CN109622947B - Preparation method of metal-graphene composite material - Google Patents
Preparation method of metal-graphene composite material Download PDFInfo
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- CN109622947B CN109622947B CN201811598244.9A CN201811598244A CN109622947B CN 109622947 B CN109622947 B CN 109622947B CN 201811598244 A CN201811598244 A CN 201811598244A CN 109622947 B CN109622947 B CN 109622947B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/16—Metallic particles coated with a non-metal
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/102—Metallic powder coated with organic material
Abstract
The invention belongs to the technical field of modified graphene, and particularly provides a preparation method of a metal-graphene composite material, which comprises the following steps: (1) carrying out surface modification on the metal powder by using a surface modifier; (2) and (2) mixing the surface-modified metal powder obtained in the step (1), graphite fluoride and a hydrazine hydrate solution, and then carrying out reduction reaction to obtain the metal-graphene composite material. According to the invention, the fluorinated graphene is reduced into the graphene while the graphene and the metal are combined, and the metal can be uniformly dispersed and wrapped in the graphene. The invention shortens the preparation process, and has simple and convenient operation and easy implementation.
Description
Technical Field
The invention relates to the technical field of modified graphene, in particular to a preparation method of a metal-graphene composite material.
Background
Graphene (Graphene) is a polymer made of carbon atoms in sp2The hexagonal honeycomb-lattice two-dimensional carbon nanomaterial formed by the hybrid tracks has excellent optical, electrical and mechanical properties, has important application prospects in the aspects of materials science, micro-nano processing, energy, biomedicine, drug delivery and the like, and is considered to be a revolutionary material in the future.
The graphene and the superfine spherical metal powder are combined to form a unique structure taking the graphene as a shell and the metal balls as a core, so that on one hand, the heat conduction and electric conduction characteristics of the metal can be maintained, and meanwhile, the thermal mechanical property of the metal can be improved. In addition, graphene is used as a stable material, and when the graphene is coated on the surface of copper, the oxidation resistance of the copper can be enhanced.
At present, few studies on graphene-coated metal materials are made, and an article entitled "Synthesis, growth mechanism and thermal stability" of graphene nanoparticles encapsulated by multi-layer graphene, which is published by wang et al in Carbon (2012, 50, 6, 2119-2125), has been reported, and means for preparing graphene-coated spherical copper powder by using a chemical vapor deposition method and the oxidation resistance of the material are reported. However, the conventional method for preparing graphene-coated spherical copper powder by using a chemical vapor deposition method has high production cost because special equipment is required.
Chinese patent publication No. CN 103817336a also discloses a technical scheme of graphene-coated copper. However, in the patent, a graphene oxide-coated copper product needs to be prepared first, and then the graphene oxide is reduced, so that the operation method is still complicated.
Disclosure of Invention
The invention aims to provide a preparation method of a metal-graphene composite material, which is simple and convenient to operate and easy to implement.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of a metal-graphene composite material, which comprises the following steps:
(1) carrying out surface modification on the metal powder by using a surface modifier;
(2) and (2) mixing the surface-modified metal powder obtained in the step (1), graphite fluoride and a hydrazine hydrate solution, and then carrying out reduction reaction to obtain the metal-graphene composite material.
Preferably, the surface modifier in the step (1) is a mixture of 3-aminopropyltriethoxysilane and 3-aminopropyltrimethoxysilane;
the mass ratio of the 3-aminopropyltriethoxysilane to the 3-aminopropyltrimethoxysilane is 1: 2-4.
Preferably, the metal powder in the step (1) is copper powder, iron powder, gold powder or silver powder, and the particle size of the metal powder is 0.1-2 μm.
Preferably, the specific process of surface modification in step (1) is as follows:
and mixing the metal powder, the surface modifier and the organic solvent, and then carrying out heating treatment to obtain the surface modified metal powder.
Preferably, the mass ratio of the metal powder to the surface modifier is (1-5) to (2-10);
the organic solvent is a mixture of toluene and isobutanol, and the volume ratio of the toluene to the isobutanol is (2-4) to (1-3);
the mass ratio of the surface modifier to the organic solvent is (1-5) to 100.
Preferably, the temperature of the heating treatment is 50-80 ℃, and the time is 20-24 h.
Preferably, the mass ratio of the metal powder subjected to surface modification in the step (2) to the graphite fluoride is (5-10) to 1;
the mass concentration of the hydrazine hydrate solution is 60-70%;
the ratio of the volume of the hydrazine hydrate solution to the mass of the graphite fluoride is 1L to (5-10) g.
