CN109244321B - Heat-resistant water-based coating for lithium battery diaphragm and preparation method and application thereof - Google Patents
Heat-resistant water-based coating for lithium battery diaphragm and preparation method and application thereof Download PDFInfo
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- CN109244321B CN109244321B CN201811085270.1A CN201811085270A CN109244321B CN 109244321 B CN109244321 B CN 109244321B CN 201811085270 A CN201811085270 A CN 201811085270A CN 109244321 B CN109244321 B CN 109244321B
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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
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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
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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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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/10—Energy storage using batteries
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Abstract
The invention discloses a heat-resistant water-based coating for a lithium battery diaphragm, which is a composite coating containing water-based PVDF spherical particles and a water-based high-temperature-resistant polymer; the mass ratio of the waterborne PVDF spherical particles to the waterborne high-temperature-resistant polymer is 80-90:3-7, and the particle size of the waterborne PVDF spherical particles is 100-300 nm. According to the invention, the aqueous high-temperature-resistant polymer can enter the inside of the micelle of the PVDF emulsion through the regulation and optimization of the three rotating speeds of low speed, high speed and low speed, so as to obtain uniform PVDF/high-temperature-resistant polymer composite slurry; the high-temperature-resistant polymer in the composite slurry is attached to the surface of each PVDF particle, so that the problem that the PVDF and the high-temperature-resistant adhesive are not uniformly distributed is solved; the heat-resistant water-based coating formed by coating the slurry on the polyolefin diaphragm substrate has extremely high uniformity, so that the electrochemical comprehensive performance and the high-temperature resistance of the heat-resistant water-based coating are well improved, and the high-temperature resistance and the battery cycle performance of the lithium battery diaphragm can be effectively improved.
Description
Technical Field
The invention belongs to the field of new energy materials, and particularly relates to a heat-resistant water-based coating for a lithium battery diaphragm, and a preparation method and application thereof.
Background
With the continuous development of electric automobiles, the performance of a lithium battery must be further improved to meet the requirements of the electric automobiles, the diaphragm serving as a barrier between a positive electrode and a negative electrode plays a crucial role in the performance of the lithium ion battery, the performance of the diaphragm directly influences the capacity and the cycle of the battery, particularly the important factor influencing the safety performance of the battery, and coating the surface of the diaphragm is an effective method for improving the safety of the diaphragm. Patent application No. CN201210000157.5 discloses a diaphragm, which is composed of a ceramic material layer coated on the surface of a base film and a polymer bonding layer coated on the outer surface of the ceramic layer, so that the heat resistance and the mechanical strength of the diaphragm are improved to a certain extent, but compared with the base film, the ventilation loss of the coated diaphragm is large, and the conduction of lithium ions is hindered; the internal resistance of the lithium battery is increased, and the thickness and the weight of the diaphragm are greatly increased.
The lithium ion battery diaphragm coated with the water-based PVDF (polyvinylidene fluoride) is prepared by coating a PVDF material on the surface of a traditional diaphragm through a special process. Compared with the traditional ceramic diaphragm, the air permeability loss is large, and the conduction of lithium ions is hindered; the internal resistance of the lithium battery is increased, the thickness and the weight of the diaphragm are greatly increased, the problems of effectively utilizing the space of the anode and cathode materials in the battery and the like are solved, the PVDF coating layer can be combined with the electrolyte in the lithium ion battery into a stable gel conductive polymer, and the performance of the lithium ion battery is obviously improved. The PVDF coating diaphragm can increase the cycle performance of the battery; the diaphragm and the pole piece are bonded, so that the hardness of the pole piece is high, the battery is thinner and firmer, and the processing and the transportation are convenient.
The conventional aqueous PVDF coating and the composite coating of the aqueous PVDF and the polymer or inorganic particles are simply stirred and mixed to obtain the coating slurry. For example, patent CN 106784532 a discloses a preparation method of composite coating of aqueous PVDF and its copolymer, which prepares aqueous coating slurry by blending aqueous PVDF and inorganic particles. Patent CN 105119000 a discloses an aqueous PVDF slurry for lithium ion batteries and a preparation method thereof, which uses mechanical agitation to disperse PVDF and a binder by using a large amount of auxiliaries. The technology plays a certain role in improving the cycle performance of the lithium battery, but the problem that the adhesives and PVDF particles are not uniformly distributed and the high-temperature-resistant adhesives and PVDF in the coating of the diaphragm are separated still exists.
