CN110190249A - A kind of conjunction paste-making method of silicon-carbon cathode - Google Patents
A kind of conjunction paste-making method of silicon-carbon cathode Download PDFInfo
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- CN110190249A CN110190249A CN201910317563.6A CN201910317563A CN110190249A CN 110190249 A CN110190249 A CN 110190249A CN 201910317563 A CN201910317563 A CN 201910317563A CN 110190249 A CN110190249 A CN 110190249A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- H01M4/362—Composites
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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
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/386—Silicon or alloys based on silicon
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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
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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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 invention discloses a kind of conjunction paste-making methods of silicon-carbon cathode, comprising the following steps: and binder is soluble in water, it stirs evenly and glue A is made；Liquid conduction agent is added into the glue A, stirs evenly and glue liquid B is made；Negative electrode active material, solid conduction agent and solvent are added into the glue liquid B, after continuing stirring, adjusts viscous completion to close slurry, obtains silicon-carbon cathode slurry.Binder and liquid conduction agent are mixed in the present invention, continuesd to mix again with other cathode raw materials after being uniformly dispersed, the damage of pairing slurry cylinder and rod climbing phenomenon during dry method conjunction is starched is avoided, it is lower also to solve the problems, such as that general wet process closes solid content in slurry.
Description
Technical field
The invention belongs to technical field of lithium ion, and in particular to a kind of conjunction paste-making method of silicon-carbon cathode.
Background technique
With the promotion that people require energy density, the positive and negative anodes active material of lithium ion battery is constantly updated, and is made
It obtains that positive and negative anodes are closed to starch and suffers from new requirement.
Silicon possesses the energy density that higher theoretical specific capacity is up to 3572mAh/g, but in charge and discharge process, exists
Biggish volume expansion (about 300%).SiO is with its lesser cubical expansivity (150%) and higher theoretical specific capacity
1200mAh/g and by new concern.During use in order to make cathode obtain preferable cyclical stability, ion and electricity
Subconductivity, so cathode is often with the use of SiOx/C compound system.
Traditional dry method slurry-stirring process step is more complicated, and dry mixing process early period meeting pairing slurry cylinder generates certain abrasion,
And rod-climbing effect is easy to cause since the viscosity of powder is bigger during conjunction slurry, it is most important that dry method closes the solid content of slurry
It is relatively low, there is certain requirement to slurry-stirring process parameter in powder wet processes.And traditional wet process slurry-stirring process, it is generally existing
The lower problem of slurry solid content, these all bring many inconvenience to the industrialized production of silicon-carbon cathode.
Summary of the invention
Based on this, the present invention provides a kind of conjunction paste-making method of silicon-carbon cathode, to wet process slurry-stirring process improve with it is excellent
Change, first binder and liquid conduction agent are mixed, continuesd to mix again with other cathode raw materials after being uniformly dispersed, avoids dry method conjunction
The damage of pairing slurry cylinder and rod climbing phenomenon during slurry, it is lower also to solve the problems, such as that general wet process closes solid content in slurry.
To achieve the goals above, the invention adopts the following technical scheme:
A kind of conjunction paste-making method of silicon-carbon cathode, comprising the following steps:
It is S1, binder is soluble in water, it stirs evenly and glue A is made；
Liquid conduction agent is added in S2, Xiang Suoshu glue A, stirs evenly and glue liquid B is made, wherein the liquid conduction agent is CNT
It is dispersed in water the solution to be formed；
Negative electrode active material, solid conduction agent and solvent are added in S3, Xiang Suoshu glue liquid B, after continuing stirring, viscous completion is adjusted to close
Slurry, obtains silicon-carbon cathode slurry.
Further, the binder is PP type binder, and the polyacrylic binder is by two kinds small point
Sub- polyacrylic acid unit polymerization, and modification formation is carried out with SBR polymer branch.
Further, in step S1, the stirring for forming the glue A is to stir at low speed, and the parameter stirred at low speed is
10 ~ 100rpm of rotation, revolve 10 ~ 100rpm, and mixing time is 0.5 ~ 3h, wherein the solid content of the glue A is 5% ~ 10%.
Further, in step S2, the solid content of the liquid conduction agent is 0.2% ~ 0.8%.
Further, in step S2, the stirring for forming the glue liquid B is high-speed stirred, and the parameter of the high-speed stirred is
400 ~ 2400rpm of rotation, revolve 400 ~ 2400rpm, and mixing time is 3 ~ 5h.
