CN118016900A - Composite aluminum foil current collector and preparation method thereof - Google Patents

Composite aluminum foil current collector and preparation method thereof Download PDF

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Publication number
CN118016900A
CN118016900A CN202410417314.5A CN202410417314A CN118016900A CN 118016900 A CN118016900 A CN 118016900A CN 202410417314 A CN202410417314 A CN 202410417314A CN 118016900 A CN118016900 A CN 118016900A
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current collector
aluminum foil
foil current
composite aluminum
conductive layer
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CN118016900B (en
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张松林
刘建
鞠金虎
汤蕾
接道良
左黎明
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Jiangsu Kanghui New Material Technology Co ltd
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Jiangsu Kanghui New Material Technology Co ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
    • B05D5/12—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain a coating with specific electrical properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D1/00—Processes for applying liquids or other fluent materials
    • B05D1/36—Successively applying liquids or other fluent materials, e.g. without intermediate treatment
    • B05D1/38—Successively applying liquids or other fluent materials, e.g. without intermediate treatment with intermediate treatment
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    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
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    • B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
    • B05D3/02—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by baking
    • B05D3/0254—After-treatment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B05D7/24—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials for applying particular liquids or other fluent materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
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    • B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
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Abstract

The invention belongs to the technical field of lithium ion batteries, and relates to a composite aluminum foil current collector and a preparation method thereof. The preparation method comprises the following steps: coating the conductive layer coating liquid uniformly dispersed with the flaky aluminum silver powder and the nanometer tin powder on at least one side surface of a base material by adopting a scraper, and drying to obtain a composite aluminum foil current collector; the sheet resistance of the prepared composite aluminum foil current collector is below 20mΩ, the battery capacity retention rate is above 85% after 1000 cycles at 1C charge-discharge multiplying power, the adhesive force of the conductive layer is 95-100%, and the needling test has no short circuit. The composite aluminum foil current collector has good binding force and good conductive path, and can be produced in a large scale; the preparation method of the invention has high efficiency and low cost.

Description

Composite aluminum foil current collector and preparation method thereof
Technical Field
The invention belongs to the technical field of lithium ion batteries, and relates to a composite aluminum foil current collector and a preparation method thereof.
Background
In electrochemical applications of lithium ion batteries, current collectors are a key component, mainly for carrying electrode materials and conducting electrons, and since lithium ion batteries are commercially used, commercial lithium ion batteries have adopted aluminum foils and copper foils as positive and negative current collectors. The reasonable selection of the current collector is the precondition of successful operation of the lithium ion battery, improves the conductivity and corrosion resistance of the current collector, and is beneficial to improving the capacity, charge and discharge efficiency and cycle stability of the lithium ion battery.
Although the application of aluminum foil and copper foil is very mature, alternative composite current collectors have the following advantages:
high security: the composite current collector adopts a sandwich structure and consists of a high polymer material layer in the middle and metal accumulation layers on two sides. The structure can prevent the battery from thermal runaway, only smoking and not firing, and improves the safety performance of the battery.
High specific energy: the composite current collector has high energy density and good cycle life, and can provide sufficient overcharge protection and stable large-current discharge capacity.
Therefore, it is important to study how to prepare the composite current collector. At present, a composite current collector mainly forms a sandwich-type composite structure by plating copper or aluminum metal layers with certain thickness on two sides of a high polymer material layer (taking PET, PP or PI as a base material). The thickness of the middle polymer material layer is generally about 4 μm, and the thicknesses of the upper and lower metal layers are each 1 μm, which amounts to about 6 μm. The material of the high polymer material layer can be PET (polyethylene terephthalate), PP (polypropylene) or PI (polyimide).
Patent application CN117080455A (publication No. 2023, 11, 17) discloses a composite current collector and a preparation method thereof, wherein an electroplated copper foil is formed on the surface of a cathode roller by electroplating, and the thickness of the electroplated copper foil is less than 6 μm; obtaining a supporting layer, wherein the supporting layer comprises an insulating high polymer material layer, and an adhesive layer is formed on the surface to be bonded of the insulating high polymer material layer; and (3) attaching the adhesive layer on the supporting layer to the surface of the electroplated copper foil, bonding the supporting layer and the electroplated copper foil to form a composite structure, and stripping the composite structure from the cathode roller.
Therefore, the composite current collector in the prior art generally adopts an electroplating mode to obtain a metal layer of copper or aluminum, but aluminum is amphoteric metal, can be dissolved in acid and alkali and is unstable in acid and alkali electroplating solutions, so that the composite aluminum foil current collector with high safety and high specific energy cannot be prepared in a large scale, high efficiency and low cost by adopting the traditional electroplating mode.
Therefore, research is needed to provide a novel preparation method of the composite aluminum foil current collector, which not only ensures that the composite aluminum foil current collector has high safety and high specific energy, but also has high efficiency, easy mass production and low production cost.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a composite aluminum foil current collector and a preparation method thereof.
