CN108823615A - High heat conducting nano copper-graphite film composite material preparation method - Google Patents
High heat conducting nano copper-graphite film composite material preparation method Download PDFInfo
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- CN108823615A CN108823615A CN201810499651.8A CN201810499651A CN108823615A CN 108823615 A CN108823615 A CN 108823615A CN 201810499651 A CN201810499651 A CN 201810499651A CN 108823615 A CN108823615 A CN 108823615A
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- graphite film
- copper
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- heat conducting
- high heat
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/38—Electroplating: Baths therefor from solutions of copper
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/54—Electroplating of non-metallic surfaces
Abstract
The invention discloses a kind of preparation methods of high heat conducting nano copper-graphite film composite material, it includes step in detail below：（1）Graphite film is subjected to chemical roughening treatment；（2）Graphite film after roughening treatment is subjected to corona treatment；（3）Graphite film after corona treatment is subjected to plating Copper treatment；（4）By electro-coppering, treated that graphite film is passivated processing, and high heat conducting nano copper-graphite film composite products are obtained after being cleaned, being dried again after Passivation Treatment.
Description
Technical field
The present invention relates to high thermal conductivity cooling fin technical fields, compound more particularly to a kind of high heat conducting nano copper-graphite film
The preparation method of material.
Background technique
Smart phone, tablet computer etc. are at one of necessity for people's lives, but during device miniaturization, with
The use of huge size integrated circuit, the promotion of element collection on a large scale, unit volume generate thermal power also become larger, so
And device heat dissipation area is constant, and the heat dissipation of unit area is caused not reach requirement.Therefore, dissipation from electronic devices efficiency pair is improved
Develop in microelectronic industry most important.
Macroscopical copper has good electric conductivity and higher heating conduction, is applied as electronic product heat conduction and heat radiation and electricity
Magnetic shielding part.But since copper has greater density and is difficult into ultrathin film, it is light, thin electronic product is not able to satisfy gradually
Demand for development.
New carbon is such as：Electrographite, graphene, carbon nanotube etc. have brilliant heating conduction.But graphene system
Standby complex process, yield rate are low, it is difficult to realize large-scale continuous production.Carbon nanotube is due at high cost, generally as adding
Add agent, to be difficult to obtain the composite material of high thermal conductivity.Electrographite film has class graphene-structured, and between layers
Queueing discipline is orderly, and defect is less, has high thermal conductivity energy, and mature production technology, has been widely used for electronic device
Heat conduction and heat radiation.But electrographite film longitudinal direction Z thermal coefficient is lower, only 5-20 W/m K.
Characteristic is led in carbon materials charge level in order to effectively keep, while improving its longitudinal direction Z heating conduction again, in the prior art,
The method as disclosed in patent CN 105584122A passes through carbon material film and copper foil together with adhered by double sided plaster；Patent CN
103476227A discloses a kind of copper carbon composite radiating piece preparation method, coats carbon material coating on the two sides of copper foil；Patent CN
106847757A discloses a kind of graphite copper foil heat sink compound, by calendering by carbon material film and copper mesh it is compound obtain it is compound
Cooling fin.
Longitudinal Z heating conduction of graphite film can be improved in above-mentioned technology to a certain extent, but the use of adhesive can be tight
The thermal coefficient for reducing carbon material layer again, the heat for causing graphite film to shed can not be transmitted on copper in time, seriously undermine stone
The heat dissipation effect of ink film.Therefore, urgent need, which seeks one kind, can prepare method of the graphite without the attached copper composite membrane of glue, and perfection embodies graphite
The high-termal conductivity of film and isotropic thermal conductivity of copper.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of preparations of high heat conducting nano copper-graphite film composite material
Method, technical solution used by it are：A kind of preparation method of high heat conducting nano copper-graphite film composite material, feature exist
In, including step in detail below：
（1）Graphite film is subjected to chemical roughening treatment：Graphite film is embathed using sodium hydroxide solution or Piranha solution, is embathed
Temperature is 20-90 DEG C, and embathing the time is 1-30min, then rinses graphite film using deionized water and dries；
（2）Graphite film after roughening treatment is subjected to corona treatment：The corona treatment is will be after gas ionization
In film surface, processing atmosphere is at least one of air, oxygen, nitrogen, argon gas for directly bombardment, and processing speed is 1-10 m/
Min is handled 1-5 times；
（3）Graphite film after corona treatment is subjected to plating Copper treatment：Using cyanide-free alkaline copper plating or cyanide electroplating side
Method carries out plating Copper treatment, and thickness of coating is 50-800 nm；
（4）By electro-coppering, treated that graphite film is passivated processing, and height is obtained after being cleaned, being dried again after Passivation Treatment and is led
Hot Nanometer Copper-graphite film composite products.
