CN110760898A - Preparation method of high-tensile electrolytic copper foil for lithium battery - Google Patents
Preparation method of high-tensile electrolytic copper foil for lithium battery Download PDFInfo
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- CN110760898A CN110760898A CN201911171583.3A CN201911171583A CN110760898A CN 110760898 A CN110760898 A CN 110760898A CN 201911171583 A CN201911171583 A CN 201911171583A CN 110760898 A CN110760898 A CN 110760898A
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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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Abstract
The invention discloses a preparation method of a high-tensile electrolytic copper foil for a lithium battery, which comprises the following steps: the method comprises the following steps: preparing an electrolyte; step two: adding an additive into the electrolyte; the additive comprises hydroxyethyl cellulose, leveling agent, brightening agent, thiourea compound and chloride ion; step three: filtering the electrolyte added with the additive and sending the electrolyte into an electrolytic cell for electrolytic foil generation. On the basis of the prior art, the tensile strength of the lithium electrolytic copper foil is improved by one step.
Description
Technical Field
The invention relates to a preparation method of an electrolytic copper foil, in particular to a preparation method of a high-tensile electrolytic copper foil for a lithium battery.
Background
With the improvement of the energy density requirement of the lithium battery, the high tensile strength becomes the main development direction of the lithium battery copper foil. The lithium electrolytic copper foil in the prior art is mainly produced by additives such as hydroxyethyl cellulose, brightening agent (sodium polydithio-dipropyl sulfonate or 3-mercapto-1-propane sulfonate), collagen and the like; the specification range is 6-10 μm, and the tensile strength is above 320MPa and below 450 MPa. However, with the increase of the energy density requirement of the lithium battery, the tensile strength of the lithium electrolytic copper foil prepared by the prior art cannot meet the requirement, so that improvement on the prior art process method is necessary to obtain the lithium electrolytic copper foil with higher tensile strength.
Disclosure of Invention
The invention relates to a preparation method of a high-tensile electrolytic copper foil for a lithium battery, and the tensile strength of the produced lithium battery copper foil is more than 500 MPa.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a preparation method of a high tensile electrolytic copper foil for a lithium battery is characterized by comprising the following steps:
the method comprises the following steps: preparing an electrolyte;
step two: adding an additive into the electrolyte; the additive comprises hydroxyethyl cellulose, leveling agent, brightening agent, thiourea compound and chloride ion;
step three: filtering the electrolyte added with the additive and sending the electrolyte into an electrolytic cell for electrolytic foil generation.
Further, the first step is specifically that the copper material is blown to oxidize in a copper dissolving tank, then reacts with 45-60 ℃ dilute sulfuric acid solution to form copper sulfate solution, and then is filtered by diatomite, activated carbon and an oil removal filter bag, and the temperature is adjusted to 45-55 ℃ by adopting a plate heat exchanger to prepare the electrolyte with higher purity.
Furthermore, the content of copper ions in the electrolyte is 75-100 g/L, the content of sulfuric acid is 80-130g/L, the bath temperature is 45-55 ℃, and the electrolytic current density is 4000-.
Further, the leveling agent adopts collagen or polyethyleneimine.
Furthermore, thiourea or 1, 2-ethylene thiourea is adopted as the thiourea compound.
Further, the brightening agent comprises one or more of sodium polydithio-dipropyl sulfonate, sodium 3-mercapto-1-propane sulfonate or sodium polydithio-ethane sulfonate.
Further, the additive comprises 2-10 ppm of hydroxyethyl cellulose, 3-10 ppm of a leveling agent, 1-4 ppm of sodium polydithio dipropyl sulfonate or sodium 3-mercapto-1-propane sulfonate or sodium polydithio-ethane sulfonate, 1-5 ppm of thiourea or 1, 2-ethylene thiourea and 10-40 ppm of chloride ions.
Further, hydrochloric acid is adopted as the chloride ions.
And further, filtering the electrolyte added with the additive by 0.45 mu m to obtain high-purity electrolyte, conveying the high-purity electrolyte into the electrolytic cell according to the flow of 30-50m for carrying out thin film generation under the conditions of 4000-6000A/square meter.
