CN109244464A - A kind of graphene anode sizing agent and efficient controllable method for preparing - Google Patents
A kind of graphene anode sizing agent and efficient controllable method for preparing Download PDFInfo
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- CN109244464A CN109244464A CN201811041862.3A CN201811041862A CN109244464A CN 109244464 A CN109244464 A CN 109244464A CN 201811041862 A CN201811041862 A CN 201811041862A CN 109244464 A CN109244464 A CN 109244464A
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- graphene
- sizing agent
- anode sizing
- dry powder
- slurry
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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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
-
- 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
- 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
-
- 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 is a kind of graphene anode sizing agent and efficient controllable method for preparing, the graphene anode sizing agent is the compound of positive electrode active materials, graphene and other conductive carbon materials, binder (PVDF), N-Methyl pyrrolidone (NMP), appropriate positive electrode active materials dry powder, PVDF dry powder is added into double-planet stirring dispersion machine first, stirs certain time slowly；Then amount of conductive slurry is added portionwise and stirs, disperse, soaked, mediated, wet mixing；It is eventually adding appropriate nmp solvent and adjusts slurry viscosity, stir dispersion fastly enough for a long time, obtain final slurry.Graphene dispersion in the graphene anode sizing agent is good, can form good covered effect to positive electrode active materials particle, can form high efficiency charge transmission network in the electrodes, can accelerate the diffusion velocity of electronics, reduces battery polarization, improves battery performance.The slurry viscosity controllability of the method for the present invention is high, has better stability and rheological behavior.
Description
Technical field
The present invention is a kind of graphene anode sizing agent and high efficiency controllable method for preparing, belongs to cell manufacturing techniques field.
Background technique
Graphene is a kind of New Two Dimensional nano material, and electric conductivity with super strength is the best material of current electric conductivity
Material.There is the electron mobility (200000cm of superelevation simultaneously2/ V.S), thermal conductivity (5000W/m.K).It is excellent using graphene
The modified positive electrode active materials of electric conductivity, the specific surface area of super large, unique two-dimensional network structure, will greatly improve the conduction of material
Performance, can effectively shorten the transmission path of electronics in battery charge and discharge process, the transmission speed both accelerated.This is for improving lithium
High rate performance, cycle life of battery etc. are of great significance.Using graphene as main raw material(s), the conductive paste of dispersed is made
Material is added in the form of conductive auxiliary agent in lithium battery anode slurry technique, is current realization graphene engineering on lithium battery
Change the important means of application.
Slurry technique is greater than 30% to the qualitative effects degree of product in the entire production technology of lithium ion battery, is entire electricity
Most important link in the production technology of pond.However, graphene is difficult to high by domestic Battery Plant as novel lithium battery conductive auxiliary agent
Effect even effectively application.Its conventional positive slurry technique is difficult to ensure graphene fine dispersion, causes stacking, the group of graphene
It is poly-, it is difficult to form effective charge transmission network, or even can also hinder the transmission of lithium ion, cause serious polarization.Mesh simultaneously
The preceding positive slurry process time is too long, inefficiency, and poor controllability, finally formed stock quality be not high.These are all
Strongly limit the raising of battery manufacture level and the promotion of Business Economic Benefit.
Summary of the invention
It is an object of the invention to the deficiency of defect and positive slurry technique for positive electrode current active material ontology
Design provides a kind of graphene anode sizing agent and efficient controllable method for preparing, and the preparation method is not change existing Battery Plant mixed
Under the premise of starching equipment, using the unique two-dimensional structure of graphene and excellent electric conductivity, modified current positive electrode active materials,
Improve high rate performance, the cycle life etc. of lithium electricity positive electrode.Slurry efficiency and anode sizing agent quality are improved simultaneously, shorten battery
Manufacturing cycle, it is horizontal to improve battery manufacture.
