CN105086659A - Preparation method of high-thermal-conductivity nano carbon copper foil - Google Patents

Preparation method of high-thermal-conductivity nano carbon copper foil Download PDF

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CN105086659A
CN105086659A CN201510491809.3A CN201510491809A CN105086659A CN 105086659 A CN105086659 A CN 105086659A CN 201510491809 A CN201510491809 A CN 201510491809A CN 105086659 A CN105086659 A CN 105086659A
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copper foil
nano carbon
preparation
high heat
heat conducting
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CN105086659B (en
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屈洁昊
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Li Peng
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JIAXING ZHONGYI CARBON Technology Co Ltd
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Abstract

The invention relates to a preparation method of high-thermal-conductivity nano carbon copper foil. The method includes the following technological steps that a) binding agents are prepared; b) cooling slurry is prepared; c) coating and heating and drying treatment are performed, wherein the cooling slurry prepared in the b step is evenly coated to the surface of the copper foil, then the copper foil is heated and dried, and then the needed high-thermal-conductivity nano carbon copper foil can be obtained.

Description

The preparation method of high heat conducting nano carbon Copper Foil
Technical field
The present invention relates to a kind of preparation method of high-heat-conductive composite material, particularly a kind of preparation method of high heat conducting nano carbon Copper Foil.
Background technology
Along with the high speed development of microelectronics integrated technology, size, the volume of electronic devices and components sharply reduce, the heat radiation difficulty brought thus has badly influenced precision and the life-span of electron device, become the technical bottleneck of device miniaturization, constrain further developing of integrated technology to a great extent.Have data to show, temperature often raises 2 DEG C, and the stability of electron device reduces about 10%; If reach 50 DEG C, when so its life-span is only 25 DEG C about 17%.Therefore, carrying out dispelling the heat in time and efficiently to electron device is the key that it reliably uses.As metal, inorganic ceramic and metal oxide etc., though thermal conductivity is good, there is many defects, as single use metallic substance is difficult to meet the requirement such as insulativity, chemical stability in conventional thermal conductive material; Then there is the problems such as shock resistance difference, not easily processing in inorganic ceramic.Day by day grow up instantly in science and technology and national economy, having higher requirement to the functional diversity of thermally conductive material is also corresponding, having as required thermally conductive material that lightweight, easily machine-shaping, mechanical property are good, resistance to chemical attack, electrical isolation, over-all properties that low cost etc. is excellent.Conventional thermal conductive material cannot meet the growth requirement of industry and science and technology because of self limitation while using (be mainly manifested in single), high thermal conductivity flexible polymer interface material needed for electronic devices and components, and there is in chemical industry interchanger the lightweight thermal conductive polymer material etc. of remarkable resistance to chemical attack.
In the recent period, heat-conductive composite material is paid close attention to widely with advantages such as its low costs, easily processing, good mechanics and electrical insulating property, its application enumerates such as LED illumination, sun power, microelectronics, the electrically field such as electrician, aerospace especially, defines a kind of trend progressively replacing conventional thermal conductive material.So high-heat-conductive composite material and preparation method thereof becomes current study hotspot.
At present, high-heat-conductive composite material, based on filled-type, is about to have high thermal conductivity filler particle dispersion in macromolecule matrix, forms the matrix material with excellent mechanical and heat conductivility, its capacity of heat transmission available heat conductance is weighed, and the heat conductivility of the larger expression material of numerical value is better.For filled-in composite, thermal conductivity depends primarily on the intrinsic heat dispersion of macromolecule matrix and heat conductive filler, and the dispersion state of filler, and wherein the dispersiveness of heat conductive filler in macromolecule matrix is the important factor affecting material thermal conductivity.Based on the catalytic effect of Nano filling, nanoparticle is easier forms passage of heat in macromolecule matrix inside, reduces the porosity of material internal; Under the same terms, more can improve thermal conductivity and the mechanical property of material than micron particle, and resistance to fatigue is more excellent.But the easy agglomeration of nanoparticle seriously can hinder effective transmission of heat, therefore the scattering problem of nanoparticle becomes the difficult point studied in heat-conductive composite material preparation method.In addition, when amount of filler is less, isolate each other between filler grain, do not contact with each other, the thermal conductivity of system cannot significantly improve; Along with the increase of filler content, particle starts to contact with each other, and when exceeding the threshold value forming passage of heat, heat could carry out rapid diffusion through this passage, and the capacity of heat transmission of material just can significantly improve.