Further, the copper foil produced by electrolysis in the third step is subjected to the procedures of electrolyte pickling, pure water washing and drying to obtain the copper foil with high surface cleanliness; installing an anti-oxidation treatment tank with micro-electroplating on a foil forming machine, carrying out anti-oxidation treatment on a copper foil with high surface cleanliness, wherein the anti-oxidation adopts a chemical plating or chemical micro-electroplating process, and then adopting an air drying process after treatment to obtain a dry anti-oxidation copper foil; and cutting the copper foil subjected to the anti-oxidation and drying treatment by a cutting machine.
Compared with the prior art, the invention has the following advantages and effects: the electrolytic copper foil with the specification of 6-10 microns produced by the preparation method provided by the invention has the tensile strength of more than or equal to 500MPa, the elongation of more than or equal to 5%, and the rough surface roughness Rz of less than or equal to 2.0 microns, and the tensile strength of the lithium electrolytic copper foil is improved by one section on the basis of the prior art.
Detailed Description
The present invention is further illustrated by the following examples, which are illustrative of the present invention and are not to be construed as being limited thereto.
Example 1:
a preparation method of a high-tensile electrolytic copper foil for a lithium battery comprises the following steps:
the method comprises the following steps: preparing an electrolyte; after the copper material is blown and oxidized in a copper dissolving tank, the copper material reacts with 55 ℃ dilute sulfuric acid solution to form copper sulfate solution, and then the copper sulfate solution is filtered by diatomite, activated carbon, an oil removing filter bag and the like, and the temperature is adjusted to 50 ℃ by adopting a plate heat exchanger to prepare the electrolyte with higher purity. In a copper sulfate electrolyte, the concentration of Cu < 2+ > is 85g/L, and the concentration of H2SO4 is 100 g/L; the temperature of the electrolyte is controlled at 50 ℃, and the conveying flow rate of the electrolyte is 40 m/h.
Step two: adding an additive into the electrolyte; the additive comprises 6ppm of hydroxyethyl cellulose, 8ppm of polyethyleneimine, 2ppm of sodium 3-mercapto-1-propane sulfonate, 2ppm of thiourea and 20ppm of chloride ions.
Step three: filtering the electrolyte added with the additive and sending the electrolyte into an electrolytic cell for electrolytic foil generation. Filtering the electrolyte added with the additive by 0.45 mu m to obtain high-purity electrolyte, then conveying the high-purity electrolyte into an electrolytic cell according to the flow of 40 m/h, and electrolyzing to generate foil under the condition of 5000A/square meter. The copper foil generated by electrolysis is subjected to the processes of electrolyte pickling, pure water washing and drying to obtain the copper foil with high surface cleanliness; installing an anti-oxidation treatment tank with micro-electroplating on a foil forming machine, carrying out anti-oxidation treatment on a copper foil with high surface cleanliness, wherein the anti-oxidation adopts a chemical plating or chemical micro-electroplating process, and then adopting an air drying process after treatment to obtain a dry anti-oxidation copper foil; and cutting the copper foil subjected to the oxidation prevention and drying treatment by a cutting machine, packaging after the detection is qualified, and leaving the factory.
The electrolytic copper foil produced by the additive has the tensile strength of 560MPa, the elongation of 7 percent and the rough surface roughness Rz of 1.8 mu m.
Example 2:
a preparation method of a high-tensile electrolytic copper foil for a lithium battery comprises the following steps:
the method comprises the following steps: preparing an electrolyte; after the copper material is blown and oxidized in a copper dissolving tank, the copper material reacts with 55 ℃ dilute sulfuric acid solution to form copper sulfate solution, the copper sulfate solution is filtered by diatomite, active carbon, an oil removing filter bag and the like, the temperature is adjusted to 45 ℃ by adopting a plate heat exchanger, and the electrolyte with higher purity is prepared. In a copper sulfate electrolyte, the concentration of Cu < 2+ > is 85g/L, and the concentration of H2SO4 is 100 g/L; the temperature of the electrolyte is controlled at 45 ℃, and the conveying flow of the electrolyte is 30 m/h.
