CN113013375A - Coating process of thick film lithium battery and thick film lithium battery - Google Patents
Coating process of thick film lithium battery and thick film lithium battery Download PDFInfo
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/04—Processes of manufacture in general
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- H—ELECTRICITY
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- 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
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
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Abstract
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a coating process of a thick film lithium battery and a lithium battery prepared by the coating process, wherein the lithium ion coating process comprises the following steps: firstly coating the pre-coating electrode on a current collector, then covering the surface of the pre-coating electrode with a surfactant, and then covering the surface of the pre-coating electrode with a working layer electrode in a coating mode. The process method is suitable for thick film battery production, avoids the problems of electrode wrinkling, cracking, pulverization and the like caused by the increase of the thickness of the electrode, further improves the internal compactness of the electrode, and is beneficial to improving the overall performance of the battery. The invention has simple preparation process and good repeatability, and can be produced in large scale.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a coating process of a thick film battery and a prepared thick film lithium battery.
Background
As a new generation of green high-energy battery system, the lithium ion battery has the characteristics of high discharge platform, long cycle performance, environmental friendliness and the like, and is widely applied to various fields of digital products, electric automobiles and the like. With increasing commercialization demand, the largest bottleneck currently restricting lithium ion batteries is energy density. According to the proposal of the long-term development plan in the automobile industry, the energy density of the power battery monomer is required to reach 300 Wh/kg. The commercial lithium ion batteries at present mainly comprise lithium iron phosphate batteries and ternary lithium batteries according to the classification of positive electrode materials, and the energy densities of the single batteries are only 140-.
The main methods for increasing the energy density of lithium ion batteries include the use of novel systems, such as lithium sulfur batteries, lithium air batteries, and the like. The theoretical specific energy of the lithium-sulfur battery can reach 2600Wh/kg, but the problems of poor conductivity, shuttle effect and the like are still difficult to solve at present, while the theoretical specific energy of the lithium-air battery can reach 11430Wh/kg, which is similar to the specific energy of gasoline, but the lithium-sulfur battery has the fatal defects of low catalytic efficiency, re-decomposition of discharge products and the like. Another method is to use the anode material with higher gram capacity, such as high nickel ternary material, lithium-rich manganese material, etc. Although the theoretical gram capacity of the material is improved by increasing the proportion of nickel element, the irreversible capacity and the safety performance of the high nickel material are improved. Other methods include increasing the overall energy density of lithium batteries by reducing the proportion of inactive materials such as casing materials, electrode current collectors, electrolytes, etc., and most of the methods adopted by the manufacturers at present are realized on the premise of sacrificing the cycle performance or safety performance of the batteries.
The energy density of the lithium ion battery is improved, and the safety performance of the lithium ion battery is reduced to a certain extent. According to the GB/T31485-2015 regulations, the lithium ion battery should not be ignited and explode in the safety test processes of overcharge, falling, needling and the like. Most manufacturers of commercial batteries currently use a safety valve or other device mounted on the housing to delay the thermal runaway time rather than optimizing the electrode design.
Disclosure of Invention
The invention aims to provide a coating process of a thick film lithium battery for overcoming the defects of low energy density and low safety performance of the conventional lithium battery.
The invention also aims to provide a thick film lithium battery prepared by the coating process.
In order to achieve the purpose, the invention adopts the following technical scheme:
a coating process for a thick film lithium battery, the coating process comprising the steps of:
s1: covering a pre-coating layer on the current collector in a coating mode;
s2: coating a surface active layer on the pre-coating layer obtained in the step S1 in a coating mode;
s3: covering the surface active layer obtained in the step S2 with a working layer in a coating mode;
wherein the thickness of the precoating layer is 5-1000 μm, the thickness of the surface active layer is 0.1-20 μm, and the thickness of the working layer is 5-1000 μm; the precoating layer and the working layer are equally divided into a positive electrode and a negative electrode.
In a preferred embodiment of the present invention, the coating method includes any one of blade coating, roll coating transfer coating, and slit die coating.
In a preferable embodiment of the invention, in the current collector, the thickness of the positive current collector is 5-100 μm; the thickness of the negative electrode current collector is 3-100 μm.
As a preferable scheme of the invention, the formula of the precoating layer of the positive electrode is the same as that of the working layer, and the formula is a positive electrode material: adhesive: the conductive agent is 60-99:0-20: 0-20.
As a preferable scheme of the present invention, the positive electrode material includes any one of lithium nickel cobalt manganese oxide, lithium iron phosphate, lithium cobaltate, lithium manganese oxide, lithium nickelate, or lithium nickel cobalt aluminate; the binder includes polyvinylidene fluoride, and the conductive agent includes conductive carbon black.
