CN111769323B - High-hardness polymer battery cell and preparation method thereof - Google Patents
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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 electrode plate, at least one positive electrode plate and at least one gel electrolyte layer; the gel electrolyte layer is prepared by absorbing electrolyte after gel layers are formed on the surfaces of at least one positive electrode plate and/or negative electrode plate by polymer solution; 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 core has excellent electrochemical performance, high conductivity, good multiplying power 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 carbonate organic solvent. For liquid electrolytes, there are limited suitable anode materials; the liquid electrolyte is easy to decompose to generate gas in the discharging process, and form excessive vapor pressure, so that the cell shell is easy to corrode, and liquid leakage is caused; the ignition point and 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, the internal temperature of the battery is increased in the charging and discharging process, and safety problems such as fire explosion and the like are very easy to occur; consumption of electrolyte also reduces battery life. The polymer battery has the advantages of high voltage, large specific energy, stable discharge flattening, good cycle performance, good safety performance, long storage life and the like, and the technical problems can be effectively solved by using the polymer gel electrolyte to replace the organic system liquid electrolyte.
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. Both methods are to initiate polymerization of polymer monomers by an initiator in an organic environment containing a plasticizer under a high temperature environment to form a high molecular polymer matrix. Thermal expansion and thermal bulging may occur in the thermal polymerization process, the thermal polymerization reaction is incomplete, and the remaining monomer may affect the electrochemical performance of the battery. The high-hardness polymer battery core has excellent electrochemical performance, high conductivity, good multiplying power performance and cycle performance, high hardness and good safety. Due to the existence of the small molecular solvent, the gel polymer electrolyte has the defects of higher volatility, poor electrochemical stability and thermal stability, low mechanical strength, poor interface stability between the electrolyte and the electrode, 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 multiplying power 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 electrode plate, at least one positive electrode plate and at least one gel electrolyte layer; the gel electrolyte layer is prepared by absorbing electrolyte after gel layers are formed on the surfaces of at least one positive electrode plate and/or negative electrode plate by polymer solution; 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, polyalcohol polyacrylate, polystyrene, polyethylene and methyl methacrylate.
Further, the organic solvent is at least one of N-methylpyrrolidone, dimethyl sulfoxide, dimethylformamide, ethyl acetate, ethylene carbonate, propylene carbonate, butylene carbonate, 1, 2-dimethylethylene carbonate, ethylene carbonate, methyl butyl carbonate, dibutyl carbonate, diethyl carbonate, dimethyl carbonate, trifluoromethyl ethylene carbonate, di-N-propyl carbonate, diisopropyl carbonate, methyl ethyl carbonate, ethylene propyl carbonate, ethylene isopropyl carbonate, methyl propyl 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, γ -butyrolactone, methyl formate, ethyl formate, methyl acetate, methyl propionate, ethyl propionate, methyl butyrate, ethyl butyrate, ethylene carbonate, propane sultone, ethylene sulfite.
Further, the additive is composed of 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 multi-wall carbon nano tubes; the dispersing agent is saturated fatty acid modified acrylic ester, N-vinyl pyrrolidone and alpha, beta-vinyl unsaturated acid.
Further, the lithium salt is at least one of lithium bis (fluorosulfonyl) imide, lithium bis (trifluoromethylsulfonyl) imide, lithium bis (pentafluoroethylsulfonyl) imide, lithium difluorooxalato borate, lithium bis (fluorosulfonyl) imide, and lithium difluorooxalato borate.
Further, the polyvinyl chloride plasticizing 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 auxiliary agent, a wetting agent and a flame retardant.
Further, the film forming additive is at least one of ethylene carbonate, fluoroethylene carbonate, ethylene carbonate, sultone, sulfobutyrolactone, ethylene sulfate, ethylene sulfite, butylene sulfite, biphenyl and succinonitrile.