To achieve the above object, the invention adopts the following technical scheme:
The step of this kind of graphene anode sizing agent and efficient controllable method for preparing, is as follows:
Step 1: positive electrode active materials dry powder and PVDF dry powder is added, into double-planet stirring dispersion machine with 5~20r/
The speed of min is stirred, and the time is 10min or more；
The positive electrode active materials dry powder accounts for 95%~99%, the PVDF dry powder of solid gross mass in graphene anode sizing agent
Account for 0.5%~3% of solid gross mass in graphene anode sizing agent；
Step 2: graphene composite conductive slurry is added, solid content in mixture is made to be reached for 85%~95%, with 5~
The speed stirring of 20r/min carries out wettability treatment, and the time is 10min or more；
Step 3: graphene composite conductive slurry is added, solid content in mixture is made to reach 75%~85%, with 5~
With the Rate Dispersion of 100~500r/min while the speed stirring of 20r/min, carry out kneading processing, the time be 10min with
On；
Step 4: graphene composite conductive slurry is added, account for the conductive dry powder in mixture in graphene anode sizing agent
The 0.3%~3% of solid gross mass, conductive dry powder is in graphene composite conductive slurry, with the speed of 20~30r/min
With the Rate Dispersion of 1000~3000r/min while stirring, the time is 1h or more；
Step 5: nmp solvent, which is added, adjusts slurry viscosity to 5000~8000mPa.s, with the side of being dispersed with stirring of step 4
Formula carries out 30min or more, obtains graphene anode sizing agent.
Further, positive electrode active materials are LiFePO4, ternary material, LiMn2O4, cobalt acid lithium or lithium-rich manganese base material.
Further, graphene film diameter is having a size of 1 μm~30 μm in conductive dry powder, other conductive carbon materials are in conductive dry powder
The mixture of one or more of carbon black, carbon nanotube, carbon fiber.
Further, the solvent of graphene composite conductive slurry is NMP.
Technical solution of the present invention during slurry, graphene in the form of the dispersed composite conducting slurry rather than dry powder
Form is added；Technical solution of the present invention use dry method slurry form, it is dry-mixed to positive electrode active materials, PVDF first, after gradually plus
The feeding sequence of graphene composite conductive slurry wet mixing.
Compared with prior art, the beneficial effect comprise that
Firstly, breaching the technical bottleneck of graphene difficulty dispersion, the side of graphene composite conductive slurry is added by substep
Formula and be suitably dispersed with stirring technological parameter, keep graphene well compound with positive electrode active materials, and with other conductive carbon materials
Cooperatively form high efficiency charge transmission network；
Secondly, the technique uses dry pigmentation slurrying, using the mixing method of first dry-mixed rear solubilizer, more conventional slurry work
Skill, flexibly, slurry viscosity is controllable for solid content control, and final anode sizing agent is made to have better sedimentation stability and rheological behavior；
Again, the charging sequence of the rational technology and it is suitably dispersed with stirring technological parameter, slurry viscosity is made to reach stable
State for time is shorter, compared with traditional slurry technique, substantially reduces the mixing procedure time, improves the manufacture efficiency of battery,
Improve the economic benefit of Battery Plant.
Preparation method through the invention realizes the good compound of graphene and positive electrode active materials particle, readily available
The anode sizing agent that rheological behavior is good, stability is high, while the slurry process time is shortened, improve battery manufacture efficiency.This work
Skill is simple, and does not influence the industrialization technology of the production of positive electrode current material and battery manufacture, is conducive to engineering application.
Specific embodiment
Below with reference to embodiment, the following further describes the technical solution of the present invention.
