CN109962009A - Graphene/copper composite radiating film preparation method and heat dissipation film obtained and application - Google Patents
Graphene/copper composite radiating film preparation method and heat dissipation film obtained and application Download PDFInfo
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- CN109962009A CN109962009A CN201910165155.3A CN201910165155A CN109962009A CN 109962009 A CN109962009 A CN 109962009A CN 201910165155 A CN201910165155 A CN 201910165155A CN 109962009 A CN109962009 A CN 109962009A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 156
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 145
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 115
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 94
- 239000010949 copper Substances 0.000 title claims abstract description 94
- 239000002131 composite material Substances 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 230000017525 heat dissipation Effects 0.000 title abstract description 22
- 238000000576 coating method Methods 0.000 claims abstract description 79
- 239000011248 coating agent Substances 0.000 claims abstract description 75
- 238000000034 method Methods 0.000 claims abstract description 44
- 238000007731 hot pressing Methods 0.000 claims abstract description 37
- 239000006185 dispersion Substances 0.000 claims abstract description 19
- 238000003490 calendering Methods 0.000 claims abstract description 14
- 150000001875 compounds Chemical class 0.000 claims description 41
- 238000010438 heat treatment Methods 0.000 claims description 23
- 239000011889 copper foil Substances 0.000 claims description 21
- 238000001035 drying Methods 0.000 claims description 21
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 14
- 239000007789 gas Substances 0.000 claims description 13
- 238000010792 warming Methods 0.000 claims description 13
- 239000011261 inert gas Substances 0.000 claims description 10
- 239000002904 solvent Substances 0.000 claims description 10
- 229910052786 argon Inorganic materials 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical group O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000012298 atmosphere Substances 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 8
- 238000005265 energy consumption Methods 0.000 abstract description 6
- 230000001681 protective effect Effects 0.000 abstract description 4
- 230000005855 radiation Effects 0.000 abstract description 3
- 238000010924 continuous production Methods 0.000 abstract description 2
- 239000005749 Copper compound Substances 0.000 abstract 3
- 150000001880 copper compounds Chemical class 0.000 abstract 3
- 230000002035 prolonged effect Effects 0.000 abstract 1
- 229910002804 graphite Inorganic materials 0.000 description 11
- 239000010439 graphite Substances 0.000 description 11
- 239000012300 argon atmosphere Substances 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000001291 vacuum drying Methods 0.000 description 3
- 229910000838 Al alloy Inorganic materials 0.000 description 2
- 229910000881 Cu alloy Inorganic materials 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 229910003460 diamond Inorganic materials 0.000 description 2
- 239000010432 diamond Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000004528 spin coating Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- WURBVZBTWMNKQT-UHFFFAOYSA-N 1-(4-chlorophenoxy)-3,3-dimethyl-1-(1,2,4-triazol-1-yl)butan-2-one Chemical compound C1=NC=NN1C(C(=O)C(C)(C)C)OC1=CC=C(Cl)C=C1 WURBVZBTWMNKQT-UHFFFAOYSA-N 0.000 description 1
- 235000002918 Fraxinus excelsior Nutrition 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 239000002956 ash Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 230000005670 electromagnetic radiation Effects 0.000 description 1
- 238000005274 electrospray deposition Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
- B05D1/28—Processes for applying liquids or other fluent materials performed by transfer from the surfaces of elements carrying the liquid or other fluent material, e.g. brushes, pads, rollers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/04—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to gases
- B05D3/0466—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to gases the gas being a non-reacting gas
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/04—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to gases
- B05D3/0493—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to gases using vacuum
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/14—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to metal, e.g. car bodies
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/48—Manufacture or treatment of parts, e.g. containers, prior to assembly of the devices, using processes not provided for in a single one of the subgroups H01L21/06 - H01L21/326
- H01L21/4814—Conductive parts
- H01L21/4871—Bases, plates or heatsinks
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/34—Arrangements for cooling, heating, ventilating or temperature compensation ; Temperature sensing arrangements
- H01L23/36—Selection of materials, or shaping, to facilitate cooling or heating, e.g. heatsinks