The preparation method of the high-hardness polymer battery cell comprises the following steps:
a. ball milling the polymer at high speed until the particle size is less than 1 mu m, adding an organic solvent and an additive, and uniformly dispersing to prepare a polymer solution; mixing lithium salt, polyvinyl chloride plasticizing composition and electrolyte additive, and uniformly dispersing to obtain electrolyte;
b. coating the polymer solution on the surface of at least one positive electrode plate and/or negative electrode plate, vacuum drying at 70-85 ℃, drying pressure of 1-6Mpa, drying time of 60s-30min, and forming a gel layer after drying;
c. c, soaking the positive electrode plate and/or the negative electrode plate obtained in the step b in electrolyte for 5-60min to obtain a gel electrolyte layer;
d. and arranging at least one positive pole piece and at least one negative pole piece in a laminated mode to obtain the high-hardness polymer battery cell.
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 5-60min.
The invention has the following beneficial effects:
the polymer solution selected by the invention can be dried in vacuum to form a gel layer with a porous net structure on the surface of the positive electrode plate and/or the negative electrode plate in situ, the compatibility between the gel layer and the electrode plate interface is good, the gel surface is in a completely dry state, the liquid locking capacity of the hole structure on the gel surface is strong, the liquid retention stability is good, and the adsorption quantity of electrolyte in the gel electrolyte layer can be greatly improved. The nanometer 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 liquid can be adsorbed in the bracket structure, so that the adsorption quantity of the gel layer to the electrolyte is further improved, the transmission of lithium ions in the gel polymer is enhanced, the ion conductivity is improved, and the hardness of a lithium ion battery is improved; the nanometer conductive carbon has stable electrochemical property and thermal stability, and can improve the temperature and safety of the internal structure of the battery in the charge and discharge process.
The electrolyte selected by the invention comprises a polyvinyl chloride plasticizing composition, wherein an organic solvent and a polymer have good compatibility, the plasticizing effect of the plasticizer is promoted, the conduction effect of lithium ions in the polymer is improved, and the conductivity of a lithium battery and the mechanical strength of a gel layer are effectively improved. By adjusting the types and the proportion of lithium salt in the electrolyte, the formation reaction of the SEI film can be controlled, and the components and the properties of the SEI film are adjusted, so that the improvement of the cycling performance of the electrode is realized.
Detailed Description
The present invention will be described in detail with reference to the following examples, which are only preferred embodiments of the present invention and are not limiting thereof.
Example 1
A high-hardness polymer battery cell comprises a negative electrode plate, a positive electrode plate and four gel electrolyte layers; the gel electrolyte layer is prepared by absorbing electrolyte after gel layers formed on the surfaces of the positive electrode plate and the negative electrode plate by polymer solution;
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 is composed of 60% of nano conductive carbon, 20% of polyvinylidene fluoride and 20% of dispersing agent; the nanometer conductive carbon is graphene and multi-wall carbon nanotubes; the dispersing agent is saturated fatty acid modified acrylic ester, 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 plasticizing 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 auxiliary agent; the film forming auxiliary agent is fluoroethylene carbonate, biphenyl and succinonitrile.
Example 2
A high-hardness polymer battery cell comprises a negative electrode plate, a positive electrode plate and four gel electrolyte layers; the gel electrolyte layer is prepared by absorbing electrolyte after gel layers formed on the surfaces of the positive electrode plate and the negative electrode plate by polymer solution;
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-methyltetrahydrofuran; the additive is 70% of nano conductive carbon, 15% of polyvinylidene fluoride and 15% of dispersing agent; the nanometer conductive carbon is graphene and multi-wall carbon nanotubes; the dispersing agent is saturated fatty acid modified acrylic ester, N-vinyl pyrrolidone and alpha, beta-vinyl unsaturated acid;
the electrolyte comprises the following components in percentage by mass: 20% of lithium salt, 40% of polyvinyl chloride plasticizing composition and 40% of electrolyte additive; the lithium salt is lithium bis (trifluoromethyl) sulfonyl imide and lithium difluoro (oxalato) borate; the polyvinyl chloride plasticizing 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 auxiliary agent; the film forming auxiliary agent is fluoroethylene carbonate and ethylene carbonate.
