CN110707266A - PVDF (polyvinylidene fluoride) mixed coating slurry, preparation method thereof and diaphragm - Google Patents
PVDF (polyvinylidene fluoride) mixed coating slurry, preparation method thereof and diaphragm Download PDFInfo
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- CN110707266A CN110707266A CN201910900991.1A CN201910900991A CN110707266A CN 110707266 A CN110707266 A CN 110707266A CN 201910900991 A CN201910900991 A CN 201910900991A CN 110707266 A CN110707266 A CN 110707266A
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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
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/411—Organic material
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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
- 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
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/403—Manufacturing processes of separators, membranes or diaphragms
-
- 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
Abstract
The invention discloses PVDF mixed coating slurry, a preparation method thereof and a diaphragm, wherein the preparation method comprises the following steps: adding 0.1-0.2 part by mass of a dispersing agent and 1-3 parts by mass of PVDF into 12-18 parts by mass of a dispersing medium, uniformly dispersing, sanding, adding 0.5-3 parts by mass of a thickening agent, 0.5-1 part by mass of a binder, 1 part by mass of a pore-forming agent and 1-2 parts by mass of a coating emulsion, uniformly stirring to obtain the PVDF mixed coating slurry. The surface of the final PVDF agglomerate is interspersed or coated with a more strongly adherent substance. The diaphragm of the invention can improve the single-point height and the adhesive force of spraying, and the further improvement of the adhesive force can meet the design requirements of more customers on batteries.
Description
Technical Field
The invention belongs to the technical field of battery diaphragms, and particularly relates to PVDF (polyvinylidene fluoride) mixed coating slurry, a preparation method thereof and a diaphragm.
Background
The diaphragm is one of the most critical inner layer components in the power battery structure, and the main function of the diaphragm is to separate positive and negative plates in the battery and prevent the positive and negative plates from being in direct contact to generate short circuit. Meanwhile, the diaphragm is provided with a large number of through micropores, positive and negative ions in the battery can freely pass through the micropores, the positive and negative electrodes migrate between the positive and negative plates to form an internal conductive loop of the battery, and electrons migrate between the positive and negative electrodes through an external loop to form current for utilization by electric equipment.
Therefore, the performance of the separator not only determines the interface structure, internal resistance and the like of the battery, but also directly affects the characteristics of the battery such as capacity, cycle and safety performance, and the separator with excellent performance plays an important role in improving the comprehensive performance of the battery.
In the application of the PVDF coating diaphragm in the battery, the hardness of the battery core is increased mainly by the gel electrolyte principle and the function of bonding the diaphragm and the pole piece. The commonly used sizing agent is water-based PVDF sizing agent, but the binding force between the coating coated by the water-based PVDF sizing agent and the battery pole piece is not ideal. While the comparison document CN108841026A blends PMMA into PVDF to improve the binding power, the uneven coating under the micro-morphology indicates that the performance of the additive does not perform well.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a preparation method of PVDF mixed coating slurry.
Another object of the present invention is to provide a PVDF slurry for mixed coating obtained by the above-mentioned preparation method.
The invention also aims to provide a diaphragm based on the PVDF mixed coating slurry.
Another object of the present invention is to provide a method for preparing the above separator.
The purpose of the invention is realized by the following technical scheme.
A preparation method of PVDF mixed coating slurry comprises the following steps: adding 0.1-0.2 part by mass of a dispersing agent and 1-3 parts by mass of PVDF into 12-18 parts by mass of a dispersion medium, uniformly dispersing, sanding, adding 0.5-3 parts by mass of a thickening agent, 0.5-1 part by mass of a binder, 1 part by mass of a pore-forming agent and 1-2 parts by mass of a coating emulsion, and uniformly stirring to obtain the PVDF mixed coating slurry, wherein the dispersion medium is deionized water, the dispersing agent is a modified polyether polymer, fatty alcohols, sodium polyethylene glycol alkylaryl ether sulfonate, alkylphenol ethoxylates, polyoxyethylene alkylphenol ether or sodium polyacrylate, the thickening agent is PVA (polyvinyl alcohol), PEG (polyethylene glycol), PVP (polyvinylpyrrolidone) or CMC (sodium carboxymethylcellulose), the binder is polymethyl acrylate, SBR (styrene butadiene rubber) or xanthan gum, and the pore-forming agent is ethanol, sodium hydroxide, sodium, Ether, propanol, isopropanol or acetone, and the coating emulsion is at least one of polymethyl acrylate, polyethyl acrylate, alpha-cyano acrylate and styrene butadiene rubber.