Step two: adding an additive into the electrolyte; the additive contains 5ppm of hydroxyethyl cellulose, 7ppm of collagen, 1.5ppm of sodium polydithio-diethyl alkane sulfonate, 2ppm of thiourea and 20ppm of chloride ions.
Step three: filtering the electrolyte added with the additive and sending the electrolyte into an electrolytic cell for electrolytic foil generation. Filtering the electrolyte added with the additive by 0.45 mu m to obtain high-purity electrolyte, then conveying the high-purity electrolyte into an electrolytic cell according to the flow of 30 m/h, and electrolyzing to generate foil under the condition of 4000A/square meter. The copper foil generated by electrolysis is subjected to the processes of electrolyte pickling, pure water washing and drying to obtain the copper foil with high surface cleanliness; installing an anti-oxidation treatment tank with micro-electroplating on a foil forming machine, carrying out anti-oxidation treatment on a copper foil with high surface cleanliness, wherein the anti-oxidation adopts a chemical plating or chemical micro-electroplating process, and then adopting an air drying process after treatment to obtain a dry anti-oxidation copper foil; and cutting the copper foil subjected to the oxidation prevention and drying treatment by a cutting machine, packaging after the detection is qualified, and leaving the factory.
The electrolytic copper foil produced by the additive has the tensile strength of 540MPa, the elongation of 7.5 percent and the rough surface roughness Rz of 1.7 mu m.
Example 3:
a preparation method of a high-tensile electrolytic copper foil for a lithium battery comprises the following steps:
the method comprises the following steps: preparing an electrolyte; after the copper material is blown and oxidized in a copper dissolving tank, the copper material reacts with 55 ℃ dilute sulfuric acid solution to form copper sulfate solution, and then the copper sulfate solution is filtered by diatomite, activated carbon, an oil removing filter bag and the like, and the temperature is adjusted to 60 ℃ by adopting a plate heat exchanger to prepare the electrolyte with higher purity. In a copper sulfate electrolyte, the concentration of Cu < 2+ > is 85g/L, and the concentration of H2SO4 is 100 g/L; the temperature of the electrolyte is controlled at 55 ℃, and the conveying flow of the electrolyte is 50 m/h.
Step two: adding an additive into the electrolyte; the additive comprises 6ppm of hydroxyethyl cellulose, 8ppm of polyethyleneimine, 2ppm of sodium polydithiodipropylsulfonate, 3ppm of 1, 2-ethylenethiourea and 20ppm of chloride ions.
Step three: filtering the electrolyte added with the additive and sending the electrolyte into an electrolytic cell for electrolytic foil generation. Filtering the electrolyte added with the additive by 0.45 mu m to obtain high-purity electrolyte, then conveying the high-purity electrolyte into an electrolytic cell according to the flow of 50 m/h, and electrolyzing to generate foil under the condition of 6000A/square meter. The copper foil generated by electrolysis is subjected to the processes of electrolyte pickling, pure water washing and drying to obtain the copper foil with high surface cleanliness; installing an anti-oxidation treatment tank with micro-electroplating on a foil forming machine, carrying out anti-oxidation treatment on a copper foil with high surface cleanliness, wherein the anti-oxidation adopts a chemical plating or chemical micro-electroplating process, and then adopting an air drying process after treatment to obtain a dry anti-oxidation copper foil; and cutting the copper foil subjected to the oxidation prevention and drying treatment by a cutting machine, packaging after the detection is qualified, and leaving the factory.
The electrolytic copper foil produced by the additive has the tensile strength of 550MPa, the elongation of 8 percent and the rough surface roughness Rz of 1.6 mu m.
Example 4:
a preparation method of a high-tensile electrolytic copper foil for a lithium battery comprises the following steps:
the method comprises the following steps: preparing an electrolyte; after the copper material is blown and oxidized in a copper dissolving tank, the copper material reacts with 55 ℃ dilute sulfuric acid solution to form copper sulfate solution, and then the copper sulfate solution is filtered by diatomite, activated carbon, an oil removing filter bag and the like, and the temperature is adjusted to 50 ℃ by adopting a plate heat exchanger to prepare the electrolyte with higher purity. In a copper sulfate electrolyte, the concentration of Cu < 2+ > is 85g/L, and the concentration of H2SO4 is 100 g/L; the temperature of the electrolyte is controlled at 50 ℃, and the conveying flow rate of the electrolyte is 40 m/h.