In order to achieve the above purpose, the invention adopts the following technical scheme:
A preparation method of a composite aluminum foil current collector comprises the steps of coating conductive layer coating liquid uniformly dispersed with flaky aluminum silver powder and nanometer tin powder on at least one side surface of a base material by adopting a scraper, and drying to obtain the composite aluminum foil current collector;
The conductive layer coating liquid comprises the following components in parts by weight: 4.6-4.8 parts of flaky aluminum silver powder, 0.2-0.4 part of nano tin powder, 79 parts of water and 1 part of auxiliary agent;
The D50 particle size of the flaky aluminum silver powder is 9-11 mu m, and the thickness of the flaky aluminum silver powder is 20-30nm; the average grain diameter of the nano tin powder is 50nm;
the temperature of the drying is T 1,T1 which is higher than the melting point of the nano tin powder and is lower than the melting point of the flaky aluminum silver powder and the use temperature of the base material.
When the conductive layer coating liquid is coated on the substrate by a scraper, the flaky aluminum silver powder is tiled on the surface of the substrate, the content of the flaky aluminum silver powder in the conductive layer coating liquid is controlled, and meanwhile, the size of the flaky aluminum silver powder is controlled, so that different flaky aluminum silver powder on the surface of the substrate is separated by a certain distance.
As a preferable technical scheme:
According to the preparation method of the composite aluminum foil current collector, the auxiliary agent is the mixture of the alkyne diol wetting agent and the polyurethane thickener, the alkyne diol wetting agent can quickly reduce the surface tension, ensure good wetting and full contact of the flaky aluminum silver powder and the nano tin powder, and the polyurethane thickener can effectively improve the shear viscosity, has higher thickening rate and improves the film forming property.
According to the preparation method of the composite aluminum foil current collector, the weight part ratio of the alkyne diol wetting agent to the polyurethane thickener is 1:1, so that the flaky aluminum silver powder and the nanometer tin powder are more fully wetted and contacted, and the whole system has a better thickening effect and provides better leveling property and film forming property.
According to the preparation method of the composite aluminum foil current collector, the wet weight of the coating of the conductive layer coating liquid on the single side surface of the substrate is 20-25g/m 2, the thickness of the conductive layer can be controlled by controlling the wet weight of the coating, and the wet weight range can ensure that the thickness of the conductive layer is good, so that good conductivity can be ensured, and the composite aluminum foil current collector is favorable for being firmly combined on the substrate.
According to the preparation method of the composite aluminum foil current collector, T 1 is 225-235 ℃, the melting point of the nano tin powder is related to the size of the nano tin powder, and when the average particle size of the nano tin powder is 50nm, the nano tin powder can be micro-melted at 225-235 ℃.
According to the preparation method of the composite aluminum foil current collector, the drying time is more than or equal to 20s; the drying is carried out under the protection of nitrogen or inert gas, so that oxidation of the metal conductive material can be avoided.
According to the preparation method of the composite aluminum foil current collector, before the conductive layer coating liquid is coated on the substrate, the adhesive layer is formed on the surface of the substrate to be coated with the conductive layer coating liquid, so that the conductive layer and the substrate can be combined more firmly.
The preparation method of the composite aluminum foil current collector comprises the following steps of: the adhesive layer is formed by drying the adhesive layer coating liquid after the adhesive layer coating liquid is coated on the surface of the substrate to be coated with the conductive layer coating liquid, the drying temperature is T 2,T2<T1, the forming modes of the adhesive layer can be various, and the adhesive layer is preferably formed by adopting a coating mode in view of simple and convenient operation of the coating mode.
The preparation method of the composite aluminum foil current collector comprises the following components in parts by weight: 40 parts of water, 2 parts of single-walled carbon nanotubes, 0.5 part of multifunctional wetting agent, 40 parts of aqueous polyurethane and 2 parts of aqueous closed curing agent, wherein the single-walled carbon nanotubes have excellent electronic, mechanical and mechanical properties, can form a three-dimensional reinforced conductive network, enhance conductivity and improve the material strength of an adhesive layer; the multifunctional wetting agent reduces the surface tension, improves the surface smoothness and wettability, and improves the blocking resistance in an aqueous system; the waterborne polyurethane is mainly solidified by cohesive force and adhesion force generated by polar groups in molecules, and carboxyl, hydroxyl and the like in the waterborne polyurethane can also participate in the reaction to crosslink, so that better adhesive effect is generated; the aqueous closed type curing agent can enhance the crosslinking reaction and the binding force.
According to the preparation method of the composite aluminum foil current collector, the pipe diameter of the single-wall carbon nano-tube is 1-2nm, the length of the single-wall carbon nano-tube is 0.55-2 mu m, the conductivity is more than 150S/cm, the small size of the single-wall carbon nano-tube is better dispersed in a coating to form a conductive network, and the conductivity is enhanced.