In the technical scheme, the sanding speed is 500-1000 RPM, and the time is 10-30 min.
The PVDF mixed coating slurry obtained by the preparation method.
A PVDF washcoat slurry-based separator comprising: the coating comprises a base film, an aluminum oxide coating covering one side of the base film and a PVDF mixed coating slurry coating covering the aluminum oxide coating.
In the technical scheme, the thickness of the aluminum oxide coating is 2-4 um.
In the technical scheme, the thickness of the PVDF mixed coating slurry coating is 1-5 um.
In the above technical scheme, the base film is a PP film, a PE film or a composite film, and the composite film is a composite film of PP and PE.
The preparation method of the diaphragm comprises the following steps: and coating a layer of aluminum oxide on the base film, drying to form the aluminum oxide coating, coating the PVDF mixed coating slurry, and keeping the temperature at 60-90 ℃ for 0.3-0.5 min to form the PVDF mixed coating slurry coating.
In the technical scheme, the PVDF mixed coating slurry is coated by rotary spraying, the coating speed of the rotary spraying is 40-50 m/min, and the rotor speed is 6000-8000 rpm/min.
In the technical scheme, the method for coating the aluminum oxide is micro-gravure roll coating.
In the technical scheme, the drying temperature is 35-85 ℃, and the drying time is 0.1-3.0 min.
The PVDF mixed coating slurry is applied to improving the adhesive force of the diaphragm.
The PVDF mixed coating slurry is applied to improving the capacity retention rate of the battery.
The present invention uses PVDF aggregate particles as carriers to add emulsion and carry out secondary spraying granulation. The surface of the final PVDF agglomerate is interspersed or coated with a more strongly adherent substance. The diaphragm of the invention can improve the single-point height and the adhesive force of spraying, and the further improvement of the adhesive force can meet the design requirements of more customers on batteries.
The concrete advantages are that:
(1) the method provides higher adhesive force in the assembly process of the lithium ion battery and improves the strength of the battery core.
(2) After the battery is assembled, the interface is improved due to the binding force between the diaphragm and the battery pole piece, and the cycle performance of the lithium ion battery is further improved.
Drawings
FIG. 1 is an SEM of the separator obtained in example 1 of the present invention.
Detailed Description
The technical scheme of the invention is further explained by combining specific examples.
The following examples relate to the following types of instruments:
thickness-marpachymeter-C1216;
air permeability-air permeability tester-4340;
acupuncture-shimadzu acupuncture instrument-AGS-X;
shimadzu intelligent electronic tension tester-AGS-X
Example 1
A preparation method of PVDF mixed coating slurry (single-point coating spraying slurry) comprises the following steps:
adding 0.2kg of dispersing agent and 3kg of PVDF into 17.7kg of deionized water, stirring for 2h until the materials are uniformly dispersed, sanding (1000rpm for 15min), adding 2.8kg of thickening agent, 1kg of binder, 1kg of pore-forming agent and 2kg of coating emulsion, and stirring uniformly (40rpm for 15min) to obtain PVDF mixed coating slurry, wherein the dispersing agent is alkylphenol polyvinyl ether, the thickening agent is CMC, the binder is SBR, the pore-forming agent is ethanol, and the coating emulsion is polyethylacrylate.
A PVDF blend coating slurry based separator comprising: the base film, cover the aluminium oxide coating on base film one side and cover the PVDF thoughtlessly scribbles the thick liquids coating on the aluminium oxide coating, the thickness of aluminium oxide coating is 2um, and the thickness that the thick liquids coating was thoughtlessly scribbled to PVDF is 2um, and the base film is the PE base film.
