CN113897504A - Preparation method of metal-based graphene composite material and metal-based graphene electrical contact - Google Patents

Preparation method of metal-based graphene composite material and metal-based graphene electrical contact Download PDF

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CN113897504A
CN113897504A CN202010572579.4A CN202010572579A CN113897504A CN 113897504 A CN113897504 A CN 113897504A CN 202010572579 A CN202010572579 A CN 202010572579A CN 113897504 A CN113897504 A CN 113897504A
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metal
powder
based graphene
composite material
reaction chamber
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马瑜
吕雪超
沈晗睿
曹函星
钱天宝
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Shanghai Simbatt Energy Technology Co ltd
Zhejiang Chint Electrics Co Ltd
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Shanghai Simbatt Energy Technology Co ltd
Zhejiang Chint Electrics Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/05—Mixtures of metal powder with non-metallic powder
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/26—Deposition of carbon only
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/4418—Methods for making free-standing articles
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01H—ELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
    • H01H1/00—Contacts
    • H01H1/02—Contacts characterised by the material thereof
    • H01H1/021—Composite material
    • H01H1/027—Composite material containing carbon particles or fibres

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  • Metallurgy (AREA)
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  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Composite Materials (AREA)
  • Inorganic Chemistry (AREA)
  • Powder Metallurgy (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

A preparation method of a metal-based graphene composite material and a metal-based graphene electrical contact are provided, wherein the preparation method comprises the following steps: step S1: grinding and mixing graphene powder and metal powder to form mixed powder; step S2: and forming the metal-based graphene composite material by the mixed powder through a chemical vapor deposition method in an oxygen-free environment at 950-1050 ℃. The metal-based graphene electrical contact is formed by preparing a metal-based graphene composite material. The overall preparation process is simple and efficient, the prepared metal-based graphene composite material improves the performance of the original metal material, and the electric contact prepared from the material has excellent electric and thermal conductivity, oxidation resistance and corrosion resistance, so that the excellent performance of the electric contact in the use process is ensured.

Description

Preparation method of metal-based graphene composite material and metal-based graphene electrical contact
Technical Field
The invention relates to the technical field of electric contact materials, in particular to a preparation method of a metal-based graphene composite material and a metal-based graphene electric contact.
Background
The electric contact is widely used in the field of electric switches such as relays, contactors, circuit breakers and the like, is a key contact element in electric switches and instruments, and comprises an electric contact material for opening and closing and a sliding contact material which is in electrical contact and simultaneously slides along with machinery, and the reliability and the service life of switching electric appliances and related products are directly influenced by the performance of the electric contact material. The traditional medium-low voltage contact material mainly comprises Ag, the price of silver continuously rises along with the increasing exhaustion of precious metal resources, the labor cost is rapidly increased, and the rising trend of the cost of the electrical contact material cannot be reversed. To meet customer requirements, electrical contact manufacturers achieve cost reduction by improving production efficiency, digging cost reduction potential, and reducing scrap rates. The copper base replaces the silver base, has obvious advantages in cost and performance, and particularly introduces other elements to prepare the composite powder of copper and a second phase so as to improve the oxidation resistance of the copper alloy and improve the performance of the product, thereby becoming the development trend of modern copper base electric contacts. The micro-morphology and wettability of the second phase are of great importance, and the material of the second phase can be rare earth elements, metal oxides or carbon materials.
Graphene is the thinnest material found in the world at present and is sp which is a carbon atom2Two-dimensional films of hybrid orbital joints, the structure imparting graphiteThe graphene material has many characteristics, such as a forbidden band width close to zero, excellent electrical and thermal conductivity, a large specific surface area, very high carrier mobility and excellent mechanical properties, and the characteristics make the graphene an ideal reinforcement in the electrical contact material.
The traditional copper-based graphene material is complex in preparation process and complicated in procedure, and the finally formed copper-based graphene material cannot meet the requirements of an electric contact material, so that great hidden dangers are caused to an electric switch and an instrument. In addition, in the traditional preparation process of the copper-based graphene material, the anti-sintering agent is doped in the copper powder to avoid sintering and agglomeration of the copper powder, and the anti-sintering agent needs to be treated again subsequently to remove the anti-sintering agent in the product, so that the preparation process and the preparation cost of the copper-based graphene material are increased.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a simple and efficient preparation method capable of preparing a metal-based graphene composite material with excellent heat conduction and electric conductivity and a metal-based graphene electric contact.
