CN106848202A - A kind of preparation method of anode plate for lithium ionic cell - Google Patents
A kind of preparation method of anode plate for lithium ionic cell Download PDFInfo
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- CN106848202A CN106848202A CN201710034632.3A CN201710034632A CN106848202A CN 106848202 A CN106848202 A CN 106848202A CN 201710034632 A CN201710034632 A CN 201710034632A CN 106848202 A CN106848202 A CN 106848202A
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
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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 relates to a kind of preparation method of anode plate for lithium ionic cell, it is comprised the following steps：(1) negative electrode active material and conductive agent are carried out dry-mixed, obtains dry-blend；(2) cathode additive agent, thickener and the first solvent are added to the dry-blend, obtains the first mixture；(3) to binding agent and the second solvent is added in the first mixture, the second mixture is obtained；(4) to the 3rd solvent is added in the second mixture, prefabricated slurry is obtained, is coated by the prefabricated slurry, obtain anode plate for lithium ionic cell, wherein, the cathode additive agent is polyether-modified organic silicone oil.By adding polyether-modified organic silicone oil, bubble removing can be effectively removed, and reach emulsifying effectiveness, thus can obtain the anode plate for lithium ionic cell of uniformity, and then improve the security of lithium ion battery.The preparation method can complete whole pulping process without previously prepared colloid in same equipment, and production efficiency is higher, and cost is relatively low.
Description
Technical field
The present invention relates to field of lithium ion battery, more particularly to a kind of preparation method of anode plate for lithium ionic cell.
Background technology
Lithium ion battery be a new generation environmental protection power supply, with energy density it is big, voltage is high, self discharge is small, without note
The advantages of recalling effect, thus, it is widely used in mobile phone, camera, notebook computer, electric tool, electric bicycle and electronic vapour
The products such as car.With the development of power lithium-ion battery, uniformity and self discharge level to battery propose higher wanting
Ask, whether slurry is uniform and stable to directly affect the coating quality of pole piece, so as to influence the final performance of battery.
Lithium ion battery negative material is broadly divided into following three kinds：Embedded type negative material, alloying type negative material and
Transformant negative material.The more of business is embedded type negative material, i.e. graphitized carbon material at present.Embedded type negative plate
Oiliness and aqueous two kinds is broadly divided into, because aqueous pole piece cost of manufacture is less than oiliness pole piece, has obtained extensive in the factory
Use.
The preparation of embedded type water-base cathode piece typically uses the following two kinds method：The first is first by negative material, bonding
Agent, conductive agent and solvent are inserted in mixer and stirred according to a certain percentage, and then coating, drying, roll-in is formed, and wherein solvent can
Disposable or muptiple-use addition；Second is that binding agent and solvent first are made into colloid, then by colloid, negative material and is led
Electric agent is placed in mixer and stirs, and then coating, drying, roll-in is formed.The two methods have a disadvantage that：First method
In, easily reunite because binding agent and other materials are added together, so as to influence the uniformity of negative plate；In second method, glue
The preparation of body needs to take a substantial amount of time, while needing to take bunkerage, which increases equipment investment and energy ezpenditure,
Influence production efficiency.
The content of the invention
The invention provides a kind of preparation method of anode plate for lithium ionic cell, the preparation method method is simple, without accounting for
With extras, production efficiency is high.The negative plate uniformity that this is obtained, security is preferable.
The present invention provides the preparation method of kind of anode plate for lithium ionic cell, and it is comprised the following steps：
(1) negative electrode active material and conductive agent are carried out dry-mixed, obtains dry-blend；
(2) cathode additive agent, thickener and the first solvent are added to the dry-blend, obtains the first mixture；
(3) to binding agent and the second solvent is added in the first mixture, the second mixture is obtained；
(4) to the 3rd solvent is added in the second mixture, prefabricated slurry is obtained, is coated by the prefabricated slurry,
Obtain anode plate for lithium ionic cell,
Wherein, the cathode additive agent is polyether-modified organic silicone oil, the chemistry of the polyether-modified organic silicone oil
Formula is：
Wherein, x is 2~8 integer, and m is 5~8 integer, and n is 5~8 integer, R1、R2、R3It is hydrogen or amino modified
C1~C5Alkyl, Z is C1~C5Alkyl or halogen, first solvent, the second solvent be identical with the 3rd solvent, described
First solvent, the second solvent, the mass ratio of the 3rd solvent are：(2~4):(2~3):(3~6).
