CN107313102B - A kind of preparation method of aluminium base graphene, carbon nanotube composite heat dissipation material - Google Patents
A kind of preparation method of aluminium base graphene, carbon nanotube composite heat dissipation material Download PDFInfo
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- CN107313102B CN107313102B CN201710532799.2A CN201710532799A CN107313102B CN 107313102 B CN107313102 B CN 107313102B CN 201710532799 A CN201710532799 A CN 201710532799A CN 107313102 B CN107313102 B CN 107313102B
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- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
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- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
Abstract
The present invention relates to the preparation methods of a kind of aluminium base graphene, carbon nanotube composite heat dissipation material, belong to the preparation technical field of heat sink material, this method comprises: equivalent graphene, carbon nanotube powder and aluminium salt are added in ethanol solution, and the mixing electrophoresis liquid of evenly dispersed graphene, carbon nanotube is obtained with ultrasonic wave dispersion;Using aluminium base thin slice, after being surface-treated with dust technology, deionized water, dehydrated alcohol and ultrasonic wave, as cathode;Using graphite flake as anode, cathode and anode are immersed in together in mixing electrophoresis liquid and carry out electrophoretic deposition;Then by aluminium base thin slice from one end laminated multi-layer, and cold moudling, a circle will be wrapped up in outside the sample of compression moulding with the other end and be fixedly welded on its side, then make annealing treatment in a nitrogen atmosphere, to obtain aluminium base graphene, carbon nanotube composite heat dissipation material.The method of the present invention simple process, energy conservation and environmental protection, at low cost, the radiating efficiency of the composite heat dissipation material of preparation is high, mechanical strength is big.
Description
Technical field
The invention belongs to the preparation technical fields of heat sink material, multiple more particularly to a kind of aluminium base graphene, carbon nanotube
Close the preparation method of heat sink material.
Background technique
Electronics, electrical component, high power optical devices microprocessor and integrated circuit in generally can all generate it is very high
Heat, if these electronic components generate heat be more than its allow range, shadow not only is caused to their own performance
Ring, and may performance to whole system and stabilization cause immeasurable damage, so as to cause the collapse of system.And it is electric
The temperature of son, the performance of electrical equipment, reliability and service life and running environment is inversely.For example, high-capacity LED or liquid crystal
In module, the raising of substrate radiating rate can greatly improve their brightness, service life and the stability of operation.Therefore, it is
The performance and stability for improving electronic component and its system, prolong its service life, reduce the environment temperature of operation extremely
Important, this relies primarily on the raising of radiator heat-dissipation speed.Since alumina-base material has, light-weight (density is in the prior art
2.7g/cm3), thermal coefficient high (thermal conductivity about 200W/mk), anti-corrosion property can be good, cheap the features such as, be widely used in
Computer, air-conditioning, mobile phone, LED illumination, communication, rectifier, a variety of field of radiating such as medical treatment and industrial equipment.But as electronics produces
The continuous renewal of product and the promotion of performance, the requirement to original heat sink material radiating rate are also increasingly strict.
Graphene is a kind of ultralight, ultra-thin, superpower and extra specific surface area quasi- two-dimensional material, surface density about 0.77mg/
m2, the thickness of single-layer graphene about 0.34nm, the toughness of graphene is fabulous, elasticity modulus 1.0TPa, and microstrength is reachable
30GPa is more than 100 times of traditional steel, theoretical specific surface area 2630m2/ g, and there is very high conductive, thermal conductivity
Can, if resistivity is 2 × 10-6Ω .cm, electron mobility is up to 2 × 105cm2/ V.S, horizontal thermal conductivity is about 5 at room temperature
×103W/m.K.Meanwhile graphene has high thermal stability, chemical stability and excellent permeability resistance and wear resistence
Energy.Therefore, graphene has been owned by each field such as mechanics, electronics, optics, calorifics and new energy be widely applied before
Scape has especially attracted the extensive concern of people in terms of the synthesis application of heat sink material.