In order to achieve the purpose, the invention adopts the following technical scheme: a preparation method of a metal-based graphene composite material comprises the following steps:
step S1: grinding and mixing graphene powder and metal powder to form mixed powder;
step S2: and growing a graphene film on the surface of the metal powder by using the mixed powder in an oxygen-free environment at 950-1050 ℃ by using a chemical vapor deposition method to form the metal-based graphene composite material.
Preferably, the metal powder in step S1 is one or more of copper powder and nickel powder.
Preferably, in the step S1, the graphene powder and the metal powder are ground and mixed by a ball mill, the grinding and mixing time of the ball mill is 3-12 hours, the ball-to-material ratio in the ball mill is 2: 1-10: 1, and the particle size of the metal powder is ground to 500 nm-75 μm.
Preferably, the content of the metal powder in the step S1 is 90 wt% to 99.5 wt%.
Preferably, the step S2 includes the steps of:
step S21: the mixed powder is put into a quartz carrier and sent into a reaction chamber of chemical vapor deposition equipment;
step S22: discharging oxygen in the reaction chamber, introducing protective gas, and heating to 950-1050 ℃;
step S23: introducing growth gas into the reaction chamber to enable the surface of the metal powder to grow to form a graphene film;
step S24: and after the reaction is finished, cooling to prepare the metal-based graphene composite material.
Preferably, the step S22 is: the reaction chamber was first evacuated to 1X10-2Introducing argon of 100-300 sccm into the reaction chamber to normal pressure below kPa to ensure that the reaction chamber is in a state of being filled with argon; and then, heating the reaction chamber at the speed of 10-20 ℃/min until the temperature in the reaction chamber reaches 950-1050 ℃, and preserving the heat.
Preferably, the growth gas in the step S23 is CH4And H2Said CH4The flow rate of (A) is 5-10 sccm, and the flow rate of (H) is2The flow rate of (A) is 20 to 40sccm, and the growth time in S23 is 0.5 to 1 hour.
The metal-based graphene electrical contact is prepared from any one of the metal-based graphene composite materials, and comprises graphene powder, metal powder and a graphene film formed by growing on the metal powder.
Preferably, the metal powder is one or more of copper powder and nickel powder.
According to the preparation method of the metal-based graphene composite material and the metal-based graphene electrical contact, the metal powder and the graphene powder are mixed as initial raw materials, the existing graphene powder is added, and the graphene film grows on the surface of the metal powder through a chemical vapor deposition method to prepare the metal-based graphene composite material. Furthermore, the metal-based graphene composite material is used for preparing and forming the electric contact, so that the performance of the original metal material is improved, and the prepared electric contact has better electrical performance and has the characteristics of oxidation resistance and corrosion resistance.
In addition, the mixed powder of the metal powder and the graphene powder is placed into a chemical vapor deposition device for co-sintering, the graphene powder has large specific surface area and good high-temperature stability, the metal powder can be well separated, and the anti-sintering agent does not need to be added into the metal powder, so that the metal powder is prevented from sintering and agglomerating, and the anti-sintering agent does not need to be cleaned subsequently.
The preparation method of the metal-based graphene composite material is simple in preparation process, and the prepared metal-based graphene electrical contact material is low in cost and can be used in large-scale industrial production.
Drawings
Fig. 1 is a raman spectrum of a copper-based graphene composite powder according to a first embodiment of the present invention;
fig. 2 is a field emission scanning electron microscope image of the copper-based graphene composite powder according to the first embodiment of the present invention;
FIG. 3 is a micrograph of a cross section of a copper-based graphene electrical contact according to an embodiment of the present invention;
FIG. 4 is a Raman spectrum of a nickel-based graphene composite according to a second embodiment of the present invention;
FIG. 5 is a scanning electron microscope image of a field emission of a nickel-based graphene composite material according to a second embodiment of the present invention;
FIG. 6 is a micrograph of a cross section of a nickel-based graphene electrical contact according to a second embodiment of the invention;
fig. 7 is a raman spectrum of the copper nickel-based graphene composite material in the third embodiment of the present invention;
fig. 8 is a field emission scanning electron microscope image of the copper nickel-based graphene composite material in the third embodiment of the present invention;
FIG. 9 is a micro-topography of a cross-section of a nickel-based graphene electrical contact according to a third embodiment of the invention.