The preparation method of the composite aluminum foil current collector has the characteristics that the water-based closed curing agent does not release isocyanate (-NCO) groups at T 2 and releases isocyanate groups at T 1; the surface of the substrate contains hydroxyl and/or ester groups (the groups can be self-contained groups of the film or groups generated after corona treatment, and the groups can carry out crosslinking reaction with isocyanate groups released by the water-based sealing curing agent to form a firmer combination between the substrate and the adhesive layer); in the preparation process of the composite aluminum foil current collector, an adhesive layer is formed on the surface of a substrate, and then a conductive layer is formed on the surface of the adhesive layer, and as the water-based closed curing agent has the characteristics of not releasing isocyanate groups under T 2 and releasing isocyanate groups under T 1, and meanwhile, the surface of the substrate contains hydroxyl groups and/or ester groups, when the adhesive layer is prepared, only solvents are evaporated in the drying process, when the conductive layer is prepared, not only are solvents evaporated in the drying process, but also the water-based closed curing agent releases isocyanate groups, and the isocyanate groups react with hydroxyl groups, ester groups and other groups on the surface of the substrate, and hydroxyl groups, carboxyl groups and other groups on the surface of the conductive layer simultaneously to form a crosslinked structure to generate firm chemical bonds, so that the binding force of the substrate and the conductive layer is obviously improved.
According to the preparation method of the composite aluminum foil current collector, the weight content of isocyanate groups of the water-based closed curing agent is 6-7%, and the proper curing agent content directly influences the reactivity and crosslinking density of the curing agent.
According to the preparation method of the composite aluminum foil current collector, the thickness of the base material is 4-6 mu m, and the type of the base material is not limited as long as the melting point of the base material is higher than T 1.
According to the preparation method of the composite aluminum foil current collector, the wet weight of the adhesive layer coating liquid coating on the surface of one side of the substrate is 3-5g/m 2, and after the coating wet weight in the range is dried, the adhesive layer is ensured to have proper thickness and viscosity, so that the bonding force between the conductive layer and the substrate is better.
According to the preparation method of the composite aluminum foil current collector, the T 2 is 105-110 ℃, the temperature range is favorable for timely and rapid drying of the adhesive layer, the deactivation of the water-based closed curing agent in the adhesive layer can be avoided, and the premature release of isocyanate groups can be avoided.
The invention also provides the composite aluminum foil current collector prepared by the preparation method of the composite aluminum foil current collector, the sheet resistance of the composite aluminum foil current collector is below 20mΩ, the battery capacity retention rate is above 85% after 1000 cycles at 1C charge-discharge multiplying power, the adhesive force of the conductive layer is 95-100%, and the needling test does not have short circuit.
The beneficial effects are that:
(1) According to the invention, after the conductive layer coating liquid is coated on the substrate by adopting the scraper, flaky aluminum silver powder is uniformly paved on the surface of the substrate, and in the drying process at the temperature T1, especially at 235-245 ℃, the surfaces of nanometer tin powder among flaky aluminum silver powder are slightly melted, the physical space distance is reduced, metal bonding is formed, different flaky aluminum silver powder are connected together, a good conductive path is formed, and a composite structure with an excellent aluminum metal layer is obtained;
(2) The adhesive layer is dried at the temperature T 2, water is evaporated to form a film, and then the aqueous closed curing agent of the adhesive layer releases isocyanate groups at the temperature T 1, especially at 235-245 ℃, so that the isocyanate groups react with hydroxyl groups, ester groups and other groups generated by PET corona serving as a base material, and react with hydroxyl groups, carboxyl groups and other groups on the surface of the conductive layer to form a crosslinked structure, so that a firm chemical bond is generated, and the obtained composite aluminum foil current collector has better binding force;
(3) The preparation method provided by the invention avoids the electroplating mode, is easy to operate and control no matter in the process of conductive coating, coating mode or high-temperature baking, is easy for large-scale mass production, has high production efficiency and low cost, can produce single wires, and is favorable for obtaining the composite aluminum foil current collector with high safety and high specific energy.
(4) The composite aluminum foil current collector prepared by the invention has good conductivity, sheet resistance of less than 20mΩ, circulation performance similar to that of an aluminum foil current collector soft package battery, and similar charge and discharge capacity, and under the same test conditions, the battery capacity retention rate of the composite aluminum foil current collector is more than 85%, which indicates that the composite aluminum foil current collector is completely suitable for the existing battery preparation technology, has no influence on the electrochemical performance of the battery, has a great improvement effect on the needling safety of the battery, and inhibits the internal short circuit in the needling process of the battery.
Drawings
Fig. 1 is a schematic structural view of a composite aluminum foil current collector of the present invention;
wherein, 1-substrate, 2-cross linker layer, 3-conductive layer.
Detailed Description
The application is further described below in conjunction with the detailed description. It is to be understood that these examples are illustrative of the present application and are not intended to limit the scope of the present application. Furthermore, it should be understood that various changes and modifications can be made by one skilled in the art after reading the teachings of the present application, and such equivalents are intended to fall within the scope of the application as defined in the appended claims.
The following are test methods for the relevant performance indicators in each of the examples and comparative examples:
sheet resistance: the prepared composite aluminum foil current collector sample was placed on a sample stage, and the sheet resistance of the sample was tested using four probes Fang Zuyi (manufacturer is su lattice electronics limited, model ST 2258C).
Adhesion of the conductive layer: the conductive layer was tested for adhesion according to JISK-5600, where 100% represents no drop and 0% represents complete drop.