Preferably, the temperature of the reduction reaction in the step (2) is 80-100 ℃, and the time is 2-8 h.
The invention provides a preparation method of a metal-graphene composite material, which comprises the following steps: (1) carrying out surface modification on the metal powder by using a surface modifier; (2) and (2) mixing the surface-modified metal powder obtained in the step (1), graphite fluoride and a hydrazine hydrate solution, and then carrying out reduction reaction to obtain the metal-graphene composite material. According to the invention, the fluorinated graphene is reduced into the graphene while the graphene and the metal are combined, and the metal can be uniformly dispersed and wrapped in the graphene. The invention shortens the preparation process, and has simple and convenient operation and easy implementation.
Detailed Description
The invention provides a preparation method of a metal-graphene composite material, which comprises the following steps:
(1) carrying out surface modification on the metal powder by using a surface modifier;
(2) and (2) mixing the surface-modified metal powder obtained in the step (1), graphite fluoride and a hydrazine hydrate solution, and then carrying out reduction reaction to obtain the metal-graphene composite material.
The invention uses surface modifier to modify the surface of metal powder. In the present invention, the surface modifier in the step (1) is preferably a mixture of 3-aminopropyltriethoxysilane and 3-aminopropyltrimethoxysilane; the mass ratio of the 3-aminopropyltriethoxysilane to the 3-aminopropyltrimethoxysilane is preferably 1: 2-4, and more preferably 1: 3. According to the invention, 3-aminopropyltriethoxysilane and 3-aminopropyltrimethoxysilane are mixed according to a fixed proportion, so that the modification effect of the modified metal powder can be improved to the maximum extent, and the combination between the modified metal powder and graphene is further promoted.
In the present invention, the metal powder in step (1) is preferably copper powder, iron powder, gold powder or silver powder, and the particle size of the metal powder is preferably 0.1 to 2 μm, and more preferably 0.5 to 1 μm.
In the present invention, the specific process of surface modification in the step (1) is preferably as follows:
and mixing the metal powder, the surface modifier and the organic solvent, and then carrying out heating treatment to obtain the surface modified metal powder.
In the invention, the mass ratio of the metal powder to the surface modifier is preferably (1-5) to (2-10), and more preferably (2-3) to (5-8); the organic solvent is preferably a mixture of toluene and isobutanol, the volume ratio of the toluene to the isobutanol is preferably (2-4): (1-3), and more preferably 3: 2; the mass ratio of the surface modifier to the organic solvent is preferably (1-5) to 100, and more preferably (3-4) to 100. According to the invention, the toluene and the isobutanol are mixed, so that the dispersion uniformity of the metal powder and the surface modifier in the organic solvent can be improved.
In the invention, the temperature of the heating treatment is preferably 50-80 ℃, and more preferably 60-70 ℃; the time is preferably 20 to 24 hours, and more preferably 22 to 23 hours.
After the heating treatment is finished, the obtained system is preferably filtered, and filter residues obtained by filtering are dried to obtain the surface-modified metal powder. The invention has no special requirements on the drying temperature and time, and can realize the drying purpose. The surface modification can promote the combination between the metal powder and the graphene.
The method comprises the steps of mixing the surface-modified metal powder obtained in the step (1), graphite fluoride and a hydrazine hydrate solution, and then carrying out reduction reaction to obtain the metal-graphene composite material.
In the invention, the mass ratio of the metal powder subjected to surface modification in the step (2) to the graphite fluoride is preferably (5-10) to 1, and more preferably (6-8) to 1; the mass concentration of the hydrazine hydrate solution is preferably 60-70%, and more preferably 62-68%; the ratio of the volume of the hydrazine hydrate solution to the mass of the graphite fluoride is preferably 1L to (5-10) g, and more preferably 1L to (6-8) g.
In the invention, the temperature of the reduction reaction in the step (2) is preferably 80-100 ℃, and more preferably 85-95 ℃; the time is preferably 2 to 8 hours, and more preferably 4 to 6 hours.
The invention preferably mixes the surface modified metal powder, graphite fluoride and hydrazine hydrate solution to obtain a system, and carries out ultrasonic treatment to promote the dispersion of the surface modified metal powder and graphite fluoride in the mixed system; the time of the ultrasonic treatment is preferably 25-35 min, and the frequency of the ultrasonic treatment can be known by those skilled in the art.
The technical solutions provided by the present invention are described in detail below with reference to examples, but they should not be construed as limiting the scope of the present invention.
