CN106450334B - Positive plate of lithium battery, lithium battery and preparation method with graphene conductive skeleton - Google Patents
Positive plate of lithium battery, lithium battery and preparation method with graphene conductive skeleton Download PDFInfo
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- CN106450334B CN106450334B CN201611044711.4A CN201611044711A CN106450334B CN 106450334 B CN106450334 B CN 106450334B CN 201611044711 A CN201611044711 A CN 201611044711A CN 106450334 B CN106450334 B CN 106450334B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/058—Construction or manufacture
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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
- H01M4/133—Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- 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
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Abstract
The invention discloses a kind of positive plate of lithium battery with graphene conductive skeleton, lithium battery and preparation methods, solve existing using LiFePO4 as the low technical problem low with diffusion rate of the lithium ion battery conductivity of positive electrode.Including positive electrode substrate, graphene conductive skeleton and positive electrode active materials；Graphene conductive skeleton is made of multiple unit groove bodies being connected with each other；Graphene conductive skeleton is printed on positive electrode substrate with 3D printing technique；Positive electrode active materials are filled in multiple unit groove bodies.Conducting matrix grain with graphene can effectively improve electronic conductivity and lithium ion diffusion rate in positive electrode active materials, can be improved lithium battery volume and capacity ratio and energy density, and then improve charging rate, improve the high rate performance and cycle performance of lithium battery.
Description
Technical field
The invention belongs to battery technology fields, specifically, being to be related to a kind of lithium battery with graphene conductive skeleton just
Pole piece, lithium battery and preparation method.
Background technique
Lithium ion battery is a kind of secondary cell namely rechargeable battery, it rely primarily on lithium ion anode and cathode it
Between move to realize the charge and discharge of battery.
In the positive electrode of existing lithium ion battery, LiFePO4 (LiFePO4) anode with olivine framework
Material extensive, cheap, nontoxic, environmentally friendly, no hygroscopicity, theoretical specific volume height, operating voltage phase with its raw material sources
To it is moderate the advantages that become lithium ion battery first choice positive electrode；But the low electronic conductivity of LiFePO4 and low lithium ion expand
Scattered rate causes its performance in high current charge-discharge poor, constrains LiFePO 4 material in the popularization in power battery field
Using.
What is proposed in the industry solves the problems, such as the major technique packet of the low electronic conductivity of LiFePO4 and low lithium ion diffusion rate
It includes: 1, adding conductive agent in LiFePO4 to improve crystal grain electronic conductivity, mainly there is surface carbon package and metal micro particles
Calking, so that preparing LiFePO4/C or LiFePO4/M(M is metal) composite material, while using nanotechnology increase
Inter-granular contact areas simultaneously reduces lithium ion diffusion path；2, the cation position containing transition metal in LiFePO4 lattice from
Son improves electronic conductivity and lithium ion diffusion rate in crystal grain.But these methods are because there are complex process and be easy to cause
LiFePO4 tap density decline the problem of and be difficult to industrialization.
Summary of the invention
This application provides a kind of lithium battery and preparation method thereof with graphene conductive skeleton solves existing with phosphoric acid
Iron lithium is the low technical problem low with diffusion rate of lithium ion battery conductivity of positive electrode.
In order to solve the above technical problems, the application is achieved using following technical scheme:
It is proposed a kind of positive plate of lithium battery with graphene conductive skeleton, including positive electrode substrate, graphene conductive skeleton and
Positive electrode active materials；The graphene conductive skeleton is made of multiple unit groove bodies being connected with each other；The graphene conductive bone
Frame is printed on the positive electrode substrate with 3D printing technique；The filling positive electrode active materials in the multiple unit groove body.
Further, the 3D printing material of the graphene conductive skeleton is graphene and Kynoar in mass ratio 9:
1 mixed mixing material.
Further, the 3D printing height of the graphene conductive skeleton is 0.05mm-0.1mm, the graphene conductive
The wall thickness of skeleton is 0.03mm-0.05mm.
