CN111769323A - High-hardness polymer battery cell and preparation method thereof - Google Patents
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- H01M10/00—Secondary cells; Manufacture thereof
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Abstract
The invention belongs to the technical field of lithium ion batteries. A high-hardness polymer battery cell comprises at least one negative pole piece, at least one positive pole piece and at least one gel electrolyte layer; the gel electrolyte layer is prepared by absorbing electrolyte after a polymer solution forms a gel layer on the surface of at least one positive pole piece and/or negative pole piece; the polymer solution comprises the following components in percentage by mass: 40-60% of polymer, 20-30% of organic solvent and 10-30% of additive; the electrolyte comprises the following components in percentage by mass: 5-25% of lithium salt, 30-60% of polyvinyl chloride plasticizing composition and 15-65% of electrolyte additive. The high-hardness polymer battery cell has excellent electrochemical performance, high conductivity, good rate performance and cycle performance, high hardness and good safety.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a high-hardness polymer battery cell and a preparation method thereof.
Background
The traditional lithium ion battery adopts liquid electrolyte, and the liquid electrolyte is formed by dissolving lithium salt in a carbonate organic solvent. For liquid electrolytes, the applicable negative electrode materials are limited; the liquid electrolyte is easy to decompose to generate gas and form overlarge vapor pressure in the discharging process, and the battery cell shell is easy to corrode to cause liquid leakage; the ignition point and the boiling point of the lithium ion battery electrolyte are low, the internal resistance of the lithium ion battery electrolyte is continuously increased in the use process, and the internal temperature of the battery is increased in the charge and discharge processes, so that safety problems such as fire and explosion are easily caused; the consumption of electrolyte also reduces the battery life. The polymer battery has the advantages of high voltage, large specific energy, stable discharge, good cycle performance, good safety performance, long storage life and the like, and the polymer gel electrolyte is used for replacing an organic system liquid electrolyte to effectively solve the technical problems.
The existing gel electrolyte is prepared by adding polymerizable monomers into liquid electrolyte, and the preparation method mainly comprises the following steps: a porous gel polymer electrolyte preparation method and a uniform gel polymer electrolyte preparation method. In both methods, in an organic environment containing a plasticizer, an initiator initiates polymerization of polymer monomers in a high-temperature environment to form a high-molecular polymer matrix. The thermal polymerization process may cause thermal expansion and thermal bulging, the thermal polymerization reaction is incomplete, and the remaining monomers may affect the electrochemical performance of the battery. The high-hardness polymer battery cell has excellent electrochemical performance, high conductivity, good rate performance and cycle performance, high hardness and good safety. Due to the existence of the micromolecular solvent, the gel polymer electrolyte also has the defects of higher volatility, poorer electrochemical stability and thermal stability, low mechanical strength, poor stability of an electrolyte and an electrode interface and the like.
Disclosure of Invention
The invention aims to solve the technical problem of providing a high-hardness polymer battery cell which has excellent electrochemical performance, high conductivity, good rate performance and cycle performance, high hardness and good safety.
The technical scheme of the invention is as follows:
a high-hardness polymer battery cell comprises at least one negative pole piece, at least one positive pole piece and at least one gel electrolyte layer; the gel electrolyte layer is prepared by absorbing electrolyte after a polymer solution forms a gel layer on the surface of at least one positive pole piece and/or negative pole piece; the polymer solution comprises the following components in percentage by mass: 40-60% of polymer, 20-30% of organic solvent and 10-30% of additive; the electrolyte comprises the following components in percentage by mass: 5-25% of lithium salt, 30-60% of polyvinyl chloride plasticizing composition and 15-65% of electrolyte additive.
Further, the polymer is at least one of polymethyl methacrylate, polyacrylonitrile, polyethylene oxide, polyvinylidene fluoride, vinylidene fluoride-hexafluoropropylene copolymer, polyacrylate, polyacrylic polyol ester, polystyrene, polyethylene and methyl methacrylate.