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of preparation method of high heat conducting nano carbon Copper Foil, and it comprises following processing step:
A) configure binding agent: this binding agent comprises by weight percentage: 5 ~ 40% resins and 60 ~ 95% polar solvent, resin to be poured in polar solvent and at room temperature to stir 0.5 ~ 2 hour;
B) configuration heat radiation slurry: this heat radiation slurry comprises 1 ~ 20% Graphene, 1 ~ 15% carbon nanotube, 1 ~ 20% silicon carbide by weight percentage with, 2 ~ 25% boron nitride, 4 ~ 25% polar solvents and 5 ~ 20% the binding agent prepared by step a, first Graphene, carbon nanotube, silicon carbide, boron nitride being poured into respectively by above-mentioned weight percent is equipped with in the container of polar solvent, at room temperature stir 0.5 ~ 3 hour, then add in the binding agent prepared by step a of above-mentioned weight percent, continue stirring 2 ~ 8 hours;
C) coating and drying and processing: the heat radiation slurry even spread prepared by step b is to copper foil surface, and then heating, drying process, can obtain required high heat conducting nano carbon Copper Foil.
The present invention further technical characteristic is:
Resin in described step a is polyvinylidene difluoride (PVDF) or epoxy resin or urethane or polyacrylic ester.
When polar solvent in described step a and step b is N-Methyl pyrrolidone, in the heating, drying process of described step c, Heating temperature is 85 ~ 95 DEG C, and heat-up time is 2 ~ 10 minutes.
When polar solvent in described step a and step b is DMF, in the heating, drying process of described step c, Heating temperature is 75 ~ 85 DEG C, and heat-up time is 2 ~ 10 minutes.
When polar solvent in described step a and step b is acetone, in the heating, drying process of described step c, Heating temperature is 45 ~ 55 DEG C, and heat-up time is 2 ~ 10 minutes.
When polar solvent in described step a and step b is water, in the heating, drying process of described step c, Heating temperature is 65 ~ 75 DEG C, and heat-up time is 2 ~ 10 minutes.
The invention has the beneficial effects as follows:
Because binding agent of the present invention selects resin and polar solvent, membrane formation mechanism is volatilization film forming, and period, without any chemical reaction, makes the quality of finished product more stable; In addition, slurry configuration makes the dispersion of high heat conductive filler in macromolecule matrix more even, achieves the excellent dispersion of high heat conducting nano filler in binder system; Coating adopts smooth roll coating process in addition, heat radiation slurry is transferred to copper foil surface thus completes coating, can glue spread be controlled by the gap adjusting upper glue roller and coating roll, Painting effect is better, coat-thickness flexibly controlled, coating accuracy is high.
Embodiment
Embodiment 1:
A preparation method for high heat conducting nano carbon Copper Foil, it comprises following processing step:
A) binding agent is configured: poured in the N-Methyl pyrrolidone of 95% by 5% polyvinylidene difluoride (PVDF) by weight percentage, and at room temperature stir 0.5 ~ 2 hour;
B) configuration heat radiation slurry: 1% Graphene, 15% carbon nanotube, 20% silicon carbide are poured in 25%N-methyl-2-pyrrolidone with, 20% boron nitride by percentage by weight, at room temperature stir 0.5 ~ 3 hour, then add in the binding agent prepared by step a of 19%, continue stirring 2 ~ 8 hours;
C) coating and drying and processing: the heat radiation slurry light roll coating process even spread prepared by step b is to copper foil surface, then heating, drying process, Heating temperature is 85 ~ 95 DEG C, and heat-up time is 2 ~ 10 minutes, can obtain required high heat conducting nano carbon Copper Foil.
Embodiment 2:
A preparation method for high heat conducting nano carbon Copper Foil, it comprises following processing step:
A) binding agent is configured: poured in the DMF of 60% by 40% epoxy resin by weight percentage, and at room temperature stir 0.5 ~ 2 hour;
B) configuration heat radiation slurry: percentage pours 15% Graphene, 14% carbon nanotube, 1% silicon carbide into 25%N with, 25% boron nitride by weight, in dinethylformamide, at room temperature stir 0.5 ~ 3 hour, then add in the binding agent prepared by step a of 20%, continue stirring 2 ~ 8 hours;