The further technical characteristic of the present invention is：
The step（1）Middle concentration of sodium hydroxide solution is 50-500 g/L；
The step（1）The concentrated sulfuric acid and dioxygen water volume ratio are 3 in middle Piranha solution:1.
The Passivation Treatment is that graphite film is immersed directly in copper passivator, and copper passivator concentration is 5-100 g/L, blunt
Changing temperature is 0-90 DEG C, passivation time 0.1-10min.
The graphite film is with a thickness of 10-200 μm.
The graphite film is natural stone ink film or electrographite film or graphene heat dissipation film.
The beneficial effects of the invention are as follows：
Simple process of the invention, raw material sources are extensive, are suitble to industrialized production, obtained Nanometer Copper-graphite film composite wood
Material has excellent thermally conductive, heat dissipation performance.In addition preparation method provided by the invention is easily realized on traditional material process equipment,
Industrialized production easy to accomplish, high heat conducting nano copper-graphite film composite material obtained have high thermal conductivity coefficient and heat dissipation effect
Fruit, in-plane thermal coefficient have good flexibility more than 500 W/m K, can be with various gums and insulation material
Expect compound and carry out cross cutting processing, is widely used in smart phone, liquid crystal display panel, tablet computer, laptop, power electronics
The radiating treatment of equipment, vehicle electronics etc..
Specific embodiment：
Embodiment one,
A kind of preparation method of high heat conducting nano copper-graphite film composite material, including step in detail below：
（1）The graphene heat dissipation film of 10 μ m-thicks is subjected to chemical roughening treatment：10 μ m-thicks are embathed using sodium hydroxide solution
Graphene heat dissipation film, embathing temperature is 20 DEG C, and embathing the time is 30min, then rinses graphene heat dissipation film using deionized water
And dry, concentration of sodium hydroxide solution is 50 g/L in this step；Graphene heat dissipation film surface microscopic through chemical roughening treatment
Rustic degree increases, and surface chemistry inertia reduces.
（2）Graphene heat dissipation film after roughening treatment is subjected to corona treatment：The corona treatment is by gas
In film surface, processing atmosphere is air for directly bombardment after body ionization, and processing speed 1m/min is handled 1-5 times；Stone after processing
Black alkene heat dissipation film tension reaches 50 dynes or more.By corona treatment, graphite film surface chemical structure and microcosmic
Structure can change a lot, and form a large amount of carbon and oxygen functional groups, and graphite film surface hydrophilicity enhances.
（3）Graphene heat dissipation film after corona treatment is subjected to plating Copper treatment：Using cyanide-free alkaline copper plating method
Carry out plating Copper treatment, thickness of coating 50nm；
（4）By electro-coppering, treated that graphene heat dissipation film is immersed directly in copper passivator is passivated processing, copper passivator
Concentration is 5 g/L, and passivation temperature is 0 DEG C, passivation time 10min, obtains height after being cleaned, dried again after Passivation Treatment and leads
Hot Nanometer Copper-graphite film composite products, after Passivation Treatment, nanometer layers of copper inoxidizability and resistance to acid and alkali are improved.
Embodiment two,
A kind of preparation method of high heat conducting nano copper-graphite film composite material, including step in detail below：
（1）The graphene heat dissipation film of 100 μ m-thicks is subjected to chemical roughening treatment：100 μ m-thicks are embathed using sodium hydroxide solution
Graphene heat dissipation film, embathe temperature be 50 DEG C, embathe the time be 10min, then using deionized water rinse graphene heat dissipation
Film is simultaneously dried, and concentration of sodium hydroxide solution is 500 g/L in this step；Graphene heat dissipation film surface through chemical roughening treatment is micro-
It sees rustic degree to increase, surface chemistry inertia reduces.
（2）Graphene heat dissipation film after roughening treatment is subjected to corona treatment：The corona treatment is by gas
In film surface, processing atmosphere is oxygen for directly bombardment after body ionization, and processing speed 10m/min is handled 1-5 times；After processing
Graphene heat dissipation film tension reaches 50 dynes or more.By corona treatment, graphite film surface chemical structure and micro-
Seeing structure can change a lot, and form a large amount of carbon and oxygen functional groups, and graphite film surface hydrophilicity enhances.
（3）Graphene heat dissipation film after corona treatment is subjected to plating Copper treatment：Using cyanide-free alkaline copper plating method
Carry out plating Copper treatment, thickness of coating 800nm；
（4）By electro-coppering, treated that graphene heat dissipation film is immersed directly in copper passivator is passivated processing, copper passivator
Concentration is 100 g/L, and passivation temperature is 90 DEG C, passivation time 0.1min, cleaned after Passivation Treatment again, dry after obtain
High heat conducting nano copper-graphite film composite products.After Passivation Treatment, nanometer layers of copper inoxidizability and resistance to acid and alkali are improved.
