CN106807606A - A kind of graphene composite film and preparation method thereof - Google Patents
A kind of graphene composite film and preparation method thereof Download PDFInfo
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- CN106807606A CN106807606A CN201710048251.0A CN201710048251A CN106807606A CN 106807606 A CN106807606 A CN 106807606A CN 201710048251 A CN201710048251 A CN 201710048251A CN 106807606 A CN106807606 A CN 106807606A
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- 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
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- 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
- C23C16/50—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 using electric discharges
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- 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
- C23C16/50—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 using electric discharges
- C23C16/511—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 using electric discharges using microwave discharges
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Abstract
The invention provides a kind of graphene composite film, the graphene composite film includes heat conduction basic unit and the graphene layer being arranged in the heat conduction basic unit；The material of the heat conduction basic unit is one or more in CNT, boron nitride nano-tube and nano silver wire.Due to nano material and the excellent heat conductivility of grapheme material, when for diode part, graphene layer is contacted the graphene composite film with chip, and heat conduction basic unit contacts with metallic matrix, can greatly improve the heat dispersion of electronic device.Present invention also offers a kind of preparation method of graphene composite film, the preparation method that the application is provided being capable of direct deposited graphite alkene laminated film on the metallic substrate, it is to avoid need to carry out the destruction that secondary transferring brings graphene-structured after preparing graphene film in the prior art.
Description
Technical field
The present invention relates to diode parts technical field, more particularly to a kind of graphene composite film and its preparation side
Method.
Background technology
Mixed type Schottky diode (MPS) has blocking voltage high, low-leakage current, faster switching speed, bigger
The a series of outstanding feature such as conducting electric current and smaller conducting voltage.For the MPS of vertical stratification, in device encapsulation structure
Metallic matrix not only acts as the effect of support to chip, and is one of electrode of chip operation.
As developing rapidly for third generation semiconductor technology, the power density of MPS are increasing, the heat of generation is increasingly
Many, junction temperature of chip rises rapidly, and when temperature exceedes maximum allowable temperature, MPS will be damaged because of overheat.
However, power-type MPS heat-sinking capabilities are completely dependent on metallic matrix in itself in the prior art, thermal conductivity factor is extremely low, difficult
To meet requirements of the MPS to heat dispersion.
The content of the invention
It is an object of the invention to provide the Graphene that a kind of graphene composite film and preparation method thereof, the present invention are provided
Laminated film has excellent heat conductivility, may be disposed between metallic matrix and chip, to improve the heat dispersion of MPS.
In order to realize foregoing invention purpose, the present invention provides following technical scheme：
The invention provides a kind of preparation method of graphene composite film, comprise the following steps：
In metal base surface coated with nano solution, the nano-solution is carbon nano-tube solution, boron nitride nano-tube is molten
One or more in liquid and nano silver wire solution；
Under an inert atmosphere, the solvent in the nano-solution is removed, obtains being coated with the composition metal base of heat conduction basic unit
Body；
Under the mixed atmosphere of hydrogen and inert gas, with organic vapors carbon source as raw material, in the composite metal matrices
Surface chemistry vapour deposition graphene layer, obtains the graphene composite film in metal base surface generation.
Preferably, the concentration of the nano-solution is 0.1~5mg/mL.
Preferably, the solvent in removing the nano-solution by way of heating, the temperature of the heating is 75~100
℃；
The time of the heating is 5~15 minutes.
Preferably, volume content of the hydrogen in mixed atmosphere is 10~30%；
The total flow of the hydrogen and inert gas is 90~110sccm.
Preferably, the organic vapors carbon source is one or more in gas phase alkane, gas-phase olefin and gas phase alkynes；
The flow of the organic vapors carbon source is 10~100sccm.
Preferably, the temperature of the chemical vapor deposition is 800~1000 DEG C；
The time of the chemical vapor deposition is 10~30 minutes.
Preferably, in the chemical vapor deposition processes, the gaseous mixture comprising hydrogen, inert gas and organic vapors carbon source
The gas pressure intensity of body is 500~650Pa.
Preferably, the chemical vapor deposition be plasma reinforced chemical vapour deposition method, radio-frequency power be 350~
450W。
Preferably, the chemical vapor deposition is Microwave Irradiation Assisted Chemical vapour deposition process, and microwave power is 750~850W,
Frequency is 2~3GHz.
