CN115425184A - Preparation method of lithium ion battery negative pole piece - Google Patents
Preparation method of lithium ion battery negative pole piece Download PDFInfo
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- CN115425184A CN115425184A CN202210695477.0A CN202210695477A CN115425184A CN 115425184 A CN115425184 A CN 115425184A CN 202210695477 A CN202210695477 A CN 202210695477A CN 115425184 A CN115425184 A CN 115425184A
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- 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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1395—Processes of manufacture of electrodes based on metals, Si or alloys
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- 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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- 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
- H01M4/04—Processes of manufacture in general
- H01M4/0402—Methods of deposition of the material
- H01M4/0404—Methods of deposition of the material by coating on electrode collectors
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/386—Silicon or alloys based on silicon
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- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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- 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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/621—Binders
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- H—ELECTRICITY
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/621—Binders
- H01M4/622—Binders being polymers
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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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
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Abstract
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a preparation method of a lithium ion battery negative electrode plate. Adding a silicon-based negative electrode active material, a conductive agent and a novel binder in a certain mass ratio into a liquid reagent, stirring and mixing at 20-60 ℃ to form viscous slurry, then uniformly coating the obtained slurry on the surface of copper foil by using a coating machine, and performing forced air drying at 50-80 ℃ for 0.5-1 h and vacuum drying at 100-160 ℃ for 8-20 h respectively to obtain the negative electrode piece of the lithium ion battery. The preparation method of the lithium ion negative pole piece has the advantages of simple process and low cost, and the prepared pole piece shows high specific capacity, high rate discharge, good first coulombic efficiency and excellent cycle performance after being assembled into a battery.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a preparation method of a lithium ion battery negative electrode plate.
Background
Lithium ion batteries stand out of numerous energy storage devices with their advantages of high energy efficiency, long life, portability, light weight, and the like, and have achieved great success in the past decades. However, new technologies represented by electric vehicles have a strong demand for higher energy density of lithium ion batteries while ensuring high safety. Silicon has a high theoretical specific capacity (4200 mAhg), compared to graphite (Si-Si) -1 ) The lithium ion battery cathode material has the advantages of low working voltage, abundant reserves and the like, and is hopeful to replace a graphite cathode material to serve as a next-generation high-energy-density lithium ion battery cathode material. However, the large volume change of silicon during lithium intercalation and deintercalation (up to 300%) destroys the integrity of the electrode, resulting in a rapid decline in the electrode capacity. The current scientific community has recognized that binders can greatly improve the cycling stability of silicon anodes. The traditional CMC + SBR binder has an undesirable application effect in a silicon negative pole piece, and due to weak van der Waals interaction between the CMC + SBR binder and a silicon material and a copper current collector, silicon is continuously pulverized, cracked and separated from the current collector in the process of repeatedly releasing and embedding lithium, so that the capacity is sharply attenuated to lose efficacy. Therefore, a preparation method is urgently needed to improve the service life of the silicon-based negative electrode plate.
Disclosure of Invention
The invention aims to provide a method for preparing a lithium ion battery negative pole piece with excellent electrochemical performance, which has simple process and low cost.
In order to realize the purpose, the invention adopts the technical scheme that:
the invention provides a preparation method of a lithium ion battery negative pole piece, which comprises the following steps:
(1) The silicon-based negative electrode material with the mass ratio of 75-90%, the conductive agent with the mass ratio of 5-20%, the novel binder with the mass ratio of 5-10% and the liquid reagent with the total mass ratio of 400-600% are magnetically stirred for 10h-24h (preferably 16 h) at the temperature of 20-60 ℃ (preferably 25 ℃) to form slurry.
(2) The mixed slurry is uniformly coated on the surface of the copper foil by using a coating machine, and the coating thickness is controlled to be 8-20 um (preferably 12 um).
(3) And (3) respectively carrying out air blast drying on the coated pole piece for 0.5h-1h at 50-80 ℃ (preferably 70 ℃) and vacuum drying for 8h-20h (preferably 12 h) at 100-160 ℃ (preferably 120-150 ℃) to obtain the lithium ion battery negative pole piece.
(4) The pole pieces were assembled into button cells to test their performance.
Preferably, the silicon-based negative electrode material accounts for 78-79%.
