CN108492907B - Nano-metal modified graphene conductive material and preparation method thereof - Google Patents
Nano-metal modified graphene conductive material and preparation method thereof Download PDFInfo
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- CN108492907B CN108492907B CN201810251698.2A CN201810251698A CN108492907B CN 108492907 B CN108492907 B CN 108492907B CN 201810251698 A CN201810251698 A CN 201810251698A CN 108492907 B CN108492907 B CN 108492907B
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- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
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Abstract
The invention relates to a nano metal modified graphene conductive material and a preparation method thereof, wherein the preparation method comprises the following steps: mixing and dispersing graphene and a dispersing agent to obtain a graphene dispersion system; dissolving a metal salt in a solvent to obtain a metal salt solution; ultrasonically dispersing the metal salt solution and the graphene dispersion system, and adding a stabilizer to obtain a mixed solution; heating the mixed solution by microwave, filtering, cleaning and drying to obtain mixed powder; and sintering the mixed powder in an inert atmosphere, and crushing and ball-milling to obtain the nano metal modified graphene conductive material. According to the invention, the metal salt solution is reduced by a microwave reduction method, and the reduced nano metal particles are deposited at the contact position and the defect position of two adjacent graphene sheets, so that the contact resistance between the graphene sheets is reduced, and the conductivity of the graphene material is further enhanced.
Description
Technical Field
The invention relates to a graphene conductive material and a preparation method thereof, in particular to a nano-metal modified graphene conductive material and a preparation method thereof.
Background
Graphene is a material consisting of carbon atoms in sp2The honeycomb planar film formed by the hybridization mode is a quasi-two-dimensional material with the thickness of only one atomic layer, so the film is called monoatomic layer graphite, and is a novel nano material which is the thinnest, the highest in strength and the strongest in electric conduction and heat conduction performance and is discovered at present.
The theoretical conductivity of the graphene can reach 106S/cm, far exceeding that of common carbon materials. But inIn practical application, due to contact resistance between graphene sheets and internal defects, the conductivity actually exerted by graphene is 103The level of S/cm or less is equivalent to the performance of materials such as carbon nanotubes and vapor grown carbon nanofibers. At present, graphene has played a better role as a conductive agent or a composite conductive coating material in the application fields of lithium batteries, conductive ink, printed circuits and the like.
Disclosure of Invention
The invention mainly aims to provide a novel nano-metal modified graphene conductive material and a preparation method thereof, and aims to solve the technical problems of solving the contact resistance between sheets in the material application process of graphene and improving the conductivity, so that the novel nano-metal modified graphene conductive material is more practical.
The purpose of the invention and the technical problem to be solved are realized by adopting the following technical scheme. The preparation method of the nano-metal modified graphene conductive material provided by the invention comprises the following steps:
mixing and dispersing graphene and a dispersing agent to obtain a graphene dispersion system;
dissolving a metal salt in a solvent to obtain a metal salt solution;
ultrasonically dispersing the metal salt solution and the graphene dispersion system, and adding a stabilizer to obtain a mixed solution;
heating the mixed solution by microwave, filtering, cleaning and drying to obtain mixed powder;
and sintering the mixed powder in an inert atmosphere, and crushing and ball-milling to obtain the nano metal modified graphene conductive material.
The object of the present invention and the technical problems solved thereby can be further achieved by the following technical measures.
Preferably, in the preparation method of the nano-metal modified graphene conductive material, the number of layers of the graphene is 1-10, and the sheet diameter is 0.1-20 μm;
the dispersing agent is at least one of glycol, glycerol, ethanol, isopropanol, N-methyl pyrrolidone, tetrahydrofuran and water;
the mass ratio of the graphene to the dispersing agent is 1-5: 95-99.
Preferably, in the preparation method of the nanometal-modified graphene conductive material, the metal salt is at least one of nitrate, perchlorate and chloride; the metal element in the metal salt is at least one of gold, platinum, silver, ruthenium, palladium, cobalt, manganese and nickel;
the solvent is water and/or alcohol; the concentration of the metal salt solution is 0.05-1 mol/L.
Preferably, in the preparation method of the nano-metal modified graphene conductive material, the stabilizer is citric acid 1-5%; the stabilizer accounts for 1-5% of the total mass of the metal salt and the graphene.
Preferably, in the preparation method of the nano-metal modified graphene conductive material, the microwave heating power is 500-1000W, and the heating time is 0.5-5 min.
Preferably, in the preparation method of the nanometal-modified graphene conductive material, the inert atmosphere is a mixed gas of argon and hydrogen, and the molar ratio of argon to hydrogen is 5-10: 1.
