CN109622947A - A kind of preparation method of metal-graphite alkene composite material - Google Patents
A kind of preparation method of metal-graphite alkene composite material Download PDFInfo
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- CN109622947A CN109622947A CN201811598244.9A CN201811598244A CN109622947A CN 109622947 A CN109622947 A CN 109622947A CN 201811598244 A CN201811598244 A CN 201811598244A CN 109622947 A CN109622947 A CN 109622947A
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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 modified graphene technical fields, specifically provide a kind of preparation method of metal-graphite alkene composite material, comprise the following steps: (1) being surface modified using coating material to metal powder；(2) reduction reaction is carried out after mixing the metal powder, fluorographite and hydrazine hydrate solution of surface modification obtained by step (1), obtains metal-graphite alkene composite material.The present invention is reduced into graphene while by graphene and metal bonding, by fluorinated graphene, can be by the uniform dispersed encapsulated of metal inside graphene.Present invention reduces preparation flow, and it is easy to operate, it is easy to implement.
Description
Technical field
The present invention relates to modified graphene technical field more particularly to a kind of preparation sides of metal-graphite alkene composite material
Method.
Background technique
Graphene (Graphene) be one kind by carbon atom with sp2Hybridized orbit forms the two dimension that hexangle type is in honeycomb lattice
Carbon nanomaterial has excellent optics, electricity, mechanical characteristic, in materialogy, micro-nano technology, the energy, biomedicine and drug
Transmitting etc. is with important application prospects, it is considered to be a kind of future revolutionary material.
Graphene is combined with superfine spherical metal powder, forms uniqueness using graphene as shell, metal ball is the knot of core
Structure, on the one hand, be both able to maintain thermally conductive, the conductive characteristic of metal, while can also promote the thermomechanical property of metal.Also, graphite
Alkene is as a kind of stable material, when being coated on the surface of copper, moreover it is possible to enhance the inoxidizability of copper.
Currently, the research in terms of graphene coated metal material is less, existing report has wang et al. to exist
Entitled " Synthesis, the growth mechanism delivered on " Carbon " (2012,50,6,2119-2125)
andthermal stability of copper nanoparticles encapsulated by multi-layer
The article of graphene " (synthesis, growth mechanism and the thermal stability of multi-layer graphene cladding spherical copper powder), it was recently reported that utilizationization
It learns vapour deposition process and prepares the means of graphene coated spherical copper powder and the antioxygenic property of the material.However, traditional use
The method that process for preparing graphenes by chemical vapour deposition coats spherical copper powder, since it is desired that using special equipment, thus production cost
It is higher.
The Chinese patent of Publication No. CN 103817336A also discloses a kind of technical solution of graphene coated copper.But
It is that the patent needs first to prepare graphene oxide cladding copper products, then again restores graphene oxide, operating method is still
It is old comparatively laborious.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of metal-graphite alkene composite material, and this method is easy to operate,
It is easy to implement.
In order to achieve the above-mentioned object of the invention, the present invention the following technical schemes are provided:
The present invention provides a kind of preparation methods of metal-graphite alkene composite material, comprise the following steps:
(1) metal powder is surface modified using coating material；
(2) it is restored after mixing the metal powder, fluorographite and hydrazine hydrate solution of surface modification obtained by step (1)
Reaction, obtains metal-graphite alkene composite material.
Preferably, coating material is 3-aminopropyltriethoxysilane and 3- aminopropyl three in the step (1)
The mixture of methoxy silane；
The mass ratio of the 3-aminopropyltriethoxysilane and 3- TSL 8330 is 1: (2~4).
Preferably, metal powder is copper powder, iron powder, bronze or silver powder in the step (1), and the partial size of the metal powder is
0.1~2 μm.
Preferably, detailed process is as follows for surface modification in the step (1):
Heat after the metal powder, coating material and organic solvent are mixed, obtains surface modification
Metal powder.
Preferably, the mass ratio of the metal powder and coating material is (1~5): (2~10)；
The organic solvent is the mixture of toluene and isobutanol, and the volume ratio of the toluene and isobutanol is (2~4):
(1~3)；
The mass ratio of the coating material and organic solvent is (1~5): 100.
Preferably, the temperature of the heat treatment be 50~80 DEG C, the time be 20~for 24 hours.