Preferably, the silicon-based negative electrode material is at least one of pure silicon, carbon-coated silicon and a silicon-carbon composite material, wherein the carbon content in the carbon-coated silicon is less than 5%, and the silicon content in the silicon-carbon composite material is more than 1%. The silicon-based negative electrode material is preferably pure silicon.
More preferably, the conductive agent is at least one of Super-P, ketjen black, carbon Nanotubes (CNTs), graphene and carbon fibers. The conductive agent is preferably Super-P and CNTs which account for 9 percent and 1 percent respectively.
Preferably, the novel binder is at least one of cinnamic acid, salicylic acid, gallic acid, benzoic acid, terephthalic acid, trimesic acid, pyromellitic acid or a product obtained by combining any of the above materials with sodium carboxymethyl cellulose, and preferably the content ratio of pyromellitic acid or the product obtained by combining pyromellitic acid with sodium carboxymethyl cellulose is 1.
More preferably, the liquid reagent is at least one of ethanol, water, acetone and ethylene glycol, preferably water and ethanol (preferably in a ratio of 3.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention has simple operation and low cost;
2. the novel adhesive adopted by the invention can form hydrogen bonds and covalent bonds between the surface of a silicon atom and the inside of the adhesive, and effectively inhibit the volume expansion of silicon in the process of lithium intercalation and deintercalation;
3. the product of the invention has excellent electrical property, high first coulombic efficiency, long cycle life and good multiplying power performance;
4. the pole piece prepared by the technology has good consistency, stable property and easy industrialization.
Detailed Description
The invention provides a preparation method of a lithium ion battery negative electrode plate, which is to facilitate understanding of the invention through specific embodiments, and the following detailed description of the technical scheme of the invention is provided, and it is to be noted that the following specific embodiments are intended to further describe without departing from the concept of the invention, and may make several modifications, and are not intended to limit the scope of the invention.
Example 1
Respectively weighing 0.8g of pure silicon, 0.1g of super-P, 0.05g of CMC and 0.05g of pyromellitic acid according to the mass fractions of 80%, 10%, 5% and 5% into a penicillin bottle, adding 5ml of deionized water and 0.5ml of absolute ethyl alcohol, stirring for 10 hours and uniformly mixing at 25 ℃ by using a magnetic stirrer to obtain slurry, uniformly coating the slurry on a copper foil on a coating machine, drying for 0.5 hour in a blast drying oven at 70 ℃, transferring the slurry into a vacuum drying oven, drying for 12 hours at 120 ℃, slicing into slices, assembling into a button cell in a glove box under low-water and low-oxygen atmosphere, and finally activating for one circle in a test cabinet at the current density of 100mA/g and then performing a cycle test at the current density of 1000 mA/g. The test results (as shown in table 1) show that the performance of the silicon negative electrode plate prepared by the novel binder is far better than that of the electrode plate prepared by the traditional process in the comparative example 1.
Example 2
Respectively weighing 0.81g of pure silicon, 0.1g of Ketjen black, 0.05g of CMC and 0.04g of pyromellitic acid according to mass fractions of 81%, 10%, 5% and 4%, adding into a penicillin bottle, adding 5.5ml of deionized water and 0.5ml of ethylene glycol, stirring and uniformly mixing at 35 ℃ by using a magnetic stirrer to obtain slurry, uniformly coating the slurry on a copper foil on a coating machine, drying for 0.5h in a 70 ℃ blast drying oven, transferring into a vacuum drying oven, drying for 16h at 150 ℃, slicing into a glove box under low-water and low-oxygen atmosphere, assembling into a button cell, and finally activating for one turn in a test cabinet at a current density of 100mA/g and performing a cycle test at a current density of 1000 mA/g. The test results (as shown in table 1) show that the performance of the silicon negative electrode plate prepared by the novel binder is far better than that of the electrode plate prepared by the traditional process in the comparative example 1.
Example 3
Respectively weighing 0.8g of pure silicon, 0.09g of super-P, 0.02g of CNTs, 0.06g of CMC and 0.03g of pyromellitic acid according to the mass fractions of 80%, 9%, 2%, 6% and 3%, adding into a penicillin bottle, adding 4.5ml of deionized water and 0.5ml of absolute ethyl alcohol, stirring for 16 hours at 45 ℃ by using a magnetic stirrer, uniformly mixing to obtain slurry, uniformly coating the slurry on a copper foil on a coating machine, drying for 0.5 hour in a blast drying box at 70 ℃, transferring into a vacuum drying box, drying for 12 hours at 150 ℃, slicing into a glove box in a low-water low-oxygen atmosphere to assemble a button cell, activating for one circle in a test cabinet at the current density of 100mA/g, and performing a cycle test at the current density of 1000 mA/g. The test results (shown in table 1) show that the performance of the silicon negative electrode pole piece prepared by the novel adhesive is far better than that of the pole piece prepared by the traditional process in the comparative example 1.
