copper foil for medium-tensile-strength lithium battery - Google Patents
Production process of double-optical copper foil for medium-tensile-strength lithium battery Download PDFInfo
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- CN115287715A CN115287715A CN202211029436.4A CN202211029436A CN115287715A CN 115287715 A CN115287715 A CN 115287715A CN 202211029436 A CN202211029436 A CN 202211029436A CN 115287715 A CN115287715 A CN 115287715A
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- copper foil
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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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- 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
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/134—Electrodes based on metals, Si or alloys
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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
Abstract
The invention discloses a production process of a double-optical copper foil for a tensile strength-resistant lithium battery, which comprises the following steps of: and (3) utilizing the early-stage additive and the electrolyte to carry out electrolytic foil making, and adding the later-stage additive to continue electrolysis when the tensile strength of the copper foil reaches a fixed value to obtain the copper foil. According to the invention, through improvement of the production process and addition of the early-stage additive and the later-stage additive, the tensile strength of the copper foil is improved, the roughness of the smooth surface and the rough surface is reduced, and the problem of warping of the ultrathin copper foil is effectively avoided.
Description
Technical Field
The invention belongs to the technical field of lithium battery copper foil manufacturing, and particularly relates to a production process of a double-optical copper foil for a medium-tensile-strength lithium battery.
Background
With the rapid development of the new generation of electric vehicles, the requirements of the vehicles on power sources are higher and higher. The lithium ion secondary battery has become an ideal power source for a new generation of electric vehicles by virtue of excellent performance. The electrolytic copper foil is a base material of the lithium ion battery. With the rapid development of the field of power batteries, particularly lithium batteries, higher requirements are put on the energy density of lithium ion batteries, and correspondingly, electrolytic copper foil serving as a cathode material of the lithium ion batteries is developed towards ultra-thinning of 8 micrometers and below 6 micrometers, so that higher requirements are put on the performance and quality of the lithium ion battery copper foil.
CN110629257A discloses a method for manufacturing a high tensile strength lithium electrolytic copper foil, which comprises the steps of dissolving copper to prepare a main electrolyte, mixing the main electrolyte with an additive solution after multi-stage filtration to obtain an electrolyte, and electrolyzing at 30-70 ℃ and a current density of 30-85A/dm < 2 > to prepare a raw foil with a thickness of 6-9 mu m. The lithium electro-copper foil manufactured by the method has good tensile strength and elongation, and the color and the brightness of the copper foil are stable and easy to control.
CN114059107A discloses a production process of a high-elasticity-modulus lithium electrolytic copper foil, which comprises the following steps: s1, dissolving raw material copper in a sulfuric acid solution to form a dissolved solution, filtering and removing impurities, and mixing with a composite additive to obtain an electrolyte; wherein, the composite additive comprises collagen, polyethylene glycol, sodium thiolpropane sulfonate and hexyl benzylamine salt; s2, adding the electrolyte into a foil forming machine, and electroplating to obtain a copper foil primary product; and S3, carrying out surface treatment on the copper foil primary product by adopting a direct current deposition process, and rolling to obtain the ultrathin lithium electrolytic copper foil with the thickness of 4.5 micrometers and 6 micrometers. According to the invention, the composite additive is added into the electrolyte, so that the microscopic crystal grains of the lithium electro-copper foil are improved, the crystal grain size of the lithium electro-copper foil is reduced, the brightness of the lithium electro-copper foil is increased, and the tensile strength and the elongation of the lithium electro-copper foil are improved.
Warping is a difficult problem often encountered in the production process of ultrathin electrolytic copper foil, and is generally caused by the production process. The warping of the copper foil influences the cutting of the slitting machine row on one hand, and on the other hand, the electrolytic copper foil is easy to generate wrinkles, bubbles and the like to influence the adhesion between the electrolytic copper foil and the substrate, thereby influencing the quality of the copper-clad plate. Therefore, the development of the production process of the lithium battery copper foil with low warping degree has important significance.
Disclosure of Invention
In order to solve the technical problems, the invention provides a production process of a dual-optical copper foil for a lithium battery with medium tensile strength.
In order to achieve the purpose, the invention adopts the following technical scheme:
a production process of a double-optical copper foil for a tensile strength lithium battery comprises the following steps: and (3) utilizing the early-stage additive and the electrolyte to carry out electrolytic foil making, and adding the later-stage additive to continue electrolysis when the tensile strength of the copper foil reaches a fixed value to obtain the copper foil.