Further, in step S3, the negative electrode active material is SiOx/C, and the solid conduction agent is SP and KS-6,
The solvent is water.
Preferably, in the silicon-carbon cathode slurry, the mass ratio of each component is polyacrylic binder: liquid conduction
Agent: SP:KS-6:SiOx/C=(5 ~ 7): (0.1 ~ 0.3): (1.5 ~ 2.0): (1 ~ 1.5): (89.2 ~ 92.4).
Further, in step S3, the gram volume of the SiOx/C is not less than 500mAh/g.
Further, in step S3, first to stir at low speed high-speed stirred again, the parameter stirred at low speed is for the stirring
10 ~ 100rpm of rotation, revolve 10 ~ 100rpm, and mixing time is 0.1 ~ 1h, the parameter of the high-speed stirred be rotation 400 ~
2400rpm, revolve 400 ~ 2400rpm, and mixing time is 3 ~ 5h.
Further, in step S3, viscous the adjusting the specific steps are low speed defoaming after addition water of the tune is glued, and the low speed disappears
The parameter of bubble is 10 ~ 30rpm of rotation, and foam time is 0.15 ~ 0.5h, the viscosity of the silicon-carbon cathode slurry is 2000 ~
5000mPas, solid content are 35% ~ 45%.
Compared with prior art, the invention has the following advantages:
Due to the characteristic of the more difficult dispersion of CNT and the gluing process of binder, the present invention is first by binder and liquid conduction agent
Mixing solves the dispersing uniformity of CNT on the basis of guaranteeing the dispersion of glue stability, then again with other groups in slurry
Divide mixing, active material and conductive agent is allowed to absorb liquid simultaneously, soak solid particle, slurry good dispersion closes and starches knot
Higher solid content can be possessed in the case where same slurry viscosity when beam, it is low to solve solid content in traditional slurry-stirring process
The problem of, the wet process slurry-stirring process that optimizes also avoids damage and pole-climbing that dry method closes pairing slurry cylinder during slurry in the present invention
Phenomenon.
Detailed description of the invention
Fig. 1 is to be schemed using pole piece SEM made of silicon-carbon cathode slurry in embodiment 1；
Fig. 2 is to be schemed using pole piece SEM made of silicon-carbon cathode slurry in embodiment 2；
Fig. 3 is to be schemed using pole piece SEM made of silicon-carbon cathode slurry in embodiment 3.
Specific embodiment
To facilitate the understanding of the present invention, below in conjunction with specific embodiments to invention is more fully described.But
It is that the invention can be realized in many different forms, however it is not limited to embodiments described herein.On the contrary, providing
The purpose of these embodiments is to make to make the present disclosure more fully understandable.
Unless otherwise defined, all technical and scientific terms used herein and belong to technical field of the invention
The normally understood meaning of technical staff is identical.Term as used herein in the specification of the present invention is intended merely to description tool
The purpose of the embodiment of body, it is not intended that in the limitation present invention.
Embodiment 1
Specific step is as follows for the conjunction paste-making method of silicon-carbon cathode in the present embodiment:
S1,1kg mass fraction is stirred under conditions of vacuum for 12.8% polyacrylic binder and 1.3kg water
100min obtains glue A, and mixing parametric is 30 rpm of rotation, and revolve 30rpm；
Stirring 240min obtains glue liquid B after S2, the liquid conduction agent CNT that addition 0.5kg solid content is 0.4% into glue A, stirs
Parameter is mixed as rotation 1000rpm, revolution 1000rpm；
S3,2kg cathode powder SiOx/C-600A, 0.04kgSP, 0.02kgKS-6 and 0.3kg water is added into glue liquid B, first exists
Stir at low speed 10min(rotation 30rpm, revolution 30rpm), then high-speed stirred (rotation 1000rpm, revolution 1000rpm)
After 240min, water is added, and rotation 20rpm 30min defoaming tune is viscous under vacuum conditions, obtains silicon-carbon cathode slurry.
