CN106450336A - Lithium ion battery negative electrode slurry and preparation method thereof - Google Patents

Lithium ion battery negative electrode slurry and preparation method thereof Download PDF

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Publication number
CN106450336A
CN106450336A CN201611110223.9A CN201611110223A CN106450336A CN 106450336 A CN106450336 A CN 106450336A CN 201611110223 A CN201611110223 A CN 201611110223A CN 106450336 A CN106450336 A CN 106450336A
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lithium ion
ion battery
solvent
additive
active substance
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CN106450336B (en
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钟发平
伍文
彭争
朱祥
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NATIONAL ENGINEERING RESEARCH CENTER OF ADVANCE ENERGY STORAGE MATERIALS
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NATIONAL ENGINEERING RESEARCH CENTER OF ADVANCE ENERGY STORAGE MATERIALS
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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
    • 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
    • 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
    • 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 invention provides lithium ion battery negative electrode slurry. The lithium ion battery negative electrode slurry comprises an active substance, a binding agent, a thickening agent and an additive, wherein the mass ratio of the active substance to the binding agent to the thickening agent to the additive is (80-98):(1.0-5.0):(0.5-5.0):(0.5-10.0); the additive is a mixture of graphene, conductive zinc oxide and MoS2; the active substance is one or more of artificial graphite, natural graphite, mesocarbon microbeads, hard carbon and soft carbon; the binding agent is butadiene styrene rubber; and the thickening agent is sodium carboxymethylcellulose. The invention also provides a preparation method of the lithium ion battery negative electrode slurry. The method is simple, and a lithium ion battery prepared by the lithium ion battery negative electrode slurry has high safety and long cycle life.