- H01L23/373—Cooling facilitated by selection of materials for the device or materials for thermal expansion adaptation, e.g. carbon
- H01L23/3735—Laminates or multilayers, e.g. direct bond copper ceramic substrates
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/34—Arrangements for cooling, heating, ventilating or temperature compensation ; Temperature sensing arrangements
- H01L23/36—Selection of materials, or shaping, to facilitate cooling or heating, e.g. heatsinks
- H01L23/373—Cooling facilitated by selection of materials for the device or materials for thermal expansion adaptation, e.g. carbon
- H01L23/3736—Metallic materials
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/34—Arrangements for cooling, heating, ventilating or temperature compensation ; Temperature sensing arrangements
- H01L23/36—Selection of materials, or shaping, to facilitate cooling or heating, e.g. heatsinks
- H01L23/373—Cooling facilitated by selection of materials for the device or materials for thermal expansion adaptation, e.g. carbon
- H01L23/3738—Semiconductor materials
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K7/00—Constructional details common to different types of electric apparatus
- H05K7/20—Modifications to facilitate cooling, ventilating, or heating
- H05K7/2039—Modifications to facilitate cooling, ventilating, or heating characterised by the heat transfer by conduction from the heat generating element to a dissipating body
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Abstract
The present invention relates to graphene radiation material field, the preparation method and heat dissipation film obtained and application of a kind of graphene/copper composite radiating film are disclosed.This method comprises: 1) the step of preparing graphene oxide dispersion；2) the step of preparing graphene oxide/copper compound wet coating；3) the step of dry graphene oxide/copper compound wet coating；4) the step of redox graphene/copper compound dry coating；5) hot pressing calendaring processes.Preparation method provided by the invention is simple, environmentally protective, can continuous production and it is at low cost, low energy consumption, graphene obtained/copper composite radiating film excellent thermal conductivity, when being used on electronic product, the heat dissipation capacity of equipment can be greatly reduced, prolonged the service life, and then accelerate and promote graphene in the application of field of radiating.
Description
Technical field
The present invention relates to graphene radiation material and telecommunications fields, and in particular to a kind of graphene/copper composite radiating
The preparation method graphene of film/copper composite radiating film preparation method and heat dissipation film obtained and application.
Background technique
As electronics is integrated and the rapid development of package technique and the integrated application of high power density device, electronic device
Towards micromation, intelligence, lightweight, high power densityization development, the heat that the power consumptions such as CPU generate is also increasing, in turn
Caused temperature rise substantially reduces the reliability of electronic device and service life, failure rate increases, and results even in electronic component
Thoroughly damage.Thus, heat dissipation problem has become the serious problem that electronic information industry faces.
Common heat sink material has copper alloy, aluminium alloy, common graphite, diamond thin, graphite film and soft graphite
(expanded graphite) etc..Wherein, copper alloy due to density it is big, in the electronic product for having strict demand to weight and volume using limit
It makes more；Aluminum alloy heat conductance is low；Graphite film again since its lamellar structure is unobvious, internal voids and fold are difficult to eliminate etc. because
Element limits the further promotion of its heating conduction, and can not do thickness, is typically limited to only in nanoscale or micro-scaled range；
Diamond thin can not equally do thickness, and higher cost；And soft graphite can generate a large amount of acid in preparation process
Property waste liquid, pollute environment.
In view of problems existing for above-mentioned material, it is badly in need of that a kind of density is low, thermal conductivity is high, radiation coefficient is high, thermal conductivity
Not size-limited heat sink material.
Thermal conductivity is up to 5300W/ (m in the theoretical face of single-layer graphene2K), high compared to the thermal conductivity of traditional material
An order of magnitude out is the highest material of thermal conductivity found so far.It has simultaneously density is low, thermal expansion coefficient is low,
Satisfactory mechanical property and to excellent characteristics such as high band (30MHz or more) electromagnetic radiation shield effectiveness with higher.And
Its lamellar structure can not only be well adapted for all kinds of surfaces, shielding heat source and component, moreover it is possible to enable the performance of electronic product
It improves.