Battery capacity retention after 1000 cycles at 1C charge-discharge rate: the lithium ion battery is assembled, an aluminum foil (thickness is 12 μm) is adopted as a positive electrode current collector, liNi 0.6Mn0.2Co0.2O2 (NCM 622) is adopted as a positive electrode current collector, the composite aluminum foil current collector prepared in the embodiment is adopted as a negative electrode current collector, artificial graphite (manufactured by Guangdong Jin Xin energy technology Co., ltd., brand name AML403 ST) is adopted as a negative electrode material, a polyethylene diaphragm (thickness is 25 μm) is coated by alumina ceramic, 1 mol.L -1 LiPF6 carbonate solution is adopted as electrolyte, a mixture of propylene carbonate, ethylene carbonate and methyl ethyl carbonate with mass ratio of 1:1:1 is adopted as carbonate, the assembled battery is charged and discharged for 1000 times in a circulating manner, and the battery capacity retention rate after the charging and discharging is recorded.
Needling test: the needling test is carried out on a 200mAh soft package battery using a composite aluminum foil current collector, the battery is in a state of 100% of charge depth, the voltage is 4V, and after needling, if the voltage has no obvious change and no fire and smoke phenomena, the battery is indicated to have no short circuit.
Example 1
The preparation method of the composite aluminum foil current collector comprises the following specific steps:
(1) Preparing raw materials;
Water;
Single-wall carbon nanotubes: the manufacturer is Beijing Deke island gold technology Co., ltd, the model is CNT400, the pipe diameter is 1-2nm, the length is 0.55-2 μm, and the conductivity is >150S/cm;
Multifunctional wetting agent: the manufacturer is Pick auxiliary agent (Shanghai) limited company, and the model is BYK-333;
Aqueous polyurethane: the manufacturer is Anhui An Dahua Tai New Material Co., ltd, and the model is AH-1604F;
aqueous blocked curing agent: the manufacturer is Anhui An Dahua Tai New Material Co., ltd, the model is A05, and the weight content of isocyanate groups is 6%;
Flake aluminum silver powder: the manufacturer is Hunan Jin new material science and technology Co., ltd, the model is CYH-15, the D50 grain diameter is 9-11 mu m, and the thickness is 20-30nm;
Nano tin powder: manufacturer is Shanghai super-Wei nano technology Co., ltd, model is CW-Sn-001, average grain diameter is 50nm, melting point is 231.9 ℃;
Auxiliary agent: a mixture of 1:1 parts by weight of an acetylenic diol wetting agent (manufacturer is Yingzhu specialty Chemie (Shanghai) Co., model number Surfynol 440) and a polyurethane thickener (manufacturer is Suzhou cloud chemical Co., ltd., model number YZ-516);
A base material: the PI film with the surface subjected to corona treatment is manufactured by DuPont Dongli, the model is Kapton 20EN, and the thickness is 5 mu m;
Protective gas: nitrogen or inert gas;
(2) Preparing adhesive layer coating liquid;
The adhesive layer coating liquid comprises the following components in parts by weight: 40 parts of water, 2 parts of single-walled carbon nanotubes, 0.5 part of multifunctional wetting agent, 40 parts of aqueous polyurethane and 2 parts of aqueous closed curing agent;
(3) Preparing a conductive layer coating liquid;
The conductive layer coating liquid comprises the following components in parts by weight: 4.6 parts of flaky aluminum silver powder, 0.2 part of nano tin powder, 79 parts of water and 1 part of auxiliary agent;
(4) Coating adhesive layer coating liquid on the two side surfaces of the substrate, and drying at 105 ℃ to form an adhesive layer; wherein the wet weight of the adhesive layer coating liquid coating on the surface of one side of the substrate is 3g/m 2;
(5) Under the protection of protective gas, coating the conductive layer coating liquid on the surfaces of both sides of the substrate by adopting a scraper, and drying at 235 ℃ to obtain a composite aluminum foil current collector; wherein the wet weight of the conductive layer coating liquid coating on the surface of one side of the substrate is 20g/m 2.
The structure of the finally prepared composite aluminum foil current collector is shown in fig. 1, and the structure of the finally prepared composite aluminum foil current collector consists of a conductive layer 3, an adhesive layer 2, a base material 1, the adhesive layer 2 and the conductive layer 3 from top to bottom, wherein the sheet resistance of the composite aluminum foil current collector is 20mΩ, the battery capacity retention rate after 1000 cycles at a charge-discharge rate of 1C is 85%, the adhesive force of the conductive layer is 100%, and the needling test does not have short circuit.
Comparative example 1
A method of preparing a current collector, substantially the same as in example 1, except that: in the step (3), the addition part of the flaky aluminum silver powder is 4.2 parts.
The sheet resistance of the finally prepared current collector was 134mΩ.
The conductive properties of the current collector were significantly reduced compared to example 1, because the addition amount of the plate-like aluminum silver powder in comparative example 1 was too small to form a conductive path.
Comparative example 2
A method of preparing a current collector, substantially the same as in example 1, except that: in the step (5), the temperature of the drying is 200 ℃.
The sheet resistance of the finally prepared current collector was 78mΩ.
The conductivity of the current collector is significantly reduced compared to that of comparative example 2, because the drying temperature in comparative example 2 is lower than the melting point of the nano-tin powder, and a portion of the tin powder does not complete melting to form a conductive path.