Wherein, the cathode additive agent is single polyether-modified organic silicone oil, double polyether-modified organic silicone oils, polyether ester
Organic silicone oil, the pi-allyl containing epoxide group and the polyethers that modified organic silicone oil, chain alkyl ether and polyethers are modified altogether change altogether
At least one in organic silicone oil, the polyether-modified organic silicone oil of lithiumation of property.
Wherein, the negative electrode active material is at least one in hard carbon, soft carbon or graphite.
Wherein, the conductive agent is in carbon black, electrically conductive graphite, Ketjen black, CNT, Nano carbon fibers peacekeeping Graphene
It is at least one.
Wherein, the binding agent is at least in fluorinated polyethylene, polyvinyl alcohol, butadiene-styrene rubber and Kynoar
Kind.
Wherein, the thickener is carboxymethylcellulose calcium, hydroxyethyl cellulose, hydroxypropyl methyl cellulose, hydroxypropyl fibre
At least one in dimension element.
Wherein, first solvent is 1-METHYLPYRROLIDONE or water.
Wherein, the negative electrode active material described in step (1) and the mass ratio of conductive agent are 90~96:0.2~1.5.
Wherein, the cathode additive agent described in step (2) and the mass ratio of the negative electrode active material are 1.5~4.5:90
~96, the thickener is 1~2 with the mass ratio of the negative electrode active material:90~96.
Wherein, the binding agent described in step (3) and the mass ratio of the negative electrode active material are 1~2:90~96.
The preparation method of anode plate for lithium ionic cell of the present invention has advantages below：
First, in step (1), negative electrode active material and conductive agent are carried out into dry mixed in advance, can be with negative electrode active
Material is more sufficiently mixed uniformly with conductive agent；
Second, in step (2), add polyether-modified this cathode additive agent of organic silicone oil, on the one hand, change in polyethers
Property organic silicone oil emulsification under, negative electrode active material and conductive agent can be uniformly dispersed in the first mixture this colloid
In；On the other hand, polyether-modified organic silicone oil can reduce the surface tension of negative electrode active material, so as to avoid when binding agent with
Aggregate is formed during this colloid contact of the first mixture, is more conducive to obtain well mixed prefabricated slurry；In follow-up step
In,
A on the one hand () can effectively remove bubble removing by adding polyether-modified organic silicone oil, ensureing slurry stabilization
Shorten the slurry time simultaneously；On the other hand, emulsifying effectiveness is can reach, can be made in the case of the consumption of thickener in reducing slurry
Slurry is uniform, and avoids layering.
B () dries anode plate for lithium ionic cell after, the polyether-modified organic silicone oil of a part can be coated or is interspersed in
Between the surface of negative electrode active material or crystal grain, this can both play a part of cladding, and top layer chanza can be played again, so that
The final cycle performance for improving lithium ion battery.
C () both dissolves in oil slurry due to the polyether-modified organic silicone oil, also dissolve in water paste, thus should
The prefabricated slurry for obtaining can be aqueous or oiliness, and the preparation method scope of application is wider.
D () polyether-modified organic silicone oil can fully be soaked to the surface of mixture in step (1), make step
(1) mixture in is easier to disperse in colloid.
Finally ensure the uniformity of the anode plate for lithium ionic cell, and then improve the security of lithium ion battery.
In addition, the method is without previously prepared colloid, and whole pulping process can be completed in same equipment, thus greatly
Production efficiency is improve greatly, equipment investment and energy consumption is saved.
Brief description of the drawings
Fig. 1 is that the cycle performance of the lithium ion battery of the lithium ion electronics negative plate of the embodiment of the present invention 1 and comparative example 1 is surveyed
Attempt.
Specific embodiment
In order to the present invention is better described, specific embodiment of the invention is described in detail below in conjunction with accompanying drawing.
It will be appreciated by those skilled in the art that illustrated embodiment is served only for explaining the present invention, the scope of the present invention is not intended to limit.
The invention provides a kind of preparation method of anode plate for lithium ionic cell.The preparation method is comprised the following steps：
S1, negative electrode active material and conductive agent is carried out dry-mixed, obtains dry-blend；
S2, cathode additive agent, thickener and the first solvent are added to the dry-blend, obtain the first mixture；
S3, to binding agent and the second solvent is added in the first mixture, obtains the second mixture；
S4, to the 3rd solvent is added in the second mixture, obtains prefabricated slurry, is coated by the prefabricated slurry,
Obtain anode plate for lithium ionic cell.