Currently, the preparation method of graphene heat dissipation film is more, for example, CVD method, spin-coating method, suction method, electrochemical process, quiet
The methods of electrospray deposition method and self assembly.The factor for wherein influencing graphene heat dissipation film heating conduction specifically includes that graphite
Size, the number of plies, compactness and crystallinity of alkene etc..But there is problems, such as CVD preparation in above-mentioned all kinds of methods again
Higher cost；The uniformity of film and compactness of spin-coating method and suction method preparation are lower；Electrochemical process, electrostatic spray, from group
Dress method energy consumption is higher.
Therefore, it is badly in need of providing a kind of preparation method of the thin heat dissipation film of graphene environmentally protective, inexpensive, that low energy consumption.
Summary of the invention
The purpose of the invention is to overcome, production technology is complicated, at high cost, energy consumption is high in existing heat dissipation film preparation process
And the problems such as seriously polluted, and the defects of there are heat dissipation film uniformity obtained and poor compactness, provide a kind of graphene/
The preparation method of copper composite radiating film, this method is simple, environmentally protective, can continuous production and it is at low cost, low energy consumption, obtained
Graphene/copper composite radiating film excellent thermal conductivity, when being used on electronic product, can greatly reduce the heat dissipation of equipment
It measures, prolong the service life, and then accelerate and promote graphene in the application of field of radiating.
To achieve the goals above, first aspect present invention provides a kind of preparation side of graphene/copper composite radiating film
Method, wherein the method includes the following steps:
1) graphene oxide is distributed in solvent, obtains graphene oxide dispersion；
2) graphene oxide dispersion is coated on copper foil, obtains the compound wet coating of graphene oxide/copper；
3) the compound wet coating of graphene oxide/copper is dried, obtains the compound dry coating of graphene oxide/copper；
4) the compound dry coating of graphene oxide/copper is heat-treated in atmosphere of inert gases, obtain graphene/
Copper composite coating；
5) graphene/copper composite coating is subjected to hot pressing calendering, obtains graphene/copper composite radiating film.
Preferably, in step 1), the solvent is deionized water.
Preferably, 10-300 μm of the partial size of the graphene oxide.
Preferably, relative to the graphene oxide of 1g, the dosage of the solvent is 10-150mL, more preferably 10-
120mL, further preferably 20-100mL.
Preferably, in step 2), the coating is coated by coating machine.
Preferably, the film speed of the coating machine is 20-100m/s, blade width 30-100mm, and blade thickness is
0.01-10mm。
Preferably, the film speed of the coating machine is 20-60m/s, blade width 30-70mm, and blade thickness is
0.1-30mm。
Preferably, the copper foil with a thickness of 10-60 μm.
Preferably, the copper foil with a thickness of 20-50 μm.
Preferably, the compound wet coating of graphene oxide/copper with a thickness of 20-60 μm.
Preferably, in step 3), the condition of the drying includes: that vacuum degree is 0-100Pa, drying temperature 70-120
DEG C, drying time 1-6h.
Preferably, it is 20-100Pa that the condition of the drying, which includes: vacuum degree, and drying temperature is 80-110 DEG C, when dry
Between be 2-4h.
Preferably, in step 4), the heat treatment carries out in high temperature furnace.
Preferably, the power of the high temperature furnace is 10-40KW.
Preferably, the condition of the heat treatment includes: that 300-500 DEG C is warming up in 10-20min, keeps the temperature 1-3h, cooling
To room temperature.
Preferably, the condition of the heat treatment includes: that 300-500 DEG C is warming up in 10-20min, keeps the temperature 2-3h, cooling
To room temperature.
Preferably, the inert gas is argon gas or nitrogen.
Preferably, in step 4), the hot pressing calendering uses hot pressing calender.
Preferably, it is 20-80MPa that the condition of the hot pressing calendering, which includes: the pressure of hot pressing calender, and heating rate is
It 10-40 DEG C/min, after keeping the temperature 10-60min at 500-1000 DEG C, is cooled to room temperature.
Preferably, in step 4), the condition of the hot pressing calendering includes: that the pressure of hot pressing calender is 40-60MPa, is risen
Warm rate is that 10-30 DEG C/min is cooled to room temperature after keeping the temperature 10-40min at 600-900 DEG C.
