CN113659144A - Graphene-based composite conductive agent, and preparation method and application thereof - Google Patents
Graphene-based composite conductive agent, and preparation method and application thereof Download PDFInfo
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- CN113659144A CN113659144A CN202110908645.5A CN202110908645A CN113659144A CN 113659144 A CN113659144 A CN 113659144A CN 202110908645 A CN202110908645 A CN 202110908645A CN 113659144 A CN113659144 A CN 113659144A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 89
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 81
- 239000002131 composite material Substances 0.000 title claims abstract description 51
- 239000006258 conductive agent Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000002002 slurry Substances 0.000 claims abstract description 32
- 239000002270 dispersing agent Substances 0.000 claims abstract description 25
- 238000003756 stirring Methods 0.000 claims abstract description 25
- 239000000843 powder Substances 0.000 claims abstract description 19
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000002904 solvent Substances 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 4
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims description 13
- 229910001416 lithium ion Inorganic materials 0.000 claims description 13
- 239000006229 carbon black Substances 0.000 claims description 9
- 239000002356 single layer Substances 0.000 claims description 9
- 239000002135 nanosheet Substances 0.000 claims description 7
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 7
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 7
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 7
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical group CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 6
- 229910009819 Ti3C2 Inorganic materials 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 239000006230 acetylene black Substances 0.000 claims description 4
- 238000009826 distribution Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 239000003273 ketjen black Substances 0.000 claims description 3
- 239000010410 layer Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 2
- 239000011149 active material Substances 0.000 description 6
- 239000007787 solid Substances 0.000 description 5
- 238000013329 compounding Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000002041 carbon nanotube Substances 0.000 description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 229910003481 amorphous carbon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000003446 memory effect Effects 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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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
-
- 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
-
- 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 relates to the field of conductive agents, in particular to a preparation method of a graphene-based composite conductive agent, which comprises the following steps: a. adding a certain mass of dispersant into a solvent, and uniformly mixing to obtain a dispersant solution; b. adding a certain mass of graphene powder into a dispersant solution, and stirring under an ultrasonic condition to obtain graphene slurry; c. adding MXenes powder with a certain mass into the graphene slurry, and stirring under an ultrasonic condition to obtain graphene/MXenes composite slurry; d. adding a certain mass of conductive carbon black powder into the graphene/MXenes composite slurry, stirring under an ultrasonic condition to obtain the graphene/MXenes/conductive carbon black composite slurry, and finally vibrating and separating by using a screen to obtain the graphene-based composite conductive agent. The invention provides a graphene-based composite conductive agent, which effectively reduces the internal resistance of a battery and improves the high-rate performance of the battery. The invention also provides a preparation method of the graphene-based composite conductive agent, which is simple and convenient in process.
Description
Technical Field
The invention relates to the field of conductive agents, in particular to a graphene-based composite conductive agent, and a preparation method and application thereof.
Background
The lithium ion battery has the characteristics of low cost, environmental friendliness, high specific energy, no memory effect, light weight, excellent safety performance, long service life and the like, is more and more widely applied to the fields of micro electronic device equipment, power energy equipment and large-scale energy storage equipment, and meets greater challenges due to diversified development of the application field. However, in the application research of the existing lithium ion battery for energy storage, it is found that the performance of the active material can be effectively improved by modulating the conductive agent, such as: enhance the conductivity among the active materials, improve the high and low temperature performance, improve the high rate performance and the like.
The current commonly used lithium ion battery conductive agents comprise carbon black, conductive graphite, carbon fiber, carbon nanotube, graphene and mixed conductive slurry thereof. The carbon black is composed of chain or grape-shaped amorphous carbon particles, is in point contact with the active material, and has the function of preserving electrolyte; due to the unique flaky two-dimensional structure, the graphene is in point-surface contact with the active material; the two-dimensional transition metal carbon/nitride MXenes can be directly used as an electrode material as a graphene-like two-dimensional flaky material, and can still be completely dispersed in deionized water and N-methylpyrrolidone without a dispersant. Recent researches show that the performance indexes of the lithium ion battery can not be effectively improved by using the conductive agent alone, the use of the carbon black, the carbon nano tube and the graphene in a mixed manner is still a technical problem for improving the use amount and the solid content of the dispersant, and if the carbon black, the MXenes and the graphene are mixed and used according to different proportions, the use amount of the dispersant can be reduced, the solid content can be improved, the synergistic effect among different materials can be exerted, the advantages are complementary, and the performance indexes of the lithium ion battery can be further improved.
Disclosure of Invention
In order to solve the technical problems, the invention provides the graphene-based composite conductive agent, which effectively reduces the internal resistance of the battery and improves the high-rate performance of the battery.
The invention also provides a preparation method of the graphene-based composite conductive agent, which is simple and convenient in process.
