CN111850620B - Preparation method and preparation system of 4.5-micrometer ultrathin copper foil for lithium battery - Google Patents
Preparation method and preparation system of 4.5-micrometer ultrathin copper foil for lithium battery Download PDFInfo
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Abstract
The invention discloses a preparation method and a preparation system of a 4.5-micron ultrathin copper foil for a lithium battery, which comprises the following steps: preparing an electrolyte; adding an additive into the prepared electrolyte, wherein the additive comprises cellulose, polyethylene glycol, thiourea compounds and a leveling agent; filtering the electrolyte added with the additive, and feeding the electrolyte into an electrolytic cell for electrolytic foil formation, wherein the cellulose comprises one or more of hydroxyethyl cellulose, hydroxypropyl cellulose and hydroxypropyl methyl cellulose, one or two of 2-mercaptoethane sulfonic acid sodium salt and 2-propenyl thiourea are adopted as thiourea compounds, and one or two of polyethyleneimine and 9-phenylacridine are adopted as leveling agents. The invention can realize the preparation of the 4.5 mu m ultra-thin copper foil only by using a small amount of additives, reduces organic matters in the finished copper foil and improves the internal performance of the copper foil.
Description
Technical Field
The invention relates to a preparation method and a preparation system of a copper foil, in particular to a preparation method and a preparation system of a 4.5-micrometer ultrathin copper foil for a lithium battery, and belongs to the field of copper foil manufacturing processes.
Background
With the development of battery manufacturing technology, the thickness of the electrolytic copper foil used by the lithium ion battery is gradually reduced; the ultra-thin copper foil is required to have high tensile strength and high ductility at the same time, so that the defects of breakage, deformation and the like cannot occur in the production, processing and use processes of the battery, the thickness of the coated active substance is uniform, and the service life of the battery is prolonged. The 4,5 μm copper foil can inject more electrolyte into the same volume of battery case due to the ultra-thin characteristic, thereby increasing the capacity of the battery. However, it is known that the thinner the thickness of the electrolytic copper foil is, the higher the technical content is, the more difficult the production is; in the method for producing the thin and double-sided smooth copper foil in the prior art, a large amount of additives are required to be added for pursuing low roughness, so that a large amount of organic matters are mixed in the copper foil, and the inherent performance of the copper foil is reduced. Chinese patent publication nos. CN110396704A and CN110438531A disclose two methods for preparing ultra-thin electrolytic copper foil, respectively, but the additive amount of each component is several tens to several hundreds mg/L (i.e., ppm), and the organic content is relatively large.
Disclosure of Invention
The invention aims to provide a preparation method and a preparation system of a 4.5-micrometer ultrathin copper foil for a lithium battery, and the content of an additive is reduced.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a preparation method of a 4.5 mu m ultrathin 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 prepared electrolyte, wherein the additive comprises cellulose, polyethylene glycol, thiourea compounds and a leveling agent;
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 into a copper dissolving tank for oxidation treatment and then reacts with a dilute sulfuric acid solution at the temperature of 40-75 ℃ to form a copper sulfate solution, the copper sulfate solution is filtered by diatomite, activated carbon and an oil removal filter bag, the temperature is adjusted to 35-82 ℃ by adopting a plate heat exchanger, and the electrolyte with higher purity is prepared.
Further, the content of copper ions in the electrolyte is 60-110 g/L, the content of sulfuric acid is 40-150 g/L, the bath temperature is 40-60 ℃, the electrolytic current density is 10000A/square meter for 2000-.
Further, the cellulose comprises a combination of one or more of hydroxyethyl cellulose, hydroxypropyl cellulose, and hydroxypropyl methyl cellulose.
Furthermore, the thiourea compound adopts one or two of 2-mercaptoethane sulfonic acid sodium salt and 2-propenyl thiourea.
Further, the leveling agent adopts one or two of polyethyleneimine and 9-phenylacridine.
Further, the additive comprises 5-10 ppm of cellulose, 0.1-2 ppm of leveling agent, 0.1-0.4 ppm of thiourea compound and 0.25-3 ppm of polyethylene glycol.
