CN110335991B - Long-cycle-life battery and manufacturing method thereof - Google Patents

Long-cycle-life battery and manufacturing method thereof Download PDF

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CN110335991B
CN110335991B CN201910632961.7A CN201910632961A CN110335991B CN 110335991 B CN110335991 B CN 110335991B CN 201910632961 A CN201910632961 A CN 201910632961A CN 110335991 B CN110335991 B CN 110335991B
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battery
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negative
constant current
electrolyte
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CN110335991A (en
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郑康
胡金星
张宝华
娄勇刚
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Camel Group Wuhan Optics Valley R&d Center Co ltd
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Camel Group Wuhan Optics Valley R&d Center Co ltd
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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
    • 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
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
    • H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
    • H01M10/0566—Liquid materials
    • H01M10/0567—Liquid materials characterised by the additives
    • 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
    • H01M10/058—Construction or manufacture
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139—Processes of manufacture
    • H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/64—Carriers or collectors
    • H01M4/66—Selection of materials
    • H01M4/661—Metal or alloys, e.g. alloy coatings
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/64—Carriers or collectors
    • H01M4/66—Selection of materials
    • H01M4/663—Selection of materials containing carbon or carbonaceous materials as conductive part, e.g. graphite, carbon fibres
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/64—Carriers or collectors
    • H01M4/66—Selection of materials
    • H01M4/665—Composites
    • H01M4/667—Composites in the form of layers, e.g. coatings
    • 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
    • H01M50/10—Primary casings, jackets or wrappings of a single cell or a single battery
    • H01M50/116—Primary casings, jackets or wrappings of a single cell or a single battery characterised by the material
    • H01M50/124—Primary casings, jackets or wrappings of a single cell or a single battery characterised by the material having a layered structure
    • 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
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

Abstract

The invention relates to the technical field of lithium batteries, in particular to a battery with long cycle life and a manufacturing method thereof. In order to meet the requirement of a power battery on long service life, a long-cycle-life lithium ion monomer battery is developed, a battery system is nickel-cobalt lithium manganate and lithium titanate, the lithium-nickel lithium ion monomer battery comprises a positive plate, a negative plate, a diaphragm, electrolyte and a packaging film, positive and negative dressing materials are coated on a carbon-coated aluminum foil, a high-porosity base film is adopted for lamination, an aluminum-plastic packaging film and the long-life electrolyte are adopted for packaging and liquid injection, the long-cycle-life battery is prepared by adopting a high-temperature high-pressure formation-aging process, and the problem of low cycle life of the.

Description

Long-cycle-life battery and manufacturing method thereof
Technical Field
The invention relates to the technical field of lithium batteries, in particular to a battery with long cycle life and a manufacturing method thereof.
Background
With the progress of the times and the development of technologies, the requirements on lithium ion batteries are higher and higher. Lithium ion batteries need to have not only high energy density, power density and high safety, but also long service life, and especially in the fields of electric vehicles and large-scale energy storage, the requirement on the service life of the lithium ion batteries is higher and higher.
The lithium ion power battery is used as a core component of an electric automobile, the lithium ion power battery has better safety performance and is a lithium iron phosphate system, the single-core cycle life of the lithium iron phosphate system is 1C which is more than or equal to 3000 times, the lithium iron phosphate system is mainly applied to a pure electric passenger car, but the energy density of the lithium iron phosphate system is obviously insufficient along with the development of a pure electric/plug-in hybrid power passenger car, a ternary system (NCM) gradually becomes a main battery of the pure electric passenger car due to higher energy density, the single-core cycle life of the lithium iron phosphate system is 1C which is more than or equal to 2000 times.
Therefore, in order to satisfy the use requirements of the power battery by taking safety and long cycle life into consideration, a lithium ion battery with long cycle life needs to be developed.
Disclosure of Invention
The invention discloses a lithium ion single battery with long cycle life, which is designed to meet the requirement of a power supply system on the long cycle life of the battery.
The technical purpose of the invention is realized by the following technical scheme:
the battery with long cycle life comprises a positive plate, a negative plate, a diaphragm, electrolyte and a packaging film, wherein the electrolyte comprises a solvent, electrolyte and an additive, the solvent is a mixture of ethyl methyl carbonate, diethyl carbonate and ethylene carbonate, and the electrolyte is LiPF6、LiClO4、LiBF4、LiAsF6、LiB(C6F5)3(CF3)、LiCF3SO3Is a combination of vinylene carbonate, succinonitrile and fluoroether 1, 1, 2, 2-tetrafluoroethyl-2, 2, 3, 3-tetrafluoropropyl ether.
Further, the mass ratio of vinylene carbonate, succinonitrile and fluorine-containing ether 1, 1, 2, 2-tetrafluoroethyl-2, 2, 3, 3-tetrafluoropropyl ether in the additive is 9-12: 1: 1.
furthermore, the mass fraction of the electrolyte in the electrolyte is 13-26%, and the mass fraction of the additive in the electrolyte is 3.5-7.0%.
Further, the positive plate comprises a positive carbon-coated aluminum foil current collector and a positive dressing, the negative plate comprises a negative carbon-coated aluminum foil current collector and a negative dressing, and the positive dressing comprises the following components in percentage by mass: 90-96% of positive active substance, 2-5% of positive conductive agent and 2-5% of positive binder.