Second aspect, the present invention provides the graphene as made from method of the present invention/copper composite radiating films.
The third aspect, the present invention provides graphene of the present invention/copper composite radiating films to prepare mobile phone and/or show
Show the application in device.
In the present invention, by first be made graphene oxide/copper composite coating, recycle thermal reduction be reduced into graphene/
Copper composite radiating film, further ensures that defect in film obtained is few, film even compact, to guarantee the continuity of film；Into one
Step ground, graphene/copper composite radiating film, be not only utilized graphene towards thermal conductivity, but also when graphene and copper be utilized being bonded
Longitudinal thermal conductivity, it is efficient simultaneously at horizontal and vertical two aspects when enabling this composite radiating film for electronic product radiating
Rate outward it is thermally conductive, without formed hot polymerization chalaza；Meanwhile the composite radiating film can be easily attached at electronic product heat source,
Be effectively reduced hot(test)-spot temperature, and will not shielded signal, the performance of electronic product can be efficiently modified.
Specifically, preparation method provided by the invention have it is following the utility model has the advantages that
1) it is simple, environmentally protective to provide preparation method by the present invention, at low cost and low energy consumption；
2) preparation method provided by the invention can be carried out continuously volume production, further improve process efficiency；
3) graphene/copper composite radiating film obtained is not size-limited by means of the present invention, horizontal, thickness
It is controllable；
4) graphene/copper composite radiating film obtained has anisotropy by means of the present invention, not only thermally conductive in face
Property it is preferable, vertical heat transfer is also preferable, be used for electronic product radiating when, can make heat in the horizontal and vertical directions simultaneously quickly
Ground export, will not cause hot-spot phenomenon；
5) graphene and copper are tightly combined in graphene/copper composite radiating film obtained by means of the present invention, are not easy
Layering, and heat dissipation film defect obtained is few, even compact, further ensures the continuity of film；
6) graphene/copper composite radiating film obtained can easily be attached to electronic product heat source by means of the present invention
Place, is effectively reduced hot(test)-spot temperature, and will not shielded signal, the performance of electronic product can be efficiently modified.
Other features and advantages of the present invention will the following detailed description will be given in the detailed implementation section.
Detailed description of the invention
Fig. 1 is the application graphene/copper composite radiating film process flow chart.
Specific embodiment
Detailed description of the preferred embodiments below.It should be understood that described herein specific
Embodiment is merely to illustrate and explain the present invention, and is not intended to restrict the invention.
In a first aspect, the present invention provides a kind of graphene/copper composite radiating film preparation methods, wherein the method
Include the following steps:
1) graphene oxide is distributed in solvent, obtains graphene oxide dispersion；
2) graphene oxide dispersion is coated on copper foil, obtains the compound wet coating of graphene oxide/copper；
3) the compound wet coating of graphene oxide/copper is dried, obtains the compound dry coating of graphene oxide/copper；
4) the compound dry coating of graphene oxide/copper is heat-treated in atmosphere of inert gases, obtain graphene/
Copper composite coating；
5) graphene/copper composite coating is subjected to hot pressing calendering, obtains graphene/copper composite radiating film.
For above-mentioned solvent, there is no particular limitation, and it is evenly dispersed to can be realized graphene oxide, of the invention
In method, it is preferable that in step 1), the solvent is deionized water.
For the source of above-mentioned graphene oxide, there is no particular limitation, can be commercially available, can also be using changing
Into Hummers method be prepared, it is preferable that the purity of the graphene oxide be 98 weight % or more, tenor is less than
100ppm, content of ashes are 1 weight % hereinafter, pH >=5.
For the partial size of above-mentioned graphene oxide, also there is no particular limitation, in the method for the invention, it is preferable that described
The partial size of graphene oxide is 10-300 μm.
For the concentration of above-mentioned graphene oxide dispersion, also there is no particular limitation, in order to guarantee the property of final heat dissipation film
Can, in the method for the invention, it is preferable that relative to the graphene oxide of 1g, the dosage of the solvent is 10-150mL,
More preferably 10-120mL, further preferably 20-100mL.