As a preferable scheme of the invention, the formula of the precoating layer of the negative electrode is the same as that of the working layer, and the formula is the following negative electrode materials: adhesive: the conductive agent is 60-99:0-20: 0-20.
As a preferable scheme of the invention, the negative electrode material comprises any one of artificial graphite, natural graphite, mesocarbon microbeads, lithium titanate or a silicon-based material; the binder comprises styrene-butadiene rubber emulsion; the conductive agent includes conductive carbon black.
As a preferable scheme of the invention, the slurry of the surface active layer comprises 15-25% of surfactant, 1-3% of binder, 0.1-0.5% of dispersant and the balance of water by mass fraction.
In a preferred embodiment of the present invention, the surfactant includes any one of a primary, secondary, tertiary amine salt, a carboxylate, a sulfate salt, a sulfonate, a phosphate ester salt, a polyoxyethylene type, and a polyol type.
A thick film lithium battery is a lithium battery manufactured by adopting the coating process.
Compared with the prior art, the invention has the beneficial effects that:
1) the precoating layer and the working layer adopt the same formula, the thickness of the precoating layer and the working layer is selected to mainly meet the transmission rate of electrons in the electrode, and performance indexes such as design capacity, cycle performance, rate performance and the like required by battery design are provided on the premise of not influencing the performance of the electrode;
2) because the electrode loading capacity of the invention is several times higher than that of the conventional lithium battery, if the precoating layer and the working layer are combined into single coating, the solvent in the electrode is not uniformly volatilized in the coating process until the solvent is cracked, so that the performance of the electrode is influenced; the surface active layer is added, so that a relatively thin pre-coating layer can be coated firstly, and the pre-coating layer is fully adhered to the current collector on the premise of not cracking;
3) the surface active layer can enable the working layer and the precoating layer to be combined more tightly, and can prevent the working layer and the precoating layer from falling off from the current collector due to the fact that the electrode is too thick;
4) the surface active layer has the property of being compatible with the conventional electrolyte, so that the battery performance is not influenced by side reaction in the working process;
5) the invention has reasonable design, greatly reduces the proportion of inactive substances such as current collector materials and the like to improve the overall energy density of the battery, and simultaneously takes a thicker electrode layer as a way for delaying the thermal runaway of the battery to improve the safety.
Drawings
FIG. 1 is a schematic diagram of a thick film electrode structure;
fig. 2 is a cycle curve for the thick film battery of example 1;
fig. 3 is a thick film battery rate discharge curve of example 1;
fig. 4 is a thick film battery cycling profile of example 2;
fig. 5 is a thick film battery rate discharge curve of example 2;
fig. 6 is a cycle curve for the thick film battery of example 3;
fig. 7 is a thick film battery rate discharge curve of example 3.
In the figure, 1 is a current collector; 2 is a precoat; 3 is a surface active layer; and 4, a working layer.
Detailed Description
The present invention will be described in further detail with reference to the following detailed description and accompanying drawings. Wherein like reference numerals refer to like parts unless otherwise specified. It should be emphasized that the following description is merely exemplary in nature and is not intended to limit the scope of the invention or its application.
Referring to fig. 1, the invention provides a thick film lithium battery, comprising a shell, a positive electrode, a negative electrode, an electrolyte, a diaphragm and an electrolyte, wherein the electrode is structured in such a way that a pre-coating layer 2 is coated on the surface of a current collector 1, a surface active layer 3 is covered on the surface of the pre-coating layer 2, and a working layer 4 is covered on the surface of the surface active layer 3.
The thickness of the precoat layer 2 is 5-1000 μm, the thickness of the surface active layer 3 is 0.1-20 μm, and the thickness of the working layer 4 is 5-1000 μm.
Example 1
The embodiment provides a coating process of a thick film lithium battery electrode and a preparation method of a thick film battery, wherein the method comprises the following steps:
step S1: preparing a positive electrode, adding 92.5% of lithium iron phosphate, 4% of polyvinylidene fluoride and 3.5% of conductive carbon black into an N-methylpyrrolidone solvent according to the mass percentage, uniformly stirring, and preparing positive electrode slurry, wherein the mass of the solvent is 1.2 times of the total mass of the dry powder. The positive electrode slurry is uniformly coated on the surface of an aluminum foil with the thickness of 100 mu m to form a precoating layer.