A method of making a separator comprising: coating a layer of aluminum oxide on a base film, drying (75 ℃ for 2min) to form an aluminum oxide coating, coating PVDF mixed coating slurry, and keeping the temperature at 90 ℃ for 0.5min to form a PVDF mixed coating slurry coating. The PVDF mixed coating slurry is coated by rotary spraying, wherein the coating speed of the rotary spraying is 50m/min, and the rotor speed is 8000 rpm/min. The method for coating the aluminum oxide is micro gravure roll coating.
The properties of the separator obtained in example 1 are shown in table 1.
TABLE 1
From table 1, it can be seen that the separator has good thickness controllability, air permeability rationality and heat resistance (shrinkage), and can meet the use requirements of lithium ion batteries.
Example 2
A preparation method of PVDF mixed coating slurry comprises the following steps:
adding 0.1kg of dispersing agent and 1kg of PVDF into 13kg of deionized water, stirring for 2h until the materials are uniformly dispersed, sanding (500rpm for 20min), adding 2kg of thickening agent, 0.6kg of binder, 1kg of pore-forming agent and 1kg of coating emulsion, and stirring uniformly (40rpm for 15min) to obtain PVDF mixed coating slurry, wherein the dispersing agent is polyoxyethylene alkylphenol ether, the thickening agent is PVP, the binder is SBR, the pore-forming agent is acetone, and the coating emulsion is styrene butadiene rubber.
A PVDF blend coating slurry based separator comprising: the base film, cover the aluminium oxide coating on base film one side and cover the PVDF thoughtlessly scribbles the thick liquids coating on the aluminium oxide coating, the thickness of aluminium oxide coating is 2um, and the thickness that the thick liquids coating was thoughtlessly scribbled to PVDF is 2um, and the base film is the PE base film.
A method of making a separator comprising: coating a layer of aluminum oxide on a base film, drying (70 ℃, 1.5min) to form an aluminum oxide coating, coating PVDF mixed coating slurry, and keeping at 60 ℃ for 0.4min to form the PVDF mixed coating slurry coating. The PVDF mixed coating slurry is coated by a rotary spraying method, wherein the coating speed of the rotary spraying is 45m/min, and the rotor speed is 7000 rpm/min. The method for coating the aluminum oxide is micro gravure roll coating.
The properties of the separator obtained in example 2 are shown in table 2.
TABLE 2
| Thickness of the diaphragm | um | 15.9 |
| Degree of air permeability | s/100ml | 175.6 |
| Areal density | g/m2 | 10.8 |
| Tensile Strength MD | kgf/cm2 | 1776.6 |
| Tensile Strength TD | kgf/cm2 | 1508.1 |
| Strength of needling | N | 6.2 |
| Shrinkage of 105 x 1 h% | MD/TD | 0.6/0.2 |
Example 3
A preparation method of PVDF mixed coating slurry comprises the following steps:
adding 0.2kg of dispersing agent and 1kg of PVDF into 12kg of deionized water, stirring for 2h until the materials are uniformly dispersed, sanding (800rpm for 18min), adding 0.8kg of thickening agent, 0.5kg of binder, 1kg of pore-forming agent and 1.5kg of coating emulsion, and stirring uniformly (40rpm for 20min) to obtain PVDF mixed coating slurry, wherein the dispersing agent is sodium polyacrylate, the thickening agent is PEG, the binder is xanthan gum, the pore-forming agent is isopropanol, and the coating emulsion is alpha-cyano acrylate.
A PVDF blend coating slurry based separator comprising: the base film, cover the aluminium oxide coating on base film one side and cover the PVDF thoughtlessly scribbles the thick liquids coating on the aluminium oxide coating, the thickness of aluminium oxide coating is 2um, and the thickness that the thick liquids coating was thoughtlessly scribbled to PVDF is 2um, and the base film is the PE base film.
