CN105792598B - A kind of graphene composite metallic material - Google Patents
A kind of graphene composite metallic material Download PDFInfo
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- CN105792598B CN105792598B CN201410816025.9A CN201410816025A CN105792598B CN 105792598 B CN105792598 B CN 105792598B CN 201410816025 A CN201410816025 A CN 201410816025A CN 105792598 B CN105792598 B CN 105792598B
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Abstract
The present invention provides a kind of graphene composite metallic materials comprising the metal foil containing multiple through holes and the graphene for being grown in the surface of metal foil and the hole wall of through hole.The aperture of the through hole is 1 μm~1000 μm, hole density 101A/cm2~106A/cm2.The thermal conductivity on the direction perpendicular to metal foil surface can be improved in graphene in the through hole of the graphene composite metallic material, to substantially increase the overall thermal conductivity of graphene composite metallic material.
Description
Technical field
The invention belongs to a kind of radiating element more particularly to a kind of high thermal conductivity graphene composite metallic materials.
Background technique
With the development of science and technology, the miniaturization, micromation of electronic product, high-performance and low cost, to people's
Production and life bring dramatic change.But since electronic product volume is too small, under high-frequency work frequency, electronic component
The heat generated when operating can accumulate rapidly, increase, if cannot pass in time, be easy to cause equipment performance decline or
Person's damage, or even explosion.Therefore, for electronic component remains to work normally with high reliability, the ability to radiate in time becomes
Influence the critical limiting factor of its service life.Existing radiating mode has the modes such as air-cooled, liquid cooling, is to expand local pyrexia
Greater room is opened up, heat is taken away by air or liquid.Cooling fin is often used in field of electronics to radiate.Heat dissipation
Piece is usually that can be passed heat from heat generating components by modes such as conduction, convection current or radiation made of the metal of high thermal conductivity
It is sent in environment.But metal material heating conduction is limited, for example the thermal conductivity 377W/mK of copper, the thermal conductivity of aluminium are
230W/m·K。
In recent years, graphene was attracted wide attention as a kind of new material in the whole world.It is by carbon atom with
sp2What the monoatomic layer of hydridization connection was constituted, theoretic throat is only 0.35nm, is the most thin two-dimentional material found at present
Material.Graphene is the basic unit for constituting other carbon materials, can be warped into the fullerene of zero dimension, curls into one-dimensional CNTs
Or it is stacked to three-dimensional graphite.This special construction has contained abundant and peculiar physical phenomenon, and graphene is made to show to be permitted
Mostly excellent physicochemical properties.Referred to herein is its thermal property, it has as a kind of low-dimensional nano-carbon material
The up to thermal conductivity of 3000W/mK~6000W/mK is the best material of presently found heating conduction.But graphene
Material also has a shortcoming, for example its folding resistance is poor, and the intensity of material is weak, can tear easily or because adhered to position occurs
It is displaced and generates damaged and entry material and fall off, therefore it can not be applied separately as heat sink material.
Graphene is usually to be deposited or be coated in metallic substrate surface in the application of thermally conductive aspect, prepares height with this
Thermally conductive composite construction.Such as, the method on copper (111) monocrystal thin films through chemical vapor deposition (CVD) grows graphene and (asks
Referring to Chinese public patent application CN 102859032A), and using the mode being coated in the graphene coated coating of copper foil surface
Prepare copper carbon composite copper foil cooling fin (referring to Chinese 103476227 A of public patent application CN).But above method is deposited
In shortcoming: 1. vertical direction thermal conductivity is not high enough (< 400W/mK)；2. graphene layer is poor in conjunction with copper foil.Cause
The not high reason of vertical direction thermal conductivity be graphene it is thermally conductive be it is anisotropic, the thermal conductivity of longitudinal Z-direction is lower, one
As 5W/mK~30W/mK.It is that the two interface cohesion is poor that graphene layer, which adheres to poor reason in copper foil surface, is existed very strong
Stress, be easy to cause graphene layer to remove.Therefore, the compound gold of graphene of high bond strength, high heat conductance is developed
Belonging to film not only has great creativeness, also has huge impetus for electronics industry heat dissipation.
