CN106179923B - The preparation method of graphene metallic composite - Google Patents
The preparation method of graphene metallic composite Download PDFInfo
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- CN106179923B CN106179923B CN201610541944.9A CN201610541944A CN106179923B CN 106179923 B CN106179923 B CN 106179923B CN 201610541944 A CN201610541944 A CN 201610541944A CN 106179923 B CN106179923 B CN 106179923B
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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
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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
- 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
- B05D3/02—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 baking
- B05D3/0254—After-treatment
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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
- 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
- B05D3/12—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 mechanical means
-
- 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
- B05D5/10—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain an adhesive surface
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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
- B05D7/24—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 for applying particular liquids or other fluent materials
-
- 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
- B05D7/50—Multilayers
- B05D7/52—Two layers
- B05D7/54—No clear coat specified
- B05D7/542—No clear coat specified the two layers being cured or baked together
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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
- B05D2202/00—Metallic substrate
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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
- B05D2451/00—Type of carrier, type of coating (Multilayers)
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- Engineering & Computer Science (AREA)
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- Carbon And Carbon Compounds (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention belongs to heat sink material preparation fields, and in particular to a kind of preparation method of graphene metallic composite.Graphene is prepared into graphene slurry by being ultrasonically treated dispersion in a solvent, one layer of adhesive is coated in clean metal material surface, solvent is removed after surface of pressure-sensitive adhesive coats one layer of graphene slurry, graphene is set to be attached to surface of pressure-sensitive adhesive, being then fed into rolling equipment and carrying out pressing makes the even closer of graphene and metal bonding, and increases graphene compacted density.This method preparation process is simple, and the graphene layer thickness controllability for the graphene metal material being prepared is high, industrially scalable production.
Description
Technical field
The present invention relates to a kind of preparation methods of graphene metallic composite.
Technical background
Graphene is 2004 isolated from fragment graphite by a simple method, it is a kind of with single
Layer carbon atom forms special novel carbon group material, therefore finder obtains the Nobel Prize in physics in 2010 years.With
Graphene is found, and the conclusion that single layer atom cannot form independent molecule is broken, and scientific circles cause great disturbance.With stone
Black alkene is found, and has been proved many unique performances, according to the thermal diffusivity of high electric conductivity, the intensity of superelevation, superelevation
Energy is equal, causes the concern of every profession and trade scholar and brainstrust.
In terms of thermodynamics, graphene shows extremely excellent performance, and average conduction is 6000W/ (mK),
Much higher than all Heat Conduction Materials being currently known.Graphene heating conduction is although excellent, but the use of industrial application also
There is difficulties, because the bad mechanical strength of simple graphene, needs basis material to support, wherein metal base is a kind of comparison
Good selection, and the preparation method of graphene metallic composite is not met by requirement at present.A kind of preparation method is chemistry
Vapour deposition process can deposit single layer or few layer graphene in metal surface, and heat dissipation performance is excellent, but it prepares somewhat expensive,
Preparation process is complicated, can not industrially scalable production.Another method is that graphene and metal powder are added as heat dissipation powder
Into heat radiation coating, heat dissipation performance also can be improved, but its heat dissipation performance is poor, is only applicable to coating industry.
Summary of the invention
The object of the present invention is to provide a kind of preparation method preparation process is simple, preparation cost is cheap, can be mass-produced,
The preparation method of the stronger graphene metallic composite of practicability.The technical scheme is that a kind of graphene metal is multiple
The preparation method of condensation material, step 1: solvent is added in the Graphene powder that partial size is 100-3000 mesh, the amount of solvent is graphene
10-100 times of quality, ultrasonic disperse prepare graphene slurry；
Step 2: in one layer of adhesive of clean metal material surface roller coating, with a thickness of 3-30 μm；
Step 3: the graphene slurry prepared in step 1 is rolled onto the one side that metal material in step 2 is coated with adhesive,
The material of preparation is dried, rolling equipment is then fed into, it is closer in conjunction with adhesive to make graphene layer, and increase graphite
Alkene compacted density to get arrive graphene metallic composite.
Graphene powder described in step 1 be mechanical stripping graphene, redox graphene, graphene oxide wherein one
Kind, the number of plies of graphene used is 5-100 layers.
