CN114597584B - Lithium ion battery diaphragm with charging protection function and preparation method thereof - Google Patents
Lithium ion battery diaphragm with charging protection function and preparation method thereof Download PDFInfo
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- CN114597584B CN114597584B CN202210293232.5A CN202210293232A CN114597584B CN 114597584 B CN114597584 B CN 114597584B CN 202210293232 A CN202210293232 A CN 202210293232A CN 114597584 B CN114597584 B CN 114597584B
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- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000000576 coating method Methods 0.000 claims abstract description 159
- 239000011248 coating agent Substances 0.000 claims abstract description 158
- 239000011230 binding agent Substances 0.000 claims abstract description 60
- 239000003960 organic solvent Substances 0.000 claims abstract description 58
- 239000002994 raw material Substances 0.000 claims abstract description 50
- 239000010954 inorganic particle Substances 0.000 claims abstract description 44
- 239000002270 dispersing agent Substances 0.000 claims abstract description 33
- 239000003063 flame retardant Substances 0.000 claims abstract description 26
- 239000004952 Polyamide Substances 0.000 claims abstract description 21
- 229920002647 polyamide Polymers 0.000 claims abstract description 21
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 claims abstract description 20
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 16
- LXIZRZRTWSDLKK-UHFFFAOYSA-N 1,3-dibromo-5-[2-[3,5-dibromo-4-(2,3-dibromopropoxy)phenyl]propan-2-yl]-2-(2,3-dibromopropoxy)benzene Chemical compound C=1C(Br)=C(OCC(Br)CBr)C(Br)=CC=1C(C)(C)C1=CC(Br)=C(OCC(Br)CBr)C(Br)=C1 LXIZRZRTWSDLKK-UHFFFAOYSA-N 0.000 claims abstract description 4
- RVHUMFJSCJBNGS-UHFFFAOYSA-N 2-[2,6-dibromo-4-[2-[3,5-dibromo-4-(2-hydroxyethoxy)phenyl]propan-2-yl]phenoxy]ethanol Chemical compound C=1C(Br)=C(OCCO)C(Br)=CC=1C(C)(C)C1=CC(Br)=C(OCCO)C(Br)=C1 RVHUMFJSCJBNGS-UHFFFAOYSA-N 0.000 claims abstract description 4
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 claims abstract description 4
- VEORPZCZECFIRK-UHFFFAOYSA-N 3,3',5,5'-tetrabromobisphenol A Chemical group C=1C(Br)=C(O)C(Br)=CC=1C(C)(C)C1=CC(Br)=C(O)C(Br)=C1 VEORPZCZECFIRK-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000000155 melt Substances 0.000 claims abstract description 3
- 239000011267 electrode slurry Substances 0.000 claims description 73
- 238000003756 stirring Methods 0.000 claims description 43
- 238000002156 mixing Methods 0.000 claims description 31
- 238000000034 method Methods 0.000 claims description 27
- 238000001035 drying Methods 0.000 claims description 21
- 238000000605 extraction Methods 0.000 claims description 20
- PHTQWCKDNZKARW-UHFFFAOYSA-N isoamylol Chemical group CC(C)CCO PHTQWCKDNZKARW-UHFFFAOYSA-N 0.000 claims description 16
- 239000000843 powder Substances 0.000 claims description 14
- 229920003048 styrene butadiene rubber Polymers 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000007756 gravure coating Methods 0.000 claims description 8
- 239000002033 PVDF binder Substances 0.000 claims description 6
- 229920002401 polyacrylamide Polymers 0.000 claims description 6
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 6
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 4
- 229920002319 Poly(methyl acrylate) Polymers 0.000 claims description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 4
- 229910001593 boehmite Inorganic materials 0.000 claims description 4
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 4
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 claims description 4
- 150000002191 fatty alcohols Chemical class 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 229920003366 poly(p-phenylene terephthalamide) Polymers 0.000 claims description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 2
- 229920003190 poly( p-benzamide) Polymers 0.000 claims description 2
- 229920000889 poly(m-phenylene isophthalamide) Polymers 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- MHSKRLJMQQNJNC-UHFFFAOYSA-N terephthalamide Chemical compound NC(=O)C1=CC=C(C(N)=O)C=C1 MHSKRLJMQQNJNC-UHFFFAOYSA-N 0.000 claims description 2
- 239000011247 coating layer Substances 0.000 claims 1
- 230000003647 oxidation Effects 0.000 abstract description 8
- 238000007254 oxidation reaction Methods 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 5
- 239000002002 slurry Substances 0.000 abstract description 5
- 229920000642 polymer Polymers 0.000 abstract description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 15
- 229910052744 lithium Inorganic materials 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 9
- 239000003795 chemical substances by application Substances 0.000 description 6
- 239000002174 Styrene-butadiene Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 239000000243 solution Substances 0.000 description 4
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 102000004310 Ion Channels Human genes 0.000 description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000007773 negative electrode material Substances 0.000 description 2
- 238000009783 overcharge test Methods 0.000 description 2
- 239000007774 positive electrode material Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 description 2