Further, the negative electrode dressing comprises the following components in percentage by mass: 89-96% of negative electrode active material, 2-6% of negative electrode conductive agent and 2-5% of negative electrode binder; the negative active material is lithium titanate Li4Ti5O12。
Further, the negative electrode adhesive is a mixture of one or two of polyvinylidene fluoride and polytetrafluoroethylene and styrene butadiene rubber, and the negative electrode conductive agent is one or a mixture of more of conductive carbon black SP, conductive graphite KS-6 and carbon nano tubes.
Further, the positive electrode active material is LiNi0.5Co0.2Mn0.3O2、LiNi0.6Co0.2Mn0.2O2And LiFemNPO4One or more mixtures thereof.
The invention also provides a manufacturing method for preparing the long-cycle-life lithium ion battery, which comprises the following steps:
s1: manufacturing a positive plate and a negative plate: dissolving a positive electrode material in an organic solvent, uniformly stirring to prepare a positive electrode dressing, coating the positive electrode dressing on a carbon-coated aluminum foil, drying in an oven at 100-120 ℃, and rolling to obtain a positive electrode plate; dissolving a negative electrode material in an organic solvent, uniformly stirring to prepare a negative electrode dressing, coating the negative electrode dressing on the carbon-coated aluminum foil, drying in an oven at 100-120 ℃, and rolling to obtain a negative electrode sheet;
s2: baking the pole piece: placing the positive and negative pole pieces into a vacuum oven for baking at the temperature of 120-140 ℃ for 40-50h, continuously vacuumizing, changing air every 2h, and controlling the moisture content of the positive and negative pole pieces to be less than or equal to 200 ppm;
s3: manufacturing an electric core: die-cutting the positive and negative plates obtained in the step S2, and then manufacturing the battery cell by adopting a laminated structure or a winding structure according to the sequence of the diaphragm, the negative plate, the diaphragm, the positive plate and the diaphragm;
s4: and (3) welding and packaging: welding a positive plate and a negative plate in a battery cell with an aluminum tab to form a positive lead-out end and a negative lead-out end, putting the battery cell into an aluminum-plastic packaging film, leading out the positive tab and the negative tab respectively, heating the tab glue to fuse the plastic of an aluminum-plastic bag with the tab glue to obtain a soft package battery, wherein one side of the soft package battery is in an open state, and after an electrolyte is injected;
s5: packaging and injecting liquid: after the electrolyte is injected into the battery core, the electrolyte injection port is sealed;
s6: formation and aging: and (3) forming, aging and secondary sealing the packaged battery, and then carrying out capacity grading to obtain the lithium ion battery with long cycle life.
Further, the temperature of the battery formation process in the step S6 is 60-80 ℃, the formation pressure is 0.3-0.6MPa, and the final cut-off voltage is 1.5-2.0V when the battery formation is finished; the aging temperature is 60-80 ℃, the aging pressure is 0.3-0.6MPa, and the aging time is 48-60 h.
Further, the formation process in step S6 includes the following steps:
(1) charging the battery for 5 hours at a constant current of 0.02-0.03C;
(2) charging the battery for 5 hours at a constant current of 0.05-0.06C;
(3) charging the battery for 2h at a constant current of 0.1C;
(4) charging the battery for 2h at a constant current of 0.2C;
(5) taking out the battery, standing for 1h at room temperature, and then performing first air extraction; continuing to form after air exhaust is completed;
(6) performing constant current discharge on the battery for 5h at the current of 0.2C;
(7) charging the battery for 5 hours at a constant current of 0.02-0.03C;
(8) charging the battery for 6 hours at a constant current of 0.05-0.06C;
(9) charging the battery for 5 hours at a constant current of 0.1C;
(10) taking out the battery, standing for 1h at room temperature, and then performing secondary air extraction; continuing to form after air exhaust is completed;
(11) performing constant current discharge on the battery for 5h at the current of 0.2C;
(12) charging the battery for 7 hours at a constant current of 0.05-0.06C;
(13) charging the battery for 6h at a constant current of 0.1C;
(14) the cell was discharged for 5h at a constant current of 0.2C.
The invention has the beneficial effects that:
1. the invention develops a long-cycle-life ionic monomer battery, wherein a nickel cobalt lithium manganate system is adopted as a positive electrode of the battery, a lithium titanate system is adopted as a negative electrode of the battery to coat positive and negative electrode dressings containing an active substance, a binder and a conductive agent on a carbon-coated aluminum foil, a high-porosity base film is adopted for lamination, an aluminum-plastic packaging film and a special long-life electrolyte are adopted for packaging and injecting, and a novel high-temperature high-pressure formation-aging process is matched to prepare the long-cycle-life battery, so that the problem of low cycle life of the lithium ion battery is effectively solved.
2. The electrolyte of the battery adopts the composition of a film-forming additive, namely vinylene carbonate, succinonitrile and fluoroether 1, 1, 2, 2-tetrafluoroethyl-2, 2, 3, 3-tetrafluoropropyl ether, and the three substances have synergistic effect, so that gas generation in the circulation process of a lithium titanate battery is avoided, the circulation stability of the battery is improved, and the circulation performance of the battery is greatly improved.
