CN105118950A - Method for preparing lithium ion battery diaphragm - Google Patents
Method for preparing lithium ion battery diaphragm Download PDFInfo
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- CN105118950A CN105118950A CN201510577175.3A CN201510577175A CN105118950A CN 105118950 A CN105118950 A CN 105118950A CN 201510577175 A CN201510577175 A CN 201510577175A CN 105118950 A CN105118950 A CN 105118950A
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- lithium ion
- graphene
- kynoar
- ion battery
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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
-
- 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
-
- 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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- General Chemical & Material Sciences (AREA)
- Cell Separators (AREA)
Abstract
The invention relates to a method for preparing a lithium ion battery diaphragm. The method includes the steps that (1) a polyvinylidene fluoride and graphene blend polymer diaphragm is prepared from, by mass, 8-25% of polyvinylidene fluoride, 0.00001-0.01% of graphene nanosheet dispersion solution, 0.05-5.0% of pore-forming agent and the balance dimethylacetamide; (2) a commercial diaphragm and the polyvinylidene fluoride and graphene blend polymer diaphragm are composited after being wetted through an alcohol aqueous solution. The prepared lithium ion composite battery diaphragm has excellent mechanical properties (MD: 1600 kg/cm<2> and TD: 1200 kg/cm<2>) and excellent heat stability, and after electrolyte activation, the remaining mass of the composite diaphragm which is heated for one hour at the temperature of 120 DEG C accounts for 90% that of the composite diaphragm which is not heated. Meanwhile, decomposition voltage is as high as 4.5 V and is improved to a certain extent compared with the decomposition voltage of 4.3 V of the commercial diaphragm. Compared with lithium ion conductivity of the commercial diaphragm, the lithium ion conductivity of the lithium ion battery diaphragm is improved by 340%, the lithium ion transference number is 0.56, and a prepared lithium ion battery shows good cycle performance and rate capability.
Description
Technical field
The present invention relates to battery diaphragm field, particularly relate to a kind of preparation method of lithium ion battery separator.
Background technology
Along with the development of lithium ion battery and the variation of battery process, especially power vehicle and Large Copacity energy-storage battery propose very high requirement in order to realize high magnification repid discharge to lithium battery diaphragm, both wished that barrier film had higher porosity and through hole, again resistance to elevated temperatures and film-strength are had higher requirement, traditional lithium ion battery separator is polyolefin, as the porous membrane that polypropylene (PP) and polyethylene (PE) are prepared through physics (as pulling method) or chemistry (as extraction) drill process, as Japanese Asahi Chemical Industry Asahi, east burning Tonen, space portion Ube, the separator product of the foreign corporations such as U.S. Celgard.But the maximum defect of polyalkene diaphragm is that the contact of organic electrolyte is poor, is not easily soaked by electrolyte, easily causes the leakage of electrolyte, have a strong impact on ionic conductivity and the security performance of lithium ion battery.
Polyvinylidene fluoride polymer, as the research of gel polymer electrolyte, starts from the phase at the beginning of the eighties in last century.Repetitive-the CH of Kynoar
2-CF
2-, be a kind of white powder crystalline polymer, relative density is 1.75-1.78, vitrification point-39 DEG C, molten point 180 DEG C, and heat decomposition temperature is 350 DEG C, can processing temperature wide ranges, easily processes.Polymer chain makes this material list reveal fabulous electrochemical stability and fire retardancy containing very strong polar group, simultaneously dielectric constant higher (8.9), be conducive to promoting that lithium salts dissolves, increasing carrier concentration, is comparatively ideal matrix.Although the Kynoar system barrier film that the method for simple phase separation prepares has higher porosity, ionic conductivity, thermal stability and chemical property, but its mechanical strength that has by the gel electrolyte that formed after electrolyte activation reduce significantly, and traditional polyalkene diaphragm does not have this shortcoming.Adopt the Kynoar barrier film of polyalkene diaphragm and modification to carry out compound, the new types of diaphragm obtaining having concurrently polyalkene diaphragm good mechanical strength and Kynoar barrier film good electrical chemical property and thermal stability has realistic feasibility and practicality for this reason.