Solvent in step 1 is N-Methyl pyrrolidone, N,N-dimethylformamide, dioxane, water, ethyl alcohol, second two
Alcohol, butanone, any one in toluene.
Ultrasonic power is 200-800W in step 1, and ultrasonic temperature is 30-90 DEG C, ultrasonic time 1-4h.
In step 2 metal be copper, aluminium, iron or tinplate any of them, the metal layer with a thickness of 10-300 μm.
Pressure is 200-500 tons when graphene layer and adhesive press in step 3, and linear velocity is 2-15m/min.
Advantageous effects of the invention:
(1) graphene slurry is prepared using the method for the invention, coats slurry after adhesive is arranged in metal surface
Up, it is pressed after drying, prepares the excellent graphene metal heat dissipation material of heat dissipation performance.
(2) the graphene thickness of metal surface can be adjusted by the concentration and roller coating technology condition of graphene slurry, from
And prepare the graphene metallic composite for adapting to different purposes.
(3) the production method simple production process, controllability are high, application is strong, industrially scalable production.
The present invention passes through the dense of graphene slurry by preparing graphene slurry by adhesive for graphene and metal composite
Graphene layer thickness, while the graphene of the graphene metallic composite of this method preparation is adjusted in degree and roller coating technology condition
Layer uniform ground, thus it is also more uniform to radiate.Preparation process is simple compared with remaining preparation method, and cost is less expensive, can work
Industryization large-scale production, it is practical.
Detailed description of the invention
Fig. 1 is the rate of heat dissipation table of graphene metallic composite obtained by embodiment 1-8
Specific embodiment
A kind of preparation method of graphene metallic composite:
Step 1: solvent is added in the Graphene powder that partial size is 100-3000 mesh, the amount of solvent is the 10- of graphene quality
100 times, ultrasonic disperse prepares graphene slurry；
Step 2: in one layer of adhesive of clean metal material surface roller coating, with a thickness of 3-30 μm；
Step 3: the graphene slurry prepared in step 1 is rolled onto the one side that metal material in step 2 is coated with adhesive,
The material of preparation is dried, rolling equipment is then fed into, it is closer in conjunction with adhesive to make graphene layer, and increase graphite
Alkene compacted density to get arrive graphene metallic composite.
Graphene powder described in step 1 be mechanical stripping graphene, redox graphene, graphene oxide wherein one
Kind, the number of plies of graphene used is 5-100 layers.
Solvent in step 1 is N-Methyl pyrrolidone, N,N-dimethylformamide, dioxane, water, ethyl alcohol, second two
Alcohol, butanone, any one in toluene.
Ultrasonic power is 200-800W in step 1, and ultrasonic temperature is 30-90 DEG C, ultrasonic time 1-4h.
In step 2 metal be copper, aluminium, iron or tinplate any of them, the metal layer with a thickness of 10-300 μm.
Pressure is 200-500 tons when graphene layer and adhesive press in step 3, and linear velocity is 2-15m/min.
In order to make the objectives, technical solutions, and advantages of the present invention clearer, the present invention is carried out below further
Detailed description.It should be appreciated that specific embodiment described herein is used only for explaining the present invention, it is not used to limit this hair
It is bright.On the contrary, the present invention covers any substitution made in the scope of the present invention being defined by the claims, modification, equivalent method
And scheme.
Embodiment 1
Taking partial size is the mechanical stripping graphene 10kg of 100 mesh, and graphene number of plies is 5 layers, and mechanical stripping graphene is added
N-Methyl pyrrolidone 100kg.Ultrasonic disperse, ultrasonic power 200W, 30 DEG C of temperature, ultrasonic time 4h.In clean 10 μm of copper
Foil surface coats one layer of thermal paste as gluing oxidant layer, and coating thickness is 3 μm.Graphene slurry is rolled onto copper foil and is coated with gluing
The one side of agent.Then it is baked to, then rolling equipment will be sent into after material after drying, pressure is 200 tons when pressing, and linear velocity is
2m/min keeps graphene layer closer in conjunction with adhesive.