Detailed Description
The following embodiments are provided to further illustrate the preparation method of the metal-based graphene composite material and the specific implementation of the metal-based graphene electrical contact. The preparation method of the metal-based graphene composite material and the metal-based graphene electrical contact of the present invention are not limited to the description of the following embodiments.
The preparation method of the metal-based graphene composite material comprises the following steps:
step S1: and grinding and mixing the graphene powder and the metal powder to form mixed powder.
Step S2: and growing a graphene film on the surface of the metal powder by using the mixed powder in an oxygen-free environment at 950-1050 ℃ by using a chemical vapor deposition method to form the metal-based graphene composite material.
Specifically, the metal powder can be copper powder, nickel powder or mixed metal powder of copper powder and nickel powder, and the content of the metal powder in the mixed powder is 90 wt% -99.5 wt%.
And step S1, putting the metal powder and the graphene powder into a ball mill in a ball milling mode, and grinding and mixing the metal powder and the graphene powder, wherein the grinding and mixing time of the ball mill is controlled to be 3-12 h, and the ball-to-material ratio is 2: 1-10: 1, so that the metal powder and the graphene powder are ground to be smaller in particle size and are uniformly mixed to form mixed powder, and the particle size of the ground metal powder in the mixed powder is 500 nm-75 microns. Of course, the method of grinding the metal powder and the graphene powder is not limited to the ball milling method, and other methods of grinding and mixing the metal powder and the graphene powder may be applied to the present invention.
According to the invention, the mixed powder of the metal powder and the graphene powder is put into a chemical vapor deposition device for co-sintering, the graphene powder is used as an anti-sintering agent, the specific surface area is large, the high-temperature stability is good, the metal powder can be well separated, other anti-sintering agents are not required to be added into the metal powder, the metal powder sintering agglomeration phenomenon is prevented, the quality of the thin-film graphene formed by subsequent growth is improved, the anti-sintering agent is not required to be cleaned subsequently, and the time and the cost of the whole process are saved. The preparation of this embodiment forms likepowder metal base graphite alkene combined material, makes things convenient for industrial-grade production, and the powder material that the production formed is convenient for encapsulate and preserve, is convenient for the post-processing.
And (5) placing the mixed powder formed in the step (S1) into a chemical vapor deposition device to prepare and form the metal-based graphene mixed powder according to the step (S2).
Step S2 specifically includes the following steps:
step S21: the mixed powder is loaded into a quartz carrier and sent into a reaction chamber of chemical vapor deposition equipment.
Besides the quartz carrier, graphite boat, ceramic boat, etc. can be used to hold the mixed powder.
Step S22: discharging oxygen in the reaction chamber, introducing protective gas, and heating to 950-1050 ℃.
The protective gas in the invention is argon, the reaction chamber is firstly vacuumized to 1x10-2And introducing 100-300 sccm of argon into the reaction chamber to normal pressure below kPa, and opening an exhaust valve of the chemical vapor deposition equipment to ensure that the reaction chamber is in a state of being filled with the argon. And then heating the reaction chamber at the speed of 10-20 ℃/min until the temperature in the reaction chamber reaches 950-1050 ℃, and preserving the heat.
Step S23: introducing growth gas into the reaction chamber to enable the surface of the metal powder to grow to form a graphene film;
specifically, the growth gas is CH4And H2In which CH4The flow rate of (A) is 5 to 10sccm, H2The flow rate of the silicon dioxide is 20-40 sccm, and the growth time is 0.5-1 h.
Step S24: and after the reaction is finished, cooling the reaction chamber to obtain the metal-based graphene composite material.
The copper-based graphene electrical contact is prepared by adopting the metal-based graphene composite material through processes of sample pressing, sintering, rolling, extruding and stamping, and the preparation processes of the sample pressing, sintering, rolling, extruding and stamping are the traditional preparation processes of the electrical contact, so that the details are not described herein. The metal-based graphene electrical contact is prepared, the total content of graphene and metal powder in the electrical contact is 100 wt%, wherein the content of the metal powder is 90 wt% -99.5 wt%, and the graphene powder added in the step S1 not only plays a role of an anti-sintering agent, but also is beneficial to improving the electrical conductivity and the thermal conductivity of the electrical contact.