Summary of the invention
The main object of the present invention is to provide a kind of graphene composite metallic material of high thermal conductivity, the graphene composite metallic material
Not only thermal conductivity with higher, bond strength also with higher, is applied to integrated circuit, electronic device, heat exchange
In the radiator of the electronic equipments such as device, LED, plays rapid cooling and ensure that electronic component is efficient, stable, long-life operation
Effect.
In order to achieve the goal above, the present invention proposes following technical scheme:
A kind of graphene composite metallic material comprising the metal foil containing multiple through holes and the surface for being grown in metal foil
With the graphene of the hole wall of through hole.The aperture of the through hole is 1 μm~1000 μm, hole density 101A/cm2~106A/
cm2。
The metal foil with a thickness of 5 μm~500 μm.
The metal foil with a thickness of 10 μm~100 μm.
The number of plies of the graphene is 1 layer~100 layers, with a thickness of 0.01 μm~10 μm.
The thermal conductivity of the graphene composite metallic material is 500W/mK~2000W/mK.
The bond strength of the graphene and metal foil is 1Mpa~100Mpa.
The aperture of the through hole is 10 μm~500 μm, hole density 102A/cm2~104A/cm2。
The graphene is basically parallel to the surface of metal foil or the hole wall of through hole.
A kind of graphene composite metallic material a comprising metal foil runs through the gold perpendicular to the multiple of metal foil setting
Belong to the heat pipe of foil and the graphene of the upper and lower surfaces opposite with the metal foil is distributed in.The heat pipe is by running through the metal foil
Graphene formed, and form the graphene of the heat pipe basically perpendicular to the metal foil.The upper and lower of the metal foil is set
The graphene on surface is basically parallel to metal foil.
The graphene composite metallic material is applied to integrated circuit, electronic device, heat exchanger or LED as heat dissipation element
Radiator in.
Compared to the prior art, it is excellent to have the advantages that (1) has for graphene composite metallic material provided by the invention
Heat dissipation performance.Although the thermal conductivity of graphene is high, its heating conduction has anisotropy, the i.e. heat in graphene planes direction
Conductance can achieve 6000W/mK, but its vertical direction thermal conductivity only has 5W/mK~30W/mK.Prior art preparation
Graphene is to be laid in metal foil surface, and direction of heat flow causes final heat dissipation effect unsatisfactory perpendicular to graphene planes.
And graphene composite metallic material of the present invention, two surfaces of metal foil and hole wall have graphene layer.The graphene layer of bottom
Not only can be by heat rapid dispersion that heat source transmits on the surface of graphene, but also it can be by obtained heat by investing hole wall
Graphene layer is quickly transferred to metal foil top graphene layer.The heat for being transferred to top is quickly spread by graphene surface,
Rapid cooling is realized eventually by the mode of convection current and radiation.That is, in the through hole of the graphene composite metallic material
Graphene the thermal conductivity on the direction perpendicular to metal foil surface can be improved, to substantially increase graphene composite metallic material
Overall thermal conductivity.Also, by carrying out reasonable aperture design and hole density design to through hole, the compound gold of graphene can be made
Belong to the thermally conductive more uniform of foil.(2) graphene layer and metal foil bond strength are high.The graphene of prior art preparation is flat due to it
It is layered on metal foil surface, there are interfacial stresses between the two, thus graphene is easy to cause to remove.And graphene of the present invention is multiple
Metal foil is closed, graphene therein is not placed only in two surfaces up and down of metal foil, and is distributed in the hole wall of through hole,
The layer structure that the graphene for being distributed in upper and lower surface and hole wall is connected, metal foil is clipped in the middle and is entangled firm, thus
Greatly improve the bond strength of graphene and metal foil.(3) antiseptic property is excellent, long service life.The stone of prior art preparation
Black alkene cannot achieve the protection to metal foil due to its poor, easy peeling of graphene in conjunction with metal foil.And it is of the invention
The graphene composite metallic material of preparation, since graphene and metal foil are combined into one, graphene is a fine and close netted knot
Structure, thus can effectively stop the erosion of corrosive medium, to greatly improve its service life.