Disclosure of Invention
The invention aims to solve the technical problem of providing the water-based coating for the heat-resistant lithium ion battery diaphragm and the preparation method thereof aiming at the defects in the prior art, solving the problem of uneven distribution of PVDF and a high-temperature-resistant adhesive, and well improving the electrochemical comprehensive performance and the high-temperature-resistant performance of the coating.
The technical scheme adopted by the invention for solving the problems is as follows:
a hot water-resistant coating for a lithium battery diaphragm is a composite coating consisting of water-based PVDF spherical particles and a water-based high-temperature-resistant polymer, wherein the mass ratio of the water-based PVDF spherical particles to the water-based high-temperature-resistant polymer is 80-90:3-7, and the particle size of the water-based PVDF spherical particles is 100-300 nm.
According to the scheme, the water-based high-temperature-resistant polymer is any one of non-water-based polyimide or water-based polytetrafluoroethylene.
The preparation method of the heat-resistant water-based coating for the lithium battery diaphragm comprises the steps of mixing polyvinylidene fluoride water-based emulsion and a water-based high-temperature-resistant polymer, and sequentially carrying out primary low-speed stirring, high-speed stirring and secondary low-speed stirring to obtain heat-resistant water-based coating slurry for the lithium battery diaphragm; and then, coating the heat-resistant water-based coating slurry for the lithium battery diaphragm on the surface of the polyolefin diaphragm base material in a blade coating, roller coating and spraying manner, and drying to form a heat-resistant water-based coating on the surface of the polyolefin diaphragm base material.
According to the scheme, the mass ratio of the polyvinylidene fluoride aqueous emulsion to the aqueous high-temperature-resistant resin is 80-90:3-7 in terms of effective solid content.
According to the scheme, the solid content of the polyvinylidene fluoride aqueous emulsion is 20-40%, and the contained aqueous PVDF powder is spherical particles with the particle size of 100-300 nm.
According to the scheme, any one of the commercially available models RC-10246, RC-10278, RC-10280, XPH-838, XPH-882, XPH-884 and the like can be selected as the polyvinylidene fluoride aqueous emulsion.
According to the scheme, the water-based high-temperature-resistant polymer is any one of commercially available models such as water-based polyimide YH-1066, PIW-015, RY-5002, water-based polytetrafluoroethylene D1610F, D2512F, DISP30 and TE 3893.
According to the scheme, the low-speed stirring range is 1000-1500rpm, the first low-speed stirring time is 30-40min, and the second low-speed stirring time is 20-30 min; the high-speed stirring speed range is 3000-.
The invention also provides a lithium battery diaphragm containing the hot water resistant coating, which consists of a polyolefin diaphragm base material and the hot water resistant coating coated on the surface of the polyolefin diaphragm base material. The preparation method of the lithium battery diaphragm comprises the following steps: the heat-resistant water-based coating slurry for the lithium battery diaphragm is coated on the surface of a polyolefin diaphragm base material in a blade coating, roller coating and spraying mode, and the lithium battery diaphragm containing the heat-resistant water-based coating is obtained after drying.
According to the scheme, the coating mode can be selected from knife coating, roller coating, spraying and the like.
According to the scheme, the drying temperature is 60-80 ℃, and the drying time is 5-30 s.
According to the scheme, the polyolefin diaphragm base material can be any one of a polyethylene diaphragm, a polypropylene diaphragm or a polyethylene-polypropylene composite diaphragm.
According to the scheme, the thickness of the hot water-resistant coating is 0.2-2 mu m.
Compared with the prior art, the invention has the beneficial effects that:
comprehensively considering the problem of uneven distribution of PVDF and adhesives in the traditional PVDF coating and the requirement of the safety performance of the diaphragm, the invention enables the water-based high-temperature-resistant polymer to enter the inside of the micelle of the PVDF emulsion by regulating and optimizing the three rotating speeds of low speed, high speed and low speed, thereby obtaining uniform PVDF/high-temperature-resistant polymer composite slurry; the high-temperature resistant polymer in the composite slurry is attached to the surface of each PVDF particle, so that the problem of uneven distribution of the PVDF and the high-temperature resistant adhesive is fundamentally solved; the hot water-resistant coating formed by coating the slurry on the polyolefin diaphragm substrate has extremely high uniformity, so that the electrochemical comprehensive performance and the high temperature resistance of the hot water-resistant coating are well improved. The heat-resistant water-based coating is applied to a lithium battery diaphragm coating, and can effectively improve the high temperature resistance and the battery cycle performance of the lithium battery diaphragm.