Example 4
Respectively weighing 0.85g of pure silicon, 0.08g of carbon fiber, 0.02g of graphene, 0.025g of CMC and 0.025g of gallic acid according to the mass fractions of 85%, 8%, 2%, 2.5% and 2.5% into a penicillin bottle, adding 4.5ml of deionized water and 0.5ml of absolute ethyl alcohol, stirring and uniformly mixing at 40 ℃ by using a magnetic stirrer to obtain slurry, uniformly coating the slurry on a copper foil on a coating machine, drying for 0.5h in a blast drying oven at 70 ℃, transferring the slurry into a vacuum drying oven, drying for 18h at 120 ℃, slicing into a glove box in a low-water low-oxygen atmosphere to assemble a button cell, activating for one turn in a test cabinet at the current density of 100mA/g, and performing a cycle test at the current density of 1000 mA/g. The test results (as shown in table 1) show that the performance of the silicon negative electrode plate prepared by the novel binder is far better than that of the electrode plate prepared by the traditional process in the comparative example 1.
Example 5
Weighing 0.82g of pure silicon, 0.1g of super-P, 0.05g of CMC and 0.03g of cinnamic acid according to the mass fractions of 82%, 10%, 5% and 3% respectively, adding the pure silicon, 0.1g of super-P, 0.05g of CMC and 0.03g of cinnamic acid into a penicillin bottle, adding 5ml of deionized water and 0.5ml of acetone, stirring for 10 hours and uniformly mixing at 40 ℃ by using a magnetic stirrer to obtain slurry, uniformly coating the slurry on a copper foil on a coating machine, drying for 0.5 hour at 70 ℃ in a forced air drying oven, transferring the slurry into a vacuum drying oven, drying for 12 hours at 120 ℃, slicing the slurry into a glove box in a low-water low-oxygen atmosphere, and finally activating for one circle in a test cabinet at a button current density of 100mA/g, and performing a cycle test at a current density of 1000 mA/g. The test results (as shown in table 1) show that the performance of the silicon negative electrode plate prepared by the novel binder is far better than that of the electrode plate prepared by the traditional process in the comparative example 1.
Example 6
Respectively weighing 0.85g of pure silicon, 0.05g of Ketjen black, 0.05g of CMC and 0.05g of trimesic acid according to the mass fractions of 85%, 5% and 5% into a penicillin bottle, adding 6ml of deionized water and 0.5ml of absolute ethyl alcohol, stirring and uniformly mixing for 20 hours at 40 ℃ by using a magnetic stirrer to obtain slurry, uniformly coating the slurry on a copper foil on a coating machine, drying for 0.5 hour in a 70 ℃ blast drying oven, transferring the slurry into a vacuum drying oven, drying for 12 hours at 120 ℃, slicing the slurry into a glove box in a low-water low-oxygen atmosphere, preparing a button cell, activating for one circle in a test cabinet at a current density of 100mA/g, and performing a cycle test at a current density of 1000 mA/g. The test results (as shown in table 1) show that the performance of the silicon negative electrode plate prepared by the novel binder is far better than that of the electrode plate prepared by the traditional process in the comparative example 1.
Example 7
Respectively weighing 0.90g of pure silicon, 0.05g of super-P, 0.025g of CMC and 0.025g of pyromellitic acid according to the mass fractions of 90%, 5%, 2.5% and 2.5% into a penicillin bottle, adding 5.5ml of deionized water and 0.5ml of absolute ethyl alcohol, stirring and uniformly mixing at 60 ℃ by using a magnetic stirrer to obtain slurry, uniformly coating the slurry on a copper foil on a coating machine, drying for 0.5h in a 70 ℃ blast drying oven, transferring the slurry into a vacuum drying oven, drying for 12h at 120 ℃, slicing into a glove box in a low-water low-oxygen atmosphere to assemble a battery, and finally activating for one circle in a button type test cabinet at the current density of 100mA/g and performing a circulation test at the current density of 1000 mA/g. The test results (as shown in table 1) show that the performance of the silicon negative electrode plate prepared by the novel binder is far better than that of the electrode plate prepared by the traditional process in the comparative example 1.
