CN109360976A - A kind of negative electrode material of lithium battery and its preparation method and application - Google Patents
A kind of negative electrode material of lithium battery and its preparation method and application Download PDFInfo
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- CN109360976A CN109360976A CN201811465684.7A CN201811465684A CN109360976A CN 109360976 A CN109360976 A CN 109360976A CN 201811465684 A CN201811465684 A CN 201811465684A CN 109360976 A CN109360976 A CN 109360976A
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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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
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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
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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
- H01M4/621—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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The present invention provides a kind of negative electrode material of lithium battery, the graphite including 80-98wt%, the conductive agent of 0.5-6wt%, the carboxymethyl cellulose lithium of 0.5-6wt%, the butadiene-styrene latex of 1-10wt%.When cathode of this negative electrode material as lithium battery, Li ion can be additionally provided for lithium battery, increase lithium ion decentralised control efficiency, improve the quantity of lithium ion insertion and abjection between positive and negative anodes, shorten the path that lithium ion moves between positive and negative, and then conductivity and conductivity between positive and negative anodes are effectively increased, the lithium battery using this negative electrode material as cathode has higher specific capacity and cycle efficieny.
Description
Technical field
The present invention relates to field of lithium, in particular to a kind of negative electrode material of lithium battery and its preparation method and application.
Background technique
It is growing with economic fast development and people's demand, on the one hand, various electric appliances, electric product increasingly increase
More, also increasing to the demand of battery, on the other hand, China is faced with huge environmental protection pressure and energy problem, therefore,
While guaranteeing normal production with life, how to realize that environmental protection becomes research emphasis.
Lithium ion battery has the characteristics that high-energy density, long circulation life and free of contamination, thus is widely used in
In each electric appliances and electrical equipment.However the lower specific capacity of commercialized graphite cathode material has been unable to satisfy at present
The growing energy demand of people, especially in electric vehicle industry field.Therefore, novel high performance lithium-ion electric is researched and developed
Pond negative electrode material is those skilled in the art's urgent problem to be solved.
Summary of the invention
The present invention provides a kind of electrode material of lithium battery, includes carboxymethyl cellulose lithium, the carboxymethyl cellulose
Purity >=99% of lithium, 200 mesh residue of aqueous solution≤1ppm, degree of substitution 0.65-1.2,1% wet button water Brookfield viscosity
> 100cps is the high-purity, high grade of transparency, the carboxymethyl cellulose lithium for lacking fiber, few insolubles content, the carboxymethyl of this parameter
Cellulose lithium is used as dispersing agent, bonding agent in electrode material, can effectively improve the specific capacity and circulating effect of lithium battery.
The present invention also provides a kind of negative electrode material of lithium battery, the graphite including 80-98wt%, the conduction of 0.5-6wt%
Agent, the carboxymethyl cellulose lithium of 0.5-6wt%, the butadiene-styrene latex of 1-10wt%, cathode of this negative electrode material as lithium battery
When, Li ion can be additionally provided for lithium battery, increase lithium ion decentralised control efficiency, improve between positive and negative anodes lithium ion insertion and
The quantity of abjection, shortens the path of lithium ion movement between positive and negative, and then effectively increases the conductivity between positive and negative anodes and biography
Conductance.
Preferably, the negative electrode material of lithium battery includes the graphite of 90-96wt%, the conductive agent of 0.5-4wt%, 0.5-
The carboxymethyl cellulose lithium of 3wt%, the butadiene-styrene latex of 1-8wt%.
Preferably, purity >=99% of the carboxymethyl cellulose lithium, 200 mesh residue of aqueous solution≤1ppm, degree of substitution
0.65-1.2,1% wet button water Brookfield viscosity > 100cps are the high-purity, high grade of transparency, few fiber, few insolubles content
Carboxymethyl cellulose lithium.
Preferably, the conductive agent is any one of carbon black, electrically conductive graphite, conductive carbon fibre, carbon nanotube, graphene
Or several mixing.
The preparation method of the negative electrode material of above-mentioned lithium battery, has follow steps:
1) feeding in proportion；
2) carboxymethyl cellulose lithium is added to the water, dissolution is complete；
3) conductive agent is added, stirs and evenly mixs；
4) graphite is added, stirs and evenly mixs, is evacuated to bubble-free and emerges；
5) styrene-butadiene latex is added, stirs and evenly mixs, is adjusted to required viscosity according to actual demand plus water, obtains negative electrode material.