Summary of the invention
For this reason, the invention provides a kind of lithium ion battery separator and preparation method thereof, the method comprises the following steps:
(1) preparation of Kynoar and Graphene polymer blend barrier film: under normal temperature by graphene nanometer sheet and dimethylacetylamide blended, prepare by ultrasonic more than 5min the graphene nanometer sheet dispersion liquid that concentration is less than 0.1g/L; Add thermal agitation together with Kynoar, graphene nanometer sheet dispersion liquid and pore former being added to respectively in organic solvent dimethylacetylamide and obtain Kynoar and the blended even casting solution of Graphene, wherein Kynoar, graphene nanometer sheet dispersion liquid and pore former are respectively 8-25%, 0.00001%-0.01% and 0.05%-5.0% of gross mass mark, and residual mass is that then dimethylacetylamide obtains poly-Kynoar and the blended lithium ion battery separator of Graphene by immersion precipitation.Non-solvent used be deionized water and dimethylacetylamide by volume 2:1 ~ 4:1 proportioning obtain, first film formation time is 5s-3h, and prepared membrane thicknesses is at 10 μm to 40 μm.
(2) compound of commercial barrier film and Kynoar and Graphene polymer blend barrier film: thickness is less than 30 μm, porosity be greater than 30% commercial polypropylene or polyethylene diagrams be laid on a clean glass plate, upper surface volume ratio is that the ethanol water of 1:1 soaks, the Kynoar prepared and Graphene polymer blend barrier film are laid on commercial film, Kynoar and Graphene polymer blend diaphragms also soak with ethanol water, by another commercial membrane cover thereon.End of operation, is sandwiched in the wet film of preparation between two pieces of clean glass plates, is placed in 10-70 DEG C of oven drying 3-20h, and obtain commercial barrier film and Kynoar and Graphene polymer blend composite diaphragm, prepared composite film thickness is 40-90 μm.
Preferably, graphene nanometer sheet is prepared in described step (1) and dimethylacetylamide blended liquid ultrasonic time is more than 0.1h.
Preferably, the pore former described in described step (1) is the one in polyvinylpyrrolidone, polyethylene glycol, acetone, organic molecule or LiCl inorganic salts.
Preferably, in Kynoar described in described step (1) and the blended even casting solution of Graphene, Kynoar mass fraction is 10%-20%, and pore former mass fraction is 1%-3%, Graphene mass fraction is 0.0001%-0.01%, and residual mass is dimethylacetylamide.
Preferably, in described step (1), first film formation time is 5s-2h, and prepared membrane thicknesses is at 15 μm to 40 μm.
Preferably, in described step (2), commercial polypropylene used or polyethylene diagrams thickness are 15 to 30 μm, and porosity is 30-50%.
Preferably, in described step (2), oven drying temperature is 30-70 DEG C, and drying time is 3-10h.Prepared composite film thickness is 45-90 μm.
The lithium ion battery separator that the present invention prepares not only possesses Kynoar hexafluoropropylene and Graphene polymer blend barrier film porosity is high, the good Sum decomposition voltage of ionic conductivity is high chemical property feature, simultaneously by the compound with commercial barrier film, the feature of the gel electrolyte bad mechanical strength formed after avoiding electrolyte activation.Lithium ion composite battery separator film prepared by the present invention shows excellent mechanical performance (MD:1600kg/cm
2, TD:1200kg/cm
2) and thermal stability (residual mass that the rear composite diaphragm of electrolyte activation heats 1h at 120 DEG C is 90% of quality before heating), decomposition voltage is up to 4.5V simultaneously, the 4.3V of more commercial barrier film has a certain upgrade, the more commercial barrier film of lithium ion conductivity promotes 340%, lithium ion transference number is 0.56, and prepared lithium ion battery shows good cycle performance and high rate performance.
Embodiment
Below by way of specific embodiment, the present invention is described in further detail.
Embodiment 1
(1) preparation of Kynoar and Graphene polymer blend barrier film: take 0.01g graphene nanometer sheet (volume can be ignored) under normal temperature respectively and 100ml dimethylacetylamide blended, then ultrasonic 1h prepares the graphene nanometer sheet dispersion liquid that concentration is 0.1g/L; Then the Kynoar (weight average molecular weight is 1,000,000) taking 10.0g adds conical flask, add 3.0g polyvinylpyrrolidone simultaneously, then the graphene uniform dispersion of 10ml0.1g/L is added, i.e. 0.001g Graphene, add dimethylacetylamide more subsequently, make the mass percent of Kynoar, polyvinylpyrrolidone, Graphene and dimethylacetylamide be respectively 10%, 3.0%, 0.001% and 87%; Poly-Kynoar and the blended lithium ion battery separator of Graphene is obtained finally by immersion precipitation.Non-solvent used be deionized water and dimethylacetylamide by volume 3:1 proportioning obtain, first film formation time is 10s, and prepared membrane thicknesses is 20 μm.
