CN106654285B - Flexible current collector for lithium battery and preparation method thereof - Google Patents
Flexible current collector for lithium battery and preparation method thereof Download PDFInfo
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/64—Carriers or collectors
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a flexible current collector for a lithium battery and a preparation method thereof, wherein the flexible current collector comprises a flexible substrate layer, a metal conductive coating and a conductive oxidation resistant layer which are tightly combined in sequence; the flexible substrate layer is one of polyvinyl chloride, polyethylene, polypropylene, polystyrene, polyethylene terephthalate, polydimethylsiloxane and polyimide, and the thickness of the flexible substrate layer is 1-20 micrometers; the metal conductive coating is one of Cu, Al, Ni, Au and Ag, and the thickness of the metal conductive coating is 0.1-5 mu m; the conductive oxidation resistant layer comprises at least one of conductive graphite, graphene, carbon nanotubes and carbon nanofibers, and the thickness of the conductive oxidation resistant layer is more than 0 and less than 1 μm. The flexible current collector has the advantages of strong mechanical processability, strong thermal stability and oxidation resistance energy and small overall mass density.
Description
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to a flexible current collector for a lithium battery and a preparation method thereof.
Background
Because of high energy density, good reliability and excellent environmental protection performance, lithium batteries have become one of the most important energy storage devices in the market, and are widely applied to portable electronic products such as digital cameras, mobile phones and notebook computers.
With the recent rise and rapid development of electric vehicles, the energy density and stability of lithium ion batteries are further improved and improved. The lithium ion battery manufactured at present comprises a main structure of a positive plate, a diaphragm and a negative plate which are stacked or wound mutually, wherein the diaphragm separates the positive plate from the negative plate in an insulating way, and electrolyte permeating into the diaphragm ensures the conduction of lithium ions between the positive plate and the negative plate. The positive plate comprises a positive current collector and a positive material layer on the surface of the positive current collector; the negative plate comprises a negative current collector and a negative material layer on the surface of the negative current collector. The current collector has the function of collecting small currents of all parts of the positive electrode active material layer or the negative electrode active material layer on the surface of the current collector to form a large current to be output outwards.
At present, the current collector adopted by the lithium battery is mainly made of metal foil. The positive current collector adopts aluminum foil with the thickness of about 14 mu m, and the negative current collector adopts copper foil with the thickness of about 8 mu m. The metal foil has good conductivity, but has poor mechanical properties at the thickness, and is characterized by overall brittleness and insufficient toughness, irreversible traces and even holes can be generated once the metal foil is impacted by external force or deformed by the external force, so that the performance efficiency of the whole battery is influenced, and even serious safety problems can occur.
In addition, the traditional copper foil and aluminum foil account for 8 percent of the whole battery mass, and the conductivity of the traditional copper foil and aluminum foil exceeds the power supply requirement of a single-layer pole piece, so that the leading overseas peers seek a thinner production mode of a metal foil to reduce the quality of the metal foil and finally reduce the quality of the whole battery, thereby effectively improving the energy density.
The Chinese patent document with the publication number of CN101071860 discloses a flexible current collector, which consists of a supporting layer/a conductive layer, wherein the supporting layer is a windable organic thin film material, and the thickness of the supporting layer is 10-100 mu m; the conducting layer is 1-500 layers of conducting film materials, and the thickness is 10 nm-10 mu m; the conducting layer material of the flexible current collector is nickel, platinum, gold, ruthenium, cobalt or manganese metal film material; RuO2、NiO、TiO2、SnO2、ZrO2、V2O5Or MnO2A transition metal oxide thin film material; polyaniline, polypyrrole or polythiophene conductive polymer film material. The flexible current collector has poor electrical conductivity.
Disclosure of Invention
The invention provides a flexible current collector for a lithium battery, which is light and thin, can effectively improve the energy density of the lithium battery, has enough mechanical toughness and strong machinability, and also provides a preparation method of the flexible current collector.