3. The lithium titanate material adopted by the negative electrode can continuously generate gas in the cycle use due to the characteristics of the lithium titanate material, so that the battery pack is swelled, the contact of the positive electrode and the negative electrode is affected, the impedance of the battery is increased, and the performance of the battery is affected, the invention adds two charging and discharging cycles on the basis of the existing formation process, adds two air pumping steps among three formation stages, pumps out the internal gas after the gas generation of the battery, increases two charging and discharging cycles, avoids the occurrence of side reactions, and the actual test result proves that the battery produced by adopting the process of the invention does not generate gas after 6C cycles at normal temperature for 15000 times, thereby greatly improving the stability of the battery.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 is a graph of room temperature 6C cycles with the abscissa of the sample being the number of cycles and the ordinate being the percent volume, wherein reference numeral 1 is example 1, reference numeral 2 is example 2, reference numeral 3 is example 3, reference numeral 4 is example 4 and reference numeral 5 is a comparative example.
Detailed Description
The technical solution of the present invention will be clearly and completely described below with reference to the specific embodiments. It is to be understood that the described embodiments are merely a few embodiments of the invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without making any creative effort, shall fall within the protection scope of the present invention.
In the invention, EMC is ethyl methyl carbonate, DEC is diethyl carbonate, EC is ethylene carbonate, VC is vinylene carbonate, SN is succinonitrile, D2 is fluorine-containing ether 1, 1, 2, 2-tetrafluoroethyl-2, 2, 3, 3-tetrafluoropropyl ether, and PE is polyethylene.
A long cycle life battery and a manufacturing method thereof are disclosed, which comprises the following embodiments:
example 1
A method for manufacturing a long-cycle-life lithium ion battery comprises the following steps:
s1: a. manufacturing a positive plate: firstly, polyvinylidene fluoride (PVDF) and N-methyl pyrrolidone (NMP) are prepared into a solution with the mass fraction of 6.7% for standby. Adding half of positive active material LiNi-Co-Mn acid lithium into a new material preparing cylinder0.5Co0.2Mn0.3O2And a conductive agent SP, stirring at a low speed for 20min, and then adding 1/3 amounts of PVDF glue solution and the other half of positive electrode active material nickel cobalt lithium manganate LiNi0.5Co0.2Mn0.3O2Stirring at low speed for 30min, adding 1/3 wt% PVDF glue solution and conductive agent KS-6, stirring at low speed for 60min, adding 1/3 wt% PVDF glue solution, adding NMP solvent to adjust solid content to 68%, and stirring at high speed for 180 min. Testing the viscosity in the range of 4000-8000mPa.s, sieving with a 150-mesh double-layer metal net, uniformly coating the sieved positive dressing on a 17-mu m-thick carbon-coated aluminum foil to form a positive pole piece, drying at 120 ℃, and feeding the dried positive pole piece into a drying furnaceLine rolling, the thickness of the rolled positive plate is 81 μm, and the compaction density is 2.8g/cm3(ii) a The positive dressing comprises the following components in percentage by mass: 91% of positive electrode active material and 5% of positive electrode conductive agent, wherein the mass ratio of the carbon black conductive agent SP to the carbon nano tube is 3: 2, 3% of positive electrode binder;
b. manufacturing a negative plate: preparing solution with mass fraction of 60% by using Polytetrafluoroethylene (PTFE) and deionized water, adding a conductive agent SP, stirring at a low speed for 45min, adding a conductive agent KS-6, stirring at a low speed for 45min, then stirring at a high speed for 60min, and then adding half of lithium titanate Li4Ti5O12Stirring at low speed for 60min, and adding the other half amount of lithium titanate Li4Ti5O12Stirring at low speed for 60min, stirring at high speed for 180min, adding deionized water to adjust solid content to 55%, and stirring at high speed for 120 min. Testing the viscosity in the range of 4000-8000mPa.s, sieving by a 150-mesh double-layer metal net, uniformly coating the negative dressing prepared by sieving on a carbon-coated aluminum foil with the thickness of 17 mu m to form a negative pole piece, drying at 120 ℃, rolling the dried negative pole piece, wherein the rolled thickness of the negative pole piece is 107 mu m, and the compaction density is 1.8g/cm3(ii) a The negative dressing comprises the following components in percentage by mass: 89% of negative electrode active material and 6% of negative electrode conductive agent, wherein the mass ratio of carbon black conductive agent SP to carbon nano tube is 4: 2 and 5% of negative electrode binder.
S2: baking the pole piece: and (3) putting the positive and negative pole pieces into a vacuum oven, baking for 48h at 120 ℃, continuously vacuumizing, changing gas every 2h, and controlling the water content of the positive and negative pole pieces to be less than or equal to 200 pm.
S3: manufacturing an electric core: and (4) cutting the positive and negative plates obtained in the step (S2), and preparing the battery cell by adopting a laminated structure according to the sequence of the diaphragm-the negative plate-the diaphragm-the positive plate-the diaphragm-the negative plate-the diaphragm, wherein the diaphragm is a wet-process PE diaphragm, the thickness of the diaphragm is 12 microns, the porosity of the diaphragm is 50%, and the air permeability of the diaphragm is 150S/100 mL.