The invention adopts the following technical scheme:
a preparation method of a graphene-based composite conductive agent comprises the following steps:
a. adding a certain mass of dispersant into a solvent, and uniformly mixing to obtain a dispersant solution;
b. adding a certain mass of graphene powder into a dispersant solution, and stirring under an ultrasonic condition to obtain graphene slurry;
c. adding MXenes powder with a certain mass into the graphene slurry, and stirring under an ultrasonic condition to obtain graphene/MXenes composite slurry;
d. adding a certain mass of conductive carbon black powder into the graphene/MXenes composite slurry, stirring under an ultrasonic condition to obtain the graphene/MXenes/conductive carbon black composite slurry, and finally vibrating and separating by using a screen to obtain the graphene-based composite conductive agent.
The technical scheme is further improved in the steps b, c and d, wherein the power of the ultrasonic wave is 2-4 KW, the linear speed of stirring is 10-15 m/s, and the stirring time is 2-4 hours.
In the step d, the screen is an electric screen.
The technical scheme is further improved in that the mass ratio of the graphene to the MXenes to the conductive carbon black to the dispersing agent to the solvent is 1-10:1-5:1-5:1-10: 80-95.
The technical scheme is further improved in that the number of layers of the graphene is 1-10, and the particle size distribution is 10-20 microns.
The technical proposal is further improved in that MXenes is single-layer Ti3C2TxNanosheet, single layer of Ti2CTxNanosheet, monolayer V2CTxOne or more than one of the nano sheets are mixed, and the particle size distribution of the Mxenes is 1-2 microns.
The technical proposal is further improved in that the conductive carbon black is one or a mixture of acetylene black, superconducting carbon black and Ketjen black.
The technical proposal is further improved in that the dispersant is one or a mixture of polyvinylpyrrolidone and modified polyvinylpyrrolidone; the solvent is N-methyl pyrrolidone.
The graphene-based composite conductive agent is prepared by the preparation method.
The application of the graphene-based composite conductive agent is applied to a lithium ion battery.
The invention has the beneficial effects that:
according to the graphene-based composite conductive agent, graphene is used as a main body, MXenes and conductive carbon black are introduced in a certain proportion, the using amount of a dispersing agent is reduced, the solid content is improved, the formed graphene-based composite conductive agent can realize rapid transmission of electrons in the plane and between layers, the internal resistance of a battery is effectively reduced, and the high-rate performance of the battery is improved.
Drawings
Fig. 1 is a graph illustrating a rate capability test performed on the graphene-based composite conductive paste prepared in example 3 of the present invention.
Detailed Description
The present invention will be further described with reference to the following examples for better understanding of the present invention, but the embodiments of the present invention are not limited thereto.
Example 1
Adding 20g of polyvinylpyrrolidone into 2Kg of N-methyl pyrrolidone solvent, and stirring at a linear speed of 3m/s for 1h to obtain a dispersant solution;
adding 50g of graphene powder into the dispersant solution obtained in the step (1), stirring for 3 hours at a linear speed of 10m/s with an ultrasonic power of 3KW to obtain graphene slurry;
20g of monolayer V2CTxAdding the powder into the graphene slurry obtained in the step (2), stirring for 30min at a linear speed of 12m/s with an ultrasonic power of 3KW to obtain graphene/V2CTxCompounding the slurry;
adding 30g of superconducting carbon black powder into the graphene/V obtained in the step (3)2CTxIn the composite slurry, stirring for 1h at a linear speed of 15m/s with ultrasonic power of 4KW to obtain graphene/V2CTxAnd finally, vibrating and separating the superconducting carbon black composite slurry by using a screen to obtain the graphene-based composite conductive agent.
Example 2
Adding 40g of polyvinylpyrrolidone into 3Kg of N-methyl pyrrolidone solvent, and stirring at a linear speed of 3m/s for 1h to obtain a dispersant solution;
adding 120g of graphene powder into the dispersant solution obtained in the step (1), and stirring for 3 hours at a linear speed of 12m/s with an ultrasonic power of 3KW to obtain graphene slurry;
50g of a single layer of Ti2CTxAdding the powder into the graphene slurry obtained in the step (2), stirring for 30min at a linear speed of 15m/s with an ultrasonic power of 3KW to obtain graphene/Ti2CTxCompounding the slurry;
adding 50g of acetylene black powder into the graphene/Ti powder obtained in the step (3)2CTxIn the composite slurry, stirring for 2 hours at a linear speed of 15m/s with ultrasonic power of 4KW to obtain graphene/Ti2CTxAnd finally, vibrating and separating the acetylene black composite slurry by using a screen to obtain the graphene-based composite conductive agent.