Further, the third step is specifically to filter the electrolyte added with the additive by 0.45 μm to obtain high-purity electrolyte, then convey the high-purity electrolyte to the electrolytic cell according to the flow of 50-200m for carrying out thin film electrolytic production under the conditions of 10000A/square meter of 2000.
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 of 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 to obtain a dry anti-oxidation copper foil; and rolling the copper foil subjected to the anti-oxidation and drying treatment by a rolling roller, and slitting and packaging.
A4.5 mu m ultra-thin copper foil preparation system for lithium battery is characterized in that: contain the wind-up roll, acid mist updraft ventilator, the anti-oxidation groove, the anode plate, the cathode roll, drying device, clean cistern, the additive jar, overflow mouth and electrolysis trough, the additive jar is connected with clean cistern and is used for adding the additive to clean cistern, clean cistern is connected with the electrolysis trough and is used for adding electrolyte to the electrolysis trough, the cathode roll rotates and sets up in the electrolysis trough, two anode plate symmetries set up the downside in cathode roll both sides, the overflow mouth sets up the upper end at the electrolysis trough, acid mist updraft ventilator fixes at the electrolysis trough upside and is located electrolyte liquid level top, drying device sets up in cathode roll one side top, anti-oxidation groove sets up on the copper foil route of advancing between cathode roll and wind-up roll.
Compared with the prior art, the invention has the following advantages and effects: the invention improves the types of additives in the electrolyte of the electrolytic copper foil, thereby realizing the preparation of 4.5 mu m ultrathin copper foil only by using a small amount of additives, wherein the additives are in the order of single-digit ppm, and the content of the additives except cellulose can be below 1ppm, and is greatly lower than that of organic additives in the prior art, thereby reducing the organic matters in the finished copper foil and improving the inherent performance of the copper foil.
Drawings
Fig. 1 is a schematic view of a system for manufacturing an ultra-thin 4.5 μm copper foil for a lithium battery according to the present invention.
Detailed Description
To elaborate on technical solutions adopted by the present invention to achieve predetermined technical objects, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, it is obvious that the described embodiments are only partial embodiments of the present invention, not all embodiments, and technical means or technical features in the embodiments of the present invention may be replaced without creative efforts, and the present invention will be described in detail below with reference to the drawings and in conjunction with the embodiments.
As shown in figure 1, the system for preparing the 4.5 mu m ultrathin copper foil for the lithium battery comprises a winding roller 1, an acid mist air draft device 2, an anti-oxidation groove 3, an anode plate 4 and a cathode roller 5, drying device 6, net liquid groove 7, additive jar 8, overflow mouth 9 and electrolysis trough 10, additive jar 8 is connected with net liquid groove 7 and is used for adding the additive to net liquid groove 7, net liquid groove 7 is connected with electrolysis trough 10 and is used for adding electrolyte to electrolysis trough 10, cathode roll 5 rotates and sets up in electrolysis trough 10, the downside in cathode roll 5 both sides is set up to two anode plate 4 symmetries, overflow mouth 9 sets up the upper end at electrolysis trough 10, acid mist updraft ventilator 2 fixes at electrolysis trough 10 upside and is located electrolyte liquid level top, drying device 6 sets up in cathode roll 5 one side top, anti-oxidation groove 3 sets up on the copper foil route of advancing between cathode roll 5 and wind-up roll 1.
A preparation method of a 4.5 mu m ultrathin copper foil for a lithium battery is characterized by comprising the following steps:
the method comprises the following steps: and preparing an electrolyte.
Preparing electrolyte in a liquid purifying tank 7; the copper material is blown and oxidized in a copper dissolving tank and then reacts with dilute sulfuric acid solution at the temperature of 40-75 ℃ to form copper sulfate solution, and then the copper sulfate solution is filtered by diatomite, activated carbon and an oil removal filter bag, and the temperature is adjusted to 35-82 ℃ by adopting a plate heat exchanger to prepare the electrolyte with higher purity.