Further, the organic solvent is N-methyl pyrrolidone, dimethyl sulfoxide, dimethylformamide, ethyl acetate, ethylene carbonate, propylene carbonate, butylene carbonate, 1, 2-dimethyl ethylene carbonate, ethylbutyl carbonate, methylbutyl carbonate, dibutyl carbonate, diethyl carbonate, dimethyl carbonate, trifluoromethyl ethylene carbonate, di-N-propyl carbonate, diisopropyl carbonate, methylethyl carbonate, ethylpropyl carbonate, ethylisopropyl carbonate, methylpropyl carbonate, dimethoxyethane, diethoxyethane, acetone, ethanol, tetrahydrofuran, 2-methyl tetrahydrofuran, diethylene glycol dimethyl ether, triethylene glycol dimethyl ether, tetraethylene glycol dimethyl ether, 1, 3-dioxolane, sulfolane, 4-methyl-1, 3-butyrolactone, gamma-butyrolactone, methyl methacrylate, ethyl methacrylate, methyl methacrylate, ethyl methacrylate, methyl, At least one of methyl formate, ethyl formate, methyl acetate, methyl propionate, ethyl propionate, methyl butyrate, ethyl butyrate, ethylene carbonate, propane sultone and ethylene sulfite.
Further, the additive comprises 60-80% of nano conductive carbon, 10-20% of polyvinylidene fluoride and 10-20% of dispersing agent.
Further, the nano conductive carbon is graphene and a multi-walled carbon nanotube; the dispersing agent is saturated fatty acid modified acrylate, N-vinyl pyrrolidone and alpha, beta-vinyl unsaturated acid.
Further, the lithium salt is at least one of lithium bis (fluorosulfonyl) imide, lithium bis (trifluoromethanesulfonyl) imide, lithium bis (pentafluoroethylsulfonyl) imide, lithium difluoro (oxalato) borate, lithium bis (fluorosulfonato) imide, and lithium difluoro (oxalato) borate.
Further, the polyvinyl chloride plasticized composition comprises the following components in percentage by mass: 55-85% of polyvinyl chloride and 15-45% of plasticizer; the plasticizer is succinate and epoxidized castor oil.
Further, the electrolyte is added into at least one of a surfactant, a film forming aid, a wetting agent and a flame retardant.
Further, the film-forming assistant is at least one of vinylene carbonate, fluoroethylene carbonate, ethylene carbonate, propiolactone sulfonate, butyrolactone sulfonate, ethylene sulfate, ethylene sulfite, butylene sulfite, biphenyl and succinonitrile.
A preparation method of the high-hardness polymer battery cell comprises the following steps:
a. ball-milling the polymer at a high speed until the particle size is less than 1 mu m, adding an organic solvent and an additive, and uniformly dispersing to obtain a polymer solution; mixing the lithium salt, the polyvinyl chloride plasticizing composition and an electrolyte additive, and uniformly dispersing to obtain an electrolyte;
b. coating the polymer solution on the surface of at least one positive pole piece and/or negative pole piece, and drying in vacuum at 70-85 ℃ under 1-6Mpa for 60s-30min to form a gel layer;
c. b, soaking the positive pole piece and/or the negative pole piece obtained in the step b in electrolyte for 5-60min to obtain a gel electrolyte layer;
d. and overlapping and laminating at least one positive pole piece and at least one negative pole piece to obtain the high-hardness polymer battery cell.
Further, in the step a, the dispersing method is one or more of stirring, high-speed stirring, ball milling, high-speed ball milling and ultrasonic dispersing, and the dispersing time is 5-60 min.
The invention has the following beneficial effects:
the polymer solution selected by the invention can generate a gel layer with a porous net structure in situ on the surface of the positive pole piece and/or the negative pole piece after being dried in vacuum, the compatibility of the gel layer and the interface of the pole pieces is good, the surface of the gel is in a completely dry state, the pore structure on the gel layer has strong liquid locking capacity and good liquid holding stability, and the adsorption capacity of the electrolyte in the gel electrolyte layer can be greatly improved. The nano conductive carbon in the polymer solution additive can be uniformly distributed in the gel layer under the action of the dispersing agent to form a stable bracket structure, and the electrode solution can be adsorbed in the bracket structure, so that the adsorption capacity of the gel layer on the electrolyte is further improved, the transmission of lithium ions in the gel polymer is enhanced, the ionic conductivity is improved, and the hardness of the lithium ion battery is improved; the nano conductive carbon has stable electrochemical property and thermal stability, and can improve the temperature and safety of an internal structure of a battery in the charging and discharging processes.
The electrolyte selected by the invention comprises a polyvinyl chloride plasticizing composition, wherein the organic solvent has good compatibility with the polymer, the plasticizing effect of the plasticizer is promoted, the conduction effect of lithium ions in the polymer is favorably improved, and the conductivity of the lithium battery and the mechanical strength of the gel layer are effectively improved. By adjusting the types and the proportion of lithium salts in the electrolyte, the formation reaction of an SEI film can be controlled, and the components and the properties of the SEI film can be adjusted, so that the cycle performance of the electrode is improved.