The invention provides a flexible current collector for a lithium battery, which comprises a flexible substrate layer, a metal conductive coating and a conductive oxidation resistant layer which are sequentially and tightly combined;
the flexible substrate layer is one of polyvinyl chloride, polyethylene, polypropylene, polystyrene, polyethylene terephthalate, polydimethylsiloxane and polyimide, and the thickness of the flexible substrate layer is 1-20 micrometers;
the metal conductive coating is one of Cu, Al, Ni, Au and Ag, and the thickness of the metal conductive coating is 0.1-5 mu m;
the conductive oxidation resistant layer comprises at least one of conductive graphite, graphene, carbon nanotubes and carbon nanofibers, and the thickness of the conductive oxidation resistant layer is more than 0 and less than 1 μm.
The flexible current collector can be single-sided or double-sided, the single-sided flexible current collector is formed by sequentially plating a metal conductive plating layer and a conductive oxidation resistant layer on one surface of a flexible substrate layer, and the double-sided flexible current collector is formed by sequentially plating a metal conductive plating layer and a conductive oxidation resistant layer on two surfaces of the flexible substrate layer.
Preferably, the thickness of the flexible substrate layer is 1-5 μm.
The flexible substrate layer with the thickness can ensure the mechanical strength of the flexible current collector, and meanwhile, the weight of the flexible current collector is further reduced.
Preferably, the thickness of the metal conductive coating is 0.2-5 μm.
When the thickness of the metal conductive coating is 0.2-5 mu m, the current collecting effect is good, and the weight of the flexible current collector can be effectively reduced.
Preferably, the flexible substrate layer is polyethylene terephthalate; the metal conductive coating is Cu or Al.
The binding force between the polyethylene glycol terephthalate and Cu or Al is large, when the polyethylene glycol terephthalate is used as the flexible substrate layer and the Cu or Al is used as the metal conductive coating, the mechanical property of the flexible current collector is good.
The flexible current collector comprises a negative current collector and a positive current collector, preferably, the flexible substrate layer of the negative current collector is polyethylene terephthalate, and the metal conductive coating is Cu; the flexible substrate layer of the positive current collector is polyethylene glycol terephthalate, and the metal conductive coating is Al.
The outermost layer of the flexible current collector is the conductive oxidation-resistant layer, the conductive oxidation-resistant layer can prevent the metal conductive coating from being oxidized at high temperature, the service life of the flexible current collector is prolonged, meanwhile, the conductive oxidation-resistant layer can reduce the contact resistance of the flexible current collector, and the rapid charging and discharging performance of the lithium battery is improved.
Preferably, the conductive antioxidation layer comprises graphene or carbon nanotubes, and the thickness of the conductive antioxidation layer is 80-100 nm.
When the conductive oxidation resistant layer is graphene or a carbon nano tube, the oxidation resistance of the conductive oxidation resistant layer is better, and the thickness of the conductive oxidation resistant layer can be thinner on the premise of not influencing the oxidation resistance of the conductive oxidation resistant layer, so that the weight of the flexible current collector is further reduced.
Preferably, the bonding force between the metal conductive plating layer and the flexible substrate layer is 15-30N/cm.
The binding force between the metal conductive coating and the flexible substrate layer is larger, so that the whole structure of the flexible current collector is stable, the metal conductive coating is not easy to fall off, and otherwise, the reject ratio of products is increased in the production process of the flexible current collector.
Preferably, the tensile strength of the flexible current collector is 100-200 MPa, and the elongation is more than 5%.
The tensile strength and the elongation of the flexible current collector are important indexes of the mechanical strength of the flexible current collector, the tensile strength of the flexible current collector is 100-200 MPa, and the use requirement of the flexible current collector is met when the elongation is more than 5%.
Preferably, the flexible current collector for the lithium battery comprises a flexible substrate layer, a metal conductive coating and a conductive oxidation resistant layer which are tightly combined in sequence;
the flexible substrate layer is made of polyethylene glycol terephthalate, and the thickness of the flexible substrate layer is 1-5 microns;
the metal conductive coating is Cu or Al, and the thickness of the metal conductive coating is 0.2-5 mu m;
the conductive antioxidation layer is graphene or a carbon nano tube, and the thickness of the conductive antioxidation layer is 80-100 nm.