S4: and (3) welding and packaging: welding positive and negative plates in the battery core with aluminum tabs respectively to form positive and negative lead-out ends, putting the battery core into an aluminum-plastic packaging film, leading out the positive and negative tabs respectively, heating the tab glue position to fuse the plastic film PP glue of the aluminum-plastic bag with the tab glue, and leaving the right side of the battery in an open state for electrolyte injection.
S5: packaging and injecting liquid: after the electrolyte is injected into the battery core, the electrolyte injection port is sealed; wherein the electrolyte solvent is a mixture of ethyl methyl carbonate, diethyl carbonate and ethylene carbonate (the proportion is 1:1: 4); the electrolyte is LiPF6；LiPF6The concentration is 1.6mol/L, the mass fraction of the electrolyte in the electrolyte is 13%, the additive is a mixture of SN and D2 with the mass fraction of 3.5%, and the mass ratio of the components is 1: 1.
7) formation and aging: the temperature of the hot-pressing formation cabinet is set to 80 ℃, and the pressure of the clamp is set to 0.3 MPa.
(1) Charging the battery for 5 hours at a constant current of 0.02C;
(2) charging the battery for 5 hours at a constant current of 0.05C;
(3) charging the battery for 2h at a constant current of 0.1C;
(4) charging the battery for 2h at a constant current of 0.2C;
(5) taking out the battery, standing for 1h at room temperature, and then performing first air extraction; continuing to form after air exhaust is completed;
(6) performing constant current discharge on the battery for 5h at the current of 0.2C;
(7) charging the battery for 5 hours at a constant current of 0.02C;
(8) charging the battery for 6h at a constant current of 0.05C;
(9) charging the battery for 5 hours at a constant current of 0.1C;
(10) taking out the battery, standing for 1h at room temperature, and then performing secondary air extraction; continuing to form after air exhaust is completed;
(11) performing constant current discharge on the battery for 5h at the current of 0.2C;
(12) charging the battery for 7h at a constant current of 0.05C;
(13) charging the battery for 6h at a constant current of 0.1C;
(14) the cell was discharged for 5h at a constant current of 0.2C.
Wherein the final cut-off voltage at the end of the formation is 1.5-2.0V. And after the formation is finished, the battery continues to be aged on the formation cabinet.
Example 2
A method for manufacturing a long-cycle-life lithium ion battery comprises the following steps:
s1: a. manufacturing a positive plate: firstly, preparing polyvinylidene fluoride (PVDF) and N-methyl pyrrolidone (NMP) into a solution with the mass fraction of 6.7%, then adding a conductive agent SP, stirring at a low speed for 45min, adding a conductive agent KS-6, stirring at a low speed for 45min, then stirring at a high speed for 60min, and then adding half of LiNi-Co lithium manganate LiNi0.6Co0.2Mn0.2O2Stirring at low speed for 60min, and adding the other half amount of LiNi0.6Co0.2Mn0.2O2Stirring at low speed for 60min, stirring at high speed for 120min, adding NMP solvent to adjust solid content to 68%, and stirring at high speed for 120 min. Testing the viscosity within the range of 4000-3(ii) a The positive dressing comprises the following components in percentage by mass: 96% of positive electrode active material and 10% of positive electrode conductive agent, wherein the mass ratio of the carbon black conductive agent SP to the graphite conductive agent KS-6 is 1:1, and the positive electrode binder is 10%.
b. Manufacturing a negative plate: preparing Styrene Butadiene Rubber (SBR) and deionized water into a solution with the mass fraction of 1.5%, adding a conductive agent SP, stirring at a low speed for 45min, adding a conductive agent KS-6, stirring at a low speed for 45min, then stirring at a high speed for 60min, and then adding half of lithium titanate Li4Ti5O12Stirring at low speed for 60min, and adding the other half amount of lithium titanate Li4Ti5O12Stirring at low speed for 60min, stirring at high speed for 180min, adding deionized water to adjust solid content to 55%, and stirring at high speed for 120 min. After the viscosity is tested to be within the range of 3000-6000mPa.s, sieving the mixture by using a 150-mesh double-layer metal net to prepare a negative dressing, uniformly coating the negative dressing on a 17-mu m-thick carbon-coated aluminum foil, drying the negative dressing at 120 ℃, rolling the dried negative pole piece, wherein the rolled thickness of the negative pole piece is 107 mu m, and the compaction density is 1.8g/cm 3; the mass percentage of each component in the negative dressing is: 94% of negative electrode active material and 9% of negative electrode conductive agent, wherein the mass ratio of carbon black conductive agent SP to graphite conductive agent KS-6 is 1:1 and 7 percent of negative electrode binder.
S2: baking the pole piece: and (3) putting the pole piece into a vacuum oven for baking for 48h at 140 ℃, continuously vacuumizing, changing gas every 2h, and controlling the moisture content of the positive pole piece and the negative pole piece to be less than or equal to 200 pm.
S3: manufacturing an electric core: and (4) cutting the positive and negative plates obtained in the step (S2), and preparing the battery cell by adopting a laminated structure according to the sequence of the diaphragm-the negative plate-the diaphragm-the positive plate-the diaphragm-the negative plate-the diaphragm, wherein the diaphragm is a wet-process PE diaphragm, the thickness of the diaphragm is 12 microns, the porosity of the diaphragm is 50%, and the air permeability of the diaphragm is 150S/100 mL.