- 235000011152 sodium sulphate Nutrition 0.000 description 2
- 230000001960 triggered effect Effects 0.000 description 2
- YCGKJPVUGMBDDS-UHFFFAOYSA-N 3-(6-azabicyclo[3.1.1]hepta-1(7),2,4-triene-6-carbonyl)benzamide Chemical compound NC(=O)C1=CC=CC(C(=O)N2C=3C=C2C=CC=3)=C1 YCGKJPVUGMBDDS-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical group [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910013870 LiPF 6 Inorganic materials 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical group [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- MTAZNLWOLGHBHU-UHFFFAOYSA-N butadiene-styrene rubber Chemical compound C=CC=C.C=CC1=CC=CC=C1 MTAZNLWOLGHBHU-UHFFFAOYSA-N 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 210000004027 cell Anatomy 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000006255 coating slurry Substances 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 210000001787 dendrite Anatomy 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 125000000373 fatty alcohol group Chemical group 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000004816 latex Substances 0.000 description 1
- 229920000126 latex Polymers 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- -1 polyethylene Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000011115 styrene butadiene Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Classifications
-
- 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
-
- 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
-
- 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
- H01M50/414—Synthetic resins, e.g. thermoplastics or thermosetting resins
- H01M50/423—Polyamide resins
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Secondary Cells (AREA)
- Cell Separators (AREA)
Abstract
The invention discloses a lithium ion battery diaphragm with a charging protection function and a preparation method thereof, wherein the lithium ion battery diaphragm comprises: the positive electrode coating is coated on one surface of the base film corresponding to the positive electrode, and the negative electrode coating is coated on one surface of the base film corresponding to the negative electrode, wherein the raw materials for forming the positive electrode coating comprise: organic solvents, binders and polyamides; the raw materials for forming the anode coating comprise: inorganic particles, binders, molten flame retardants, dispersants and organic solvents; the melt flame retardant is tetrabromobisphenol A bis (allyl) ether, tetrabromobisphenol A bis (2-hydroxyethyl) ether or tetrabromobisphenol A bis (2, 3-dibromopropyl) ether. The invention coats polymer slurry with oxidation resistance on the positive electrode, solves the problem of strong oxidation effect on the isolating film caused by collapse of the positive electrode structure, coats slurry combining inorganic particles and a molten flame retardant on the negative electrode.
Description
Technical Field
The invention belongs to the technical field of battery diaphragms, and particularly relates to a lithium ion battery diaphragm with a charging protection function and a preparation method thereof.
Background
For the charging problem of lithium ion batteries, some battery manufacturers avoid potential safety hazards by adding an explosion-proof safety valve and a safety helmet, but the above methods do not thoroughly solve the fundamental problem of battery charging. The separator is one of materials in the lithium battery, is a transfer station in the charging process of the lithium ion battery, and the important position of the separator is that when the lithium battery is overcharged, lithium ions in the positive electrode excessively deviate, so that the positive electrode structure collapses, the unstable structure enables the positive electrode structure to be in a strong oxidation state, a strong oxidation effect is generated on the isolating film, meanwhile, lithium ions deviate from the positive electrode to be greatly separated out on the surface of the negative electrode to form lithium dendrites, challenges are initiated on the mechanical strength of the separator, and the two processes are accompanied by a large amount of Joule heat, finally, the isolating film is triggered to shrink, melt to generate internal short circuit, and the thermal failure of the battery core is completely triggered.
Today, most solutions to the above problems are to reinforce the mechanical properties and stability of the separator by coating the separator with an inorganic coating, but the solutions have more problems such as: the inoxidizability of the inorganic coating is relatively weak, and when the lithium battery is extremely overcharged, the inorganic coating is oxidized and powder is dropped in the electrolyte, so that the impedance of the lithium battery is increased; secondly, when overcharging, a large amount of heat is generated in the battery, even if the inorganic separator does not shrink, the capacity is continuously increased during overcharging, the voltage is correspondingly increased, and finally, the heat generated by the reaction of the anode and the cathode with the electrolyte is overlarge, and the battery catches fire and even explodes.