Preferably, the mass ratio of the metal powder of surface modification and fluorographite is (5~10) in the step (2): 1；
The mass concentration of the hydrazine hydrate solution is 60~70%；
The volume of the hydrazine hydrate solution and the mass ratio of fluorographite are 1L: (5~10) g.
Preferably, the temperature of reduction reaction is 80~100 DEG C in the step (2), and the time is 2~8h.
The present invention provides a kind of preparation methods of metal-graphite alkene composite material, comprise the following steps: (1) using table
Face dressing agent is surface modified metal powder；(2) by metal powder, fluorographite and the water of surface modification obtained by step (1)
Reduction reaction is carried out after closing hydrazine solution mixing, obtains metal-graphite alkene composite material.The present invention is by graphene and metal bonding
While, fluorinated graphene is reduced into graphene, it can be by the uniform dispersed encapsulated of metal inside graphene.Present invention contracting
Short preparation flow, and it is easy to operate, it is easy to implement.
Specific embodiment
The present invention provides a kind of preparation methods of metal-graphite alkene composite material, comprise the following steps:
(1) metal powder is surface modified using coating material；
(2) it is restored after mixing the metal powder, fluorographite and hydrazine hydrate solution of surface modification obtained by step (1)
Reaction, obtains metal-graphite alkene composite material.
The present invention is surface modified metal powder using coating material.In the present invention, surface in the step (1)
Dressing agent is preferably the mixture of 3-aminopropyltriethoxysilane and 3- TSL 8330；The 3- amino
The mass ratio of propyl-triethoxysilicane and 3- TSL 8330 is preferably 1: (2~4), more preferably 1: 3.This
Invention 3-aminopropyltriethoxysilane is carried out with 3- TSL 8330 according to fixed proportion it is mixed, can
Its modification effect is promoted to greatest extent, and then promotes the combination between the metal powder and graphene after modification.
In the present invention, metal powder is preferably copper powder, iron powder, bronze or silver powder in the step (1), the metal powder
Partial size is preferably 0.1~2 μm, and more preferably 0.5~1 μm.
In the present invention, the detailed process of surface modification is preferably as follows in the step (1):
Heat after the metal powder, coating material and organic solvent are mixed, obtains surface modification
Metal powder.
In the present invention, the mass ratio of the metal powder and coating material is preferably (1~5): (2~10), more preferably
For (2~3): (5~8)；The organic solvent is preferably the mixture of toluene and isobutanol, the volume of the toluene and isobutanol
Than preferably (2~4): (1~3), more preferably 3: 2；The mass ratio of the coating material and organic solvent be preferably (1~
5): 100, more preferably (3~4): 100.The present invention mixes toluene and isobutanol, can be improved metal powder and coating material
Dispersing uniformity in organic solvent.
In the present invention, the temperature of the heat treatment is preferably 50~80 DEG C, and more preferably 60~70 DEG C；Time is preferred
For 20~for 24 hours, more preferably 22~23h.
After the heat treatment, the present invention is preferably filtered obtained system, to the filter residue being obtained by filtration into
The metal powder of surface modification described in row drying to obtain.The present invention does not have particular/special requirement to the temperature and time of the drying,
It can be realized drying purpose.Surface modification of the present invention can promote the combination between metal powder and graphene.
The present invention carries out after mixing the metal powder, fluorographite and hydrazine hydrate solution of surface modification obtained by step (1)
Reduction reaction obtains metal-graphite alkene composite material.
In the present invention, the mass ratio of the metal powder of surface modification and fluorographite is preferably (5 in the step (2)
~10): 1, more preferably (6~8): 1；The mass concentration of the hydrazine hydrate solution is preferably 60~70%, more preferably 62~
68%；The volume of the hydrazine hydrate solution and the mass ratio of fluorographite are preferably 1L: (5~10) g, and more preferably 1L: (6
~8) g.
In the present invention, the temperature of reduction reaction is preferably 80~100 DEG C, more preferably 85~95 in the step (2)
℃；Time is preferably 2~8h, more preferably 4~6h.
The system that the metal powder, fluorographite and hydrazine hydrate solution of the surface modification are preferably mixed to get by the present invention
It is ultrasonically treated, to promote the dispersion of the metal powder and fluorographite of surface modification in mixed system；The ultrasonic treatment
Time be preferably 25~35min, the frequency of the ultrasonic treatment is using well-known to those skilled in the art.
