CN118486836A - Composite current collector, preparation method and battery - Google Patents
Composite current collector, preparation method and battery Download PDFInfo
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- CN118486836A CN118486836A CN202410556434.3A CN202410556434A CN118486836A CN 118486836 A CN118486836 A CN 118486836A CN 202410556434 A CN202410556434 A CN 202410556434A CN 118486836 A CN118486836 A CN 118486836A
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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
- H01M4/66—Selection of materials
- H01M4/665—Composites
- H01M4/667—Composites in the form of layers, e.g. coatings
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- 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
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Abstract
本申请提供一种复合集流体及制备方法、电池，复合集流体的制备方法包括如下步骤：提供含氟聚合物，将含氟聚合物溶于有机溶剂，得到含氟聚合物溶液；提供集流体本体，将含氟聚合物溶液涂覆于集流体本体表面；对涂覆有含氟聚合物溶液的集流体本体进行热处理，在集流体本体表面形成修饰层，得到复合集流体。由于碳膜具有较低的成核过电位，通过在集流体本体形成致密的碳膜，使得锂金属倾向于在其表面沉积，从而避免锂金属在金属集流体表面沉积时候产生尖端效应，导致锂枝晶生长的问题；此外，使用含氟聚合物作为形成修饰层的原料，能够使碳膜中含有丰富的氟元素，氟元素同样能够作为亲锂位点，进一步诱导锂金属在集流体表面均匀沉积。
The present application provides a composite current collector and a preparation method and a battery. The preparation method of the composite current collector includes the following steps: providing a fluorine-containing polymer, dissolving the fluorine-containing polymer in an organic solvent to obtain a fluorine-containing polymer solution; providing a current collector body, coating the fluorine-containing polymer solution on the surface of the current collector body; heat-treating the current collector body coated with the fluorine-containing polymer solution to form a modified layer on the surface of the current collector body to obtain a composite current collector. Since the carbon film has a low nucleation overpotential, by forming a dense carbon film on the current collector body, lithium metal tends to deposit on its surface, thereby avoiding the problem of lithium metal depositing on the metal current collector surface. The tip effect causes the growth of lithium dendrites; in addition, the use of fluorine-containing polymers as a raw material for forming the modified layer can make the carbon film contain rich fluorine elements, and the fluorine element can also serve as a lithium-philic site to further induce the uniform deposition of lithium metal on the current collector surface.
Description
Technical Field
The application belongs to the technical field of battery materials, and particularly relates to a composite current collector, a preparation method and a battery.
Background
Lithium metal batteries have been frequently seen in the field of view of people due to their advantages of higher theoretical specific capacity, high rate capability, lower operating potential, and lower density, and have made much breakthrough progress in recent years. However, the lithium metal battery has serious lithium dendrite growth and volume expansion, which can cause the lithium metal battery to generate fire, explosion and other safety problems, and the practical application of the lithium metal battery is also restricted. Copper foil is used as a most common current collector in a lithium metal battery, and due to the inherent lithium-repellent property, a tip effect is generated when lithium metal is deposited on the surface of the copper foil, so that lithium dendrites grow wantonly, and the problems of uncontrollable lithium dendrites, dead lithium and the like exist, which can limit the display of the electrochemical performance of the lithium metal on one hand and are one of main reasons for causing serious safety problems on the other hand.
Therefore, how to improve the lithium affinity of the lithium metal battery current collector and inhibit the growth of lithium dendrites is a problem to be solved at present.
Disclosure of Invention
The invention provides a composite current collector, a preparation method and a battery, which solve the problems of lithium dendrite and the like existing in the use of a lithium metal battery and improve the safety and electrochemical performance of the lithium metal battery by constructing a reasonable modification layer on the surface of the current collector.
The first embodiment of the application provides a preparation method of a composite current collector, which comprises the following steps:
providing a fluorine-containing polymer, and dissolving the fluorine-containing polymer in an organic solvent to obtain a fluorine-containing polymer solution;
providing a current collector body, and coating the fluoropolymer solution on the surface of the current collector body;
And carrying out heat treatment on the current collector body coated with the fluoropolymer solution, and forming a modification layer on the surface of the current collector body to obtain the composite current collector.
In some embodiments, the fluoropolymer comprises one or more of polytetrafluoroethylene, chlorotrifluoroethylene, polyvinylidene fluoride, ethylene-tetrafluoroethylene copolymer, and polyvinyl fluoride.
In some embodiments, the organic solvent is N-methylpyrrolidone.
In some embodiments, the current collector body comprises copper foil or aluminum foil.
In some embodiments, the concentration of the fluoropolymer in the fluoropolymer solution is 200 to 600mg/ml.
