CN110838567A - PVDF (polyvinylidene fluoride) diaphragm slurry, preparation method thereof, diaphragm prepared from PVDF diaphragm slurry and battery cell - Google Patents
PVDF (polyvinylidene fluoride) diaphragm slurry, preparation method thereof, diaphragm prepared from PVDF diaphragm slurry and battery cell Download PDFInfo
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- CN110838567A CN110838567A CN201911024978.0A CN201911024978A CN110838567A CN 110838567 A CN110838567 A CN 110838567A CN 201911024978 A CN201911024978 A CN 201911024978A CN 110838567 A CN110838567 A CN 110838567A
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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
- 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
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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
- H01M50/449—Separators, membranes or diaphragms characterised by the material having a layered structure
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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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- Cell Separators (AREA)
Abstract
The invention discloses PVDF membrane slurry, which comprises the following components in percentage by mass (2-6): (2.5-3): 0.1: (0.8-1): (1.0-1.2): (17-23.36) high binding power emulsion, PVDF, dispersant, thickening agent, binder and deionized water. The diaphragm slurry is added with an additive with high adhesive force with a negative plate on the basis of PVDF slurry so as to improve the adhesive force between the diaphragm prepared from the diaphragm slurry and the negative plate. The diaphragm prepared by applying the diaphragm slurry has good adhesive force with the negative plate, and the prepared battery core is remarkably improved in fault phenomenon after being hot-pressed, so that the design requirement is met.
Description
Technical Field
The invention relates to the technical field of battery diaphragms, in particular to PVDF diaphragm slurry, a preparation method and a diaphragm and a battery cell prepared from the PVDF diaphragm slurry.
Background
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.
When the battery is shaped by hot pressing, the adhesive force between the PVDF coating and the positive plate is stronger. In contrast, the adhesion with the negative electrode sheet is poor. The phenomenon of cell middle fault is probabilistically caused in the preparation process of the battery, namely the phenomenon that the cell is not compacted. With the occurrence of the lamination process in a battery enterprise, the phenomenon of middle fault is easier to occur in the preparation of the battery.
Disclosure of Invention
The invention aims to provide PVDF diaphragm slurry aiming at the defect of poor adhesion between a PVDF coating and a negative plate in the prior art.
Another object of the present invention is to provide a method for preparing the PVDF separator slurry, which has simple steps and is suitable for industrial production.
The invention also aims to provide a diaphragm prepared from the PVDF diaphragm slurry, which has better adhesive force with a negative plate.
The invention also aims to provide the battery cell prepared by the diaphragm, and the battery cell is subjected to hot pressing, so that the fault phenomenon is better improved due to good adhesion between the diaphragm and a negative electrode, and the design requirement is met.
The technical scheme adopted for realizing the purpose of the invention is as follows:
a preparation method of PVDF membrane slurry comprises the following steps:
step 1: adding deionized water into the high-adhesion emulsion, and diluting to 10% of solid content to obtain a solution A;
step 2: adding PVDF and a dispersing agent into deionized water, and uniformly dispersing to obtain a solution B;
and step 3: uniformly mixing the solution A and the solution B, and then sanding to obtain a mixed solution;
and 4, step 4: and adding a thickening agent and a binder into the mixed solution, and uniformly dispersing to obtain the PVDF membrane slurry.
In the above technical solution, the sanding speed in step 3 is 500-1000RPM, and the time is 10-30 min.
In the technical scheme, the mass ratio of the high-adhesion emulsion, the PVDF, the dispersant, the thickening agent, the binder and the deionized water is (2-6): (2.5-3.0): 0.1: (0.8-1.0): (1.0-1.2): (17.00-23.36).
In the technical scheme, the high-adhesion emulsion is one or a mixture of polyacrylonitrile, epoxy resin and styrene butadiene rubber in any proportion;
the dispersing agent is one or a mixture of modified polyether polymer, fatty alcohol, polyethylene glycol alkyl aryl ether sodium sulfonate, alkylphenol polyethenoxy ether, polyoxyethylene alkyl phenol ether and sodium polyacrylate in any proportion;
the thickening agent is one or a mixture of PVA, PEG, PVP and CMC in any proportion;
the binder is one or a mixture of polymethyl acrylate and xanthan gum in any proportion.
The PVDF membrane slurry prepared by the preparation method is also another object of the invention.
Another object of the present invention is a separator comprising a base film and a PVDF coating layer coated on one side of the base film, wherein the PVDF coating layer is prepared by:
and coating the PVDF membrane slurry on one side of the base membrane by a rotary spraying process, and drying to obtain the PVDF coating.
In the technical scheme, the drying time is 1.5-2min, and the drying temperature is 55-75 ℃.
In the technical scheme, the thickness of the PVDF coating is 2-4 microns, and the thickness of the base film is 12 microns.
The transverse heat shrinkage rate is 0.1-0.5%, and the longitudinal heat shrinkage rate is 0.1-1.0%; the needling strength is 4.8-6.5N; the film breaking temperature is 140-160 ℃, and the breakdown voltage is 1000-2000V.