Detailed description of the invention
Fig. 1 is that the structural schematic diagram of graphene composite metallic material of the present invention (wherein, 1 indicates metal foil；2 indicate to pass through
Perforation；3 indicate graphene layer).
Fig. 2 is the microscope photo for the graphene composite metallic material that the embodiment of the present invention 1 obtains.
Fig. 3 a is Raman map measured by the location A of graphene composite metallic material described in Fig. 2.
Fig. 3 b is Raman map measured by the B location of graphene composite metallic material described in Fig. 2.
Specific embodiment
Graphene composite metallic material provided by the invention and preparation method thereof is described further below with reference to attached drawing.
Substance provided by the present invention can be synthesized by marketable material or traditional chemical transform mode.
Other aspects of the present invention are apparent to those skilled in the art due to this disclosure
's.
Below in conjunction with specific embodiment, the present invention is furture elucidated.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.
Unless otherwise defined or described herein, all professional and scientific terms used herein and the skilled people of art technology
Meaning known to member is identical.Furthermore any method similar to or equal to what is recorded and material all can be applied to the present invention
In method.
Referring to Fig. 1, the present invention provides a kind of graphene composite metallic material, it is available by following preparation method.Institute
State preparation method the following steps are included:
(1) metal foil 1 is subjected to surface cleaning processing, treatment process includes: that oil removing, pickling, washing, alcohol are washed, dried；
Wherein, the metal foil 1 with a thickness of 5 μm~500 μm.Preferably, the metal foil 1 with a thickness of 10 μm~
100μm。
(2) metal foil 1 after cleaning is subjected to aperture processing, aperture mode includes laser boring, plasma punching, machinery
Drilling, chemical etching hole etc., obtain multiple through holes 2；
Wherein, the aperture of the through hole 2 is 1 μm~1000 μm, hole density 101A/cm2~106A/cm2.In order to
Make the heat dissipation of metal foil 1 more evenly, it is preferred that the aperture of the through hole 2 is 10 μm~500 μm, hole density 102A/cm2
~104A/cm2；
(3) metal foil 1 for carrying out aperture processing is put into chemical deposition reaction zone, carbon-source gas and carrier gas is passed through, one
Determine at temperature and pressure conditions, it is heavy on the surface of metal foil 1 and the hole wall of through hole 2 to be realized by chemical vapour deposition technique
Graphene in product.
Wherein, the carbon source is one or more of the hydrocarbon gas such as methane, ethylene, acetylene mixed gas；
The carrier gas is reducibility gas (H2), the mixed gas of inert gas (Ar, He) or both；
The pressure is 10-3Pa~105Pa；
The reaction temperature is 800 DEG C~1100 DEG C.
This is deposited on the surface of metal foil and the graphene of the hole wall of through hole is connected to form graphene layer 3, and incite somebody to action
Metal foil is clipped in the middle and entangles firm.The i.e. described graphene layer 3 covers the surface of the metal foil 1 and the hole wall of through hole 2.It is described
Graphene layer 3 is made of the pure graphene of multilayer.The number of plies of graphene is 1 layer~100 layers in the graphene layer 3.The stone
Black alkene layer 3 with a thickness of 0.01 μm~10 μm.The thermal conductivity of obtained graphene composite metallic material is 500W/mK~2000W/
The bond strength of mK, graphene and metal foil 1 is 1Mpa~100Mpa.The graphene composite metallic material is as heat dissipation element
In radiator applied to integrated circuit, electronic device, heat exchanger or LED.
Compared to the prior art, it is excellent to have the advantages that (1) has for graphene composite metallic material provided by the invention
Heat dissipation performance.Although the thermal conductivity of graphene is high, its heating conduction has anisotropy, the i.e. heat in graphene planes direction
Conductance can achieve 6000W/mK, but its vertical direction thermal conductivity only has 5W/mK~30W/mK.Prior art preparation
Graphene is to be laid in metal foil surface, and direction of heat flow causes final heat dissipation effect unsatisfactory perpendicular to graphene planes.