It adds graphene or carbon nanotube in right amount in alumina-base material, its heat dissipation performance, mechanical property can be effectively improved
Energy and electric property etc..Graphene or carbon nanotube and the synthetic method of aluminum matrix composite have in the prior art: 1, in aluminium
Graphene coated or carbon nanotube thermal dispersant coatings on sill surface;2, solid powder synthetic method;3, refining method etc. altogether is melted.But
Since graphene and carbon nanotube are all easier to reunite, there is graphene and carbon nanometer in the composite material of above method preparation
Pipe dispersion is uneven or tends to the problems such as inconsistent, so as to cause the heat dissipation effect for reducing graphene or carbon nano tube compound material
Fruit.In addition to this, organic coating is often utilized between graphene or carbon nanotube and metal base surface in the first method
It is bonded, and the thermal coefficient of general organic coating is all very low, be unfavorable for the raising of heat dissipation performance.Latter two method is to improve
The common method of aluminum matrix composite comprehensive performance, but technique is more complex, and time consumption and energy consumption is all very big, especially in the third method
High temperature burns the reduction for being also possible to phenomena such as generating oxidation or interfacial reaction when refining and leading to material property.
Summary of the invention
Present invention aims at for the problems of in the prior art, proposing a kind of aluminium base graphene, carbon nanotube
The preparation method of composite heat dissipation material, this method preparation process is simple, energy conservation and environmental protection, it is at low cost and, good heat dissipation effect.
To achieve the above object, the present invention adopts the following technical scheme:
The preparation method of a kind of aluminium base graphene, carbon nanotube composite heat dissipation material, which is characterized in that including following step
It is rapid:
(1) graphene powder and carbon nanotube of equivalent are respectively put into ethanol solution, being made into concentration is 0.02
The mixed liquor of the graphene of~0.1mg/ml, carbon nanotube, adds aluminum salt solution, and being made into aluminium salt concentration is 0.4~4mg/ml
Aluminium salt graphene, carbon nanotube mixed liquor, then with ultrasonic wave disperse 3~5h, obtain evenly dispersed aluminium salt graphene, carbon is received
The mixing electrophoresis liquid of mitron;
(2) will be 5~10 minutes ultrasonic in ethanol solution with a thickness of the aluminum or aluminum alloy thin slice of 0.01~0.1mm,
It is repeatedly rinsed with after 0.5~1min of immersion in 5~8% dust technology with deionized water again, after drying, as cathode;
(3), as anode, the cathode and the anode to be immersed in together with the comparable graphite flake of the cathode size
The aluminium salt graphene, carbon nanotube mixing electrophoresis liquid under the DC electric field of 60~100V/cm carry out electrophoretic deposition 1~
8min;
(4) cathode is taken out, with hydraulic forming machine cold pressing 10~sample is made for 24 hours after laminated multi-layer from the cathode one end
Then the other end of the cathode is wrapped up a circle wherein the superposition number of plies is 300 layers or more by product outside the sample of compression moulding
After be fixedly welded on its side;
(5) 3~5h is handled with 450~550 DEG C of annealing temperature in a nitrogen atmosphere, after Temperature fall, can be obtained
The aluminium base graphene, carbon nanotube composite heat dissipation material.
The preparation method of aluminium base graphene according to the present invention, carbon nanotube composite heat dissipation material, which is characterized in that described
Graphene powder is the single layer or few layer graphene by CVD method growth, and the graphene powder partial size is 10~30 microns, thickness
For 2nm hereinafter, the carbon nanotube is multi-walled carbon nanotube, the length of the multi-walled carbon nanotube is 5~30 microns, and diameter is
10nm is hereinafter, the graphene and the deposition thickness of carbon nanotube are 20nm or less.
The preparation method of aluminium base graphene according to the present invention, carbon nanotube composite heat dissipation material, which is characterized in that described
Aluminium salt is aluminum nitrate or aluminum sulfate.
