CN110629257A - Manufacturing method of high-tensile-strength lithium-ion battery copper foil - Google Patents
Manufacturing method of high-tensile-strength lithium-ion battery copper foil Download PDFInfo
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- CN110629257A CN110629257A CN201910606427.9A CN201910606427A CN110629257A CN 110629257 A CN110629257 A CN 110629257A CN 201910606427 A CN201910606427 A CN 201910606427A CN 110629257 A CN110629257 A CN 110629257A
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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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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/38—Electroplating: Baths therefor from solutions of copper
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Abstract
The invention discloses a manufacturing method of a high tensile 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 adding the electrolyte into a solution prepared by mixing the electrolyte and the additive solution at a temperature of 30-70 DEG CoC temperature and 30-85A/dm2The original foil was prepared by electrolysis at the current density of (1). The lithium battery copper foil manufactured by the invention has good tensile strength and elongation, and the color and the brightness of the copper foil are stable and easy to control. The thiourea compound is adopted as the C additive to obviously increase the tensile strength of the copper foil.
Description
Technical Field
The invention relates to the technical field of lithium electrolytic copper foil manufacturing, in particular to a manufacturing method of a high-tensile lithium electrolytic copper foil.
Background
The electrolytic copper foil is used as a functional base material of the lithium ion battery, and the potential, the conduction and the support function of the electrolytic copper foil are not replaced by other materials at present under the technical condition, so that the electrolytic copper foil is one of necessary materials of the lithium ion battery. With the rapid development of power batteries, particularly in the field of lithium batteries, higher requirements are put forward on the energy density of lithium ion batteries, and correspondingly, the electrolytic copper foil of the cathode material of the lithium ion battery is developed towards ultra-thinning with the thickness of 12 micrometers and below 8 micrometers, so that higher requirements are put forward on the performance and quality of the lithium ion battery copper foil: the copper foil has higher requirements on tensile strength, elongation and consistency; the thickness is thinner to meet the high energy density requirement of the lithium ion battery.
In addition, in the lithium ion battery, since the quality of the negative copper foil current collector is inferior to that of the positive electrode material in the whole battery, in order to obtain a lithium ion battery negative current collector with good performance, a double-smooth copper foil material with high brightness and good leveling performance is required, and under the condition that the thickness and the quality of the copper foil are constant, the leveling property and the brightness of the copper foil are improved, and the improvement of the surface roughness, the compactness, the thickness uniformity and the appearance are necessary for obtaining the lithium ion battery with high performance.
At present, the manufacturing process of the lithium electrolytic copper foil in China is unstable, and a plurality of difficulties exist in the technology to overcome, so that the research of a whole set of stable and efficient lithium electrolytic copper foil production process suitable for industrial production is very urgent, and the characteristics of the electrolytic copper foil are determined by corresponding additives according to the manufacturing principle of the copper foil. Therefore, in the production process of the lithium electrolytic copper foil, the additive containing a specific tissue structure and the electrolyte with a proportion are selected to effectively control the growth of copper crystal grains so as to obtain the electrolytic copper foil with required physical and chemical parameters.
An effective solution to the problems in the related art has not been proposed yet.
Disclosure of Invention
In view of the above technical problems in the related art, the present invention provides a method for manufacturing a high tensile lithium electrolytic copper foil, which can overcome the above disadvantages in the prior art.
In order to achieve the technical purpose, the technical scheme of the invention is realized as follows:
the high-tensile lithium electrolytic copper foil has a normal-temperature tensile strength of 500MPa-600MPa, a normal-temperature elongation of more than or equal to 5% (6 mu m lithium electrolytic copper foil elongation of more than or equal to 3%), a roughness Rz of less than or equal to 2.0 mu m and a glossiness of 50-400. The manufacturing method of the high-tensile-strength lithium electrolytic copper foil comprises the following steps:
(1) adding a simple substance of metal copper into a copper dissolving tank containing sulfuric acid, blowing high-temperature air by using a screw fan, dissolving copper to prepare a main electrolyte, and mixing the main electrolyte with an additive solution after multi-stage filtration to obtain an electrolyte; the electrolyte exchanges heat to 30-70 percent by a heat exchangeroC, throwing into an electrolytic bath; the electrolysis cathode is a seamless drum-type titanium roller, and the anode of the electrolysis bath is a dimensionally stable anode;
(2) at 30-70oC and 30-85A/dm2Performing electrolysis under the current density of the anode and cathode to prepare a raw foil;
(3) the prepared original foil is subjected to anti-oxidation treatment by adopting a conventional chromic anhydride aqueous solution to obtain an uncut finished product lithium electrolytic copper foil;
the additive comprises an agent A, an agent B, an agent C and chloride ions, wherein the agent A is an organic divalent sulfur compound, the agent B is a nitrogen-containing natural or synthetic high molecular compound, and the agent C is a thiourea compound.