Example 2
A method for preparing a composite aluminum foil current collector, which is basically the same as in example 1, and is different only in that: the manufacturer of the water-based sealing type curing agent in the step (1) is Dongguan Jiang Xing Utility company, and the brand is JX-82.
The sheet resistance of the finally prepared composite aluminum foil current collector is 20mΩ, the battery capacity retention rate is 85% after 1000 cycles at a 1C charge-discharge rate, the adhesive force of the conductive layer is 97%, and the needling test has no short circuit.
Example 3 has reduced adhesion to 97% compared to example 1 because the aqueous blocked curing agent of example 1 has the property of not releasing isocyanate groups at T 2 and releasing isocyanate groups at T 1, and the isocyanate groups react with the hydroxyl groups, carboxyl groups, imide groups, and the like on the surface of the substrate and the hydroxyl groups and carboxyl groups, and the like on the surface of the conductive layer simultaneously to form a crosslinked structure to generate a strong chemical bond, thereby significantly improving the bonding force between the substrate and the conductive layer, compared to example 3.
Example 3
A method for preparing a composite aluminum foil current collector, which is basically the same as in example 1, and is different only in that: step (2) and step (4) are not performed.
The sheet resistance of the finally prepared composite aluminum foil current collector is 20mΩ, the battery capacity retention rate is 85% after 1000 cycles at a 1C charge-discharge rate, the adhesive force of the conductive layer is 95%, and the needling test has no short circuit.
Example 4
The preparation method of the composite aluminum foil current collector comprises the following specific steps:
(1) Preparing raw materials;
Water;
Single-wall carbon nanotubes: the manufacturer is Beijing Deke island gold technology Co., ltd, the model is CNT400, the pipe diameter is 1-2nm, the length is 0.55-2 μm, and the conductivity is >150S/cm;
Multifunctional wetting agent: the manufacturer is Pick auxiliary agent (Shanghai) limited company, and the model is BYK-333;
Aqueous polyurethane: the manufacturer is Anhui An Dahua Tai New Material Co., ltd, and the model is AH-1604F;
Aqueous blocked curing agent: the manufacturer is Anhui An Dahua Tai New Material Co., ltd, the model is A05, and the weight content of isocyanate groups is 7%;
Flake aluminum silver powder: the manufacturer is Hunan Jin new material science and technology Co., ltd, the model is CYH-15, the D50 grain diameter is 9-11 mu m, and the thickness is 20-30nm;
Nano tin powder: manufacturer is Shanghai super-Wei nano technology Co., ltd, model is CW-Sn-001, average grain diameter is 50nm, melting point is 231.9 ℃;
Auxiliary agent: a mixture of 1:1 parts by weight of an acetylenic diol wetting agent (manufacturer is Yingzhu specialty Chemie (Shanghai) Co., model number Surfynol 440) and a polyurethane thickener (manufacturer is Suzhou cloud chemical Co., ltd., model number YZ-516);
A base material: the PI film with the surface subjected to corona treatment is manufactured by DuPont Dongli, the model is Kapton 20EN, and the thickness is 5 mu m;
Protective gas: nitrogen or inert gas;
(2) Preparing adhesive layer coating liquid;
The adhesive layer coating liquid comprises the following components in parts by weight: 40 parts of water, 2 parts of single-walled carbon nanotubes, 0.5 part of multifunctional wetting agent, 40 parts of aqueous polyurethane and 2 parts of aqueous closed curing agent;
(3) Preparing a conductive layer coating liquid;
the conductive layer coating liquid comprises the following components in parts by weight: 4.8 parts of flaky aluminum silver powder, 0.4 part of nano tin powder, 79 parts of water and 1 part of auxiliary agent;
(4) Coating adhesive layer coating liquid on the surfaces of both sides of a substrate, and drying at 110 ℃ to form an adhesive layer; wherein, the wet weight of the adhesive layer coating liquid coating on the surface of one side of the substrate is 5g/m 2;
(5) Under the protection of protective gas, coating the conductive layer coating liquid on the surfaces of both sides of the substrate by adopting a scraper, and drying at 245 ℃ to obtain a composite aluminum foil current collector; wherein the wet weight of the conductive layer coating liquid coating on the surface of one side of the substrate is 25g/m 2.
The sheet resistance of the finally prepared composite aluminum foil current collector is 10mΩ, the battery capacity retention rate after 1000 cycles at 1C charge-discharge multiplying power is 92%, the adhesive force of the conductive layer is 95%, and the needling test has no short circuit.
Example 5
A method for preparing a composite aluminum foil current collector, which is basically the same as in example 4, except that: in the step (4), the adhesive layer coating liquid is coated on only one side surface of the substrate; in the step (5), the conductive layer coating liquid is applied only to the surface of one side (the side coated with the adhesive layer coating liquid) of the substrate.
The sheet resistance of the finally prepared composite aluminum foil current collector is 20mΩ, the battery capacity retention rate is 90% after 1000 cycles at a 1C charge-discharge rate, the adhesive force of the conductive layer is 95%, and the needling test has no short circuit.