The flexible current collector in the technical scheme has small mass density and unit area mass of 1-10 g/m2To (c) to (d); the mechanical property is good, the tensile strength is between 100 and 200MPa, and the elongation is more than 5 percent; the product has good thermal stability and high-temperature oxidation resistance, the thermal shrinkage rate is less than 3% at 120 ℃, and the surface of the product is free from oxidation discoloration after being baked for 2 hours at 180 ℃; has excellent conductivity, square resistance of 1m omega-50 omega, conductivity of 1 x 103～6×105The lithium battery has the advantages that the lithium battery is S/cm, meanwhile, the contact resistance is small, and the rapid charge and discharge performance of the lithium battery is greatly improved.
The invention also provides a preparation method of the flexible current collector, which comprises the following steps:
(1) removing oil stains on the surface of the flexible substrate material by using acetone and/or alcohol, and cleaning and activating the surface of the flexible substrate material by using ultraviolet light;
(2) at 1X 10-4Pa adopts a vacuum coating mode to plate a metal conductive coating on the surface of the cleaned and activated flexible substrate material;
(3) and coating a conductive oxidation resistant layer on the metal conductive coating, and drying to obtain the flexible current collector.
Preferably, in the step (1), acetone is firstly used for spraying and cleaning for 1-15 min, and then alcohol is used for cleaning for 3-15 min in an ultrasonic water bath.
Under the specific cleaning sequence, the oil stain on the surface of the flexible substrate material can be effectively removed.
Preferably, in the step (1), the power of the ultraviolet light is 500W to 20000W, and the cleaning activation time is 3min to 1 h.
The ultraviolet cleaning can increase the smooth finish of the surface of the flexible substrate material, is beneficial to the subsequent evaporation process, and enhances the binding force between the metal conductive coating and the flexible substrate.
The preparation method of the invention uses a high vacuum evaporation environment, can reduce the loss of metal particles in the evaporation process and ensure the uniformity of the metal conductive coating.
The preparation method of the invention can adopt a roll-to-roll production mode, which not only can ensure the uniformity of the metal conductive coating, but also can improve the overall production efficiency and reduce the overall production cost.
Compared with the prior art, the invention has the beneficial effects that:
(1) the flexible current collector adopts a three-layer structure, and the mechanical processability of the flexible current collector is enhanced by utilizing the flexible substrate layer; the metal conductive coating can greatly reduce the overall mass density of the flexible current collector without influencing the practical conductivity of the flexible current collector, and the mass density of the metal conductive coating is only 1/10-1/5 of the traditional copper foil and aluminum foil, so that the quality of a lithium battery can be greatly reduced, and the energy density of the lithium battery can be improved; the conductive oxidation resistant layer can improve the thermal stability and the oxidation resistant energy of the flexible current collector, reduce the contact resistance of the flexible current collector and improve the rapid charging and discharging performance of the lithium battery;
(2) in the preparation method of the flexible current collector, acetone spraying and alcohol ultrasonic cleaning are sequentially adopted, and then ultraviolet cleaning and activation are carried out, so that the binding force between the flexible substrate layer and the metal conductive coating can be greatly enhanced; the high vacuum evaporation environment is used, so that the loss of metal particles in the evaporation process can be reduced, and the uniformity of the metal conductive coating is ensured.
Drawings
Fig. 1 is a schematic structural view of a single-sided flexible current collector of the present invention;
fig. 2 is a schematic structural view of a double-sided flexible current collector of the present invention.
Detailed Description
The flexible current collector of the invention can be single-sided or double-sided, as shown in fig. 1 and 2, the single-sided flexible current collector sequentially comprises a flexible substrate layer 1, a metal conductive coating layer 2 and a conductive oxidation resistant layer 3 which are tightly combined, and the double-sided flexible current collector sequentially comprises a conductive oxidation resistant layer 3, a metal conductive coating layer 2, a flexible substrate layer 1, a metal conductive coating layer 2 and a conductive oxidation resistant layer 3 which are tightly combined.