Preferably, water described in step 2) is deionized water, or to be free of or containing less solubility calcium, magnesium compound
Soft water.
Preferably, the time of the step 3) stirring is 0.5-1h；The time of the step 4) stirring is 1.5-3h；Step
4) vacuum degree vacuumized is≤- 0.01KPa.
Preferably, step 5) stirs and evenly mixs, and is separated into even suspension slurry by sieve, obtains negative electrode material.
The present invention also provides a kind of lithium batteries, comprising any above-mentioned negative electrode material as cathode.
The effect of each component is as follows in negative electrode material of the present invention:
1. graphite: as the active material in lithium cell cathode material, electronic conductivity is high, crystallization degree is high, lithium from
Sub- diffusion coefficient is big, has good layer structure, provides space, path, while its layer for insertion-deintercalation repeatedly of lithium ion
Shape structure volume change before and after embedding lithium is small, embedding lithium capacity is high, intercalation potential is low.If the content of graphite is lower than 80wt%, lithium
Lithium ion repeatedly be obstructed by space, path needed for insertion-deintercalation in battery, and battery efficiency is poor, capacity is low, cycle performance
Difference；If the content of graphite is higher than 98wt%, other auxiliary agents such as conductive agent, dispersing agent, stabilizer, binder in negative electrode material
Dosage is few, influence cell size uniformly, stability, battery material coating adhesion, and battery pole piece resistance is high, eventually leads to
Battery performance is poor.
2. conductive agent: improving electronic conductivity, promote electronics to pass rapidly through active material and reach collector, in addition, conductive
Agent can also be improved pole piece processability, promotes infiltration of the electrolyte to pole piece, resistivity is reduced, to improve the use of lithium battery
Service life.If conductive agent content is lower than 0.5wt%, the conductivity of battery is low, and resistance is high, and battery efficiency is poor, cyclicity
It can be poor；If conductive agent content is higher than 6wt%, active material, dispersing agent, stabilizer, consumption of binder are few, and lithium ion is repeatedly embedding
Enter-deintercalation needed for space, path be obstructed, while influence cell size uniformly, stability, battery material coating adhesion, most
Cause battery performance poor eventually.
3. carboxymethyl cellulose lithium (CMC-Li): dispersing agent, stabilizer, binder as lithium battery material.As point
Powder can preferably disperse electrode material, and electrode material granules is made to be evenly distributed, stablize, and avoid cell size each group
Wadding is divided to gather, layering；Meanwhile as binder, lithium ion content is improved, improves battery diffuser efficiency and specific capacity, and can will be electric
Pond material and current-collector are combined closely, and stabilization of the battery in charge and discharge process is kept；In addition, as stabilizer, can also hinder point
It dissipates uniform styrene-butadiene latex to volatilize and migrate with moisture content in battery material drying process, improves styrene-butadiene latex caking property, play
Assist cementation.If carboxymethyl cellulose lithium content is lower than 0.5wt%, the dispersion of battery material slurry, stability are poor, influence to starch
Material coating, influences electrode coating uniformity, leads to electrode electro Chemical degradation；If the content of carboxymethyl cellulose lithium is higher than
On the one hand 6wt% makes cell size viscosity excessive, mobility is deteriorated, and influences slurry coating and coating uniformity, on the other hand
Active material, conductive agent, consumption of binder are few, and lithium ion repeatedly be obstructed by space, path needed for insertion-deintercalation, ionic conductivity
Impacted, battery pole piece resistance is high, poor circulation.
4. styrene-butadiene latex (SBR): as the binder of lithium ion battery material, comprehensive performance and chemical stability compared with
It is good, play the role of binder in lithium ion battery.If the content of styrene-butadiene latex is lower than 1wt%, battery material slurry bonding
Power is inadequate, and coating adhesive strength is poor, easily loses powder, and lithium ion insertion-deintercalation process is caused to be obstructed, and battery performance is deteriorated；If
The content of styrene-butadiene latex is higher than 10wt%, on the one hand makes cell size binder excessive, and coating film forming is fine and close, and active material is empty
Between tail off, another aspect active material, conductive agent, amount of stabilizer are few, lithium ion repeatedly space needed for insertion-deintercalation,
Path is obstructed, and ionic conductivity is impacted, and battery pole piece resistance is high, poor circulation.
