CN106179923A - The preparation method of Graphene metallic composite - Google Patents

The preparation method of Graphene metallic composite Download PDF

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Publication number
CN106179923A
CN106179923A CN201610541944.9A CN201610541944A CN106179923A CN 106179923 A CN106179923 A CN 106179923A CN 201610541944 A CN201610541944 A CN 201610541944A CN 106179923 A CN106179923 A CN 106179923A
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graphene
preparation
layer
metallic composite
adhesive
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CN201610541944.9A
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CN106179923B (en
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任睿
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Heilongjiang Carbon Era Graphene Technology Co Ltd
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Heilongjiang Carbon Era Graphene Technology Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D7/00Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B05D7/14Processes, 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D3/00Pretreatment 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
    • B05D3/02Pretreatment 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
    • B05D3/0254After-treatment
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D3/00Pretreatment 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
    • B05D3/12Pretreatment 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D5/00Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
    • B05D5/10Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain an adhesive surface
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D7/00Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B05D7/24Processes, 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D7/00Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B05D7/50Multilayers
    • B05D7/52Two layers
    • B05D7/54No clear coat specified
    • B05D7/542No clear coat specified the two layers being cured or baked together
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D2202/00Metallic substrate
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D2451/00Type of carrier, type of coating (Multilayers)

Abstract

The invention belongs to heat sink material preparation field, be specifically related to the preparation method of a kind of Graphene metallic composite.Disperse to prepare Graphene slurry in a solvent by supersound process by Graphene, at clean metal material surface one layer of adhesive of coating, after surface of pressure-sensitive adhesive coats a layer graphene slurry, solvent is removed, Graphene is made to be attached to surface of pressure-sensitive adhesive, it is then fed into rolling equipment to carry out pressing and make combined with metal more tight of Graphene, and increases Graphene compacted density.This method preparation technology is simple, and the Graphene layer thickness controllability of the Graphene metal material prepared is high, and industrially scalable produces.