Example 1
(1) Carrying out surface modification on the metal powder by using a surface modifier: mixing the metal powder, the surface modifier and the organic solvent and then carrying out heating treatment; and after the heating treatment is finished, filtering the obtained system, and drying filter residues obtained by filtering to obtain the surface-modified metal powder.
Wherein the surface modifier is a mixture of 3-aminopropyltriethoxysilane and 3-aminopropyltrimethoxysilane, and the mass ratio of the 3-aminopropyltriethoxysilane to the 3-aminopropyltrimethoxysilane is 1: 3;
the metal powder is copper powder, and the particle size range is 0.5-1 mu m;
the mass ratio of the metal powder to the surface modifier is 1: 5;
the organic solvent is a mixture of toluene and isobutanol, and the volume ratio of the toluene to the isobutanol is 3: 2;
the mass ratio of the surface modifier to the organic solvent is 3: 100;
the temperature of the heat treatment was 75 ℃ and the time was 22 hours.
(2) Ultrasonically mixing the surface-modified metal powder obtained in the step (1), graphite fluoride and hydrazine hydrate solution for 25min, and then carrying out reduction reaction to obtain a metal-graphene composite material:
wherein the mass ratio of the surface-modified metal powder to the graphite fluoride is 6: 1;
the mass concentration of the hydrazine hydrate solution is 68 percent;
the ratio of the volume of the hydrazine hydrate solution to the mass of the graphite fluoride is 1L: 7 g;
the temperature of the reduction reaction is 85 ℃ and the time is 4 h.
When the composite material obtained in the embodiment is detected, an electron microscope result shows that a plurality of curled graphene exists around the spherical copper, which indicates that the graphene covers the surface of the spherical copper.
The conductivity of the composite material obtained in this example was measured by a four-probe method, and the conductivity was 3420S/m.
The transmission electron microscope scanning is carried out on the product obtained in the embodiment, and the result shows that the copper particles are uniformly distributed and have the particle size of 0.5-1 μm.
Example 2
(1) Carrying out surface modification on the metal powder by using a surface modifier: mixing the metal powder, the surface modifier and the organic solvent and then carrying out heating treatment; and after the heating treatment is finished, filtering the obtained system, and drying filter residues obtained by filtering to obtain the surface-modified metal powder.
Wherein the surface modifier is a mixture of 3-aminopropyltriethoxysilane and 3-aminopropyltrimethoxysilane, and the mass ratio of the 3-aminopropyltriethoxysilane to the 3-aminopropyltrimethoxysilane is 1: 4;
the metal powder is silver powder with the particle size range of 0.5-1 mu m;
the mass ratio of the metal powder to the surface modifier is 1: 4;
the organic solvent is a mixture of toluene and isobutanol, and the volume ratio of the toluene to the isobutanol is 3: 1;
the mass ratio of the surface modifier to the organic solvent is 5: 100;
the temperature of the heat treatment was 65 ℃ and the time was 22 hours.
(2) Ultrasonically mixing the surface-modified metal powder obtained in the step (1), graphite fluoride and hydrazine hydrate solution for 25min, and then carrying out reduction reaction to obtain a metal-graphene composite material:
wherein the mass ratio of the surface-modified metal powder to the graphite fluoride is 7: 1;
the mass concentration of the hydrazine hydrate solution is 68 percent;
the ratio of the volume of the hydrazine hydrate solution to the mass of the graphite fluoride is 1L: 8 g;
the temperature of the reduction reaction was 95 ℃ and the time was 4 hours.
When the composite material obtained in the embodiment is detected, an electron microscope result shows that a plurality of curled graphene exists around the spherical silver, which indicates that the graphene covers the surface of the spherical silver.
The conductivity of the composite material obtained in this example was measured by a four-probe method, and it was found that the conductivity was 3230S/m.
The transmission electron microscope scanning is carried out on the product obtained in the embodiment, and the result shows that the silver particles are uniformly distributed and have the particle size of 0.5-1 μm.
Example 3
(1) Carrying out surface modification on the metal powder by using a surface modifier: mixing the metal powder, the surface modifier and the organic solvent and then carrying out heating treatment; and after the heating treatment is finished, filtering the obtained system, and drying filter residues obtained by filtering to obtain the surface-modified metal powder.
