CN111628172A - Production process of graphene-based battery conductive agent - Google Patents
Production process of graphene-based battery conductive agent Download PDFInfo
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- CN111628172A CN111628172A CN202010395943.4A CN202010395943A CN111628172A CN 111628172 A CN111628172 A CN 111628172A CN 202010395943 A CN202010395943 A CN 202010395943A CN 111628172 A CN111628172 A CN 111628172A
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- graphene
- conductive agent
- based battery
- battery conductive
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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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- 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 production process of a graphene-based battery conductive agent, which comprises the steps of preparing a graphene material by a mechanical stripping method, carrying out secondary stripping on the graphene material by a chemical intercalation method, further improving the dispersibility and stability of the graphene material, and then preparing the conductive agent. According to the method, the graphene material is subjected to secondary chemical stripping treatment by using an intercalation method, so that the dispersion degree of graphene is improved, the surface contact effect of graphene sheet layers is better, and the graphene-based battery conductive agent prepared by the method is better in conductive performance and more stable in performance.
Description
Technical Field
The invention relates to the technical field of graphene materials, in particular to a production process of a graphene-based battery conductive agent.
Background
The lithium ion battery has the advantages of high and stable working voltage, large specific capacity, stable discharge, small volume, light weight, no memory effect, environmental friendliness and the like, and has wide application prospect in the fields of portable electronic equipment, electric automobiles, space technology, national defense industry and the like. With the rapid development of power lithium batteries, people have looked to materials such as manganese oxide, phosphate and the like which are rich in resources, environment-friendly and low in price from expensive cobalt oxide, but the conductivity of the materials is very low, and the materials also have good high-rate charge-discharge characteristics and long service life, so that the conductive agent serving as an important component of the lithium ion battery is required to play an important role in improving the performance of the battery.
The conductive agents used in the market at present are granular conductive agents, such as acetylene black, carbon black, artificial graphite, natural graphite and the like; fibrous conductive agents such as metal fibers, vapor grown carbon fibers, carbon nanotubes, and the like; flake conductive agents such as graphene and the like. The granular conductive agent is low in price and convenient to use, and is a conductive agent commonly used for the lithium ion battery at present; the fibrous conductive agent has a larger length-diameter ratio, which is beneficial to forming a conductive network and improving the bonding firmness between machine collectors among the active materials; the flaky conductive agent can fully utilize the excellent conductivity to improve the capacity of an electrode material, reduce the internal resistance of a battery and prolong the cycle life of the battery.
Since the graphene material is found to be a novel two-dimensional nanomaterial, more and more excellent properties of graphene, such as high strength, high conductivity, high sensing sensitivity, and the like, have been found. In the existing graphene manufacturing method, the graphene is prepared by a mechanical stripping method with high efficiency, but the graphene product has poor dispersibility, the lamella stripping is not thorough, the product is mostly multilayer graphite, good dispersion is not easy to form during the preparation of the conductive agent, the performance is not stable enough, and the conductive performance is greatly reduced.
Disclosure of Invention
The technical scheme adopted by the invention for solving the technical problems is as follows: a production process of a graphene-based battery conductive agent comprises the following steps:
(1) preparing a graphene material by a mechanical stripping method;
(2) adding a graphene material and an intercalation agent into a ball milling tank, carrying out ball milling treatment for 30-60 min to obtain a mixture precursor, and carrying out the ball milling treatment in inert gas;
(3) mixing the mixture precursor with an intercalation solvent, and carrying out ultrasonic treatment;
(4) sequentially adding polydopamine and a dispersing agent, uniformly stirring, and performing microwave treatment to obtain secondary stripping graphene mixture slurry;
(5) leaching and filtering the secondary stripping graphene mixture slurry by using deionized water to obtain a secondary stripping graphene slurry;
(6) freezing and drying the secondary stripping graphene slurry to obtain secondary stripping graphene;
(7) adding 1 part of binder into 20-200 parts of solvent according to parts by weight, and fully and uniformly stirring to obtain a binder mixed solution;
(8) and (2) fully stirring and mixing 100 parts of binder mixed liquor and 1-10 parts of secondary stripping graphene for 1-3 hours, continuously adding 0.5-5 parts of other conductive components, fully stirring and mixing for 0.5-2 hours, and carrying out ultrasonic treatment on the mixed slurry for 1-3 hours to obtain the graphene-based battery conductive agent.