Detailed Description
The present invention will be described in detail with reference to examples, which are only preferred embodiments of the present invention and are not intended to limit the present invention.
Example 1
A high-hardness polymer battery cell comprises a negative pole piece, a positive pole piece and four gel electrolyte layers; the gel electrolyte layer is prepared by absorbing electrolyte after polymer solution forms gel layers on the surfaces of the positive pole piece and the negative pole piece;
the polymer solution comprises the following components in percentage by mass: 40% of polymer, 30% of organic solvent and 30% of additive; the polymer is polymethyl methacrylate and polyethylene; the organic solvent is N-methyl pyrrolidone; the additive comprises 60% of nano conductive carbon, 20% of polyvinylidene fluoride and 20% of dispersing agent; the nano conductive carbon is graphene and a multi-walled carbon nanotube; the dispersing agent is saturated fatty acid modified acrylate, N-vinyl pyrrolidone and alpha, beta-vinyl unsaturated acid;
the electrolyte comprises the following components in percentage by mass: 25% of lithium salt, 30% of polyvinyl chloride plasticizing composition and 45% of electrolyte additive; the lithium salt is lithium bis (fluorosulfonyl) imide and lithium difluoro (oxalato) borate; the polyvinyl chloride plasticized composition comprises the following components in percentage by mass: 85% of polyvinyl chloride and 15-45% of plasticizer; the plasticizer is succinate and epoxidized castor oil; the electrolyte is added as a film forming aid; the film-forming auxiliary agent is fluoroethylene carbonate, biphenyl and succinonitrile.
Example 2
A high-hardness polymer battery cell comprises a negative pole piece, a positive pole piece and four gel electrolyte layers; the gel electrolyte layer is prepared by absorbing electrolyte after polymer solution forms gel layers on the surfaces of the positive pole piece and the negative pole piece;
the polymer solution comprises the following components in percentage by mass: 50% of polymer, 30% of organic solvent and 20% of additive; the polymer is methyl butyl carbonate and 2-methyl tetrahydrofuran; the additive comprises 70% of nano conductive carbon, 15% of polyvinylidene fluoride and 15% of dispersing agent; the nano conductive carbon is graphene and a multi-walled carbon nanotube; the dispersing agent is saturated fatty acid modified acrylate, N-vinyl pyrrolidone and alpha, beta-vinyl unsaturated acid;
the electrolyte comprises the following components in percentage by mass: lithium salt 20%, polyvinyl chloride plasticizing composition 40% and electrolyte additive 40%; the lithium salt is bis (trifluoromethyl) sulfonyl imide lithium and difluoro oxalic acid lithium borate; the polyvinyl chloride plasticized composition comprises the following components in percentage by mass: 85% of polyvinyl chloride and 15% of plasticizer; the plasticizer is succinate and epoxidized castor oil; the electrolyte is added as a film forming aid; the film forming auxiliary agent is fluoroethylene carbonate and ethylene carbonate.
Example 3
A high-hardness polymer battery cell comprises a negative pole piece, a positive pole piece and four gel electrolyte layers; the gel electrolyte layer is prepared by absorbing electrolyte after a polymer solution forms a gel layer on the surfaces of at least the positive pole piece and the negative pole piece;
the polymer solution comprises the following components in percentage by mass: 60% of polymer, 20% of organic solvent and 20% of additive; the polymer is a vinylidene fluoride-hexafluoropropylene copolymer; the organic solvent is 1, 2-dimethyl ethylene carbonate, sulfolane, 4-methyl-1, 3-butyrolactone and ethylene sulfite; the additive comprises 60% of nano conductive carbon, 20% of polyvinylidene fluoride and 20% of dispersing agent; the nano conductive carbon is graphene and a multi-walled carbon nanotube; the dispersing agent is saturated fatty acid modified acrylate, N-vinyl pyrrolidone and alpha, beta-vinyl unsaturated acid;
the electrolyte comprises the following components in percentage by mass: 5% of lithium salt, 30% of polyvinyl chloride plasticized composition and 65% of electrolyte additive; the lithium salt is bis (trifluoromethyl sulfonyl) lithium and lithium difluoro oxalate borate; the polyvinyl chloride plasticized composition comprises the following components in percentage by mass: 55% of polyvinyl chloride and 45% of plasticizer; the plasticizer is succinate and epoxidized castor oil; the electrolyte is added as a surfactant.