Preferably, the concentration of copper ions in the electrolyte is 50-100 g/L, the content of sulfuric acid is 80-140 g/L, and the concentration of chloride ions is 30-100 mg/L. More preferably, the chloride ion concentration is 40-60 mg/L.
Preferably, the agent A is one or a mixture of more than two of sodium polydithio-dipropyl sulfonate, sodium thiol-propane sulfonate, 3-mercapto-1-propane sulfonate and mercaptobenzimidazole.
Preferably, the content of the agent A in the electrolyte is 3-70 mg/L.
Preferably, the agent B is one or a mixture of more than two of collagen, polyethyleneimine and polyether ammonia.
Preferably, the content of the agent B in the electrolyte is 5-80 mg/L.
Preferably, the agent C is one or a mixture of more than two of thiourea, ethylene thiourea, diethyl thiourea, tetramethyl thiourea and thiosemicarbazide.
Preferably, the content of the agent C in the electrolyte is 5-70 mg/L.
The invention has the beneficial effects that: in the invention, the organic sulfur compound, the water-soluble nitrogen-containing natural or synthetic polymer, the thiourea compound and the chloride ion are added into the electrolyte composed of the sulfuric acid-copper sulfate aqueous solution according to a specific proportion, and the electrolytic copper foil is manufactured by the manufacturing method, so that the growth process of crystal grains can be effectively controlled, the density of crystal grains is increased, and the crystal growth defects are reduced. The lithium-ion battery 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. The thiourea compound is adopted as the C additive to obviously increase the tensile strength of the copper foil.
Detailed Description
Example 1
Adding a metal copper simple substance into a copper dissolving tank containing sulfuric acid, blowing high-temperature air by using a screw fan, dissolving copper to prepare an acidic copper sulfate main electrolyte, performing multi-stage filtration on the main electrolyte, and mixing the main electrolyte with an additive solution to obtain an electrolyte, wherein in the obtained electrolyte, the copper ion concentration is 50 g/L, the acid content is 80 g/L, the chloride ion concentration is 30 mg/L, and the other additives comprise the following components:
sodium polydithio-dipropane sulfonate: 1 mg/L;
mercaptobenzimidazole: 2 mg/L;
collagen (number average molecular weight 3000-: 3 mg/L;
polyethyleneimine (average molecular weight 1200): 2 mg/L
Thiourea: 5 mg/L;
the electrolyte exchanges heat to 30 through a heat exchangeroAnd C, throwing the mixture into an electrolytic tank. The cathode of the electrolytic cell is a seamless drum-type titanium roller, and the anode is a size limiting anode. At 30A/dm2At a current density of 30oAnd C, electrolyzing to prepare a raw foil, wherein the raw foil is subjected to anti-oxidation treatment by adopting a conventional chromic anhydride aqueous solution to obtain an uncut finished electrolytic copper foil.
Example 2
Adding a metal copper simple substance into a copper dissolving tank containing sulfuric acid, blowing high-temperature air by using a screw fan, dissolving copper to prepare an acidic copper sulfate main electrolyte, performing multi-stage filtration on the main electrolyte, and mixing the main electrolyte with an additive solution to obtain an electrolyte, wherein in the obtained electrolyte, the copper ion concentration is 100 g/L, the acid content is 140 g/L, the chloride ion concentration is 100 mg/L, and the other additives comprise the following components:
sodium mercaptopropane sulfonate: 20 mg/L;
sodium 3-mercapto-1-propanesulfonate: 50 mg/L;
collagen (number average molecular weight 3000-: 30 mg/L;
polyether amine (average molecular weight 4000): 50 mg/L
Ethylene thiourea: 70 mg/L;
the electrolyte is subjected to heat exchange to 70 ℃ through a heat exchangeroAnd C, throwing the mixture into an electrolytic tank. Electrolytic bath cathodeThe roller is a seamless roller type titanium roller, and the anode is a size limiting anode. At 85A/dm2At a current density of 70oAnd C, electrolyzing to prepare a raw foil, wherein the raw foil is subjected to anti-oxidation treatment by adopting a conventional chromic anhydride aqueous solution to obtain an uncut finished electrolytic copper foil.