The invention also relates to application of the high-adhesion emulsion in PVDF (polyvinylidene fluoride) separator slurry, wherein the adhesion between a separator formed by the PVDF separator slurry and a negative plate is 30-100N/m units.
Another object of the present invention is a battery cell comprising a positive electrode, a negative electrode and the separator of claim 6, wherein the PVDF-coated side of the separator is opposite to the negative electrode sheet. Wherein the anode is a ternary material, and the cathode is a graphite material.
Compared with the prior art, the invention has the beneficial effects that:
1. the PVDF diaphragm slurry provided by the invention is added with high-adhesion emulsion which has high adhesion with a negative plate on the basis of the PVDF slurry so as to improve the adhesion between the diaphragm prepared from the PVDF diaphragm slurry and the negative plate.
2. The electric core prepared by the diaphragm provided by the invention is better improved in fault phenomenon after being hot-pressed, and meets the design requirements.
Drawings
FIG. 1 is an electron micrograph of PVDF membrane slurry in example 1.
Fig. 2 is an internal view of the cell obtained in comparative example 1.
Fig. 3 is a side view of the cell obtained in comparative example 1.
Fig. 4 is an internal view of the cell obtained in example 1.
Fig. 5 is a side view of a cell obtained in example 1.
Detailed Description
The present invention will be described in further detail with reference to specific examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Comparative example 1
3kg of PVDF and 0.1kg of modified polyether polymer were added to 23.36kg of deionized water, mixed and stirred for 2 hours to disperse the mixture uniformly, and then the mixture was sanded at 500RPM for 30 minutes. After sanding, sequentially adding 1.0kg of PVA and 1.2kg of polymethyl acrylate, and uniformly stirring to obtain the PVDF membrane slurry. And coating the PVDF diaphragm slurry on one side of a base film or a ceramic film by a rotary spraying process, and then drying the base film or the ceramic film in a 55-DEG C oven for 1.5min to form a 2-micrometer coating, thereby obtaining the diaphragm.
A battery cell comprising the separator of comparative example 1, wherein the side of the separator coated with the PVDF coating is opposite to a negative electrode sheet. As shown in fig. 2, the battery cell using the separator of comparative example 1 had poor adhesion between the separator and the negative electrode sheet after hot pressing. Fig. 3 is a side view of the battery core, and it can be seen that after hot pressing, due to poor adhesion between the separator and the negative plate, a fault exists in the middle of the winding core, and the design requirement is not met.
Example 1
This example added a high adhesion emulsion as compared to comparative example 1.
6kg of deionized water was added to 6kg of polyacrylonitrile to dilute the solution to obtain a solution A. To 17.36kg of deionized water, 3kg of PVDF and 0.1kg of modified polyether polymer were added, and the mixture was stirred for 2 hours to disperse the mixture uniformly, thereby obtaining a solution B. Stirring and mixing the A and the B, and sanding together after uniform mixing, wherein the sanding speed is 500RPM and the sanding time is 30 min. After sanding, 1.0kg of PVA and 1.2kg of polymethyl acrylate are sequentially added, and after uniform stirring, the No. 1 PVDF membrane slurry can be obtained, and an electron microscope image of the PVDF membrane slurry is shown in figure 1, wherein, the PVDF and the high-binding-force emulsion are mixed into a whole, and the compatibility is good.
And coating the PVDF diaphragm slurry on one side of a base film or a ceramic film by a rotary spraying process, and then drying the base film or the ceramic film in a 55-DEG C oven for 1.5min to form a 2-micrometer coating, thereby obtaining the No. 1 diaphragm.
Baking at 120 ℃ for 1 hour to obtain a No. 1 diaphragm with the transverse thermal shrinkage rate of 0.3 percent and the longitudinal thermal shrinkage rate of 0.8 percent; the needling strength is 5.5N; the film breaking temperature is 148 ℃, and the breakdown voltage is 1242V.
The peel strength was measured using a tensile machine (100 mm/min). The adhesion between the No. 1 separator and the negative electrode sheet was 50N/m units. The adhesion between the separator and the negative electrode sheet in the comparative example was 25N/m units.
A battery cell comprises a No. 1 diaphragm, wherein the positive electrode is made of a ternary material, the negative electrode is made of graphite, and one side of the diaphragm coated with a PVDF coating is opposite to a negative plate. Hot pressing parameters: 85 ℃, 0.3MPa, 60 s. As shown in fig. 3, the separator had adhered the graphite on the negative electrode sheet after hot pressing, indicating that the adhesion between the separator and the negative electrode sheet was good. Fig. 4 is a side view of the battery cell, and it can be seen that after hot pressing, due to good adhesion between the separator and the negative plate, no fault occurs after the battery cell is hot pressed, and the design requirements are met.