Step two: adding an additive into the electrolyte; the additive comprises 5ppm of hydroxyethyl cellulose, 8ppm of collagen, 1.5ppm of sodium 3-mercapto-1-propane sulfonate, 3ppm of 1, 2-ethylenethiourea and 20ppm of chloride ions.
Step three: filtering the electrolyte added with the additive and sending the electrolyte into an electrolytic cell for electrolytic foil generation. Filtering the electrolyte added with the additive by 0.45 mu m to obtain high-purity electrolyte, then conveying the high-purity electrolyte into an electrolytic cell according to the flow of 40 m/h, and electrolyzing to generate foil under the condition of 5000A/square meter. The copper foil generated by electrolysis is subjected to the processes of electrolyte pickling, pure water washing and drying to obtain the copper foil with high surface cleanliness; installing an anti-oxidation treatment tank with micro-electroplating on a foil forming machine, carrying out anti-oxidation treatment on a copper foil with high surface cleanliness, wherein the anti-oxidation adopts a chemical plating or chemical micro-electroplating process, and then adopting an air drying process after treatment to obtain a dry anti-oxidation copper foil; and cutting the copper foil subjected to the oxidation prevention and drying treatment by a cutting machine, packaging after the detection is qualified, and leaving the factory.
The electrolytic copper foil produced by the additive has the tensile strength of 540MPa, the elongation of 8 percent and the rough surface roughness Rz of 1.7 mu m.
From the above examples, it can be seen that the electrolytic copper foil with the specification of 6-10 μm produced by the preparation method provided by the invention has the tensile strength of more than or equal to 500MPa, the elongation of more than or equal to 5% and the matte surface roughness Rz of less than or equal to 2.0 μm, and on the basis of the prior art, the tensile strength of the lithium electrolytic copper foil is improved by one section, and the performances of the lithium electrolytic copper foil on the elongation and the matte surface roughness are also improved.
The additive of the invention is composed of one or more of hydroxyethyl cellulose, collagen or polyethyleneimine, sodium polydithio-dipropyl sulfonate or sodium 3-mercapto-1-propane sulfonate or sodium polydithio-ethane sulfonate, thiourea or 1, 2-ethylene thiourea, hydrochloric acid and the like.
Wherein, the content of hydroxyethyl cellulose is 2-10 ppm, the content of collagen or polyethyleneimine is 3-10 ppm, the content of polydithio dipropyl sodium sulfonate or 3-mercapto-1-propane sodium sulfonate or polydithio ethane sodium sulfonate is 1-4 ppm, the content of thiourea or 1, 2-ethylene thiourea is 1-5 ppm, and the content of chloride ions is 10-40 ppm.
Wherein the molecular weight of the hydroxyethyl cellulose is 200000-800000; collagen molecular weight not more than 3000; polyethyleneimine molecular weight of 1200-.
The hydroxyethyl cellulose has the functions of refining crystal grains and changing tensile strength and elongation; collagen and polyethyleneimine have a good leveling effect; one of the sodium polydithio-dipropyl sulfonate or the sodium 3-mercapto-1-propane sulfonate or the sodium polydithio-ethane sulfonate has the functions of brightening and leveling, refining crystal grains, improving current density and having a brighter effect when being matched with thiourea compounds; the thiourea or the 1, 2-ethylene thiourea is a sulfur-containing and nitrogen-containing compound and has the function of obtaining higher tensile strength. The hydrochloric acid has the function of providing chloride ions and has the function of a carrier, and the additive is helped to move to the surface of the cathode roller.
The above description of the present invention is intended to be illustrative. Various modifications, additions and substitutions for the specific embodiments described may be made by those skilled in the art without departing from the scope of the invention as defined in the accompanying claims.
