CN106450336B - A kind of lithium ion battery anode slurry and preparation method thereof - Google Patents
A kind of lithium ion battery anode slurry and preparation method thereof Download PDFInfo
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- CN106450336B CN106450336B CN201611110223.9A CN201611110223A CN106450336B CN 106450336 B CN106450336 B CN 106450336B CN 201611110223 A CN201611110223 A CN 201611110223A CN 106450336 B CN106450336 B CN 106450336B
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
-
- 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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/621—Binders
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
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- 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
Abstract
The present invention provides a kind of lithium ion battery anode slurries, including active material, binder, thickener and additive, the active material, binder, thickener and additive mass ratio be (80~98): (1.0~5.0): (0.5~5.0): (0.5~10.0)；The additive is graphene, conductive zinc oxide and MoS2Mixture；The active material is one of artificial graphite, natural graphite, mesocarbon microspheres, hard carbon, soft carbon or a variety of；The binder is butadiene-styrene rubber；The thickener is sodium carboxymethylcellulose.The present invention also provides the methods for preparing lithium ion battery anode slurry, and method is simple, and the lithium ion battery made using lithium ion battery anode slurry of the invention has preferable security performance and longer cycle life.
Description
Technical field
The present invention relates to a kind of negative electrode slurry and preparation method thereof, in particular to a kind of lithium ion battery anode slurry and its
Preparation method.
Background technique
Since the 1990s, lithium ion secondary battery has obtained answering extensively in various portable electronic products
With.With the rapid development and electric powered motor power supply of modern society's electronic product research and development further deeply,
Demand of the people to high performance lithium ion battery is increasingly strong, and there is an urgent need to develop long-lives, the lithium-ion electric of high safety performance
Pond product.Cycle performance is not necessarily to superfluous words to the significance level of lithium ion battery, and for macroscopic view, longer cycle life means
Less resource consumption.Moreover, report oneself commonplace, lithium that the fire caused in recent years about lithium ion battery even explodes
The concern that the safety problem of ion battery also causes people universal.
Summary of the invention
The present invention is intended to provide a kind of can be improved lithium ion battery safety performance and extend cycle life of lithium ion battery
Lithium ion battery anode slurry, while preparation method being provided.
The present invention is realized by the following scheme:
A kind of lithium ion battery anode slurry, it is characterised in that: including negative electrode active material, binder, thickener and add
Add agent, the active material, binder, thickener and additive mass ratio be (80~98): (1.0~5.0): (0.5~
5.0): (0.5~10.0)；The additive is graphene, conductive zinc oxide and MoS2Mixture；The active material is behaved
Make one of graphite, natural graphite, mesocarbon microspheres, hard carbon, soft carbon or a variety of；The binder is styrene butadiene rubber sbr；
The thickener is sodium carboxymethylcellulose CMC.
Further, graphene, conductive zinc oxide and MoS in the additive2Mass ratio be (20~45): (20~
45): (10~40).
In view of the operability and quality level of painting process, the solid content general control of negative electrode slurry is 35~
60%, viscosity general control is 1000~5000mPas.
A method of lithium ion battery anode slurry as described above is prepared, is sequentially included the following steps:
(1) active material, binder, thickener, additive and solvent have been weighed in proportion, by active material, thickener
Low speed premixing in agitating device is all added with additive, mixing time control is 10~60min；General active material can be first
Sieving, sieve select 150 mesh screens；
(2) open agitating device circulation, first into agitating device addition account for total amount 50% needed for solvent~
70% solvent is repeatedly stirred --- and scraper, each mixing time control is in 10~60min, periphery scraper of stopping later；It stirs
The revolution revolving speed for mixing device is 20~50rpm, and the rotation revolving speed of agitating device is 400~1500rpm；It is typically repeated stirring ---
Scraper number is 2~4 times, and the revolution revolving speed and rotation revolving speed of agitating device increase with number and be stepped up；
(3) again into agitating device be added account for total amount 20%~40% needed for solvent solvent it is agitated --- scraper is stirred
Time control is mixed in 10~60min, periphery scraper of stopping；The revolution revolving speed of agitating device be 20~50rpm, agitating device from
Speed of walking around is 1500~1800rpm；
(4) last that binder and remaining stirring solvent are added into agitating device, until the solid content of negative electrode slurry with
Viscosity reaches standard；The revolution revolving speed of agitating device is 20~50rpm, and the rotation revolving speed of agitating device is 800~1300rpm；
The solid content general control of negative electrode slurry is 35~60%, and viscosity general control is 1000~5000mPas, works as negative electrode slurry
Solid content and viscosity can stop stirring when reaching standard, mixing time is generally 10~30min during actual fabrication.