A method of making a separator comprising: coating a layer of aluminum oxide on a base film, drying (55 ℃,2.5min) to form an aluminum oxide coating, coating PVDF mixed coating slurry, and keeping at 70 ℃ for 0.3min to form a PVDF mixed coating slurry coating. The PVDF mixed coating slurry is coated by rotary spraying, wherein the coating speed of the rotary spraying is 40m/min, and the rotor speed is 6000 rpm/min. The method for coating the aluminum oxide is micro gravure roll coating.
The properties of the separator obtained in example 3 are shown in table 3.
TABLE 3
| Thickness of the diaphragm | um | 15.9 |
| Degree of air permeability | s/100ml | 177.9 |
| Areal density | g/m2 | 10.8 |
| Tensile Strength MD | kgf/cm2 | 1775.7 |
| Tensile Strength TD | kgf/cm2 | 1525.1 |
| Strength of needling | N | 6.1 |
| Shrinkage of 105 x 1 h% | MD/TD | 0.7/0.1 |
FIG. 1 is an SEM of the separator obtained in example 1 of the present invention. It can be seen from the picture that after the second granulation, the surface of the PVDF aggregate is decorated with a substance with stronger viscosity.
Comparative example 1
The separator described in example 1 of publication No. CN 108841026A.
Comparative example 2
A method of preparing a hybrid coating slurry, comprising:
adding 0.2kg of dispersing agent and 3kg of PVDF into 17.7kg of deionized water, stirring for 2h until the materials are uniformly dispersed, sanding (1000rpm for 15min), adding 2.8kg of thickening agent, 1kg of binder and 1kg of pore-forming agent, and stirring uniformly (40rpm for 15min) to obtain mixed coating slurry, wherein the dispersing agent is alkylphenol ethoxylates, the thickening agent is CMC, the binder is SBR and the pore-forming agent is ethanol.
A hybrid coating slurry based separator comprising: the base film, cover the aluminium oxide coating on the base film one side and cover the thick liquids coating that scribbles in mixture on the aluminium oxide coating, the thickness of aluminium oxide coating is 2um, and the thickness of scribbling the thick liquids coating in mixture is 2um, and the base film is the PE base film.
A method of making a separator comprising: coating a layer of aluminum oxide on a base film, drying (75 ℃ for 2min) to form an aluminum oxide coating, coating mixed coating slurry, and keeping the temperature at 90 ℃ for 0.5min to form a PVDF coating. Wherein, the method for coating the mixed coating slurry is rotary spraying, the coating speed of the rotary spraying is 50m/min, and the rotor speed is 8000 rpm/min. The method for coating the aluminum oxide is micro gravure roll coating.
The properties of the separator obtained in comparative example 2 are shown in table 4.
TABLE 4
| Thickness of the diaphragm | um | 15.3 |
| Degree of air permeability | s/100ml | 183.5 |
| Areal density | g/m2 | 10.8 |
| Tensile Strength MD | kgf/cm2 | 1823.5 |
| Tensile Strength TD | kgf/cm2 | 1487.5 |
| Strength of needling | N | 6.2 |
| Shrinkage of 105 x 1 h% | MD/TD | 0.6/0.2 |
It can be seen from table 4 that the coating obtained in comparative example 2 has a smaller thickness, a higher air permeability and more normal other properties under the same spray conditions.
The diaphragms obtained in comparative examples 1 and 2 and examples 1-3 are respectively assembled into 5000mA soft package batteries. After standing for 7 days under the same conditions, the batteries were disassembled, the adhesion between the separator and the pole piece was tested, and the test results were shown in table 5. As can be seen from the data in table 5, the separator obtained according to the present invention has a greater thickness, better air permeability, and better adhesion.
TABLE 5
TABLE 6
The positive electrode material is lithium iron phosphate, the negative electrode material is graphite, the solvent of the electrolyte is EC/DMC/EMC 1:1 (mass ratio), the electrolyte is standard electrolyte with the solute of lithium hexafluorophosphate, the concentration of the lithium hexafluorophosphate in the electrolyte is 1mol/L, and the square battery is manufactured by a winding process. The 2.4Ah prismatic cell test results are shown in table 6. The data show that the capacity retention rate of example 1 after 422 cycles is higher than that of comparative example 1, and the surface example 1 has better cycle performance.