Claims (10)
1. A preparation method of a high tensile electrolytic copper foil for a lithium battery is characterized by comprising the following steps:
the method comprises the following steps: preparing an electrolyte;
step two: adding an additive into the electrolyte; the additive comprises hydroxyethyl cellulose, leveling agent, brightening agent, thiourea compound and chloride ion;
step three: filtering the electrolyte added with the additive and sending the electrolyte into an electrolytic cell for electrolytic foil generation.
2. The method for preparing a high tensile electrolytic copper foil for a lithium battery according to claim 1, wherein: the first step is specifically that after the copper material is blown and oxidized in a copper dissolving tank, the copper material reacts with 45-60 ℃ dilute sulfuric acid solution to form copper sulfate solution, and then the copper sulfate solution is filtered by diatomite, active carbon and an oil removal filter bag, and the temperature is adjusted to 45-55 ℃ by adopting a plate heat exchanger to prepare the electrolyte with higher purity.
3. The method for preparing a high tensile electrolytic copper foil for a lithium battery according to claim 1, wherein: the content of copper ions in the electrolyte is 75-100 g/L, the content of sulfuric acid is 80-130g/L, the bath temperature is 45-55 ℃, and the electrolytic current density is 4000-6000A/square meter.
4. The method for preparing a high tensile electrolytic copper foil for a lithium battery according to claim 1, wherein: the leveling agent adopts collagen or polyethyleneimine.
5. The method for preparing a high tensile electrolytic copper foil for a lithium battery according to claim 1, wherein: the thiourea compound adopts thiourea or 1, 2-ethylene thiourea.
6. The method for preparing a high tensile electrolytic copper foil for a lithium battery according to claim 5, wherein: the brightener comprises one or more of sodium polydithio-dipropyl sulfonate, sodium 3-mercapto-1-propane sulfonate or sodium polydithio-ethane sulfonate.
7. The method for preparing a high tensile electrolytic copper foil for a lithium battery as claimed in claim 6, wherein: the additive comprises 2-10 ppm of hydroxyethyl cellulose, 3-10 ppm of a leveling agent, 1-4 ppm of polydithio dipropyl sodium sulfonate or 3-mercapto-1-propane sodium sulfonate or polydithio-ethane sodium sulfonate, 1-5 ppm of thiourea or 1, 2-ethylene thiourea and 10-40 ppm of chloride ions.
8. The method for preparing a high tensile electrolytic copper foil for a lithium battery according to claim 1, wherein: hydrochloric acid is adopted as the chloride ions.
9. The method for preparing a high tensile electrolytic copper foil for a lithium battery according to claim 1, wherein: and step three, specifically, filtering the electrolyte added with the additive by 0.45 mu m to obtain high-purity electrolyte, then conveying the high-purity electrolyte into the electrolytic cell according to the flow of 30-50m for each h, and electrolyzing the green foil under the conditions of 4000-6000A/square meter.
