CN109698349A - Preparation method suitable for the binder of high capacity silicon-based anode, cathode and high specific energy lithium ion battery - Google Patents
Preparation method suitable for the binder of high capacity silicon-based anode, cathode and high specific energy lithium ion battery Download PDFInfo
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- CN109698349A CN109698349A CN201811479003.2A CN201811479003A CN109698349A CN 109698349 A CN109698349 A CN 109698349A CN 201811479003 A CN201811479003 A CN 201811479003A CN 109698349 A CN109698349 A CN 109698349A
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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
- H01M4/622—Binders being polymers
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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
-
- 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
- H01M10/058—Construction or manufacture
-
- 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
- H01M4/134—Electrodes based on metals, Si or alloys
-
- 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
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention belongs to field of batteries more particularly to a kind of preparation methods of the binder suitable for high capacity silicon-based anode, and the cathode and high specific energy lithium ion battery that are prepared using the binder.Specifically: it uses in amino aqueous solution with PAA solution, the aqueous binders that pH value is 7-8 is prepared.Novel binders prepared by the present invention have the advantage that no coupling product and foreign ion introduce, and processing performance is excellent, is suitable for the biggish high-capacity cathode material of volume change, and silicon substrate cycle performance of lithium ion battery obtained is excellent.
Description
Technical field
The invention belongs to field of batteries more particularly to a kind of preparation sides of the binder suitable for high capacity silicon-based anode
Method, and the cathode and high specific energy lithium ion battery that are prepared using the binder.
Background technique
Lithium ion battery as a kind of novel energy-storing power supply be widely used in the market 3C, electric tool, electric car,
The fields such as aerospace, as the demand to lithium ion battery energy density is higher and higher, the capacity of traditional positive and negative pole material is sent out
It waves and has been approached the limit, be badly in need of the positive and negative pole material of exploitation higher capacity.In recent years, the silicium cathode material (theoretical capacity of ultra-high capacity
4200mAh/g) receive extensive concern both domestic and external, it is considered to be the ideal candidates material of next-generation high specific energy lithium ion battery
Material.But serious bulk effect and loop attenuation are the deadly defects of silicium cathode material, silicium cathode is in charge and discharge process
Volume expansion will lead to active material particle and cracking, dusting occur, or even remove with collector, lose electrical contact, this is to cause
One of the main reason for cathode circulation failure.Therefore, binder as between active material and active material and collector it
Between connection bridge, played a crucial role in the application study of silicium cathode.
Polyacrylic acid (poly (acrylic acid), abbreviation PAA) binder has a large amount of-COOH group, can be with silicon
- OH the group of negative terminal surface forms hydrogen bond, enhances the binding force between binder and active material, and hydrogen bond is different from other
Chemical bond, it constantly can be broken and live again, and this self-reparing capability can buffer volume of the silicon-based anode in cyclic process
Stress effectively promotes the long circulating stability of pole piece.But due to the presence of a large amount of-COOH group, PAA binder it is water-soluble
Liquid pH value generally in 2-4 or so, easily causes particle agglomeration when being directly used in the preparation of silicon-based anode, influences negative electrode slurry dispersion,
Lead to capacity of negative plates and cyclical stability degradation.
Summary of the invention
In view of the above-mentioned problems, it is an object of the invention to propose a kind of novel binders suitable for high capacity silicon-based anode
Preparation method, which can be directly used for the preparation of high capacity silicon-based anode and high specific energy lithium ion battery.Preparation process
Middle amino-compound is heated when cathode coats to be decomposed completely, and decomposition product volatilizees together with aqueous solvent, is finally prepared into performance
Stable silicon-based anode pole piece.
In order to realize upper purpose, the preparation method of the binder provided by the invention suitable for high capacity silicon-based anode, tool
Body are as follows: using in amino aqueous solution and PAA solution, being prepared the aqueous binders that pH value is 7-8, dosage be according to ph value come
Fixed, experimentation is that amino aqueous solution is gradually added into PAA solution, until entire solution ph reaches 7~8.
The amino aqueous solution is one or both of ammonium hydroxide or carbonic acid hydrogen ammonium, Solute mass fraction 0.1%-
50%；The PAA solution is the aqueous solution of polyacrylic acid, and the molecular weight of polyacrylic acid is 1000-450000, Solute mass point
Number is 0.1%-50%.
