CN115992375A - Production process for improving bubble yarn of lithium electric copper foil - Google Patents
Production process for improving bubble yarn of lithium electric copper foil Download PDFInfo
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- CN115992375A CN115992375A CN202310186025.4A CN202310186025A CN115992375A CN 115992375 A CN115992375 A CN 115992375A CN 202310186025 A CN202310186025 A CN 202310186025A CN 115992375 A CN115992375 A CN 115992375A
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Abstract
The invention discloses a production process for improving bubble yarns of lithium electric copper foil, which relates to the technical field of lithium electric copper foil and comprises the following steps: s1, preparing electrolyte: mixing sulfuric acid and lead carbonate solution to prepare electrolyte, heating and preserving the electrolyte; s2, preparing an additive: preparing a grain refiner, a wetting agent and a high leveling agent, and mixing and stirring the grain refiner, the wetting agent and the high leveling agent according to the installation proportion to form a mixed additive; s3, cutting the Harlin groove into pieces: adding the electrolyte and the mixed additive into a Halin tank, and tabletting the electrolyte in the Halin tank; s4, electroplating a lithium electric copper foil; s5, detecting a finished product; by adding the grain refiner, the wetting agent and the high-order leveling agent into the electrolyte, the copper foil is uniform and consistent in the continuous production process of the copper foil, no color difference stripes are formed, and from the microstructure, after the additive process is adjusted, the overall grain size of the copper foil is reduced, the foil surface is smoother, and the uniformity of the foil surface is increased.
Description
Technical Field
The invention relates to the technical field of lithium electric copper foil, in particular to a production process for improving bubble yarns of the lithium electric copper foil.
Background
The copper foil is one of key materials for producing lithium ion batteries, the quality of the copper foil directly influences the manufacturing process and the comprehensive performance of the lithium ion batteries, and as shown in fig. 2 and 4, electroplating unevenness easily occurs to the copper foil in the production process, electroplating color difference stripes appear on the surface of the copper foil, and fine seersucker easily appears on the surface of the copper foil;
the copper foil is used as a negative current collector, which can cause coating wrinkling in the process of coating to influence the production of the pole piece, or inconsistent thickness at the position of the seersucker in the coating process to influence the product quality of the pole piece.
Disclosure of Invention
In order to overcome the technical problems, the invention aims to provide an improved production process of the bubble yarn of the lithium electric copper foil, by adding a grain refiner, a wetting agent and a high leveling agent into electrolyte, the grain refiner is adsorbed on the surface of a cathode to form a compact adsorption layer or is selectively adsorbed in a cathode high-current density area, reduction is carried out at the position to block the discharging process of metal ions or the surface diffusion of metal adsorption atoms, so that the reaction speed of the cathode is slowed down, the grains are tiny, the wetting agent reduces the surface tension of the cathode, the electrolyte is more uniformly deposited on the cathode, the high leveling agent is non-uniform in the surface roughness of the cathode, the grains are continuously accumulated and grown in the deposition process, the high leveling agent can inhibit the grains from being further increased, so that the copper foil is uniformly and uniformly deposited in the continuous production process, no color difference stripes are formed, and from the aspect of microstructure, the overall grain size of the copper foil is reduced, the foil surface is more flat, and the foil surface uniformity is increased.
The aim of the invention can be achieved by the following technical scheme:
the production process for improving the seersucker of the lithium electric copper foil comprises the following steps of:
s1, preparing electrolyte: mixing sulfuric acid and lead carbonate solution to prepare electrolyte, heating and preserving the electrolyte;
s2, preparing an additive: preparing a grain refiner, a wetting agent and a high leveling agent, and mixing and stirring the grain refiner, the wetting agent and the high leveling agent according to the installation proportion to form a mixed additive;
s3, cutting the Harlin groove into pieces: adding the electrolyte and the mixed additive into a Halin tank, and tabletting the electrolyte in the Halin tank;
s4, electroplating a lithium electric copper foil: placing the lithium electric copper foil into electrolyte in a Halin tank for electroplating, and sequentially washing the electroplated lithium electric copper foil with water, passivating with chromic anhydride and drying;
s5, detecting a finished product: and stripping the dried lithium electric copper foil from the cathode plate, and detecting glossiness and tensile strength.