Example 1
(1) Selecting a polyethylene terephthalate (PET) film with the thickness of 3.8 mu m, firstly spraying and cleaning the PET film for 3min by using acetone, then cleaning the PET film for 10min in an ultrasonic water bath by using alcohol, and cleaning and activating the surface of the PET film by using ultraviolet light after cleaning;
(2) putting the cleaned and activated PET film and the industrial-grade pure copper base material into roll-to-roll vacuum evaporation equipment, debugging a program, and preparing for evaporation; setting the vacuum environment and technological parameters for evaporation, and vacuumizing to 1 × 10 in a vacuum device-4When the pressure is lower than Pa, starting vacuum coating, setting the voltage to be 380V, the current to be 50A and the coating speed to be 60 cm/min; executing the program, and performing evaporation, wherein the single-layer thickness of the copper plating layer reaches 1 mu m;
(3) placing the copper-plated film on a film coating machine, setting the film coating speed to be 2m/min and the feeding speed to be 5g/min, and coating Carbon Nano Tube (CNT)/N-methylpyrrolidone (NMP) slurry with the mass concentration of 5% on a copper coating;
(4) and after the film coating is finished, drying at 100 ℃, then trimming to obtain a semi-finished product, and then performing shearing and packaging to obtain the flexible current collector.
Example 2
(1) Selecting a PET film with the thickness of 3.8 mu m, firstly spraying and cleaning the PET film for 3min by using acetone, then cleaning the PET film for 10min in an ultrasonic water bath by using alcohol, and cleaning and activating the surface of the PET film by using ultraviolet light after cleaning;
(2) putting the cleaned and activated PET film and the industrial pure aluminum substrate into roll-to-roll vacuum evaporation equipment, debugging a program, and preparing for evaporation; setting the vacuum environment and technological parameters for evaporation, and vacuumizing to 1 × 10 in a vacuum device-4When the pressure is lower than Pa, starting vacuum coating, setting the voltage to be 380V, the current to be 50A and the coating speed to be 100 cm/min; executing the program, and performing evaporation, wherein the single-layer thickness of the copper plating layer reaches 1.8 mu m;
(3) placing the copper-plated film on a film coating machine, setting the film coating speed to be 2m/min and the feeding speed to be 5g/min, and coating Carbon Nano Tube (CNT)/N-methylpyrrolidone (NMP) slurry with the mass concentration of 5% on a copper coating;
(4) and after the film coating is finished, drying at 100 ℃, then trimming to obtain a semi-finished product, and then performing shearing and packaging to obtain the flexible current collector.
Comparing the mechanical properties of the flexible current collectors prepared in examples 1 and 2 with those of conventional copper foils and aluminum foils, as shown in table 1, it can be seen that the flexible current collectors prepared in examples 1 and 2 have low mass density and high mechanical properties.
Table 1 comparison of mechanical properties of flexible current collectors prepared in examples 1 and 2 with conventional copper foil and aluminum foil
Comparative example 1
(1) Selecting a polyethylene terephthalate (PET) film with the thickness of 3.8 mu m, firstly spraying and cleaning the PET film for 3min by using acetone, then cleaning the PET film for 10min in an ultrasonic water bath by using alcohol, and cleaning and activating the surface of the PET film by using ultraviolet light after cleaning;
(2) putting the cleaned and activated PET film and the industrial-grade pure copper base material into roll-to-roll vacuum evaporation equipment, debugging a program, and preparing for evaporation; setting the vacuum environment and technological parameters for evaporation, and vacuumizing to 1 × 10 in a vacuum device-4When the pressure is lower than Pa, starting vacuum coating, setting the voltage to be 380V, the current to be 50A and the coating speed to be 60 cm/min; executing the program, and performing evaporation, wherein the single-layer thickness of the copper plating layer reaches 1 mu m;
(3) and then trimming to obtain a semi-finished product, and then performing slitting and packaging to obtain the flexible current collector without the conductive oxidation resistant layer.