Another object of the present invention, the present invention also provides a kind of preparation method of high capacity silicon-based anode, specifically: it will
High-capacity cathode material, conductive agent and binder prepared by the present invention with M:N:L (M+N+L=1,0.7≤M≤0.98,0.01≤
N≤0.2,0.01≤L≤0.2) mass ratio be uniformly mixed, be made negative electrode slurry；Negative electrode slurry is coated on copper foil, single side
Coating surface density is 0.1~15mg/cm2, for 24 hours through 60~100 DEG C of bakings, 60~90 DEG C of vacuum drying, it is prepared into pole piece.
The negative electrode material is the mixture or silicon-carbon, silicon of one or more of silicon-carbon, silicon oxygen, nano-silicon
The mixture of one or more of oxygen, nano-silicon and graphite cathode material.
Another object of the present invention, the present invention also provides a kind of preparation method of high specific energy lithium ion battery, specifically:
In a manner of Z-type lamination, anode pole piece, diaphragm, the alternate lamination of cathode pole piece prepared by the present invention are formed into battery core, injection electrolysis
Liquid is packed with aluminum plastic film, aluminum hull or stainless steel case, battery is prepared.
The positive active material of the anode pole piece is LiNixCoyMnzO2(x+y+z=1), LiNixCoyAlzO2(x+y+z
=1), xLi2MnO3·(1-x)[LiNiyCozMn(1-y-z)O2] in (0≤x≤1,0≤y≤1,0≤z≤1 and 0≤y+z≤1)
One or more mixtures.
Significant technical effect of the invention: novel binders prepared by the present invention have the advantage that no coupling product and miscellaneous
Matter ion introduces, and processing performance is excellent, is suitable for the biggish high-capacity cathode material of volume change, silicon substrate lithium-ion electric obtained
Pond cycle performance is excellent.
Detailed description of the invention
Fig. 1 is the circulation volume curve that embodiment 1 and comparative example 1 prepare battery.
Specific embodiment
Combined with specific embodiments below, technical solution of the present invention is described in further detail, but the present invention is not
It is limited to these embodiments.
Embodiment 1
Using the deionized water of 93 mass parts as solvent, the polyacrylic acid powder of 7 mass parts is added, is filled by mechanical agitator
Divide dissolution, tests solution ph.Meanwhile using the deionized water of 95 mass parts as solvent, the ammonium hydrogen carbonate of 5 mass parts is added, leads to
It crosses mechanical agitator sufficiently to dissolve, ammonium bicarbonate soln is made.Ammonium bicarbonate soln is added dropwise in polyacrylic acid solution, it is real
When monitor solution ph, until solution ph is adjusted to 7.5, novel bonding agent solution is made.
Using the deionized water of 100 mass parts as solvent, the binder of 6 mass parts, the SP of 2 mass parts, 80 matter are sequentially added
The graphite of part and the oxidation Asia silicon of 12 mass parts are measured, stirs evenly to form slurry in double-planet power mixer, is uniformly coated
On the copper foil of affluxion body of 6 μ m-thicks, 80 DEG C of vacuum drying carry out roll-in with roll squeezer afterwards for 24 hours, and punching is prepared into negative electrode tab.
Using the NMP of 50 mass parts as solvent, the PVDF-5130 of 4 mass parts, the SP of 2 mass parts and 94 mass are sequentially added
The NCA positive electrode of part, stirs evenly to form slurry in double-planet power mixer, is coated uniformly on the aluminium foil of 13 μ m-thicks
On, 100 DEG C of vacuum drying carry out roll-in with roll squeezer afterwards for 24 hours, and punching is prepared into positive plate.
In a manner of Z-type lamination, anode pole piece, diaphragm, the alternate lamination of cathode pole piece are formed into battery core, welding, aluminum plastic film
Encapsulation, injects electrolyte, and sealing is prepared into flexible packing lithium ion battery.Wherein, diaphragm is nano oxidized using dual coating
The ceramic diaphragm of alumina particles, with a thickness of 25 μm；Electrolyte is 1.0mol/L LiPF6, EC/EMC/DMC=1:1:1,2%VC.
Comparative example 1
Using the deionized water of 93 mass parts as solvent, the polyacrylic acid powder of 7 mass parts is added, is filled by mechanical agitator
Divide dissolution, binder solution is made.