Technical solution provided by the invention is described in detail below with reference to embodiment, but they cannot be understood
For limiting the scope of the present invention.
Embodiment 1
(1) metal powder is surface modified using coating material: by the metal powder, coating material and organic molten
Heated after agent mixing；After the heat treatment, obtained system is filtered, to the filter residue being obtained by filtration
It is dried and obtains the metal powder of the surface modification and obtain the metal powder of surface modification.
Wherein, coating material is the mixing of 3-aminopropyltriethoxysilane and 3- TSL 8330
The mass ratio of object, the 3-aminopropyltriethoxysilane and 3- TSL 8330 is 1: 3；
Metal powder is copper powder, and particle size range is 0.5~1 μm；
The mass ratio of metal powder and coating material is 1: 5；
Organic solvent is the mixture of toluene and isobutanol, and the volume ratio of the toluene and isobutanol is 3: 2；
The mass ratio of coating material and organic solvent is 3: 100；
The temperature of heat treatment is 75 DEG C, time 22h.
(2) by metal powder, fluorographite and the hydrazine hydrate solution ultrasonic mixing 25min of surface modification obtained by step (1)
After carry out reduction reaction, obtain metal-graphite alkene composite material:
Wherein, the mass ratio of the metal powder of surface modification and fluorographite is 6: 1；
The mass concentration of hydrazine hydrate solution is 68%；
The volume of hydrazine hydrate solution and the mass ratio of fluorographite are 1L: 7g；
The temperature of reduction reaction is 85 DEG C, time 4h.
The composite material that the present embodiment obtains is detected, Electronic Speculum is the result shows that there are many stones crimped around spherical copper
Black alkene exists, and illustrates that graphene is covered on spherical copper surface.
The conductivity for the composite material that the present embodiment obtains is tested by four probe method, the results show that its conductivity is
3420S/m。
Transmission electron microscopy is carried out to the product that the present embodiment obtains, as the result is shown copper even particle distribution, partial size 0.5
~1 μm.
Embodiment 2
(1) metal powder is surface modified using coating material: by the metal powder, coating material and organic molten
Heated after agent mixing；After the heat treatment, obtained system is filtered, to the filter residue being obtained by filtration
It is dried and obtains the metal powder of the surface modification and obtain the metal powder of surface modification.
Wherein, coating material is the mixing of 3-aminopropyltriethoxysilane and 3- TSL 8330
The mass ratio of object, the 3-aminopropyltriethoxysilane and 3- TSL 8330 is 1: 4；
Metal powder is silver powder, and particle size range is 0.5~1 μm；
The mass ratio of metal powder and coating material is 1: 4；
Organic solvent is the mixture of toluene and isobutanol, and the volume ratio of the toluene and isobutanol is 3: 1；
The mass ratio of coating material and organic solvent is 5: 100；
The temperature of heat treatment is 65 DEG C, time 22h.
(2) by metal powder, fluorographite and the hydrazine hydrate solution ultrasonic mixing 25min of surface modification obtained by step (1)
After carry out reduction reaction, obtain metal-graphite alkene composite material:
Wherein, the mass ratio of the metal powder of surface modification and fluorographite is 7: 1；
The mass concentration of hydrazine hydrate solution is 68%；
The volume of hydrazine hydrate solution and the mass ratio of fluorographite are 1L: 8g；
The temperature of reduction reaction is 95 DEG C, time 4h.
The composite material that the present embodiment obtains is detected, Electronic Speculum is the result shows that there are many stones crimped around spherical silver
Black alkene exists, and illustrates that graphene is covered on spherical silver surface.
The conductivity for the composite material that the present embodiment obtains is tested by four probe method, the results show that its conductivity is
3230S/m。
Transmission electron microscopy is carried out to the product that the present embodiment obtains, Argent grain is evenly distributed as the result is shown, partial size 0.5
~1 μm.
Embodiment 3
(1) metal powder is surface modified using coating material: by the metal powder, coating material and organic molten
Heated after agent mixing；After the heat treatment, obtained system is filtered, to the filter residue being obtained by filtration
It is dried and obtains the metal powder of the surface modification and obtain the metal powder of surface modification.