C) coating and drying and processing: the heat radiation slurry light roll coating process even spread prepared by step b is to copper foil surface, then heating, drying process, Heating temperature is 75 ~ 85 DEG C, and heat-up time is 2 ~ 10 minutes, can obtain required high heat conducting nano carbon Copper Foil.
Embodiment 3:
A preparation method for high heat conducting nano carbon Copper Foil, it comprises following processing step:
A) binding agent is configured: poured in the acetone of 70% by 30% urethane by weight percentage, and at room temperature stir 0.5 ~ 2 hour;
B) configuration heat radiation slurry: 20% Graphene, 1% carbon nanotube, 15% silicon carbide are poured in 25% acetone with, 25% boron nitride by percentage by weight, at room temperature stir 0.5 ~ 3 hour, then add in the binding agent prepared by step a of 14%, continue stirring 2 ~ 8 hours;
C) coating and drying and processing: the heat radiation slurry light roll coating process even spread prepared by step b is to copper foil surface, then heating, drying process, Heating temperature is 45 ~ 55 DEG C, and heat-up time is 2 ~ 10 minutes, can obtain required high heat conducting nano carbon Copper Foil.
Embodiment 4:
A preparation method for high heat conducting nano carbon Copper Foil, it comprises following processing step:
A) binding agent is configured: poured in the water of 80% by 20% polyacrylic ester by weight percentage, and at room temperature stir 0.5 ~ 2 hour;
B) configuration heat radiation slurry: 19% Graphene, 14% carbon nanotube, 20% silicon carbide are poured in 25% water with, 2% boron nitride by percentage by weight, at room temperature stir 0.5 ~ 3 hour, then add in the binding agent prepared by step a of 20%, continue stirring 2 ~ 8 hours;
C) coating and drying and processing: the heat radiation slurry light roll coating process even spread prepared by step b is to copper foil surface, then heating, drying process, Heating temperature is 65 ~ 75 DEG C, and heat-up time is 2 ~ 10 minutes, can obtain required high heat conducting nano carbon Copper Foil.
Embodiment 5:
A preparation method for high heat conducting nano carbon Copper Foil, it comprises following processing step:
A) binding agent is configured: poured in the water of 85% by 15% polyacrylic ester by weight percentage, and at room temperature stir 0.5 ~ 2 hour;
B) configuration heat radiation slurry: 20% Graphene, 15% carbon nanotube, 20% silicon carbide are poured in 4% water with, 21% boron nitride by percentage by weight, at room temperature stir 0.5 ~ 3 hour, then add in the binding agent prepared by step a of 20%, continue stirring 2 ~ 8 hours;
C) coating and drying and processing: the heat radiation slurry light roll coating process even spread prepared by step b is to copper foil surface, then heating, drying process, Heating temperature is 65 ~ 75 DEG C, and heat-up time is 2 ~ 10 minutes, can obtain required high heat conducting nano carbon Copper Foil.
Embodiment 6:
A preparation method for high heat conducting nano carbon Copper Foil, it comprises following processing step:
A) binding agent is configured: poured in the DMF of 75% by 25% epoxy resin by weight percentage, and at room temperature stir 0.5 ~ 2 hour;
B) configuration heat radiation slurry: percentage pours 20% Graphene, 10% carbon nanotube, 20% silicon carbide into 20%N with, 25% boron nitride by weight, in dinethylformamide, at room temperature stir 0.5 ~ 3 hour, then add in the binding agent prepared by step a of 5%, continue stirring 2 ~ 8 hours;
C) coating and drying and processing: the heat radiation slurry light roll coating process even spread prepared by step b is to copper foil surface, then heating, drying process, Heating temperature is 75 ~ 85 DEG C, and heat-up time is 2 ~ 10 minutes, can obtain required high heat conducting nano carbon Copper Foil.
Because binding agent of the present invention selects resin and polar solvent, membrane formation mechanism is volatilization film forming, and period, without any chemical reaction, makes the quality of finished product more stable; In addition, slurry configuration makes the dispersion of high heat conductive filler in macromolecule matrix more even, achieves the excellent dispersion of high heat conducting nano filler in binder system; Coating adopts smooth roll coating process in addition, heat radiation slurry is transferred to copper foil surface thus completes coating, can glue spread be controlled by the gap adjusting upper glue roller and coating roll, Painting effect is better, coat-thickness flexibly controlled, coating accuracy is high.
Although describe embodiment herein, should be understood that, embodiment disclosed is here only exemplary of the present invention, and it can be presented as various forms.Therefore, here the detail disclosed is not considered to restrictive, and be only as the basis of claim and as instructing those skilled in the art differently to apply representational basis of the present invention in appropriate mode any in reality, the various features comprising employing disclosed here also combine the feature that may clearly not disclose here.Protection scope of the present invention is as the criterion with claims.