And graphene composite metallic material of the present invention, two surfaces of metal foil and hole wall have graphene layer.The graphene layer of bottom
Not only can be by heat rapid dispersion that heat source transmits on the surface of graphene, but also it can be by obtained heat by investing hole wall
Graphene layer is quickly transferred to metal foil top graphene layer.The heat for being transferred to top is quickly spread by graphene surface,
Rapid cooling is realized eventually by the mode of convection current and radiation.That is, in the through hole of the graphene composite metallic material
Graphene the thermal conductivity on the direction perpendicular to metal foil surface can be improved, to substantially increase graphene composite metallic material
Overall thermal conductivity.Also, by carrying out reasonable aperture design and hole density design to through hole, the compound gold of graphene can be made
Belong to the thermally conductive more uniform of foil.(2) graphene layer and metal foil bond strength are high.The graphene of prior art preparation is flat due to it
It is layered on metal foil surface, there are interfacial stresses between the two, thus graphene is easy to cause to remove.And graphene of the present invention is multiple
Metal foil is closed, graphene therein is not placed only in two surfaces up and down of metal foil, and is distributed in the hole wall of through hole,
This is distributed in upper and lower surface and the graphene of hole wall is connected, and metal foil is clipped in the middle and is entangled firm, to greatly improve stone
The bond strength of black alkene and metal foil.(3) antiseptic property is excellent, long service life.The graphene of prior art preparation is due to it
Poor in conjunction with metal foil, graphene is easy to peel off, thus cannot achieve the protection to metal foil.And graphite prepared by the present invention
Alkene composite metallic material, since graphene and metal foil are combined into one, graphene is a fine and close reticular structure, thus can be with
The erosion for effectively stopping corrosive medium, to greatly improve its service life.
To further describe the present invention, here is the preparation method of the graphene composite film-stuck, under different parameters
Specific embodiment:
Embodiment 1:
The copper foil of 35 μ m-thicks is chosen, and carries out oil removing to it, the cleaning treatments such as pickling, washing, alcohol are washed, dried.It will cleaning
Copper foil afterwards carries out laser boring processing, obtains multiple through holes.The aperture of the through hole is 100 μm, hole density 2000
A/cm2.Then the processed copper foil of aperture will be carried out and be put into chemical vapor deposition reaction zone, be passed through methane and reductive hydrogen,
Under 1000 DEG C and 50Pa pressure conditions, graphene layer is deposited in the hole wall of copper foil surface and through hole.Finally obtain graphene
Composite copper foil.The graphene layer with a thickness of 0.05 μm.
The graphene composite copper foil is tested for the property.Specifically, being measured by heat reflection method film coefficient of heat transfer
Instrument (model Nano TR, German NETZSCH company) measures its thermal conductivity；By pulling open method adhesion-force tester (model
PosiTest AT, DeFelsko company, the U.S.) measure the bond strength of graphene and metal foil.Test result are as follows: the graphite
The thermal conductivity of alkene composite copper foil is 1000W/mK, and the bond strength of graphene and copper foil is 10Mpa.
Also the graphene composite copper foil take pictures under microscope and Raman spectrum test.Referring to Fig. 2,
It can be seen that being evenly distributed with multiple through holes on the surface of copper foil.Please refer to Fig. 3 a and Fig. 3 b, it is seen then that copper foil surface and pass through
The obtained Raman figure in the position of perforation is in 1600cm-1And 2700cm-1Position nearby occurs corresponding respectively to graphene
The peak G and the peak 2D absorption peak, this explanation on the surface of copper foil and the inner wall of through hole is all covered with the graphene.
Embodiment 2:
The goldleaf of 5 μ m-thicks is chosen, and carries out oil removing to it, the cleaning treatments such as pickling, washing, alcohol are washed, dried.After cleaning
Goldleaf carry out plasma aperture processing, obtain multiple through holes.The aperture of the through hole is 1 μm, hole density 105A/
cm2.Then the processed goldleaf of aperture will be carried out and be put into chemical vapor deposition reaction zone, be passed through ethylene and argon gas, at 800 DEG C and
103Under Pa pressure conditions, graphene layer is deposited in the hole wall of goldleaf surface and through hole.Finally obtain the compound goldleaf of graphene.
The graphene layer with a thickness of 0.01 μm.