Present invention also offers the graphene composite film that preparation method described in a kind of above-mentioned technical proposal is obtained, comprising leading
Hot radical layer and graphene layer；The material of the heat conduction basic unit is the one kind in CNT, boron nitride nano-tube and nano silver wire
Or it is several, the nano material in the heat conduction basic unit is embedded in graphene layer in whole or in part；The thickness of the heat conduction basic unit is 1
~100nm；The thickness of the graphene layer is 0.2~0.5nm.
The invention provides a kind of graphene composite film, the graphene composite film is comprising heat conduction basic unit and is arranged on
Graphene layer in the heat conduction basic unit；The material of the heat conduction basic unit is CNT, boron nitride nano-tube and nano silver wire
In one or more, nano material in the heat conduction basic unit is embedded in graphene layer in whole or in part.Due to nano material
The heat conductivility excellent with grapheme material, the graphene composite film when for diode part, graphene layer it is heavy
Product surface contacts with chip, and heat conduction basic unit and graphene layer bottom surface contact with metallic matrix, can greatly improve electronic device
Heat dispersion.
Present invention also offers a kind of preparation method of graphene composite film, the preparation method that the application is provided can be straight
The alkene laminated film of deposited graphite on the metallic substrate for connecing, it is to avoid need to carry out two after preparing graphene film in the prior art
It is secondary to shift the destruction brought to graphene-structured.
Brief description of the drawings
Fig. 1 is a kind of schematic diagram of graphene composite film concrete structure of the invention；
Fig. 2 is the Raman spectrum of the carbon-coating that the embodiment of the present invention 1 is obtained.
Specific embodiment
The invention provides a kind of preparation method of graphene composite film, comprise the following steps：
In metal base surface coated with nano solution, the nano-solution is carbon nano-tube solution, boron nitride nano-tube is molten
One or more in liquid and nano silver wire solution；
Under an inert atmosphere, the solvent in the nano-solution is removed, obtains being coated with the composition metal base of heat conduction basic unit
Body；
Under the mixed atmosphere of hydrogen and inert gas, with organic vapors carbon source as raw material, in the composite metal matrices
Surface chemistry vapour deposition graphene layer, obtains the graphene composite film in metal base surface generation.
In metal base surface coated with nano solution, the nano-solution is carbon nano-tube solution to the present invention, boron nitride is received
One or more in mitron solution and nano silver wire solution.In the present invention, the material of the metallic matrix be preferably copper,
Iron, nickel, platinum or corronil.Metallic matrix described in preferred pair of the present invention is cleaned, and the cleaning preferably comprises following steps：
Metallic matrix is sequentially cleaned in acetone, absolute ethyl alcohol and water；
After cleaning terminates, acid treatment is carried out in hydrochloric acid solution；
After acid treatment terminates, washed again, obtained pure metallic matrix.
The present invention does not have particular/special requirement to the implementation method of the cleaning, using cleaning well-known to those skilled in the art
Mode is carried out.
In the present invention, the volumetric concentration of the hydrochloric acid solution is preferably 5~15%, more preferably 8~13%, most preferably
It is 10%.In the present invention, the time of the acid treatment be preferably 3~7 minutes, more preferably 4~6 minutes, most preferably 5 points
Clock.
The present invention does not have particular/special requirement to the structure of the CNT and boron nitride nano-tube, can be specifically single wall
Or many walls.In the present invention, the diameter of the CNT be preferably 1~10nm, more preferably 2~8nm, most preferably 4~
6nmμm.In the present invention, the diameter of the boron nitride nano-tube is preferably 5~100nm, more preferably 20~80nm, most preferably
It is 40~60nm.In the present invention, the diameter of the nano silver wire is preferably 5~100nm, more preferably 20~80nm, optimal
Elect 65~70nm as.The present invention is not particularly limited to the source of the CNT, boron nitride nano-tube and nano silver wire, adopts
With above-mentioned substance well-known to those skilled in the art, the specific commercially available prod of specific material as described above.
In the present invention, the concentration of the nano-solution is preferably 0.1~5mg/mL, more preferably 1~4mg/mL, optimal
Elect 2~3mg/mL as.In the present invention, the solvent of the nano-solution is preferably water, ethanol or isopropanol.In the present invention,
The coating thickness of the nano-solution is directly related with the thickness of the heat conduction basic unit to be obtained, and is entered according to actual technical requirements
Row is set, and it is 1~100nm, preferably 20~80nm specifically to enable to the thickness of heat conduction basic unit for obtaining, more
Preferably 40~60nm.