Preferably, in the preparation method of the nano-metal modified graphene conductive material, the sintering temperature is 500-700 ℃, and the sintering time is 3-10 h.
The object of the present invention and the technical problem to be solved are also achieved by the following technical means. According to the nano metal modified graphene conductive material provided by the invention, the nano metal modified graphene conductive material is prepared by the method; the nano metal modified graphene conductive material comprises the following components in percentage by mass:
nano metal particles: 1 to 50 percent;
graphene: 50 to 99 percent.
The object of the present invention and the technical problems solved thereby can be further achieved by the following technical measures.
Preferably, the nano-metal modified graphene conductive material has a particle size of 5-300 nm.
Preferably, the conductivity of the nanometal-modified graphene conductive material is greater than 103S/cm。
By the technical scheme, the nano-metal modified graphene conductive material and the preparation method thereof at least have the following advantages:
fully grinding graphene powder and a dispersing agent, dispersing for the first time, adding a metal salt solution taking alcohols as a solvent into a uniform phase of the graphene powder, fully dispersing for the second time, and then heating and reducing by using microwaves to deposit reduced metal particles on the surface of a graphene lamellar structure; due to the surface energy effect, metal particles deposited on particle defects or contact interfaces are denser, and the purpose of reducing contact resistance can be achieved. And then filtering, drying, high-temperature calcining and other processes are carried out to achieve the purposes of removing functional groups on the surfaces of the particles of the mixture material and increasing the crystallinity. The conductivity of the nano metal modified graphene conductive material is obviously improved and can reach 103And more than S/cm.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical solutions of the present invention more clearly understood and to implement them in accordance with the contents of the description, the following detailed description is given with reference to the preferred embodiments of the present invention and the accompanying drawings.
Drawings
Fig. 1 is a schematic view of the microstructure of graphene.
Fig. 2 is a schematic microstructure diagram of a nanometal-modified graphene conductive material.
Fig. 3 is a microscopic view of a contact portion between graphene sheets of the nanometal-modified graphene conductive material.
Detailed Description
To further illustrate the technical means and effects of the present invention for achieving the predetermined objects, the following detailed description will be given to the embodiments, structures, features and effects of the nano-metal modified graphene conductive material and the preparation method thereof according to the present invention with reference to the accompanying drawings and preferred embodiments. In the following description, different "one embodiment" or "an embodiment" refers to not necessarily the same embodiment. Furthermore, the particular features, structures, or characteristics may be combined in any suitable manner in one or more embodiments.
One embodiment of the present invention provides a method for preparing a nano-metal modified graphene conductive material, including:
mixing graphene with a dispersing agent, and performing ball milling, stirring and ultrasonic dispersion to obtain a graphene dispersion system;
dissolving a metal salt in a solvent to obtain a metal salt solution;
ultrasonically dispersing the metal salt solution and the graphene dispersion system, and adding a stabilizer to obtain a mixed solution;
microwave heating the mixed solution, filtering, washing with ethanol, and vacuum drying to obtain mixed powder;
and sintering the mixed powder in an inert atmosphere, and crushing and ball-milling. And obtaining the nano metal modified graphene conductive material.
Preferably, the number of layers of the graphene is 1-10, and the sheet diameter is 0.1-20 μm.
Preferably, the dispersant is at least one of ethylene glycol, glycerol, ethanol, isopropanol, N-methylpyrrolidone, tetrahydrofuran, and water.
Preferably, the mass ratio of the graphene to the dispersing agent is 1-5: 95-99.
Preferably, the metal salt is at least one of nitrate, perchlorate and chloride; the metal element in the metal salt is at least one of gold, platinum, silver, ruthenium, palladium, cobalt, manganese and nickel
Preferably, the solvent is water and/or alcohol; the concentration of the metal salt solution is 0.05-1 mol/L.
Preferably, the stabilizer is citric acid; the stabilizer accounts for 1-5% of the total mass of the metal salt and the graphene.
Preferably, the power of microwave heating is 500-. Depositing the reduced metal particles on the surface of the graphene lamellar structure by using a microwave heating reduction method; due to the surface energy effect, metal particles deposited on particle defects or contact interfaces are denser, and the purpose of reducing contact resistance can be achieved.
The preferred inert atmosphere is a mixed gas of argon and hydrogen in a molar ratio of 5-10: 1.
Preferably, the sintering temperature is 500-700 ℃, and the sintering time is 3-10 h. So as to achieve the purposes of removing the functional groups on the surfaces of the particles of the mixture material and increasing the crystallinity.