Wherein, the cathode additive agent is polyether-modified organic silicone oil, the chemistry of the polyether-modified organic silicone oil
Formula is：
Wherein, x is 2~8 integer, and m is 5~8 integer, and n is 5~8 integer, R1、R2、R3It is hydrogen or amino modified
C1~C5Alkyl, Z is C1~C5Alkyl or halogen, first solvent, the second solvent be identical with the 3rd solvent, described
First solvent, the second solvent, the mass ratio of the 3rd solvent are：(2~4):(2~3):(3~6).
In step sl, the negative electrode active material is at least one in hard carbon, soft carbon or graphite.The conductive agent is used
In the electric conductivity for improving the anode plate for lithium ionic cell.The conductive agent is carbon black, electrically conductive graphite, Ketjen black, carbon nanometer
At least one in pipe, Nano carbon fibers peacekeeping Graphene.The negative electrode active material is 90~96 with the mass ratio of conductive agent:
0.2~1.5.Preferably, negative electrode active material and the mass ratio of conductive agent are 90~96:0.5~1.3.
In step s 2, to be polyether-modified organic silicone oil or alkyl modified organic altogether with polyethers for the cathode additive agent
Silicone oil, wherein, polyether chain is bonded on the end of linear silicones or side chain.Specifically, the cathode additive agent is single poly-
The ester modified organic silicone oil of the modified organic silicone oil of ether, double polyether-modified organic silicone oils, polyethers, chain alkyl ether and polyethers are common
Modified organic silicone oil or the pi-allyl containing epoxide group has with the polyether-modified of the organic silicone oil, lithiumation that polyethers is modified altogether
Machine silicone oil.Preferably, the cathode additive agent is organic silicone oil, the lithiumation that the pi-allyl containing epoxide group is modified altogether with polyethers
Polyether-modified organic silicone oil.
First solvent is 1-METHYLPYRROLIDONE (NMP) or water.The cathode additive agent and the negative electrode active material
The mass ratio of matter is 1.5~4.5:90~96.Preferably, the cathode additive agent is with the mass ratio of the negative electrode active material
2~3:90~96.
The thickener is carboxymethylcellulose calcium (CMC), hydroxyethyl cellulose (HEC), hydroxypropyl methyl cellulose
(HPMC), at least one in hydroxypropyl cellulose (H-HPC).The thickener is with the mass ratio of the negative electrode active material
1~2:90~96.Preferably, the thickener is carboxymethylcellulose calcium, the matter of the thickener and the negative electrode active material
Amount is than being 1.3~1.5:90~96.
In step s3, the binding agent is viscous with collector during coating for improving the prefabricated slurry for obtaining
Close intensity.The binding agent is fluorinated polyethylene (PDFE), polyvinyl alcohol (PVA), butadiene-styrene rubber (SBR) and Kynoar
(PVDF) at least one in.Preferably, the binding agent is SBR or PVDF.
The binding agent is 1~2 with the mass ratio of the negative electrode active material:90~96.Preferably, the binding agent with
The mass ratio of the negative electrode active material is 1.5~2:90~96.
For a better understanding of the present invention, below by specific embodiment to anode plate for lithium ionic cell of the invention
Preparation method is further described.
Embodiment 1
93g negative electrode active materials and 1.5g conductive agents are carried out dry-mixed, obtain dry-blend, wherein negative electrode active material is behaved
Graphite is made, conductive agent is Super P.
2g cathode additive agents, 2gCMC and 45g water are added to the dry-blend, the first mixture, wherein negative pole addition is obtained
Agent is the organic silicone oil that the pi-allyl containing epoxide group is modified altogether with polyethers.
To 1.5g binding agents and 35g water is added in the first mixture, the second mixture is obtained, wherein binding agent is.
To 40g water is added in the second mixture, prefabricated slurry is obtained, be coated by the prefabricated slurry, obtain lithium
Ion battery negative plate.
Embodiment 2
95.5g negative electrode active materials and 0.5g conductive agents are carried out dry-mixed, obtain dry-blend, wherein negative electrode active material is
Graphite, conductive agent is CNT.
2g cathode additive agents and 35g NMP are added to the dry-blend, the first mixture is obtained, wherein cathode additive agent is
The polyether-modified organic silicone oil of lithiumation.
To 2g binding agents and 35g NMP is added in the first mixture, the second mixture is obtained, wherein binding agent is PVDF.
To 50g NMP are added in the second mixture, prefabricated slurry is obtained, be coated by the prefabricated slurry, obtained
Anode plate for lithium ionic cell.
Embodiment 3
93g negative electrode active materials and 1.5g conductive agents are carried out dry-mixed, obtain dry-blend, wherein negative electrode active material is behaved
Graphite is made, conductive agent is Super P.