Embodiment 2
Taking partial size is the mechanical stripping graphene 10kg of 150 mesh, and 10 layers of graphene number of plies, N is added in mechanical stripping graphene,
Dinethylformamide 200kg.Ultrasonic disperse, ultrasonic power 200W, 90 DEG C of temperature, ultrasonic time 4h.In clean 300 μm of copper
Foil surface coats one layer of thermal paste as gluing oxidant layer, and coating thickness is 30 μm.Graphene slurry is rolled onto copper foil and is coated with glue
The one side of stick.Then it is baked to, then rolling equipment will be sent by material after drying, pressure is 250 tons when pressing, and linear velocity is
4m/min keeps graphene layer closer in conjunction with adhesive.
Embodiment 3
Taking partial size is the mechanical stripping graphene 10kg of 400 mesh, and 100 layers of graphene number of plies, mechanical stripping graphene is added
Dioxane 200kg.Ultrasonic disperse, ultrasonic power 400W, temperature 50 C, ultrasonic time 3h.In clean 150 μm of aluminium foil surfaces
One layer of thermal paste is coated as gluing oxidant layer, coating thickness is 20 μm.Graphene slurry is rolled onto aluminium foil and is coated with adhesive
On one side.Then it is baked to, then rolling equipment will be sent by material after drying, pressure is 300 tons when pressing, linear velocity 10m/
Min keeps graphene layer closer in conjunction with adhesive.
Embodiment 4
Taking partial size is the redox graphene 10kg of 800 mesh, and graphene number of plies is 50 layers, and redox graphene is added
Water 400kg.Ultrasonic disperse, ultrasonic power 600W, 30 DEG C of temperature, ultrasonic time 2h.One is coated on clean 200 μm of iron foil surfaces
For layer thermal paste as gluing oxidant layer, coating thickness is 10 μm.Graphene slurry is rolled onto the one side that iron foil is coated with adhesive.So
After be baked to, then rolling equipment will be sent by material after drying, pressure is 400 tons, linear velocity 12m/min when pressing, makes stone
Black alkene layer is closer in conjunction with adhesive.
Embodiment 5
Taking partial size is the mechanical stripping graphene 10kg of 1000 mesh, and 40 layers of graphene number of plies, mechanical stripping graphene is added
Ethyl alcohol 50kg.Ultrasonic disperse, ultrasonic power 600W, temperature 60 C, ultrasonic time 1h.It is applied on clean 250 μm of tinplate surfaces
One layer of thermal paste is covered as gluing oxidant layer, and coating thickness is 15 μm.Graphene slurry is rolled onto tinplate and is coated with adhesive
On one side.Then it is baked to, then rolling equipment will be sent by material after drying, pressure is 500 tons when pressing, linear velocity 15m/
Min keeps graphene layer closer in conjunction with adhesive.
Embodiment 6
Taking partial size is 1500 graphene oxide 10kg, and 10 layers of graphene number of plies, ethylene glycol 1000kg is added in graphene oxide.
Ultrasonic disperse, ultrasonic power 600W, 30 DEG C of temperature, ultrasonic time 2h.One layer of thermal paste is coated on clean 80 μm of silver foil surfaces
As gluing oxidant layer, coating thickness is 25 μm.Graphene slurry is rolled onto the one side that silver foil is coated with adhesive.Then it is dried
Dry, then will be sent into rolling equipment by material after drying, pressure is 400 tons, linear velocity 10m/min when pressing, make graphene layer with
Adhesive combines closer.
Embodiment 7
Taking partial size is the redox graphene 10kg of 3000 mesh, and 30 layers of graphene number of plies, redox graphene is added
Butanone 800kg.Ultrasonic disperse, ultrasonic power 500W, 30 DEG C of temperature, ultrasonic time 1h.It is coated on clean 50 μm of tinfoil paper surfaces
For one layer of thermal paste as gluing oxidant layer, coating thickness is 25 μm.Graphene slurry is rolled onto the one side that tinfoil paper is coated with adhesive.
Then it is baked to, then rolling equipment will be sent by material after drying, pressure is 250 tons, linear velocity 8m/min when pressing, makes stone
Black alkene layer is closer in conjunction with adhesive.