Wherein the surface modifier is a mixture of 3-aminopropyltriethoxysilane and 3-aminopropyltrimethoxysilane, and the mass ratio of the 3-aminopropyltriethoxysilane to the 3-aminopropyltrimethoxysilane is 1: 2;
the metal powder is gold powder, and the particle size range is 0.5-1 mu m;
the mass ratio of the metal powder to the surface modifier is 1: 8;
the organic solvent is a mixture of toluene and isobutanol, and the volume ratio of the toluene to the isobutanol is 3: 1;
the mass ratio of the surface modifier to the organic solvent is 2: 100;
the temperature of the heat treatment was 80 ℃ and the time was 24 hours.
(2) Ultrasonically mixing the surface-modified metal powder obtained in the step (1), graphite fluoride and hydrazine hydrate solution for 25min, and then carrying out reduction reaction to obtain a metal-graphene composite material:
wherein the mass ratio of the surface-modified metal powder to the graphite fluoride is 5: 1;
the mass concentration of the hydrazine hydrate solution is 68 percent;
the ratio of the volume of the hydrazine hydrate solution to the mass of the graphite fluoride is 1L: 5 g;
the temperature of the reduction reaction is 85 ℃ and the time is 4 h.
When the composite material obtained in the embodiment is detected, an electron microscope result shows that a plurality of curled graphene exists around the spherical gold, which indicates that the graphene covers the surface of the spherical gold.
The conductivity of the composite material obtained in this example was measured by a four-probe method, and the result showed that the conductivity was 3190S/m.
The transmission electron microscope scanning is carried out on the product obtained in the embodiment, and the result shows that the gold particles are uniformly distributed and have the particle size of 0.5-1 μm.
As can be seen from the above embodiments, the present invention provides a method for preparing a metal-graphene composite material, comprising the following steps: (1) carrying out surface modification on the metal powder by using a surface modifier; (2) and (2) mixing the surface-modified metal powder obtained in the step (1), graphite fluoride and a hydrazine hydrate solution, and then carrying out reduction reaction to obtain the metal-graphene composite material. According to the invention, the fluorinated graphene is reduced into the graphene while the graphene and the metal are combined, and the metal can be uniformly dispersed and wrapped in the graphene. The invention shortens the preparation process, and has simple and convenient operation and easy implementation.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (1)
1. A preparation method of a metal-graphene composite material comprises the following steps:
(1) carrying out surface modification on the metal powder by using a surface modifier;
(2) mixing the surface-modified metal powder obtained in the step (1), graphite fluoride and a hydrazine hydrate solution, and then carrying out reduction reaction to obtain a metal-graphene composite material;
the metal powder in the step (1) is gold powder or silver powder, and the particle size of the metal powder is 0.1-2 mu m;
the surface modifier in the step (1) is a mixture of 3-aminopropyltriethoxysilane and 3-aminopropyltrimethoxysilane; the mass ratio of the 3-aminopropyltriethoxysilane to the 3-aminopropyltrimethoxysilane is 1: 2-4;
the specific process of surface modification in the step (1) is as follows:
mixing the metal powder, a surface modifier and an organic solvent, and then carrying out heating treatment to obtain surface-modified metal powder;
the mass ratio of the metal powder to the surface modifier is (1-5) to (2-10);
the organic solvent is a mixture of toluene and isobutanol, and the volume ratio of the toluene to the isobutanol is (2-4) to (1-3);
the mass ratio of the surface modifier to the organic solvent is (1-5) to 100;
the heating treatment temperature is 50-80 ℃, and the time is 20-24 hours;
the mass ratio of the metal powder subjected to surface modification in the step (2) to the graphite fluoride is (5-10) to 1;
the mass concentration of the hydrazine hydrate solution is 60-70%;
the volume ratio of the hydrazine hydrate solution to the mass of the graphite fluoride is 1L to (5-10) g;
the temperature of the reduction reaction in the step (2) is 80-100 ℃, and the time is 2-8 h.
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| CN104032154A (en) * | 2014-06-27 | 2014-09-10 | 武汉大学 | Graphene/metal matrix composite material and preparation method thereof |
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| CN106670476A (en) * | 2016-12-30 | 2017-05-17 | 尹宗杰 | Graphene-nonmetal-metal composite material for 3D printing, preparation method and application |
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- 2018-12-26 CN CN201811598244.9A patent/CN109622947B/en active Active
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| JPS63260807A (en) * | 1987-04-17 | 1988-10-27 | Osaka Gas Co Ltd | Interlaminar graphite compound having coating layer and production thereof |
| JPH05156316A (en) * | 1991-12-02 | 1993-06-22 | Nippon Telegr & Teleph Corp <Ntt> | Water-repellent structural material and its production |
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