(2) compound of commercial barrier film and Kynoar and Graphene polymer blend barrier film: (thickness is 25 μm by commercial for Celgard2400 polypropylene diaphragm, porosity is 41%) be laid on a clean glass plate, upper surface volume ratio is that the ethanol water of 1:1 soaks, the Kynoar prepared and Graphene polymer blend barrier film are laid on commercial film, Kynoar and Graphene polymer blend diaphragms also soak with ethanol water, by commercial for another Celgard2400 polypropylene diaphragm lid thereon.End of operation, is sandwiched in the wet film of preparation between two pieces of clean glass plates, is placed in 50 DEG C of oven drying 20h, and obtain commercial barrier film and Kynoar and Graphene polymer blend composite diaphragm, prepared composite film thickness is 70 μm.
The lithium ion battery separator of this example preparation, not only have higher porosity, porosity reaches 58%; Further, place 30 minutes at 140 DEG C, its thermal contraction about 3.5%, namely has good resistance to elevated temperatures.Excellent mechanical performance (MD:1200kg/cm
2, TD:800kg/cm
2) and thermal stability (residual mass that the rear composite diaphragm of electrolyte activation heats 1h at 120 DEG C is 85% of quality before heating), decomposition voltage is up to 4.5V simultaneously, the 4.3V of more commercial barrier film has a certain upgrade, the more commercial barrier film of lithium ion conductivity promotes 300%, and lithium ion transference number is 0.60.
Embodiment 2
(1) preparation of Kynoar and Graphene polymer blend barrier film: take 0.01g graphene nanometer sheet (volume can be ignored) under normal temperature respectively and 100ml dimethylacetylamide blended, then ultrasonic 1h prepares the graphene nanometer sheet dispersion liquid that concentration is 0.1g/L; Then the Kynoar (weight average molecular weight is 1,000,000) taking 15.0g adds conical flask, add 3.0g polyvinylpyrrolidone simultaneously, then the graphene uniform dispersion of 10ml0.1g/L is added, i.e. 0.001g Graphene, add dimethylacetylamide more subsequently, make the mass percent of Kynoar, polyvinylpyrrolidone, Graphene and dimethylacetylamide be respectively 15%, 3.0%, 0.001% and 82%; Poly-Kynoar and the blended lithium ion battery separator of Graphene is obtained finally by immersion precipitation.Non-solvent used be deionized water and dimethylacetylamide by volume 3:1 proportioning obtain, first film formation time is 10s, and prepared membrane thicknesses is 20 μm.
(2) compound of commercial barrier film and Kynoar and Graphene polymer blend barrier film: (thickness is 25 μm by commercial for Celgard2400 polypropylene diaphragm, porosity is 41%) be laid on a clean glass plate, upper surface volume ratio is that the ethanol water of 1:1 soaks, the Kynoar prepared and Graphene polymer blend barrier film are laid on commercial film, Kynoar and Graphene polymer blend diaphragms also soak with ethanol water, by commercial for another Celgard2400 polypropylene diaphragm lid thereon.End of operation, is sandwiched in the wet film of preparation between two pieces of clean glass plates, is placed in 50 DEG C of oven drying 20h, and obtain commercial barrier film and Kynoar and Graphene polymer blend composite diaphragm, prepared composite film thickness is 70 μm.
The lithium ion battery separator of this example preparation, not only have higher porosity, porosity reaches 51%; Further, place 30 minutes at 140 DEG C, its thermal contraction about 1.5%, namely has good resistance to elevated temperatures.Excellent mechanical performance (MD:1600kg/cm
2, TD:1000kg/cm
2) and thermal stability (residual mass that the rear composite diaphragm of electrolyte activation heats 1h at 120 DEG C is 90% of quality before heating), decomposition voltage is up to 4.5V simultaneously, the 4.3V of more commercial barrier film has a certain upgrade, the more commercial barrier film of lithium ion conductivity promotes 340%, and lithium ion transference number is 0.56.