A method of making the high durometer polymer cell of embodiments 1-3, comprising the steps of:
a. ball-milling the polymer at a high speed until the particle size is less than 1 mu m, adding an organic solvent and an additive, and uniformly dispersing to obtain a polymer solution; mixing the lithium salt, the polyvinyl chloride plasticizing composition and an electrolyte additive, and uniformly dispersing to obtain the electrolyte, wherein the dispersion method comprises one or more of stirring, high-speed stirring, ball milling, high-speed ball milling and ultrasonic dispersion, and the dispersion time is 5-60 min.
b. Coating the polymer solution on the surface of at least one positive pole piece and/or negative pole piece, and drying in vacuum at 70-85 ℃ under 1-6Mpa for 60s-30min to form a gel layer;
c. b, soaking the positive pole piece and/or the negative pole piece obtained in the step b in electrolyte for 5-60min to obtain a gel electrolyte layer;
d. and overlapping and laminating at least one positive pole piece and at least one negative pole piece to obtain the high-hardness polymer battery cell.
Comparative example 1
The only difference from example 1 is that the additive described in comparative example 1 is nano titanium dioxide.
Comparative example 2
The only difference from example 1 is that comparative example 2 replaces the polyvinyl chloride plasticized composition with the plasticizer ethyl acetate.
Comparative example 3
The only difference from example 1 is that the lithium salt in comparative example 3 is lithium perchlorate, and the polymer in step a of the preparation method is directly mixed and dispersed with an organic solvent and an additive without high-speed ball milling.
The high hardness polymer cells of the invention of examples 1-3 and comparative examples 1-3 were tested for various properties:
(1) and (3) hardness testing: the AI7000S model high-speed rail tension meter, the test module and the center position of the cell plane long axis direction are coincided, the bending strength; the advancing speed of the probe module is 10 mm/min. Recording a strain versus tensile strength curve, and uniformly taking the tensile force when the deformation of the battery cell is 0.5mm as the hardness of the battery cell;
(2) and (3) testing capacity and cycle performance: charging to 4.2V at constant current of 0.5C, standing for 5 minutes, charging to 40mA at constant voltage of 4.2V, standing for 5 minutes, discharging to 3.0V at current of 0.5C, and recording a discharge curve and a discharge capacity; after standing for 15 minutes, repeating the steps for n times;
(3) and (3) rate performance test: the method is used for testing the same capacity, the charging is uniformly carried out by adopting 0.5C full charge, when discharging, the discharging is stopped when discharging is carried out by respectively taking 0.2C, 0.5C, 1C, 1.5C and 2C to discharge to 3.0V, the discharging capacity of 0.2C as a reference, the discharging capacity of 2C is divided by the discharging capacity of 0.2C, and the more the capacity percentage of 2C/0.2C is close to 100 percent, the more excellent the multiplying power performance of the battery cell is;
(4) and (3) nail penetration testing: the test method comprises an automatic nail penetration experiment, a stainless steel nail with the diameter of 3mm and the nail advancing speed of 10mm/S, and a temperature curve of the position close to the electric core piercing part is tested by a multi-path thermodetector. Quantitatively recording the temperature rise curve and the peak temperature of the battery cell, and qualitatively recording whether the battery cell smokes, catches fire and burns or not;
the test results are given in the following table:
therefore, the high-hardness polymer provided by the invention has the advantages of high capacity retention rate of the battery cell, good electrical properties, high hardness and good safety.
Claims (10)
1. A high-hardness polymer battery cell is characterized by comprising at least one negative pole piece, at least one positive pole piece and at least one gel electrolyte layer; the gel electrolyte layer is prepared by absorbing electrolyte after a polymer solution forms a gel layer on the surface of at least one positive pole piece and/or negative pole piece;
the polymer solution comprises the following components in percentage by mass: 40-60% of polymer, 20-30% of organic solvent and 10-30% of additive;
the electrolyte comprises the following components in percentage by mass: 5-25% of lithium salt, 30-60% of polyvinyl chloride plasticizing composition and 15-65% of electrolyte additive.
2. The high-hardness polymer cell core according to claim 1, wherein the polymer is at least one of polymethyl methacrylate, polyacrylonitrile, polyethylene oxide, polyvinylidene fluoride, vinylidene fluoride-hexafluoropropylene copolymer, polyacrylate, polyacrylic polyol ester, polystyrene, polyethylene, and methyl methacrylate.