Example 8
Respectively weighing 80g of pure silicon, 0.1g of super-P and 0.1g of gallic acid according to the mass fractions of 80%, 10% and 10% to be added into a penicillin bottle, then adding 5ml of deionized water and 1ml of absolute ethyl alcohol, stirring for 16 hours at the temperature of 40 ℃ by using a magnetic stirrer to be uniformly mixed to obtain slurry, uniformly coating the slurry on copper foil on a coating machine, drying for 0.5 hour at a 70 ℃ blast drying box, then transferring the slurry to a vacuum drying box, drying for 12 hours at the temperature of 120 ℃, then slicing the dried slurry into button cells in a glove box in a low-water low-oxygen atmosphere, finally activating the button cells for one circle in a test cabinet at the current density of 100mA/g, and then carrying out a cycle test at the current density of 1000 mA/g. The test results (as shown in table 1) show that the performance of the silicon negative electrode plate prepared by the novel binder is far better than that of the electrode plate prepared by the traditional process in the comparative example 1.
Example 9
Weighing 84%, 10%, 3% and 3% of silicon-carbon-coated material 0.84g, super-P0.1 g, CMC 0.03g and salicylic acid 0.03g respectively according to mass fraction, adding into a penicillin bottle, adding 5ml of deionized water and 0.5ml of absolute ethyl alcohol, stirring for 14h and mixing uniformly at 50 ℃ in a water bath by using a magnetic stirrer to obtain slurry, uniformly coating the slurry on a copper foil on a coating machine, drying for 0.5h in a blast drying oven at 70 ℃, transferring into a vacuum drying oven, drying for 12h at 130 ℃, slicing into a glove box in a low-water low-oxygen atmosphere to assemble a button cell, and finally activating for one turn in a test cabinet at a current density of 100mA/g and performing a cycle test at a current density of 1000 mA/g. The test results (as shown in table 1) show that the performance of the carbon-coated silicon negative electrode plate prepared by the novel adhesive is far better than that of the electrode plate prepared by the traditional process in the comparative example 1.
Example 10
Respectively weighing 0.8g of pure silicon material, 0.1g of super-P and 0.1g of pyromellitic acid according to the mass fractions of 80%, 10% and 10% into a penicillin bottle, adding 5ml of deionized water and 0.5ml of absolute ethyl alcohol, stirring for 14 hours at 25 ℃ in a water bath by using a magnetic stirrer to obtain slurry, uniformly coating the slurry on a copper foil on a coating machine, drying for 0.5 hour at 70 ℃ in a blast drying box, transferring the slurry into a vacuum drying box, drying for 12 hours at 130 ℃, slicing into slices, assembling into a glove box in a low-water low-oxygen atmosphere to obtain a button cell, and finally activating for one circle in a test cabinet at a current density of 100mA/g and then performing a cycle test at a current density of 1000 mA/g. The test results (shown in table 1) show that the performance of the silicon negative electrode pole piece prepared by the novel adhesive is far better than that of the pole piece prepared by the traditional process in the comparative example 2.
Example 11
Respectively weighing 0.81g of silicon-carbon composite material, 0.09g of super-P, 0.05g of CMC and 0.05g of pyromellitic acid according to mass fractions of 81%, 9%, 5% and 5%, adding into a penicillin bottle, adding 4ml of deionized water and 0.5ml of absolute ethyl alcohol, stirring and uniformly mixing at 50 ℃ by using a magnetic stirrer to obtain slurry, uniformly coating the slurry on a copper foil on a coating machine, drying for 0.5h in a 70 ℃ blast drying box, transferring into a vacuum drying box, drying for 12h at 120 ℃, slicing into a box in low-water and low-oxygen atmosphere to assemble a button cell, and finally, activating a glove for one turn in a test cabinet at a current density of 100mA/g, and performing a cycle test at a current density of 400 mA/g. The test results (as shown in table 1) show that the performance of the silicon-carbon composite negative pole piece prepared by the novel binder is far better than that of the pole piece prepared by the traditional process in the comparative example 3.