The metal-based graphene composite material and the metal-based graphene electrical contact according to the present invention will be described in more detail in examples one to three.
Example one
The preparation method of the metal-based graphene composite material comprises the following specific steps:
step S1: and (2) putting the copper powder and the graphene powder into a planetary ball mill for grinding for 12 hours, wherein the ball material ratio is 2:1, grinding and mixing are uniformly carried out to form mixed powder, the particle size of the metal powder in the mixed powder is 500 nm-75 mu m, and the content of the copper powder is 94.5 wt%.
Step S21: the mixed powder is loaded into a quartz carrier and sent into a reaction chamber of chemical vapor deposition equipment.
Step S22: the reaction chamber was evacuated to 1x10-2And introducing 150sccm of argon to the reaction chamber under normal pressure, and opening an exhaust valve of the chemical vapor deposition equipment to ensure that the reaction chamber is in a state of being filled with the argon. Then the temperature of the reaction chamber is increased at a speed of 20 ℃/min until the temperature in the reaction chamber reaches 1000 ℃.
Step S23: CH is introduced into the reaction chamber4And H2In which CH4The flow rate of (2) is 5sccm, H2The flow rate of the reaction chamber is 40sccm, the temperature of the reaction chamber is kept for 0.5h, and the reaction is carried out to grow the surface of the copper powder to form a graphene film.
Step S24: after the reaction is finished, CH is closed4And H2And cooling the reaction chamber to room temperature to prepare the copper-based graphene composite material.
The raman spectrogram of the copper-based graphene composite material prepared in the embodiment is shown in fig. 1, and the raman spectrogram can calculate the positions of 2D, G and a D peak and a peak area, so that the number of graphene layers is 2, the structural defects are few, and the quality is good. FIG. 2 is a scanning electron microscope image of the copper-based graphene composite material, and it can be seen from the image that the coverage rate of graphene on the surface of copper powder is high.
The copper-based graphene electrical contact is formed by preparing the copper-based graphene composite material, the section of the prepared copper-based graphene electrical contact is shown in figure 3, and the total content of graphene and copper powder in the copper-based graphene electrical contact is 100 wt%. According to the calculation according to the raw materials and the product quality, the copper powder content in the copper-based graphene electrical contact in the embodiment is 94.5%.
Through detection, the resistivity of the prepared copper-based graphene electrical contact is 1.6x10-6Omega cm, the thermal conductivity is 398 w/m.k, and compared with pure copper, the copper-based graphene electric contact has better electric conduction and heat conduction performance.
Example two
The preparation method of the metal-based graphene composite material comprises the following specific steps:
step S1: putting the nickel powder and the graphene powder into a planetary ball mill for grinding for 3 hours, wherein the ball-material ratio is 10:1, grinding and mixing uniformly to form mixed powder, wherein the particle size of the metal powder in the mixed powder is 500 nm-75 mu m, and the content of the nickel powder is 93 wt%.
Step S21: the mixed powder is loaded into a quartz carrier and sent into a reaction chamber of chemical vapor deposition equipment.
Step S22: the reaction chamber was evacuated to 1x10-2And introducing 100sccm of argon to the reaction chamber under normal pressure, and opening an exhaust valve of the chemical vapor deposition equipment to ensure that the reaction chamber is in a state of being filled with the argon. Then the temperature of the reaction chamber is increased at a speed of 10 ℃/min until the temperature in the reaction chamber reaches 1050 ℃.
Step S23: CH is introduced into the reaction chamber4And H2In which CH4The flow rate of (2) is 10sccm, H2The flow rate of the reaction chamber is 30sccm, the reaction chamber is insulated for 1h, and reaction is carried out, so that the graphene film is formed on the surface of the nickel powder.
Step S24: after the reaction is finished, CH is closed4And H2And cooling the reaction chamber to room temperature to obtain the nickel-based graphene composite material.