Further, the cross-sectional area of the unit groove body is 500mm*350mm.
Further, the positive electrode active materials are LiFePO4 or cobalt acid lithium, LiMn2O4, nickel-cobalt-manganese ternary material.
It is proposed a kind of lithium battery with graphene conductive skeleton, just including the above-mentioned lithium battery with graphene conductive skeleton
Pole piece.
It proposes a kind of lithium battery anode piece preparation method with graphene conductive skeleton, is used to prepare above-mentioned band graphene
The positive plate of lithium battery of conducting matrix grain, comprising: graphene is put into ball mill after mixing with Kynoar 9:1 in mass ratio and grinds
Mill, and add N-Methyl pyrrolidone after the completion of grinding and be adjusted to printing slurry；Using the printing slurry as raw material, using 3D
The printing slurry is printed to formation graphene conductive skeleton on positive electrode substrate by printing technology；The graphene conductive skeleton by
Multiple unit groove body compositions being connected with each other；The positive electrode substrate for being formed with graphene conductive skeleton is placed in drying box dry；
Kynoar is dissolved using N-Methyl pyrrolidone, by positive electrode active materials and the Kynoar solution of dissolution according to quality
It is ground than being put into ball mill after 9:1 mixing, and is placed in drying in drying box after grinding, be prepared into positive electrode active materials slurry
Material；By the positive electrode active materials filled therewith in multiple unit groove bodies of the graphene conductive skeleton after, be placed in drying
It is dry in case, it is prepared into the positive plate of lithium battery with graphene conductive skeleton.
It is proposed a kind of lithium battery preparation method with graphene conductive skeleton, comprising: using above-mentioned band graphene conductive
The lithium battery anode piece preparation method of skeleton prepares positive plate of lithium battery；Micro powder graphites and CMC aqueous solution more than 300 mesh is mixed
It closes, after vacuum stirring to graphite solid content is 60%, is stirred evenly with 300 turns of revolving speeds hourly；With butadiene-styrene rubber and CMC
Mass ratio is that 1%-1.5% addition butadiene-styrene rubber stirs evenly, and obtains the slurries of cathode of lithium battery active material；By the lithium battery
The slurries of negative electrode active material are coated on cathode matrix and lithium battery cathode plate are made；Using polypropylene screen as diaphragm, with carbonic acid second
Enester and dimethyl carbonate solution are electrolyte, and the lithium electricity is assembled in the glove box that water and oxygen content are respectively less than 0.5ppm
Pond positive plate and the lithium battery cathode plate, are prepared into the lithium battery with graphene conductive skeleton.
Compared with prior art, the advantages of the application and good effect is: the band graphene conductive skeleton that the application proposes
Positive plate of lithium battery, in lithium battery and preparation method, on the positive electrode substrate of lithium battery, graphite is constituted using 3D printing technique
Alkene conducting matrix grain, the positive electrode active materials of the interior filling such as LiFePO4 of skeleton, the conducting matrix grain with graphene can be mentioned effectively
Electronic conductivity and lithium ion diffusion rate in high positive electrode active materials solve existing using LiFePO4 as positive electrode
The low technical problem low with diffusion rate of lithium ion battery electronic conduction rate, can be improved lithium battery volume and capacity ratio and energy
Density, and then charging rate is improved, improve the high rate performance and cycle performance of lithium battery.
After the detailed description of the application embodiment is read in conjunction with the figure, other features and advantages of the application will become more
Add clear.
Detailed description of the invention
Fig. 1 is the structure chart for the positive plate of lithium battery with graphene conductive skeleton that the application proposes；
Fig. 2 is the structure chart for the positive plate of lithium battery with graphene conductive skeleton that the application proposes；
Fig. 3 is the flow chart for the lithium battery anode piece preparation method with graphene conductive skeleton that the application proposes.
Specific embodiment
The specific embodiment of the application is described in more detail with reference to the accompanying drawing.