In view of the current situation, if a functional coating separator capable of solving the above problems can be developed, the solution of the charge protection problem of the lithium ion battery will advance by a large step.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide the lithium ion battery diaphragm with the charging protection function, which can solve the problems that an inorganic coating is oxidized and powder falls in the overcharging process, and strengthen the oxidation resistance and the stability of the diaphragm facing the positive electrode surface; the problem that the conventional inorganic coating cannot terminate the reaction process under the condition of original characteristics can be avoided, the charging process can be thoroughly cut off, and the overcharge-resistant protection function is enhanced.
The invention also aims to provide a preparation method of the lithium ion battery separator with the charging protection function.
The aim of the invention is achieved by the following technical scheme.
A lithium ion battery separator with charge protection function, comprising: a base film, a positive electrode coating coated on one surface of the base film corresponding to the positive electrode, and a negative electrode coating coated on one surface of the base film corresponding to the negative electrode,
the raw materials for forming the positive electrode coating comprise: organic solvents, binders and polyamides;
the raw materials for forming the negative electrode coating comprise: inorganic particles, binders, molten flame retardants, dispersants and organic solvents;
the organic solvent is at least one of acetone, N-methyl pyrrolidone and ethanol;
the polyamide is one or a mixture of more of poly (paraphenylene terephthalamide), poly (m-phenylene isophthalamide), poly (p-benzamide) and poly (p-phenylene terephthalamide);
the inorganic particles are alumina powder, aluminum nitride powder or boehmite powder;
the melt flame retardant is tetrabromobisphenol A bis (allyl) ether, tetrabromobisphenol A bis (2-hydroxyethyl) ether or tetrabromobisphenol A bis (2, 3-dibromopropyl) ether.
In the above technical scheme, the thickness of the positive electrode coating is 1.0-1.5 μm.
In the technical scheme, the thickness of the negative electrode coating is 1.0-1.5 mu m.
In the technical scheme, the dispersing agent is polyacrylamide or fatty alcohol ether sodium sulfate.
In the above technical solution, the binder is polyvinylidene fluoride, polymethyl acrylate or SBR (styrene butadiene rubber).
In the above technical scheme, in the raw materials for forming the positive electrode coating, the ratio of the organic solvent, the binder and the polyamide is (10-20) in parts by weight: (1.5-3): (2-4.2); in the raw materials for forming the anode coating, the ratio of inorganic particles, a binder, a molten flame retardant, a dispersing agent and an organic solvent is (1.8-3.5) in parts by mass: (1.8-3.2): (0.8-1.5): (0.35-0.8): (12-22).
The preparation method of the lithium ion battery diaphragm with the charging protection function comprises the following steps:
and coating positive electrode slurry on the surface of the base film opposite to the positive electrode to form the positive electrode coating, and coating negative electrode slurry on the surface of the base film opposite to the negative electrode to form the negative electrode coating, wherein the positive electrode slurry is formed by mixing raw materials for forming the positive electrode coating, and the negative electrode slurry is formed by mixing raw materials for forming the negative electrode coating.
In the technical scheme, the coating speed is 10-25 m/min, and the coating mode is gravure coating.
In the technical scheme, extraction is carried out after coating, the extractant is 3-methyl-1-butanol, and the extraction time is 15-25 min.
In the technical scheme, the extraction is followed by drying, and the drying temperature is 55-70 ℃.
In the above technical scheme, the method for preparing the positive electrode slurry comprises the following steps: mixing the organic solvent and the binder, stirring at 1300-2000 rpm for 35-55 min to uniformity, adding the polyamide, and stirring at 1200-1800 rpm for 35-50 min to uniformity; the method for preparing the negative electrode slurry comprises the following steps: mixing an organic solvent, a dispersing agent and a binder, stirring at 1400-2000 rpm for 40-60 min to uniformity, adding the inorganic particles, stirring at 1200-1800 rpm for 35-50 min to uniformity, adding a molten flame retardant, and stirring at 1300-2000 rpm for 40-55 min to uniformity.