Using the deionized water of 100 mass parts as solvent, the binder of 6 mass parts, the SP of 2 mass parts, 80 matter are sequentially added
The graphite of part and the oxidation Asia silicon of 12 mass parts are measured, stirs evenly to form slurry in double-planet power mixer, is uniformly coated
On the copper foil of affluxion body of 6 μ m-thicks, 80 DEG C of vacuum drying carry out roll-in with roll squeezer afterwards for 24 hours, and punching is prepared into negative electrode tab.
Using the NMP of 50 mass parts as solvent, the PVDF-5130 of 4 mass parts, the SP of 2 mass parts and 94 mass are sequentially added
The NCA positive electrode of part, stirs evenly to form slurry in double-planet power mixer, is coated uniformly on the aluminium foil of 13 μ m-thicks
On, 100 DEG C of vacuum drying carry out roll-in with roll squeezer afterwards for 24 hours, and punching is prepared into positive plate.
In a manner of Z-type lamination, anode pole piece, diaphragm, the alternate lamination of cathode pole piece are formed into battery core, welding, aluminum plastic film
Encapsulation, injects electrolyte, and sealing is prepared into flexible packing lithium ion battery.Wherein, diaphragm is nano oxidized using dual coating
The ceramic diaphragm of alumina particles, with a thickness of 25 μm；Electrolyte is 1.0mol/L LiPF6, EC/EMC/DMC=1:1:1,2%VC.
Embodiment 1 and comparative example 1 prepare the electrical property comparison of battery, are shown in Table 1；Embodiment 1 and comparative example 1 prepare battery
Circulation volume curve, is shown in Fig. 1.
1 embodiment 1 of table and comparative example 1 prepare the electrical property comparison of battery.
Embodiment 2.
Using the deionized water of 92 mass parts as solvent, the polyacrylic acid powder of 8 mass parts is added, is filled by mechanical agitator
Divide dissolution, tests solution ph.Meanwhile using the deionized water of 94 mass parts as solvent, the ammonium hydrogen carbonate of 6 mass parts is added, leads to
It crosses mechanical agitator sufficiently to dissolve, ammonium bicarbonate soln is made.Ammonium bicarbonate soln is added dropwise in polyacrylic acid solution, it is real
When monitor solution ph, until solution ph is adjusted to 8.0, novel bonding agent solution is made.
Using the deionized water of 100 mass parts as solvent, the binder of 6 mass parts, the SP of 3 mass parts, 70 matter are sequentially added
The graphite of part and the oxidation Asia silicon of 21 mass parts are measured, stirs evenly to form slurry in double-planet power mixer, is uniformly coated
On the copper foil of affluxion body of 6 μ m-thicks, 80 DEG C of vacuum drying carry out roll-in with roll squeezer afterwards for 24 hours, and punching is prepared into negative electrode tab.
Using the NMP of 50 mass parts as solvent, the PVDF-5130 of 4 mass parts, the SP of 3 mass parts and 93 mass are sequentially added
The lithium-rich anode material of part, stirs evenly to form slurry in double-planet power mixer, is coated uniformly on the aluminium foil of 13 μ m-thicks
On, 100 DEG C of vacuum drying carry out roll-in with roll squeezer afterwards for 24 hours, and punching is prepared into positive plate.
In a manner of Z-type lamination, anode pole piece, diaphragm, the alternate lamination of cathode pole piece are formed into battery core, welding, aluminum plastic film
Encapsulation, injects electrolyte, and sealing is prepared into flexible packing lithium ion battery.Wherein, diaphragm is using three layers of polyalkene diaphragm,
With a thickness of 25 μm；Electrolyte is 1.2mol/L LiPF6, EC/EMC=3:7,2%VC.
For flexible packing lithium ion battery obtained in the voltage range of 2.0V-4.6V, 0.1C discharge capacity is 22.8Ah, is put
Electric specific energy 380Wh/kg, 0.2C/0.5C are recycled 100 times, and capacity retention ratio is greater than 70%.
Embodiment 3.
Using the deionized water of 90 mass parts as solvent, the polyacrylic acid powder of 10 mass parts is added, passes through mechanical agitator
Solution ph is tested in sufficiently dissolution.Meanwhile using the deionized water of 92 mass parts as solvent, the ammonium hydrogen carbonate of 8 mass parts is added,
It is sufficiently dissolved by mechanical agitator, ammonium bicarbonate soln is made.Ammonium bicarbonate soln is added dropwise in polyacrylic acid solution,
Novel bonding agent solution is made until solution ph is adjusted to 7.0 in real-time monitoring solution ph.