Example 6
The preparation method of the composite aluminum foil current collector comprises the following specific steps:
(1) Preparing raw materials;
Water;
Single-wall carbon nanotubes: the manufacturer is Beijing Deke island gold technology Co., ltd, the model is CNT400, the pipe diameter is 1-2nm, the length is 0.55-2 μm, and the conductivity is >150S/cm;
Multifunctional wetting agent: the manufacturer is Pick auxiliary agent (Shanghai) limited company, and the model is BYK-333;
Aqueous polyurethane: the manufacturer is Anhui An Dahua Tai New Material Co., ltd, and the model is AH-1604F;
Aqueous blocked curing agent: the manufacturer is Anhui An Dahua Tai New Material Co., ltd, the model is A05, and the weight content of isocyanate groups is 6.5%;
Flake aluminum silver powder: the manufacturer is Hunan Jin new material science and technology Co., ltd, the model is CYH-15, the D50 grain diameter is 9-11 mu m, and the thickness is 20-30nm;
Nano tin powder: manufacturer is Shanghai super-Wei nano technology Co., ltd, model is CW-Sn-001, average grain diameter is 50nm, melting point is 231.9 ℃;
Auxiliary agent: a mixture of 1:1 parts by weight of an acetylenic diol wetting agent (manufacturer is Yingzhu specialty Chemie (Shanghai) Co., model number Surfynol 440) and a polyurethane thickener (manufacturer is Suzhou cloud chemical Co., ltd., model number YZ-516);
A base material: the PI film with the surface subjected to corona treatment is manufactured by DuPont Dongli, the model is Kapton 20EN, and the thickness is 5 mu m;
Protective gas: nitrogen or inert gas;
(2) Preparing adhesive layer coating liquid;
The adhesive layer coating liquid comprises the following components in parts by weight: 40 parts of water, 2 parts of single-walled carbon nanotubes, 0.5 part of multifunctional wetting agent, 40 parts of aqueous polyurethane and 2 parts of aqueous closed curing agent;
(3) Preparing a conductive layer coating liquid;
The conductive layer coating liquid comprises the following components in parts by weight: 4.6 parts of flaky aluminum silver powder, 0.2 part of nano tin powder, 79 parts of water and 1 part of auxiliary agent;
(4) Coating adhesive layer coating liquid on the two side surfaces of the substrate, and drying at 105 ℃ to form an adhesive layer; wherein, the wet weight of the adhesive layer coating liquid coating on the surface of one side of the substrate is 5g/m 2;
(5) Under the protection of protective gas, coating the conductive layer coating liquid on the surfaces of both sides of the substrate by adopting a scraper, and drying at the temperature of 239 ℃ to obtain a composite aluminum foil current collector; wherein, the wet weight of the conductive layer coating liquid coating on the surface of one side of the substrate is 21g/m 2.
The sheet resistance of the finally prepared composite aluminum foil current collector is 16mΩ, the battery capacity retention rate after 1000 cycles at 1C charge-discharge multiplying power is 86%, the adhesive force of the conductive layer is 99%, and the needling test has no short circuit.
Example 7
The preparation method of the composite aluminum foil current collector comprises the following specific steps:
(1) Preparing raw materials;
Water;
Single-wall carbon nanotubes: the manufacturer is Beijing Deke island gold technology Co., ltd, the model is CNT400, the pipe diameter is 1-2nm, the length is 0.55-2 μm, and the conductivity is >150S/cm;
Multifunctional wetting agent: the manufacturer is Pick auxiliary agent (Shanghai) limited company, and the model is BYK-333;
Aqueous polyurethane: the manufacturer is Anhui An Dahua Tai New Material Co., ltd, and the model is AH-1604F;
Aqueous blocked curing agent: the manufacturer is Anhui An Dahua Tai New Material Co., ltd, the model is A05, and the weight content of isocyanate groups is 7%;
Flake aluminum silver powder: the manufacturer is Hunan Jin new material science and technology Co., ltd, the model is CYH-15, the D50 grain diameter is 9-11 mu m, and the thickness is 20-30nm;
Nano tin powder: manufacturer is Shanghai super-Wei nano technology Co., ltd, model is CW-Sn-001, average grain diameter is 50nm, melting point is 231.9 ℃;
Auxiliary agent: a mixture of 1:1 parts by weight of an acetylenic diol wetting agent (manufacturer is Yingzhu specialty Chemie (Shanghai) Co., model number Surfynol 440) and a polyurethane thickener (manufacturer is Suzhou cloud chemical Co., ltd., model number YZ-516);
A base material: the PI film with the surface subjected to corona treatment is manufactured by DuPont Dongli, the model is Kapton 20EN, and the thickness is 5 mu m;
Protective gas: nitrogen or inert gas;
(2) Preparing adhesive layer coating liquid;
The adhesive layer coating liquid comprises the following components in parts by weight: 40 parts of water, 2 parts of single-walled carbon nanotubes, 0.5 part of multifunctional wetting agent, 40 parts of aqueous polyurethane and 2 parts of aqueous closed curing agent;
(3) Preparing a conductive layer coating liquid;
The conductive layer coating liquid comprises the following components in parts by weight: 4.7 parts of flaky aluminum silver powder, 0.4 part of nano tin powder, 79 parts of water and 1 part of auxiliary agent;
(4) Coating adhesive layer coating liquid on the surfaces of both sides of a substrate, and drying at 108 ℃ to form an adhesive layer; wherein, the wet weight of the adhesive layer coating liquid coating on the surface of one side of the substrate is 4g/m 2;
(5) Under the protection of protective gas, coating the conductive layer coating liquid on the surfaces of both sides of the substrate by adopting a scraper, and drying at the temperature of 239 ℃ to obtain a composite aluminum foil current collector; wherein the wet weight of the conductive layer coating liquid coating on the surface of one side of the substrate is 22g/m 2.