Example 2
4kg of deionized water was added to 4kg of epoxy resin to dilute the epoxy resin to obtain a solution A. 2.5kg of PVDF and 0.1kg of fatty alcohol were added to 15kg of deionized water, and the mixture was stirred for 2 hours to disperse the mixture uniformly, thereby obtaining a solution B. Stirring and mixing the A and the B, sanding the A and the B together after uniform mixing, wherein the sanding speed is 1000RPM, and the time is 20min. And stirring uniformly to obtain No. 2 PVDF membrane slurry.
And coating the PVDF spraying slurry on one side of a base film or a ceramic film by a rotary spraying process, and then, drying in a 65 ℃ oven for 2.0min to form a coating of 3um, thereby obtaining the No. 2 diaphragm.
Baking at 120 ℃ for 1 hour to obtain a No. 2 diaphragm with the transverse heat shrinkage rate of 0.4 percent and the longitudinal heat shrinkage rate of 1.0 percent; the needling strength is 5.3N; the film breaking temperature is 149 ℃, and the breakdown voltage is 1238V.
Example 3
2kg of deionized water was added to 2kg of styrene-butadiene rubber to dilute the solution to obtain a solution A. 2.5kg of PVDF and 0.1kg of sodium polyethylene glycol alkyl aryl ether sulfonate are added into 15kg of deionized water, and the mixture is mixed and stirred for 2 hours to be uniformly dispersed, so that a solution B is obtained. Stirring and mixing the A and the B, sanding the A and the B after uniform mixing, and then sequentially adding 0.8kg of CMC and 1.0kg of xanthan gum after sanding. And stirring uniformly to obtain No. 3 PVDF membrane slurry.
And coating the PVDF spraying slurry on one side of a base film or a ceramic film by a rotary spraying process, and then drying the base film or the ceramic film in a baking oven at 75 ℃ for 1.5min to form a coating of 4um, thereby obtaining the No. 3 diaphragm.
Baking at 120 ℃ for 1 hour to obtain a No. 3 diaphragm with the transverse thermal shrinkage rate of 0.4 percent and the longitudinal thermal shrinkage rate of 0.8 percent; the needling strength is 5.6N; the film breaking temperature is 148 ℃, and the breakdown voltage is 1251V.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The preparation method of the PVDF membrane slurry is characterized by comprising the following steps:
step 1: adding deionized water into the high-adhesion emulsion, and diluting to obtain a solution A;
step 2: adding PVDF and a dispersing agent into deionized water, and uniformly dispersing to obtain a solution B;
and step 3: uniformly mixing the solution A and the solution B, and then sanding to obtain a mixed solution;
and 4, step 4: and adding a thickening agent and a binder into the mixed solution, and uniformly dispersing to obtain the PVDF membrane slurry.
2. The method as claimed in claim 1, wherein the sanding speed in step (b) is 500-1000RPM for 10-30 min.
3. The preparation method according to claim 1, wherein the mass ratio of the high-binding-force emulsion to the PVDF to the dispersant to the thickener to the binder to the deionized water is (2-6): (2.5-3.0): 0.1: (0.8-1.0): (1.0-1.2): (17.00-23.36).
4. The method according to claim 1, wherein the reaction mixture,
the high-binding-force emulsion is one or a mixture of polyacrylonitrile, epoxy resin and styrene butadiene rubber in any proportion;
the dispersing agent is one or a mixture of modified polyether polymer, fatty alcohol, polyethylene glycol alkyl aryl ether sodium sulfonate, alkylphenol polyethenoxy ether, polyoxyethylene alkyl phenol ether and sodium polyacrylate in any proportion;
the thickening agent is one or a mixture of PVA, PEG, PVP and CMC in any proportion;
the binder is one or a mixture of polymethyl acrylate and xanthan gum in any proportion.
5. PVDF membrane slurry prepared by the preparation method according to any one of claims 1 to 4.
6. A separator comprising a base film and a PVDF coating layer coated on one side of the base film, wherein the PVDF coating layer is prepared by:
coating the PVDF membrane slurry as defined in claim 5 on one side of the base membrane by a rotary spraying process, and drying to obtain the PVDF coating.
7. The membrane of claim 6, wherein the drying time is 1.5-2min and the drying temperature is 55-75 ℃.
8. The separator of claim 6, wherein the PVDF coating has a thickness of 2-4 microns and the base film has a thickness of 5-16 um.
9. The application of the high-adhesion emulsion in PVDF (polyvinylidene fluoride) diaphragm slurry is characterized in that the adhesion between a diaphragm formed by the PVDF diaphragm slurry and a negative plate is 30-100N/m units.
10. A battery cell comprising a positive electrode, a negative electrode and the separator of claim 6, wherein the PVDF-coated side of the separator is opposite to the negative electrode sheet.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN111640901A (en) * | 2020-05-26 | 2020-09-08 | 湖南中锂新材料科技有限公司 | Preparation method of lithium ion battery diaphragm, lithium ion battery and preparation method thereof |
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 |
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CN111640901A (en) * | 2020-05-26 | 2020-09-08 | 湖南中锂新材料科技有限公司 | Preparation method of lithium ion battery diaphragm, lithium ion battery and preparation method thereof |
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 |
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