Using the deionized water of 100 mass parts as solvent, the binder of 8 mass parts, the SP of 2 mass parts, 80 matter are sequentially added
The graphite of part and the oxidation Asia silicon of 10 mass parts are measured, stirs evenly to form slurry in double-planet power mixer, is uniformly coated
On the copper foil of affluxion body of 8 μ m-thicks, 80 DEG C of vacuum drying carry out roll-in with roll squeezer afterwards for 24 hours, and punching is prepared into negative electrode tab.
Using the NMP of 50 mass parts as solvent, the PVDF-5130 of 4 mass parts, the SP of 1 mass parts and 95 mass are sequentially added
The tertiary cathode material of part, stirs evenly to form slurry in double-planet power mixer, is coated uniformly on the aluminium foil of 15 μ m-thicks
On, 100 DEG C of vacuum drying carry out roll-in with roll squeezer afterwards for 24 hours, and punching is prepared into positive plate.
In a manner of Z-type lamination, anode pole piece, diaphragm, the alternate lamination of cathode pole piece are formed into battery core, pole welding enters
Shell, injects electrolyte, and sealing is prepared into hermetically sealed lithium ion battery.Wherein, diaphragm is thick using monolayer polyethylene diaphragm
Degree is 20 μm；Electrolyte is 1.0mol/L LiPF6, EC/EMC=3:7,2%VC, 2%FEC.
For hermetically sealed lithium ion battery obtained in the voltage range of 3.0V-4.1V, 0.2C discharge capacity is 52Ah, electric discharge
Specific energy 250Wh/kg.
Although the contents of the present invention are explained in detail by above preferred embodiment, but it should be appreciated that above-mentioned
Illustrate to be not considered as limitation of the present invention.After those skilled in the art have read above content, for of the invention
A variety of modifications and substitutions all will be apparent.Therefore, protection scope of the present invention should be limited to the appended claims.
Claims (6)
1. a kind of preparation method of the binder suitable for high capacity silicon-based anode, which is characterized in that specifically: use amino water
With PAA solution in solution, the aqueous binders that pH value is 7-8 are prepared.
2. the preparation method suitable for the binder of high capacity silicon-based anode as described in claim 1, which is characterized in that described
Amino aqueous solution be one or both of ammonium hydroxide or carbonic acid hydrogen ammonium, Solute mass fraction 0.1%-50%；The PAA
Solution is the aqueous solution of polyacrylic acid, and the molecular weight of polyacrylic acid is 1000-450000, Solute mass fraction 0.1%-
50%.
3. a kind of preparation method of high capacity silicon-based anode, which is characterized in that specifically: by high-capacity cathode material, conductive agent
It is uniformly mixed with binder of any of claims 1 or 2, negative electrode slurry is made；Negative electrode slurry is coated on copper foil, through drying
Roasting, vacuum drying, is prepared into pole piece.
4. the preparation method of high capacity silicon-based anode as claimed in claim 3, which is characterized in that the negative electrode material be comprising
One of materials such as silicon-carbon, silicon oxygen, nano-silicon or a variety of mixtures, or comprising silicon materials and graphite cathode material
One or more mixtures.
5. a kind of preparation method of high specific energy lithium ion battery, which is characterized in that specifically: it, will be positive in a manner of Z-type lamination
Pole piece, diaphragm, the alternate lamination of cathode pole piece described in claim 3 or 4 form battery core, electrolyte are injected, with aluminum plastic film, aluminum hull
Or stainless steel case packaging, battery is prepared.
6. the preparation method of high specific energy lithium ion battery as claimed in claim 5, which is characterized in that the anode pole piece is just
Pole active material is LiNixCoyMnzO2、LiNixCoyAlzO2、xLi2MnO3·(1-x)[LiNiyCozMn(1-y-z)O2One of]
Or two or more mixture, wherein x+y+z=1,0≤x≤1,0≤y≤1,0≤z≤1 and 0≤y+z≤1.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114122331A (en) * | 2021-11-19 | 2022-03-01 | 蜂巢能源科技(无锡)有限公司 | Modified silicon-based negative electrode plate and preparation method and application thereof |
| CN116613390A (en) * | 2023-07-21 | 2023-08-18 | 宁德新能源科技有限公司 | Battery and electronic equipment |
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