The compound goldleaf of the graphene is tested for the property.Test method is the same as embodiment 1.Test result are as follows: the stone
The thermal conductivity of the black compound goldleaf of alkene is 2000W/mK, and the bond strength of graphene and goldleaf is 50Mpa.
Embodiment 3:
The silver foil of 100 μ m-thicks is chosen, and carries out oil removing to it, the cleaning treatments such as pickling, washing, alcohol are washed, dried.It will cleaning
Silver foil afterwards carries out chemical etching aperture processing, obtains multiple through holes.The aperture of the through hole is 10 μm, hole density is
104A/cm2.Then the processed silver foil of aperture will be carried out and be put into chemical vapor deposition reaction zone, be passed through acetylene and helium,
900 DEG C and 105Under Pa pressure conditions, graphene layer is deposited in the hole wall of silver foil surface and through hole.It is multiple to finally obtain graphene
Close silver foil.The graphene layer with a thickness of 1 μm.
The compound silver foil of the graphene is tested for the property.Test method is the same as embodiment 1.Test result are as follows: the stone
The thermal conductivity of the black compound silver foil of alkene is 1500W/mK, and the bond strength of graphene and silver foil is 100Mpa.
Embodiment 4:
The aluminium foil of 500 μ m-thicks is chosen, and carries out oil removing to it, the cleaning treatments such as pickling, washing, alcohol are washed, dried.It will cleaning
Aluminium foil afterwards carries out machine drilling processing, obtains multiple through holes.The aperture of the through hole is 500 μm, hole density 102
A/cm2.Then the processed aluminium foil of aperture will be carried out and be put into chemical vapor deposition reaction zone, be passed through methane and hydrogen and argon gas
Gaseous mixture, at 900 DEG C and 10-3Under Pa pressure conditions, graphene layer is deposited in the hole wall of aluminium foil surface and through hole.Finally
To graphene clad aluminum foil.The graphene layer with a thickness of 10 μm.
The graphene clad aluminum foil is tested for the property.Test method is the same as embodiment 1.Test result are as follows: the stone
The thermal conductivity of black alkene clad aluminum foil is 800W/mK, and the bond strength of graphene and aluminium foil is 1Mpa.
Embodiment 5:
The nickel plating copper foil of 200 μ m-thicks is chosen, and carries out oil removing to it, the cleaning treatments such as pickling, washing, alcohol are washed, dried.It will
Nickel plating copper foil after cleaning carries out laser boring processing, obtains multiple through holes.The aperture of the through hole is 50 μm, hole density
It is 103A/cm2.Then the processed nickel plating copper foil of aperture will be carried out and be put into chemical vapor deposition reaction zone, be passed through methane and hydrogen
Gas deposits graphene layer in the hole wall of nickel plating copper foil surface and through hole under 1100 DEG C and 0.1Pa pressure conditions.Finally
To graphene composite nickel-plating copper foil.The graphene layer with a thickness of 0.1 μm.
The graphene composite nickel-plating copper foil is tested for the property.Test method is the same as embodiment 1.Test result are as follows: institute
The thermal conductivity of graphene composite nickel-plating copper foil is stated as 1200W/mK, the bond strength of graphene and nickel plating copper foil is 5Mpa.
The above description of the embodiment is only used to help understand the method for the present invention and its core ideas.It should be pointed out that pair
For those skilled in the art, without departing from the principle of the present invention, the present invention can also be carried out
Some improvements and modifications, these improvements and modifications also fall within the scope of protection of the claims of the present invention.To these embodiments
A variety of modifications are it will be apparent that the general principles defined herein can be not for those skilled in the art
It is realized in other embodiments in the case where being detached from the spirit or scope of the present invention.Therefore, the present invention is not intended to be limited to this
These embodiments shown in text, and it is to fit to the widest scope consistent with the principles and novel features disclosed herein.