Embodiment 1
Prepare LiFePO4The step of/graphene anode sizing agent, preparation process, is as follows:
Step 1: 5kg LiFePO4 dried powder, PVDF dried powder 100g are added into double-planet stirring dispersion machine,
It is stirred with the speed of 15r/min, time 30min；
Step 2: addition graphene composite conductive slurry 0.6kg (graphene composite conductive slurry solid content is 6%, wherein
Dispersing agent accounts for 1%, 5%) remaining conductive carbon material accounts for, and solid content in mixture is made to reach 90.1%, is stirred with the speed of 15r/min
Mix carry out wettability treatment, time 30min；
Step 3: addition graphene composite conductive slurry 0.8kg (graphene composite conductive slurry solid content is 6%, wherein
Dispersing agent accounts for 1%, 5%) remaining conductive carbon material accounts for, and solid content in mixture is made to reach 79.8%, is stirred with the speed of 15r/min
With the Rate Dispersion of 300r/min while mixing, kneading processing, time 60min are carried out；
Step 4: addition graphene composite conductive slurry 1.6kg (graphene composite conductive slurry solid content is 6%, wherein
Dispersing agent accounts for 1%, 5%) remaining conductive carbon material accounts for, and so that the conductive dry powder in mixture is accounted for solid in graphene anode sizing agent total
The 2.8% of quality, conductive dry powder in the graphene composite conductive slurry, with while the speed stirring of 30r/min with
The Rate Dispersion of 3000r/min, time 1h；
Step 5: nmp solvent, which is added, adjusts slurry viscosity to 5000~8000mPa.s, with the side of being dispersed with stirring of step 4
Formula carries out 30min, obtains graphene anode sizing agent.
Embodiment 2
Prepare LiNi0.5Co0.2Mn0.3O2The step of/graphene anode sizing agent, preparation process, is as follows:
Step 1: 5kg LiNi is added into double-planet stirring dispersion machine0.5Co0.2Mn0.3O2Dried powder, PVDF are dry
Powder 100g is stirred with the speed of 15r/min, time 30min；
Step 2: addition graphene composite conductive slurry 0.6kg (graphene composite conductive slurry solid content is 6%, wherein
Dispersing agent accounts for 1%, 5%) remaining conductive carbon material accounts for, and solid content in mixture is made to reach 90.1%, is stirred with the speed of 15r/min
Mix carry out wettability treatment, time 30min；
Step 3: addition graphene composite conductive slurry 0.8kg (graphene composite conductive slurry solid content is 6%, wherein
Dispersing agent accounts for 1%, 5%) remaining conductive carbon material accounts for, and solid content in mixture is made to reach 79.8%, is stirred with the speed of 15r/min
With the Rate Dispersion of 300r/min while mixing, kneading processing, time 60min are carried out；
Step 4: addition graphene composite conductive slurry 1.6kg (graphene composite conductive slurry solid content is 6%, wherein
Dispersing agent accounts for 1%, 5%) remaining conductive carbon material accounts for, and so that the conductive dry powder in mixture is accounted for solid in graphene anode sizing agent total
The 2.8% of quality, conductive dry powder in the graphene composite conductive slurry, with while the speed stirring of 30r/min with
The Rate Dispersion of 3000r/min, time 1h；
Step 5: nmp solvent, which is added, adjusts slurry viscosity to 5000~8000mPa.s, with the side of being dispersed with stirring of step 4
Formula carries out 30min, obtains graphene anode sizing agent.
Embodiment 3
Prepare LiNi0.8Co0.15Al0.05O2The step of/graphene anode sizing agent, preparation process, is as follows:
Step 1: 5kg LiNi is added into double-planet stirring dispersion machine0.8Co0.15Al0.05O2Dried powder, PVDF are dry
Powder 100g is stirred with the speed of 15r/min, time 30min；
Step 2: addition graphene composite conductive slurry 0.6kg (graphene composite conductive slurry solid content is 6%, wherein
Dispersing agent accounts for 1%, 5%) remaining conductive carbon material accounts for, and solid content in mixture is made to reach 90.1%, is stirred with the speed of 15r/min
Mix carry out wettability treatment, time 30min；
Step 3: addition graphene composite conductive slurry 0.8kg (graphene composite conductive slurry solid content is 6%, wherein
Dispersing agent accounts for 1%, 5%) remaining conductive carbon material accounts for, and solid content in mixture is made to reach 79.8%, is stirred with the speed of 15r/min
With the Rate Dispersion of 300r/min while mixing, kneading processing, time 60min are carried out；
Step 4: addition graphene composite conductive slurry 1.6kg (graphene composite conductive slurry solid content is 6%, wherein
Dispersing agent accounts for 1%, 5%) remaining conductive carbon material accounts for, and so that the conductive dry powder in mixture is accounted for solid in graphene anode sizing agent total
The 2.8% of quality, conductive dry powder in the graphene composite conductive slurry, with while the speed stirring of 30r/min with
The Rate Dispersion of 3000r/min, time 1h；
Step 5: nmp solvent, which is added, adjusts slurry viscosity to 5000~8000mPa.s, with the side of being dispersed with stirring of step 4
Formula carries out 30min, obtains graphene anode sizing agent.