Another embodiment of the present invention provides a nano-metal modified graphene conductive material prepared by the foregoing method. As shown in fig. 1, which is a schematic view of a microstructure of graphene, contact between graphene sheet 1, graphene sheet 2, and graphene sheet 3 is overlapped, contact resistance exists, and conductivity actually exerted by graphene is 10 due to internal defects thereof3A level of S/cm or less. Fig. 2 is a schematic view of a microstructure of a nano-metal modified graphene conductive material, and a nano-metal particle 7 is deposited on a contact interface by a graphene sheet 4, a graphene sheet 5 and a graphene sheet 6, so that the purpose of reducing contact resistance can be achieved. Fig. 3 is a microscopic schematic view of a contact part between graphene sheets of the nano-metal modified graphene conductive material, and the graphene sheets 8 and 9 deposit more nano-metal particles 10 on a contact interface, so as to reduce contact resistance.
The nano metal modified graphene conductive material comprises the following components in percentage by mass:
nano metal particles: 1 to 50 percent;
graphene: 50 to 99 percent.
Preferably, the metal nanoparticles have a particle size of 5 to 300 nm.
Preferably, the conductivity of the nano metal modified graphene conductive material is more than 103S/cm。
Example 1
One embodiment of the present invention provides a method for preparing a nano-metal modified graphene conductive material, including:
mixing graphene and a dispersing agent according to a mass ratio of 1:99, and performing ball milling dispersion to obtain a graphene dispersion system; wherein the average number of layers of the graphene is 3, and the average sheet diameter is 0.5 mu m; the dispersing agent is a mixed solution of ethanol and glycerol, and the volume ratio of the ethanol to the glycerol is 5: 2;
dissolving silver nitrate in a mixed solvent of water and ethanol in a volume ratio of 1:1 to obtain 0.05mol/L metal salt solution;
ultrasonically dispersing the metal salt solution and the graphene dispersion system, and adding citric acid to obtain a mixed solution; wherein the citric acid accounts for 1% of the total mass of the metal salt and the graphene;
heating the mixed solution by 500W microwave for 5min, filtering, washing with ethanol, and vacuum drying to obtain mixed powder;
and sintering the mixed powder for 10 hours at 500 ℃ in a mixed atmosphere of argon and hydrogen with a molar ratio of 9:1, and crushing and ball-milling to obtain the nano metal modified graphene conductive material.
Another embodiment of the present invention provides a nano metal modified graphene conductive material prepared by the method of embodiment 1; the nano metal modified graphene conductive material comprises the following components in percentage by mass:
nano metal particles: 1 percent; the average particle diameter of the metal nanoparticles is 10 nm;
graphene: 99 percent.
The conductivity of the nanometal-modified graphene conductive material of example 1 is 1.1 × 10 or more3S/cm。
Example 2
One embodiment of the present invention provides a method for preparing a nano-metal modified graphene conductive material, including:
mixing graphene and a dispersing agent according to a mass ratio of 5:95, and performing ball milling dispersion to obtain a graphene dispersion system; wherein the average number of layers of the graphene is 5, and the average sheet diameter is 20 mu m; the dispersing agent is a mixed solution of ethylene glycol and isopropanol, and the volume ratio of the ethylene glycol to the isopropanol is 1: 2;
dissolving nickel chloride in a mixed solvent of water and ethylene glycol in a volume ratio of 1:5 to obtain 1mol/L metal salt solution;
ultrasonically dispersing the metal salt solution and the graphene dispersion system, and adding citric acid to obtain a mixed solution; wherein the citric acid accounts for 5% of the total mass of the metal salt and the graphene;
heating the mixed solution by 1000W microwave for 0.5min, filtering, washing with ethanol, and vacuum drying to obtain mixed powder;
and sintering the mixed powder for 3h at 700 ℃ in a mixed atmosphere of argon and hydrogen with a molar ratio of 8:1, and crushing and ball-milling to obtain the nano-metal modified graphene conductive material.
Another embodiment of the present invention provides a nano-metal modified graphene conductive material prepared by the method of embodiment 2; the nano metal modified graphene conductive material comprises the following components in percentage by mass:
nano metal particles: 50 percent; the average particle diameter of the metal nanoparticles is 50 nm;
graphene: 50 percent.