The sheet resistance of the finally prepared composite aluminum foil current collector is 15mΩ, the battery capacity retention rate is 88.5% after 1000 cycles at 1C charge-discharge multiplying power, the adhesive force of the conductive layer is 98%, and the needling test has no short circuit.
Example 8
The preparation method of the composite aluminum foil current collector comprises the following specific steps:
(1) Preparing raw materials;
Water;
Single-wall carbon nanotubes: the manufacturer is Beijing Deke island gold technology Co., ltd, the model is CNT400, the pipe diameter is 1-2nm, the length is 0.55-2 μm, and the conductivity is >150S/cm;
Multifunctional wetting agent: the manufacturer is Pick auxiliary agent (Shanghai) limited company, and the model is BYK-333;
Aqueous polyurethane: the manufacturer is Anhui An Dahua Tai New Material Co., ltd, and the model is AH-1604F;
Aqueous blocked curing agent: the manufacturer is Anhui An Dahua Tai New Material Co., ltd, the model is A05, and the weight content of isocyanate groups is 6.5%;
Flake aluminum silver powder: the manufacturer is Hunan Jin new material science and technology Co., ltd, the model is CYH-15, the D50 grain diameter is 9-11 mu m, and the thickness is 20-30nm;
Nano tin powder: manufacturer is Shanghai super-Wei nano technology Co., ltd, model is CW-Sn-001, average grain diameter is 50nm, melting point is 231.9 ℃;
Auxiliary agent: a mixture of 1:1 parts by weight of an acetylenic diol wetting agent (manufacturer is Yingzhu specialty Chemie (Shanghai) Co., model number Surfynol 440) and a polyurethane thickener (manufacturer is Suzhou cloud chemical Co., ltd., model number YZ-516);
A base material: the PI film with the surface subjected to corona treatment is manufactured by DuPont Dongli, the model is Kapton 20EN, and the thickness is 5 mu m;
Protective gas: nitrogen or inert gas;
(2) Preparing adhesive layer coating liquid;
The adhesive layer coating liquid comprises the following components in parts by weight: 40 parts of water, 2 parts of single-walled carbon nanotubes, 0.5 part of multifunctional wetting agent, 40 parts of aqueous polyurethane and 2 parts of aqueous closed curing agent;
(3) Preparing a conductive layer coating liquid;
The conductive layer coating liquid comprises the following components in parts by weight: 4.6 parts of flaky aluminum silver powder, 0.2 part of nano tin powder, 79 parts of water and 1 part of auxiliary agent;
(4) Coating adhesive layer coating liquid on the two side surfaces of the substrate, and drying at 105 ℃ to form an adhesive layer; wherein the wet weight of the adhesive layer coating liquid coating on the surface of one side of the substrate is 3g/m 2;
(5) Under the protection of protective gas, coating the conductive layer coating liquid on the surfaces of both sides of the substrate by adopting a scraper, and drying at 244 ℃ to obtain a composite aluminum foil current collector; wherein, the wet weight of the conductive layer coating liquid coating on the surface of one side of the substrate is 21g/m 2.
The sheet resistance of the finally prepared composite aluminum foil current collector is 16mΩ, the battery capacity retention rate after 1000 cycles at 1C charge-discharge multiplying power is 86%, the adhesive force of the conductive layer is 99%, and the needling test has no short circuit.