Preferably, the electrolyte contains 80-85g/L Cu 2+ 、100-110g/L H 2 SO 4 And 25-30mg/L Cl - 。
Preferably, the addition amount of the early-stage additive is 3.0-4.0L/h.
Further preferably, the early additive comprises 3-4g/L of sodium polydithio-dipropyl sulfonate, 11-12g/L of collagen, 0.6-0.7g/L of hydroxyethyl cellulose, 0.2-0.4g/L of polyethylene glycol and 0.1-0.3g/L of N, N-dimethyl-dithiocarbonyl propane.
Still more preferably, the pre-additive comprises 3.2-3.8g/L sodium polydithio-dipropyl sulfonate, 11.2-11.5g/L collagen, 0.61-0.68g/L hydroxyethyl cellulose, 0.25-0.35g/L polyethylene glycol and 0.15-0.25g/L N, N-dimethyl-dithio-carbonyl propane.
Most preferably, the pre-additive comprises sodium polydithio-dipropyl sulfonate 3.5g/L, collagen 11.3g/L, hydroxyethyl cellulose 0.64g/L, polyethylene glycol 0.3g/L and N, N-dimethyl-dithiocarbonyl propane 0.2g/L.
The conditions for electrolytic foil production are as follows: the temperature is 51-53 ℃, and the current density is 50-85A/dm 2 。
Preferably, the fixed value is 280-320MPa.
Preferably, the addition amount of the late-stage additive is 1.0-2.0L/h.
Further preferably, the late-stage additive contains 6-7ml/L of hexyl benzylamine salt and 3-5mg/L of sodium dimethylaminobenzoate.
Even more preferably, the post-additive further comprises vanillin 3-5mg/L.
Preferably, the copper foil has a thickness of 4.5 to 6 μm.
Preferably, the copper foil has a warp of not more than 8.
The beneficial effects of the invention are as follows:
the invention improves the production process, improves the tensile strength of the copper foil by adding the early-stage additive and the later-stage additive, reduces the roughness of the smooth surface and the rough surface, and effectively avoids the problem of warping of the ultrathin copper foil (4.5-6 mu m).
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
Before the present embodiments are further described, it is to be understood that the scope of the invention is not limited to the particular embodiments described below; it is also to be understood that the terminology used in the examples is for the purpose of describing particular embodiments only, and is not intended to limit the scope of the present invention.
When numerical ranges are given in the examples, it is understood that both endpoints of each of the numerical ranges and any value therebetween can be selected unless the invention otherwise indicated. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
The sources of the raw materials used in the present invention are not limited, and the raw materials used in the present invention are all those commonly available in the art unless otherwise specified. Unless otherwise specified, the solvents used in the solutions of the present application are all water, preferably tap water.
Example 1
The production process of the double-optical copper foil for the medium-tensile-strength lithium battery sequentially comprises the following steps of: dissolving copper, filtering to obtain electrolyte, adding early-stage additive into the electrolyte at a speed of 4.0L/h at 50A/dm 2 Electrolyzing at current density to obtain raw foil, adding post-additive into electrolyte at a speed of 1.0L/h when the tensile strength of copper foil reaches 280MPa, and adding the post-additive at a speed of 50A/dm 2 Continuously electrolyzing under the current density to obtain the copper foil;
wherein the concentration of the electrolyte is: cu 2+ 80g/L、H 2 SO 4 100g/L、T 51～53℃、Cl - 25mg/L；
Concentration of the early stage additive: 3g/L of sodium polydithio-dipropyl sulfonate, 12g/L of collagen, 0.6g/L of hydroxyethyl cellulose, 0.4g/L of polyethylene glycol and 0.1g/L of N, N-dimethyl-dithio carbonyl propane;
concentration of late-stage additive: 6ml/L hexyl benzyl amine salt and 5mg/L sodium dimethylaminocarbamate.
Example 2
The production process of the double-optical copper foil for the medium-tensile-strength lithium battery sequentially comprises the following steps of: dissolving copper, filtering to obtain electrolyte, adding early-stage additive at a speed of 3.0L/h into the electrolyte at 85A/dm 2 Electrolyzing at current density to obtain raw foil, adding post-additive into electrolyte at 2.0L/h speed when the copper foil tensile strength reaches 320MPa, and adding the post-additive at 85A/dm 2 Continuously electrolyzing under the current density to obtain the copper foil;
wherein the concentration of the electrolyte is: cu (copper) 2+ 85(g/L)、H 2 SO 4 110(g/L)、T 51～53(℃)、Cl - 30mg/L；
Concentration of the early stage additive: 4g/L of sodium polydithio-dipropyl sulfonate, 11g/L of collagen, 0.7g/L of hydroxyethyl cellulose, 0.2g/L of polyethylene glycol and 0.3g/L of N, N-dimethyl-dithio carbonyl propane;
concentration of late-stage additive: 7ml/L hexyl benzyl amine salt and 3mg/L sodium dimethylaminocarbamate.