2gCMC and 45g water is added to the dry-blend, the first mixture is obtained.
To 1.5g binding agents and 35g water is added in the first mixture, the second mixture is obtained, wherein binding agent is.
To 40g water is added in the second mixture, prefabricated slurry is obtained, be coated by the prefabricated slurry, obtain lithium
Ion battery negative plate.
It is also special that a contrast is provided in order to better illustrate the advantage of the preparation method of anode plate for lithium ionic cell of the invention
Example 1 and comparative example 2.
Comparative example 1
The preparation method of the lithium-ion negative pole piece of the comparative example 1 is as follows：
By 93g negative materials, 1.5g binding agents, 1.5g conductive agents, 2g thickener CMC and 120g solvents according to certain matter
Amount ratio insert in mixer stir, be then coated, dry, roll-in and obtain lithium-ion negative pole piece.Wherein, negative material
It is Delanium, binding agent is SBR, and conductive agent is Super P, and solvent is water.
Comparative example 2
The preparation method of the lithium-ion negative pole piece of the comparative example 2 is as follows：
1.5g binding agents, 2g thickener CMC and 120g solvents are made colloid, then by colloid, 93g negative materials and
1.5g conductive agents insert in mixer stir, then be coated with, drying, roll-in and obtain lithium-ion negative pole piece.Wherein, binding agent is
SBR, solvent is water, and negative material is Delanium, and conductive agent is Super P.
The anode plate for lithium ionic cell that embodiment 1 and 2, comparative example 1 and 2 are obtained is made lithium ion battery, and tests it
Cycle performance of battery and security performance.Test result is shown in Table 1.
Table 1
From table 1 and Fig. 1, for comparative example 1,2, the circulation of the lithium ion battery that the present embodiment 1 and 2 is obtained
Better performances, more than 95% is held in by capability retention after 1C/1C circulations in 500 weeks, and comparative example 1,2 was by 500 weeks
Capability retention is held in less than 90% after 1C/1C circulations, while the electric discharge first of the lithium ion battery that embodiment 1,2 is obtained
Capacity also will height compared with comparative example 1,2.The security performance percent of pass of lithium ion battery is more than 80% in embodiment 1,2, and right
The security performance testing differentia of ratio 1,2 is larger, this further illustrates anode plate for lithium ionic cell manufactured in the present embodiment tool
There is good uniformity, its cycle performance and security performance difference are smaller, relatively stable.Embodiment 3 is not added with cathode additive agent,
Its first discharge capacity it is lower than embodiment 1,2, and comparative example 1,2 quite, this illustrate cathode additive agent can improve lithium from
The efficiency first of sub- battery and first discharge capacity, its cycle performance and security performance have declined than embodiment 1,2, but compare
Ratio 1,2 is high, and this illustrates that the negative pole preparation method and cathode additive agent rise to the cycle performance and security performance of negative plate
Important effect.
Embodiment described above only expresses several embodiments of the invention, and its description is more specific and detailed, but simultaneously
Therefore the limitation to the scope of the claims of the present invention can not be interpreted as.It should be pointed out that for one of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to guarantor of the invention
Shield scope.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (10)
1. a kind of preparation method of anode plate for lithium ionic cell, it is characterised in that it is comprised the following steps：
(1) negative electrode active material and conductive agent are carried out dry-mixed, obtains dry-blend；
(2) cathode additive agent, thickener and the first solvent are added to the dry-blend, obtains the first mixture；
(3) to binding agent and the second solvent is added in the first mixture, the second mixture is obtained；
(4) to the 3rd solvent is added in the second mixture, prefabricated slurry is obtained, is coated by the prefabricated slurry, obtained
Anode plate for lithium ionic cell,
Wherein, the cathode additive agent is polyether-modified organic silicone oil, the chemical general formula of the polyether-modified organic silicone oil
For：
Wherein, x is 2~8 integer, and m is 5~8 integer, and n is 5~8 integer, R1、R2、R3It is hydrogen or amino modified C1~
C5Alkyl, Z is C1~C5Alkyl or halogen, first solvent, the second solvent be identical with the 3rd solvent, and described first is molten
Agent, the second solvent, the mass ratio of the 3rd solvent are：(2~4):(2~3):(3~6).