S4: and (3) welding and packaging: welding positive and negative plates in the battery core with aluminum tabs respectively to form positive and negative lead-out ends, putting the battery core into an aluminum-plastic packaging film, leading out the positive and negative tabs respectively, heating the tab glue position to fuse the PP glue of the aluminum-plastic film with the tab glue, and leaving the right side of the battery in an open state for electrolyte injection.
S5: packaging and injecting liquid: after the electrolyte is injected into the battery core, the electrolyte injection port is sealed; wherein the electrolyte solvent is a mixture of ethyl methyl carbonate, diethyl carbonate and ethylene carbonate (the ratio is 1:1: 4); the electrolyte contains LiPF6；LiPF6The concentration is 1.6mol/L, the mass fraction of the electrolyte in the electrolyte is 26%, the additive is a mixture of VC, SN and D2 with the mass fraction of 7.0%, and the mass ratio of the components is 12: 1: 1.
s6: formation and aging: the temperature of the hot-pressing formation cabinet is set to be 100 ℃, and the pressure of the clamp is set to be 0.6 Mpa.
(1) Charging the battery for 5 hours at a constant current of 0.02C;
(2) charging the battery for 5 hours at a constant current of 0.05C;
(3) charging the battery for 2h at a constant current of 0.1C;
(4) charging the battery for 2h at a constant current of 0.2C;
(5) taking out the battery, standing for 1h at room temperature, and then performing first air extraction; continuing to form after air exhaust is completed;
(6) performing constant current discharge on the battery for 5h at the current of 0.2C;
(7) charging the battery for 5 hours at a constant current of 0.02C;
(8) charging the battery for 6h at a constant current of 0.05C;
(9) charging the battery for 5 hours at a constant current of 0.1C;
(10) taking out the battery, standing for 1h at room temperature, and then performing secondary air extraction; continuing to form after air exhaust is completed;
(11) performing constant current discharge on the battery for 5h at the current of 0.2C;
(12) charging the battery for 7h at a constant current of 0.05C;
(13) charging the battery for 6h at a constant current of 0.1C;
(14) the cell was discharged for 5h at a constant current of 0.2C.
Wherein the final cut-off voltage at the end of the formation is 1.5-2.0V. And after the formation is finished, the battery continues to be aged on the formation cabinet.
Example 3
A method for manufacturing a long-cycle-life lithium ion battery comprises the following steps:
s1: a. manufacturing a positive plate: firstly, preparing polyvinylidene fluoride (PVDF) and N-methyl pyrrolidone (NMP) into a solution with the mass fraction of 6.7%, then adding a conductive agent SP, stirring at a low speed for 45min, adding a conductive agent KS-6, stirring at a low speed for 45min, then stirring at a high speed for 60min, and then adding half of LiNi-Co lithium manganate LiNi0.5Co0.2Mn0.3O2Stirring at low speed for 60min, and adding the other half amount of LiNi0.5Co0.2Mn0.3O2Stirring at low speed for 60min, stirring at high speed for 120min, adding NMP solvent to adjust solid content to 68%, and stirring at high speed for 120 min. Testing the viscosity within the range of 4000-3(ii) a The positive dressing comprises the following components in percentage by mass: 92% of positive electrode active material and 4% of positive electrode conductive agent, wherein the carbon black conductive agent SP and graphiteThe mass ratio of the conductive agent KS-6 is 1.5: 2.5 and 4 percent of positive electrode binder.
b. Manufacturing a negative plate: preparing polyvinylidene fluoride (PVDF) and N-methyl pyrrolidone (NMP) into a solution with the mass fraction of 6.7%, then adding a conductive agent SP, stirring at a low speed for 45min, adding a conductive agent Carbon Nano Tube (CNT), stirring at a low speed for 45min, then stirring at a high speed for 60min, and then adding half of lithium titanate Li4Ti5O12Stirring at low speed for 60min, and adding the other half amount of lithium titanate Li4Ti5O12Stirring at low speed for 60min, stirring at high speed for 180min, adding NMP solvent to adjust solid content to 55%, and stirring at high speed for 120 min. Testing the viscosity within the range of 3000-plus 6000mPa.s, sieving by a 150-mesh double-layer metal net, preparing a negative dressing after sieving, uniformly coating the negative dressing on a carbon-coated aluminum foil with the thickness of 17 mu m, drying at 120 ℃, rolling the dried negative pole piece, wherein the rolled thickness of the negative pole piece is 107 mu m, and the compaction density is 1.8g/cm3(ii) a The negative dressing comprises the following components in percentage by mass: 92.5% of negative electrode active material and 3% of negative electrode conductive agent, wherein the mass ratio of the carbon black conductive agent SP to the carbon nano tube is 1: 2, 3.5 percent of negative pole binder.
S2: baking the pole piece: and (3) putting the pole piece into a vacuum oven to bake for 40h at 120 ℃, continuously vacuumizing, changing gas every 2h, and controlling the moisture content of the positive and negative pole pieces to be less than or equal to 200 pm.