The invention has the following advantages:
The high-performance lithium battery electrode material of the lithium according to the present invention containing carboxymethyl cellulose is a kind of containing high-purity, high
The electrode material of lithium battery of lightness, less fiber, less the carboxymethyl cellulose lithium of insolubles content, both can be applied in daily life
The lithium battery of all kinds of electric equipment products is equally applicable for all kinds of dynamic lithium batteries, is used especially for new-energy automobile dynamic lithium battery.
Using the carboxymethyl cellulose lithium of this parameter and content, when as negative electrode material, it can be additionally provided Li ion for lithium battery, increased
Add the decentralised control of lithium ion total amount, improve positive and negative anodes between lithium ion insertion abjection quantity, shorten positive and negative anodes between lithium from
The path of son movement, and then improves the conductivity between positive and negative anodes and conductivity, can effectively improve lithium battery specific capacity and
Circulating battery efficiency.Compared with traditional electrode material of lithium battery using CMC-Na as electrode material additive, using this
Invention negative electrode material preparation lithium battery specific capacity improve 20% or more, cycle efficieny improves 4% or more, with use other
Parameter CMC-Li is compared as the electrode material of lithium battery of electrode material additive, using the lithium electricity of negative electrode material of the present invention preparation
Pond specific capacity improves 10% or more, and cycle efficieny improves 2% or more.
Carboxymethyl cellulose lithium of the present invention is high-purity one kind, the high grade of transparency, the carboxylic for lacking fiber, few insolubles content
Methylcellulose lithium salts can be different degree of substitution, different viscosities range level product, specific range according to concrete application demand
Are as follows: degree of substitution 0.65-1.2,1% wet button water Brookfield viscosity > 100cps, purity >=99%, 200 mesh of aqueous solution are remaining
Its aqueous solution tool high grade of transparency lacks fiber properties to object≤1ppm simultaneously, and has few insolubles content.This carboxymethyl cellulose
Lithium plays the role of " dispersing agent " in negative electrode material, can preferably disperse to negative electrode material, makes negative electrode material particle point
Cloth is uniform, stablizes, and avoids cell size each component wadding from gathering, layering, conducive to rear process operations and the even property of coating, to improve electricity
Pole chemical property；Carboxymethyl cellulose lithium also acts as the effect of " binder " in negative electrode material, and binding force is strong, can be by battery
Negative electrode material and current-collector are combined closely, and are kept stabilization of the battery in charge and discharge process, and the content of lithium ion can be improved, are mentioned
High battery diffuser efficiency and specific capacity；Carboxymethyl cellulose lithium also acts as the effect of " stabilizer " in negative electrode material, can hinder
Finely dispersed styrene-butadiene latex migrates in battery material drying process with moisture evaporation, improves styrene-butadiene latex caking property, rises
To auxiliary cementation.If the degree of substitution of CMC-Li is lower than 0.65, it is insufficient that Li ion energy is provided to negative electrode material, and bond
Power is poor, causes lithium battery cycle performance, chemical property poor；If the degree of substitution of CMC-Li is higher than the production cost of 1.2, CMC-Li
Height, and product viscosity is low, applies the cohesive force in lithium cell cathode material poor, meanwhile, dosage increases, and leads to the cost of lithium battery
It is excessively high；If the wet button water Brookfield viscosity of the 1% of CMC-Li is lower than 100cps, the CMC-Li cohesive force for crossing low viscosity is poor, leads
Lithium battery cycle performance, chemical property is caused to be deteriorated.
Specific embodiment
In the present invention, for the graphite used purchased from Hunan Star City graphite Science and Technology Co., Ltd., the conductive agent used is to lead
Electric carbon black, is purchased from Shenzhen Tai Neng new material Co., Ltd, and the carboxymethyl cellulose lithium used is that power macro fine chemistry industry in Chongqing has
Products are limited, the styrene-butadiene latex used is purchased from LG chemistry.