Wherein, coating material is the mixing of 3-aminopropyltriethoxysilane and 3- TSL 8330
The mass ratio of object, the 3-aminopropyltriethoxysilane and 3- TSL 8330 is 1: 2；
Metal powder is bronze, and particle size range is 0.5~1 μm；
The mass ratio of metal powder and coating material is 1: 8；
Organic solvent is the mixture of toluene and isobutanol, and the volume ratio of the toluene and isobutanol is 3: 1；
The mass ratio of coating material and organic solvent is 2: 100；
The temperature of heat treatment is 80 DEG C, and the time is for 24 hours.
(2) by metal powder, fluorographite and the hydrazine hydrate solution ultrasonic mixing 25min of surface modification obtained by step (1)
After carry out reduction reaction, obtain metal-graphite alkene composite material:
Wherein, the mass ratio of the metal powder of surface modification and fluorographite is 5: 1；
The mass concentration of hydrazine hydrate solution is 68%；
The volume of hydrazine hydrate solution and the mass ratio of fluorographite are 1L: 5g；
The temperature of reduction reaction is 85 DEG C, time 4h.
The composite material that the present embodiment obtains is detected, Electronic Speculum is the result shows that there are many stones crimped around spherical gold
Black alkene exists, and illustrates that graphene is covered on spherical gold surface.
The conductivity for the composite material that the present embodiment obtains is tested by four probe method, the results show that its conductivity is
3190S/m。
Transmission electron microscopy is carried out to the product that the present embodiment obtains, gold particle is evenly distributed as the result is shown, partial size 0.5
~1 μm.
As seen from the above embodiment, the present invention provides a kind of preparation methods of metal-graphite alkene composite material, comprising such as
Lower step: (1) using coating material metal powder is surface modified；(2) by the metal of surface modification obtained by step (1)
Reduction reaction is carried out after powder, fluorographite and hydrazine hydrate solution mixing, obtains metal-graphite alkene composite material.The present invention is inciting somebody to action
While graphene and metal bonding, fluorinated graphene is reduced into graphene, it can be by the uniform dispersed encapsulated of metal in stone
Inside black alkene.Present invention reduces preparation flow, and it is easy to operate, it is easy to implement.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (8)
1. a kind of preparation method of metal-graphite alkene composite material, comprises the following steps:
(1) metal powder is surface modified using coating material；
(2) restore after mixing the metal powder, fluorographite and hydrazine hydrate solution of surface modification obtained by step (1) anti-
It answers, obtains metal-graphite alkene composite material.
2. preparation method according to claim 1, which is characterized in that coating material is 3- amino in the step (1)
The mixture of propyl-triethoxysilicane and 3- TSL 8330；
The mass ratio of the 3-aminopropyltriethoxysilane and 3- TSL 8330 is 1: (2~4).
3. preparation method according to claim 1, which is characterized in that in the step (1) metal powder be copper powder, iron powder,
Bronze or silver powder, the partial size of the metal powder are 0.1~2 μm.
4. preparation method according to any one of claims 1 to 3, which is characterized in that surface modification in the step (1)
Detailed process is as follows:
Heat after the metal powder, coating material and organic solvent are mixed, obtains the metal of surface modification
Powder.
5. the preparation method according to claim 4, which is characterized in that the mass ratio of the metal powder and coating material is
(1~5): (2~10)；
The organic solvent is the mixture of toluene and isobutanol, and the volume ratio of the toluene and isobutanol is (2~4): (1~
3)；
The mass ratio of the coating material and organic solvent is (1~5): 100.
6. the preparation method according to claim 4, which is characterized in that the temperature of the heat treatment is 50~80 DEG C, when
Between for 20~for 24 hours.
7. preparation method according to claim 1, which is characterized in that the metal powder of surface modification in the step (2)
Mass ratio with fluorographite is (5~10): 1；
The mass concentration of the hydrazine hydrate solution is 60~70%；
The volume of the hydrazine hydrate solution and the mass ratio of fluorographite are 1L: (5~10) g.
8. preparation method according to claim 1 or claim 7, which is characterized in that the temperature of reduction reaction is in the step (2)
80~100 DEG C, the time is 2~8h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113488624A (en) * | 2021-07-08 | 2021-10-08 | 中国恩菲工程技术有限公司 | Silicon-carbon composite material and preparation method and application thereof |
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