The present invention does not have particular/special requirement to the mode of the coating, is coated using liquid well-known to those skilled in the art
Mode.In the present invention, the coating is preferably hand painting, spin coating or brushing.
After the coating, under an inert atmosphere, the solvent in removal nano-solution obtains being coated with heat conduction basic unit the present invention
Composite metal matrices.The present invention preferably heating by way of remove nano-solution in solvent.In the present invention, it is described to add
The temperature of heat is preferably 75~100 DEG C, most preferably more preferably 80~90 DEG C, 85 DEG C；The time of the heating is preferably 5~
15 minutes, most preferably more preferably 6~12 minutes, 8~10 minutes.In the present invention, the inert atmosphere is preferably nitrogen
Or argon gas.
The present invention does not have special requirement to the arrangement mode of the nano material in the heat conduction basic unit, can be according to any
Mode arranged.In the present invention, the heat conduction basic unit is preferably the height of individual layer nano material, i.e., described heat conduction basic unit
Thickness be preferably the diameter of nano material.
After being coated with the composite metal matrices of heat conduction basic unit described in obtaining, the present invention is in hydrogen and the gaseous mixture of inert gas
Under atmosphere, with organic vapors carbon source as raw material, chemical vapor deposition graphene layer, obtains on the heat-conducting layer of the composite metal matrices
To the graphene composite film generated in metal base surface.In the present invention, the inert atmosphere is preferably nitrogen or argon gas.
In the present invention, volume content of the hydrogen in mixed atmosphere is preferably 10~30%, more preferably 15~25%, optimal
Elect 20% as；The total flow of the hydrogen and inert gas is preferably 90~110sccm, more preferably 95~105sccm, optimal
Elect 100sccm as.
In the present invention, the organic vapors carbon source is preferably the one kind in gas phase alkane, gas-phase olefin and gas phase alkynes
Or it is several.In the present invention, the gas phase alkane is preferably one or more in methane, ethane and propane；The gas phase alkene
Hydrocarbon is preferably ethene；The gas phase alkynes is preferably acetylene.In the present invention, the flow of the organic vapors carbon source is preferably 10
~100sccm, more preferably 20~80sccm, most preferably 40~60sccm.
In the present invention, the temperature of the chemical vapor deposition is preferably 800~1000 DEG C, more preferably 850~950
DEG C, most preferably 900 DEG C；The time of the chemical vapor deposition is preferably 10~30 minutes, more preferably 20~25 minutes, most
Preferably 22~23 minutes.In the present invention, in the chemical vapor deposition processes, comprising hydrogen, inert gas and organic gas
The gas pressure intensity of the mixed gas of phase carbon source be preferably 500~650Pa, more preferably 550~600Pa, most preferably 570~
580Pa。
In the present invention, the chemical vapor deposition is preferably plasma reinforced chemical vapour deposition method, its radio-frequency power
Preferably 350~450W, more preferably 380~430W, most preferably 400W.
In the present invention, the chemical vapor deposition is preferably Microwave Irradiation Assisted Chemical vapour deposition process, the microwave radiation technology
Microwave power is preferably 750~850W, more preferably 780~830W in chemical vapour deposition technique；The Microwave Irradiation Assisted Chemical gas
Frequency is preferably 2~3GHz, most preferably more preferably 2.2~2.6GHz, 2.45GHz in phase sedimentation.
Present invention also offers the graphene composite film that preparation method described in a kind of above-mentioned technical proposal is obtained, comprising leading
Hot radical layer and graphene layer；The material of the heat conduction basic unit is the one kind in CNT, boron nitride nano-tube and nano silver wire
Or it is several, the nano material in the heat conduction basic unit is embedded in graphene layer in whole or in part；The thickness of the heat conduction basic unit is 1
~100nm；The thickness of the graphene layer is 0.2~0.5nm.
In the present invention, the thickness of the heat conduction basic unit be 1~100nm, preferably 20~80nm, more preferably 40~
60nm；The thickness of the graphene layer is 0.2~0.5nm, more preferably preferably 0.25~0.45nm, 0.3~0.34nm.
A kind of schematic diagram of concrete structure of the graphene composite film that the present invention is provided is as shown in figure 1, Fig. 1 is the present invention
A kind of schematic diagram of graphene composite film concrete structure.Apparent in order to what is expressed, Graphene described in Fig. 1 of the present invention is answered
Film is closed to be arranged on metallic matrix, but the graphene composite film and not comprising metallic matrix part.Such as Fig. 1 institutes
Show, the graphene composite film includes nano material and Graphene two parts, the Graphene is filled in the nano material
Between.In Fig. 1, the Graphene is not completely covered nano material, but the specific schematic construction not represents Ben Fa
Bright all of graphene composite film.Specifically, Graphene can be complete described in the graphene composite film of present invention offer
Covering not exclusively covers the nano material.