Drawings
FIG. 1 is an electron scanning micrograph (SEM image) of the apparent morphology of a hot water resistant coating (example 1) for a lithium ion battery separator according to the present invention.
Detailed Description
In order to better understand the present invention, the following examples are further provided to illustrate the present invention, but the present invention is not limited to the following examples.
Example 1
A preparation method of a lithium battery diaphragm with a heat-resistant water-based coating and a lithium battery diaphragm containing the heat-resistant water-based coating comprises the following specific steps:
(1) mixing polyvinylidene fluoride aqueous emulsion RC-10246 and aqueous polyimide YH-1066 according to the mass ratio of 80:3, stirring for 30min at the rotating speed of 1200rpm, uniformly mixing, stirring for 1h at the rotating speed of 3500rpm, and finally stirring for 20min at 1100rpm to obtain uniformly dispersed composite aqueous coating slurry;
(2) and coating the composite water-based coating slurry on the surface of a polypropylene diaphragm by adopting a blade coating method, drying for 18s at 70 ℃, and forming a 0.6um thick heat-resistant water-based coating for the lithium ion battery diaphragm on the surface of the polypropylene diaphragm to obtain the lithium battery diaphragm containing the heat-resistant water-based coating.
As can be seen from FIG. 1, the hot water-resistant coating for the lithium battery diaphragm, which is obtained by the invention, has high uniformity, and the aqueous PVDF and the adhesive are dispersed and uniformly mixed, so that the comprehensive performance of the diaphragm is favorably improved.
Example 2
A preparation method of a lithium battery diaphragm with a heat-resistant water-based coating and a lithium battery diaphragm containing the heat-resistant water-based coating comprises the following specific steps:
(1) mixing polyvinylidene fluoride aqueous emulsion RC-10280 and aqueous polytetrafluoroethylene D1610F according to the effective solid content mass ratio of 85:4, stirring for 40min at the rotating speed of 1100rpm, uniformly mixing, stirring for 2h at the rotating speed of 3800rpm, and finally stirring for 30min at 1000rpm to obtain uniformly dispersed composite aqueous coating slurry;
(2) and (3) coating the composite water-based coating slurry on the surface of a polyethylene diaphragm by adopting a spraying method, drying at 60 ℃ for 30s to form a 1-micron-thick heat-resistant water-based coating for the lithium ion battery diaphragm on the surface of the polyethylene diaphragm, and simultaneously obtaining the lithium battery diaphragm containing the heat-resistant water-based coating.
Example 3
A preparation method of a lithium battery diaphragm with a heat-resistant water-based coating and a lithium battery diaphragm containing the heat-resistant water-based coating comprises the following specific steps:
(1) mixing polyvinylidene fluoride water-based emulsion XPH-838 and water-based polyimide PIW-1066 according to an effective solid content mass ratio of 86:7, stirring for 45min at a rotating speed of 1300rpm, uniformly mixing, stirring for 1.5h at a rotating speed of 3600rpm, and finally stirring for 25min at 1200rpm to obtain uniformly dispersed composite water-based coating slurry;
(2) and (3) coating the composite water-based coating slurry on the surface of a polypropylene diaphragm by adopting a roller coating method, drying at 65 ℃ for 25s to form a 1.5 um-thick heat-resistant water-based coating for the lithium ion battery diaphragm on the surface of the polypropylene diaphragm, and simultaneously obtaining the lithium battery diaphragm containing the heat-resistant water-based coating.
Example 4
A preparation method of a lithium battery diaphragm with a heat-resistant water-based coating and a lithium battery diaphragm containing the heat-resistant water-based coating comprises the following specific steps:
(1) mixing polyvinylidene fluoride aqueous emulsion RC-10278 and aqueous polytetrafluoroethylene DISP30 according to the effective solid content mass ratio of 90:5, stirring at 1400rpm for 35min, then stirring at 4000rpm for 0.5h, and finally stirring at 1300rpm for 30min to obtain uniformly dispersed composite aqueous coating slurry;
(2) and (3) coating the composite water-based coating slurry on the surface of the polyethylene diaphragm by adopting a spraying method, drying at 75 ℃ for 10s to form a 2 um-thick heat-resistant water-based coating for the lithium ion battery diaphragm on the surface of the polyethylene diaphragm, and simultaneously obtaining the lithium battery diaphragm containing the heat-resistant water-based coating.