It, can be using ultrasound in a specific embodiment of the invention in order to further ensure graphene oxide is evenly dispersed
The ancillary measures such as dispersion, such as by ultrasonic disperse 1-5h so that the graphene oxide being further ensured that in dispersion liquid uniformly divides
Cloth.
In order to improve the uniformity of coating, it is further ensured that the performance of subsequent thermal dissipation film, in the method for the invention, preferably
Ground, in step 2), the coating is coated by coating machine.
For the application conditions of coating machine, those skilled in the art can be specific determines according to actual conditions, in the present invention
Method in, in order to further increase the uniformity of coating, to guarantee the performance of subsequent thermal dissipation film, it is preferable that the coating
The film speed of machine is 20-100m/s, blade width 30-100mm, blade thickness 0.01-10mm；It is highly preferred that described
The film speed of coating machine is 20-60m/s, blade width 30-80mm, blade thickness 0.1-5mm；It is further preferred that
The film speed of the coating machine is 30-50m/s, and scraper width is 30-70mm, blade thickness 0.1-3mm.
In the present invention, for above-mentioned copper foil, there is no particular limitation, can be commonly all kinds of for those skilled in the art
Copper foil, the copper foil used in a preferred embodiment of the present invention is electronics copper foil, single-sided conductive.
For the thickness of above-mentioned copper foil, there is no particular limitation, in order to further ensure the performance of subsequent thermal dissipation film, at this
In the method for invention, it is preferable that the copper foil with a thickness of 10-60 μm；Further preferably 15-55 μm；Still more preferably
It is 20-50 μm.
For the thickness of the above-mentioned compound wet coating of graphene oxide/copper, also there is no particular limitation, in order to further ensure
The performance of subsequent thermal dissipation film, in the method for the invention, it is preferable that the compound wet coating of graphene oxide/copper with a thickness of
20-60 μm, more preferably 30-50 μm.
For the mode that is dried, there is no particular limitation, it is preferable that the condition of the drying includes: that vacuum degree is 0-
100Pa, drying temperature are 70-120 DEG C, drying time 1-6h；It is highly preferred that the condition of the drying includes: that vacuum degree is
10-100Pa, drying temperature are 80-120 DEG C, drying time 2-5h；It is further preferred that the condition of the drying includes: true
Reciprocal of duty cycle is 20-100Pa, and drying temperature is 80-110 DEG C, drying time 2-4h.
The drying can for example carry out in an oven.
In the method for the invention, it is preferable that in step 4), the heat treatment carries out in high temperature furnace.
In the method for the invention, it is preferable that the power of the high temperature furnace is 10-40KW.
In the method for the invention, the condition of the heat treatment includes: that 300-500 DEG C is warming up in 10-20min, is protected
Warm 1-3h, is cooled to room temperature.
In the method for the invention, it is preferable that the inert gas is argon gas or nitrogen.
In the method for the invention, it is preferable that the air-flow velocity of the inert gas is 20-100sccm；It is highly preferred that
The air-flow velocity of the inert gas is 30-80sccm.
In a preferred embodiment of the invention, the power of the high temperature furnace is 20-30KW, the heat treatment
Condition includes: that 300-500 DEG C is warming up in 20min, keeps the temperature 2-3h, is cooled to room temperature；The inert gas is argon gas；It is described
The air-flow velocity of inert gas is 40-60sccm.
In the method for the invention, it is preferable that in step 5), the hot pressing calendering uses hot pressing calender.
For the condition of hot pressing calendering, those skilled in the art can determines according to actual conditions, in method of the invention
In, it is preferable that the condition of the hot pressing calendering includes: that the pressure of hot pressing calender is 20-80MPa, heating rate 10-40
DEG C/min, at 500-1000 DEG C keep the temperature 10-60min after, be cooled to room temperature；It is highly preferred that the condition packet of the hot pressing calendering
Include: the pressure of hot pressing calender is 30-70MPa, and heating rate is 15-35 DEG C/min, keeps the temperature 20- at 600-1000 DEG C
After 50min, it is cooled to room temperature；It is further preferred that the pressure that the condition of the hot pressing calendering includes: hot pressing calender is 40-
60MPa, heating rate are that 20-30 DEG C/min is cooled to room temperature after keeping the temperature 30-40min at 700-900 DEG C.