Step S2: preparing slurry of a surface active layer, adding 15% of sodium dodecyl benzene sulfonate, 3% of binder and 0.5% of dispersant by mass into a deionized water solvent, uniformly stirring to prepare surfactant slurry, wherein the balance is water for dissolving. The surfactant was uniformly applied to the surface of the precoat layer in step S1 to a thickness of 5 μm. And then coating the positive electrode slurry obtained in the step S1 on a surfactant layer to form a working layer with the thickness of 400 microns.
Step S3: preparing a negative electrode, adding 96.5% of artificial graphite, 2% of styrene-butadiene rubber emulsion and 1.5% of conductive carbon black into a water solvent according to the mass percentage, uniformly stirring, and preparing into negative electrode slurry, wherein the mass of the solvent is 1.1 times of the total mass of the dry powder. The negative electrode slurry was uniformly coated on the surface of a 6 μm copper foil to a thickness of 100 μm to form a precoat layer.
Step S4: the slurry of the surface active layer in the step S2 was uniformly applied to the surface of the precoat layer in the step S3, and the thickness was 5 μm. And then coating the negative electrode slurry obtained in the step S3 on a surfactant layer to form a working layer with the thickness of 250 μm.
Step S5: and rolling, winding, baking, encapsulating, injecting and the like the prepared positive and negative electrodes to obtain the thick film lithium battery.
The cycle performance test and the rate discharge test of the thick film lithium battery prepared in example 1 are shown in fig. 2 and fig. 3, and fig. 2 is a cycle curve of the thick film battery prepared in example 1, wherein lithium iron phosphate is used as a positive electrode, artificial graphite is used as a negative electrode, the thickness of a positive electrode working layer is 400 micrometers, the thickness of a negative electrode working layer is 250 micrometers, and a surfactant is sodium dodecyl benzene sulfonate. The testing method comprises the steps of charging to 3.7V at a constant current and constant voltage of 0.5C current density, discharging to 2V at a constant current of 1C current density after standing for 10min, and then charging to 3.7V at a constant current and constant voltage of 0.5C current density again after standing for 10min to repeatedly circulate to obtain a circulation curve. As can be seen, the capacity decayed to 80% after 1260 cycles.
Fig. 3 is a rate discharge curve of a thick film battery in example 1, in which lithium iron phosphate is used as a positive electrode, artificial graphite is used as a negative electrode, the thickness of a positive electrode working layer is 400 μm, the thickness of a negative electrode working layer is 250 μm, and a surfactant is sodium dodecyl benzene sulfonate. The test method comprises the steps of charging to 3.7V at a constant current and a constant voltage of 0.5C current density, and discharging to 2V at a constant current of 0.5C, 1C, 3C and 8C current densities after standing for 30min to obtain discharge curves with different multiplying powers respectively. As can be seen from the graph, the discharge capacities at 0.5C, 1C, 3C and 8C were 26.4Ah, 26.3Ah, 25.9Ah and 23.9Ah, respectively.
Example 2
The embodiment provides a coating process of a thick film lithium battery electrode and a preparation method of a thick film battery, wherein the method comprises the following steps:
step S1: preparing a positive electrode, adding 92.5% of lithium iron phosphate, 4% of polyvinylidene fluoride and 3.5% of conductive carbon black into an N-methylpyrrolidone solvent according to the mass percentage, uniformly stirring, and preparing positive electrode slurry, wherein the mass of the solvent is 1.2 times of the total mass of the dry powder. The positive electrode slurry is uniformly coated on the surface of an aluminum foil with the thickness of 100 mu m to form a precoating layer.
Step S2: preparing slurry of a surface active layer, adding 15% of sodium dodecyl benzene sulfonate, 3% of binder and 0.5% of dispersant by mass into a deionized water solvent, uniformly stirring to prepare surfactant slurry, wherein the balance is water for dissolving. The surfactant was uniformly applied to the surface of the precoat layer in step S1 to a thickness of 5 μm. And then coating the positive electrode slurry obtained in the step S1 on a surfactant layer to form a working layer with the thickness of 600 microns.
Step S3: preparing a negative electrode, adding 96.5% of artificial graphite, 2% of styrene-butadiene rubber emulsion and 1.5% of conductive carbon black into a water solvent according to the mass percentage, uniformly stirring, and preparing into negative electrode slurry, wherein the mass of the solvent is 1.1 times of the total mass of the dry powder. The negative electrode slurry was uniformly coated on the surface of a 6 μm copper foil to a thickness of 100 μm to form a precoat layer.
Step S4: the slurry of the surface active layer in the step S2 was uniformly applied to the surface of the precoat layer in the step S3, and the thickness was 5 μm. And then coating the negative electrode slurry obtained in the step S3 on a surface active agent layer to form a working layer with the thickness of 350 mu m.