Example 3
Adding a metal copper simple substance into a copper dissolving tank containing sulfuric acid, blowing high-temperature air by using a screw fan, dissolving copper to prepare an acidic copper sulfate main electrolyte, performing multi-stage filtration on the main electrolyte, and mixing the main electrolyte with an additive solution to obtain an electrolyte, wherein in the obtained electrolyte, the copper ion concentration is 85 g/L, the acid content is 100 g/L, the chloride ion concentration is 30 mg/L, and the other additives comprise the following components:
sodium polydithio-dipropane sulfonate: 20 mg/L;
sodium 3-mercapto-1-propanesulfonate: 3 mg/L;
polyether ammonia (number average molecular weight 4000): 25 mg/L;
polyethyleneimine (average molecular weight 1200): 12 mg/L
Diethyl thiourea: 15 mg/L;
the electrolyte is subjected to heat exchange to 55 by a heat exchangeroAnd C, throwing the mixture into an electrolytic tank. The cathode of the electrolytic cell is a seamless drum-type titanium roller, and the anode is a size limiting anode. At 55A/dm2At a current density of 55oAnd C, electrolyzing to prepare a raw foil, wherein the raw foil is subjected to anti-oxidation treatment by adopting a conventional chromic anhydride aqueous solution to obtain an uncut finished electrolytic copper foil.
Example 4
Adding a metal copper simple substance into a copper dissolving tank containing sulfuric acid, blowing high-temperature air by using a screw fan, dissolving copper to prepare an acidic copper sulfate main electrolyte, performing multi-stage filtration on the main electrolyte, and mixing the main electrolyte with an additive solution to obtain an electrolyte, wherein in the obtained electrolyte, the copper ion concentration is 85 g/L, the acid content is 100 g/L, the chloride ion concentration is 30 mg/L, and the other additives comprise the following components:
sodium polydithio-dipropane sulfonate: 30 mg/L;
collagen (number average molecular weight 3000-: 27 mg/L;
polyethyleneimine (average molecular weight 1200): 15 mg/L
Tetramethyl thiourea: 22 mg/L;
the electrolyte exchanges heat to 45 degrees through a heat exchangeroAnd C, throwing the mixture into an electrolytic tank. The cathode of the electrolytic cell is a seamless drum-type titanium roller, and the anode is a size limiting anode. At 40A/dm2At a current density of 45oAnd C, electrolyzing to prepare a raw foil, wherein the raw foil is subjected to anti-oxidation treatment by adopting a conventional chromic anhydride aqueous solution to obtain an uncut finished electrolytic copper foil.
Example 5
Adding a metal copper simple substance into a copper dissolving tank containing sulfuric acid, blowing high-temperature air by using a screw fan, dissolving copper to prepare an acidic copper sulfate main electrolyte, performing multi-stage filtration on the main electrolyte, and mixing the main electrolyte with an additive solution to obtain an electrolyte, wherein in the obtained electrolyte, the copper ion concentration is 85 g/L, the acid content is 100 g/L, the chloride ion concentration is 30 mg/L, and the other additives comprise the following components:
sodium polydithio-dipropane sulfonate: 30 mg/L;
collagen (number average molecular weight 3000-: 27 mg/L;
polyethyleneimine (average molecular weight 1200): 15 mg/L
Thiosemicarbazide: 22 mg/L;
diethyl thiourea: 25 mg/L
The electrolyte exchanges heat to 65 through a heat exchangeroAnd C, throwing the mixture into an electrolytic tank. The cathode of the electrolytic cell is a seamless drum-type titanium roller, and the anode is a size limiting anode. At 65A/dm2At a current density of 65oAnd C, electrolyzing to prepare a raw foil, wherein the raw foil is subjected to anti-oxidation treatment by adopting a conventional chromic anhydride aqueous solution to obtain an uncut finished electrolytic copper foil.
Comparative example 1
An electrodeposited copper foil was produced in the same manner as in example 1, except that thiourea was replaced with polyethylene glycol (both having a molecular weight of 6000), and the other parameters were not changed.
Comparative example 2
An electrodeposited copper foil was produced in the same manner as in example 2, except that thiourea was changed to polyethylene glycol (both having a molecular weight of 6000), and the other parameters were not changed.