Comparative example 1
Respectively weighing 0.8g of pure silicon, 0.1g of super-P, 0.05g of CMC and 0.05g of SBR according to the mass fractions of 80%, 10%, 5% and 5%, adding into a penicillin bottle, adding 5.5ml of deionized water and 0.5ml of absolute ethyl alcohol, stirring and uniformly mixing at 25 ℃ by using a magnetic stirrer to obtain slurry, uniformly coating the slurry on a copper foil on a coating machine, drying for 0.5h in a 70 ℃ forced air drying oven, transferring into a vacuum drying oven, drying for 12h at 120 ℃, slicing into a low-water low-oxygen atmosphere box, assembling into a button cell, activating a glove in a test cabinet for one circle at a current density of 100mA/g, and performing a cycle test at a current density of 1000mA/g, wherein the test results are shown in Table 1.
Comparative example 2
Respectively weighing 0.85g of carbon-coated silicon, 0.05g of super-P, 0.05g of CMC and 0.05g of SBR according to the mass fractions of 85%, 5% and adding into a penicillin bottle, then adding 5.5ml of deionized water and 0.5ml of absolute ethyl alcohol, stirring and uniformly mixing for 12 hours at 25 ℃ by using a magnetic stirrer to obtain slurry, uniformly coating the slurry on a copper foil on a coating machine, drying for 0.5 hour in a 70 ℃ forced air drying oven, then transferring into a vacuum drying oven to dry for 12 hours at 120 ℃, then slicing into a low-water and low-oxygen atmosphere box to assemble a button cell, finally activating a glove in a test cabinet for one circle at a current density of 100mA/g and then carrying out a cycle test at a current density of 1000mA/g, wherein the test results are shown in Table 1.
Comparative example 3
Respectively weighing 0.85g of silicon-carbon composite material, 0.05g of super-P, 0.05g of CMC and 0.05g of SBR according to the mass fractions of 85%, 5% and 5% into a penicillin bottle, adding 5ml of deionized water and 0.5ml of absolute ethyl alcohol, stirring and uniformly mixing at 25 ℃ by using a magnetic stirrer to obtain slurry, uniformly coating the slurry on a copper foil on a coating machine, drying for 0.5h in a 70 ℃ forced air drying oven, transferring the slurry into a vacuum drying oven, drying for 12h at 120 ℃, slicing the slurry into a glove box in a low-water low-oxygen atmosphere, assembling a button cell, activating for one turn in a test cabinet at a current density of 100mA/g, and performing a cycle test at a current density of 400mA/g, wherein the test results are shown in Table 1.
Table 1: comparison of electrochemical Performance of samples of each example and related comparative samples
Claims (5)
1. A preparation method of a lithium ion battery negative pole piece is characterized by comprising the following steps: adding a silicon-based negative electrode active material, a conductive agent and a novel binder in a certain mass ratio into a liquid reagent, and stirring and mixing at 20-60 ℃ to form viscous slurry; and then uniformly coating the obtained slurry on the surface of the copper foil by using a coating machine, and respectively carrying out forced air drying at the temperature of 50-80 ℃ for 0.5-1 h and vacuum drying at the temperature of 100-160 ℃ for 8-20 h to obtain the lithium ion battery negative pole piece.
2. The preparation method of the lithium ion battery negative electrode piece according to claim 1, characterized in that: the mass sum of the silicon-based negative electrode active material, the conductive agent and the novel binder is taken as the total mass, the mass percentage of the silicon-based negative electrode active material to the total mass is 75-90%, the mass percentage of the conductive agent to the total mass is 5-20%, and the mass percentage of the novel binder to the total mass is 5-10%.
3. The preparation method of the lithium ion battery negative electrode piece according to claim 1, characterized in that: the silicon-based negative electrode active material is at least one of pure silicon, carbon-coated silicon and a silicon-carbon composite material, wherein the carbon content in the carbon-coated silicon is less than 5%, and the silicon content in the silicon-carbon composite material is more than 1%.
4. The preparation method of the lithium ion battery negative electrode piece according to claim 1, characterized in that: the conductive agent is at least one of Super-P, ketjen black, carbon nano tubes, graphene and carbon fibers; the liquid reagent is at least one of ethanol, water, acetone and glycol.
5. The preparation method of the lithium ion battery negative electrode piece according to claim 1, characterized in that: the novel binder is at least one of cinnamic acid, salicylic acid, gallic acid, benzoic acid, terephthalic acid, trimesic acid, pyromellitic acid or a product obtained by combining any of the above materials with sodium carboxymethylcellulose.
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