Description

The preparation method of Graphene metallic composite
Technical field
The present invention relates to the preparation method of a kind of Graphene metallic composite.
Technical background
Graphene is to pass through simple method isolated from fragment graphite in 2004, and it is that one has list The novel carbon group material that layer carbon atom composition is special, therefore finder obtains the Nobel Prize in physics in 2010 years.Along with Graphene is found, and monolayer atom can not form the conclusion of independent molecule and be broken, and scientific circles cause great disturbance.Along with stone Ink alkene is found, and is proved a lot of unique performance, according to high electric conductivity, the intensity of superelevation, the thermal diffusivity of superelevation Can etc., cause the concern of every profession and trade scholar and brainstrust.
In terms of thermodynamics, Graphene shows extremely excellent performance, and its average conduction is 6000W/ (m K), Far above all Heat Conduction Materials being currently known.Although Graphene heat conductivility is excellent, but industrial application use also There is difficulty, because the bad mechanical strength of simple Graphene, need matrix material support, wherein metal base is that one compares 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 be at metal surface deposition monolayer or few layer graphene, and heat dispersion is excellent, but it prepares somewhat expensive, Complicated process of preparation, can not produce by industrially scalable.Another kind of method is to be added as heat radiation powder with metal powder by Graphene In heat radiation coating, it is possible to improve heat dispersion, but its heat dispersion is poor, is only applicable to coating industry.
Summary of the invention
It is an object of the invention to provide a kind of preparation method preparation technology simple, preparation cost is cheap, can be mass-produced, The preparation method of the Graphene metallic composite that practicality is stronger.The technical scheme is that a kind of Graphene metal is multiple The preparation method of condensation material, step 1: the Graphene powder that particle diameter is 100-3000 mesh is added solvent, and the amount of solvent is Graphene 10-100 times of quality, ultrasonic disperse prepares Graphene slurry;
Step 2: at one layer of adhesive of clean metal material surface roller coat, thickness is 3-30 μm;
Step 3: the Graphene slurry of preparation in step 1 is rolled onto metal material in step 2 and scribbles the one side of adhesive, This material of preparation is dried, is then fed into rolling equipment, make that graphene layer is combined with adhesive more closely, and increase graphite Alkene compacted density, i.e. obtains Graphene metallic composite.
Graphene powder described in step 1 be mechanical stripping Graphene, redox graphene, wherein the one of graphene oxide Kind, the number of plies of Graphene used is 5-100 layer.
Solvent in step 1 is N-Methyl pyrrolidone, N,N-dimethylformamide, dioxane, water, ethanol, second two Any one in alcohol, butanone, toluene.
In step 1, ultrasonic power is 200-800W, and ultrasonic temperature is 30-90 DEG C, and ultrasonic time is 1-4h.
In step 2, metal is copper, aluminum, ferrum or tinplate any of which, and the thickness of described metal level is 10-300 μm.
In step 3, when graphene layer and adhesive pressing, pressure is 200-500 ton, and linear velocity is 2-15m/min.
The Advantageous Effects of the present invention:
(1) utilize the method for the invention to prepare Graphene slurry, after metal surface arranges adhesive, slurry is coated Up, pressing after drying, prepare heat dispersion excellence Graphene heat dissipation metal material.
(2) the Graphene thickness of metal surface can be regulated by the concentration of Graphene slurry and roller coating technology condition, from And prepare the Graphene metallic composite adapting to different purposes.
(3) this production method production technology is simple, controllability is high, application is strong, industrially scalable produce.
The present invention by preparing Graphene slurry by adhesive by Graphene and metal composite, dense by Graphene slurry Degree and roller coating technology condition scalable graphene layer thickness, the Graphene of the Graphene metallic composite that simultaneously prepared by the method Layer uniform ground, thus heat radiation is the most uniform.Preparation technology is simple compared with remaining preparation method, and cost is less expensive, can work Industry large-scale production, practical.
Accompanying drawing explanation
Fig. 1 is the rate of heat dissipation table of Graphene metallic composite obtained by embodiment 1-8
Detailed description of the invention
A kind of preparation method of Graphene metallic composite:
Step 1: the Graphene powder that particle diameter is 100-3000 mesh is added solvent, and the amount of solvent is the 10-of Graphene quality 100 times, ultrasonic disperse prepares Graphene slurry;
Step 2: at one layer of adhesive of clean metal material surface roller coat, thickness is 3-30 μm;
Step 3: the Graphene slurry of preparation in step 1 is rolled onto metal material in step 2 and scribbles the one side of adhesive, This material of preparation is dried, is then fed into rolling equipment, make that graphene layer is combined with adhesive more closely, and increase graphite Alkene compacted density, i.e. obtains Graphene metallic composite.
Graphene powder described in step 1 be mechanical stripping Graphene, redox graphene, wherein the one of graphene oxide Kind, the number of plies of Graphene used is 5-100 layer.
Solvent in step 1 is N-Methyl pyrrolidone, N,N-dimethylformamide, dioxane, water, ethanol, second two Any one in alcohol, butanone, toluene.
In step 1, ultrasonic power is 200-800W, and ultrasonic temperature is 30-90 DEG C, and ultrasonic time is 1-4h.
In step 2, metal is copper, aluminum, ferrum or tinplate any of which, and the thickness of described metal level is 10-300 μm.
