CN105086659B - The preparation method of high heat conducting nano carbon copper foil - Google Patents

The preparation method of high heat conducting nano carbon copper foil Download PDF

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CN105086659B
CN105086659B CN201510491809.3A CN201510491809A CN105086659B CN 105086659 B CN105086659 B CN 105086659B CN 201510491809 A CN201510491809 A CN 201510491809A CN 105086659 B CN105086659 B CN 105086659B
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copper foil
high heat
heat conducting
preparation
nano carbon
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CN105086659A (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 present invention relates to a kind of preparation method of high heat conducting nano carbon copper foil, comprise the following steps that:a)Configure binding agent;B) configuration radiating slurry;C) coating and heating, drying processing:By radiating slurry even spread prepared by step b to copper foil surface, then heating, drying processing, you can obtain required high heat conducting nano carbon copper foil.

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, more particularly to a kind of high heat conducting nano carbon copper foil Preparation method.
Background technology
With the high speed development of microelectronics integrated technology, size, the volume of electronic component drastically reduce, thus band The radiating difficulty come seriously affects precision and the life-span of electronic device, turns into the technical bottleneck of device miniaturization, very big The further development of integrated technology is constrained in degree.There is data to show, temperature often raises 2 DEG C, the stability drop of electronic device Low about 10%;If reach 50 DEG C, then 17% or so when its life-span is only 25 DEG C.Therefore, electronic device is carried out high in time The radiating of effect is the key that it is reliably used.Conventional thermal conductive material such as metal, inorganic ceramic and metal oxide etc., though thermal conductivity Well, but many defects be present, such as single use metal material is difficult to meet insulating properties, chemical stability requirement;Inorganic pottery Porcelain then exist shock resistance it is poor, not easy processing the problems such as.Increasingly grow up instantly, to heat conduction in science and technology and national economy The functional diversity of material also accordingly proposes higher requirement, such as requires that Heat Conduction Material has lightweight, easy processing shaping, mechanics The excellent combination property such as excellent performance, resistant to chemical etching, electric insulation, low cost.Conventional thermal conductive material is because of the limitation of itself(It is main When showing single use)The growth requirement of industry and science and technology, the high heat conduction as needed for electronic component can not have been met There is remarkable lightweight thermal conductive polymer material resistant to chemical etching etc. in flexible polymer boundary material, and chemical industry heat exchanger.
In the recent period, heat-conductive composite material is with advantages such as its low cost, easy processing, good mechanics and electrical insulating properties and by wide Pay close attention to generally, its application is even more to enumerate the fields such as LED illumination, solar energy, microelectronics, electric electrician, Aero-Space, shape Into a kind of trend for progressively substituting conventional thermal conductive material.Ground at present so high-heat-conductive composite material and preparation method thereof turns into Study carefully focus.
At present, high-heat-conductive composite material will have high thermal conductivity filler particle to be scattered in macromolecule based on filled-type Matrix, the composite with excellent mechanical and heat conductivility is formed, its capacity of heat transmission can be weighed with thermal conductivity, and numerical value is bigger Represent that the heat conductivility of material is better.For filled-in composite, thermal conductivity depends primarily on macromolecule matrix with leading The intrinsic heat dispersion of hot filler, and the dispersity of filler, wherein dispersiveness of the heat filling in macromolecule matrix are An important factor for influenceing material thermal conductivity.Catalytic effect based on Nano filling, nano-particle are more easy to inside macromolecule matrix Passage of heat is formed, reduces the porosity of material internal;Under the same terms, can more