Comparing the performance of the flexible current collector prepared in example 1 with that of the flexible current collector prepared in comparative example 1 without the conductive oxidation resistant layer, as shown in table 2, it can be seen that the conductive oxidation resistant layer can enhance the thermal stability and oxidation resistance of the flexible current collector, and at the same time, can reduce the contact resistance of the flexible current collector.
Table 2 comparison of the properties of the flexible current collector prepared in example 1 with those of the flexible current collector prepared in comparative example 1
Example 3
(1) Selecting a polypropylene (PP) film with the thickness of 1 mu m, firstly spraying and cleaning the PP film for 3min by using acetone, then cleaning the PP film for 10min in ultrasonic water bath by using alcohol, and cleaning and activating the surface of the PP film by using ultraviolet light after cleaning;
(2) placing the cleaned and activated PP film and the industrial-grade pure copper base material into roll-to-roll vacuum evaporation equipment, debugging a program, and preparing for evaporation; setting the vacuum environment and technological parameters for evaporation, and vacuumizing to 1 × 10 in a vacuum device-4When the pressure is lower than Pa, starting vacuum coating, setting the voltage to be 380V, the current to be 50A and the coating speed to be 120 cm/min; executing the program, and performing evaporation, wherein the single-layer thickness of the copper plating layer reaches 0.1 mu m;
(3) placing the copper-plated film on a film coating machine, setting the film coating speed to be 2m/min and the feeding speed to be 5g/min, and coating graphene/N-methylpyrrolidone (NMP) slurry with the mass concentration of 5% on a copper coating;
(4) and after the film coating is finished, drying at 100 ℃, then trimming to obtain a semi-finished product, and then performing shearing and packaging to obtain the flexible current collector.
Example 4
(1) Selecting a Polyimide (PI) film with the thickness of 5 mu m, firstly spraying and cleaning the PI film for 3min by using acetone, then cleaning the PI film for 10min in an ultrasonic water bath by using alcohol, and then cleaning and activating the surface of the PI film by using ultraviolet light after cleaning;
(2) putting the cleaned and activated PI film and an industrial-grade pure copper substrate into roll-to-roll vacuum evaporation equipment, debugging a program, and preparing for evaporation; setting the vacuum environment and technological parameters for evaporation, and vacuumizing to 1 × 10 in a vacuum device-4When the pressure is lower than Pa, starting vacuum coating, setting the voltage to be 380V, the current to be 50A and the coating speed to be 40 cm/min; executing the program, and performing evaporation, wherein the single-layer thickness of the copper plating layer reaches 5 mu m;
(3) placing the copper-plated film on a film coating machine, setting the film coating speed to be 2m/min and the feeding speed to be 5g/min, and coating Carbon Nano Tube (CNT)/N-methylpyrrolidone (NMP) slurry with the mass concentration of 5% on a copper coating;
(4) and after the film coating is finished, drying at 100 ℃, then trimming to obtain a semi-finished product, and then performing shearing and packaging to obtain the flexible current collector.
The above-mentioned embodiments are intended to illustrate the technical solutions and advantages of the present invention, and it should be understood that the above-mentioned embodiments are only specific embodiments of the present invention, and are not intended to limit the present invention, and any modifications, additions, equivalents, etc. made within the scope of the principles of the present invention should be included in the scope of the present invention.