The invention respectively faces different polar surfaces of the lithium battery by coating two different kinds of coating slurries. The polymer slurry with oxidation resistance is coated on the positive electrode, the problem that the positive electrode structure collapses and has strong oxidation effect on the isolating film is solved, the slurry with inorganic particles and molten flame retardant combined is coated on the negative electrode, the slurry has flame retardant effect and strong mechanical strength, and the molten flame retardant can be molten and absorbed into ceramic particles and micropores of a diaphragm matrix under high-temperature overcharging to achieve the function of breaking circuit, and thoroughly cuts off a lithium ion channel under the condition of overcharging of the battery to achieve the effect of safety protection.
Drawings
FIG. 1 is an SEM image of a positive electrode coating of example 1;
fig. 2 is an SEM image of the negative electrode coating in example 1.
Detailed Description
The technical scheme of the invention is further described below with reference to specific embodiments.
The base film used in the following examples and comparative examples was a polyethylene-based film having a thickness of 12. Mu.m.
Example 1
A lithium ion battery separator with charge protection function, comprising: the base film, the positive electrode coating coated on one surface of the base film corresponding to the positive electrode and the negative electrode coating coated on one surface of the base film corresponding to the negative electrode, wherein the thickness of the positive electrode coating is 1 mu m, the thickness of the negative electrode coating is 1 mu m,
the raw materials for forming the positive electrode coating comprise: organic solvents, binders and polyamides;
the raw materials for forming the anode coating comprise: inorganic particles, binders, molten flame retardants, dispersants and organic solvents;
the organic solvent is acetone;
the polyamide is poly (p-phenylene terephthalamide);
the inorganic particles are alumina powder;
the melting flame retardant is tetrabromobisphenol A bis (allyl) ether, the dispersing agent is polyacrylamide, and the binder is polyvinylidene fluoride.
In the raw materials for forming the positive electrode coating, the ratio of the organic solvent to the binder to the polyamide is 12:2:2.5; in the raw materials for forming the anode coating, the ratio of inorganic particles, a binder, a molten flame retardant, a dispersing agent and an organic solvent is 2.5:2.5:0.8:0.35:13.
the preparation method of the lithium ion battery diaphragm with the charging protection function comprises the following steps:
coating positive electrode slurry on the surface of the base film opposite to the positive electrode to form a positive electrode coating, wherein the SEM of the positive electrode coating is shown in figure 1, standing for 10min at normal temperature, coating negative electrode slurry on the surface of the base film opposite to the negative electrode to form a negative electrode coating, and SEM of the negative electrode coating is shown in figure 2, wherein the positive electrode slurry is formed by mixing raw materials for forming the positive electrode coating, the negative electrode slurry is formed by mixing raw materials for forming the negative electrode coating, the coating speed is 10m/min, the coating mode is gravure coating, extraction is carried out after the coating of both the positive electrode slurry and the negative electrode slurry is completed, the extracting agent is 3-methyl-1-butanol, the extraction time is 15min, drying is carried out after the extraction, and the drying temperature is 55 ℃ and the drying time is 20min.
The method for preparing the positive electrode slurry comprises the following steps: mixing the organic solvent and the binder in a stirring tank, stirring at 1500rpm for 40min to uniformity, adding polyamide, and stirring at 1300rpm for 35min to uniformity; the method for preparing the negative electrode slurry comprises the following steps: mixing an organic solvent, a dispersing agent and a binder in a stirring tank, stirring at 1400rpm for 40min to uniformity, adding inorganic particles, stirring at 1400rpm for 35min to uniformity, adding a molten flame retardant, and stirring at 1500rpm for 40min to uniformity.
Example 2
A lithium ion battery separator with charge protection function, comprising: the base film, the positive electrode coating coated on one surface of the base film corresponding to the positive electrode and the negative electrode coating coated on one surface of the base film corresponding to the negative electrode, wherein the thickness of the positive electrode coating is 1.2 mu m, the thickness of the negative electrode coating is 1.3 mu m,
the raw materials for forming the positive electrode coating comprise: organic solvents, binders and polyamides;
the raw materials for forming the anode coating comprise: inorganic particles, binders, molten flame retardants, dispersants and organic solvents;
the organic solvent is N-methyl pyrrolidone;
the polyamide is poly m-phenylene isophthalamide;
the inorganic particles are aluminum nitride powder;
the melting flame retardant is tetrabromobisphenol A bis (2-hydroxyethyl) ether, the dispersing agent is fatty alcohol ether sodium sulfate, and the binder is polymethyl acrylate.