Graphene composite film provided the present invention with reference to embodiment and preparation method thereof is described in detail,
But they can not be interpreted as limiting the scope of the present invention.
Embodiment 1
Copper base is put into ultrasonic oscillation in acetone to process 2 minutes, is put into afterwards in absolute ethyl alcohol at ultrasonic oscillation
Reason 2 minutes, is put into the salt acid soak 5 minutes that volumetric concentration is 10% after then being rinsed with deionized water, finally use deionized water
Rinsing copper base.
The carbon nano-tube aqueous solutions of 5mg/ml are spun to the surface of the copper base of above-mentioned gained, control the thickness of coating big
About single-layer carbon nano-tube.Then put and dried on 100 DEG C of hot dry plates in a nitrogen environment 10min to remove copper-based plate surface
Solvent.
Above-mentioned gained copper base is placed in PECVD reative cells (contacted with chip faces up), reaction is evacuated to
Pressure is down to below 1Pa in room, is passed through hydrogen/argon gas mixed gas (hydrogen 30%) to normal pressure, after repeating this step 3 time, control
Mixed gas flow processed is 100sccm, is warming up to 800 DEG C, and adjustment radio-frequency power supply power is that 400W produces homogeneous tube plasma glow,
It is passed through carbon source presoma CH4, flow is 100sccm, is kept for 15 minutes under pressure 500Pa, before growth cuts off carbon source after finishing
Body is driven, keeps mixed gas flow velocity constant, be cooled to room temperature, obtain the graphene composite film generated on copper base.
The present invention has carried out Raman spectrum detection to the carbon-coating that the present embodiment deposition is obtained, and testing result is as shown in Figure 2.Figure
2 is the Raman spectrum of the carbon-coating that the embodiment of the present invention 1 is obtained, and as shown in Figure 2, the carbon-coating for obtaining is graphene-structured.
Embodiment 2
Copper base is put into ultrasonic oscillation in acetone to process 2 minutes, is put into afterwards in absolute ethyl alcohol at ultrasonic oscillation
Reason 2 minutes, is put into the salt acid soak 5 minutes that volumetric concentration is 10% after then being rinsed with deionized water, finally use deionized water
Rinsing copper base.
The carbon nano-tube aqueous solutions of 5mg/ml are spun to the surface of the copper base of above-mentioned gained, control the thickness of coating big
About single-layer carbon nano-tube.Then put and dried on 100 DEG C of hot dry plates in a nitrogen environment 10min to remove copper-based plate surface
Solvent.
Copper-based bottom after by cleaning is placed in CVD reative cells (contacted with chip faces up), is evacuated to reative cell
Middle pressure is down to below 1Pa, is passed through hydrogen/argon gas mixed gas (hydrogen 10%) to normal pressure, after repeating this step 3 time, control
Mixed gas flow is 100sccm, is warming up to 1000 DEG C, is passed through carbon source presoma C2H2, flow is 20sccm, under pressure 650Pa
Insulation 30 minutes, cuts off carbon source presoma, keeps mixed gas flow velocity constant, is cooled to room temperature, obtains being generated on copper base
Graphene composite film.
Embodiment 3
Ni substrate is put into ultrasonic oscillation in acetone to process 2 minutes, is put into afterwards in absolute ethyl alcohol at ultrasonic oscillation
Reason 2 minutes, is put into the salt acid soak 5 minutes that volumetric concentration is 10% after then being rinsed with deionized water, finally use deionized water
Rinsing ni substrate.
The carbon nano-tube aqueous solutions of 5mg/ml are spun to the surface of the ni substrate of above-mentioned gained, control the thickness of coating big
About single-layer carbon nano-tube.Then put and dried on 100 DEG C of hot dry plates in a nitrogen environment 10min to remove Ni-based plate surface
Solvent.