Example 3
The production process of the double-optical copper foil for the medium-tensile-strength lithium battery sequentially comprises the following steps of: dissolving copper, filtering to obtain electrolyte, adding early-stage additive at a speed of 3.5L/h and adding into the electrolyte at a speed of 60A/dm 2 Electrolyzing at current density to obtain raw foil, adding post-additive into electrolyte at a speed of 1.5L/h when the tensile strength of copper foil reaches 300MPa, and adding the post-additive at 60A/dm 2 Continuously electrolyzing under the current density to obtain the copper foil;
wherein the concentration of the electrolyte is: cu 2+ 82g/L、H 2 SO 4 105g/L、T 51～53℃、Cl - 27mg/L；
Concentration of the early stage additive: 3.5g/L sodium polydithio-dipropyl sulfonate, 11.3g/L collagen, 0.64g/L hydroxyethyl cellulose, 0.3g/L polyethylene glycol and 0.2g/L N, N-dimethyl-dithio carbonyl propane;
concentration of late-stage additive: 6.5ml/L of hexyl benzylamine salt and 4mg/L of sodium dimethylaminocarbamate.
Example 4
The production process of the double-optical copper foil for the medium-tensile-strength lithium battery sequentially comprises the following steps of: dissolving copper, filtering to obtain electrolyte, adding early-stage additive at a speed of 3.5L/h and adding into the electrolyte at a speed of 60A/dm 2 Electrolyzing at current density to obtain raw foil, adding post-additive into electrolyte at a speed of 1.5L/h when the tensile strength of copper foil reaches 300MPa, and adding the post-additive at 60A/dm 2 Continuously electrolyzing under the current density to obtain the copper foil;
wherein the concentration of the electrolyte is: cu (copper) 2+ 82g/L、H 2 SO 4 105g/L、T 51～53℃、Cl - 27mg/L；
Concentration of the early stage additive: 3.5g/L of sodium polydithio-dipropyl sulfonate, 11.3g/L of collagen, 0.64g/L of hydroxyethyl cellulose, 0.3g/L of polyethylene glycol and 0.2g/L of N, N-dimethyl-dithio carbonyl propane;
concentration of late-stage additive: 6.5ml/L of hexyl benzylamine salt, 4mg/L of sodium dimethylaminocarbamate and 4mg/L of vanillin.
Comparative example 1
The production process of the double-optical copper foil for the medium-tensile-strength lithium battery sequentially comprises the following steps of: dissolving copper, filtering to obtain electrolyte, adding additive at a speed of 3.5L/h, and adding into the electrolyte at a concentration of 60A/dm 2 Electrolyzing under current density to obtain the copper foil;
wherein the concentration of the electrolyte is: cu 2+ 82g/L、H 2 SO 4 105g/L、T 51～53℃、Cl - 27mg/L；
Concentration of the additive: 3.5g/L of sodium polydithio-dipropyl sulfonate, 11.3g/L of collagen, 0.64g/L of hydroxyethyl cellulose, 0.3g/L, N of polyethylene glycol, 0.2g/L of N-dimethyl-dithio-carbonyl propane, 6.5ml/L of hexyl benzylamine salt and 4mg/L of sodium dimethyldithiocarbamate.
Comparative example 2
The production process of the double-optical copper foil for the medium-tensile-strength lithium battery sequentially comprises the following steps of: dissolving copper, filtering to obtain electrolyte, adding early-stage additive at a speed of 3.5L/h and adding into the electrolyte at a speed of 60A/dm 2 Electrolyzing at current density to obtain raw foil, adding post-additive into electrolyte at a speed of 1.5L/h when the tensile strength of copper foil reaches 250MPa, and adding the post-additive at a speed of 60A/dm 2 Continuously electrolyzing under the current density to obtain the copper foil;
wherein the concentration of the electrolyte is: cu 2+ 82g/L、H 2 SO 4 105g/L、T 51～53℃、Cl - 27mg/L；
Concentration of the early stage additive: 3.5g/L of sodium polydithio-dipropyl sulfonate, 11.3g/L of collagen, 0.64g/L of hydroxyethyl cellulose, 0.3g/L of polyethylene glycol and 0.2g/L of N, N-dimethyl-dithio carbonyl propane;
concentration of late-stage additive: 7.5ml/L of hexyl benzylamine salt and 2mg/L of sodium dimethylaminocarbamate.