Claims (10)

1. a preparation method for high heat conducting nano carbon Copper Foil, is characterized in that comprising following processing step:
A) configure binding agent: this binding agent comprises by weight percentage: 5 ~ 40% resins and 60 ~ 95% polar solvent, resin to be poured in polar solvent and at room temperature to stir 0.5 ~ 2 hour;
B) configuration heat radiation slurry: this heat radiation slurry comprises 1 ~ 20% Graphene, 1 ~ 15% carbon nanotube, 1 ~ 20% silicon carbide by weight percentage with, 2 ~ 25% boron nitride, 4 ~ 25% polar solvents and 5 ~ 20% the binding agent prepared by step a, first Graphene, carbon nanotube, silicon carbide, boron nitride being poured into respectively by above-mentioned weight percent is equipped with in the container of polar solvent, at room temperature stir 0.5 ~ 3 hour, then add in the binding agent prepared by step a of above-mentioned weight percent, continue stirring 2 ~ 8 hours;
C) coating and heating, drying process: the heat radiation slurry even spread prepared by step b is to copper foil surface, and then heating, drying process, can obtain required high heat conducting nano carbon Copper Foil.
2. the preparation method of high heat conducting nano carbon Copper Foil as claimed in claim 1, is characterized in that: the resin in described step a is polyvinylidene difluoride (PVDF) or epoxy resin or urethane or polyacrylic ester.
3. the preparation method of high heat conducting nano carbon Copper Foil as claimed in claim 1 or 2, is characterized in that: the polar solvent in described step a and step b is N-Methyl pyrrolidone.
4. the preparation method of high heat conducting nano carbon Copper Foil as claimed in claim 3, it is characterized in that: in the heating, drying process of described step c, Heating temperature is 85 ~ 95 DEG C, and heat-up time is 2 ~ 10 minutes.
5. the preparation method of high heat conducting nano carbon Copper Foil as claimed in claim 1 or 2, is characterized in that: the polar solvent in described step a and step b is DMF.
6. the preparation method of high heat conducting nano carbon Copper Foil as claimed in claim 5, it is characterized in that: in the heating, drying process of described step c, Heating temperature is 75 ~ 85 DEG C, and heat-up time is 2 ~ 10 minutes.
7. the preparation method of high heat conducting nano carbon Copper Foil as claimed in claim 1 or 2, is characterized in that: the polar solvent in described step a and step b is acetone.
8. the preparation method of high heat conducting nano carbon Copper Foil as claimed in claim 7, it is characterized in that: in the heating, drying process of described step c, Heating temperature is 45 ~ 55 DEG C, and heat-up time is 2 ~ 10 minutes.
9. the preparation method of high heat conducting nano carbon Copper Foil as claimed in claim 1 or 2, is characterized in that: the polar solvent in described step a and step b is water.
10. the preparation method of high heat conducting nano carbon Copper Foil as claimed in claim 9, it is characterized in that: in the heating, drying process of described step c, Heating temperature is 65 ~ 75 DEG C, and heat-up time is 2 ~ 10 minutes.
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Cited By (5)

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CN106221396A (en) * 2016-08-12 2016-12-14 德阳烯碳科技有限公司 A kind of Graphene heat radiation coating and preparation method thereof
CN107216726A (en) * 2016-03-21 2017-09-29 华越科技股份有限公司 The preparation method of thermal dispersant coatings and its made heat dissipation metal composite membrane
CN109608986A (en) * 2018-12-10 2019-04-12 中昊北方涂料工业研究设计院有限公司 A kind of heat exchanger graphene high thermal conductivity anticorrosive paint and preparation method thereof
CN109988484A (en) * 2019-03-14 2019-07-09 上海利物盛纳米科技有限公司 A kind of graphene water-based cooling coating and preparation method thereof
CN110105828A (en) * 2019-04-28 2019-08-09 苏州格瑞丰纳米科技有限公司 A kind of graphene slurry, preparation method and application for metal coating

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CN109608986A (en) * 2018-12-10 2019-04-12 中昊北方涂料工业研究设计院有限公司 A kind of heat exchanger graphene high thermal conductivity anticorrosive paint and preparation method thereof
CN109988484A (en) * 2019-03-14 2019-07-09 上海利物盛纳米科技有限公司 A kind of graphene water-based cooling coating and preparation method thereof
CN110105828A (en) * 2019-04-28 2019-08-09 苏州格瑞丰纳米科技有限公司 A kind of graphene slurry, preparation method and application for metal coating

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