During actual fabrication, remaining solvent can be gradually added, and be met preferably to control solid content and the viscosity of negative electrode slurry
It is required that can be adjusted by increasing appropriate solvent when the solid content of negative electrode slurry and viscosity superelevation.
A kind of lithium ion battery anode slurry of the invention, additive are graphene, conductive zinc oxide and MoS2It is mixed
Close object.Graphene is the planar material for the hexagonal honeycomb lattice being made of single layer of carbon atom, and theoretic throat is only 0.34
Nanometer, electron mobility with higher, adding graphene in negative electrode slurry can effectively improve the conduction of negative electrode active material
Performance improves the diffusion transport ability of lithium ion；Conductive zinc oxide is a kind of semiconductor material of multifunctionality, its importance
One of energy is exactly its electric conductivity, and it is not in its structure, around each ion stringent that crystal structure, which is wurtzite-type,
Symmetrically, zinc ion and the key before oxonium ion are substantially polar, that is to say, that conductive zinc oxide is polar structure body, is
One of advantage of its high conductivity, at room temperature, the resistivity of conductive zinc oxide can reach 0.068 Ω cm, even lower.
Using conductive zinc oxide as conductive agent, is played between active material, between active material and collector and collect micro-current
Effect, it is possible to reduce the contact resistance of electrode accelerates the rate travel of electronics, while can also effectively improve lithium ion in electrode
Migration rate in material extends battery 1C charge and discharge and what 1C filled that 10C puts follows to improve the high rate during charging-discharging of battery
The ring service life；MoS2It is a kind of transient metal sulfide, there is very typical S-Mo-S sandwich structure, i.e. two sulphur layer folders one
A Mo metal layer is linking together between atom by strong covalent bond in layer, and then leans on relatively weak model moral between layers
Magnificent power is connected with each other, and this structure allows lithium ion to be quickly embedded in and deviate from.It is negative to prepare lithium ion battery of the invention
The method of pole slurry, simple process directly use existing apparatus.The lithium-ion electric prepared using negative electrode slurry of the invention
Pond has longer cycle life and preferable security performance.
Detailed description of the invention
Fig. 1 is that the 1C charge-discharge cycle service life of the lithium ion battery for the negative electrode slurry preparation that 1 method of embodiment is prepared is bent
Line chart；
The 1C of the lithium ion battery for the negative electrode slurry preparation that Fig. 2 is prepared for 1 method of embodiment, which fills 10C, puts cycle life
Curve graph.
Specific embodiment
The invention will be further described with reference to embodiments, but the invention is not limited to the statements of embodiment.
Embodiment 1
A kind of preparation method of lithium ion battery anode slurry, sequentially includes the following steps:
(1) 45kg artificial graphite, 2kg styrene butadiene rubber sbr, 1kg sodium carboxymethylcellulose CMC, 0.6kg through being sieved are weighed
Graphene, 0.7kg conductive zinc oxide, 0.7kg MoS2With 61kg deionized water, by artificial graphite, sodium carboxymethylcellulose CMC,
Graphene, conductive zinc oxide and MoS2Low speed premixing in agitator is all added, stirs 30min；
(2) circulation for opening agitator, is first added into agitator and accounts for total amount 66% needed for ionized water i.e.
The deionized water of 40.26kg is stirred twice --- scraper, periphery scraper of stopping after stirring 40min for the first time, the public affairs of blender
Speed of walking around is 30rpm, and the rotation revolving speed of blender is 700rpm；It stops after second stirring 30min periphery scraper, blender
Revolution revolving speed is 40rpm, and the rotation revolving speed of blender is 1000rpm；
(3) it is added again into agitator and accounts for the total amount 30% i.e. deionized water of 18.3kg needed for ionized water, stir 60min
After stop periphery scraper, the revolution revolving speed of blender is 50rpm, and the rotation revolving speed of blender is 1600rpm；
(4) last that styrene butadiene rubber sbr and remaining deionized water stirring 20min, the public affairs of blender are added into agitator
Speed of walking around is 30rpm, and the rotation revolving speed of blender is 800rpm.
It takes and surveys its solid content and viscosity by the lithium ion battery anode slurry that above-mentioned steps are prepared on a small quantity, measure it
Solid content is 45%, viscosity 2300mPas.