Second aspect, the present invention provides the graphene as made from method of the present invention/copper composite radiating films.
The third aspect, the present invention provides graphene of the present invention/copper composite radiating films to prepare mobile phone and/or show
Show the application in device.Graphene provided by the invention/copper composite radiating film can partially solve the heat dissipation problem of electronic equipment, preferably
Ground is applied to the electronics such as mobile phone, plasma display, LCD TV, laptop, microprocessor unit, projector, power supply
In product.
In following embodiment, unless otherwise instructed, each material used can be commercially available, unless otherwise instructed,
Method used is the conventional method of this field.
Embodiment 1
1) it prepares graphene oxide dispersion: graphene oxide 10g and 1L deionized water being added in beaker, ultrasound is set
Back-up dissipates 2h, and graphene oxide dispersion is made；
2) graphite oxide ene coatings are prepared: by graphene oxide dispersion coater obtained above to copper foil
On (copper foil single-sided conductive, with a thickness of 20 μm) conducting surface, the film speed of coating machine is 30m/s, and scraper width is 30mm, and scraper is thick
Degree is 1mm, obtains the compound wet coating of graphene oxide/copper；
3) it the dry compound wet coating of graphene oxide/copper: obtains for the compound wet coating of graphene oxide/copper being put by above-mentioned
4h (vacuum degree of baking oven is 20Pa, and temperature is 80 DEG C) is dried in vacuum drying oven, obtains the compound dry coating of graphene oxide/copper；
4) the compound dry coating of redox graphene/copper: the above-mentioned compound dry coating of graphene oxide/copper is placed in be filled with it is lazy
It is heat-treated in the high temperature furnace of property gas, obtains graphene/copper composite coating；
Wherein, the power of high temperature furnace is 20KW, the condition of heat treatment are as follows: is filled with the argon gas that concentration is 99.9%, gas in advance
Stream flow velocity is 40sccm, and entire heat treatment process keeps argon atmosphere, and 300 DEG C are warming up in 20min, keeps the temperature 2h, naturally cold
But to room temperature；
5) hot pressing is rolled: graphene/copper composite coating being rolled with hot pressing calender, it is compound to obtain graphene/copper
Heat dissipation film, wherein the pressure of hot pressing calender is 40MPa, keeps the temperature 30min after being warming up to 700 DEG C with the rate of 20 DEG C/min, from
Heat is cooled to room temperature.The thermal coefficient for measuring heat dissipation film is 700W/ (m2·K)。
Embodiment 2
1) it prepares graphene oxide dispersion: graphene oxide 10g and 500mL deionized water is added in beaker, surpass
Acoustic equipment disperses 3h, and graphene oxide dispersion is made；
2) graphite oxide ene coatings are prepared: by graphene oxide dispersion coater obtained above to copper foil
On (copper foil single-sided conductive, with a thickness of 35 μm) conducting surface, the film speed of coating machine is 40m/s, and scraper width is 100mm, scraper
With a thickness of 3mm, the compound wet coating of graphene oxide/copper is obtained；
3) it the dry compound wet coating of graphene oxide/copper: obtains graphene oxide/copper wet coating being put into vacuum by above-mentioned
3h (vacuum degree of baking oven is 30Pa, and temperature is 110 DEG C) is dried in baking oven, obtains the compound dry coating of graphene oxide/copper；
4) the compound dry coating of redox graphene/copper: the above-mentioned compound dry coating of graphene oxide/copper is placed in be filled with it is lazy
It is heat-treated in the high temperature furnace of property gas, obtains graphene/copper composite coating；
Wherein, the power of high temperature furnace is 25KW, the condition of heat treatment are as follows: is filled with the argon gas that concentration is 99.9%, gas in advance
Stream flow velocity is 50sccm, and entire heat treatment process keeps argon atmosphere, and 400 DEG C are warming up in 20min, keeps the temperature 2.5h, natural
It is cooled to room temperature；