The copper ion content in the electrolyte is 60-110 g/L, the sulfuric acid content is 40-150 g/L, the bath temperature is 40-60 ℃, the electrolytic current density is 10000A/square meter for 2000-one year, and the copper foil speed, namely the winding speed of the winding roller 1 is 2-10 m/min according to the Faraday law.
Step two: and adding additives into the prepared electrolyte, wherein the additives comprise cellulose 8a, polyethylene glycol 8b, thiourea compounds 8c and leveling agents 8 d.
The cellulose comprises a combination of one or more of hydroxyethyl cellulose, hydroxypropyl cellulose, and hydroxypropyl methyl cellulose. Hydroxyethyl cellulose, hydroxypropyl cellulose and hydroxypropyl methyl cellulose are nonionic hydrocolloids and have a variety of uses such as adsorption, film formation and moderate surface activity in the copper foil electrodeposition process.
The thiourea compound adopts one or two of 2-mercaptoethane sulfonic acid sodium salt and 2-propenyl thiourea. The water-soluble thiourea compound can form a complex salt with a metal and contribute to the formation of a stable interfacial film, and preferably 2-mercaptoethanesulfonic acid sodium salt (MES) which can reduce the height of the peak while increasing the number of matte peaks in the presence of the other three additives.
The leveling agent adopts one or two of polyethyleneimine and 9-phenylacridine. The polyethyleneimine and 9-phenylacridine have the capability of forming a coordination compound with copper, and the definition of a rough surface fine morphology peak is improved in the copper foil manufacturing process, so that excellent interlocking with a polymer matrix is ensured, and excellent bondability is formed.
Polyethylene glycol (PEG) has unusual solubility, is very helpful to play a complementary role with other three additives rather than a conflicting role, and can form uniform fine morphology on the rough surface in the copper foil manufacturing process to improve the uniformity of a fine structure.
Through the combination of the additives, the additives only contain 5-10 ppm of cellulose, 0.1-2 ppm of leveling agent, 0.1-0.4 ppm of thiourea compound and 0.25-3 ppm of polyethylene glycol, and the manufacturing of the 4.5 mu m ultrathin copper foil can be realized.
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 50-200m for carrying out thin film electrolytic production under the conditions of 10000A/square meter of 2000.
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 of 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 to obtain a dry anti-oxidation copper foil; and rolling the copper foil subjected to the anti-oxidation and drying treatment by a rolling roller, and slitting and packaging.
The present application is further illustrated by the following specific examples and performance tests of copper foil.
Example 1:
a preparation method of an ultrathin copper foil with the thickness of 4.5 mu m for a lithium battery comprises the following steps:
the method comprises the following steps: preparing an electrolyte; the method comprises the steps of blowing and oxidizing a copper material in a copper dissolving tank, reacting the copper material with a dilute sulfuric acid solution at 40-50 ℃ to obtain a copper sulfate solution, filtering the copper sulfate solution by using diatomite, activated carbon, an oil removal filter bag and the like, adjusting the temperature to 35-65 ℃ by using a plate heat exchanger, and preparing the electrolyte with high purity. In a copper sulfate electrolyte, the concentration of Cu2+ is 60-85 g/L, and the concentration of H2SO4 is 40-800 g/L; the temperature of the electrolyte is controlled to be 40-500 ℃, and the conveying flow of the electrolyte is 50-90 m for each hour.
Step two: adding an additive into the electrolyte; the additive comprises one or two or three of hydroxyethyl cellulose, hydroxypropyl cellulose or hydroxypropyl methyl cellulose, the total content is 5-7 ppm, one or two of polyethyleneimine or 9-phenylacridine is 0.1-0.5 ppm, one or two of 2-mercaptoethane sulfonic acid sodium salt or 2-propenyl thiourea is 0.1-0.2 ppm, and the content of polyethylene glycol is 0.25-1.5 ppm.