Embodiment 1
Take the styrene-butadiene latex of the graphite of 912g, the conductive agent of 19g, the carboxymethyl cellulose lithium (CMC-Li) of 9.5g, 9.5g
(SBR), 1.5L deionized water is taken.Carboxymethyl cellulose lithium is added to the water, stirring is complete to dissolving；Then conductive agent is added,
1h is stirred to mix；Graphite is added, is dispersed with stirring, and vacuumizes the bubble removed in water, vacuum degree≤- 0.01KPa, until without gas
Bubble is emerged, and is eventually adding styrene-butadiene latex, and stirring 1h is mixed to sticky, obtains negative electrode material, and negative electrode material is separated by sieve
Grain object, is used to prepare the cathode pole piece of lithium battery.
It is tested through applicant, 400mAh/g is reached using the lithium battery first charge-discharge specific capacity of this negative electrode material preparation,
Recycle 100 capacity retention ratios 97.9%.Same recipe be routinely free of carboxymethyl cellulose lithium (formula are as follows: the graphite of 912g,
The conductive agent of 19g, the sodium carboxymethylcellulose (CMC-Na) of 9.5g, 9.5g styrene-butadiene latex (SBR)) lithium battery specific capacity only
For 327mAh/g, 100 capacity retention ratios 93.1% are recycled.
Embodiment 2
Take the butylbenzene of the graphite of 893g, the conductive agent of 19g, the carboxymethyl cellulose lithium (CMC-Li) of 14.25g, 23.75g
Latex (SBR), takes 1.5L deionized water.Carboxymethyl cellulose lithium is added to the water, stirring is complete to dissolving；Then it is added conductive
Agent, stirring 1h are mixed；Graphite is added, is dispersed with stirring, and vacuumizes the bubble removed in water, vacuum degree≤- 0.01KPa, until
Bubble-free is emerged, and is eventually adding styrene-butadiene latex, and stirring 1h is mixed to sticky, obtains negative electrode material, negative electrode material is dissipated by screening
For particulate matter, it is used to prepare the cathode pole piece of lithium battery.
It is tested through applicant, 420mAh/g is reached using the lithium battery first charge-discharge specific capacity of this negative electrode material preparation,
Recycle 100 capacity retention ratios 98.3%, same recipe be routinely free of carboxymethyl cellulose lithium (formula are as follows: the graphite of 893g,
The conductive agent of 19g, the sodium carboxymethylcellulose (CMC-Na) of 14.25g, 23.75g styrene-butadiene latex (SBR)) lithium ion battery
Specific capacity is only 332mAh/g, recycles 100 capacity retention ratios 93.9%.The same recipe lithium of carboxymethyl cellulose containing other parameters
(formula be the graphite of 893g, the conductive agent of 19g, 14.25g carboxymethyl cellulose lithium (CMC-Li, degree of substitution 0.59,1%
Wet button water Brookfield viscosity is 80cps), the styrene-butadiene latex (SBR) of 23.75g, 1.1L deionized water) lithium ion battery
Specific capacity is only 380mAh/g, recycles 100 capacity retention ratios 96.2%.
Embodiment 3
Take the butadiene-styrene rubber of the graphite of 798g, the conductive agent of 38g, the carboxymethyl cellulose lithium (CMC-Li) of 28.5g, 85.5g
Newborn (SBR), takes 1.3L deionized water.Carboxymethyl cellulose lithium is added to the water, stirring is complete to dissolving；Then it is added conductive
Agent, stirring 1h are mixed；Graphite is added, is dispersed with stirring, and vacuumizes the bubble removed in water, vacuum degree≤- 0.01KPa, until
Bubble-free is emerged, and is eventually adding styrene-butadiene latex, and stirring 1h is mixed to sticky, obtains negative electrode material, negative electrode material is dissipated by screening
For particulate matter, it is used to prepare the cathode pole piece of lithium battery.
It is tested through applicant, 397mAh/g is reached using the lithium battery first charge-discharge specific capacity of this negative electrode material preparation,
100 capacity retention ratios 96.4% are recycled, same recipe is routinely free of carboxymethyl cellulose lithium, and (formula is graphite, the 38g of 798g
Conductive agent, the sodium carboxymethylcellulose (CMC-Na) of 28.5g, 85.5g styrene-butadiene latex (SBR)) lithium ion battery specific volume
Amount is only 302mAh/g, recycles 100 capacity retention ratios 92.6%.