Embodiment 3
(1) preparation of Kynoar and Graphene polymer blend barrier film: take 0.01g graphene nanometer sheet (volume can be ignored) under normal temperature respectively and 100ml dimethylacetylamide blended, then ultrasonic 1h prepares the graphene nanometer sheet dispersion liquid that concentration is 0.1g/L; Then the Kynoar (weight average molecular weight is 1,000,000) taking 20.0g adds conical flask, add 3.0g polyvinylpyrrolidone simultaneously, then the graphene uniform dispersion of 10ml0.1g/L is added, i.e. 0.001g Graphene, add dimethylacetylamide more subsequently, make the mass percent of Kynoar, polyvinylpyrrolidone, Graphene and dimethylacetylamide be respectively 20%, 3.0%, 0.001% and 77%; Poly-Kynoar and the blended lithium ion battery separator of Graphene is obtained finally by immersion precipitation.Non-solvent used be deionized water and dimethylacetylamide by volume 3:1 proportioning obtain, first film formation time is 10s, and prepared membrane thicknesses is 20 μm.
(2) compound of commercial barrier film and Kynoar and Graphene polymer blend barrier film: (thickness is 25 μm by commercial for Celgard2400 polypropylene diaphragm, porosity is 41%) be laid on a clean glass plate, upper surface volume ratio is that the ethanol water of 1:1 soaks, the Kynoar prepared and Graphene polymer blend barrier film are laid on commercial film, vinylidene and Graphene polymer blend diaphragms also soak with ethanol water, by commercial for another Celgard2400 polypropylene diaphragm lid thereon.End of operation, is sandwiched in the wet film of preparation between two pieces of clean glass plates, is placed in 50 DEG C of oven drying 20h, and obtain commercial barrier film and Kynoar and Graphene polymer blend composite diaphragm, prepared composite film thickness is 70 μm.
The lithium ion battery separator of this example preparation, not only have higher porosity, porosity reaches 48%; Further, place 30 minutes at 140 DEG C, its thermal contraction about 0.5%, namely has good resistance to elevated temperatures.Excellent mechanical performance (MD:1700kg/cm
2, TD:1300kg/cm
2) and thermal stability (residual mass that the rear composite diaphragm of electrolyte activation heats 1h at 120 DEG C is 92% of quality before heating), decomposition voltage is up to 4.8V simultaneously, the 4.3V of more commercial barrier film has a certain upgrade, the more commercial barrier film of lithium ion conductivity promotes 180%, and lithium ion transference number is 0.54.
Embodiment 4
(1) preparation of Kynoar and Graphene polymer blend barrier film: take 0.01g graphene nanometer sheet (volume can be ignored) under normal temperature respectively and 100ml dimethylacetylamide blended, then ultrasonic 1h prepares the graphene nanometer sheet dispersion liquid that concentration is 0.1g/L; Then the Kynoar (weight average molecular weight is 1,000,000) taking 20.0g adds conical flask, add 3.0g polyvinylpyrrolidone simultaneously, then the graphene uniform dispersion of 10ml0.1g/L is added, i.e. 0.001g Graphene, add dimethylacetylamide more subsequently, make the mass percent of Kynoar, polyvinylpyrrolidone, Graphene and dimethylacetylamide be respectively 15%, 3.0%, 0.001% and 82%; Poly-Kynoar and the blended lithium ion battery separator of Graphene is obtained finally by immersion precipitation.Non-solvent used be deionized water and dimethylacetylamide by volume 3:1 proportioning obtain, first film formation time is 10s, and prepared membrane thicknesses is 20 μm.
(2) compound of commercial barrier film and Kynoar and Graphene polymer blend barrier film: (thickness is 15 μm by commercial polyethylene diagrams, porosity is 36%) be laid on a clean glass plate, upper surface volume ratio is that the ethanol water of 1:1 soaks, the Kynoar prepared and Graphene polymer blend barrier film are laid on commercial film, Kynoar and Graphene polymer blend diaphragms also soak with ethanol water, by another commercial polyethylene diagrams lid thereon.End of operation, is sandwiched in the wet film of preparation between two pieces of clean glass plates, is placed in 50 DEG C of oven drying 20h, and obtain commercial barrier film and Kynoar and Graphene polymer blend composite diaphragm, prepared composite film thickness is 55 μm.
The lithium ion battery separator of this example preparation, not only have higher porosity, porosity reaches 48%; Further, place 30 minutes at 140 DEG C, its thermal contraction about 3.5%, namely has good resistance to elevated temperatures.Excellent mechanical performance (MD:1300kg/cm
2, TD:1000kg/cm
2) and thermal stability (residual mass that the rear composite diaphragm of electrolyte activation heats 1h at 120 DEG C is 91% of quality before heating), decomposition voltage is up to 4.6V simultaneously, the 4.3V of more commercial barrier film has a certain upgrade, the more commercial barrier film of lithium ion conductivity promotes 240%, and lithium ion transference number is 0.60.