be improved than micro particles material thermal conductivity and Mechanical property, and fatigue durability is more excellent.However, the easy agglomeration of nano-particle can seriously hinder effective transmission of heat, Gu Na The scattering problem of rice corpuscles turns into the difficult point studied in heat-conductive composite material preparation method.In addition, when amount of filler is less, fill out It is isolated each other between material particle, does not contact with each other, the thermal conductivity of system can not significantly improve;With the increasing of filer content Add, particle starts to contact with each other, and when more than the critical value for forming passage of heat, heat could quickly be expanded through this passage Dissipate, the capacity of heat transmission of material can just significantly improve.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of preparation method of high heat conducting nano carbon copper foil, it include with Lower processing step:
a)Configure binding agent:The binding agent includes by weight percentage:5 ~ 40% resins and 60 ~ 95% polar solvent, will Resin is poured into polar solvent and is stirred at room temperature 0.5 ~ 2 hour;
B) configuration radiating slurry:The radiating slurry includes 1 ~ 20% graphene, 1 ~ 15% CNT, 1 by weight percentage ~ 20% carborundum is with, 2 ~ 25% boron nitride, 4 ~ 25% polar solvents and the binding agent prepared by 5 ~ 20% step a, first by above-mentioned Percentage by weight pours into graphene, CNT, carborundum, boron nitride in the container equipped with polar solvent respectively, in room temperature Lower stirring 0.5 ~ 3 hour, then adds in the binding agent prepared by the step a of above-mentioned percentage by weight, it is small to continue stirring 2 ~ 8 When;
C) coating and drying and processing:By radiating slurry even spread prepared by step b to copper foil surface, then heating is dried Dry-cure, you can obtain required high heat conducting nano carbon copper foil.
Technical characteristic of the invention further is:
Resin in the step a is Kynoar or epoxy resin or polyurethane or polyacrylate.
When polar solvent in the step a and step b is 1-METHYLPYRROLIDONE, in the heating, drying of the step c In processing, heating-up temperature is 85 ~ 95 DEG C, and the heat time is 2 ~ 10 minutes.
When polar solvent in the step a and step b is DMF, dried in the heating of the step c In dry-cure, heating-up temperature is 75 ~ 85 DEG C, and the heat time is 2 ~ 10 minutes.
When polar solvent in the step a and step b is acetone, in the heating, drying processing of the step c, add Hot temperature is 45 ~ 55 DEG C, and the heat time is 2 ~ 10 minutes.
When polar solvent in the step a and step b is water, in the heating, drying processing of the step c, heating Temperature is 65 ~ 75 DEG C, and the heat time is 2 ~ 10 minutes.
The beneficial effects of the invention are as follows:
Because binding agent of the present invention selects resin and polar solvent, membrane formation mechanism is volatilization film forming, during which without any chemistry Reaction so that the quality of finished product is more stable;In addition, slurry configuration make high heat conduction filler in macromolecule matrix it is scattered more Uniformly, excellent dispersion of the high heat conducting nano filler in binder system is realized;Coating uses smooth roll coating process in addition, will Radiating slurry is transferred to copper foil surface so as to complete to be coated with, the i.e. controllable coating in the gap by adjusting upper glue roller and applicator roll Amount, Painting effect is preferable, coating layer thickness is flexibly controllable, coating accuracy is high.
Embodiment
Embodiment 1:
A kind of preparation method of high heat conducting nano carbon copper foil, it is comprised the following steps that:
a)Configure binding agent:5% Kynoar is poured into by weight percentage in 95% 1-METHYLPYRROLIDONE, and Stir 0.5 ~ 2 hour at room temperature;
B) configuration radiating slurry:By weight percentage by 1% graphene, 15% CNT, 20% carborundum with, 20% nitridation Boron is poured into 25%N- methyl pyrrolidones, is stirred at room temperature 0.5 ~ 3 hour, is then added viscous prepared by 19% step a Tie in agent, continue stirring 2 ~ 8 hours;
C) coating and drying and processing:By radiating slurry light roll coating process even spread prepared by step b to copper foil table Face, then heating, drying processing, heating-up temperature are 85 ~ 95 DEG C, and the heat time is 2 ~ 10 minutes, you can obtains required high heat conduction Nano-sized carbon copper foil.