2. the preparation method of anode plate for lithium ionic cell according to claim 1, it is characterised in that the cathode additive agent
For the ester modified organic silicone oil of single polyether-modified organic silicone oil, double polyether-modified organic silicone oils, polyethers, chain alkyl ether with
Organic silicone oil that organic silicone oil that polyethers is modified altogether, the pi-allyl containing epoxide group and polyethers are modified altogether, lithiumation it is polyether-modified
Organic silicone oil at least one.
3. the preparation method of anode plate for lithium ionic cell according to claim 1, it is characterised in that the negative electrode active material
Matter is at least one in hard carbon, soft carbon or graphite.
4. the preparation method of anode plate for lithium ionic cell according to claim 1, it is characterised in that the conductive agent is carbon
At least one in black, electrically conductive graphite, Ketjen black, CNT, Nano carbon fibers peacekeeping Graphene.
5. the preparation method of anode plate for lithium ionic cell according to claim 1, it is characterised in that the binding agent is fluorine
For at least one in polyethylene, polyvinyl alcohol, butadiene-styrene rubber and Kynoar.
6. the preparation method of anode plate for lithium ionic cell according to claim 1, it is characterised in that the thickener is carboxylic
At least one in methylcellulose, hydroxyethyl cellulose, hydroxypropyl methyl cellulose, hydroxypropyl cellulose.
7. the preparation method of anode plate for lithium ionic cell according to claim 1, it is characterised in that first solvent is
1-METHYLPYRROLIDONE or water.
8. the preparation method of anode plate for lithium ionic cell according to claim 1, it is characterised in that the institute in step (1)
It is 90~96 that negative electrode active material is stated with the mass ratio of conductive agent:0.2~1.5.
9. the preparation method of anode plate for lithium ionic cell according to claim 1, it is characterised in that the institute in step (2)
It is 1.5~4.5 that cathode additive agent is stated with the mass ratio of the negative electrode active material:90~96, the thickener and the negative pole
The mass ratio of active material is 1~2:90~96.
10. the preparation method of anode plate for lithium ionic cell according to claim 1, it is characterised in that the institute in step (3)
It is 1~2 that binding agent is stated with the mass ratio of the negative electrode active material:90~96.
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| CN107507956A (en) * | 2017-07-28 | 2017-12-22 | 山东嘉寓润峰新能源有限公司 | Lithium ion battery slurry coating process |
| CN108305987A (en) * | 2018-01-31 | 2018-07-20 | 北京国能电池科技股份有限公司 | Proportioning process, anode plate for lithium ionic cell and the lithium ion battery of lithium ion battery anode slurry |
| CN108493451A (en) * | 2018-02-28 | 2018-09-04 | 北京国能电池科技股份有限公司 | Negative electrode binder and negative material and preparation method thereof and low-temperature lithium ion battery |
| CN111180746A (en) * | 2019-12-31 | 2020-05-19 | 蔚蓝(广东)新能源科技有限公司 | Air electrode preparation method and metal-air electrode |
| CN111509191A (en) * | 2020-04-24 | 2020-08-07 | 中科(马鞍山)新材料科创园有限公司 | Negative electrode slurry, preparation method thereof and lithium ion battery |
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| CN114864877A (en) * | 2022-05-20 | 2022-08-05 | 湖北亿纬动力有限公司 | Preparation method and application of negative pole piece |
| CN114976010A (en) * | 2022-06-16 | 2022-08-30 | 深圳市研一新材料有限责任公司 | Negative electrode additive and preparation method and application thereof |
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| CN111509191A (en) * | 2020-04-24 | 2020-08-07 | 中科(马鞍山)新材料科创园有限公司 | Negative electrode slurry, preparation method thereof and lithium ion battery |
| CN114864877A (en) * | 2022-05-20 | 2022-08-05 | 湖北亿纬动力有限公司 | Preparation method and application of negative pole piece |
| CN114976010A (en) * | 2022-06-16 | 2022-08-30 | 深圳市研一新材料有限责任公司 | Negative electrode additive and preparation method and application thereof |
| CN114976010B (en) * | 2022-06-16 | 2023-06-30 | 深圳市研一新材料有限责任公司 | Negative electrode additive and preparation method and application thereof |
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Effective date of registration: 20221109 Address after: No. 10-2, Shidai Road, Haining Economic Development Zone, Haining, Jiaxing, Zhejiang 314499 Patentee after: ZHEJIANG MEIDARUI NEW MATERIAL TECHNOLOGY Co.,Ltd. Address before: No. 1, Haiyuan Road, Haining Economic Development Zone, Jiaxing, Zhejiang 314400 Patentee before: HAINING JUXING NEW ENERGY TECHNOLOGY CO.,LTD. |