Description

A kind of lithium ion battery cathode slurry and preparation method thereof
Technical field
The present invention relates to a kind of cathode size and preparation method thereof, particularly to a kind of lithium ion battery cathode slurry and its Preparation method.
Background technology
Since the nineties in 20th century, lithium rechargeable battery has obtained extensively should in various portable type electronic products With.With developing rapidly of modern society's electronic product and going deep into further of the research and development of electric powered motor power supply, People are increasingly strong to the demand of high performance lithium ion battery, in the urgent need to the lithium-ion electric of exploitation long-life, high safety performance Pond product.To the significance level of lithium ion battery without superfluous words, for macroscopic view, longer cycle life means cycle performance Less resource consumption.And, own of common occurrence, the lithium of the fire even report of blast causing with regard to lithium ion battery in recent years The safety problem of ion battery also causes the universal concern of people.
Content of the invention
The present invention is intended to provide a kind of improve lithium ion battery safety performance and extend cycle life of lithium ion battery Lithium ion battery cathode slurry, provides its preparation method simultaneously.
The present invention is realized by below scheme：
A kind of lithium ion battery cathode slurry it is characterised in that：Including negative electrode active material, binding agent, thickening agent with add Plus agent, the mass ratio of described active substance, binding agent, thickening agent and additive is (80～98)：(1.0～5.0)：(0.5～ 5.0)：(0.5～10.0)；Described additive is Graphene, conductive zinc oxide and MoS2Mixture；Described active substance is behaved Make one or more of graphite, native graphite, MCMB, hard carbon, soft carbon；Described binding agent is styrene butadiene rubber sbr； Described thickening agent is sodium carboxymethyl cellulose CMC.
Further, Graphene, conductive zinc oxide and MoS in described additive2Mass ratio be (20～45)：(20～ 45)：(10～40).
Operability in view of painting process and quality level, the solid content general control of cathode size is 35～ 60%, viscosity general control is 1000～5000mPa s.
A kind of method preparing lithium ion battery cathode slurry as above, is carried out according to the following steps：
(1) active substance, binding agent, thickening agent, additive and solvent have been weighed in proportion, by active substance, thickening agent All add low speed premixing in agitating device with additive, mixing time is controlled to 10～60min；General active substance can be first Sieve, screen cloth selects 150 eye mesh screens；
(2) open the circulation of agitating device, first toward agitating device in addition account for needed for solvent total amount 50%～ 70% solvent stirs scraper through multiple, and each mixing time controls in 10～60min, periphery scraper of stopping afterwards；Stir The revolution rotating speed mixing device is 20～50rpm, and the rotation rotating speed of agitating device is 400～1500rpm；It is typically repeated stirring Scraper number of times is 2～4 times, and the revolution rotating speed of agitating device and rotation rotating speed all increase with number of times and be stepped up；
(3) add, toward in agitating device, the agitated scraper of solvent accounting for total amount 20%～40% needed for solvent again, stir Mix time control in 10～60min, periphery scraper of stopping；The revolution rotating speed of agitating device be 20～50rpm, agitating device from Speed of walking around is 1500～1800rpm；
(4) finally add binding agent and remaining stirring solvent toward in agitating device, until the solid content of cathode size and Viscosity reaches standard；The revolution rotating speed of agitating device is 20～50rpm, and the rotation rotating speed of agitating device is 800～1300rpm； The solid content general control of cathode size is 35～60%, and viscosity general control is 1000～5000mPa s, works as cathode size Solid content and viscosity all reach can stop during standard stir, during actual fabrication mixing time be generally 10～30min. During actual fabrication, remaining solvent can be gradually added, preferably to control the solid content of cathode size and viscosity to meet Require, when solid content and the viscosity superelevation of cathode size, can be adjusted by increasing appropriate solvent.
A kind of lithium ion battery cathode slurry of the present invention, its additive is Graphene, conductive zinc oxide and MoS2Mixed Compound.Graphene is by the planar material of the hexagonal honeycomb lattice of monolayer carbon atomic building, and theoretic throat is only 0.34 Nanometer, has higher electron mobility, adds the conduction that Graphene can be effectively improved negative electrode active material in cathode size Performance, improves the diffusion transport ability of lithium ion；Conductive zinc oxide is a kind of polyfunctional semi-conducting material, its importance One of energy is exactly its electric conductivity, and its crystal structure is wurtzite-type, in its structure, is not strict around each ion Symmetrical, the key before zinc ion and oxonium ion be substantially polarity that is to say, that conductive zinc oxide is polar structure body, be One of advantage of its high conductivity, under room temperature, the resistivity of conductive zinc oxide can reach 0.068 Ω cm, even lower. Using conductive zinc oxide as conductive agent, between active substance, play between active substance and collector and collect micro-current Effect, it is possible to reduce the contact resistance of electrode, accelerates the rate travel of electronics, also can effectively improve lithium ion in electrode simultaneously Migration rate in material, thus improving the high rate during charging-discharging of battery, extend that battery 1C charge and discharge and 1C fill that 10C puts follows The ring life-span；MoS2It is a kind of transient metal sulfide, there is very typical S-Mo-S sandwich structure, i.e. two sulfur layer folders one Individual Mo metal level, links together by strong covalent bond between atom in layer, and then leans on relatively weak model moral between layers Hua Li is connected with each other, and this structure allows lithium ion quickly to embed and deviate from.The lithium ion battery of the preparation present invention is born The method of pole slurry, process is simple, directly use existing apparatus.Lithium-ion electric using the cathode size preparation of the present invention Pond, has longer cycle life and preferable security performance.
Brief description
The 1C charge and discharge cycle life of the lithium ion battery of the cathode size preparation that Fig. 1 prepares for embodiment 1 method is bent Line chart；
The 1C of the lithium ion battery of the cathode size preparation that Fig. 2 prepares for embodiment 1 method fills 10C puts cycle life Curve chart.
Specific embodiment
The invention will be further described with reference to embodiments, but the invention is not limited in the statement of embodiment.