Technical effect of the invention
According to the technique and scheme of the present invention, it is capable of providing that a kind of radiating efficiency is high, mechanical strength is big, simple process, energy conservation
Aluminium base graphene environmentally friendly, at low cost, carbon nanotube composite heat dissipation material and preparation method thereof.Heat sink material of the invention, no
Containing organic matter, it is inconsistent and be unevenly distributed that the trend of graphene and carbon nanotube in the composite can be efficiently solved
Problem, but also can control the deposition thickness of graphene and carbon nanotube, to increase substantially conventional metals heat sink material
Coefficient of heat transfer.Using aluminium base graphene provided by the present invention, carbon nanotube composite heat dissipation material, electricity can be promptly reduced
The operating ambient temperature of brain, air-conditioning, mobile phone, LED illumination, communication, rectifier, medical treatment and industrial equipment, improves its radiating efficiency,
Extend the service life of equipment.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of aluminium base graphene prepared by the method for the present invention, carbon nanotube composite heat dissipation material.
Fig. 2 is that aluminium base graphene provided by the present invention, the graphene of carbon nanotube composite heat dissipation material, carbon nanotube are multiple
Close layer surface scanning electron microscope diagram.
Specific embodiment
Elaboration by the following examples, the preparation to aluminium base graphene, carbon nanotube composite heat dissipation material of the invention
Method is described in detail.
Embodiment 1:
The preparation method of a kind of aluminium base graphene, carbon nanotube composite heat dissipation material, which is characterized in that including following step
It is rapid:
(1) graphene powder and carbon nanotube of equivalent are respectively put into ethanol solution, being made into concentration is
The mixed liquor of the graphene of 0.02mg/ml, carbon nanotube, adds aluminum salt solution, is made into the aluminium that aluminium salt concentration is 0.6mg/ml
Salt graphene, carbon nanotube mixed liquor, then disperse 3h with ultrasonic wave, obtain evenly dispersed aluminium salt graphene, carbon nanotube
Mix electrophoresis liquid;
(2) will be 10 minutes ultrasonic in ethanol solution with a thickness of the aluminum slice of 0.01mm, then in 5% dust technology
It is repeatedly rinsed after impregnating 0.5min with deionized water, after drying, as cathode;
(3), as anode, the cathode and the anode to be immersed in together with the comparable graphite flake of the cathode size
The aluminium salt graphene, carbon nanotube mixing electrophoresis liquid under the DC electric field of 100V/cm carry out electrophoretic deposition 1min;
(4) cathode is taken out, sample is made with hydraulic forming machine cold pressing 10h after laminated multi-layer from the cathode one end,
Wherein the superposition number of plies is 3000 layers or more, then by the other end of the cathode after one circle of package outside the sample of compression moulding
It is fixedly welded on its side;
(5) 5h is handled with 450 DEG C of annealing temperature in a nitrogen atmosphere, after Temperature fall, the aluminium base can be obtained
Graphene, carbon nanotube composite heat dissipation material.
According to the preparation method of the aluminium base graphene of the present embodiment, carbon nanotube composite heat dissipation material, which is characterized in that institute
Stating graphene powder is the single layer or few layer graphene by CVD method growth, and the graphene powder partial size is 30 microns hereinafter, thick
Degree is 2nm hereinafter, the carbon nanotube is multi-walled carbon nanotube, and the length of the multi-walled carbon nanotube is 30 microns hereinafter, straight
Diameter is 10nm hereinafter, the graphene and the deposition thickness of carbon nanotube are 20nm or less.
According to the preparation method of the aluminium base graphene of the present embodiment, carbon nanotube composite heat dissipation material, which is characterized in that institute
Stating aluminium salt is aluminum nitrate.