Embodiment 2
Specific step is as follows for the conjunction paste-making method of silicon-carbon cathode in the present embodiment:
S1, by 1kg mass fraction be 12.8% polyacrylic binder, 0.4kg solid content be 0.5% liquid conduction agent
CNT and 1.3kg water stir 240min under conditions of vacuum and obtain glue liquid B, and mixing parametric is rotation 40rpm, and revolve 40rpm；
S2, into glue liquid B, addition 2kg cathode powder SiOx/C-600A, 0.04kg SP, 0.02kg KS-6 and 0.3kg water are first low
Speed stirring 10min(rotation 30rpm, revolution 30rpm), then high-speed stirred (1200 rpm of rotation, revolution 1200rpm) 240min
Afterwards, water is added, and rotation 25rpm 30min defoaming tune is viscous under vacuum conditions, obtains silicon-carbon cathode slurry.
Embodiment 3
S1,0.85kg mass fraction is existed for 12.8% butadiene-styrene rubber (SBR)/carboxymethyl cellulose abandoning sodium (CMC) binder and water
0.5h is stirred under conditions of vacuum and obtains the glue A that solid content is 5% ~ 8%, and mixing parametric is rotation 10rpm, and revolve 10rpm；
S2,1.08kg solid content is added into glue A to stir 3h after 0.2% liquid conduction agent CNT and obtaining glue liquid B, stirring ginseng
Number is rotation 400rpm, revolve 400rpm；
S3, into glue liquid B, addition 2kg cathode powder SiOx/C-600A, 0.03kgSP, 0.02kgKS-6 and water are first stirred at low speed
After (rotation 100rpm, revolution 100rpm) 0.1h, then high-speed stirred (rotation 400rpm, revolution 400rpm) 5h, water is then added
Rotation 30rpm 0.15h defoaming is adjusted viscous under vacuum conditions, obtains the silicon-carbon cathode slurry that solid content is 35% ~ 45%.
Embodiment 4
S1, by 1.23kg mass fraction be 12.8% PAA binder and water stir 3h under conditions of vacuum and obtain solid content and be
8% ~ 10% glue A, mixing parametric are rotation 450rpm, and revolve 450rpm；
S2,0.84kg solid content is added into glue A to stir 5h after 0.8% liquid conduction agent CNT and obtaining glue liquid B, stirring ginseng
Number is rotation 2400rpm, revolve 2400rpm；
S3, into glue liquid B, addition 2kg cathode powder SiOx/C-600A, 0.04kgSP, 0.03kgKS-6 and 2 parts of water elder generation low speed are stirred
After mixing (rotation 10rpm, revolution 10rpm) 1h, then high-speed stirred (rotation 2400rpm, revolution 2400rpm) 3h, water is added true
Rotation 10rpm 0.5h defoaming is adjusted viscous under empty condition, and obtaining solid content is 35% ~ 45% silicon-carbon cathode slurry.
Comparative example
Specific step is as follows for the conjunction paste-making method of silicon-carbon cathode in this comparative example:
S1,1kg mass fraction is stirred into (stirring for 12.8% polyacrylic binder and 1.3kg water under conditions of vacuum
Parameter rotation 20rpm, revolve 20rpm) 100min, obtain glue；
It is S2,2kg cathode powder SiOx/C-600D, 0.04kg SP, 0.02kg KS-6 is dry-mixed under conditions of rotation 800rpm
30min is stirred, mixed powder A is obtained；
S3, the CNT rotation 800rpm stirring 30min that 1kg solid content is 0.2% is added into mixed powder A, obtains mixed powder
B；
S4, mixed powder B is added in glue in three times, under conditions of revolving speed is 30rpm, stirs 10min, rotation
After stirring 240min under conditions of 1200rpm, revolution 1200rpm, water is added, and autobiography 20rpm stirs 30min under vacuum conditions
Defoaming, which is adjusted, glues, and obtains silicon-carbon cathode slurry.
Silicon-carbon cathode piece is respectively prepared using by the silicon-carbon slurry in embodiment 1,2 and comparative example, and respectively at identical times
It is scanned electron microscope observation under several, can be seen that from Fig. 1, Fig. 2 and Fig. 3 using made of conjunction paste-making method of the invention
CNT dispersion, which is substantially better than, in negative electrode tab absolutely proves conjunction paste-making method slurry dispersion of the invention made of comparative example conjunction paste-making method
Uniformly.
Silicon-carbon cathode slurry in embodiment 1,2 and comparative example is subjected to correlated performance test, detection project and detection knot
Fruit is shown in Table 1.