The positive plate of lithium battery with graphene conductive skeleton that the application proposes, as depicted in figs. 1 and 2, including positive base
Plate 101, graphene conductive skeleton 102 and positive electrode active materials 103；Graphene conductive skeleton 102 is by multiple lists being connected with each other
First groove body 1021 forms；Graphene conductive skeleton 102 is printed on positive electrode substrate 101 with 3D printing technique；Multiple unit groove bodies
Positive electrode active materials 103 are filled in 1021.
It is mixed that the 3D printing material of graphene conductive skeleton 102 is that graphene and Kynoar 9:1 in mass ratio are mixed
Condensation material；Kynoar (PVDF) is adhesive, plays the role of that printed material is enable to be bonded on positive electrode substrate.
During 3D printing, 3D printing height is controlled in 0.05mm- multiple unit groove bodies of graphene conductive skeleton
0.1mm, wall thickness control is in 0.03mm-0.05mm；The cross-sectional area control of each unit groove body 1021 is on the left side 500mm*350mm
It is right；The positive electrode substrate of printed graphene conductive skeleton is placed in 65 DEG C of drying boxes dry four hours.
Each unit groove body 1021 can be any regular or irregular shape.
Positive electrode active materials are adopted as LiFePO4 or cobalt acid lithium, LiMn2O4, nickel-cobalt-manganese ternary material, add N- methyl pyrrole
After pyrrolidone (NMP, the solvent of binder) dissolves Kynoar, by above-mentioned positive electrode active materials and Kynoar solution
It is mixed according to mass ratio 9:1, the uniform and dry printing slurry for being prepared into 3D printing is ground after mixing.
The preparation method of the specific positive plate of lithium battery set forth above with graphene conductive skeleton, as shown in figure 3, including
Following steps:
Step S31: graphene is put into ball mill grinding after mixing with Kynoar (PVDF) 9:1 in mass ratio, and
Addition N-Methyl pyrrolidone (NMP, the solvent of binder) is adjusted to printing slurry after the completion of grinding.
Step S32: to print slurry as raw material, printing slurry is printed to using 3D printing technique and is formed on positive electrode substrate
Graphene conductive skeleton.
Graphene conductive skeleton is made of multiple unit groove bodies being connected with each other；3D printing technique uses electronic microinjection 3D
Printing technology.
Step S33: the positive electrode substrate for being formed with graphene conductive skeleton is placed in drying box dry.
The positive electrode substrate for being formed with graphene conductive skeleton is placed in 65 DEG C of drying boxes dry four hours.
Step S34: Kynoar is dissolved using N-Methyl pyrrolidone, by the poly- inclined fluorine of positive electrode active materials and dissolution
Vinyl solution is put into ball mill after mixing according to mass ratio 9:1 and grinds, and dry in drying box, system is uniformly placed in grinding
For at positive electrode active materials slurry.
80 DEG C of drying temperature, drying time four hours.Positive electrode active materials are LiFePO4 or cobalt acid lithium, LiMn2O4, nickel
Cobalt-manganese ternary material.
Step S35: by positive electrode active materials filled therewith in multiple unit groove bodies of graphene conductive skeleton after, be placed in
It is dry in drying box, it is prepared into the positive plate of lithium battery with graphene conductive skeleton.
When by positive electrode active materials filled therewith in multiple unit groove bodies of graphene conductive skeleton, using small rotary
Positive electrode active materials slurries are compacted by tablet press machine, then by the positive plate of lithium battery with graphene conductive skeleton be placed in 100 DEG C-
It is four hours dry in 110 DEG C of drying property.