Example 3
A high-hardness polymer battery cell comprises a negative electrode plate, a positive electrode plate and four gel electrolyte layers; the gel electrolyte layer is prepared by absorbing electrolyte after gel layers formed on at least the surfaces of the positive electrode plate and the negative electrode plate by polymer solution;
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 vinylidene fluoride-hexafluoropropylene copolymer; the organic solvent is 1, 2-dimethyl ethylene carbonate, sulfolane, 4-methyl-1, 3-butyrolactone and ethylene sulfite; the additive is composed of 60% of nano conductive carbon, 20% of polyvinylidene fluoride and 20% of dispersing agent; the nanometer conductive carbon is graphene and multi-wall carbon nanotubes; the dispersing agent is saturated fatty acid modified acrylic ester, 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 plasticizing composition and 65% of electrolyte additive; the lithium salt is lithium bis (trifluoromethylsulfonyl) and lithium difluoro oxalato borate; the polyvinyl chloride plasticizing 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.
The preparation method of the high-hardness polymer battery cell in the embodiment 1-3 comprises the following steps:
a. ball milling the polymer at high speed until the particle size is less than 1 mu m, adding an organic solvent and an additive, and uniformly dispersing to prepare a polymer solution; mixing lithium salt, polyvinyl chloride plasticizing composition and electrolyte additive, and uniformly dispersing to obtain the electrolyte, wherein 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 5-60min.
b. Coating the polymer solution on the surface of at least one positive electrode plate and/or negative electrode plate, vacuum drying at 70-85 ℃, drying pressure of 1-6Mpa, drying time of 60s-30min, and forming a gel layer after drying;
c. c, soaking the positive electrode plate and/or the negative electrode plate obtained in the step b in electrolyte for 5-60min to obtain a gel electrolyte layer;
d. and arranging at least one positive pole piece and at least one negative pole piece in a laminated mode 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 plasticizing composition with the plasticizer ethyl acetate.
Comparative example 3
The only difference from example 1 is that the lithium salt described 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 additives without high-speed ball milling.
The high hardness polymer cells of the present invention were tested for various properties in examples 1-3 and comparative examples 1-3:
(1) Hardness testing: AI7000S type high-speed railway tension meter, test module and battery cell plane major axis direction central point position coincidence, bending strength; the advancing speed of the probe module is 10mm/min. Recording a deformation amount and tension strength curve, and uniformly taking the tension when the deformation amount of the battery cell is 0.5mm as the hardness of the battery cell;
(2) Capacity and cycle performance test: charging to 4.2V with 0.5C constant current, standing for 5 min, charging to 40mA with 4.2V constant voltage, standing for 5 min, discharging to 3.0V with 0.5C current, and recording discharge curve and discharge capacity; after standing for 15 minutes, repeating the steps n times;
(3) And (3) multiplying power performance test: the method is the same as the capacity test, the charging is uniformly carried out by adopting 0.5C full charge, when the charging is carried out, 0.2C,0.5C,1C,1.5C and 2C are respectively discharged to 3.0V cut-off, and the discharge capacity of 0.2C is taken as a reference, the discharge capacity of 2C is divided by the discharge capacity of 0.2C, and the closer the capacity percentage of 2C/0.2C is to 100%, the more excellent the multiplying power performance of the battery cell is shown;
(4) Nailing test: the testing method comprises the steps of automatically penetrating through a nail, testing a stainless steel nail with the diameter of 3mm and the nail advancing speed of 10mm/S, and testing a temperature curve of the adjacent position of the penetrating part of the electric core by using a multi-path thermometer. Quantitatively recording a temperature rise curve and a peak temperature of the battery cell, and qualitatively recording whether the battery cell emits smoke, fires and burns;
the test results are shown in the following table:
the high-hardness polymer battery cell has high capacity retention rate, good electrical property, high hardness and good safety.