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 rate of 50-90 m/h, and electrolyzing to generate foil under the condition of 2000-5000A/square meter, wherein the speed of the vehicle is 2-5 m/min. The electrolyzed copper foil is subjected to the processes of electrolyte pickling, pure water washing and drying to obtain a 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 copper foil thickness detection method comprises the following steps: and shearing the copper foil with the fixed area, putting the copper foil on a tray balance, weighing, and obtaining the thickness of the corresponding copper foil by a weighing method.
The method for detecting the organic content of the copper foil comprises the following steps: weighing quantitative electrolyte, and detecting the content of organic matters in the electrolyte through a CVS instrument to ensure that the content of the additive does not exceed the control range.
The electrolytic copper foil produced by adopting the additive and the process has the advantages that a torn edge appears at 9000-11000 meters, the thickness of the torn edge is 4.5 mu m, the tensile strength is 372N/mm2, and the elongation is 3.5%.
Example 2:
a preparation method of an ultrathin copper foil with the thickness of 4.5 mu m for a lithium battery comprises the following steps:
the method comprises the following steps: preparing an electrolyte; the method comprises the steps of carrying out blowing oxidation treatment on a copper material in a copper dissolving tank, reacting the copper material with a dilute sulfuric acid solution at 55-70 ℃ to obtain a copper sulfate solution, filtering the copper sulfate solution by diatomite, activated carbon, an oil removing filter bag and the like, adjusting the temperature to 65-80 ℃ by adopting a plate heat exchanger, and preparing the electrolyte with high purity. In a copper sulfate electrolyte, the concentration of Cu2+ is 90-110 g/L, and the concentration of H2SO4 is 80-120 g/L; the temperature of the electrolyte is controlled to be 60-70 ℃, and the conveying flow of the electrolyte is 90-1500 m for each year.
Step two: adding an additive into the electrolyte; the additive comprises one or two or three of hydroxyethyl cellulose, hydroxypropyl cellulose or hydroxypropyl methyl cellulose, the total content is 7-10 ppm, one or two of polyethyleneimine or 9-phenylacridine is 0.6-1 ppm, one or two of 2-mercaptoethane sulfonic acid sodium salt or 2-propenyl thiourea is 0.2-0.4 ppm, and the content of polyethylene glycol is 1.6-3 ppm.
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 90-1500 m/h, and electrolyzing to generate foil under the condition of 6000-10000A/square meter, wherein the speed of the vehicle is 7-10 m/min. The electrolyzed copper foil is subjected to the processes of electrolyte pickling, pure water washing and drying to obtain a 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 copper foil thickness detection method comprises the following steps: and shearing the copper foil with the fixed area, putting the copper foil on a tray balance, weighing, and obtaining the thickness of the corresponding copper foil by a weighing method.
The method for detecting the organic content of the copper foil comprises the following steps: weighing quantitative electrolyte, and detecting the content of organic matters in the electrolyte through a CVS instrument to ensure that the content of the additive does not exceed the control range.
The electrolytic copper foil produced by adopting the additive and the process has the advantages that the torn edge appears at 9000-11000 meters, the thickness of the electrolytic copper foil is 4.5 mu m, the tensile strength is 389N/mm2, and the elongation is 3.8%.
Comparative example 3:
a preparation method of an ultrathin copper foil with the thickness of 4.5 mu m for a lithium battery comprises the following steps:
the method comprises the following steps: preparing an electrolyte; the method comprises the steps of blowing and oxidizing a copper material in a copper dissolving tank, reacting the copper material with a dilute sulfuric acid solution at 40-50 ℃ to obtain a copper sulfate solution, filtering the copper sulfate solution by using diatomite, activated carbon, an oil removal filter bag and the like, adjusting the temperature to 35-65 ℃ by using a plate heat exchanger, and preparing the electrolyte with high purity. In a copper sulfate electrolyte, the concentration of Cu2+ is 60-85 g/L, and the concentration of H2SO4 is 40-800 g/L; the temperature of the electrolyte is controlled to be 40-500 ℃, and the conveying flow of the electrolyte is 50-90 m for each hour.