3. The high hardness polymer cell core according to claim 1, wherein the organic solvent is N-methylpyrrolidone, dimethyl sulfoxide, dimethylformamide, ethyl acetate, ethylene carbonate, propylene carbonate, butylene carbonate, 1, 2-dimethylethylene carbonate, ethylbutyl carbonate, methylbutyl carbonate, dibutyl carbonate, diethyl carbonate, dimethyl carbonate, ethylene trifluoromethyl carbonate, di-N-propyl carbonate, diisopropyl carbonate, methylethyl carbonate, ethylpropyl carbonate, ethylisopropyl carbonate, methylpropyl carbonate, dimethoxyethane, diethoxyethane, acetone, ethanol, tetrahydrofuran, 2-methyltetrahydrofuran, diethylene glycol dimethyl ether, triethylene glycol dimethyl ether, tetraethylene glycol dimethyl ether, 1, 3-dioxolane, sulfolane, 4-methyl-1, 3-butyrolactone, gamma-butyrolactone, methyl formate, ethyl formate, methyl acetate, methyl propionate, ethyl propionate, methyl butyrate, ethyl butyrate, ethylene carbonate, propane sultone, ethylene sulfite.
4. The high-hardness polymer battery cell of claim 1, wherein the additives are 60-80% of nano conductive carbon, 10-20% of polyvinylidene fluoride and 10-20% of dispersing agent.
5. The high durometer polymer cell of claim 4, wherein the nano conductive carbon is graphene and multi-walled carbon nanotubes; the dispersing agent is saturated fatty acid modified acrylate, N-vinyl pyrrolidone and alpha, beta-vinyl unsaturated acid.
6. The high stiffness polymer cell of claim 1, wherein the lithium salt is at least one of lithium bis-fluorosulfonylimide, lithium bis-trifluoromethylsulfonyl imide, lithium bis (trifluoromethylsulfonyl) imide, lithium bis (pentafluoroethylsulfonyl) imide, lithium difluorooxalato borate, lithium bis-fluorosulfonylimide, and lithium difluorooxalato borate.
7. The high stiffness polymer cell of claim 1, wherein the polyvinyl chloride plasticized composition comprises the following components in percent by mass: 55-85% of polyvinyl chloride and 15-45% of plasticizer, wherein the plasticizer is succinate and epoxidized castor oil.
8. The high-hardness polymer cell of claim 1, wherein the electrolyte is added as at least one of a surfactant, a film-forming aid, a wetting agent, and a flame retardant.
9. The high-hardness polymer cell core according to claim 8, wherein the film-forming assistant is at least one of vinylene carbonate, fluoroethylene carbonate, ethylene carbonate, propiolactone sulfonate, butyrolactone sulfonate, ethylene sulfate, ethylene sulfite, butylene sulfite, biphenyl, and succinonitrile.
10. A method of making a high stiffness polymer cell according to any of claims 1 to 9, comprising the steps of:
a. ball-milling the polymer at a high speed until the particle size is less than 1 mu m, adding an organic solvent and an additive, and uniformly dispersing to obtain a polymer solution; mixing the lithium salt, the polyvinyl chloride plasticizing composition and an electrolyte additive, and uniformly dispersing to obtain an electrolyte;
b. coating the polymer solution on the surface of at least one positive pole piece and/or negative pole piece, and drying in vacuum at 70-85 ℃ under 1-6Mpa for 60s-30min to form a gel layer;
c. b, soaking the positive pole piece and/or the negative pole piece obtained in the step b in electrolyte for 5-60min to obtain a gel electrolyte layer;
d. and overlapping and laminating at least one positive pole piece and at least one negative pole piece to obtain the high-hardness polymer battery cell.
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2020
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| CN1152342A (en) * | 1995-04-25 | 1997-06-18 | 弗朗西斯P·麦克卡洛 | Flexible ignition resistant biregional fiber, articles made from biregional fibers and method of manufacture |
| CN103178303A (en) * | 2013-01-22 | 2013-06-26 | 东莞新能源科技有限公司 | Method for preparing polymer gel electrolyte cell |
| CN105703004A (en) * | 2016-03-31 | 2016-06-22 | 成都国珈星际固态锂电科技有限公司 | Gel electrolyte battery core, gel polymer lithium-ion battery, preparation methods thereof and electric vehicle |
| CN106450474A (en) * | 2016-11-07 | 2017-02-22 | 上海碳源汇谷新材料科技有限公司 | Gelled polymer electrolyte membrane and preparation method thereof |
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