Example 5
A preparation method of a lithium battery diaphragm with a heat-resistant water-based coating and a lithium battery diaphragm containing the heat-resistant water-based coating comprises the following specific steps:
(1) mixing the polyvinylidene fluoride water-based emulsion XPH-884 and the water-based polyimide RY-5002 according to the effective solid content mass ratio of 88:3, stirring for 30min at the rotating speed of 1500rpm, uniformly mixing, stirring for 1h at the rotating speed of 3700rpm, and finally stirring for 25min at 1400rpm to obtain uniformly dispersed composite water-based coating slurry;
(2) and coating the composite water-based coating slurry on the surface of a polypropylene diaphragm by adopting a blade coating method, drying at 60 ℃ for 30s to form a 0.8-micrometer-thick heat-resistant water-based coating for the lithium ion battery diaphragm on the surface of the polypropylene diaphragm, and simultaneously obtaining the lithium battery diaphragm containing the heat-resistant water-based coating.
Comparative example 1
The comparative example is a polypropylene diaphragm coated with slurry prepared by blending XPH-838 aqueous PVDF emulsion and commercial polyvinyl alcohol adhesive at 1200rpm for 30min, 3500rpm for 1.2h and 1000rpm for 20 min.
Comparative example 2
The comparative example is a slurry coated polypropylene membrane prepared by blending XPH-838 aqueous PVDF emulsion and aqueous polyimide PIW-1066 adhesive for 1.5h at a high speed of 3750 rpm.
Comparative example 3
This comparative example was a slurry coated polyethylene separator prepared by blending an XPH-838 aqueous PVDF emulsion, aqueous polytetrafluoroethylene D1610F binder, only at a low speed of 1350rpm for 1.5 hours.
Performance test 1
The performance tests were performed on the separators prepared in examples 1 to 5 and comparative example, respectively, and the obtained data are recorded in table 1.
TABLE 1
From a comparison of table 1 we can find that: compared with the diaphragm coated by PVDF aqueous slurry containing the traditional aqueous adhesive in the comparative example 1, the invention forms the heat-resistant aqueous coating for the lithium ion battery diaphragm on the surface of the polypropylene diaphragm, so that the thermal shrinkage performance of the diaphragm is greatly improved, the short-circuit temperature is increased to more than 300 ℃, and the safety performance of the battery is greatly improved. In addition, comparative examples 2 and 3 only adopt single low-speed or high-speed stirring, so that the binder molecules and the aqueous PVDF particles in the slurry are in different liquid phases in the blending process, and the molecular-level mixing cannot be realized; the invention can realize that the adhesive molecules enter PVDF particle micelles and form stable composite emulsion by regulating and optimizing the low-speed, high-speed and low-speed triple rate, thoroughly solves the problems that the adhesive and PVDF are not uniformly dispersed and the adhesive and PVDF are separated after being heated, and improves the performances of the diaphragm such as air permeability, particle conductivity, short-circuit temperature and the like.
Performance test 2
The separators prepared in example 1 and example 4, comparative example 2 and comparative example 3 were respectively used to prepare button cells from lithium iron phosphate positive plates and graphite negative electrodes, and the electrical properties thereof were examined. The investigation result is as follows: under the constant current condition of 1C, after the battery is circularly charged and discharged for 400 times, the battery retention rates of the embodiment 1 and the embodiment 4 are as follows: 96.4% and 95.7%; comparative examples 1 and 2 are: 92.8% and 93.6%. It can be seen that the lithium battery assembled with the separator including the hot water resistant coating layer according to the present invention has stable performance.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, many modifications and changes can be made without departing from the inventive concept of the present invention, and these modifications and changes are within the protection scope of the present invention.