The invention has been described in an illustrative manner, and it is to be understood that any simple variations, modifications or other equivalent changes which can be made by one skilled in the art without departing from the spirit of the invention fall within the scope of the invention.
Claims (10)
1. The preparation method of the PVDF mixed coating slurry is characterized by comprising the following steps: adding 0.1-0.2 part by mass of a dispersing agent and 1-3 parts by mass of PVDF into 12-18 parts by mass of a dispersion medium, uniformly dispersing, sanding, adding 0.5-3 parts by mass of a thickening agent, 0.5-1 part by mass of a binder, 1 part by mass of a pore-forming agent and 1-2 parts by mass of a coating emulsion, and uniformly stirring to obtain the PVDF mixed coating slurry, wherein the dispersion medium is deionized water, the dispersing agent is a modified polyether polymer, fatty alcohols, sodium polyethylene glycol alkylaryl ether sulfonate, alkylphenol ethoxylates, polyoxyethylene alkylphenol ether or sodium polyacrylate, the thickening agent is PVA (polyvinyl alcohol), PEG (polyethylene glycol), PVP (polyvinylpyrrolidone) or CMC (sodium carboxymethylcellulose), the binder is polymethyl acrylate, SBR (styrene butadiene rubber) or xanthan gum, and the pore-forming agent is ethanol, sodium hydroxide, sodium, Ether, propanol, isopropanol or acetone, and the coating emulsion is at least one of polymethyl acrylate, polyethyl acrylate, alpha-cyano acrylate and styrene butadiene rubber.
2. The method of claim 1, wherein the sanding is performed at a speed of 500 to 1000RPM for 10 to 30 min.
3. PVDF dope obtained by the production method as defined in claim 1 or 2.
4. A diaphragm based on the PVDF mixed coating slurry as set forth in any one of claims 1-3, which is characterized by comprising: the coating comprises a base film, an aluminum oxide coating covering one side of the base film and a PVDF mixed coating slurry coating covering the aluminum oxide coating.
5. The separator according to claim 4, wherein the thickness of the alumina coating layer is 2-4 um, the thickness of the PVDF mixed coating slurry coating layer is 1-5 um, the base film is a PP film, a PE film or a composite film, and the composite film is a composite film of PP and PE.
6. The method for preparing a separator according to claim 4 or 5, comprising: and coating a layer of aluminum oxide on the base film, drying to form the aluminum oxide coating, coating the PVDF mixed coating slurry, and keeping the temperature at 60-90 ℃ for 0.3-0.5 min to form the PVDF mixed coating slurry coating.
7. The preparation method according to claim 6, wherein the PVDF mixed coating slurry is applied by rotary spraying, the coating speed of the rotary spraying is 40-50 m/min, and the rotor speed is 6000-8000 rpm/min; the method of coating the alumina is micro gravure roll coating.
8. The method according to claim 6, wherein the drying temperature is 35 to 85 ℃ and the drying time is 0.1 to 3.0 min.
9. Use of the PVDF mixed coating slurry as defined in claim 3 for improving the adhesion of a separator.
10. Use of the PVDF blend coating paste according to claim 3 for improving the battery capacity retention.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111613759A (en) * | 2020-05-27 | 2020-09-01 | 湖北亿纬动力有限公司 | Diaphragm slurry, preparation method thereof, diaphragm and lithium ion battery |
| CN112332028A (en) * | 2020-09-28 | 2021-02-05 | 河北金力新能源科技股份有限公司 | Functional lithium battery diaphragm slurry, functional lithium battery diaphragm and lithium battery |
| CN113540686A (en) * | 2020-04-20 | 2021-10-22 | 河北金力新能源科技股份有限公司 | Functional diaphragm for lithium-sulfur battery and preparation method thereof |
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