In the raw materials for forming the positive electrode coating, the ratio of the organic solvent to the binder to the polyamide is 13:2.5:3, a step of; in the raw materials for forming the anode coating, the ratio of inorganic particles, a binder, a molten flame retardant, a dispersing agent and an organic solvent is 2.8:2.7:1:0.4:14.
the preparation method of the lithium ion battery diaphragm with the charging protection function comprises the following steps:
coating positive electrode slurry on one surface of a base film opposite to a positive electrode to form a positive electrode coating, standing at normal temperature for 10min, coating negative electrode slurry on one surface of the base film opposite to a negative electrode to form a negative electrode coating, wherein the positive electrode slurry is formed by mixing raw materials for forming the positive electrode coating, the negative electrode slurry is formed by mixing raw materials for forming the negative electrode coating, the coating speed of the positive electrode slurry is 15m/min, the coating speed of the negative electrode slurry is 17m/min, the coating mode is gravure coating, extraction is carried out after the coating of both the positive electrode slurry and the negative electrode slurry is completed, the extracting agent is 3-methyl-1-butanol, the extracting time is 20min, drying is carried out after the extraction, the drying temperature is 60 ℃, and the drying time is 23min.
The method for preparing the positive electrode slurry comprises the following steps: mixing the organic solvent and the binder in a stirring tank, stirring at 1600rpm for 45min to uniformity, adding the polyamide, and stirring at 1400rpm for 40min to uniformity; the method for preparing the negative electrode slurry comprises the following steps: mixing an organic solvent, a dispersing agent and a binder in a stirring tank, stirring at 1500rpm for 45min to uniformity, adding inorganic particles, stirring at 1500rpm for 40min to uniformity, adding a molten flame retardant, and stirring at 1600rpm for 45min to uniformity.
Example 3
A lithium ion battery separator with charge protection function, comprising: the base film, the positive electrode coating coated on one surface of the base film corresponding to the positive electrode and the negative electrode coating coated on one surface of the base film corresponding to the negative electrode, wherein the thickness of the positive electrode coating is 1.5 mu m, the thickness of the negative electrode coating is 1.5 mu m,
the raw materials for forming the positive electrode coating comprise: organic solvents, binders and polyamides;
the raw materials for forming the anode coating comprise: inorganic particles, binders, molten flame retardants, dispersants and organic solvents;
the organic solvent is ethanol;
the polyamide is poly-p-benzamide;
the inorganic particles are boehmite powder;
the melting flame retardant is tetrabromobisphenol A bis (2, 3-dibromopropyl) ether, the dispersing agent is polyacrylamide, and the binder is SBR (styrene butadiene rubber).
In the raw materials for forming the positive electrode coating, the ratio of the organic solvent to the binder to the polyamide is 14:3:3.2; in the raw materials for forming the anode coating, the ratio of inorganic particles, a binder, a molten flame retardant, a dispersing agent and an organic solvent is 3.2:2.9:1.2:0.45:15.
the preparation method of the lithium ion battery diaphragm with the charging protection function comprises the following steps:
coating positive electrode slurry on one surface of a base film opposite to a positive electrode to form a positive electrode coating, standing at normal temperature for 10min, coating negative electrode slurry on one surface of the base film opposite to a negative electrode to form a negative electrode coating, wherein the positive electrode slurry is formed by mixing raw materials for forming the positive electrode coating, the negative electrode slurry is formed by mixing raw materials for forming the negative electrode coating, the coating speed is 20m/min, the coating mode is gravure coating, extraction is carried out after the coating of both the positive electrode slurry and the negative electrode slurry is completed, the extracting agent is 3-methyl-1-butanol, the extracting time is 25min, drying is carried out after the extraction, and the drying temperature is 65 ℃ and the drying time is 25min.
The method for preparing the positive electrode slurry comprises the following steps: mixing the organic solvent and the binder in a stirring tank, stirring at 1700rpm for 50min to uniformity, adding the polyamide, and stirring at 1500rpm for 45min to uniformity; the method for preparing the negative electrode slurry comprises the following steps: mixing an organic solvent, a dispersing agent and a binder in a stirring tank, stirring at a speed of 1600rpm for 50min to uniformity, adding inorganic particles, stirring at a speed of 1600rpm for 45min to uniformity, adding a molten flame retardant, and stirring at a speed of 1700rpm for 50min to uniformity.