In step 3, when graphene layer and adhesive pressing, pressure is 200-500 ton, and linear velocity is 2-15m/min.
In order to make the purpose of the present invention, technical scheme and advantage clearer, below the present invention is carried out further Describe in detail.Should be appreciated that specific embodiment described herein is used only for explaining the present invention, be not used to limit this Bright.On the contrary, the present invention contain any be defined by the claims the replacement made in the scope of the present invention, amendment, equivalent method And scheme.
Embodiment 1
Taking the mechanical stripping Graphene 10kg that particle diameter is 100 mesh, the Graphene number of plies is 5 layers, and mechanical stripping Graphene adds N-Methyl pyrrolidone 100kg.Ultrasonic disperse, ultrasonic power is 200W, temperature 30 DEG C, ultrasonic time 4h.At clean 10 μm copper One layer of thermal paste of paper tinsel surface-coated is as adhesive layer, and coating thickness is 3 μm.Graphene slurry is rolled onto Copper Foil and scribbles gluing The one side of agent.Then being baked to, then send into rolling equipment after material after drying, during pressing, pressure is 200 tons, and linear velocity is 2m/min, make that graphene layer is combined with adhesive is tightr.
Embodiment 2
Taking the mechanical stripping Graphene 10kg that particle diameter is 150 mesh, the Graphene number of plies 10 layers, mechanical stripping Graphene adds N, Dinethylformamide 200kg.Ultrasonic disperse, ultrasonic power is 200W, temperature 90 DEG C, ultrasonic time 4h.At clean 300 μm copper One layer of thermal paste of paper tinsel surface-coated is as adhesive layer, and coating thickness is 30 μm.Graphene slurry is rolled onto Copper Foil and scribbles glue The one side of stick.Then being baked to, then material after drying is sent into rolling equipment, during pressing, pressure is 250 tons, and linear velocity is 4m/min, make that graphene layer is combined with adhesive is tightr.
Embodiment 3
Taking the mechanical stripping Graphene 10kg that particle diameter is 400 mesh, the Graphene number of plies 100 layers, mechanical stripping Graphene adds Dioxane 200kg.Ultrasonic disperse, ultrasonic power is 400W, temperature 50 C, ultrasonic time 3h.At clean 150 μm aluminium foil surfaces Coating one layer of thermal paste as adhesive layer, coating thickness is 20 μm.Graphene slurry is rolled onto aluminium foil and scribbles adhesive Simultaneously.Then being baked to, then material after drying is sent into rolling equipment, during pressing, pressure is 300 tons, and linear velocity is 10m/ Min, make that graphene layer is combined with adhesive is tightr.
Embodiment 4
Taking the redox graphene 10kg that particle diameter is 800 mesh, the Graphene number of plies is 50 layers, and redox graphene adds Water 400kg.Ultrasonic disperse, ultrasonic power is 600W, temperature 30 DEG C, ultrasonic time 2h.In clean 200 μm iron foil surface-coated one Layer thermal paste is as adhesive layer, and coating thickness is 10 μm.Graphene slurry is rolled onto iron foil and scribbles the one side of adhesive.So After be baked to, then will dry after material send into rolling equipment, during pressing, pressure is 400 tons, and linear velocity is 12m/min, makes stone It is tightr that ink alkene layer is combined with adhesive.
Embodiment 5
Taking the mechanical stripping Graphene 10kg that particle diameter is 1000 mesh, the Graphene number of plies 40 layers, mechanical stripping Graphene adds Ethanol 50kg.Ultrasonic disperse, ultrasonic power is 600W, temperature 60 C, ultrasonic time 1h.It is coated with on clean 250 μm tinplate surfaces Covering one layer of thermal paste as adhesive layer, coating thickness is 15 μm.Graphene slurry is rolled onto tinplate and scribbles adhesive Simultaneously.Then being baked to, then material after drying is sent into rolling equipment, during pressing, pressure is 500 tons, and linear velocity is 15m/ Min, make that graphene layer is combined with adhesive is tightr.
Embodiment 6
Taking particle diameter is 1500 graphene oxide 10kg, the Graphene number of plies 10 layers, and graphene oxide adds ethylene glycol 1000kg. Ultrasonic disperse, ultrasonic power is 600W, temperature 30 DEG C, ultrasonic time 2h.In clean 80 one layer of thermal paste of μm native silver surface-coated As adhesive layer, coating thickness is 25 μm.Graphene slurry is rolled onto native silver and scribbles the one side of adhesive.Then dried Dry, then rolling equipment sent into by material after drying, during pressing, pressure is 400 tons, and linear velocity is 10m/min, make graphene layer with It is tightr that adhesive combines.
Embodiment 7
Take the redox graphene 10kg that particle diameter is 3000 mesh, the Graphene number of plies 30 layers, redox graphene, add Butanone 800kg.Ultrasonic disperse, ultrasonic power is 500W, temperature 30 DEG C, ultrasonic time 1h.In clean 50 μm tinfoil paper surface-coated One layer of thermal paste is as adhesive layer, and coating thickness is 25 μm.Graphene slurry is rolled onto tinfoil paper and scribbles the one side of adhesive. Then being baked to, then material after drying is sent into rolling equipment, during pressing, pressure is 250 tons, and linear velocity is 8m/min, makes stone It is tightr that ink alkene layer is combined with adhesive.
Embodiment 8
Taking particle diameter is 800 mesh mechanical stripping Graphene powder 10kg, and the Graphene number of plies is 40 layers, and mechanical stripping Graphene powder adds Enter toluene 500kg.Ultrasonic disperse, ultrasonic power is 500W, temperature 30 DEG C, ultrasonic time 2h.It is coated with on clean 40 μm tinfoil paper surfaces Covering one layer of thermal paste as adhesive layer, coating thickness is 20 μm.Graphene slurry is rolled onto tinfoil paper and scribbles the one of adhesive Face.Then being baked to, then material after drying is sent into rolling equipment, during pressing, pressure is 350 tons, and linear velocity is 9m/min, Make that graphene layer is combined with adhesive is tightr.