The raman spectrogram of the nickel-based graphene composite material prepared by the embodiment is shown in fig. 4, and the number of graphene layers is 5-9, the number of structural defects is less, and the quality is better as can be seen from the positions of 2D, G and a D peak in the raman spectrogram and the calculation of a peak area. Fig. 5 is a scanning electron microscope image of the nickel-based graphene composite material, and it can be seen from the image that the coverage rate of graphene on the surface of nickel powder is high.
The nickel-based graphene composite material is prepared into the nickel-based graphene electrical contact through the processes of sample pressing, sintering, rolling, extruding and stamping, the section of the nickel-based graphene electrical contact is shown in fig. 6, and the total content of graphene and nickel powder in the nickel-based graphene electrical contact is 100 wt%. According to the raw materials and the product quality, the content of the nickel powder in the nickel-based graphene electrical contact in the embodiment is 93%.
Through detection, the resistivity of the prepared nickel-based graphene electrical contact is 1.6x10-6Omega cm, the thermal conductivity is 131w/m k, and compared with pure nickel, the nickel-based graphene electric contact has better electric conduction and heat conduction performance.
EXAMPLE III
The preparation method of the metal-based graphene composite material comprises the following specific steps:
step S1: and (2) putting the copper powder, the nickel powder and the graphene powder into a planetary ball mill for grinding for 6 hours, wherein the ball material ratio is 5:1, grinding and mixing are uniformly carried out to form mixed powder, the particle size of the metal powder in the mixed powder is 500 nm-75 mu m, the total content of the copper powder and the nickel powder is 92.5 wt%, and the ratio of the copper powder to the nickel powder is 1: 1.
Step S21: the mixed powder is loaded into a quartz carrier and sent into a reaction chamber of chemical vapor deposition equipment.
Step S22: the reaction chamber was evacuated to 1x10-2And introducing 300sccm of argon to the reaction chamber under normal pressure, and opening an exhaust valve of the chemical vapor deposition equipment to ensure that the reaction chamber is in a state of being filled with the argon. Then the temperature of the reaction chamber is increased at a speed of 15 ℃/min until the temperature in the reaction chamber reaches 950 ℃.
Step S23: CH is introduced into the reaction chamber4And H2In which CH4The flow rate of (2) is 8sccm, H2The flow rate of the reaction chamber is 20sccm, the reaction chamber is insulated for 50min, and reaction is carried out to grow the surface of the copper powder and the nickel powder to form the graphene film.
Step S24: after the reaction is finished, CH is closed4And H2And cooling the reaction chamber to room temperature to obtain the copper-nickel-based graphene composite material.
The raman spectrogram of the copper-nickel-based graphene composite material prepared by the embodiment is shown in fig. 7, and the raman spectrogram can calculate the positions of peaks 2D, G and D and the peak area, so that the number of graphene layers is 6-10, the number of structural defects is few, and the quality is good. FIG. 8 is a scanning electron microscope image of the copper-nickel-based graphene composite material, and it can be seen that the coverage rate of graphene on the surfaces of copper powder and nickel powder is high. In this embodiment, the ratio of copper powder to nickel powder is 1:1, but the amount of copper powder may be greater or less than that of nickel powder.
The copper-nickel-based graphene composite material is prepared into the copper-nickel-based graphene electrical contact through the processes of sample pressing, sintering, rolling, extruding and stamping, the section of the copper-nickel-based graphene electrical contact is shown in fig. 9, and the total content of graphene, nickel powder and copper powder in the copper-nickel-based graphene electrical contact is 100 wt%. According to the raw materials and the product quality, the total content of the copper powder and the nickel powder in the copper-nickel-based graphene electrical contact is 92.5%.
The resistivity of the prepared and formed copper-nickel-based graphene electric contact is detected to be 2.1x10-6Omega cm, the thermal conductivity is 330w/m k, and the electric and thermal conductivity of the copper-nickel-based graphene electric contact is between that of pure copper and pure nickel.
Example four
The preparation process of the metal-based graphene composite material in this embodiment is the same as that in this embodiment, except that the total content of copper powder and nickel powder in the copper-nickel-based graphene electrical contact in this embodiment is 90 wt%.
The resistivity of the prepared and formed copper-nickel-based graphene electric contact is detected to be 2.3x10-6Omega cm, the thermal conductivity is 220w/m k, and the electric conductivity and the thermal conductivity of the copper-nickel-based graphene electric contact are between those of pure copper and pure nickel.