The lithium ion battery anode slurry that embodiment 1 is prepared by column lithium ion battery 18650-2300 work
Skill makes negative electrode tab, and is fabricated to battery by the technique of column lithium ion battery 18650-2300.The battery made is taken to make
It is 4.2V, cut-off current 20mA with 1C constant-current constant-voltage charging to blanking voltage, uses 1C constant-current discharge to 2.75V, circulation
Life curve figure is as shown in Figure 1, it will be seen from figure 1 that circulating battery is to 2000 times, and battery capacity conservation rate is still on 90% left side
It is right；1C charge and discharge 500 times of existing heavy-current discharge battery, battery capacity can only just be maintained at 80% or so substantially.It takes
The battery made is 4.2V using 1C constant-current constant-voltage charging to blanking voltage, and cut-off current 20mA uses 10C constant-current discharge
To 2.75V, as shown in Fig. 2, figure it is seen that circulating battery is to 500 times, battery capacity is kept cycle life curve figure
Rate is still 91% or so；And its 10C of existing heavy-current discharge battery electric discharge is recycling 300 times, battery capacity just exists substantially
80% or less.It can be seen that the column lithium ion battery for the lithium ion battery anode slurry preparation being prepared using the present embodiment,
Either 1C charge and discharge or 1C fill 10C and put, and cycle life is all very good.
Embodiment 2
A kind of preparation method of lithium ion battery anode slurry, sequentially includes the following steps:
(1) weigh 34kg natural graphite through being sieved, 2kg styrene butadiene rubber sbr, 1.6kg sodium carboxymethylcellulose CMC,
0.7kg graphene, 0.8kg conductive zinc oxide, 0.5kg MoS2With 62.4kg deionized water, by natural graphite, carboxymethyl cellulose
Plain sodium CMC, graphene, conductive zinc oxide and MoS2Low speed premixing in agitator is all added, stirs 40min；
(2) circulation for opening agitator, is first added into agitator and accounts for total amount 70% needed for ionized water i.e.
The deionized water of 43.68kg is through triple mixing --- scraper, periphery scraper of stopping after stirring 30min for the first time, the public affairs of blender
Speed of walking around is 20rpm, and the rotation revolving speed of blender is 600rpm；It stops after second stirring 30min periphery scraper, blender
Revolution revolving speed is 30rpm, and the rotation revolving speed of blender is 800rpm；It stops periphery scraper after third time stirring 25min, blender
Revolution revolving speed be 40rpm, the rotation revolving speed of blender is 1000rpm；
(3) it is added again into agitator and accounts for the total amount 20% i.e. deionized water of 12.48kg needed for ionized water, stirred
It stops after 40min periphery scraper, the revolution revolving speed of blender is 40rpm, and the rotation revolving speed of blender is 1700rpm；
(4) last that styrene butadiene rubber sbr and remaining deionized water stirring 30min, the public affairs of blender are added into agitator
Speed of walking around is 40rpm, and the rotation revolving speed of blender is 1000rpm.
It takes and surveys its solid content and viscosity by the lithium ion battery anode slurry that above-mentioned steps are prepared on a small quantity, measure it
Solid content is 39%, viscosity 1800mPas.
Embodiment 3
A kind of preparation method of lithium ion battery anode slurry, sequentially includes the following steps:
(1) 33.2kg natural graphite, 1.6kg styrene butadiene rubber sbr, 1.2kg sodium carboxymethylcellulose through being sieved are weighed
CMC, 1.6kg graphene, 0.8kg conductive zinc oxide, 1.6kg MoS2It is with 40kg deionized water, natural graphite, carboxymethyl is fine
Tie up plain sodium CMC, graphene, conductive zinc oxide and MoS2Low speed premixing in agitator is all added, stirs 60min；
(2) circulation for opening agitator, is first added into agitator and accounts for total amount 55% needed for ionized water i.e.
The deionized water of 22kg is stirred through four times --- and scraper, periphery scraper of stopping after stirring 30min for the first time, the revolution of blender turn
Speed is 25rpm, and the rotation revolving speed of blender is 700rpm；It stops after second stirring 30min periphery scraper, the revolution of blender
Revolving speed is 35rpm, and the rotation revolving speed of blender is 900rpm；It stops periphery scraper after third time stirring 15min, the public affairs of blender
Speed of walking around is 40rpm, and the rotation revolving speed of blender is 1100rpm；It stops after 4th stirring 10min periphery scraper, blender
Revolution revolving speed be 45rpm, the rotation revolving speed of blender is 1300rpm；
(3) it is added again into agitator and accounts for the total amount 40% i.e. deionized water of 16kg needed for ionized water, after stirring 60min
It stops periphery scraper, the revolution revolving speed of blender is 50rpm, and the rotation revolving speed of blender is 1800rpm；
(4) last that styrene butadiene rubber sbr and remaining deionized water stirring 15min, the public affairs of blender are added into agitator
Speed of walking around is 25rpm, and the rotation revolving speed of blender is 1300rpm.