Claims (6)

1. a preparation method for Graphene metallic composite, is characterized in that:
Step 1: the Graphene powder that particle diameter is 100-3000 mesh is added solvent, and the amount of solvent is the 10-100 of Graphene quality Times, ultrasonic disperse prepares Graphene slurry;
Step 2: at one layer of adhesive of clean metal material surface roller coat, thickness is 3-30 μm;
Step 3: the Graphene slurry of preparation in step 1 is rolled onto metal material in step 2 and scribbles the one side of adhesive, will system Standby this material is dried, and is then fed into rolling equipment, make that graphene layer is combined with adhesive more closely, and increase Graphene pressure Real density, i.e. obtains Graphene metallic composite.
The preparation method of Graphene metallic composite the most according to claim 1, is characterized in that: graphite described in step 1 Alkene powder body is the one of which of mechanical stripping Graphene, redox graphene, graphene oxide, and the number of plies of Graphene used is 5-100 layer.
The preparation method of a kind of Graphene metallic composite the most according to claim 1, is characterized in that: in step 1 Solvent is appointing in N-Methyl pyrrolidone, N,N-dimethylformamide, dioxane, water, ethanol, ethylene glycol, butanone, toluene Meaning one.
The preparation method of a kind of Graphene metallic composite the most according to claim 1, is characterized in that: super in step 1 Acoustical power is 200-800W, and ultrasonic temperature is 30-90 DEG C, and ultrasonic time is 1-4h.
Method the most according to claim 1, the preparation method of a kind of Graphene metallic composite, it is characterized in that: step 2 Middle metal is copper, aluminum, ferrum or tinplate any of which, and the thickness of described metal level is 10-300 μm.
Method the most according to claim 1, the preparation method of a kind of Graphene metallic composite, it is characterized in that: step 3 When middle graphene layer and adhesive pressing, pressure is 200-500 ton, and linear velocity is 2-15m/min.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108717887A (en) * 2018-04-04 2018-10-30 北京石墨烯技术研究院有限公司 A kind of anisotropic graphite alkene metal composite conducting 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)

* Cited by examiner, † Cited by third party
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

Patent Citations (4)

* Cited by examiner, † Cited by third party
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

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108717887A (en) * 2018-04-04 2018-10-30 北京石墨烯技术研究院有限公司 A kind of anisotropic graphite alkene metal composite conducting wire and preparation method thereof
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

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