S3: manufacturing an electric core: and (4) cutting the positive and negative plates obtained in the step (S2), and preparing the battery cell by adopting a laminated structure according to the sequence of the diaphragm-the negative plate-the diaphragm-the positive plate-the diaphragm-the negative plate-the diaphragm, wherein the diaphragm is a wet-process PE diaphragm, the thickness of the diaphragm is 12 microns, the porosity of the diaphragm is 50%, and the air permeability of the diaphragm is 150S/100 mL.
S4: and (3) welding and packaging: welding positive and negative plates in the battery core with aluminum tabs respectively to form positive and negative lead-out ends, putting the battery core into an aluminum-plastic packaging film, leading out the positive and negative tabs respectively, heating the tab glue position to fuse the PP glue of the aluminum-plastic film with the tab glue, and leaving the right side of the battery in an open state for electrolyte injection.
S5: packaging and injecting liquid: after the electrolyte is injected into the battery core, the electrolyte injection port is sealed; wherein the electrolyte solventIs a mixture of methyl ethyl carbonate, diethyl carbonate and ethylene carbonate (the mixture ratio is 1:1: 4); the electrolyte contains LiPF6；LiPF6The concentration is 1.6mol/L, the mass fraction of the electrolyte in the electrolyte is 17%, the additive is a mixture of VC and D2 with the mass fraction of 5.5%, and the mass ratio of the components is 10: 1.
s6: formation and aging: the temperature of the hot-pressing formation cabinet is set to 90 ℃, and the pressure of the clamp is set to 0.5 Mpa.
(1) Charging the battery for 5 hours at a constant current of 0.02C;
(2) charging the battery for 5 hours at a constant current of 0.05C;
(3) charging the battery for 2h at a constant current of 0.1C;
(4) charging the battery for 2h at a constant current of 0.2C;
(5) taking out the battery, standing for 1h at room temperature, and then performing first air extraction; continuing to form after air exhaust is completed;
(6) performing constant current discharge on the battery for 5h at the current of 0.2C;
(7) charging the battery for 5 hours at a constant current of 0.02C;
(8) charging the battery for 6h at a constant current of 0.05C;
(9) charging the battery for 5 hours at a constant current of 0.1C;
(10) taking out the battery, standing for 1h at room temperature, and then performing secondary air extraction; continuing to form after air exhaust is completed;
(11) performing constant current discharge on the battery for 5h at the current of 0.2C;
(12) charging the battery for 7h at a constant current of 0.05C;
(13) charging the battery for 6h at a constant current of 0.1C;
(14) the cell was discharged for 5h at a constant current of 0.2C.
Wherein the final cut-off voltage at the end of the formation is 1.5-2.0V. And after the formation is finished, the battery continues to be aged on the formation cabinet.
Example 4
A method for manufacturing a long-cycle-life lithium ion battery comprises the following steps:
s1: a. manufacturing a positive plate: firstly, the methodPreparing polyvinylidene fluoride (PVDF) and N-methylpyrrolidone (NMP) into a solution with the mass fraction of 6.7%, adding a conductive agent SP, stirring at a low speed for 45min, adding a conductive agent KS-6, stirring at a low speed for 45min, then stirring at a high speed for 60min, and then adding half of LiNi0.6Co0.2Mn0.2O and LiFemNPO4The mixture is stirred at low speed for 60min, and the other half amount of LiNi is added0.6Co0.2Mn0.2O and LiFemNPO4Stirring the mixture at low speed for 60min, then stirring at high speed for 120min, adding NMP solvent to adjust the solid content to 68%, and stirring at high speed for 120 min. After the viscosity is tested to be within the range of 4000-; the positive dressing comprises the following components in percentage by mass: 94% of positive electrode active material and 3% of positive electrode conductive agent, wherein LiNi0.6Co0.2Mn0.2O and LiFemNPO4The mass ratio of the carbon black conductive agent SP to the graphite conductive agent KS-6 is (2): 1 and 3 percent of positive electrode binder.
b. Manufacturing a negative plate: preparing polyvinylidene fluoride (PVDF) and N-methylpyrrolidone (NMP) into a solution with the mass fraction of 6.7%, then adding a conductive agent SP, stirring at a low speed for 45min, adding a conductive agent carbon nano tube, stirring at a low speed for 45min, then stirring at a high speed for 60min, and then adding half of lithium titanate Li4Ti5O12Stirring at low speed for 60min, and adding the other half amount of lithium titanate Li4Ti5O12Stirring at low speed for 60min, stirring at high speed for 180min, adding NMP solvent to adjust solid content to 55%, and stirring at high speed for 120 min. After the viscosity is tested to be within the range of 3000-6000mPa.s, sieving the mixture by using a 150-mesh double-layer metal net to prepare a negative dressing, uniformly coating the negative dressing on a 17-mu m-thick carbon-coated aluminum foil, drying the negative dressing at 120 ℃, rolling the dried negative pole piece, wherein the rolled thickness of the negative pole piece is 107 mu m, and the compaction density is 1.8g/cm 3; the negative dressing comprises the following components in percentage by mass: 92% of negative electrode active material, 5% of negative electrode conductive agent, wherein the carbon black conductive agent SP and carbonThe mass ratio of the nanotubes is 2: 3, 3% of negative electrode binder.