Comparative example 1
A lithium ion battery separator comprising: the base film, the positive electrode coating coated on one surface of the base film corresponding to the positive electrode and the negative electrode coating coated on one surface of the base film corresponding to the negative electrode, wherein the thickness of the positive electrode coating is 1 mu m, the thickness of the negative electrode coating is 1 mu m,
the raw materials for forming the positive electrode coating comprise: organic solvents, binders and inorganic particles;
the raw materials for forming the anode coating comprise: inorganic particles, a binder, a dispersant and an organic solvent;
the organic solvent is acetone;
the inorganic particles are alumina powder;
the dispersing agent is polyacrylamide, and the binder is polyvinylidene fluoride.
In the raw materials for forming the positive electrode coating, the ratio of the organic solvent, the binder and the inorganic particles is 12:2:2.5; in the raw materials for forming the anode coating, the ratio of the inorganic particles, the binder, the dispersant and the organic solvent is 2.5 in parts by mass: 2.5:0.35:13.
the preparation method of the lithium ion battery diaphragm comprises the following steps:
coating positive electrode slurry on one surface of a base film opposite to a positive electrode to form a positive electrode coating, standing at normal temperature for 10min, coating negative electrode slurry on one surface of the base film opposite to a negative electrode to form a negative electrode coating, wherein the positive electrode slurry is formed by mixing raw materials for forming the positive electrode coating, the negative electrode slurry is formed by mixing raw materials for forming the negative electrode coating, the coating speed is 10m/min, the coating mode is gravure coating, extraction is carried out after the coating of both the positive electrode slurry and the negative electrode slurry is completed, the extracting agent is 3-methyl-1-butanol, the extraction time is 15min, drying is carried out after the extraction, and the drying temperature is 55 ℃ and the drying time is 20min.
The method for preparing the positive electrode slurry comprises the following steps: mixing the organic solvent and the binder in a stirring tank, stirring at 1500rpm for 40min to uniformity, adding inorganic particles, and stirring at 1300rpm for 35min to uniformity; the method for preparing the negative electrode slurry comprises the following steps: in a stirring tank, the organic solvent, the dispersing agent and the binder are mixed and stirred at 1400rpm for 40min to uniformity, and then the inorganic particles are added and stirred at 1400rpm for 35min to uniformity.
Comparative example 2
A lithium ion battery separator comprising: the base film, the positive electrode coating coated on one surface of the base film corresponding to the positive electrode and the negative electrode coating coated on one surface of the base film corresponding to the negative electrode, wherein the thickness of the positive electrode coating is 1.2 mu m, the thickness of the negative electrode coating is 1.3 mu m,
the raw materials for forming the positive electrode coating comprise: organic solvents, binders and inorganic particles;
the raw materials for forming the anode coating comprise: inorganic particles, a binder, a dispersant and an organic solvent;
the organic solvent is N-methyl pyrrolidone;
the inorganic particles are aluminum nitride powder;
the dispersing agent is sodium fatty alcohol ether sulfate, and the binder is polymethyl acrylate.
In the raw materials for forming the positive electrode coating, the ratio of the organic solvent, the binder and the inorganic particles is 13:2.5:3, a step of; in the raw materials for forming the anode coating, the ratio of inorganic particles, a binder, a dispersing agent and an organic solvent is 2.8 in parts by mass: 2.7:0.4:14.
the preparation method of the lithium ion battery diaphragm comprises the following steps:
coating positive electrode slurry on one surface of a base film opposite to a positive electrode to form a positive electrode coating, standing at normal temperature for 10min, coating negative electrode slurry on one surface of the base film opposite to a negative electrode to form a negative electrode coating, wherein the positive electrode slurry is formed by mixing raw materials for forming the positive electrode coating, the negative electrode slurry is formed by mixing raw materials for forming the negative electrode coating, the coating speed of the positive electrode slurry is 15m/min, the coating speed of the negative electrode slurry is 17m/min, the coating mode is gravure coating, extraction is carried out after the coating of both the positive electrode slurry and the negative electrode slurry is completed, the extracting agent is 3-methyl-1-butanol, the extracting time is 20min, drying is carried out after the extraction, the drying temperature is 60 ℃, and the drying time is 23min.
The method for preparing the positive electrode slurry comprises the following steps: mixing the organic solvent and the binder in a stirring tank, stirring at 1600rpm for 45min to uniformity, adding the inorganic particles, and stirring at 1400rpm for 40min to uniformity; the method for preparing the negative electrode slurry comprises the following steps: in a stirring tank, the organic solvent, the dispersant and the binder are mixed and stirred at 1500rpm for 45min to uniformity, and then the inorganic particles are added and stirred at 1500rpm for 40min to uniformity.