As a further scheme of the invention: the concentration of sulfuric acid in the S1 is 100g/L-110g/L, the concentration of copper ions is 90g/L-95g/L, the concentration of chloride ions is 20mg/L-30mg/L, and the temperature of the electrolyte is 45-55 ℃.
As a further scheme of the invention: the grain refiner is prepared by mixing 3-mercapto-1-propane sodium sulfonate, mercapto imidazole propane sodium sulfonate or any proportion of the 3-mercapto-1-propane sodium sulfonate and the mercapto imidazole propane sodium sulfonate, and is adsorbed on the surface of a cathode to form a compact adsorption layer, or selectively adsorbed in a cathode high-current density area, reduced at the position, and blocked metal ions to obtain a discharge process or metal adsorption atoms to obtain surface diffusion, so that the reaction speed of the cathode is slowed down, and the grains are fine.
As a further scheme of the invention: the wetting agent is alkyl alcohol polyoxyethylene polyoxypropylene ether or alkyl phenol polyoxyethylene polyoxypropylene ether, and reduces the surface tension of a cathode, so that the electrolyte is deposited more uniformly on the cathode.
As a further scheme of the invention: the high leveling agent is an amine compound containing nitrogen, the high leveling agent is deposited on the cathode, the surface roughness of the cathode is inconsistent, crystal grains are continuously piled up and grown in the deposition process, and the high leveling agent can inhibit the crystal grains from further rising, so that the deposition is smooth.
As a further scheme of the invention: the electrolyte concentration of the grain refiner is 4ppm-5ppm.
As a further scheme of the invention: the electrolyte concentration of the wetting agent is 1ppm-1.5ppm.
As a further scheme of the invention: the electrolyte concentration of the high leveling agent is 10ppm-15ppm.
The invention has the beneficial effects that: the grain refiner, the wetting agent and the high leveling agent are added into the electrolyte, the grain refiner is adsorbed on the surface of a cathode to form a compact adsorption layer, or is selectively adsorbed in a cathode high-current density area, reduction is carried out at the position, a discharging process of metal ions is blocked, or surface diffusion of metal adsorption atoms is blocked, so that the reaction speed of the cathode is slowed down, crystal grains are tiny, the surface tension of the cathode is reduced by the wetting agent, the electrolyte is more uniformly deposited on the cathode, the high leveling agent is deposited on the cathode, the roughness of the surface of the cathode is inconsistent, the crystal grains are continuously stacked and grown in the deposition process, the high leveling chance inhibits the crystal grains from further rising, so that the deposition is leveled, the copper foil is uniform and consistent in the continuous production process of the copper foil, no color difference stripes are formed, and from the microstructure point of view, the whole crystal grain size of the copper foil is reduced, the foil surface is flatter, and the uniformity of the foil surface is increased.
Drawings
The invention is further described below with reference to the accompanying drawings.
FIG. 1 is a flow chart of the present invention;
FIG. 2 is a view showing 700 times the optics of a lithium electrodeposited copper foil produced by the prior art;
FIG. 3 is a view showing 700 times of the optics of the lithium electrodeposited copper foil produced by the present invention;
FIG. 4 is a 1050-fold optical view of a lithium electrodeposited copper foil produced in the prior art;
FIG. 5 is a 1050-fold optical view showing a lithium secondary copper foil produced according to the present invention
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Embodiment one:
as shown in fig. 1, raw materials of sulfuric acid, lead carbonate solution, grain refiner, wetting agent and high leveling agent are taken, and then the lithium electric copper foil is processed according to the following steps:
s1, preparing electrolyte: mixing sulfuric acid and lead carbonate solution to prepare electrolyte, heating and preserving the electrolyte, wherein the concentration of sulfuric acid is 100g/L-110g/L, the concentration of copper ions is 90g/L-95g/L, the concentration of chloride ions is 20mg/L-30mg/L, and the temperature of the electrolyte is 45-55 ℃;
s2, preparing an additive: preparing a grain refiner, a wetting agent and a high leveling agent, mixing and stirring the grain refiner, the wetting agent and the high leveling agent according to the installation proportion to form a mixed additive, wherein the grain refiner is 3-mercapto-1-propane sodium sulfonate, the wetting agent is alkyl alcohol polyoxyethylene polyoxypropylene ether, the high leveling agent is an amine compound containing nitrogen, the concentration of electrolyte of the grain refiner is 4ppm, the concentration of electrolyte of the wetting agent is 1ppm, and the concentration of electrolyte of the high leveling agent is 10ppm;
s3, cutting the Harlin groove into pieces: adding the electrolyte and the mixed additive into a Halin tank, and tabletting the electrolyte in the Halin tank;
s4, electroplating a lithium electric copper foil: three lithium electric copper foils are put into electrolyte in a Halin groove for electroplating, and the electroplated lithium electric copper foils are sequentially washed with water, passivated by chromic anhydride and dried;
s5, detecting a finished product: and stripping the dried lithium electric copper foil from the cathode plate, sequentially marking three lithium electric copper foils as No. 1, no. 2 and No. 3, and detecting glossiness and tensile strength.