Claims (7)
1. A lithium battery separator is with heat-resisting waterborne coating which characterized in that: the composite coating comprises water-based PVDF spherical particles and a water-based high-temperature-resistant polymer; the mass ratio of the waterborne PVDF spherical particles to the waterborne high-temperature-resistant polymer is 80-90:3-7, and the particle size of the waterborne PVDF spherical particles is 100-300 nm;
the heat-resistant water-based coating for the lithium battery diaphragm is formed by coating PVDF/high-temperature-resistant polymer composite slurry on the surface of a polyolefin diaphragm base material, and the thickness of the coating is 0.2-2 mu m; in the PVDF/high-temperature-resistant polymer composite slurry, the water-based high-temperature-resistant polymer enters the inside of a micelle of the PVDF emulsion, and the high-temperature-resistant polymer is attached to the surface of each PVDF particle;
the water-based high-temperature-resistant polymer is any one of water-based polyimide or water-based polytetrafluoroethylene;
the preparation method of the PVDF/high-temperature-resistant polymer composite slurry comprises the following steps: mixing polyvinylidene fluoride aqueous emulsion and aqueous high-temperature-resistant polymer, and sequentially carrying out primary low-speed stirring, high-speed stirring and secondary low-speed stirring to obtain heat-resistant aqueous coating slurry for a lithium battery diaphragm, namely PVDF/high-temperature-resistant polymer composite slurry; wherein the low-speed stirring speed range is 1000-1500rpm, the first low-speed stirring time is 30-40min, and the second low-speed stirring time is 20-30 min; the high-speed stirring speed range is 3000-.
2. The heat-resistant water-based coating layer for a lithium battery separator according to claim 1, wherein: the solid content of the polyvinylidene fluoride aqueous emulsion is 20-40%.
3. The heat-resistant water-based coating layer for a lithium battery separator according to claim 2, characterized in that: the polyvinylidene fluoride aqueous emulsion is selected from any one of models RC-10246, RC-10278, RC-10280, XPH-838, XPH-882 and XPH-884; the water-based high-temperature resistant polymer is any one of water-based polyimides YH-1066, PIW-015, RY-5002, water-based polytetrafluoroethylene D1610F, D2512F, DISP30 and TE 3893.
4. The method for preparing a hot water resistant coating for a lithium battery separator as claimed in claim 1, wherein: coating the heat-resistant water-based coating slurry for the lithium battery diaphragm on the surface of the polyolefin diaphragm base material in a blade coating, roller coating and spraying manner, and drying to form a heat-resistant water-based coating on the surface of the polyolefin diaphragm base material, namely the heat-resistant water-based coating for the lithium battery diaphragm.
5. A lithium battery separator comprising the hot water resistant coating layer according to claim 1, wherein: the polyolefin membrane is composed of a polyolefin membrane substrate and the heat-resistant water-based coating of claim 1 coated on the surface of the polyolefin membrane substrate; the thickness of the hot water resistant coating is 0.2-2 μm.
6. The method for preparing a lithium battery separator as claimed in claim 5, wherein: coating the slurry of the heat-resistant water-based coating for the lithium battery separator according to claim 1 on the surface of the polyolefin separator substrate in a blade coating, roll coating and spraying manner, and drying to obtain the lithium battery separator containing the heat-resistant water-based coating.
7. The method for preparing a lithium battery separator according to claim 6, wherein: the polyolefin diaphragm base material is selected from any one of a polyethylene diaphragm, a polypropylene diaphragm or a polyethylene-polypropylene composite diaphragm; the drying temperature is 60-80 deg.C, and the drying time is 5-30 s.
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| CN111525074A (en) * | 2020-03-25 | 2020-08-11 | 河北金力新能源科技股份有限公司 | PTFE-PVDF (polytetrafluoroethylene-polyvinylidene fluoride) blended and sprayed lithium battery diaphragm and preparation method thereof |
| CN112226182B (en) * | 2020-08-24 | 2023-02-10 | 湖北亿纬动力有限公司 | Water-based binder, preparation method, gluing diaphragm, preparation method and lithium ion secondary battery |
| CN113644378B (en) * | 2021-08-10 | 2023-05-09 | 深圳市鼎泰祥新能源科技有限公司 | Functional coating diaphragm and preparation method and application thereof |
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Denomination of invention: A heat-resistant water-resistant coating for lithium battery diaphragm and its preparation method and Application Effective date of registration: 20220622 Granted publication date: 20211001 Pledgee: Bank of China Limited Wuhan Jianghan sub branch Pledgor: HUIQIANG (WUHAN) NEW ENERGY MATERIAL TECHNOLOGY CO.,LTD. Registration number: Y2022420000176 |
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