S2: baking the pole piece: and (3) putting the pole piece into a vacuum oven to bake for 48h at 120 ℃, continuously vacuumizing, changing gas every 2h, and controlling the moisture content of the positive pole piece and the negative pole piece to be less than or equal to 200 pm.
S3: manufacturing an electric core: and (4) cutting the positive and negative plates obtained in the step (S2), and preparing the battery cell by adopting a laminated structure according to the sequence of the diaphragm-the negative plate-the diaphragm-the positive plate-the diaphragm-the negative plate-the diaphragm, wherein the diaphragm is a wet-process PE diaphragm, the thickness of the diaphragm is 12 microns, the porosity of the diaphragm is 50%, and the air permeability of the diaphragm is 150S/100 mL.
S4: and (3) welding and packaging: welding positive and negative plates in the battery core with aluminum tabs respectively to form positive and negative lead-out ends, putting the battery core into an aluminum-plastic packaging film, leading out the positive and negative tabs respectively, heating the tab glue position to fuse the PP glue of the aluminum-plastic film with the tab glue, and leaving the right side of the battery in an open state for electrolyte injection.
S5: packaging and injecting liquid: after the electrolyte is injected into the battery core, the electrolyte injection port is sealed; wherein the electrolyte solvent is a mixture of ethyl methyl carbonate, diethyl carbonate and ethylene carbonate (the ratio is 1:1: 4); the electrolyte contains LiPF6 and LiClO4、LiBF4Mixtures of LiAsF 6; the concentration of the electrolyte is 1.6mol/L, the mass fraction of the electrolyte in the electrolyte is 14%, the additive is a mixture of VC and D2 with the mass fraction of 4.0%, and the mass ratio of the components is 11: 1.
s6: formation and aging: the temperature of the hot-pressing formation cabinet is set to 80 ℃, and the pressure of the clamp is set to 0.5 Mpa.
(1) Charging the battery for 5 hours at a constant current of 0.02C;
(2) charging the battery for 5 hours at a constant current of 0.05C;
(3) charging the battery for 2h at a constant current of 0.1C;
(4) charging the battery for 2h at a constant current of 0.2C;
(5) taking out the battery, standing for 1h at room temperature, and then performing first air extraction; continuing to form after air exhaust is completed;
(6) performing constant current discharge on the battery for 5h at the current of 0.2C;
(7) charging the battery for 5 hours at a constant current of 0.02C;
(8) charging the battery for 6h at a constant current of 0.05C;
(9) charging the battery for 5 hours at a constant current of 0.1C;
(10) taking out the battery, standing for 1h at room temperature, and then performing secondary air extraction; continuing to form after air exhaust is completed;
(11) performing constant current discharge on the battery for 5h at the current of 0.2C;
(12) charging the battery for 7h at a constant current of 0.05C;
(13) charging the battery for 6h at a constant current of 0.1C;
(14) the cell was discharged for 5h at a constant current of 0.2C.
Wherein the final cut-off voltage at the end of the formation is 1.5-2.0V. And after the formation is finished, the battery continues to be aged on the formation cabinet.
Comparative example
The prior art is as follows: aluminum-can batteries of type 2.9Ah and 20Ah from Toshiba, Japan are purchased.
Detection method
The batteries obtained in the respective examples and comparative examples were subjected to performance tests according to the following test methods, and the results obtained in the respective examples and comparative examples were plotted and compared.
The cycle life of the battery was measured with reference to the following requirements.
(1) And (3) testing temperature: 25 deg.C
(2) Temperature rise monitoring: if no special requirement exists, the temperature rise of the cell at the central point of the large surface of the 200cycle cell is tested in a natural convection environment.
(3) The testing steps are as follows:
(a) standing for 10min
(b) Constant current discharging to 1.5V at 1C
(c) Standing for 10mins
(d) Charging to 2.8V at constant current and 0.05C at constant voltage
(e) Standing for 10mins
(f) Constant current discharging to 1.5V at 1C
(g) Repeating the steps c to f until the residual capacity of the battery cell is less than 80 percent
Results of the experiment
The lithium ion batteries obtained in examples 1 to 4 of the present invention and the toshiba japonica 20Ah aluminum-shell battery were subjected to a normal temperature 6C cycle test, and the test results are shown in table 1:
TABLE 1 sample Room temperature 6C cycle Properties
Figure BDA0002129334340000111
Figure BDA0002129334340000121
As shown in table 1 and the data in fig. 1, in examples 1 to 4, the cycle numbers of examples 1 and 2 are low, example 3 is the best mode, and compared with the comparative example, the cycle numbers of examples 1 to 4 are improved by at least 168%, the battery capacity percentage of example 4 is 85.01%, the battery capacity percentage is obviously better than the battery capacity percentage of comparative example 79.88%, and the cycle performance of the battery is greatly improved.