In some embodiments, the step of applying the fluoropolymer solution to the surface of the current collector body further comprises:
Controlling the coating density of the fluorine-containing polymer on the surface of the current collector to be 5-15 mg/cm 2.
In some embodiments, the temperature of the heat treatment is 200 to 800 ℃ and the time of the heat treatment is 0.2 to 4 hours.
In some embodiments, the heat treatment is performed at a rate of 5 ℃/min,
The second embodiment of the application provides a composite current collector which is prepared by the preparation method in any embodiment, and comprises a current collector body and a modification layer arranged on the surface of the current collector body.
In some embodiments, the thickness of the modifying layer is 0.5 to 100 μm.
In some embodiments, the composite current collector has a specific surface area of 0.5-2 cm -2.
The third embodiment of the application provides a lithium metal battery, which comprises a negative electrode plate, wherein the negative electrode plate comprises the composite current collector in any embodiment.
The preparation method of the composite current collector provided by the application comprises the following steps: providing a fluorine-containing polymer, and dissolving the fluorine-containing polymer in an organic solvent to obtain a fluorine-containing polymer solution; providing a current collector body, and coating a fluorine-containing polymer solution on the surface of the current collector body; and carrying out heat treatment on the current collector body coated with the fluoropolymer solution, and forming a modification layer on the surface of the current collector body to obtain the composite current collector. The preparation method provided by the application can form a compact carbon film on the current collector body, and lithium metal tends to be deposited on the surface of the carbon film due to the lower nucleation overpotential of the carbon film, so that the problem of lithium dendrite growth caused by the tip effect generated when the lithium metal is deposited on the surface of the metal current collector is avoided; in addition, the fluorine-containing polymer is used as a raw material for forming the modification layer, so that the carbon film contains abundant fluorine elements, and the fluorine elements can also be used as lithium-philic sites to further induce uniform deposition of lithium metal on the surface of the current collector.
Drawings
The technical solution and other advantageous effects of the present application will be made apparent by the following detailed description of the specific embodiments of the present application with reference to the accompanying drawings.
Fig. 1 is a schematic diagram of a preparation process of a composite current collector according to embodiment 1 of the present application;
FIG. 2 is an SEM characterization diagram of a composite current collector according to example 1 of the present application;
FIG. 3 is an SEM characterization of a current collector provided in comparative example 1 of the present application;
Fig. 4 is a graph showing the results of performance tests of the composite current collector provided in example 1 of the present application and the current collector provided in comparative example 1.
Detailed Description
The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present application. It will be apparent that the described embodiments are only some, but not all, embodiments of the application. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to fall within the scope of the application.
In the description of the present application, it should be noted that, unless explicitly specified and limited otherwise, the terms "connected," "connected," and "connected" are to be construed broadly, and may be either fixedly connected, detachably connected, or integrally connected, for example; can be mechanically connected, electrically connected or can be communicated with each other; can be directly connected or indirectly connected through an intermediate medium, and can be communicated with the inside of two elements or the interaction relationship of the two elements. The specific meaning of the above terms in the present application can be understood by those of ordinary skill in the art according to the specific circumstances. In the description of the present application, the meaning of "a plurality" is two or more, unless explicitly defined otherwise. Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more features.
The following disclosure provides many different embodiments, or examples, for implementing different structures of the application. In order to simplify the present disclosure, components and arrangements of specific examples are described below. They are, of course, merely examples and are not intended to limit the application.
The first embodiment of the application provides a preparation method of a composite current collector, which comprises the following steps:
Providing a fluorine-containing polymer, and dissolving the fluorine-containing polymer in an organic solvent to obtain a fluorine-containing polymer solution;
Providing a current collector body, and coating a fluorine-containing polymer solution on the surface of the current collector body;
And carrying out heat treatment on the current collector body coated with the fluoropolymer solution, and forming a modification layer on the surface of the current collector body to obtain the composite current collector.
The organic polymer is coated on the surface of the metal current collector body, so that a compact carbon film can be formed, and the surface of the metal current collector body is modified: because the carbon film has lower nucleation overpotential, lithium metal tends to be deposited on the surface of the carbon film, so that the problem of lithium dendrite growth caused by tip effect generated when the lithium metal is deposited on the surface of a metal current collector is avoided; in addition, the fluorine-containing polymer can keep rich fluorine elements in the carbon film after heat treatment, and the fluorine elements can also serve as lithium-philic sites, so that uniform deposition of lithium metal on the surface of a current collector is further induced, and the electrical performance of the battery is further improved. The fluorine-containing polymer is coated on the surface of the current collector body and sintered at high temperature, so that a compact carbon film can be formed, the condition is mild, and the process is concise.