It takes and surveys its solid content and viscosity by the lithium ion battery anode slurry that above-mentioned steps are prepared on a small quantity, measure it
Solid content is 50%, viscosity 3000mPas.
The foregoing is merely the preferred embodiments of the present invention, according to the above-mentioned design, the common skill of the art
Art personnel can also make various modifications and alterations to this, without departing from the principle of the present invention, also should be considered as the present invention
Protection scope.
Claims (5)
1. a kind of lithium ion battery anode slurry, it is characterised in that: including active material, binder, thickener and additive, institute
The mass ratio for stating active material, binder, thickener and additive is (80~98): (1.0~5.0): (0.5~5.0): (0.5
~10.0)；The additive is graphene, conductive zinc oxide and MoS2Mixture, graphene, conductive zinc oxide in additive
And MoS2Mass ratio be (20~45): (20~45): (10~40)；The active material be artificial graphite, natural graphite, in
Between one of phase carbon microspheres, hard carbon, soft carbon or a variety of；The binder is butadiene-styrene rubber；The thickener is that carboxymethyl is fine
Tie up plain sodium.
2. a kind of lithium ion battery anode slurry as described in claim 1, it is characterised in that: the solid content of negative electrode slurry is
35%~60%, viscosity is 1000~5000mPas.
3. a kind of method for preparing lithium ion battery anode slurry as claimed in claim 1 or 2, it is characterised in that: in proportion
Active material, binder, thickener, additive and solvent have been weighed, active material, thickener and additive are all added and stirred
It mixes in device and is pre-mixed, open the circulation of agitating device later, be first added and account for gross mass 50%~70% needed for solvent
Solvent through repeatedly repeatedly stir --- scraper, the solvent for adding gross mass 20%~40% needed for accounting for solvent are agitated ---
Scraper is eventually adding binder and remaining stirring solvent, until the solid content of negative electrode slurry and viscosity reach standard.
4. a kind of method for preparing lithium ion battery anode slurry as claimed in claim 3, it is characterised in that: the addition accounts for
In the solvent step of gross mass 50%~70% needed for solvent, stirring --- scraper number is 2~4 times, the revolution of agitating device
Revolving speed and rotation revolving speed increase with number and are stepped up.
5. a kind of method for preparing lithium ion battery anode slurry as described in claim 3 or 4, it is characterised in that: described molten
Agent is deionized water.
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| CN107086292A (en) * | 2017-03-27 | 2017-08-22 | 湖北猛狮新能源科技有限公司 | A kind of high viscosity lithium ion battery slurry-stirring process |
| CN107403914B (en) * | 2017-07-03 | 2020-08-18 | 江西安驰新能源科技有限公司 | Dry mixing process of artificial graphite cathode slurry |
| CN107819118A (en) * | 2017-10-26 | 2018-03-20 | 深圳市斯诺实业发展股份有限公司 | A kind of shunting cathode of lithium battery blank preparation technicses |
| CN108172750A (en) * | 2017-12-07 | 2018-06-15 | 银隆新能源股份有限公司 | The preparation method of graphite negative electrode of lithium ion battery highly viscous slurry |
| CN108630884A (en) * | 2018-05-21 | 2018-10-09 | 重庆市紫建电子有限公司 | A kind of lithium ion battery anode slurry preparation method |
| EP3680962A1 (en) | 2019-01-09 | 2020-07-15 | The Provost, Fellows, Scholars and other Members of Board of Trinity College Dublin | High capacity electrodes enabled by 2d materials in a viscous aqueous ink |
| CN111180659B (en) * | 2019-12-30 | 2021-03-12 | 江西安驰新能源科技有限公司 | Preparation method of lithium ion battery cathode slurry |
| CN113178620A (en) * | 2021-04-30 | 2021-07-27 | 天能帅福得能源股份有限公司 | Preparation method of lithium ion battery with high-power charging performance |
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| US20110104551A1 (en) * | 2009-11-05 | 2011-05-05 | Uchicago Argonne, Llc | Nanotube composite anode materials suitable for lithium ion battery applications |
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| CN105470506A (en) * | 2015-11-20 | 2016-04-06 | 陕西科技大学 | Preparation method of MoS<2>/C anode material for lithium-ion battery |
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