5) hot pressing is rolled: graphene/copper composite coating being rolled with hot pressing calender, it is compound to obtain graphene/copper
Heat dissipation film, wherein the pressure of hot pressing calender is 50MPa, keeps the temperature 35min after being warming up to 800 DEG C with the rate of 25 DEG C/min, from
Heat is cooled to room temperature.Measure the thermal coefficient 800-1000W/ (m of heat dissipation film2·K)。
Embodiment 3
1) it prepares graphene oxide dispersion: graphene oxide 10g and 200mL deionized water is added in beaker, surpass
Acoustic equipment disperses 4h, and graphene oxide dispersion is made；
2) graphite oxide ene coatings are prepared: by graphene oxide dispersion coater obtained above to copper foil
On (copper foil single-sided conductive, with a thickness of 50 μm) conducting surface, the film speed of coating machine is 50m/s, and scraper width is 70mm, and scraper is thick
Degree is 0.1mm, obtains the compound wet coating of graphene oxide/copper；
3) it the dry compound wet coating of graphene oxide/copper: obtains for the compound wet coating of graphene oxide/copper being put by above-mentioned
4h (baking oven vacuum degree is 100Pa, and temperature is 100 DEG C) is dried in vacuum drying oven, obtains the compound dry coating of graphene oxide/copper；
4) the compound dry coating of redox graphene/copper: the above-mentioned compound dry coating of graphene oxide/copper is placed in be filled with it is lazy
It is heat-treated in the high temperature furnace of property gas, obtains graphene/copper composite coating；
Wherein, the power of high temperature furnace is 30KW, the condition of heat treatment are as follows: is filled with the argon gas that concentration is 99.9%, gas in advance
Stream flow velocity is 60sccm, and entire heat treatment process keeps argon atmosphere, and 500 DEG C are warming up in 20min, keeps the temperature 3h, naturally cold
But to room temperature；
5) hot pressing is rolled: graphene/copper composite coating being rolled with hot pressing calender, it is compound to obtain graphene/copper
Heat dissipation film, wherein the pressure of hot pressing calender is 60MPa, keeps the temperature 40min after being warming up to 900 DEG C with the rate of 30 DEG C/min, from
Heat is cooled to room temperature.The thermal coefficient for measuring heat dissipation film is 1200W/ (m2·K)。
Comparative example 1
One existing embodiment for preparing graphene/copper composite radiating film mode please be provided.
1) it prepares graphene dispersing solution: by 20g graphene powder and 200mL aqueous polyurethane, 3g dispersing agent K30, arriving and burn
In cup, ultrasonic device disperses 4h, and graphene dispersing solution is made；
2) graphite ene coatings are prepared: by graphene dispersing solution coater obtained above to copper foil (copper foil single side
Conduction, with a thickness of 50 μm) on conducting surface, the film speed of coating machine is 50m/s, and scraper width is 70mm, and blade thickness is
0.1mm obtains the compound wet coating of graphene/copper；
3) it the dry compound wet coating of graphene/copper: obtains the compound wet coating of graphene/copper being put into vacuum drying oven by above-mentioned
Middle drying 4h (baking oven vacuum degree is 100Pa, and temperature is 100 DEG C), obtains the compound dry coating of graphene/copper；
4) hot pressing is rolled: graphene/copper composite coating being rolled with hot pressing calender, it is compound to obtain graphene/copper
Heat dissipation film, wherein the pressure of hot pressing calender is 60MPa, keeps the temperature 40min after being warming up to 900 DEG C with the rate of 30 DEG C/min, from
Heat is cooled to room temperature.The thermal coefficient for measuring the composite radiating film is 400W/ (m2·K)。
The preferred embodiment of the present invention has been described above in detail, and still, the present invention is not limited thereto.In skill of the invention
In art conception range, can with various simple variants of the technical solution of the present invention are made, including each technical characteristic with it is any its
Its suitable method is combined, and it should also be regarded as the disclosure of the present invention for these simple variants and combination, is belonged to
Protection scope of the present invention.