In positive plate of lithium battery with graphene conductive skeleton set forth above and preparation method, in the positive base of lithium battery
On plate, graphene conductive skeleton is constituted using 3D printing technique, the positive electrode active materials of filling such as LiFePO4, band in skeleton
Graphene conductive skeleton can effectively improve electronic conductivity and lithium ion diffusion rate in positive electrode active materials, solve existing
Some is using LiFePO4 as the low technical problem low with diffusion rate of lithium ion battery electronic conduction rate of positive electrode, Neng Gouti
High lithium battery volume and capacity ratio and energy density, and then charging rate is improved, improve the high rate performance and cyclicity of lithium battery
Energy.
Based on the positive plate of lithium battery and preparation method set forth above with graphene conductive skeleton, the application also proposes one
Lithium battery of the kind with graphene conductive skeleton, the lithium battery include positive plate and negative electrode tab, and wherein positive plate is set forth above
Positive plate of lithium battery with graphene conductive skeleton.
The preparation method of the lithium battery with graphene conductive skeleton, includes the following steps:
Step S41: using the lithium battery anode piece preparation method with graphene conductive skeleton of step S31 to step S35
Prepare positive plate of lithium battery.
More than step S42:300 mesh micro powder graphite and the mixing of CMC aqueous solution, being stirred under vacuum to graphite solid content is 60%
Afterwards, it is stirred evenly with 300 turns of revolving speeds hourly；It is that 1%-1.5% addition butadiene-styrene rubber stirs with the mass ratio of butadiene-styrene rubber and CMC
It mixes uniformly, obtains the slurries of cathode of lithium battery active material.
Micro powder graphite and CMC(sanlose) after aqueous solution mixing, the original solids content of graphite is on 70% left side
The right side, de-airing mixer are stirred with the speed of 50 turns/hour, and gradually plus water, reach graphite solid content 60%, be changed to 300 turns/it is small
When stir evenly, finally plus butadiene-styrene rubber (SBR), the mass ratio of SBR and CMC are 1%-1.5%, are stirred with the speed of 50 turns/hour
It mixes uniformly.
Step S43: the slurries of cathode of lithium battery active material are coated on cathode matrix, lithium battery cathode plate is made.
Cathode of lithium battery active material is coated on cathode matrix using small size coating machine, and is done in 80 DEG C of drying box
Lithium battery cathode plate is made within dry four hours.
Step S44: using polypropylene screen as diaphragm, using ethylene carbonate and dimethyl carbonate solution as electrolyte, in water and
Oxygen content, which is respectively less than in the glove box of 0.5ppm, assembles positive plate of lithium battery and lithium battery cathode plate, is prepared into band graphene and leads
The lithium battery of electric skeleton.
Polypropylene screen uses Cellgard-2400 type, with the ethylene carbonate (EC) and carbonic acid diformazan of 1mol/L LiPF6
Ester (DMC) (volume ratio 1:1) solution is electrolyte, and lithium electricity is assembled in the glove box that water and oxygen content are respectively less than 0.5ppm
Pond positive plate and lithium battery cathode plate are prepared into the lithium battery with graphene conductive skeleton, such as CR2032 type button half-cell.
Cyclic voltammetry is carried out using CHI 660E type electrochemical workstation, its perseverance is tested using BTS-3000 tester
Current charge-discharge performance.The voltage range of cyclic voltammetry is 0.01-3 V, and sweep speed is 0.1 mV s-1；Constant current charge and discharge
The voltage range of electrical testing is 0.01-3 V, and current density is 50 mA g-1；It is tested under 200 mA g-1 current densities to follow
Ring stability；Its high rate performance is tested in the case where current density is respectively 100,200,300,500 and 1000 mA g-1.
It should be noted that the above description is not a limitation of the present invention, the present invention is also not limited to the example above,
The variations, modifications, additions or substitutions that those skilled in the art are made within the essential scope of the present invention, are also answered
It belongs to the scope of protection of the present invention.
Claims (8)
1. the positive plate of lithium battery with graphene conductive skeleton, which is characterized in that including positive electrode substrate, graphene conductive skeleton and
Positive electrode active materials；The graphene conductive skeleton is made of multiple unit groove bodies being connected with each other；
The graphene conductive skeleton is printed on the positive electrode substrate with 3D printing technique；Filling in the multiple unit groove body
The positive electrode active materials.