Step S5: and rolling, winding, baking, encapsulating, injecting and the like the prepared positive and negative electrodes to obtain the thick film lithium battery.
The cycle performance test and the rate discharge test of the thick film lithium battery prepared in example 2 are shown in fig. 4 and 5, and fig. 4 is a cycle curve of the thick film battery prepared in example 2, wherein lithium iron phosphate is used as a positive electrode, artificial graphite is used as a negative electrode, the thickness of a positive electrode working layer is 600 micrometers, the thickness of a negative electrode working layer is 350 micrometers, and a surfactant is sodium dodecyl benzene sulfonate. The testing method comprises the steps of charging to 3.7V at a constant current and constant voltage of 0.5C current density, discharging to 2V at a constant current of 1C current density after standing for 10min, and then charging to 3.7V at a constant current and constant voltage of 0.5C current density again after standing for 10min to repeatedly circulate to obtain a circulation curve. As can be seen, the capacity decayed to 80% after 640 cycles.
Fig. 5 is a rate discharge curve of a thick film battery in example 2, wherein lithium iron phosphate is used as a positive electrode, artificial graphite is used as a negative electrode, the thickness of a positive working layer is 600 μm, the thickness of a negative working layer is 350 μm, and a surfactant is sodium dodecyl benzene sulfonate. The test method comprises the steps of charging to 3.7V at a constant current and a constant voltage of 0.5C current density, and discharging to 2V at a constant current of 0.5C, 1C, 3C and 8C current densities after standing for 30min to obtain discharge curves with different multiplying powers respectively. As can be seen from the graph, the discharge capacities at 0.5C, 1C, 3C and 8C were 27.6Ah, 26.3Ah, 24Ah and 22.1Ah, respectively.
Example 3
The embodiment provides a coating process of a thick film lithium battery electrode and a preparation method of a thick film battery, wherein the method comprises the following steps:
step S1: preparing a positive electrode, adding 92.5% of lithium iron phosphate, 4% of polyvinylidene fluoride and 3.5% of conductive carbon black into an N-methylpyrrolidone solvent according to the mass percentage, uniformly stirring, and preparing positive electrode slurry, wherein the mass of the solvent is 1.2 times of the total mass of the dry powder. The positive electrode slurry is uniformly coated on the surface of an aluminum foil with the thickness of 100 mu m to form a precoating layer.
Step S2: preparing slurry of a surface active layer, adding 25 mass percent of fatty alcohol-polyoxyethylene ether sodium sulfate, 3 mass percent of binder and 0.5 mass percent of dispersant into a deionized water solvent, uniformly stirring to prepare surfactant slurry, wherein the balance is water to be dissolved. The surfactant was uniformly applied to the surface of the precoat layer in step S1 to a thickness of 5 μm. And then coating the positive electrode slurry obtained in the step S1 on a surfactant layer to form a working layer with the thickness of 400 microns.
Step S3: preparing a negative electrode, adding 96.5% of artificial graphite, 2% of styrene-butadiene rubber emulsion and 1.5% of conductive carbon black into a water solvent according to the mass percentage, uniformly stirring, and preparing into negative electrode slurry, wherein the mass of the solvent is 1.1 times of the total mass of the dry powder. The negative electrode slurry was uniformly coated on the surface of a 6 μm copper foil to a thickness of 100 μm to form a precoat layer.
Step S4: the slurry of the surface active layer in the step S2 was uniformly applied to the surface of the precoat layer in the step S3, and the thickness was 5 μm. And then coating the negative electrode slurry obtained in the step S3 on a surfactant layer to form a working layer with the thickness of 250 μm.
Step S5: and rolling, winding, baking, encapsulating, injecting and the like the prepared positive and negative electrodes to obtain the thick film lithium battery.
The cycle performance test and the rate discharge test of the thick film lithium battery prepared in example 3 are carried out, and the results are shown in fig. 6 and fig. 7, and fig. 6 is a cycle curve of the thick film battery in example 3, wherein lithium iron phosphate is used as a positive electrode, artificial graphite is used as a negative electrode, the thickness of a positive electrode working layer is 400 micrometers, the thickness of a negative electrode working layer is 250 micrometers, and a surfactant is fatty alcohol-polyoxyethylene ether sodium sulfate. The testing method comprises the steps of charging to 3.7V at a constant current and constant voltage of 0.5C current density, discharging to 2V at a constant current of 1C current density after standing for 10min, and then charging to 3.7V at a constant current and constant voltage of 0.5C current density again after standing for 10min to repeatedly circulate to obtain a circulation curve. As can be seen, the capacity decayed to 80% after 950 cycles.