Embodiment 8
Taking partial size is 800 mesh mechanical stripping Graphene powder 10kg, and graphene number of plies is 40 layers, and mechanical stripping Graphene powder adds
Enter toluene 500kg.Ultrasonic disperse, ultrasonic power 500W, 30 DEG C of temperature, ultrasonic time 2h.It is applied on clean 40 μm of tinfoil paper surfaces
One layer of thermal paste is covered as gluing oxidant layer, and coating thickness is 20 μm.Graphene slurry is rolled onto one that tinfoil paper is coated with adhesive
Face.Then it being baked to, then rolling equipment will be sent by material after drying, pressure is 350 tons, linear velocity 9m/min when pressing,
Keep graphene layer closer in conjunction with adhesive.
Claims (1)
1. a kind of preparation method of graphene metallic composite, it is characterized in that:
Step 1: solvent is added in the Graphene powder that partial size is 100-3000 mesh, the amount of solvent is the 10-100 of graphene quality
Times, ultrasonic disperse prepares graphene slurry；
Step 2: in one layer of adhesive of clean metal material surface roller coating, the adhesive is thermal paste, micro- with a thickness of 3-30
Rice；
Step 3: the graphene slurry prepared in step 1 being rolled onto the one side that metal material in step 2 is coated with adhesive, will be made
Standby material drying, is then fed into rolling equipment, it is closer in conjunction with adhesive to make graphene layer, and increase graphene pressure
Real density to get arrive graphene metallic composite；Graphene powder described in step 1 is mechanical stripping graphene, reduction-oxidation
The one of which of graphene, graphene oxide, the number of plies of graphene used are 5-100 layers；Solvent in step 1 is N- methyl pyrrole
Pyrrolidone, N,N-dimethylformamide, dioxane, water, ethyl alcohol, ethylene glycol, butanone, any one in toluene；In step 1
Ultrasonic power is 200-800W, and ultrasonic temperature is 30-90 DEG C, ultrasonic time 1-4h；In step 2 metal be copper, aluminium, iron its
In any one, metal layer with a thickness of 10-300 microns；Pressure is 200- when graphene layer and adhesive press in step 3
500 tons, linear velocity is 2-15 m/min.
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| CN201610541944.9A CN106179923B (en) | 2016-07-11 | 2016-07-11 | The preparation method of graphene metallic composite |
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| CN201610541944.9A CN106179923B (en) | 2016-07-11 | 2016-07-11 | The preparation method of graphene metallic composite |
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| CN106179923A CN106179923A (en) | 2016-12-07 |
| CN106179923B true CN106179923B (en) | 2019-07-05 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108717887B (en) * | 2018-04-04 | 2023-06-30 | 中国航发北京航空材料研究院 | Anisotropic graphene metal composite wire and preparation method thereof |
| CN109225773A (en) * | 2018-11-09 | 2019-01-18 | 西安康普瑞新材料科技有限公司 | Graphene sterilization material preparation method and graphene composite purification material preparation method |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104085143A (en) * | 2014-05-29 | 2014-10-08 | 深圳市铭晶科技有限公司 | Preparation method of composite heat conduction graphene film and composite heat conduction graphene film |
| CN104129783A (en) * | 2014-08-04 | 2014-11-05 | 中国科学院金属研究所 | Low cost clean nondestructive transfer method of large area of graphene |
| CN104475316A (en) * | 2014-12-03 | 2015-04-01 | 林前锋 | Preparing method of graphene coating |
| CN105239061A (en) * | 2015-09-25 | 2016-01-13 | 中国科学院宁波材料技术与工程研究所 | Graphene/metal composite thin film and preparation method thereof |
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- 2016-07-11 CN CN201610541944.9A patent/CN106179923B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104085143A (en) * | 2014-05-29 | 2014-10-08 | 深圳市铭晶科技有限公司 | Preparation method of composite heat conduction graphene film and composite heat conduction graphene film |
| CN104129783A (en) * | 2014-08-04 | 2014-11-05 | 中国科学院金属研究所 | Low cost clean nondestructive transfer method of large area of graphene |
| CN104475316A (en) * | 2014-12-03 | 2015-04-01 | 林前锋 | Preparing method of graphene coating |
| CN105239061A (en) * | 2015-09-25 | 2016-01-13 | 中国科学院宁波材料技术与工程研究所 | Graphene/metal composite thin film and preparation method thereof |
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