Embodiment 2:
The preparation method of a kind of aluminium base graphene, carbon nanotube composite heat dissipation material, which is characterized in that including following step
It is rapid:
(1) graphene powder and carbon nanotube of equivalent are respectively put into ethanol solution, being made into concentration is
The mixed liquor of the graphene of 0.08mg/ml, carbon nanotube, adds aluminum salt solution, is made into the aluminium that aluminium salt concentration is 0.4mg/ml
Salt graphene, carbon nanotube mixed liquor, then disperse 5h with ultrasonic wave, obtain evenly dispersed aluminium salt graphene, carbon nanotube
Mix electrophoresis liquid;
(2) will be 8 minutes ultrasonic in ethanol solution with a thickness of the aluminum slice of 0.05mm, then in 8% dust technology
It is repeatedly rinsed after impregnating 1min with deionized water, after drying, as cathode;
(3), as anode, the cathode and the anode to be immersed in together with the comparable graphite flake of the cathode size
The aluminium salt graphene, carbon nanotube mixing electrophoresis liquid under the DC electric field of 60V/cm carry out electrophoretic deposition 8min;
(4) cathode is taken out, sample is made with hydraulic forming machine cold pressing 15h after laminated multi-layer from the cathode one end,
Wherein the superposition number of plies is 800 layers or more, then by the other end of the cathode after one circle of package outside the sample of compression moulding
It is fixedly welded on its side;
(5) 3h is handled with 500 DEG C of annealing temperature in a nitrogen atmosphere, after Temperature fall, the aluminium base can be obtained
Graphene, carbon nanotube composite heat dissipation material.
According to the preparation method of the aluminium base graphene of the present embodiment, carbon nanotube composite heat dissipation material, which is characterized in that institute
Stating graphene powder is the single layer or few layer graphene by CVD method growth, and the graphene powder partial size is 30 microns hereinafter, thick
Degree is 2nm hereinafter, the carbon nanotube is multi-walled carbon nanotube, and the length of the multi-walled carbon nanotube is 5~30 microns, diameter
For 10nm hereinafter, the graphene and the deposition thickness of carbon nanotube are 20nm or less.
According to the preparation method of the aluminium base graphene of the present embodiment, carbon nanotube composite heat dissipation material, which is characterized in that institute
Stating aluminium salt is aluminum sulfate.
Embodiment 3:
The preparation method of a kind of aluminium base graphene, carbon nanotube composite heat dissipation material, which is characterized in that including following step
It is rapid:
(1) graphene powder and carbon nanotube of equivalent are respectively put into ethanol solution, being made into concentration is
The mixed liquor of the graphene of 0.1mg/ml, carbon nanotube, adds aluminum salt solution, is made into the aluminium salt stone that aluminium salt concentration is 4mg/ml
Black alkene, carbon nanotube mixed liquor, then disperse 4h with ultrasonic wave, obtain the mixing of evenly dispersed aluminium salt graphene, carbon nanotube
Electrophoresis liquid;
(2) will be 10 minutes ultrasonic in ethanol solution with a thickness of the aluminum slice of 0.1mm, then in 6% dust technology
It is repeatedly rinsed after impregnating 1min with deionized water, after drying, as cathode;
(3), as anode, the cathode and the anode to be immersed in together with the comparable graphite flake of the cathode size
The aluminium salt graphene, carbon nanotube mixing electrophoresis liquid under the DC electric field of 80V/cm carry out electrophoretic deposition 4min;
(4) cathode is taken out, sample is made for 24 hours with hydraulic forming machine cold pressing after laminated multi-layer from the cathode one end,
Wherein the superposition number of plies is 300 layers or more, then by the other end of the cathode after one circle of package outside the sample of compression moulding
It is fixedly welded on its side;
(5) 4h is handled with 550 DEG C of annealing temperature in a nitrogen atmosphere, after Temperature fall, the aluminium base can be obtained
Graphene, carbon nanotube composite heat dissipation material.
According to the preparation method of the aluminium base graphene of the present embodiment, carbon nanotube composite heat dissipation material, which is characterized in that institute
Stating graphene powder is the single layer or few layer graphene by CVD method growth, and the graphene powder partial size is 10 microns hereinafter, thick
Degree is 2nm hereinafter, the carbon nanotube is multi-walled carbon nanotube, and the length of the multi-walled carbon nanotube is 30 microns hereinafter, straight
Diameter is 10nm hereinafter, the graphene and the deposition thickness of carbon nanotube are 20nm or less.