Claims (7)
1. a preparation method for lithium ion battery separator, is characterized in that comprising the following steps:
(1) preparation of Kynoar and Graphene polymer blend barrier film: under normal temperature by graphene nanometer sheet and dimethylacetylamide blended, prepare by ultrasonic more than 5min the graphene nanometer sheet dispersion liquid that concentration is less than 0.1g/L; Add thermal agitation together with Kynoar, graphene nanometer sheet dispersion liquid and pore former being added to respectively in organic solvent dimethylacetylamide and obtain Kynoar and the blended even casting solution of Graphene, wherein Kynoar, graphene nanometer sheet dispersion liquid and pore former are respectively 8-25%, 0.00001%-0.01% and 0.05%-5.0% of gross mass mark, and residual mass is dimethylacetylamide; Then Kynoar and the blended lithium ion battery separator of Graphene is obtained by immersion precipitation, non-solvent used be deionized water and dimethylacetylamide by volume 2:1 ~ 4:1 proportioning obtain, first film formation time is 5s-3h, and prepared membrane thicknesses is at 10 μm to 40 μm;
(2) compound of barrier film and Kynoar and Graphene polymer blend barrier film: thickness is less than 30 μm, porosity be greater than 30% commercial polypropylene or polyethylene diagrams be laid on glass plate, upper surface volume ratio is that the ethanol water of 1:1 soaks, the Kynoar prepared and Graphene polymer blend barrier film are laid on commercial film, Kynoar and Graphene polymer blend diaphragms also soak with ethanol water, by another commercial membrane cover thereon; Be sandwiched in by the wet film of preparation between two pieces of clean glass plates, be placed in 10-70 DEG C of oven drying 3-20h, obtain commercial barrier film and Kynoar and Graphene polymer blend composite diaphragm, prepared composite film thickness is 40-90 μm.
2. the preparation method of a kind of lithium ion battery separator according to claim 1, is characterized in that: prepare graphene nanometer sheet in described step (1) and dimethylacetylamide blended liquid ultrasonic time is more than 0.1h.
3. the preparation method of a kind of lithium ion battery separator according to claim 1, is characterized in that: the pore former described in described step (1) is the one in polyvinylpyrrolidone, polyethylene glycol, acetone, organic molecule or LiCl inorganic salts.
4. the preparation method of a kind of lithium ion battery separator according to claim 1, it is characterized in that: in Kynoar described in described step (1) and the blended even casting solution of Graphene, Kynoar mass fraction is 10%-20%, pore former mass fraction is 1%-3%, Graphene mass fraction is 0.0001%-0.01%, and residual mass is dimethylacetylamide.
5. the preparation method of a kind of lithium ion battery separator according to claim 1, is characterized in that: in described step (1), and first film formation time is 5s-2h, and prepared membrane thicknesses is at 15 μm to 40 μm.
6. the preparation method of a kind of lithium ion battery separator according to claim 1, is characterized in that: in described step (2), and commercial polypropylene used or polyethylene diagrams thickness are 15 to 30 μm, and porosity is 30-50%.
7. the preparation method of a kind of lithium ion battery separator according to claim 1, is characterized in that: in described step (2), and oven drying temperature is 30-70 DEG C, and drying time is 3-10h, and prepared composite film thickness is 45-90 μm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108075091A (en) * | 2016-11-18 | 2018-05-25 | 中国科学院金属研究所 | A kind of preparation method of functional porous polyvinylidene fluoride film used for all-vanadium redox flow battery |
| CN108777281A (en) * | 2018-04-26 | 2018-11-09 | 合肥国轩高科动力能源有限公司 | Preparation method of lithium ion battery composite diaphragm |
| CN111584801A (en) * | 2020-04-29 | 2020-08-25 | 西安理工大学 | Lithium ion battery composite diaphragm and preparation method thereof |
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| CN108075091A (en) * | 2016-11-18 | 2018-05-25 | 中国科学院金属研究所 | A kind of preparation method of functional porous polyvinylidene fluoride film used for all-vanadium redox flow battery |
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| CN111584801A (en) * | 2020-04-29 | 2020-08-25 | 西安理工大学 | Lithium ion battery composite diaphragm and preparation method thereof |
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Application publication date: 20151202 |