In some embodiments, the fluoropolymer comprises one or more of polytetrafluoroethylene, polytrifluoroethylene, polyvinylidene fluoride (PVDF), ethylene-tetrafluoroethylene copolymer, and polyvinyl fluoride. Taking PVDF as an example, a current collector body coated with a PVDF solution is subjected to heat treatment, an organic solution, such as NMP, volatilizes at a temperature above 400 ℃, the PVDF is decomposed into HF and fluorocarbon organic compounds, and the fluorocarbon organic compounds form a compact carbon film modified layer on the surface of the current collector body.
In some embodiments, the organic solvent is N-methylpyrrolidone.
In some embodiments, the current collector body comprises copper foil or aluminum foil.
In some embodiments, the concentration of fluoropolymer in the fluoropolymer solution is 200 to 600mg/ml. It will be appreciated that the concentration of fluoropolymer may take on any of the values (in mg/ml) 200, 300, 400, 500, 600 or a range between any two. When the concentration of the fluorine-containing polymer meets the value range, the surface of the finally formed modified layer can be ensured to be uniform and compact, and meanwhile, the excessive concentration of the fluorine-containing polymer is avoided, and byproducts are formed in the reaction.
Specifically, the preparation method of the composite current collector in the embodiment can be realized through the following steps:
s1, carrying out ultrasonic treatment on fluorine-containing polymer powder and an organic solvent until the fluorine-containing polymer powder and the organic solvent are uniformly dispersed.
S2, dripping the uniformly dispersed fluorine-containing polymer dispersion liquid on the surface of the current collector body after pickling and drying, placing the current collector body in a muffle furnace, and calcining in an H 2/Ar mixed atmosphere to obtain the composite current collector.
In some embodiments, the step of applying the fluoropolymer solution to the surface of the current collector body further comprises:
The coating density of the fluorine-containing polymer on the surface of the current collector is controlled to be 5-15 mg/cm 2. It will be appreciated that the coating density of the fluoropolymer on the surface of the current collector (in mg/cm 2) may be any one or between any two of the values 5, 8, 11, 13, 15. When the coating density satisfies the above range, the final finishing layer can be ensured to have an ideal thickness and be relatively dense.
In some embodiments, the temperature of the heat treatment is 200-800 ℃ and the time of the heat treatment is 0.2-4 hours. It is understood that the temperature value (in:. Degree. C.) of the heat treatment may be any one or a range between any two of 200, 300, 400, 500, 600, 700, 800; the time of the heat treatment (unit: h) may be any one of 0.2, 0.5, 1, 2, 3, 4 or a range between any two of them. When the temperature and time of the heat treatment satisfy the above-mentioned value ranges, it is possible to ensure that the fluoropolymer is completely reacted and to prevent the fluoropolymer from being further decomposed at high temperatures.
In some embodiments, the heating rate of the heat treatment is 5 ℃/min. When the heating rate of the heat treatment meets the value, the reaction rate of the fluorine-containing polymer can be further controlled, and the generation of byproducts is avoided.
The second embodiment of the application provides a composite current collector which is prepared by the preparation method in any embodiment, and comprises a current collector body and a modification layer arranged on the surface of the current collector body, wherein the modification layer comprises carbon element and fluorine element, and the surface of the modification layer is a dense carbon film without coarse pores.
In some embodiments, the thickness of the finishing layer is 0.5 to 100 μm. It will be appreciated that the thickness of the finishing layer may take on any one or range between any two of values 0.5, 1, 5, 10, 30, 50, 100 (in μm).
In some embodiments, the specific surface area of the composite current collector is 0.5-2 cm -2. It is understood that the specific surface area of the composite current collector may have any one value or a range between any two values of 0.5, 1, 1.5 and 2 (unit: cm -2).
The third embodiment of the application provides a lithium metal battery, which comprises a negative electrode plate, wherein the negative electrode plate comprises the composite current collector in any embodiment.
The following description is made on the composite current collector, the preparation method and the battery provided by the application by combining specific embodiments:
Example 1
The embodiment provides a composite current collector, which is prepared by the following steps:
S1, preparing PVDF dispersion liquid: PVDF powder was mixed with NMP solvent (400 mg mL -1) and sonicated until it was uniformly dispersed.
S2, preparing a composite current collector: and (3) dripping the uniformly dispersed PVDF dispersion liquid on the surface of the copper foil subjected to pickling and drying, as shown in fig. 1, then placing the copper foil in a muffle furnace, and calcining at 400 ℃ for 0.5H (the heating rate is 5 ℃/min) in an H 2/Ar mixed atmosphere to prepare the composite current collector.
The composite current collector thus prepared was subjected to SEM characterization, and the results are shown in fig. 2. As can be seen from fig. 2, the composite current collector prepared by the scheme of the application has relatively uniform and compact characteristics.