Claims (10)
1. a kind of graphene/copper composite radiating film preparation method, which is characterized in that the method includes the following steps:
1) graphene oxide is distributed in solvent, obtains graphene oxide dispersion；
2) graphene oxide dispersion is coated on copper foil, obtains the compound wet coating of graphene oxide/copper；
3) the compound wet coating of graphene oxide/copper is dried, obtains the compound dry coating of graphene oxide/copper；
4) the compound dry coating of graphene oxide/copper is heat-treated in atmosphere of inert gases, it is multiple obtains graphene/copper
Close coating；
5) graphene/copper composite coating is subjected to hot pressing calendering, obtains graphene/copper composite radiating film.
2. graphene according to claim 1/copper composite radiating film preparation method, which is characterized in that in step 1), institute
Stating solvent is deionized water；
Preferably, the partial size of the graphene oxide is 10-300 μm；
Preferably, relative to the graphene oxide of 1g, the dosage of the solvent is 10-150mL, preferably 10-120mL,
More preferably 20-100mL.
3. graphene according to claim 1/copper composite radiating film preparation method, which is characterized in that in step 2), institute
Coating is stated to be coated by coating machine；
Preferably, the film speed of the coating machine is 20-100m/s, blade width 30-100mm, blade thickness 0.01-
10mm；
It is highly preferred that the film speed of the coating machine is 20-60m/s, blade width 30-70mm, blade thickness 0.1-
3mm。
4. graphene according to claim 3/copper composite radiating film preparation method, which is characterized in that the copper foil
With a thickness of 10-60 μm；
Preferably, the copper foil with a thickness of 20-50 μm；
Preferably, the compound wet coating of graphene oxide/copper with a thickness of 20-60 μm.
5. graphene according to claim 1/copper composite radiating film preparation method, which is characterized in that in step 3), institute
Stating dry condition includes: vacuum degree for 0-100Pa, and drying temperature is 70-120 DEG C, drying time 1-6h；
Preferably, it is 20-100Pa that the condition of the drying, which includes: vacuum degree, and drying temperature is 80-110 DEG C, and drying time is
2-4h。
6. graphene according to claim 1/copper composite radiating film preparation method, which is characterized in that in step 4), institute
Heat treatment is stated to carry out in high temperature furnace；
Preferably, the power of the high temperature furnace is 10-40KW；
Preferably, the condition of the heat treatment includes: that 300-500 DEG C is warming up in 10-20min, keeps the temperature 1-3h, is cooled to room
Temperature；
Preferably, the condition of the heat treatment includes: that 300-500 DEG C is warming up in 10-20min, keeps the temperature 2-3h, is cooled to room
Temperature；
Preferably, the inert gas is argon gas or nitrogen.
7. graphene according to claim 1/copper composite radiating film preparation method, which is characterized in that in step 4), institute
Hot pressing calendering is stated using hot pressing calender；
Preferably, it is 20-80MPa, heating rate 10-40 that the condition of the hot pressing calendering, which includes: the pressure of hot pressing calender,
DEG C/min, at 500-1000 DEG C keep the temperature 10-60min after, be cooled to room temperature.
8. graphene according to claim 7/copper composite radiating film preparation method, which is characterized in that in step 4), institute
Stating the pressure that the condition that hot pressing is rolled includes: hot pressing calender is 40-60MPa, and heating rate is 10-30 DEG C/min, in 600-
After keeping the temperature 10-40min at 900 DEG C, it is cooled to room temperature.
9. graphene made from the method as described in any one of claim 1-8/copper composite radiating film.
10. graphene as claimed in claim 9/copper composite radiating film is preparing the application in mobile phone and/or display.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113752666A (en) * | 2021-09-09 | 2021-12-07 | 昆明理工大学 | Preparation method of high-strength high-conductivity copper/graphene composite material |
| CN113860888A (en) * | 2021-11-04 | 2021-12-31 | 四川恒力盛泰石墨烯科技有限公司 | Preparation method of graphene heat dissipation film for electronic equipment |
| CN117702115A (en) * | 2024-02-05 | 2024-03-15 | 泰兴挚富新材料科技有限公司 | Graphene copper composite high-heat-conductivity film and preparation method thereof |
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Application publication date: 20190702 |