Comparative example 3
A lithium ion battery separator comprising: the base film, the positive electrode coating coated on one surface of the base film corresponding to the positive electrode and the negative electrode coating coated on one surface of the base film corresponding to the negative electrode, wherein the thickness of the positive electrode coating is 1.5 mu m, the thickness of the negative electrode coating is 1.5 mu m,
the raw materials for forming the positive electrode coating comprise: organic solvents, binders and inorganic particles;
the raw materials for forming the anode coating comprise: inorganic particles, a binder, a dispersant and an organic solvent;
the organic solvent is ethanol;
the inorganic particles are boehmite powder;
the dispersing agent is polyacrylamide, and the binder is SBR (styrene butadiene rubber).
In the raw materials for forming the positive electrode coating, the ratio of the organic solvent, the binder and the inorganic particles is 14:3:3.2; in the raw materials for forming the anode coating, the ratio of inorganic particles, a binder, a dispersing agent and an organic solvent is 3.2:2.9:0.45:15.
the preparation method of the lithium ion battery diaphragm comprises the following steps:
coating positive electrode slurry on one surface of a base film opposite to a positive electrode to form a positive electrode coating, standing at normal temperature for 10min, coating negative electrode slurry on one surface of the base film opposite to a negative electrode to form a negative electrode coating, wherein the positive electrode slurry is formed by mixing raw materials for forming the positive electrode coating, the negative electrode slurry is formed by mixing raw materials for forming the negative electrode coating, the coating speed is 20m/min, the coating mode is gravure coating, extraction is carried out after the coating of both the positive electrode slurry and the negative electrode slurry is completed, the extracting agent is 3-methyl-1-butanol, the extracting time is 25min, drying is carried out after the extraction, and the drying temperature is 65 ℃ and the drying time is 25min.
The method for preparing the positive electrode slurry comprises the following steps: mixing the organic solvent and the binder in a stirring tank, stirring at 1700rpm for 50min to uniformity, adding the inorganic particles, and stirring at 1500rpm for 45min to uniformity; the method for preparing the negative electrode slurry comprises the following steps: in a stirring tank, the organic solvent, the dispersant and the binder are mixed and stirred at 1600rpm for 50min to uniformity, and then the inorganic particles are added and stirred at 1600rpm for 45min to uniformity.
Lithium batteries of model NCM_606090-4000mAh were produced by using the lithium ion battery separators obtained in examples 1 to 3 and comparative examples 1 to 3, respectively, each of which was 5 lithium batteries, wherein the positive electrode material was ternary material (NCM 523) (purchased from Union solid material), the negative electrode material was graphite (Bei Terui), and the electrolyte of the electrolyte solution was LiPF 6 (the solvent is a mixture of EC (ethylene carbonate) and DMC (dimethyl carbonate), and EC: dmc=1:1 by mass) are assembled into half cells. The negative electrode slurry is prepared by uniformly mixing a negative electrode material, a conductive agent (carbon black of the family ketjen) and a binder SBR (styrene butadiene latex) (Shenzhen Yitong) according to a mass ratio of 8:0.8:1.2, and the positive electrode slurry is prepared by uniformly mixing a positive electrode material, the conductive carbon black (Shenzhen Kogyan) and a binder PVDF (PVDF) (Chengdu Korea) according to a mass ratio of 8:1:1.
Coating the positive electrode slurry on a positive electrode current collector to obtain a positive electrode, wherein the positive electrode current collector is aluminum foil, and the coating amount of the positive electrode slurry is 7mg/cm 2 The coating thickness of the positive electrode slurry is 40um; coating the negative electrode slurry on a negative electrode current collector to obtain a negative electrode, wherein the negative electrode current collector is copper foil, and the coating amount of the negative electrode slurry is 6mg/cm 2 The coating thickness of the negative electrode slurry was 40 μm. And (3) completing formation and capacity division, and performing overcharge test on the prepared lithium battery, wherein the test method and the result are as follows:
the testing method comprises the following steps: the lithium battery was placed in a test box, and the test box process flow was charged to 5.5V (rated voltage 4.8V) at 1C, and whether the lithium battery exploded, smoked, and ignited was observed. The 5 lithium battery test results of each of the examples and comparative examples are shown in table 1.