Claims (10)
1. a kind of electrode material of lithium battery, which is characterized in that it include carboxymethyl cellulose lithium, the carboxymethyl cellulose lithium
Purity >=99%, 200 mesh residue of aqueous solution≤1ppm, degree of substitution 0.65-1.2,1% wet button water Brookfield viscosity >
100cps。
2. a kind of negative electrode material of lithium battery, which is characterized in that the graphite including 80-98wt%, the conductive agent of 0.5-6wt%,
The carboxymethyl cellulose lithium of 0.5-6wt%, the butadiene-styrene latex of 1-10wt%.
3. negative electrode material according to claim 2, which is characterized in that the graphite including 90-96wt%, 0.5-4wt%'s
Conductive agent, the carboxymethyl cellulose lithium of 0.5-3wt%, the butadiene-styrene latex of 1-8wt%.
4. negative electrode material according to claim 2 or 3, which is characterized in that the purity of the carboxymethyl cellulose lithium >=
99%, 200 mesh residue of aqueous solution≤1ppm, degree of substitution 0.65-1.2,1% wet button water Brookfield viscosity > 100cps.
5. negative electrode material according to claim 2 or 3, which is characterized in that the conductive agent is carbon black, electrically conductive graphite, leads
The mixing of any one or more of electric carbon fiber, carbon nanotube, graphene.
6. the preparation method of any negative electrode material of claim 2-5, has follow steps:
1) feeding in proportion；
2) carboxymethyl cellulose lithium is added to the water, dissolution is complete；
3) conductive agent is added, stirs and evenly mixs；
4) graphite is added, stirs and evenly mixs, is evacuated to bubble-free and emerges；
5) styrene-butadiene latex is added, stirs and evenly mixs, obtains negative electrode material.
7. preparation method according to claim 6, which is characterized in that water described in step 2) is deionized water or soft water.
8. preparation method according to claim 6, which is characterized in that the time of the step 3) stirring is 0.5-1h；Step
The time of rapid 4) the described stirring is 1.5-3h；The vacuum degree that step 4) vacuumizes is≤- 0.01KPa.
9. preparation method according to claim 6, which is characterized in that step 5) stirs and evenly mixs, and is separated into uniformly by sieve
Suspended nitride obtains negative electrode material.
10. a kind of lithium battery, comprising any negative electrode material of claim 2-5 as cathode.
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| CN112635724A (en) * | 2020-10-30 | 2021-04-09 | 山东精工电子科技有限公司 | Lithium ion battery cathode slurry prepared from high-substitution-degree thickening agent and preparation method of lithium ion battery cathode slurry |
| CN112751034A (en) * | 2020-12-31 | 2021-05-04 | 远景动力技术(江苏)有限公司 | Negative electrode slurry for lithium ion battery, negative electrode, and lithium ion battery |
| CN113363589A (en) * | 2021-05-19 | 2021-09-07 | 东莞维科电池有限公司 | Lithium ion battery and preparation method thereof |
| CN113372456A (en) * | 2021-07-13 | 2021-09-10 | 重庆力宏精细化工有限公司 | Ultralow-viscosity carboxymethyl cellulose lithium and preparation method and application thereof |
| CN114335544A (en) * | 2022-01-05 | 2022-04-12 | 湖南大晶新材料有限公司 | Water-based binder, lithium ion battery cathode material and lithium ion battery |
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| CN112635724A (en) * | 2020-10-30 | 2021-04-09 | 山东精工电子科技有限公司 | Lithium ion battery cathode slurry prepared from high-substitution-degree thickening agent and preparation method of lithium ion battery cathode slurry |
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| CN113372456B (en) * | 2021-07-13 | 2022-06-10 | 重庆力宏精细化工有限公司 | Ultralow-viscosity carboxymethyl cellulose lithium and preparation method and application thereof |
| CN114335544A (en) * | 2022-01-05 | 2022-04-12 | 湖南大晶新材料有限公司 | Water-based binder, lithium ion battery cathode material and lithium ion battery |
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