Step two: conventional additives are added to the electrolyte.
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 rate of 50-90 m/h, and electrolyzing to generate foil under the condition of 2000-5000A/square meter, wherein the speed of the vehicle is 2-5 m/min. The electrolyzed copper foil is subjected to the processes of electrolyte pickling, pure water washing and drying to obtain a 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 copper foil thickness detection method comprises the following steps: and shearing the copper foil with the fixed area, putting the copper foil on a tray balance, weighing, and obtaining the thickness of the corresponding copper foil by a weighing method.
The method for detecting the organic content of the copper foil comprises the following steps: weighing quantitative electrolyte, and detecting the content of organic matters in the electrolyte through a CVS instrument to ensure that the content of the additive does not exceed the control range.
The electrolytic copper foil produced by adopting the additive and the process has the advantages that the torn edge appears in 2600-4000 meters, the thickness of the electrolytic copper foil is 4.7 mu m, the tensile strength is 288N/mm2, and the elongation is 2.8%.
As can be seen from the comparative analysis of the above examples 1 and 2 and comparative example 3, the electrolytic copper foils prepared by the preparation method of the present invention of examples 1 and 2 have much higher performance parameters such as thickness, tensile strength and elongation than comparative example 3.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (3)
1. A preparation method of a 4.5 mu m ultrathin copper foil for a lithium battery is characterized by comprising the following steps:
the method comprises the following steps: preparing an electrolyte; the first step is that copper materials are blown into a copper dissolving tank for oxidation treatment and then react with dilute sulfuric acid solution at the temperature of 40-75 ℃ 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 35-82 ℃ by adopting a plate heat exchanger to prepare electrolyte with higher purity; the copper ion content in the electrolyte is 60-110 g/L, the sulfuric acid content is 40-150 g/L, the bath temperature is 40-60 ℃, the electrolytic current density is 10000A/square meter for 2000-;
step two: adding an additive into the prepared electrolyte, wherein the additive comprises cellulose, polyethylene glycol, 2-propenyl thiourea and 9-phenylacridine;
step three: filtering the electrolyte added with the additive and sending the electrolyte into an electrolytic cell for electrolytic foil generation;
the cellulose comprises a combination of one or more of hydroxyethyl cellulose, hydroxypropyl cellulose, and hydroxypropyl methyl cellulose;
the additive comprises 5-10 ppm of cellulose, 0.1-2 ppm of 9-phenylacridine, 0.1-0.4 ppm of 2-propenyl thiourea and 0.25-3 ppm of polyethylene glycol.
2. The method for preparing an ultra-thin copper foil of 4.5 μm for a lithium battery according to claim 1, wherein: and the third step is specifically to filter the electrolyte added with the additive by 0.45 mu m to obtain high-purity electrolyte, then convey the high-purity electrolyte to an electrolytic cell according to the flow of 50-200 m/h, and electrolyze to generate foil under the conditions of 2000 plus 10000A/square meter.
3. The method for preparing an ultra-thin copper foil of 4.5 μm for a lithium battery according to claim 2, 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 of 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 to obtain a dry anti-oxidation copper foil; and rolling the copper foil subjected to the anti-oxidation and drying treatment by a rolling roller, and slitting and packaging.
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| CN110016697A (en) * | 2019-05-22 | 2019-07-16 | 青海电子材料产业发展有限公司 | A kind of method and its additive preparing high temperature high-elongation power battery electrolytic copper foil |
| CN110760898A (en) * | 2019-11-26 | 2020-02-07 | 江东电子材料有限公司 | Preparation method of high-tensile electrolytic copper foil for lithium battery |
| CN111005041A (en) * | 2019-12-30 | 2020-04-14 | 中国科学院青海盐湖研究所 | Composite multi-layer structure porous copper foil and preparation method and system thereof |
| CN111041530A (en) * | 2019-12-30 | 2020-04-21 | 中国科学院青海盐湖研究所 | High-tensile-strength copper foil and preparation method and system thereof |
| 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 |
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