According to the preparation method of the aluminium base graphene of the present embodiment, carbon nanotube composite heat dissipation material, which is characterized in that institute
Stating aluminium salt is aluminum nitrate.
Embodiment 4:
The preparation method of a kind of aluminium base graphene, carbon nanotube composite heat dissipation material, which is characterized in that including following step
It is rapid:
(1) graphene powder and carbon nanotube of equivalent are respectively put into ethanol solution, being made into concentration is
The mixed liquor of the graphene of 0.08mg/ml, carbon nanotube, adds aluminum salt solution, is made into the aluminium that aluminium salt concentration is 0.4mg/ml
Salt graphene, carbon nanotube mixed liquor, then disperse 4h with ultrasonic wave, obtain evenly dispersed aluminium salt graphene, carbon nanotube
Mix electrophoresis liquid;
(2) will be 5 minutes ultrasonic in ethanol solution with a thickness of the aluminum slice of 0.03mm, then in 8% dust technology
It is repeatedly rinsed after impregnating 0.8min with deionized water, after drying, as cathode;
(3), as anode, the cathode and the anode to be immersed in together with the comparable graphite flake of the cathode size
The aluminium salt graphene, carbon nanotube mixing electrophoresis liquid under the DC electric field of 100V/cm carry out electrophoretic deposition 6min;
(4) cathode is taken out, sample is made with hydraulic forming machine cold pressing 20h after laminated multi-layer from the cathode one end,
Wherein the superposition number of plies is 1000 layers or more, then by the other end of the cathode after one circle of package outside the sample of compression moulding
It is fixedly welded on its side;
(5) 4h is handled with 500 DEG C of annealing temperature in a nitrogen atmosphere, after Temperature fall, the aluminium base can be obtained
Graphene, carbon nanotube composite heat dissipation material.
According to the preparation method of the aluminium base graphene of the present embodiment, carbon nanotube composite heat dissipation material, which is characterized in that institute
Stating graphene powder is the single layer or few layer graphene by CVD method growth, the graphene powder partial size be 5~30 microns with
Under, with a thickness of 2nm hereinafter, the carbon nanotube is multi-walled carbon nanotube, the length of the multi-walled carbon nanotube is 5~20 micro-
Rice, diameter is 10nm hereinafter, the graphene and the deposition thickness of carbon nanotube are 20nm or less.
According to the preparation method of the aluminium base graphene of the present embodiment, carbon nanotube composite heat dissipation material, which is characterized in that institute
Stating aluminium salt is aluminum nitrate.
In addition, the aluminium base graphene described in order to which present invention be described in more detail, carbon nanotube composite heat dissipation material
Preparation method has been presented in Fig. 1 the basic of aluminium base graphene, carbon nanotube composite heat dissipation material prepared by the method for the present invention
Structural schematic diagram.As shown in Figure 1, the aluminium base graphene, carbon nanotube composite heat dissipation material is by the aluminium base thin slice 1 and institutes
State graphene, carbon nanotube composite layer 2 alternates superposition and the multi-layer compound structure of formation.It is noted that Fig. 1 only table
Show material basic structure, without indicating actual size and ratio, the graphene described in real material, carbon nanotube composite layer 2
Than thinner in Fig. 1.Aluminium base graphene of the present invention is given in Fig. 2, carbon nanotube composite heat dissipation material is deposited on
The scanning electron microscope (SEM) photograph of the compound layer surface of the graphene on aluminium base thin slice, carbon nanotube.It can be seen that the graphene more than 3
It all is covered in aluminum-based substrate surface to horizontal direction, and between each other by aluminum nanoparticles 5 or carbon nanotube 4 or directly
Connect closely, then the carbon nanotube 4, which is substantially all, lies low on 3 surface of graphene, and in the stone
There are many aluminum nanoparticles 5 for covering on 4 surface of black alkene 3 and the carbon nanotube.Show in composite heat dissipation material of the invention
The graphene 3 and the carbon nanotube 4 have had good trend in the horizontal direction, in the compression moulding and burning in later period
During knot, the aluminum nanoparticles 5 being covered on 4 surface of graphene 3 or carbon nanotube play extraordinary company between each lamination
Connect effect.Therefore, aluminium base graphene, the carbon nanotube composite heat dissipation material prepared with the method, and does not participate in graphene 3 and carbon
Alumina-base material before nanotube 4 is compared, and mechanical property and electrical and thermal conductivity can all increase substantially.