Above-mentioned gained ni substrate is placed in PECVD reative cells (contacted with chip faces up), reaction is evacuated to
Pressure is down to below 1Pa in room, is passed through hydrogen/argon gas mixed gas (hydrogen 30%) to normal pressure, after repeating this step 3 time, control
Mixed gas flow processed is 100sccm, is warming up to 800 DEG C, and adjustment radio-frequency power supply power is that 400W produces homogeneous tube plasma glow,
It is passed through carbon source presoma CH4, flow is 15sccm, is kept for 20 minutes under pressure 500Pa, and growth cuts off carbon source forerunner after finishing
Body, keeps mixed gas flow velocity constant, is cooled to room temperature, obtains the graphene composite film generated on ni substrate.
Embodiment 4
Ni substrate is put into ultrasonic oscillation in acetone to process 2 minutes, is put into afterwards in absolute ethyl alcohol at ultrasonic oscillation
Reason 2 minutes, is put into the salt acid soak 5 minutes that volumetric concentration is 10% after then being rinsed with deionized water, finally use deionized water
Rinsing ni substrate.
The carbon nano-tube aqueous solutions of 5mg/ml are spun to the surface of the ni substrate of above-mentioned gained, control the thickness of coating big
About single-layer carbon nano-tube.Then put and dried on 100 DEG C of hot dry plates in a nitrogen environment 10min to remove Ni-based plate surface
Solvent.
Nickel substrate after cleaning is placed in CVD reative cells (contacted with chip faces up), reative cell is evacuated to
Middle pressure is down to below 1Pa, is passed through hydrogen/argon gas mixed gas (hydrogen 10%) to normal pressure, after repeating this step 3 time, control
Mixed gas flow is 100sccm, is warming up to 1000 DEG C, is passed through carbon source presoma C2H2, flow is 10sccm, under pressure 600Pa
Insulation 20 minutes, cuts off carbon source presoma, keeps mixed gas flow velocity constant, is cooled to room temperature, obtains being generated on ni substrate
Graphene composite film.
Embodiment 5
Ultrasonic oscillation is processed 2 minutes during corronil substrate is put into acetone, and ultrasonic wave in absolute ethyl alcohol is put into afterwards
Concussion treatment 2 minutes, is put into the salt acid soak 5 minutes that volumetric concentration is 10% after then being rinsed with deionized water, finally spend
Ionized water rinses corronil substrate.
The carbon nano-tube aqueous solutions of 5mg/ml are spun to the surface of the corronil substrate of above-mentioned gained, control coating
Thickness is about single-layer carbon nano-tube.Then put and dried on 100 DEG C of hot dry plates in a nitrogen environment 10min to remove cupro-nickel
The solvent on alloy substrate surface.
Above-mentioned gained corronil substrate is placed in PECVD reative cells (contacted with chip faces up), is vacuumized
Pressure is down to below 1Pa into reative cell, is passed through hydrogen/argon gas mixed gas (hydrogen 30%) to normal pressure, repeats this step 3 time
Afterwards, mixed gas flow is controlled for 100sccm, 800 DEG C are warming up to, and adjustment radio-frequency power supply power is that 400W produces homogeneous tube plasma
Aura, is passed through carbon source presoma CH4, flow is 25sccm, is kept for 10 minutes under pressure 550Pa, and growth cuts off carbon after finishing
Source presoma, keeps mixed gas flow velocity constant, is cooled to room temperature, and the Graphene for obtaining being generated on corronil substrate is combined
Film.
Embodiment 6
Ultrasonic oscillation is processed 2 minutes during corronil substrate is put into acetone, and ultrasonic wave in absolute ethyl alcohol is put into afterwards
Concussion treatment 2 minutes, is put into the salt acid soak 5 minutes that volumetric concentration is 10% after then being rinsed with deionized water, finally spend
Ionized water rinses corronil substrate.
The carbon nano-tube aqueous solutions of 5mg/ml are spun to the surface of the corronil substrate of above-mentioned gained, control coating
Thickness is about single-layer carbon nano-tube.Then put and dried on 100 DEG C of hot dry plates in a nitrogen environment 10min to remove cupro-nickel
The solvent on alloy substrate surface.
Corronil substrate after cleaning is placed in CVD reative cells (contacted with chip faces up), is evacuated to
Pressure is down to below 1Pa in reative cell, is passed through hydrogen/argon gas mixed gas (hydrogen 10%) to normal pressure, repeats this step 3 time
Afterwards, control mixed gas flow for 100sccm, be warming up to 1000 DEG C, be passed through carbon source presoma C2H2, flow is 15sccm, pressure
10 minutes are incubated under 620Pa, carbon source presoma is cut off, keep mixed gas flow velocity constant, be cooled to room temperature, obtain being closed in cupro-nickel
The graphene composite film generated on gold base.