Claims (7)
1. The high-hardness polymer battery cell is characterized by comprising at least one negative electrode plate, at least one positive electrode plate and at least one gel electrolyte layer; the gel electrolyte layer is prepared by absorbing electrolyte after gel layers are formed on the surfaces of at least one positive electrode plate and/or negative electrode plate by polymer solution;
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 additive is 60-80% of nano conductive carbon, 10-20% of polyvinylidene fluoride and 10-20% of dispersing agent;
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 polyvinyl chloride plasticizing composition comprises the following components in percentage by mass: 55-85% of polyvinyl chloride and 15-45% of plasticizer, wherein the plasticizer is succinate and epoxidized castor oil;
the electrolyte additive is at least one of a surfactant, a film forming auxiliary agent, a wetting agent and a flame retardant.
2. The high hardness polymer cell of claim 1, wherein the polymer is at least one of polymethyl methacrylate, polyacrylonitrile, polyethylene oxide, polyvinylidene fluoride, vinylidene fluoride-hexafluoropropylene copolymer, polyacrylate, polyalcohol polyacrylate, polystyrene, polyethylene, and methyl methacrylate.
3. The high hardness polymer battery cell of claim 1, wherein the organic solvent is at least one of N-methylpyrrolidone, dimethyl sulfoxide, dimethylformamide, ethyl acetate, ethylene carbonate, propylene carbonate, butylene carbonate, 1, 2-dimethylethylene carbonate, ethylene carbonate, methyl butyl carbonate, dibutyl carbonate, diethyl carbonate, dimethyl carbonate, trifluoromethylethylene carbonate, di-N-propyl carbonate, diisopropyl carbonate, methylethyl carbonate, ethylene propyl carbonate, ethylene isopropyl 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, γ -butyrolactone, methyl formate, ethyl formate, methyl acetate, methyl propionate, ethyl propionate, methyl butyrate, ethyl butyrate, ethylene carbonate, propane sultone, and ethylene sulfite.
4. The high hardness polymer cell of claim 3, wherein the nano-conductive carbon is graphene and multi-walled carbon nanotubes; the dispersing agent is saturated fatty acid modified acrylic ester, N-vinyl pyrrolidone and alpha, beta-vinyl unsaturated acid.
5. The high hardness polymer battery cell of claim 1, wherein the lithium salt is at least one of lithium bis (fluorosulfonyl) imide, lithium bis (trifluoromethylsulfonyl) imide, lithium bis (pentafluoroethylsulfonyl) imide, lithium difluorooxalato borate, lithium bis (fluorosulfonyl) imide, lithium difluorooxalato borate.
6. The high hardness polymer cell of claim 1, wherein the film forming aid is at least one of vinylene carbonate, fluoroethylene carbonate, ethylene carbonate, sultone, butyrolactone, ethylene sulfate, ethylene sulfite, butylene sulfite, biphenyl, succinonitrile.
7. A method for preparing a high hardness polymer cell according to any one of claims 1 to 6, comprising the steps of:
a. ball milling the polymer at high speed to particle size smaller than 1 micron, adding organic solvent and additive, dispersing homogeneously to obtain the final product
A solution of matter; mixing lithium salt, polyvinyl chloride plasticizing composition and electrolyte additive, and uniformly dispersing to obtain electrolyte;
b. coating the polymer solution on the surface of at least one positive electrode plate and/or negative electrode plate, vacuum drying at 70-85 ℃, drying pressure of 1-6Mpa, drying time of 60s-30min, and forming a gel layer after drying;
c. c, soaking the positive electrode plate and/or the negative electrode plate obtained in the step b in electrolyte for 5-60min to obtain a gel electrolyte layer;
d. and arranging at least one positive pole piece and at least one negative pole piece in a laminated mode to obtain the high-hardness polymer battery cell.
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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 |
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