In addition to this, aluminium base graphene of the invention, carbon nanotube composite heat dissipation material, can be to perpendicular to Direction of superposition
It is cut into the flaky radiator of different-thickness, longitudinal coefficient of heat transfer also can use difference and make up to 3~6 times of aluminium alloy
The mold of type is pressed into radiator of different shapes again, and rate of heat dissipation and mechanical strength be all higher than common aluminum alloy material.
The preparation method of several aluminium base graphenes, carbon nanotube composite heat dissipation material is described in the embodiment above, and
It should be understood by those skilled in the art that the present invention is not limited to the above embodiments, described in above embodiments and description
Only illustrate the preparation principle of aluminium base graphene of the invention, carbon nanotube composite heat dissipation material, do not departing from essence of the invention
Under the premise of mind and range, various changes and improvements may be made to the invention, these changes and improvements both fall within claimed
In invention scope.
Claims (5)
1. the preparation method of a kind of aluminium base graphene, carbon nanotube composite heat dissipation material, which comprises the following steps:
(1) graphene powder and carbon nanotube of equivalent are respectively put into ethanol solution, be made into concentration be 0.02~
The mixed liquor of the graphene of 0.1mg/ml, carbon nanotube, adds aluminum salt solution, and being made into aluminium salt concentration is 0.4~4mg/ml's
Aluminium salt graphene, carbon nanotube mixed liquor, then disperse 3~5h with ultrasonic wave, obtain evenly dispersed aluminium salt graphene, carbon nanometer
The mixing electrophoresis liquid of pipe;
(2) will with a thickness of the aluminum or aluminum alloy thin slice of 0.01~0.1mm in ethanol solution ultrasound 5~10 minutes, then with 5
It is repeatedly rinsed after impregnating 0.5~1min in~8% dust technology with deionized water, after drying, as cathode;
(3), as anode, the cathode and the anode to be immersed in together described with the comparable graphite flake of the cathode size
Aluminium salt graphene, carbon nanotube mixing electrophoresis liquid under the DC electric field of 60~100V/cm carry out electrophoretic deposition 1~
8min;
(4) cathode is taken out, with hydraulic forming machine cold pressing 10~sample is made for 24 hours after laminated multi-layer from the cathode one end,
Wherein the superposition number of plies is 300 layers or more, then by the other end of the cathode after one circle of package outside the sample of compression moulding
It is fixedly welded on its side;
(5) 3~5h is handled with 450~550 DEG C of annealing temperature in a nitrogen atmosphere, after Temperature fall, can be obtained described
Aluminium base graphene, carbon nanotube composite heat dissipation material.
2. the preparation method of aluminium base graphene as described in claim 1, carbon nanotube composite heat dissipation material, which is characterized in that
The graphene powder is the single layer or few layer graphene by CVD method growth, and the graphene powder partial size is 10~30 microns,
With a thickness of 2nm or less.
3. the preparation method of aluminium base graphene as described in claim 1, carbon nanotube composite heat dissipation material, which is characterized in that
The carbon nanotube is multi-walled carbon nanotube, and the length of the multi-walled carbon nanotube is 5~30 microns, and diameter is 10nm or less.
4. the preparation method of aluminium base graphene as described in claim 1, carbon nanotube composite heat dissipation material, which is characterized in that
The graphene and the deposition thickness of carbon nanotube are 20nm or less.
5. the preparation method of aluminium base graphene as claimed in claim 1,2 or 3, carbon nanotube composite heat dissipation material, feature
It is, the aluminium salt is aluminum nitrate or aluminum sulfate.
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CN106783769A (en) * | 2017-01-06 | 2017-05-31 | 上海增华电子科技有限公司 | A kind of conductive and heat-conductive film assembly |
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