Comparative example 3
An electrodeposited copper foil was produced in the same manner as in example 3, except that thiourea was replaced with polyethylene glycol (both having a molecular weight of 6000), and the other parameters were not changed.
Example 6
Basic physical properties of the electrolytic copper foils prepared in examples 1 to 5 and comparative examples 1 to 3 were measured by the following methods:
and (3) testing the glossiness: the gloss in the M-plane direction of the copper foil was measured under a light incident angle of 60 ℃ according to test method GB/T13891 using WGG60-EJ gloss meter manufactured by Koshida photoelectric instruments Co.
And (3) testing tensile strength and elongation: according to test method GB/T29847-2013, HY-0230 universal material tester manufactured by Shanghai Heifyi precision instruments Co., Ltd is used at room temperature (about 25)oC) The copper foil was tested for tensile strength and elongation under the conditions.
Roughness test (Rz, ten point roughness average): according to the test method GB/T29847-2013, the roughness of the S surface and the M surface of the copper foil is tested by using a TR200 roughness meter manufactured by Beijing Time Ruidahi Tech & ltd & gt.
The results of basic physical property tests of the electrolytic copper foils prepared in examples 1 to 5 and comparative examples 1 to 3 are shown in Table 1:
table 1 performance test results of high tensile lithium electrolytic copper foil
As shown in Table 1, the present invention is in the range of 30 to 70oTemperature of C and 30-85A/dm2The lithium electrolytic copper foil prepared under the current density operating condition has good physical properties, and high tensile strength and elongation percentage. It is understood from comparative examples 1 to 3 and comparative examples 1 to 3 that the use of thiourea-based compounds as the C-based additives has a significant effect on the improvement of the tensile strength of the copper foil.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (5)
1. The manufacturing method of the high-tensile-strength lithium electrolytic copper foil is characterized by comprising the following steps of:
(1) adding a simple substance of metal copper into a copper dissolving tank containing sulfuric acid, blowing high-temperature air by using a screw fan, and dissolving copper to prepare a main electrolyte; the main electrolyte is subjected to multi-stage filtration and then is mixed with the additive solution to obtain an electrolyte; the electrolyte exchanges heat to 30-70 percent by a heat exchangeroC, throwing into an electrolytic bath; the electrolysis cathode is a seamless drum-type titanium roller, and the anode of the electrolysis bath is a dimensionally stable anode;
(2) at 30-70oC temperature and 30-85A/dm2Performing electrolysis under the current density of the anode and cathode to prepare a raw foil;
(3) the prepared original foil is subjected to anti-oxidation treatment by adopting a conventional chromic anhydride aqueous solution to obtain an uncut finished product lithium electrolytic copper foil;
the additive comprises an agent A, an agent B, an agent C and chloride ions, wherein the agent A is an organic divalent sulfur compound, the agent B is a nitrogen-containing natural or synthetic high molecular compound, and the agent C is a thiourea compound; the concentrations of copper ions, sulfuric acid, chloride ions, the agent A, the agent B and the agent C in the electrolyte are respectively 50-100 g/L, 80-140 g/L, 30-100 mg/L, 3-70 mg/L, 5-80 mg/L and 5-70 mg/L.
2. The manufacturing method of the high-tensile lithium electrolytic copper foil according to claim 1, wherein the thickness of the high-tensile lithium electrolytic copper foil is 6-9 μm.
3. The method for manufacturing a high-tensile lithium electrolytic copper foil according to claim 1, wherein the agent A is at least one selected from the group consisting of: sodium polydithio-dipropyl sulfonate, sodium thiol-propane sulfonate, sodium 3-mercapto-1-propane sulfonate and mercaptobenzimidazole.
4. The method for manufacturing a high-tensile lithium electrolytic copper foil according to claim 1, wherein the agent B is at least one selected from the group consisting of: collagen, polyethyleneimine and polyether ammonia.