Embodiment two:
as shown in fig. 1, raw materials of sulfuric acid, lead carbonate solution, grain refiner, wetting agent and high leveling agent are taken, and then the lithium electric copper foil is processed according to the following steps:
s1, preparing electrolyte: mixing sulfuric acid and lead carbonate solution to prepare electrolyte, heating and preserving the electrolyte, wherein the concentration of sulfuric acid is 100g/L-110g/L, the concentration of copper ions is 90g/L-95g/L, the concentration of chloride ions is 20mg/L-30mg/L, and the temperature of the electrolyte is 45-55 ℃;
s2, preparing an additive: preparing a grain refiner, a wetting agent and a high leveling agent, mixing and stirring the grain refiner, the wetting agent and the high leveling agent according to the installation proportion to form a mixed additive, wherein the grain refiner is 3-mercapto-1-propane sodium sulfonate, the wetting agent is alkyl alcohol polyoxyethylene polyoxypropylene ether, the high leveling agent is an amine compound containing nitrogen, the concentration of electrolyte of the grain refiner is 4ppm, the concentration of electrolyte of the wetting agent is 1.5ppm, and the concentration of electrolyte of the high leveling agent is 10ppm;
s3, cutting the Harlin groove into pieces: adding the electrolyte and the mixed additive into a Halin tank, and tabletting the electrolyte in the Halin tank;
s4, electroplating a lithium electric copper foil: three lithium electric copper foils are put into electrolyte in a Halin groove for electroplating, and the electroplated lithium electric copper foils are sequentially washed with water, passivated by chromic anhydride and dried;
s5, detecting a finished product: and stripping the dried lithium electric copper foil from the cathode plate, marking three lithium electric copper foils as No. 4, no. 5 and No. 6 in sequence, and detecting glossiness and tensile strength.
Embodiment III:
as shown in fig. 1, raw materials of sulfuric acid, lead carbonate solution, grain refiner, wetting agent and high leveling agent are taken, and then the lithium electric copper foil is processed according to the following steps:
s1, preparing electrolyte: mixing sulfuric acid and lead carbonate solution to prepare electrolyte, heating and preserving the electrolyte, wherein the concentration of sulfuric acid is 100g/L-110g/L, the concentration of copper ions is 90g/L-95g/L, the concentration of chloride ions is 20mg/L-30mg/L, and the temperature of the electrolyte is 45-55 ℃;
s2, preparing an additive: preparing a grain refiner, a wetting agent and a high leveling agent, mixing and stirring the grain refiner, the wetting agent and the high leveling agent according to the installation proportion to form a mixed additive, wherein the grain refiner is 3-mercapto-1-propane sodium sulfonate, the wetting agent is alkyl alcohol polyoxyethylene polyoxypropylene ether, the high leveling agent is an amine compound containing nitrogen, the concentration of electrolyte of the grain refiner is 5ppm, the concentration of electrolyte of the wetting agent is 1.5ppm, and the concentration of electrolyte of the high leveling agent is 10ppm;
s3, cutting the Harlin groove into pieces: adding the electrolyte and the mixed additive into a Halin tank, and tabletting the electrolyte in the Halin tank;
s4, electroplating a lithium electric copper foil: three lithium electric copper foils are put into electrolyte in a Halin groove for electroplating, and the electroplated lithium electric copper foils are sequentially washed with water, passivated by chromic anhydride and dried;
s5, detecting a finished product: and stripping the dried lithium electric copper foil from the cathode plate, sequentially marking three lithium electric copper foils as No. 7, no. 8 and No. 9, and detecting glossiness and tensile strength.