Example 9
The preparation method of the composite aluminum foil current collector comprises the following specific steps:
(1) Preparing raw materials;
Water;
Single-wall carbon nanotubes: the manufacturer is Beijing Deke island gold technology Co., ltd, the model is CNT400, the pipe diameter is 1-2nm, the length is 0.55-2 μm, and the conductivity is >150S/cm;
Multifunctional wetting agent: the manufacturer is Pick auxiliary agent (Shanghai) limited company, and the model is BYK-333;
Aqueous polyurethane: the manufacturer is Anhui An Dahua Tai New Material Co., ltd, and the model is AH-1604F;
aqueous blocked curing agent: the manufacturer is Anhui An Dahua Tai New Material Co., ltd, the model is A05, and the weight content of isocyanate groups is 6%;
Flake aluminum silver powder: the manufacturer is Hunan Jin new material science and technology Co., ltd, the model is CYH-15, the D50 grain diameter is 9-11 mu m, and the thickness is 20-30nm;
Nano tin powder: manufacturer is Shanghai super-Wei nano technology Co., ltd, model is CW-Sn-001, average grain diameter is 50nm, melting point is 231.9 ℃;
Auxiliary agent: a mixture of 1:1 parts by weight of an acetylenic diol wetting agent (manufacturer is Yingzhu specialty Chemie (Shanghai) Co., model number Surfynol 440) and a polyurethane thickener (manufacturer is Suzhou cloud chemical Co., ltd., model number YZ-516);
A base material: the PI film with the surface subjected to corona treatment is manufactured by DuPont Dongli, the model is Kapton 20EN, and the thickness is 5 mu m;
Protective gas: nitrogen or inert gas;
(2) Preparing adhesive layer coating liquid;
The adhesive layer coating liquid comprises the following components in parts by weight: 40 parts of water, 2 parts of single-walled carbon nanotubes, 0.5 part of multifunctional wetting agent, 40 parts of aqueous polyurethane and 2 parts of aqueous closed curing agent;
(3) Preparing a conductive layer coating liquid;
The conductive layer coating liquid comprises the following components in parts by weight: 4.8 parts of flaky aluminum silver powder, 0.3 part of nano tin powder, 79 parts of water and 1 part of auxiliary agent;
(4) Coating adhesive layer coating liquid on the surfaces of both sides of a substrate, and drying at 108 ℃ to form an adhesive layer; wherein the wet weight of the adhesive layer coating liquid coating on the surface of one side of the substrate is 3g/m 2;
(5) Under the protection of protective gas, coating the conductive layer coating liquid on the surfaces of both sides of the substrate by adopting a scraper, and drying at 244 ℃ to obtain a composite aluminum foil current collector; wherein the wet weight of the conductive layer coating liquid coating on the surface of one side of the substrate is 23g/m 2.
The sheet resistance of the finally prepared composite aluminum foil current collector is 12mΩ, the battery capacity retention rate after 1000 cycles at 1C charge-discharge multiplying power is 91%, the adhesive force of the conductive layer is 97%, and the needling test has no short circuit.

Claims (10)

1. The preparation method of the composite aluminum foil current collector is characterized in that conductive layer coating liquid which is uniformly dispersed with flaky aluminum silver powder and nanometer tin powder is coated on at least one side surface of a base material by adopting a scraper, and then the composite aluminum foil current collector is obtained by drying;
The conductive layer coating liquid comprises the following components in parts by weight: 4.6-4.8 parts of flaky aluminum silver powder, 0.2-0.4 part of nano tin powder, 79 parts of water and 1 part of auxiliary agent;
The D50 particle size of the flaky aluminum silver powder is 9-11 mu m, and the thickness of the flaky aluminum silver powder is 20-30nm; the average grain diameter of the nano tin powder is 50nm;
the temperature of the drying is T 1,T1 which is higher than the melting point of the nano tin powder and is lower than the melting point of the flaky aluminum silver powder and the use temperature of the base material.
2. The preparation method of the composite aluminum foil current collector of claim 1, wherein the auxiliary agent is a mixture of an alkyne diol wetting agent and a polyurethane thickener, and the weight ratio of the alkyne diol wetting agent to the polyurethane thickener is 1:1.
3. The method for preparing a composite aluminum foil current collector according to claim 1, wherein the wet weight of the conductive layer coating liquid coating on the surface of one side of the substrate is 20-25g/m 2.
4. The method for preparing a composite aluminum foil current collector according to claim 1, wherein T 1 is 235-245 ℃; the drying time is more than or equal to 20s; the drying is carried out under the protection of nitrogen or inert gas.
5. The method for preparing a composite aluminum foil current collector according to claim 4, wherein the adhesive layer is formed on the surface of the substrate to be coated with the conductive layer coating solution before the conductive layer coating solution is coated on the substrate.
6. The method for preparing a composite aluminum foil current collector according to claim 5, wherein the adhesive layer is formed by: and (3) coating the adhesive layer coating liquid on the surface of the substrate to be coated with the conductive layer coating liquid, and drying to obtain the adhesive layer, wherein the drying temperature is T 2,T2<T1.
7. The preparation method of the composite aluminum foil current collector as claimed in claim 6, wherein the adhesive layer coating liquid comprises the following components in parts by weight: 40 parts of water, 2 parts of single-walled carbon nanotubes, 0.5 part of multifunctional wetting agent, 40 parts of aqueous polyurethane and 2 parts of aqueous closed curing agent.
8. The method for preparing a composite aluminum foil current collector according to claim 7, wherein the single-walled carbon nanotubes have a tube diameter of 1-2nm, a length of 0.55-2 μm and an electrical conductivity of >150S/cm.
9. The method for preparing a composite aluminum foil current collector according to claim 7, wherein the aqueous closed-type curing agent has a characteristic of not releasing isocyanate groups at T 2 and releasing isocyanate groups at T 1; the surface of the substrate contains hydroxyl groups and/or ester groups.
10. The composite aluminum foil current collector manufactured by the manufacturing method of the composite aluminum foil current collector according to any one of claims 1 to 9, wherein the sheet resistance of the composite aluminum foil current collector is below 20mΩ, the battery capacity retention rate after 1000 cycles at a charge-discharge rate of 1C is above 85%, the adhesion force of the conductive layer is 95 to 100%, and no short circuit occurs in a needling test.
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