Example 3
Adding 50g of polyvinylpyrrolidone into 4Kg of N-methyl pyrrolidone solvent, and stirring at a linear speed of 3m/s for 1h to obtain a dispersant solution;
adding 200g of graphene powder into the dispersant solution obtained in the step (1), stirring for 3 hours at a linear speed of 10m/s with an ultrasonic power of 3KW to obtain graphene slurry;
120g of a single layer of Ti3C2TxAdding the powder into the graphene slurry obtained in the step (2), stirring for 30min at a linear speed of 13m/s with an ultrasonic power of 4KW to obtain graphene/Ti3C2TxCompounding the slurry;
adding 80g Keqin black powder into the graphene/Ti obtained in the step (3)3C2TxIn the composite slurry, stirring for 2 hours at a linear speed of 15m/s with ultrasonic power of 4KW to obtain graphene/Ti3C2TxAnd finally, vibrating and separating the Ketjen black composite slurry by using a screen to obtain the graphene-based composite conductive agent.
The invention also provides a lithium ion battery, wherein the conductive agent in the lithium ion battery is the graphene-based composite conductive agent in the invention, other components of the lithium ion battery are all common lithium ion battery materials, and meanwhile, the battery serving as a comparison group is a common commercial lithium ion battery, which is not described again.
The results of the rate performance test performed on the graphene-based composite conductive paste prepared in example 3 are shown in fig. 1.
As can be seen from fig. 1, compared with the comparative group, the performance of the graphene-based composite conductive agent is significantly improved during high-rate charge and discharge.
The invention provides a solution for the problem of improvement of the using amount and solid content of the dispersing agent in the graphene composite conductive agent, introduces the excellent conductive material MXenes capable of self-dispersing in the solvent, can effectively reduce the using amount of the dispersing agent, improves the solid content of the slurry, can effectively enhance the conductivity between active materials by adding the MXenes and the carbon black, can accelerate the rapid transfer of ions and electrons on the surface of the active material by adding the small-size MXenes nanosheets, and improves the high-rate charge-discharge performance of the lithium ion battery. +
Appropriate changes and modifications to the embodiments described above will become apparent to those skilled in the art from the disclosure and teachings of the foregoing description. Therefore, the present invention is not limited to the specific embodiments disclosed and described above, and some modifications and variations of the present invention should fall within the scope of the claims of the present invention. Furthermore, although specific terms are employed herein, they are used in a generic and descriptive sense only and not for purposes of limitation.
Claims (10)
1. A preparation method of a graphene-based composite conductive agent is characterized by comprising the following steps:
a. adding a certain mass of dispersant into a solvent, and uniformly mixing to obtain a dispersant solution;
b. adding a certain mass of graphene powder into a dispersant solution, and stirring under an ultrasonic condition to obtain graphene slurry;
c. adding MXenes powder with a certain mass into the graphene slurry, and stirring under an ultrasonic condition to obtain graphene/MXenes composite slurry;
d. adding a certain mass of conductive carbon black powder into the graphene/MXenes composite slurry, stirring under an ultrasonic condition to obtain the graphene/MXenes/conductive carbon black composite slurry, and finally vibrating and separating by using a screen to obtain the graphene-based composite conductive agent.
2. The preparation method of the graphene-based composite conductive agent according to claim 1, wherein in the steps b, c and d, the ultrasonic power is 2-4 KW, the linear speed of stirring is 10-15 m/s, and the stirring time is 2-4 hours.
3. The method of preparing the graphene-based composite conductive agent according to claim 1, wherein in the step d, the mesh is an electric mesh.
4. The preparation method of the graphene-based composite conductive agent according to claim 1, wherein the mass ratio of the graphene, the MXenes, the conductive carbon black, the dispersing agent and the solvent is 1-10:1-5:1-5:1-10: 80-95.
5. The preparation method of the graphene-based composite conductive agent according to claim 1, wherein the number of graphene layers is 1-10, and the particle size distribution is 10-20 μm.
6. The method for preparing the graphene-based composite conductive agent according to claim 1, wherein the MXenes is a single layer of Ti3C2TxNanosheet, single layer of Ti2CTxNanosheet, monolayer V2CTxOne or more than one of the nano sheets are mixed, and the particle size distribution of the Mxenes is 1-2 microns.
7. The preparation method of the graphene-based composite conductive agent according to claim 1, wherein the conductive carbon black is one or a mixture of acetylene black, superconducting carbon black and ketjen black.
8. The preparation method of the graphene-based composite conductive agent according to claim 1, wherein the dispersant is one or a mixture of polyvinylpyrrolidone and modified polyvinylpyrrolidone; the solvent is N-methyl pyrrolidone.
9. A graphene-based composite conductive agent, characterized in that the graphene-based composite conductive agent is produced using the production method according to any one of claims 1 to 8.
10. The application of the graphene-based composite conductive agent is characterized in that the graphene-based composite conductive agent is applied to a lithium ion battery.
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