The properties of the dual-optical copper foil for a medium tensile strength lithium battery prepared in examples 1 to 4 and comparative examples 1 to 2 are shown in table 1 below.
TABLE 1 Performance of dual-optical copper foil for tensile strength lithium batteries
As can be seen from the above examples 1-3, the tensile strength of the copper foil is improved, the roughness of the smooth surface and the rough surface is reduced, and the problem of warping of the ultra-thin copper foil (4.5-6 μm) is effectively avoided by improving the production process and adding the early-stage additive and the late-stage additive. Meanwhile, it can be seen from example 4 that when vanillin is added to the post-additive, roughness can be further reduced, and warpage can be reduced. According to comparative examples 1 and 2, the influence of the addition of the late-stage additive on the warping degree of the copper foil is large, and the fact that the good technical effect can be achieved only by the late-stage additive with the specific composition is proved.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and all simple modifications, changes and equivalent structural changes made to the above embodiment according to the technical spirit of the present invention still fall within the protection scope of the technical solution of the present invention.
Claims (10)
1. A production process of a double-optical copper foil for a tensile strength lithium battery is characterized by comprising the following steps: and (3) utilizing the early-stage additive and the electrolyte to carry out electrolytic foil making, and adding the later-stage additive to continue electrolysis when the tensile strength of the copper foil reaches a fixed value to obtain the copper foil.
2. The process according to claim 1, wherein the electrolyte contains 80-85g/L Cu 2+ 、100-110g/LH 2 SO 4 And 25-30mg/L Cl - 。
3. The production process according to claim 1, wherein the additive amount of the early-stage additive is 3.0 to 4.0L/h.
4. The process of claim 3, wherein the pre-additive comprises sodium polydithio-dipropyl sulfonate 3-4g/L, collagen 11-12g/L, hydroxyethyl cellulose 0.6-0.7g/L, polyethylene glycol 0.2-0.4g/L and N, N-dimethyl-dithiocarbonyl propane 0.1-0.3g/L.
5. The process of claim 4, wherein the pre-additive comprises sodium polydithio-dipropyl sulfonate 3.2-3.8g/L, collagen 11.2-11.5g/L, hydroxyethyl cellulose 0.61-0.68g/L, polyethylene glycol 0.25-0.35g/L, and N, N-dimethyl-dithiocarbonyl propane 0.15-0.25g/L.
6. The process according to claim 1, wherein the conditions for electrolytic foil production are: the temperature is 51-53 ℃, and the current density is 50-85A/dm 2 。
7. The process according to claim 1, wherein the fixed value is 280 to 320Mpa.
8. The production process according to claim 1, wherein the additive amount of the post-additive is 1.0-2.0L/h.
9. The process of claim 7, wherein the post-additive comprises hexylbenzylamine salt 6-7ml/L and sodium dimethylaminobenzoate 3-5mg/L.
10. The double-optical copper foil for a medium-tensile-strength lithium battery prepared by the production process according to any one of claims 1 to 9, wherein the copper foil has a thickness of 4.5 to 6 μm and a warp degree of not more than 8.
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| CN114059107A (en) * | 2021-12-28 | 2022-02-18 | 铜陵市华创新材料有限公司 | Production process of high-elasticity-modulus lithium-ion battery copper foil |
| CN114908386A (en) * | 2022-05-18 | 2022-08-16 | 江西理工大学 | Ultrathin multilayer structure type nanometer twin crystal copper foil and preparation method and application thereof |
-
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- 2022-08-25 CN CN202211029436.4A patent/CN115287715B/en active Active
Patent Citations (6)
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| CN102105622A (en) * | 2008-06-12 | 2011-06-22 | 古河电气工业株式会社 | Electrolytic copper coating and method of manufacture therefor, and copper electrolyte for manufacturing electrolytic copper coatings |
| CN110438531A (en) * | 2019-08-12 | 2019-11-12 | 湖北中一科技股份有限公司 | A kind of extra thin copper foil preparation method and system applied to lithium battery |
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