Claims (9)
1. a kind of graphene composite metallic material, it is characterised in that: it includes the metal foil containing multiple through holes and is grown in gold
Belong to the graphene on the surface of foil and the hole wall of through hole, the graphene is the layer structure being connected, the through hole
Aperture is 10 μm~500 μm, hole density 102A/cm2~104A/cm2。
2. graphene composite metallic material according to claim 1, which is characterized in that the metal foil with a thickness of 5 μm~
500μm。
3. graphene composite metallic material according to claim 2, which is characterized in that the metal foil with a thickness of 10 μm~
100μm。
4. graphene composite metallic material according to claim 1, it is characterised in that: the number of plies of the graphene be 1 layer~
100 layers, with a thickness of 0.01 μm~10 μm.
5. graphene composite metallic material according to claim 1, it is characterised in that: the heat of the graphene composite metallic material
Conductance is 500W/mK~2000W/mK.
6. graphene composite metallic material according to claim 1, it is characterised in that: the combination of the graphene and metal foil
Intensity is 1Mpa~100Mpa.
7. graphene composite metallic material according to claim 1, it is characterised in that: the graphene is basically parallel to metal
The hole wall of foil surface or through hole.
8. a kind of graphene composite metallic material, which is characterized in that it includes a metal foil, perpendicular to the multiple of metal foil setting
Through the metal foil heat pipe and be distributed in the graphenes of the opposite upper and lower surfaces of the metal foil, the heat pipe was by through should
The graphene of metal foil is formed, and the graphene for forming the heat pipe is arranged basically perpendicular to the metal foil in the metal foil
The graphenes of upper and lower surfaces be basically parallel to metal foil, the graphene is the layer structure being connected.
9. a kind of graphene composite metallic material according to claim 1-8, it is characterised in that: the graphene is multiple
Metal foil is closed to be applied to as heat dissipation element in the radiator of integrated circuit, electronic device, heat exchanger or LED.
Priority Applications (5)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410816025.9A CN105792598B (en) | 2014-12-24 | 2014-12-24 | A kind of graphene composite metallic material |
| TW104139658A TWI602611B (en) | 2014-12-02 | 2015-11-27 | Graphene dispersant and its application |
| EP15865917.7A EP3228592A4 (en) | 2014-12-02 | 2015-11-27 | Graphene dispersant and application thereof |
| PCT/CN2015/095742 WO2016086796A1 (en) | 2014-12-02 | 2015-11-27 | Graphene dispersant and application thereof |
| US15/607,552 US10696790B2 (en) | 2014-12-02 | 2017-05-29 | Graphene dispersant and application thereof |
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| CN201410816025.9A CN105792598B (en) | 2014-12-24 | 2014-12-24 | A kind of graphene composite metallic material |
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| CN105792598B true CN105792598B (en) | 2019-04-19 |
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| CN110013628B (en) * | 2018-01-09 | 2021-09-10 | 中国石油化工股份有限公司 | Fire arrestor |
| CN108428687B (en) * | 2018-03-12 | 2020-05-12 | 深圳天元羲王材料科技有限公司 | Graphene metal bonding pad and preparation method thereof |
| CN108517513A (en) * | 2018-04-27 | 2018-09-11 | 北京石墨烯研究院 | Graphene clad aluminum foil and preparation method thereof |
| CN109390586A (en) * | 2018-11-23 | 2019-02-26 | 天津市捷威动力工业有限公司 | A kind of cathode expansion the inhibition structure and cathode and preparation method thereof of lithium ion battery |
| CN115746594B (en) * | 2022-12-08 | 2024-04-19 | 上官俊华 | Paint for surface lacquering of tire remover and preparation method thereof |
| CN116682596B (en) * | 2023-08-03 | 2023-10-13 | 浙江正泰电器股份有限公司 | Graphene-metal composite conductor, and preparation method and application thereof |
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| CN100556264C (en) * | 2007-08-07 | 2009-10-28 | 哈尔滨工程大学 | A kind of preparation method of graphite-metal compound heat dispersion base material |
| US8081468B2 (en) * | 2009-06-17 | 2011-12-20 | Laird Technologies, Inc. | Memory modules including compliant multilayered thermally-conductive interface assemblies |
| JP6008117B2 (en) * | 2012-02-15 | 2016-10-19 | パナソニックＩｐマネジメント株式会社 | Graphite structure and electronic device using the same |
| CN203015365U (en) * | 2012-12-24 | 2013-06-19 | 郑淳展 | Cooling fin |
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