Table 1
| Embodiment 1 | Embodiment 2 | Comparative example | |
| Viscosity mPas | 2562 | 3382 | 3723 |
| Solid content % | 38.55 | 38.02 | 34.78 |
| Pole piece resistivity Ω cm | 4.25 | 4.63 | 4.51 |
| Pole piece peel strength N/m | 257 | 230 | 246 |
Remarks: viscosity is measured at 25 DEG C by HAAKE RS1；
Solid content, at 160 DEG C, is measured by LHS16 A oven drying method moisture teller under conditions of 60S registration is stable；
Pole piece resistivity is measured at room temperature by Suzhou Jingge Electronic Co., Ltd. ST2258A；
Pole piece peel strength test method: pole piece being laid on flat and smooth desktop, by 3M adhesive tape it is smooth be sticked to pole piece
On, and the adhesive tape of 10cm or so is reserved at one end, adhesive tape is reserved into one end adhesive tape and pole piece tears about 2cm or so, what is made
Pole piece sample is fixed on the steel plate, with the peel strength of XLW (PC) type Intelligent electronic tensil testing machine test pole piece sample.
It can be seen from Table 1 that the conjunction slurry scheme in the present invention possesses higher solid content within the scope of similar viscosity.
Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, not to above-mentioned reality
It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, all should be considered as described in this specification.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention
Range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (10)
1. a kind of conjunction paste-making method of silicon-carbon cathode, which comprises the following steps:
It is S1, binder is soluble in water, it stirs evenly and glue A is made；
Liquid conduction agent is added in S2, Xiang Suoshu glue A, stirs evenly and glue liquid B is made, wherein the liquid conduction agent is CNT
It is dispersed in water the solution to be formed；
Negative electrode active material, solid conduction agent and solvent are added in S3, Xiang Suoshu glue liquid B, after continuing stirring, viscous completion is adjusted to close
Slurry, obtains silicon-carbon cathode slurry.
2. closing paste-making method as described in claim 1, which is characterized in that the binder is polyacrylic binder, described
Polyacrylic binder is to be polymerize by two kinds of small molecule polyacrylic acid units, and carry out modification formation with SBR polymer branch
's.
3. closing paste-making method as described in claim 1, which is characterized in that in step S1, the stirring for forming the glue A is low speed
Stirring, the parameter stirred at low speed are 10 ~ 100rpm of rotation, and revolve 10 ~ 100rpm, and mixing time is 0.5 ~ 3h, wherein institute
The solid content for stating glue A is 5% ~ 10%.
4. closing paste-making method as described in claim 1, which is characterized in that in step S2, the solid content of the liquid conduction agent exists
0.2%~0.8%。
5. closing paste-making method as described in claim 1, which is characterized in that in step S2, form the stirring of the glue liquid B as high speed
Stirring, the parameter of the high-speed stirred are 400 ~ 2400rpm of rotation, and revolve 400 ~ 2400rpm, and mixing time is 3 ~ 5h.
6. closing paste-making method as described in claim 1, which is characterized in that in step S3, the negative electrode active material is SiOx/C,
The solid conduction agent is SP and KS-6, and the solvent is water.
7. closing paste-making method as claimed in claim 6, which is characterized in that in the silicon-carbon cathode slurry, the quality of each component
Than for binder: liquid conduction agent: SP:KS-6:SiOx/C=(5 ~ 7): (0.1 ~ 0.3): (1.5 ~ 2.0): (1 ~ 1.5): (89.2 ~
92.4)。
8. closing paste-making method as described in claim 1, which is characterized in that in step S3, the gram volume of the SiOx/C is not less than
500mAh/g。
9. closing paste-making method as described in claim 1, which is characterized in that in step S3, the stirring is high first to stir at low speed again
Speed stirring, the parameter stirred at low speed are 10 ~ 100rpm of rotation, and revolve 10 ~ 100 rpm, and mixing time is 0.1 ~ 1h, described
The parameter of high-speed stirred is 400 ~ 2400rpm of rotation, and revolve 400 ~ 2400rpm, and mixing time is 3 ~ 5h.
10. closing paste-making method as described in claim 1, which is characterized in that described to adjust that viscous the specific steps are additions in step S3
Low speed defoaming is adjusted viscous after water, and the parameter of the low speed defoaming is 10 ~ 30rpm of rotation, and foam time is 0.15 ~ 0.5h, the silicon
The viscosity of Carbon anode slurry is 2000 ~ 5000mPas, and solid content is 35% ~ 45%.
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Application publication date: 20190830 |