TABLE 1
According to the test results, explosion and fire do not occur in the examples and the comparative examples, the passing rate of the overcharge test of the examples is far higher than that of the lithium battery of the comparative examples, and the lithium ion battery diaphragms obtained in the examples 1-3 of the invention are proved to strengthen the oxidation resistance and the overcharge resistance of the lithium battery, and in the charging process, the lithium ion channels are cut off at high temperature, so that the safety and the protection of the lithium battery are enhanced.
The lithium ion battery separators obtained in examples 1 to 3 and comparative examples 1 to 3 were also tested for tensile strength and TMA film breaking temperature, as shown in Table 2.
TABLE 2
The foregoing has described exemplary embodiments of the invention, it being understood that any simple variations, modifications, or other equivalent arrangements which would not unduly obscure the invention may be made by those skilled in the art without departing from the spirit of the invention.
Claims (10)
1. A lithium ion battery separator with a charge protection function, comprising: a base film, a positive electrode coating coated on one surface of the base film corresponding to the positive electrode, and a negative electrode coating coated on one surface of the base film corresponding to the negative electrode,
the raw materials for forming the positive electrode coating comprise: organic solvents, binders and polyamides;
the raw materials for forming the negative electrode coating comprise: inorganic particles, binders, molten flame retardants, dispersants and organic solvents;
the organic solvent is at least one of acetone, N-methyl pyrrolidone and ethanol;
the polyamide is one or a mixture of more of poly (paraphenylene terephthalamide), poly (m-phenylene isophthalamide), poly (p-benzamide) and poly (p-phenylene terephthalamide);
the inorganic particles are alumina powder, aluminum nitride powder or boehmite powder;
the melt flame retardant is tetrabromobisphenol A bis (allyl) ether, tetrabromobisphenol A bis (2-hydroxyethyl) ether or tetrabromobisphenol A bis (2, 3-dibromopropyl) ether.
2. The lithium ion battery separator according to claim 1, wherein the thickness of the positive electrode coating is 1.0 to 1.5 μm and the thickness of the negative electrode coating is 1.0 to 1.5 μm.
3. The lithium ion battery separator of claim 2, wherein the dispersant is polyacrylamide or sodium fatty alcohol ether sulfate.
4. A lithium ion battery separator according to claim 3, wherein the binder is polyvinylidene fluoride, polymethyl acrylate or SBR.
5. The lithium ion battery separator according to claim 1, wherein in the raw material for forming the positive electrode coating layer, the ratio of the organic solvent, the binder and the polyamide is (10 to 20) in parts by mass: (1.5-3): (2-4.2); in the raw materials for forming the anode coating, the ratio of inorganic particles, a binder, a molten flame retardant, a dispersing agent and an organic solvent is (1.8-3.5) in parts by mass: (1.8-3.2): (0.8-1.5): (0.35-0.8): (12-22).
6. The method for preparing the lithium ion battery separator with the charge protection function according to claim 1, comprising the following steps:
and coating positive electrode slurry on the surface of the base film opposite to the positive electrode to form the positive electrode coating, and coating negative electrode slurry on the surface of the base film opposite to the negative electrode to form the negative electrode coating, wherein the positive electrode slurry is formed by mixing raw materials for forming the positive electrode coating, and the negative electrode slurry is formed by mixing raw materials for forming the negative electrode coating.
7. The method according to claim 6, wherein the coating speed is 10 to 25m/min, and the coating method is gravure coating.
8. The preparation method according to claim 6, wherein the extraction is performed after the coating, the extractant is 3-methyl-1-butanol, and the extraction time is 15-25 min.
9. The process according to claim 6, wherein the extraction is followed by drying at a temperature of 55 to 70 ℃.
10. The method of producing the positive electrode slurry according to claim 6, wherein the method of producing the positive electrode slurry comprises: mixing the organic solvent and the binder, stirring at 1300-2000 rpm for 35-55 min to uniformity, adding the polyamide, and stirring at 1200-1800 rpm for 35-50 min to uniformity; the method for preparing the negative electrode slurry comprises the following steps: mixing an organic solvent, a dispersing agent and a binder, stirring at 1400-2000 rpm for 40-60 min to uniformity, adding the inorganic particles, stirring at 1200-1800 rpm for 35-50 min to uniformity, adding a molten flame retardant, and stirring at 1300-2000 rpm for 40-55 min to uniformity.
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