In the production process of the graphene-based battery conductive agent, the intercalation agent is one of ammonium carbonate, ammonium oxalate or potassium carbonate.
In the production process of the graphene-based battery conductive agent, the intercalation solvent is one of N-methyl pyrrolidone, N-dimethylformamide, water, methanol, ethanol, ethylene glycol, acetone, butanone, tetrahydrofuran, toluene, xylene, dichlorotoluene or chloroform.
According to the production process of the graphene-based battery conductive agent, the mass ratio of the graphene material to the intercalation agent to the intercalation solvent to the polydopamine to the dispersing agent is 1:2:4:2: 1.
In the production process of the graphene-based battery conductive agent, the dispersing agent is one of sodium dodecyl benzene sulfonate, sodium dodecyl sulfate, cetyl trimethyl ammonium bromide or polyvinylpyrrolidone.
According to the production process of the graphene-based battery conductive agent, the ultrasonic treatment frequency is 20-40 kHz, and the power is 200-300W.
In the production process of the graphene-based battery conductive agent, the binder is one of polyvinylidene fluoride, polyacrylic acid, styrene butadiene rubber or polyvinyl alcohol.
In the production process of the graphene-based battery conductive agent, the solvent is one of N-methyl pyrrolidone or N, N-dimethylformamide.
In the production process of the graphene-based battery conductive agent, the other conductive component is one of conductive carbon black, acetylene black or carbon nanotubes.
The graphene-based battery conductive agent prepared by the method has better conductivity and more stable performance.
Detailed Description
In order to more clearly illustrate the technical solutions of the present invention, the present invention is further described below, and it is obvious that the following descriptions are only some embodiments of the present invention, and it is within the scope of the present invention for a person of ordinary skill in the art to obtain other embodiments based on these embodiments without any creative effort.
A production process of a graphene-based battery conductive agent comprises the following steps:
(1) preparing a graphene material by a mechanical stripping method;
(2) adding a graphene material and an intercalation agent into a ball milling tank, carrying out ball milling treatment for 60min to obtain a mixture precursor, and carrying out the ball milling treatment in inert gas;
(3) mixing the mixture precursor with an intercalation solvent, and carrying out ultrasonic treatment;
(4) sequentially adding polydopamine and a dispersing agent, uniformly stirring, and performing microwave treatment to obtain secondary stripping graphene mixture slurry;
(5) leaching and filtering the secondary stripping graphene mixture slurry by using deionized water to obtain a secondary stripping graphene slurry;
(6) freezing and drying the secondary stripping graphene slurry to obtain secondary stripping graphene;
(7) adding 1 part of binder into 150 parts of solvent according to parts by weight, and fully and uniformly stirring to obtain a binder mixed solution;
(8) and (2) fully stirring and mixing 100 parts of binder mixed liquor and 10 parts of secondary stripping graphene for 3 hours, continuously adding 5 parts of other conductive components, fully stirring and mixing for 2 hours, and carrying out ultrasonic treatment on the mixed slurry for 3 hours to obtain the graphene-based battery conductive agent.
In detail, the intercalation agent is ammonium carbonate, the intercalation solvent is methanol, and the mass ratio of the graphene material to the intercalation agent to the intercalation solvent to the polydopamine to the dispersant is 1:2:4:2: 1; the dispersing agent is sodium dodecyl benzene sulfonate, the ultrasonic treatment frequency in the step is 40kHz, and the power is 300W; the adhesive is polyvinylidene fluoride, the solvent is N, N-dimethylformamide, and the other conductive components are acetylene black.