10. The method for preparing a high tensile electrolytic copper foil for a lithium battery according to claim 1, wherein: the copper foil generated by electrolysis in the third step is subjected to the working procedures of electrolyte pickling, pure water washing and drying to obtain the copper foil with high surface cleanliness; installing an anti-oxidation treatment tank with micro-electroplating on a foil forming machine, carrying out anti-oxidation treatment on a copper foil with high surface cleanliness, wherein the anti-oxidation adopts a chemical plating or chemical micro-electroplating process, and then adopting an air drying process after treatment to obtain a dry anti-oxidation copper foil; and cutting the copper foil subjected to the anti-oxidation and drying treatment by a cutting machine.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111270273A (en) * | 2020-02-24 | 2020-06-12 | 江西铜业集团有限公司 | Additive for high-tensile electrolytic copper foil and process for preparing high-tensile electrolytic copper foil |
| CN111455416A (en) * | 2020-05-29 | 2020-07-28 | 佛冈建滔实业有限公司 | Preparation process of high-mechanical-property electrolytic copper foil of high-precision circuit board |
| CN111850620A (en) * | 2020-08-28 | 2020-10-30 | 江东电子材料有限公司 | Preparation method and preparation system of 4.5-micrometer ultrathin copper foil for lithium battery |
| CN112080768A (en) * | 2020-09-09 | 2020-12-15 | 江西省江铜耶兹铜箔有限公司 | Production process of smooth high-speed electrolytic copper foil |
| CN112144084A (en) * | 2020-10-13 | 2020-12-29 | 灵宝宝鑫电子科技有限公司 | Additive and process for preparing high-tensile electrolytic copper foil by using same |
| CN112481661A (en) * | 2020-11-27 | 2021-03-12 | 九江德福科技股份有限公司 | Preparation method of fine-grain copper foil |
| CN112516673A (en) * | 2020-11-24 | 2021-03-19 | 灵宝华鑫铜箔有限责任公司 | Slurry coating process of diatomite filter for lithium electro-copper foil system |
| CN113322495A (en) * | 2021-04-12 | 2021-08-31 | 浙江花园新能源有限公司 | High-tensile double-light lithium battery copper foil and production process thereof |
| CN113638015A (en) * | 2021-07-26 | 2021-11-12 | 新疆亿日铜箔科技股份有限公司 | Method for manufacturing 4.5 mu m electrolytic copper foil for high-capacity lithium battery |
| EP3978654A1 (en) * | 2020-09-29 | 2022-04-06 | SK Nexilis Co., Ltd. | Electrolytic copper foil of high strength, electrode comprising the same, secondary battery comprising the same, and method of manufacturing the same |
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| CN111270273A (en) * | 2020-02-24 | 2020-06-12 | 江西铜业集团有限公司 | Additive for high-tensile electrolytic copper foil and process for preparing high-tensile electrolytic copper foil |
| CN111455416A (en) * | 2020-05-29 | 2020-07-28 | 佛冈建滔实业有限公司 | Preparation process of high-mechanical-property electrolytic copper foil of high-precision circuit board |
| CN111850620B (en) * | 2020-08-28 | 2022-04-05 | 江东电子材料有限公司 | Preparation method and preparation system of 4.5-micrometer ultrathin copper foil for lithium battery |
| CN111850620A (en) * | 2020-08-28 | 2020-10-30 | 江东电子材料有限公司 | Preparation method and preparation system of 4.5-micrometer ultrathin copper foil for lithium battery |
| CN112080768A (en) * | 2020-09-09 | 2020-12-15 | 江西省江铜耶兹铜箔有限公司 | Production process of smooth high-speed electrolytic copper foil |
| EP3978654A1 (en) * | 2020-09-29 | 2022-04-06 | SK Nexilis Co., Ltd. | Electrolytic copper foil of high strength, electrode comprising the same, secondary battery comprising the same, and method of manufacturing the same |
| CN112144084A (en) * | 2020-10-13 | 2020-12-29 | 灵宝宝鑫电子科技有限公司 | Additive and process for preparing high-tensile electrolytic copper foil by using same |
| CN112516673A (en) * | 2020-11-24 | 2021-03-19 | 灵宝华鑫铜箔有限责任公司 | Slurry coating process of diatomite filter for lithium electro-copper foil system |
| CN112516673B (en) * | 2020-11-24 | 2022-05-20 | 灵宝华鑫铜箔有限责任公司 | Sizing process of diatomite filter for lithium electro-copper foil system |
| CN112481661A (en) * | 2020-11-27 | 2021-03-12 | 九江德福科技股份有限公司 | Preparation method of fine-grain copper foil |
| CN113322495A (en) * | 2021-04-12 | 2021-08-31 | 浙江花园新能源有限公司 | High-tensile double-light lithium battery copper foil and production process thereof |
| CN113322495B (en) * | 2021-04-12 | 2022-04-26 | 浙江花园新能源股份有限公司 | High-tensile double-light lithium battery copper foil and production process thereof |
| CN113638015A (en) * | 2021-07-26 | 2021-11-12 | 新疆亿日铜箔科技股份有限公司 | Method for manufacturing 4.5 mu m electrolytic copper foil for high-capacity lithium battery |
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Application publication date: 20200207 |