Embodiment 2:
A kind of preparation method of high heat conducting nano carbon copper foil, it is comprised the following steps that:
a)Configure binding agent:40% epoxy resin is poured into by weight percentage in 60% DMF, and It is stirred at room temperature 0.5 ~ 2 hour;
B) configuration radiating slurry:By weight percentage by 15% graphene, 14% CNT, 1% carborundum with, 25% nitridation Boron pours into 25%N, in dinethylformamide, is stirred at room temperature 0.5 ~ 3 hour, then adds prepared by 20% step a In binding agent, continue stirring 2 ~ 8 hours;
C) coating and drying and processing:By radiating slurry light roll coating process even spread prepared by step b to copper foil table Face, then heating, drying processing, heating-up temperature are 75 ~ 85 DEG C, and the heat time is 2 ~ 10 minutes, you can obtains required high heat conduction Nano-sized carbon copper foil.
Embodiment 3:
A kind of preparation method of high heat conducting nano carbon copper foil, it is comprised the following steps that:
a)Configure binding agent:30% polyurethane is poured into by weight percentage in 70% acetone, and be stirred at room temperature 0.5 ~ 2 hours;
B) configuration radiating slurry:By weight percentage by 20% graphene, 1% CNT, 15% carborundum with, 25% nitridation Boron is poured into 25% acetone, is stirred at room temperature 0.5 ~ 3 hour, is then added in the binding agent prepared by 14% step a, after Continuous stirring 2 ~ 8 hours;
C) coating and drying and processing:By radiating slurry light roll coating process even spread prepared by step b to copper foil table Face, then heating, drying processing, heating-up temperature are 45 ~ 55 DEG C, and the heat time is 2 ~ 10 minutes, you can obtains required high heat conduction Nano-sized carbon copper foil.
Embodiment 4:
A kind of preparation method of high heat conducting nano carbon copper foil, it is comprised the following steps that:
a)Configure binding agent:20% polyacrylate is poured into by weight percentage in 80% water, and be stirred at room temperature 0.5 ~ 2 hour;
B) configuration radiating slurry:By weight percentage by 19% graphene, 14% CNT, 20% carborundum with, 2% nitridation Boron is poured into 25% water, is stirred at room temperature 0.5 ~ 3 hour, is then added in the binding agent prepared by 20% step a, continue Stirring 2 ~ 8 hours;
C) coating and drying and processing:By radiating slurry light roll coating process even spread prepared by step b to copper foil table Face, then heating, drying processing, heating-up temperature are 65 ~ 75 DEG C, and the heat time is 2 ~ 10 minutes, you can obtains required high heat conduction Nano-sized carbon copper foil.
Embodiment 5:
A kind of preparation method of high heat conducting nano carbon copper foil, it is comprised the following steps that:
a)Configure binding agent:15% polyacrylate is poured into by weight percentage in 85% water, and be stirred at room temperature 0.5 ~ 2 hour;
B) configuration radiating slurry:By weight percentage by 20% graphene, 15% CNT, 20% carborundum with, 21% nitridation Boron is poured into 4% water, is stirred at room temperature 0.5 ~ 3 hour, is then added in the binding agent prepared by 20% step a, continue to stir Mix 2 ~ 8 hours;
C) coating and drying and processing:By radiating slurry light roll coating process even spread prepared by step b to copper foil table Face, then heating, drying processing, heating-up temperature are 65 ~ 75 DEG C, and the heat time is 2 ~ 10 minutes, you can obtains required high heat conduction Nano-sized carbon copper foil.
Embodiment 6:
A kind of preparation method of high heat conducting nano carbon copper foil, it is comprised the following steps that:
a)Configure binding agent:25% epoxy resin is poured into by weight percentage in 75% DMF, and It is stirred at room temperature 0.5 ~ 2 hour;
B) configuration radiating slurry:By weight percentage by 20% graphene, 10% CNT, 20% carborundum with, 25% nitridation Boron pours into 20%N, in dinethylformamide, is stirred at room temperature 0.5 ~ 3 hour, then adds prepared by 5% step a In binding agent, continue stirring 2 ~ 8 hours;
C) coating and drying and processing:By radiating slurry light roll coating process even spread prepared by step b to copper foil table Face, then heating, drying processing, heating-up temperature are 75 ~ 85 DEG C, and the heat time is 2 ~ 10 minutes, you can obtains required high heat conduction Nano-sized carbon copper foil.