Embodiment 1
A kind of preparation method of lithium ion battery cathode slurry, is carried out according to the following steps：
(1) 45kg Delanium through sieving, 2kg styrene butadiene rubber sbr, 1kg sodium carboxymethyl cellulose CMC, 0.6kg are weighed Graphene, 0.7kg conductive zinc oxide, 0.7kg MoS2With 61kg deionized water, by Delanium, sodium carboxymethyl cellulose CMC, Graphene, conductive zinc oxide and MoS2All add low speed premixing in agitator, stir 30min；
(2) open the circulation of agitator, first the addition total amount needed for ionized water 66% that accounts for is toward agitator in The deionized water of 40.26kg through stirring scraper twice, 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 rotating speed of blender is 700rpm；Stop after second stirring 30min periphery scraper, blender Revolution rotating speed is 40rpm, and the rotation rotating speed of blender is 1000rpm；
(3) add the deionized water that the total amount needed for ionized water 30% that accounts for is 18.3kg toward in agitator again, stir 60min After stop periphery scraper, the revolution rotating speed of blender is 50rpm, and the rotation rotating speed of blender is 1600rpm；
(4) toward in agitator, finally add styrene butadiene rubber sbr and remaining deionized water stirring 20min, the public affairs of blender Speed of walking around is 30rpm, and the rotation rotating speed of blender is 800rpm.
Take the lithium ion battery cathode slurry preparing through above-mentioned steps on a small quantity to survey its solid content and viscosity, record it Solid content is 45%, and viscosity is 2300mPa s.
The lithium ion battery cathode slurry that embodiment 1 is prepared is by the work of column lithium ion battery 18650-2300 Skill makes negative plate, 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 with 1C constant-current constant-voltage charging to blanking voltage, cut-off current is 20mA, using 1C constant-current discharge to 2.75V, its circulation Life curve figure is as shown in figure 1, it will be seen from figure 1 that circulating battery to 2000 times, battery capacity conservation rate is still on 90% left side Right；The 1C discharge and recharge of existing heavy-current discharge battery 500 times, battery capacity just can only be maintained at 80% about substantially.Take The battery made is 4.2V using 1C constant-current constant-voltage charging to blanking voltage, and cut-off current is 20mA, using 10C constant-current discharge To 2.75V, its cycle life curve chart is as shown in Fig. 2 figure it is seen that circulating battery to 500 times, battery capacity keeps Rate is still 91% about；And existing its 10C of heavy-current discharge battery electric discharge is in circulation 300 times, battery capacity just exists substantially Less than 80%.It can be seen that column lithium ion battery prepared by the lithium ion battery cathode slurry that use the present embodiment prepares, Either 1C charge and discharge or 1C fill 10C and put, and its cycle life is all very good.
Embodiment 2
A kind of preparation method of lithium ion battery cathode slurry, is carried out according to the following steps：
(1) weigh 34kg native graphite through sieving, 2kg styrene butadiene rubber sbr, 1.6kg sodium carboxymethyl cellulose CMC, 0.7kg Graphene, 0.8kg conductive zinc oxide, 0.5kg MoS2With 62.4kg deionized water, by native graphite, carboxymethyl cellulose Plain sodium CMC, Graphene, conductive zinc oxide and MoS2All add low speed premixing in agitator, stir 40min；
(2) open the circulation of agitator, first the addition total amount needed for ionized water 70% that accounts for is toward agitator in The deionized water of 43.68kg 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 rotating speed of blender is 600rpm；Stop after second stirring 30min periphery scraper, blender Revolution rotating speed is 30rpm, and the rotation rotating speed of blender is 800rpm；Stop periphery scraper after third time stirring 25min, blender Revolution rotating speed be 40rpm, the rotation rotating speed of blender is 1000rpm；
(3) deionized water that the total amount needed for ionized water 20% that accounts for is 12.48kg, stirring are added again toward in agitator Stop after 40min periphery scraper, the revolution rotating speed of blender is 40rpm, the rotation rotating speed of blender is 1700rpm；
(4) toward in agitator, finally add styrene butadiene rubber sbr and remaining deionized water stirring 30min, the public affairs of blender Speed of walking around is 40rpm, and the rotation rotating speed of blender is 1000rpm.
Take the lithium ion battery cathode slurry preparing through above-mentioned steps on a small quantity to survey its solid content and viscosity, record it Solid content is 39%, and viscosity is 1800mPa s.
Embodiment 3
A kind of preparation method of lithium ion battery cathode slurry, is carried out according to the following steps：
(1) 33.2kg native graphite through sieving, 1.6kg styrene butadiene rubber sbr, 1.2kg sodium carboxymethyl cellulose are weighed CMC, 1.6kg Graphene, 0.8kg conductive zinc oxide, 1.6kg MoS2With 40kg deionized water, will be fine to native graphite, carboxymethyl The plain sodium CMC of dimension, Graphene, conductive zinc oxide and MoS2All add low speed premixing in agitator, stir 60min；
(2) open the circulation of agitator, first the addition total amount needed for ionized water 55% that accounts for is toward agitator in Through four stirring scrapers, periphery scraper of stopping after stirring 30min for the first time, the revolution of blender turns the deionized water of 22kg Speed is 25rpm, and the rotation rotating speed of blender is 700rpm；Stop after second stirring 30min periphery scraper, the revolution of blender Rotating speed is 35rpm, and the rotation rotating speed of blender is 900rpm；Stop periphery scraper after third time stirring 15min, the public affairs of blender Speed of walking around is 40rpm, and the rotation rotating speed of blender is 1100rpm；Stop periphery scraper after 4th stirring 10min, blender Revolution rotating speed be 45rpm, the rotation rotating speed of blender is 1300rpm；
(3) add the deionized water that the total amount needed for ionized water 40% that accounts for is 16kg again toward in agitator, after stirring 60min Stop periphery scraper, the revolution rotating speed of blender is 50rpm, the rotation rotating speed of blender is 1800rpm；
(4) toward in agitator, finally add styrene butadiene rubber sbr and remaining deionized water stirring 15min, the public affairs of blender Speed of walking around is 25rpm, and the rotation rotating speed of blender is 1300rpm.
Take the lithium ion battery cathode slurry preparing through above-mentioned steps on a small quantity to survey its solid content and viscosity, record it Solid content is 50%, and viscosity is 3000mPa s.
It is only presently preferred embodiments of the present invention above, according to the above-mentioned design of the present invention, the common skill of the art Art personnel also can make various modifications and alterations to this, under the premise without departing from the principles of the invention, also should be considered as the present invention Protection domain.