The above embodiments are only exemplary embodiments of the present invention, and are not intended to limit the present invention, and the scope of the present invention is defined by the claims. Various modifications and equivalents may be made by those skilled in the art within the spirit and scope of the present invention, and such modifications and equivalents should also be considered as falling within the scope of the present invention.
Claims (9)
1. A production process of a graphene-based battery conductive agent is characterized by comprising the following steps:
(1) preparing a graphene material by a mechanical stripping method;
(2) adding a graphene material and an intercalation agent into a ball milling tank, carrying out ball milling treatment for 30-60 min to obtain a mixture precursor, and carrying out the ball milling treatment in inert gas;
(3) mixing the mixture precursor with an intercalation solvent, and carrying out ultrasonic treatment;
(4) sequentially adding polydopamine and a dispersing agent, uniformly stirring, and performing microwave treatment to obtain secondary stripping graphene mixture slurry;
(5) leaching and filtering the secondary stripping graphene mixture slurry by using deionized water to obtain a secondary stripping graphene slurry;
(6) freezing and drying the secondary stripping graphene slurry to obtain secondary stripping graphene;
(7) adding 1 part of binder into 20-200 parts of solvent according to parts by weight, and fully and uniformly stirring to obtain a binder mixed solution;
(8) and (2) fully stirring and mixing 100 parts of binder mixed liquor and 1-10 parts of secondary stripping graphene for 1-3 hours, continuously adding 0.5-5 parts of other conductive components, fully stirring and mixing for 0.5-2 hours, and carrying out ultrasonic treatment on the mixed slurry for 1-3 hours to obtain the graphene-based battery conductive agent.
2. The process of claim 1, wherein the intercalating agent is one of ammonium carbonate, ammonium oxalate or potassium carbonate.
3. The process of claim 1, wherein the intercalation solvent is one of N-methylpyrrolidone, N-dimethylformamide, water, methanol, ethanol, ethylene glycol, acetone, butanone, tetrahydrofuran, toluene, xylene, dichlorotoluene, or chloroform.
4. The production process of the graphene-based battery conductive agent according to claim 1, wherein the mass ratio of the graphene material, the intercalation agent, the intercalation solvent, the polydopamine and the dispersing agent is 1:2:4:2: 1.
5. The process for producing the graphene-based battery conductive agent according to claim 1, wherein the dispersant is one of sodium dodecylbenzene sulfonate, sodium dodecyl sulfate, cetyltrimethylammonium bromide or polyvinylpyrrolidone.
6. The production process of the graphene-based battery conductive agent according to claim 1, wherein the ultrasonic treatment frequency is 20-40 kHz, and the power is 200-300W.
7. The production process of the graphene-based battery conductive agent according to claim 1, wherein the binder is one of polyvinylidene fluoride, polyacrylic acid, styrene butadiene rubber or polyvinyl alcohol.
8. The process for producing the graphene-based battery conductive agent according to claim 1, wherein the solvent is one of N-methylpyrrolidone or N, N-dimethylformamide.
9. The process for producing the graphene-based battery conductive agent according to claim 1, wherein the other conductive component is one of conductive carbon black, acetylene black or carbon nanotubes.
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Citations (8)
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| CN108976618A (en) * | 2018-08-08 | 2018-12-11 | 南通迅达橡塑制造有限公司 | A kind of graphene modified EPT rubber composite material and preparation method thereof |
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| CN109095462A (en) * | 2018-07-26 | 2018-12-28 | 北京旭碳新材料科技有限公司 | A kind of graphene and its preparation method and application |
| CN109251733A (en) * | 2018-09-19 | 2019-01-22 | 北京沃杰知识产权有限公司 | A kind of graphene composite material heat conducting film and preparation method thereof |
| CN110759336A (en) * | 2019-11-11 | 2020-02-07 | 董影影 | Preparation method of graphene and graphene |
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-
2020
- 2020-05-12 CN CN202010395943.4A patent/CN111628172A/en active Pending
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Application publication date: 20200904 |