The graphene anode sizing agent being prepared using process above method, graphene dispersion is good, finally formed
It can play one's part to the full in electrode, form high efficiency conductive network, reduce polarization, improve battery performance；Secondly, finally just
Pole slurry is with good stability and rheological behavior, and coating process is good, improves battery manufacture level；Entire mixing time
Shorten 50% or more, greatly improves battery manufacture efficiency, reduce manufacturing cost, improve Business Economic Benefit.
Claims (5)
1. a kind of graphene anode sizing agent and efficient controllable method for preparing, it is characterised in that: the step of preparation method is as follows:
Step 1: positive electrode active materials dry powder and PVDF dry powder is added, into double-planet stirring dispersion machine with 5~20r/min's
Speed is stirred, and the time is 10min or more；
95%~99%, the PVDF dry powder that the positive electrode active materials dry powder accounts for solid gross mass in graphene anode sizing agent accounts for stone
The 0.5%~3% of solid gross mass in black alkene anode sizing agent；
Step 2: graphene composite conductive slurry is added, solid content in mixture is set to reach 85%~95%, with 5~20r/min
Speed stirring carry out wettability treatment, the time be 10min or more；
Step 3: graphene composite conductive slurry is added, solid content in mixture is set to reach 75%~85%, with 5~20r/min
Speed stirring while with the Rate Dispersion of 100~500r/min, carry out kneading processing, the time is 10min or more；
Step 4: graphene composite conductive slurry is added, the conductive dry powder in mixture is made to account for solid in graphene anode sizing agent
The 0.3%~3% of gross mass, conductive dry powder are stirred in graphene composite conductive slurry with the speed of 20~30r/min
While with the Rate Dispersion of 1000~3000r/min, the time is 1h or more；
Step 5: nmp solvent, which is added, adjusts slurry viscosity to 5000~8000mPa.s, in a manner of being dispersed with stirring of step 4 into
Row 30min or more obtains graphene anode sizing agent.
2. graphene anode sizing agent according to claim 1 and efficient controllable method for preparing, it is characterised in that: positive-active
Material is LiFePO4, ternary material, LiMn2O4, cobalt acid lithium or lithium-rich manganese base material.
3. graphene anode sizing agent according to claim 1 and efficient controllable method for preparing, it is characterised in that: conductive dry powder
Middle graphene film diameter is having a size of 1 μm~30 μm, other conductive carbon materials are carbon black, carbon nanotube, in carbon fiber in conductive dry powder
One or more of mixtures.
4. graphene anode sizing agent according to claim 1 and efficient controllable method for preparing, it is characterised in that: graphene is multiple
The solvent for closing electrocondution slurry is NMP.
5. double-planet stirring dispersion machine according to claim 1, equipment designed capacity can meet dry pigmentation slurrying requirement.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110224121A (en) * | 2019-06-10 | 2019-09-10 | 合肥众禾动力新能源科技有限公司 | A kind of preparation method of anode sizing agent |
| CN110854386A (en) * | 2019-11-21 | 2020-02-28 | 骆驼集团武汉光谷研发中心有限公司 | Preparation method of positive electrode slurry of power type lithium battery, positive plate and lithium battery |
| CN112467128A (en) * | 2020-12-09 | 2021-03-09 | 山东精工电子科技有限公司 | Lithium battery lithium titanate slurry and preparation method thereof |
| CN112582577A (en) * | 2020-07-08 | 2021-03-30 | 骆驼集团新能源电池有限公司 | Lithium iron phosphate start-stop battery anode slurry dry-process homogenizing process and prepared slurry |
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