Because binding agent of the present invention selects resin and polar solvent, membrane formation mechanism is volatilization film forming, during which without any chemistry Reaction so that the quality of finished product is more stable;In addition, slurry configuration make high heat conduction filler in macromolecule matrix it is scattered more Uniformly, excellent dispersion of the high heat conducting nano filler in binder system is realized;Coating uses smooth roll coating process in addition, will Radiating slurry is transferred to copper foil surface so as to complete to be coated with, the i.e. controllable coating in the gap by adjusting upper glue roller and applicator roll Amount, Painting effect is preferable, coating layer thickness is flexibly controllable, coating accuracy is high.
Although being described herein as embodiment, but it is to be understood that, embodiments disclosed herein Only exemplary of the invention, it can be presented as various forms.Therefore, the detail disclosed here is not considered as It is restricted, and is merely possible to the basis of claim and is used as be used to instruct those skilled in the art in practice to appoint What appropriate mode is differently using the representational basis of the present invention, including uses various features described herein and combination Here the feature that may do not disclosed clearly.Protection scope of the present invention is defined by claims.

Claims (9)

1. a kind of preparation method of high heat conducting nano carbon copper foil, it is characterised in that comprise the following steps that:
a)Configure binding agent:The composition of the binding agent is by weight percentage 5 ~ 40% resins and 60 ~ 95% polar solvent, will be set Fat is poured into polar solvent and is stirred at room temperature 0.5 ~ 2 hour, wherein, the resin is Kynoar or epoxy resin or gathered Urethane or polyacrylate;
B) configuration radiating slurry:The composition of the radiating slurry is 1 ~ 20% graphene, 1 ~ 15% CNT, 1 by weight percentage Binding agent prepared by ~ 20% carborundum, 2 ~ 25% boron nitride, 4 ~ 25% polar solvents and 5 ~ 20% step a, first by above-mentioned heavy Amount percentage pours into graphene, CNT, carborundum, boron nitride in the container equipped with polar solvent respectively, at room temperature Stirring 0.5 ~ 3 hour, then adds in the binding agent prepared by the step a of above-mentioned percentage by weight, continues stirring 2 ~ 8 hours;
C) coating and heating, drying processing:By radiating slurry even spread prepared by step b to copper foil surface, then heating is dried Dry-cure, you 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, it is characterised in that:The step a and step Polar solvent in b is 1-METHYLPYRROLIDONE.
3. the preparation method of high heat conducting nano carbon copper foil as claimed in claim 2, it is characterised in that:In adding for the step c In hot drying and processing, heating-up temperature is 85 ~ 95 DEG C, and the heat time is 2 ~ 10 minutes.
4. the preparation method of high heat conducting nano carbon copper foil as claimed in claim 1, it is characterised in that:The step a and step Polar solvent in b is N,N-dimethylformamide.
5. the preparation method of high heat conducting nano carbon copper foil as claimed in claim 4, it is characterised in that:In adding for the step c In hot drying and processing, heating-up temperature is 75 ~ 85 DEG C, and the heat time is 2 ~ 10 minutes.
6. the preparation method of high heat conducting nano carbon copper foil as claimed in claim 1, it is characterised in that:The step a and step Polar solvent in b is acetone.
7. the preparation method of high heat conducting nano carbon copper foil as claimed in claim 6, it is characterised in that:In adding for the step c In hot drying and processing, heating-up temperature is 45 ~ 55 DEG C, and the heat time is 2 ~ 10 minutes.
8. the preparation method of high heat conducting nano carbon copper foil as claimed in claim 1, it is characterised in that:The step a and step Polar solvent in b is water.
9. the preparation method of high heat conducting nano carbon copper foil as claimed in claim 8, it is characterised in that:In adding for the step c In hot drying and processing, heating-up temperature is 65 ~ 75 DEG C, and the heat time is 2 ~ 10 minutes.
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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
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
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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