The conductivity of the nanometal modified graphene conductive material of embodiment 2 is 1.8 × 10 or more3S/cm。
Example 3
One embodiment of the present invention provides a method for preparing a nano-metal modified graphene conductive material, including:
mixing graphene and a dispersing agent according to a mass ratio of 8:92, and performing ball milling dispersion to obtain a graphene dispersion system; wherein the average number of layers of the graphene is 8, and the average sheet diameter is 2 mu m; the dispersing agent is a mixed solution of glycol and water, and the volume ratio of the glycol to the water is 1: 1;
dissolving cobalt nitrate in a mixed solvent of water and isopropanol in a volume ratio of 1:2 to obtain 0.5mol/L metal salt solution;
ultrasonically dispersing the metal salt solution and the graphene dispersion system, and adding citric acid to obtain a mixed solution; wherein the citric acid accounts for 3% of the total mass of the metal salt and the graphene;
heating the mixed solution by 800W microwave for 2min, filtering, washing with ethanol, and vacuum drying to obtain mixed powder;
and sintering the mixed powder for 5 hours at 600 ℃ in a mixed atmosphere of argon and hydrogen with a molar ratio of 9:1, and crushing and ball-milling to obtain the nano metal modified graphene conductive material.
Another embodiment of the present invention provides a nano-metal modified graphene conductive material prepared by the method of embodiment 3; the nano metal modified graphene conductive material comprises the following components in percentage by mass:
nano metal particles: 30 percent; the average particle diameter of the metal nanoparticles is 20 nm;
graphene: 70 percent.
The conductivity of the nanometal-modified graphene conductive material of example 3 is 1.3 × 10 or more3S/cm。
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any simple modification, equivalent change and modification made to the above embodiment according to the technical spirit of the present invention are still within the scope of the technical solution of the present invention.
Claims (10)
1. A preparation method of a nano-metal modified graphene conductive material is characterized by comprising the following steps:
mixing and dispersing graphene and a dispersing agent to obtain a graphene dispersion system;
dissolving a metal salt in a solvent to obtain a metal salt solution;
ultrasonically dispersing the metal salt solution and the graphene dispersion system, and adding a stabilizer to obtain a mixed solution;
heating the mixed solution by microwave, filtering, cleaning and drying to obtain mixed powder;
sintering the mixed powder in an inert atmosphere, and crushing and ball-milling to obtain a nano metal modified graphene conductive material;
the number of layers of the graphene is 1-10, and the sheet diameter is 0.1-20 mu m.
2. The method for preparing the nanometal-modified graphene conductive material according to claim 1, wherein the dispersant is at least one of ethylene glycol, glycerol, ethanol, isopropanol, N-methylpyrrolidone, tetrahydrofuran and water;
the mass ratio of the graphene to the dispersing agent is 1-5: 95-99.
3. The method for preparing the nanometal-modified graphene conductive material according to claim 1, wherein the metal salt is at least one of nitrate, perchlorate and chloride; the metal element in the metal salt is at least one of gold, platinum, silver, ruthenium, palladium, cobalt, manganese and nickel;
the solvent is water and/or alcohol; the concentration of the metal salt solution is 0.05-1 mol/L.
4. The method for preparing the nano-metal modified graphene conductive material according to claim 1, wherein the stabilizer is citric acid; the stabilizer accounts for 1-5% of the total mass of the metal salt and the graphene.
5. The method as claimed in claim 1, wherein the microwave heating power is 500-1000W, and the heating time is 0.5-5 min.
6. The method for preparing the nanometal-modified graphene conductive material according to claim 1, wherein the inert atmosphere is a mixed gas of argon and hydrogen, and the molar ratio of the argon to the hydrogen is 5-10: 1.
7. The method for preparing the nano-metal modified graphene conductive material as claimed in claim 1, wherein the sintering temperature is 500-700 ℃ and the sintering time is 3-10 h.
8. A nano-metal modified graphene conductive material, which is prepared by the method of any one of claims 1 to 7; the nano metal modified graphene conductive material comprises the following components in percentage by mass:
nano metal particles: 1 to 50 percent;
graphene: 50 to 99 percent.
9. The nanometal-modified graphene conductive material of claim 8, wherein the metal nanoparticles have a particle size of 5-300 nm.
10. The nanometal-modified graphene conductive material of claim 8, wherein the conductivity of the nanometal-modified graphene conductive material is greater than 103S/cm。
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| CN109585852B (en) * | 2018-12-05 | 2021-09-21 | 南昌航空大学 | Graphene composite conductive agent and preparation method thereof |
| CN110836919B (en) * | 2019-11-29 | 2022-05-20 | 金陵科技学院 | Chiral recognition material and preparation method thereof |
| CN113593769B (en) * | 2021-07-07 | 2023-07-28 | 宁波石墨烯创新中心有限公司 | Graphene composite film and preparation method thereof |
| CN113540464A (en) * | 2021-07-16 | 2021-10-22 | 中国科学院宁波材料技术与工程研究所 | Preparation method of metal nanoparticle modified graphite material and three-dimensional graphite skeleton pole piece |
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