Preparation of lithium metal battery:
The composite current collector and a pure lithium sheet are used as a counter electrode, a polypropylene film is used as a diaphragm, and an electrolyte composed of 1M bis (trifluoromethane) sulfonyl imide 1, 2-dimethoxyethane, 1, 3-dioxolane (1:1v/v%) and 2% LiNO 3 is assembled in a glove box to prepare the button cell.
Examples 2 to 5
The preparation methods of the composite current collectors provided in examples 2 to 5 were the same as in example 1, and only the process parameters were adjusted as shown in table 1.
TABLE 1
Comparative example 1
Comparative example 1a lithium metal battery was prepared using a pure copper foil as a negative electrode current collector by the following steps:
The current collector of copper foil and a pure lithium sheet are used as a counter electrode, a polypropylene film is used as a diaphragm, and an electrolyte composed of 1M bis (trifluoromethane) sulfonyl imide 1, 2-dimethoxyethane, 1, 3-dioxolane (1:1v/v%) and 2% LiNO 3 is assembled in a glove box to prepare the button cell.
SEM characterization was performed on the copper foil current collector, and as shown in fig. 3, it can be seen from fig. 3 that the surface of the current collector lacking the modification layer is loose and has insufficient flatness.
The batteries prepared in example 1 and comparative example 1 were subjected to an electrical property test using a current density of 0.5mA cm -2 and a capacity of 1mAh cm -2; discharging with current density of 0.5mA cm -2 to voltage less than or equal to 0.01V, and charging with the same current for 2 hours, thus the charging and discharging cycle is adopted. The results are shown in FIG. 4 and Table 2.
TABLE 2
| Cycle number | |
| Example 1 | 150 |
| Comparative example 1 | 30 |
As can be seen from fig. 4, the battery prepared in example 1 was able to stably circulate for 150 cycles at a current density of 0.5mA cm -2 and a capacity of 1mAh cm -2, and the battery prepared in comparative example 1 rapidly dropped in the first 30 cycles. Thus, the current collector modified with the carbon film can effectively improve the electrochemical performance of the lithium metal battery.
The above describes a composite current collector, a preparation method and a battery provided by the embodiment of the application in detail, and specific examples are applied in the application to explain the principle and the implementation mode of the application, and the description of the above examples is only used for helping to understand the technical scheme and the core idea of the application; those of ordinary skill in the art will appreciate that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the application.
Claims (10)
1. The preparation method of the composite current collector is characterized by comprising the following steps of:
providing a fluorine-containing polymer, and dissolving the fluorine-containing polymer in an organic solvent to obtain a fluorine-containing polymer solution;
providing a current collector body, and coating the fluoropolymer solution on the surface of the current collector body;
And carrying out heat treatment on the current collector body coated with the fluoropolymer solution, and forming a modification layer on the surface of the current collector body to obtain the composite current collector.
2. The method for preparing a composite current collector according to claim 1, wherein the fluorine-containing polymer comprises one or more of polytetrafluoroethylene, polytrifluoroethylene, polyvinylidene fluoride, ethylene-tetrafluoroethylene copolymer and polyvinyl fluoride; and/or the number of the groups of groups,
The organic solvent is N-methyl pyrrolidone.
3. The method of manufacturing a composite current collector according to claim 1, wherein the current collector body comprises copper foil or aluminum foil.
4. The method for preparing a composite current collector according to claim 1, wherein the concentration of the fluoropolymer in the fluoropolymer solution is 200-600 mg/ml.
5. The method of preparing a composite current collector according to claim 1, wherein the step of applying the fluoropolymer solution to the surface of the current collector body further comprises:
Controlling the coating density of the fluorine-containing polymer on the surface of the current collector to be 5-15 mg/cm 2.
6. The method for preparing a composite current collector according to claim 1, wherein the temperature of the heat treatment is 200-800 ℃, and the time of the heat treatment is 0.2-4 hours; and/or the number of the groups of groups,
The heating rate of the heat treatment is 2-10 ℃/min.
7. A composite current collector prepared by the preparation method according to any one of claims 1 to 6, wherein the composite current collector comprises a current collector body and a modification layer arranged on the surface of the current collector body.
8. A composite current collector according to claim 7, wherein the thickness of the modification layer is 0.5 to 100 μm.
9. A composite current collector according to claim 7, having a specific surface area of 0.5-2 cm -2.
10. A lithium metal battery comprising a negative electrode tab, characterized in that the negative electrode tab comprises a composite current collector produced by the production method according to any one of claims 1 to 6 or comprises a composite current collector according to any one of claims 7 to 9.
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| CN114975847A (en) * | 2022-07-07 | 2022-08-30 | 中南大学 | A composite metal negative electrode with sandwich structure and its preparation method and application |
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