5. The method for manufacturing a high-tensile lithium electrolytic copper foil according to claim 1, wherein the agent C is at least one selected from the group consisting of: thiourea, ethylene thiourea, diethyl thiourea, tetramethyl thiourea and thiosemicarbazide.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111020644A (en) * | 2020-01-03 | 2020-04-17 | 甘肃德福新材料有限公司 | Method for manufacturing electrolytic copper foil for lithium ion secondary battery |
| 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 |
| CN112195487A (en) * | 2020-09-18 | 2021-01-08 | 九江德福科技股份有限公司 | Manufacturing method for improving tensile strength of light and thin copper foil |
| CN112323102A (en) * | 2020-11-04 | 2021-02-05 | 湖南龙智新材料科技有限公司 | Electrolytic copper foil for FPC and preparation method thereof |
| CN112376088A (en) * | 2020-11-04 | 2021-02-19 | 湖南龙智新材料科技有限公司 | Ultra-thick electrolytic copper foil for PCB and preparation method thereof |
| 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 |
| CN113337856A (en) * | 2021-05-24 | 2021-09-03 | 中国恩菲工程技术有限公司 | Additive for double-sided photoelectric copper foil and preparation method of copper foil |
| CN113481551A (en) * | 2021-08-06 | 2021-10-08 | 河南科技大学 | Electrolyte additive of electrolytic copper foil, electrolyte, electrolytic copper foil and preparation method of electrolytic copper foil |
| CN113638014A (en) * | 2021-07-06 | 2021-11-12 | 铜陵市华创新材料有限公司 | Production method of ultrathin ultrahigh double-sided light-resistant lithium battery copper foil |
| CN114351190A (en) * | 2021-12-27 | 2022-04-15 | 安徽华威铜箔科技有限公司 | Preparation method of additive for flexible copper clad laminate electrolytic copper foil, product and application thereof |
| CN114457390A (en) * | 2022-02-24 | 2022-05-10 | 阳谷祥光铜业有限公司 | Preparation method of ultra-pure copper foil |
| CN114959804A (en) * | 2022-06-20 | 2022-08-30 | 九江德福科技股份有限公司 | Preparation method of bright fine-grain copper foil |
| LU500134B1 (en) * | 2021-05-07 | 2022-11-08 | Circuit Foil Luxembourg | Method for producing an electrodeposited copper foil and copper foil obtained therewith |
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| CN111020644B (en) * | 2020-01-03 | 2021-06-15 | 甘肃德福新材料有限公司 | Method for manufacturing electrolytic copper foil for lithium ion secondary battery |
| CN111020644A (en) * | 2020-01-03 | 2020-04-17 | 甘肃德福新材料有限公司 | Method for manufacturing electrolytic copper foil for lithium ion secondary battery |
| 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 |
| CN112195487A (en) * | 2020-09-18 | 2021-01-08 | 九江德福科技股份有限公司 | Manufacturing method for improving tensile strength of light and thin copper foil |
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| CN112376088A (en) * | 2020-11-04 | 2021-02-19 | 湖南龙智新材料科技有限公司 | Ultra-thick electrolytic copper foil for PCB and preparation method thereof |
| 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 |
| LU500134B1 (en) * | 2021-05-07 | 2022-11-08 | Circuit Foil Luxembourg | Method for producing an electrodeposited copper foil and copper foil obtained therewith |
| WO2022234113A1 (en) * | 2021-05-07 | 2022-11-10 | Circuit Foil Luxembourg | Method for producing an electrodeposited copper foil and copper foil obtained therewith |
| CN113337856A (en) * | 2021-05-24 | 2021-09-03 | 中国恩菲工程技术有限公司 | Additive for double-sided photoelectric copper foil and preparation method of copper foil |
| CN113337856B (en) * | 2021-05-24 | 2024-02-06 | 中国恩菲工程技术有限公司 | Additive for double-sided photoelectrolysis copper foil and preparation method of copper foil |
| CN113638014A (en) * | 2021-07-06 | 2021-11-12 | 铜陵市华创新材料有限公司 | Production method of ultrathin ultrahigh double-sided light-resistant lithium battery copper foil |
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| CN113481551A (en) * | 2021-08-06 | 2021-10-08 | 河南科技大学 | Electrolyte additive of electrolytic copper foil, electrolyte, electrolytic copper foil and preparation method of electrolytic copper foil |
| CN114351190A (en) * | 2021-12-27 | 2022-04-15 | 安徽华威铜箔科技有限公司 | Preparation method of additive for flexible copper clad laminate electrolytic copper foil, product and application thereof |
| CN114457390A (en) * | 2022-02-24 | 2022-05-10 | 阳谷祥光铜业有限公司 | Preparation method of ultra-pure copper foil |
| CN114457390B (en) * | 2022-02-24 | 2024-06-04 | 阳谷祥光铜业有限公司 | Preparation method of ultra-high purity copper foil |
| CN114959804A (en) * | 2022-06-20 | 2022-08-30 | 九江德福科技股份有限公司 | Preparation method of bright fine-grain copper foil |
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Application publication date: 20191231 |