EXAMPLE five
The preparation process of the metal-based graphene composite material in this embodiment is the same as that in this embodiment, except that the total content of copper powder and nickel powder in the copper-nickel-based graphene electrical contact in this embodiment is 99.5 wt%.
The resistivity of the prepared and formed copper-nickel-based graphene electric contact is detected to be 2.2x10-6Omega cm, 250w/m k thermal conductivity, and electric conduction and heat conduction of copper-nickel-based graphene electric contactThe chemical property is between that of pure copper and pure nickel.
The first to fifth embodiments show that the preparation method of the metal-based graphene electrical contact is simple in overall process, the process is easy to control, and the coverage rate of the metal surface graphene in the prepared metal-based graphene material is high and the material quality is high. The metal-based graphene material is adopted to prepare the electric contact, so that the cost is low, the electric conduction and heat conduction performance is excellent, and the excellent performance of the electric contact in the use process is ensured.
As shown by comparing the first embodiment with the fifth embodiment, the copper-based graphene composite material prepared by copper powder has the most excellent material performance, the electrical contact prepared by the copper-based graphene composite material has the most excellent performance,
the foregoing is a more detailed description of the invention in connection with specific preferred embodiments and it is not intended that the invention be limited to these specific details. For those skilled in the art to which the invention pertains, several simple deductions or substitutions can be made without departing from the spirit of the invention, and all shall be considered as belonging to the protection scope of the invention.

Claims (9)

1. A preparation method of a metal-based graphene composite material is characterized by comprising the following steps:
step S1: grinding and mixing graphene powder and metal powder to form mixed powder;
step S2: and growing a graphene film on the surface of the metal powder by using the mixed powder in an oxygen-free environment at 950-1050 ℃ by using a chemical vapor deposition method to form the metal-based graphene composite material.
2. The method for preparing the metal-based graphene composite material according to claim 1, wherein the metal powder in the step S1 is one or more of copper powder and nickel powder.
3. The preparation method of the metal-based graphene composite material according to claim 1, wherein in the step S1, the graphene powder and the metal powder are ground and mixed by a ball mill, the grinding and mixing time of the ball mill is 3-12 h, the ball-to-material ratio in the ball mill is 2: 1-10: 1, and the particle size of the metal powder is ground to 500 nm-75 μm.
4. The method for preparing the metal-based graphene composite material according to claim 1, wherein the content of the metal powder in the step S1 is 90 wt% to 99.5 wt%.
5. The method for preparing a metal-based graphene composite material according to claim 1, wherein the step S2 includes the steps of:
step S21: the mixed powder is put into a quartz carrier and sent into a reaction chamber of chemical vapor deposition equipment;
step S22: discharging oxygen in the reaction chamber, introducing protective gas, and heating to 950-1050 ℃;
step S23: introducing growth gas into the reaction chamber to enable the surface of the metal powder to grow to form a graphene film;
step S24: and after the reaction is finished, cooling to prepare the metal-based graphene composite material.
6. The method for preparing the metal-based graphene composite material according to claim 5, wherein the step S22 is: the reaction chamber was first evacuated to 1X10-2Introducing argon of 100-300 sccm into the reaction chamber to normal pressure below kPa to ensure that the reaction chamber is in a state of being filled with argon; and then, heating the reaction chamber at the speed of 10-20 ℃/min until the temperature in the reaction chamber reaches 950-1050 ℃, and preserving the heat.
7. The method for preparing a metal-based graphene composite material according to claim 5, wherein the growth gas in the step S23 is CH4And H2Said CH4The flow rate of (A) is 5-10 sccm, and the flow rate of (H) is2The flow rate of (A) is 20 to 40sccm, and the growth time in S23 is 0.5 to 1 hour.
8. A metal-based graphene electrical contact, comprising: the metal-based graphene electrical contact is prepared from the metal-based graphene composite material as claimed in any one of claims 1 to 7, and comprises graphene powder, metal powder and a graphene film grown on the metal powder.
9. The metal-based graphene electrical contact according to claim 8, wherein the metal powder is one or more of copper powder and nickel powder.
CN202010572579.4A 2020-06-22 2020-06-22 Preparation method of metal-based graphene composite material and metal-based graphene electrical contact Pending CN113897504A (en)

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