Embodiment four:
as shown in fig. 1, raw materials of sulfuric acid, lead carbonate solution, grain refiner, wetting agent and high leveling agent are taken, and then the lithium electric copper foil is processed according to the following steps:
s1, preparing electrolyte: mixing sulfuric acid and lead carbonate solution to prepare electrolyte, heating and preserving the electrolyte, wherein the concentration of sulfuric acid is 100g/L-110g/L, the concentration of copper ions is 90g/L-95g/L, the concentration of chloride ions is 20mg/L-30mg/L, and the temperature of the electrolyte is 45-55 ℃;
s2, preparing an additive: preparing a grain refiner, a wetting agent and a high leveling agent, mixing and stirring the grain refiner, the wetting agent and the high leveling agent according to the installation proportion to form a mixed additive, wherein the grain refiner is sodium mercaptoimidazole propane sulfonate, the wetting agent is alkyl alcohol polyoxyethylene polyoxypropylene ether, the high leveling agent is an amine compound containing nitrogen, the concentration of electrolyte of the grain refiner is 5ppm, the concentration of electrolyte of the wetting agent is 1ppm, and the concentration of electrolyte of the high leveling agent is 10ppm;
s3, cutting the Harlin groove into pieces: adding the electrolyte and the mixed additive into a Halin tank, and tabletting the electrolyte in the Halin tank;
s4, electroplating a lithium electric copper foil: three lithium electric copper foils are put into electrolyte in a Halin groove for electroplating, and the electroplated lithium electric copper foils are sequentially washed with water, passivated by chromic anhydride and dried;
s5, detecting a finished product: and stripping the dried lithium electric copper foil from the cathode plate, sequentially marking three lithium electric copper foils as No. 10, no. 11 and No. 12, and detecting glossiness and tensile strength.
The physical properties of the lithium copper foil prepared in the above four examples were measured, and the optical enlarged diagrams of the lithium copper foil were shown in fig. 3 and 5, and the specific properties are shown in the following table:
from the above table data, it can be seen that different types of grain refiners have a certain influence on the glossiness of the copper foil, and sodium thioimidazole propane sulfonate can improve the glossiness of the copper foil, so that the mixed grain refiner is used for production, wherein 3-mercapto-1-propane sulfonate and sodium thioimidazole propane sulfonate are mixed in a ratio of 1:1 to prepare the grain refiner, and then the grain refiner is produced according to the following steps:
s1, preparing electrolyte: mixing sulfuric acid and lead carbonate solution to prepare electrolyte, heating and preserving the electrolyte, wherein the concentration of sulfuric acid is 100g/L-110g/L, the concentration of copper ions is 90g/L-95g/L, the concentration of chloride ions is 20mg/L-30mg/L, and the temperature of the electrolyte is 45-55 ℃;
s2, preparing an additive: preparing a grain refiner, a wetting agent and a high leveling agent, mixing and stirring the grain refiner, the wetting agent and the high leveling agent according to the installation proportion to form a mixed additive, wherein the grain refiner is prepared by mixing 3-mercapto-1-propane sodium sulfonate and sodium mercaptoimidazole propane sulfonate in a ratio of 1:1, the wetting agent is alkyl alcohol polyoxyethylene polyoxypropylene ether, the high leveling agent is a nitrogen-containing amine compound, the concentration of electrolyte of the grain refiner is 5ppm, the concentration of electrolyte of the wetting agent is 1.5ppm, and the concentration of electrolyte of the high leveling agent is 10ppm;
s3, cutting the Harlin groove into pieces: adding the electrolyte and the mixed additive into a Halin tank, and tabletting the electrolyte in the Halin tank;
s4, electroplating a lithium electric copper foil: placing seven pieces of lithium electric copper foil into electrolyte in a Halin groove for electroplating, and sequentially washing the electroplated lithium electric copper foil with water, passivating with chromic anhydride and drying;
s5, detecting a finished product: and stripping the dried lithium electric copper foil from the cathode plate, and detecting glossiness and tensile strength.