Fig. 7 is a rate discharge curve of the thick film battery in example 3, wherein lithium iron phosphate is used as the positive electrode, artificial graphite is used as the negative electrode, the thickness of the positive electrode working layer is 400 μm, the thickness of the negative electrode working layer is 250 μm, and the surfactant is fatty alcohol-polyoxyethylene ether sodium sulfate. The test method comprises the steps of charging to 3.7V at a constant current and a constant voltage of 0.5C current density, and discharging to 2V at a constant current of 0.5C, 1C, 3C and 8C current densities after standing for 30min to obtain discharge curves with different multiplying powers respectively. As can be seen from the graph, the discharge capacities of 0.5C, 1C, 3C and 8C were 27Ah, 27.2Ah, 24.1Ah and 23.1Ah, respectively.
As can be seen from comparison of the experimental results of fig. 2, fig. 3, fig. 4 and fig. 5, the cycle performance of the battery is significantly reduced after the load of the positive electrode and the negative electrode is increased, and the difference in capacity exertion under low-rate current discharge is not significant, but the capacity exertion of the battery with high load is significantly reduced under high-rate current discharge, mainly because the rate performance is reduced due to the reduction of the electron transmission efficiency along with the increase of the load; as can be seen from comparison of the experimental results shown in fig. 2, fig. 3, fig. 6 and fig. 7, the cycle times of the thick film battery using sodium dodecylbenzenesulfonate as the surfactant are significantly higher than those of the thick film battery using sodium fatty alcohol polyoxyethylene ether sulfate as the surfactant, and the discharge capacity at high rate current is also higher, which indicates that sodium dodecylbenzenesulfonate can make the electrode layer more compact than sodium fatty alcohol polyoxyethylene ether sulfate, and is favorable for electron conduction, thereby improving the rate capability of the battery.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein, and any element in the claims should not be construed as limiting the claim as designed.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment includes only a single embodiment, and such description is for clarity only, and those skilled in the art should make the description as a whole, and the embodiments may be appropriately combined to form other embodiments understood by those skilled in the art.
Claims (10)
1. A coating process for a thick film lithium battery, the coating process comprising the steps of:
s1: covering a pre-coating layer on the current collector in a coating mode;
s2: coating a surface active layer on the pre-coating layer obtained in the step S1 in a coating mode;
s3: covering the surface active layer obtained in the step S2 with a working layer in a coating mode;
wherein the thickness of the precoating layer is 5-1000 μm, the thickness of the surface active layer is 0.1-20 μm, and the thickness of the working layer is 5-1000 μm; the precoating layer and the working layer are equally divided into a positive electrode and a negative electrode.
2. The process of claim 1, wherein the coating is knife coating, roll coating transfer coating or slot die coating.
3. The process of claim 1, wherein the positive electrode current collector has a thickness of 5-100 μm; the thickness of the negative electrode current collector is 3-100 μm.
4. The process of claim 1, wherein the formulation of the pre-coating layer of the positive electrode is the same as the formulation of the working layer, and the formulation is the positive electrode material: adhesive: the conductive agent is 60-99:0-20: 0-20.
5. The coating process of claim 4, wherein the positive electrode material comprises any one of lithium nickel cobalt manganese oxide, lithium iron phosphate, lithium cobalt oxide, lithium manganese oxide, lithium nickel oxide or lithium nickel cobalt aluminate; the binder includes polyvinylidene fluoride, and the conductive agent includes conductive carbon black.
6. The process of claim 1, wherein the formulation of the pre-coating layer of the negative electrode is the same as the formulation of the working layer, and the formulation is the negative electrode material: adhesive: the conductive agent is 60-99:0-20: 0-20.
7. The coating process of claim 6, wherein the negative electrode material comprises any one of artificial graphite, natural graphite, mesocarbon microbeads, lithium titanate or silicon-based material; the binder comprises styrene-butadiene rubber emulsion; the conductive agent includes conductive carbon black.
8. The process of claim 1, wherein the slurry of the surface active layer comprises 15-25% surfactant, 1-3% binder, 0.1-0.5% dispersant and balance water by mass fraction.
9. The process of claim 8, wherein the surfactant comprises any one of primary and secondary tertiary amine salts, carboxylic acid salts, sulfate salts, sulfonate salts, phosphate salts, polyoxyethylene type or polyol type.
10. A thick film lithium battery, characterized in that the lithium battery is made by the coating process according to any of claims 1-9.
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