As seen from the above embodiment, the invention provides a kind of graphene composite film, the graphene composite film bag
Basic unit containing heat conduction and the graphene layer being arranged in the heat conduction basic unit；The material of the heat conduction basic unit is CNT, nitridation
One or more in boron nanotube and nano silver wire.It is described due to nano material and the excellent heat conductivility of grapheme material
When for diode part, graphene layer is contacted graphene composite film with chip, and heat conduction basic unit contacts with metallic matrix, energy
Enough greatly improve the heat dispersion of electronic device.
Present invention also offers a kind of preparation method of graphene composite film, the preparation method that the application is provided can be straight
The alkene laminated film of deposited graphite on the metallic substrate for connecing, it is to avoid need to carry out two after preparing graphene film in the prior art
It is secondary to shift the destruction brought to graphene-structured.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of preparation method of graphene composite film, comprises the following steps：
In metal base surface coated with nano solution, the nano-solution be carbon nano-tube solution, boron nitride nano-tube solution and
One or more in nano silver wire solution；
Under an inert atmosphere, the solvent in the nano-solution is removed, obtains being coated with the composite metal matrices of heat conduction basic unit；
Under the mixed atmosphere of hydrogen and inert gas, with organic vapors carbon source as raw material, on the composite metal matrices surface
Chemical vapor deposition graphene layer, obtains the graphene composite film in metal base surface generation.
2. preparation method according to claim 1, it is characterised in that the concentration of the nano-solution is 0.1~5mg/mL.
3. preparation method according to claim 1 and 2, it is characterised in that it is molten by way of heating to remove the nanometer
Solvent in liquid, the temperature of the heating is 75~100 DEG C；
The time of the heating is 5~15 minutes.
4. preparation method according to claim 1, it is characterised in that volume content of the hydrogen in mixed atmosphere be
10~30%；
The total flow of the hydrogen and inert gas is 90~110sccm.
5. preparation method according to claim 1, it is characterised in that the organic vapors carbon source is gas phase alkane, gas phase
One or more in alkene and gas phase alkynes；
The flow of the organic vapors carbon source is 10~100sccm.
6. preparation method according to claim 1, it is characterised in that the temperature of the chemical vapor deposition is 800~
1000℃；
The time of the chemical vapor deposition is 10~30 minutes.
7. preparation method according to claim 1, it is characterised in that in the chemical vapor deposition processes, comprising hydrogen,
The gas pressure intensity of the mixed gas of inert gas and organic vapors carbon source is 500~650Pa.
8. the preparation method according to claim 4~7 any one, it is characterised in that the chemical vapor deposition for etc.
Plasma enhanced chemical vapor sedimentation, radio-frequency power is 350~450W.
9. the preparation method according to claim 4~7 any one, it is characterised in that the chemical vapor deposition is micro-
Ripple auxiliary chemical vapor deposition method, microwave power is 750~850W, and frequency is 2~3GHz.
10. the graphene composite film that preparation method described in claim 1~9 any one is obtained, comprising heat conduction basic unit and stone
Black alkene layer；The material of the heat conduction basic unit is one or more in CNT, boron nitride nano-tube and nano silver wire, described
Nano material in heat conduction basic unit is embedded in graphene layer in whole or in part；The thickness of the heat conduction basic unit is 1~100nm；Institute
The thickness for stating graphene layer is 0.2~0.5nm.
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| CN108548852A (en) * | 2018-06-27 | 2018-09-18 | 北京镭硼科技有限责任公司 | A kind of graphene-based film-type hydrogen gas sensor and preparation method thereof |
| CN109520339A (en) * | 2017-09-19 | 2019-03-26 | 逢甲大学 | Graphene temperature equalization plate structure and manufacturing method thereof |
| CN109534314A (en) * | 2017-09-22 | 2019-03-29 | 中国科学院物理研究所 | The preparation method of carbon nanocapsule thin film/nano-micrometer network combined film and fiber |
| CN109534315A (en) * | 2017-09-22 | 2019-03-29 | 中国科学院物理研究所 | A kind of amorphous carbon/nano-micrometer network thin-film and preparation method thereof |
| CN111283334A (en) * | 2020-03-18 | 2020-06-16 | 常熟通乐电子材料有限公司 | Processing technology of composite heating body |
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| CN114639508A (en) * | 2020-12-15 | 2022-06-17 | 安徽宇航派蒙健康科技股份有限公司 | Method for preparing high-temperature-resistant electric heating device based on transparent conductive film |
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