From the aspect of performance obtained by continuous production, the physical properties of the copper foil meet the requirements of our department, and the performance is stable. In the continuous production process, the copper foil is uniform and consistent, no color difference stripes exist, and from the microstructure, after the additive process is adjusted, the overall grain size of the copper foil is reduced, the foil surface is smoother, and the uniformity of the foil surface is increased;
the additive process is adjusted, and a novel additive combination is used, so that the 6 mu m copper foil system is used for producing the normal-temperature tensile strength average value of 70.9kgf/mm 2 Average baking tensile strength of 33.332kgf/mm 2 The average value of the baking elongation is 9.33%, the foil surface of the 6 mu m copper foil is uniform, the appearance of the copper foil is free of color difference stripes, the crystal grains of the copper foil are fine, and the whole is uniform.
The foregoing describes one embodiment of the present invention in detail, but the description is only a preferred embodiment of the present invention and should not be construed as limiting the scope of the invention. All equivalent changes and modifications within the scope of the present invention are intended to be covered by the present invention.
Claims (8)
1. The production process for improving the seersucker of the lithium electric copper foil is characterized by comprising the following steps of:
s1, preparing electrolyte: mixing sulfuric acid and lead carbonate solution to prepare electrolyte, heating and preserving the electrolyte;
s2, preparing an additive: preparing a grain refiner, a wetting agent and a high leveling agent, and mixing and stirring the grain refiner, the wetting agent and the high leveling agent according to the installation proportion to form a mixed additive;
s3, cutting the Harlin groove into pieces: adding the electrolyte and the mixed additive into a Halin tank, and tabletting the electrolyte in the Halin tank;
s4, electroplating a lithium electric copper foil: placing the lithium electric copper foil into electrolyte in a Halin tank for electroplating, and sequentially washing the electroplated lithium electric copper foil with water, passivating with chromic anhydride and drying;
s5, detecting a finished product: and stripping the dried lithium electric copper foil from the cathode plate, and detecting glossiness and tensile strength.
2. The process for producing the seersucker with the improved lithium electric copper foil according to claim 1, wherein the concentration of sulfuric acid in the S1 is 100g/L-110g/L, the concentration of copper ions is 90g/L-95g/L, the concentration of chloride ions is 20mg/L-30mg/L, and the temperature of the electrolyte is 45-55 ℃.
3. The process for producing the seersucker of the lithium-ion copper foil according to claim 1, wherein the grain refiner is prepared from 3-mercapto-1-propane sodium sulfonate, sodium mercaptoimidazole propane sulfonate or any ratio of the two.
4. The process for producing seersucker with improved lithium-ion copper foil as claimed in claim 1, wherein the wetting agent is alkyl alcohol polyoxyethylene polyoxypropylene ether or alkyl phenol polyoxyethylene polyoxypropylene ether.
5. The process for producing seersucker with improved lithium-ion copper foil as claimed in claim 1, wherein said high leveling agent is an amine compound containing nitrogen.
6. The process for producing seersucker with improved lithium-ion copper foil as claimed in claim 1, wherein the electrolyte concentration of said grain refiner is 4ppm to 5ppm.
7. The improved process for producing a seersucker with a lithium-ion copper foil as claimed in claim 1, wherein the electrolyte concentration of said wetting agent is 1ppm to 1.5ppm.
8. The process for producing seersucker with improved lithium-ion copper foil as claimed in claim 1, wherein the electrolyte concentration of the high leveling agent is 10ppm to 15ppm.
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| CN202310186025.4A CN115992375A (en) | 2023-03-01 | 2023-03-01 | Production process for improving bubble yarn of lithium electric copper foil |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117187893A (en) * | 2023-09-13 | 2023-12-08 | 广东盈华电子科技有限公司 | Electrolytic copper foil for lithium battery and preparation method and application thereof |
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- 2023-03-01 CN CN202310186025.4A patent/CN115992375A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117187893A (en) * | 2023-09-13 | 2023-12-08 | 广东盈华电子科技有限公司 | Electrolytic copper foil for lithium battery and preparation method and application thereof |
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