Claims (8)

1. The long-cycle-life battery is characterized by comprising a positive plate, a negative plate, a diaphragm, electrolyte and a packaging film, wherein the electrolyte comprises a solvent, an electrolyte and an additive, the solvent is a mixture of ethyl methyl carbonate, diethyl carbonate and ethylene carbonate, the additive is a composition of vinylene carbonate, succinonitrile and fluorine-containing ether 1, 1, 2, 2-tetrafluoroethyl-2, 2, 3, 3-tetrafluoropropyl ether, and the method for preparing the long-cycle-life lithium ion battery comprises the following steps: s1: manufacturing a positive plate and a negative plate: dissolving a positive electrode material in an organic solvent, uniformly stirring to prepare a positive electrode dressing, coating the positive electrode dressing on a carbon-coated aluminum foil, drying in an oven at 100-120 ℃, and rolling to obtain a positive electrode plate; dissolving a negative electrode material in an organic solvent, uniformly stirring to prepare a negative electrode dressing, coating the negative electrode dressing on the carbon-coated aluminum foil, drying in an oven at 100-120 ℃, and rolling to obtain a negative electrode sheet;
s2: baking the pole piece: placing the positive and negative pole pieces into a vacuum oven for baking at the temperature of 120-140 ℃ for 40-50h, continuously vacuumizing, changing air every 2h, and controlling the moisture content of the positive and negative pole pieces to be less than or equal to 200 ppm;
s3: manufacturing an electric core: die-cutting the positive and negative plates obtained in the step S2, and then manufacturing the battery cell by adopting a laminated structure or a winding structure according to the sequence of the diaphragm, the negative plate, the diaphragm, the positive plate and the diaphragm;
s4: and (3) welding and packaging: welding a positive plate and a negative plate in a battery cell with an aluminum tab to form a positive lead-out end and a negative lead-out end, putting the battery cell into an aluminum-plastic packaging film, leading out the positive tab and the negative tab respectively, heating the tab glue to fuse the plastic of an aluminum-plastic bag with the tab glue to obtain a soft package battery, wherein one side of the soft package battery is in an open state, and after an electrolyte is injected;
s5: packaging and injecting liquid: after the electrolyte is injected into the battery core, the electrolyte injection port is sealed;
s6: formation and aging: the packaged battery is subjected to formation, aging and secondary sealing, and then the capacity is divided to obtain the lithium ion battery with long cycle life; the formation process in step S6 includes the steps of:
(1) charging the battery for 5 hours at a constant current of 0.02-0.03C;
(2) charging the battery for 5 hours at a constant current of 0.05-0.06C;
(3) charging the battery for 2h at a constant current of 0.1C;
(4) charging the battery for 2h at a constant current of 0.2C;
(5) taking out the battery, standing for 1h at room temperature, and then performing first air extraction; continuing to form after air exhaust is completed;
(6) performing constant current discharge on the battery for 5h at the current of 0.2C;
(7) charging the battery for 5 hours at a constant current of 0.02-0.03C;
(8) charging the battery for 6 hours at a constant current of 0.05-0.06C;
(9) charging the battery for 5 hours at a constant current of 0.1C;
(10) taking out the battery, standing for 1h at room temperature, and then performing secondary air extraction; continuing to form after air exhaust is completed;
(11) performing constant current discharge on the battery for 5h at the current of 0.2C;
(12) charging the battery for 7 hours at a constant current of 0.05-0.06C;
(13) charging the battery for 6h at a constant current of 0.1C;
(14) the cell was discharged for 5h at a constant current of 0.2C.
2. The battery of claim 1, wherein the mass ratio of vinylene carbonate, succinonitrile and fluoroether 1, 1, 2, 2-tetrafluoroethyl-2, 2, 3, 3-tetrafluoropropyl ether in the additive is 9-12: 1:1, the mass fraction of the additive in the electrolyte is 3.5-7.0%.
3. The long cycle life battery of claim 1, wherein said electrolyte is LiPF6、LiClO4、LiBF4、LiAsF6、LiB(C6F5)3(CF3)、LiCF3SO3The mass fraction of the electrolyte in the electrolyte is 13-26%.
4. The battery of claim 1, wherein the positive plate comprises a positive carbon-coated aluminum foil current collector and a positive dressing, the negative plate comprises a negative carbon-coated aluminum foil current collector and a negative dressing, and the positive dressing comprises the following components in percentage by mass: 90-96% of positive active substance, 2-5% of positive conductive agent and 2-5% of positive binder.
5. The long-cycle-life battery of claim 1, wherein the negative dressing comprises the following components in percentage by mass: 89-96% of negative electrode active material, 2-6% of negative electrode conductive agent and 2-5% of negative electrode binder; the negative active material is lithium titanate Li4Ti5O12。
6. The battery as claimed in claim 5, wherein the negative electrode binder is one or a mixture of polyvinylidene fluoride and polytetrafluoroethylene and styrene butadiene rubber, and the negative electrode conductive agent is one or a mixture of conductive carbon black SP, conductive graphite KS-6 and carbon nanotubes.
7. The long cycle life battery of claim 4, wherein the positive electrode active material is LiNi0.5Co0.3Mn0.2O2、LiNi0.6Co0.2Mn0.2O2And LiFemNPO4One or more mixtures thereof.
8. The long-cycle-life battery according to claim 1, wherein the temperature of the battery formation process in step S6 is 60 to 80 ℃, the formation pressure is 0.3 to 0.6MPa, and the final cut-off voltage at the end of the battery formation is 1.5 to 2.0V; the aging temperature is 60-80 ℃, the aging pressure is 0.3-0.6MPa, and the aging time is 48-60 h.
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