Claims (6)

1. a kind of lithium ion battery cathode slurry it is characterised in that：Including active substance, binding agent, thickening agent and additive, institute The mass ratio stating active substance, binding agent, thickening agent and additive is (80～98)：(1.0～5.0)：(0.5～5.0)：(0.5 ～10.0)；Described additive is Graphene, conductive zinc oxide and MoS2Mixture；Described active substance is Delanium, sky So one or more of graphite, MCMB, hard carbon, soft carbon；Described binding agent is butadiene-styrene rubber；Described thickening agent is Sodium carboxymethyl cellulose.
2. as claimed in claim 1 a kind of lithium ion battery cathode slurry it is characterised in that：Graphene in described additive, Conductive zinc oxide and MoS2Mass ratio be (20～45)：(20～45)：(10～40).
3. as claimed in claim 1 or 2 a kind of it is characterised in that：The solid content of cathode size is 35%～60%, and viscosity is 1000～5000mPa s.
4. a kind of method preparing described lithium ion battery cathode slurry as arbitrary in claims 1 to 3 it is characterised in that：Press Ratio has weighed active substance, binding agent, thickening agent, additive and solvent, and active substance, thickening agent and additive are all added Enter premixing in agitating device, open the circulation of agitating device afterwards, be initially charged account for needed for solvent total amount 50%～ 70% solvent, through repeatedly repeatedly stirring scraper, adds the solvent accounting for total amount 20%～40% needed for solvent through stirring Mix scraper, be eventually adding binding agent and remaining stirring solvent, until the solid content of cathode size and viscosity reach standard.
5. as claimed in claim 4 a kind of method preparing lithium ion battery cathode slurry it is characterised in that：Described addition accounts for In the solvent step of total amount 50%～70% needed for solvent, stirring scraper number of times is 2～4 times, and the revolution of agitating device turns Speed and rotation rotating speed all increase with number of times and are stepped up.
6. a kind of method preparing lithium ion battery cathode slurry as described in claim 4 or 5 it is characterised in that：Described molten Agent is deionized water.
CN201611110223.9A 2016-12-06 2016-12-06 A kind of lithium ion battery anode slurry and preparation method thereof Active CN106450336B (en)

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Cited By (8)

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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
CN107403914A (en) * 2017-07-03 2017-11-28 江西安驰新能源科技有限公司 A kind of dry mixing process of artificial plumbago negative pole 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
CN111180659A (en) * 2019-12-30 2020-05-19 江西安驰新能源科技有限公司 Preparation method of lithium ion battery cathode slurry
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
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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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN107403914A (en) * 2017-07-03 2017-11-28 江西安驰新能源科技有限公司 A kind of dry mixing process of artificial plumbago negative pole 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
WO2020144289A1 (en) 2019-01-09 2020-07-16 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
CN111180659A (en) * 2019-12-30 2020-05-19 江西安驰新能源科技有限公司 Preparation method of lithium ion battery cathode slurry
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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