Claims (4)
1. A flexible current collector for a lithium battery is characterized by comprising a flexible substrate layer, a metal conductive coating and a conductive oxidation resistant layer which are tightly combined in sequence;
the flexible substrate layer is made of polyethylene glycol terephthalate, and the thickness of the flexible substrate layer is 1-5 microns;
the metal conductive coating is Cu or Al, and the thickness of the metal conductive coating is 0.2-5 mu m;
the conductive antioxidation layer comprises graphene or carbon nano tubes, and the thickness of the conductive antioxidation layer is 80-100 nm;
the bonding force between the metal conductive coating and the flexible substrate layer is 15-30N/cm;
the tensile strength of the flexible current collector is 100-200 MPa, and the elongation is more than 5%;
the mass per unit area of the flexible current collector is 1-10 g/m2(ii) a The heat shrinkage rate of the flexible current collector at 120 DEG C<3 percent, the surface of the product is not oxidized and discolored after being baked for 2 hours at 180 ℃; the sheet resistance is 1m omega-50 omega, and the conductivity is 1 multiplied by 103 ~ 6×105 S/cm。
2. A method for preparing a flexible current collector as claimed in claim 1, comprising the steps of:
(1) removing oil stains on the surface of the flexible substrate material by using acetone and/or alcohol, and cleaning and activating the surface of the flexible substrate material by using ultraviolet light;
(2) at 1X 10-4Pa adopts a vacuum coating mode to plate a metal conductive coating on the surface of the cleaned and activated flexible substrate material;
(3) and coating a conductive oxidation resistant layer on the metal conductive coating, and drying to obtain the flexible current collector.
3. The preparation method of the flexible current collector as claimed in claim 2, wherein in the step (1), the cleaning is performed by spraying acetone for 1-15 min, and then the cleaning is performed by using alcohol in an ultrasonic water bath for 3-15 min.
4. The method for preparing the flexible current collector as claimed in claim 2, wherein in the step (1), the power of the ultraviolet light is 500W-20000W, and the cleaning and activating time is 3 min-1 h.
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| CN112234210A (en) | 2020-09-30 | 2021-01-15 | 江苏卓高新材料科技有限公司 | Composite current collector, preparation method thereof and battery |
| CN112599785B (en) * | 2021-03-03 | 2021-05-18 | 浙江艾罗网络能源技术股份有限公司 | Self-temperature-control current collector of lithium ion battery and preparation method and application thereof |
| CN113381026B (en) * | 2021-06-15 | 2022-07-01 | 湖南科技大学 | Polyimide-based flexible electrode and preparation and application thereof |
| CN114188543A (en) * | 2021-11-15 | 2022-03-15 | 深圳市宝明科技股份有限公司 | Composite conductive copper foil and preparation method thereof |
| CN114540802B (en) * | 2022-01-27 | 2023-12-01 | 江阴纳力新材料科技有限公司 | Method for preparing composite current collector with low energy consumption |
| CN114360773A (en) * | 2022-02-15 | 2022-04-15 | 单县多米石墨烯科技有限公司 | Anti-oxidation flexible conductive film and preparation method thereof |
| CN114792807B (en) * | 2022-04-20 | 2023-10-27 | 江阴纳力新材料科技有限公司 | Positive electrode lithium-rich composite current collector and preparation method thereof |
| CN114824179A (en) * | 2022-04-28 | 2022-07-29 | 南昌大学 | Preparation method of solid-state lithium battery |
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| US6933077B2 (en) * | 2002-12-27 | 2005-08-23 | Avestor Limited Partnership | Current collector for polymer electrochemical cells and electrochemical generators thereof |
| CN101071860A (en) * | 2007-06-08 | 2007-11-14 | 大连理工大学 | Flexible current-collecting body |
| CN103072333B (en) * | 2013-01-05 | 2015-04-01 | 郑州航空工业管理学院 | Copper material provided with anti-oxidative protection layer and manufacture method thereof |
| CN103326029A (en) * | 2013-06-07 | 2013-09-25 | 深圳市海太阳实业有限公司 | Negative electrode sheet, positive electrode sheet, and lithium ion battery |
| CN104078164B (en) * | 2014-07-10 | 2016-03-09 | 厦门大学 | A kind of preparation method of Cu nanowire network of Graphene carbon film parcel |
| CN105870429B (en) * | 2016-06-15 | 2018-06-19 | 中物院成都科学技术发展中心 | A kind of carbon-coated thermal battery electrode materials and preparation method thereof |
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