2. the positive plate of lithium battery according to claim 1 with graphene conductive skeleton, which is characterized in that the graphene
The 3D printing material of conducting matrix grain is the mixing material that graphene and Kynoar 9:1 in mass ratio are mixed.
3. the positive plate of lithium battery according to claim 1 with graphene conductive skeleton, which is characterized in that the graphene
The 3D printing height of conducting matrix grain is 0.05mm-0.1mm, and the wall thickness of the graphene conductive skeleton is 0.03mm-0.05mm.
4. the positive plate of lithium battery according to claim 1 with graphene conductive skeleton, which is characterized in that the unit groove
The cross-sectional area of body is 500mm*350mm.
5. the positive plate of lithium battery according to claim 1 with graphene conductive skeleton, which is characterized in that the anode is living
Property material be LiFePO4 or cobalt acid lithium, LiMn2O4, nickel-cobalt-manganese ternary material.
6. the lithium battery with graphene conductive skeleton, which is characterized in that including as described in any one of claim 1-5 claim
The positive plate of lithium battery with graphene conductive skeleton.
7. the lithium battery anode piece preparation method with graphene conductive skeleton, is used to prepare such as any one of claim 1-5 right
It is required that the positive plate of lithium battery with graphene conductive skeleton characterized by comprising
Graphene is put into ball mill grinding after mixing with Kynoar 9:1 in mass ratio, and N- first is added after the completion of grinding
Base pyrrolidones is adjusted to printing slurry；
Using the printing slurry as raw material, the printing slurry is printed to using 3D printing technique and forms graphite on positive electrode substrate
Alkene conducting matrix grain；The graphene conductive skeleton is made of multiple unit groove bodies being connected with each other；
The positive electrode substrate for being formed with graphene conductive skeleton is placed in drying box dry；
Dissolve Kynoar using N-Methyl pyrrolidone, by positive electrode active materials and the Kynoar solution of dissolution according to
It is put into ball mill and grinds after mass ratio 9:1 mixing, and be placed in drying in drying box after grinding, be prepared into positive electrode active materials
Slurry；
By the positive electrode active materials filled therewith in multiple unit groove bodies of the graphene conductive skeleton after, be placed in drying
It is dry in case, it is prepared into the positive plate of lithium battery with graphene conductive skeleton.
8. the lithium battery preparation method with graphene conductive skeleton characterized by comprising
Lithium battery anode is prepared using the lithium battery anode piece preparation method as claimed in claim 7 with graphene conductive skeleton
Piece；
More than 300 mesh micro powder graphite and the mixing of CMC aqueous solution, it is every with 300 turns after vacuum stirring to graphite solid content is 60%
The revolving speed of hour stirs evenly；It is that 1%-1.5% addition butadiene-styrene rubber stirs evenly with the mass ratio of butadiene-styrene rubber and CMC, obtains
The slurries of cathode of lithium battery active material；
The slurries of the cathode of lithium battery active material are coated on cathode matrix, lithium battery cathode plate is made；
It is small in water and oxygen content using ethylene carbonate and dimethyl carbonate solution as electrolyte using polypropylene screen as diaphragm
The positive plate of lithium battery and the lithium battery cathode plate are assembled in the glove box of 0.5ppm, are prepared into band graphene conductive bone
The lithium battery of frame.
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| CN110635109B (en) * | 2019-07-29 | 2021-07-16 | 北京航空航天大学 | Lithium metal electrode prepared by 3D printing technology and preparation method thereof |
| CN113895051A (en) * | 2021-10-08 | 2022-01-07 | 北京化工大学 | Preparation method of high-load-bearing polymer functional composite material based on 3D printing technology |
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| CN105609328A (en) * | 2015-09-06 | 2016-05-25 | 广东风华高新科技股份有限公司 | Preparation method of electrode slice |
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