Embodiment three,
A kind of preparation method of high heat conducting nano copper-graphite film composite material, including step in detail below：
（1）The graphene heat dissipation film of 200 μ m-thicks is subjected to chemical roughening treatment：200 μ m-thicks are embathed using sodium hydroxide solution
Graphene heat dissipation film, embathe temperature be 90 DEG C, embathe the time be 1min, then using deionized water rinse graphene heat dissipation film
And dry, concentration of sodium hydroxide solution is 200 g/L in this step；Graphene heat dissipation film surface microscopic through chemical roughening treatment
Rustic degree increases, and surface chemistry inertia reduces.
（2）Graphene heat dissipation film after roughening treatment is subjected to corona treatment：The corona treatment is by gas
In film surface, processing atmosphere is nitrogen for directly bombardment after body ionization, and processing speed 6m/min is handled 1-5 times；Stone after processing
Black alkene heat dissipation film tension reaches 50 dynes or more.By corona treatment, graphite film surface chemical structure and microcosmic
Structure can change a lot, and form a large amount of carbon and oxygen functional groups, and graphite film surface hydrophilicity enhances.
（3）Graphene heat dissipation film after corona treatment is subjected to plating Copper treatment：It is carried out using cyanide electroplating method
Copper treatment, thickness of coating 200nm is electroplated；
（4）By electro-coppering, treated that graphene heat dissipation film is immersed directly in copper passivator is passivated processing, copper passivator
Concentration is 60 g/L, and passivation temperature is 60 DEG C, passivation time 5min, is obtained after being cleaned, dried again after Passivation Treatment high
Heat conducting nano copper-graphite film composite products.After Passivation Treatment, nanometer layers of copper inoxidizability and resistance to acid and alkali are improved.
Performance test comparison
Comparative example：No any processing with a thickness of 25 μm electrographite membrane sample and according to relevant criterion sample is carried out scattered
Thermal performance test, every test result are included in table 1.
It should be noted that the thermal coefficient to products obtained therefrom in the above various embodiments and comparative example uses thermal conductivity factor instrument
（DR-SM）It is tested at room temperature by standard GB/T 8722-1988.
1 embodiment of table and comparative example performance parameter
As can be seen from the above table, comparative example 1,1 ~ 3 gained high heat conducting nano copper of embodiment-graphite film composite material tool are compared
There is thermal coefficient in high face, while axial thermal conductivity coefficient is promoted obviously.Result above sufficiently proves that the content of present invention is pair
A breakthrough of the conventional graphite film on heat dissipation performance.
In practical applications, the graphite film can also select natural stone ink film or electrographite film to the present invention；It is chemical thick
Change processing can also use Piranha solution, and the concentrated sulfuric acid and dioxygen water volume ratio are 3 in Piranha solution:1；Corona treatment
Atmosphere can also be two kinds, three kinds or four kinds in argon gas or air, oxygen, nitrogen, argon gas.
Optionally, the plating Copper treatment is any one of cyanide-free alkaline copper plating or cyanide electroplating.Made with graphite film
It is cathode, anaerobic pure copper sheet as anode；Wherein mantoquita is in copper sulphate, copper nitrate, copper chloride, cupric pyrophosphate or copper acetate
Any one；Complexing agent is one of sodium tartrate, sodium ethylene diamine tetracetate, ammonium citrate, sodium citrate or potassium pyrophosphate
Or two kinds.On graphite film, graphite film is improved significantly Nanometer Copper growth in situ with layers of copper binding force, and nanometer copper layer thickness is
50-800 nm。
From the above it can be seen that a kind of preparation of high heat conducting nano copper-graphite film composite material provided by the invention
Method is only handled graphite surface, has not been changed its internal structure, on graphite thermal property substantially without influence, and Nanometer Copper with
Without using any adhesive between graphite, greatly reduces interface resistance and ensure that good combination between Nanometer Copper and graphite
Power improves Nanometer Copper-graphite film composite shaft to heating conduction.In addition, nanometer layers of copper increases the ratio table of composite material
Area provides more heat dissipations, thermal conducting path.
The preparation method provided according to the present invention easily realizes on traditional material process equipment, industry metaplasia easy to accomplish
It produces, high heat conducting nano copper-graphite film composite material obtained has high thermal conductivity coefficient and heat dissipation effect, and in-plane is thermally conductive
Coefficient has good flexibility more than 500 W/m K, can be compound with various gums and insulating materials and be die cut
Processing, is widely used in smart phone, liquid crystal display panel, tablet computer, laptop, power electronic equipment, automotive electronics and sets
The standby radiating treatment waited.
The above is only specific embodiments of the present invention are specifically described, should not be understood as to the scope of the present invention
Limitation, the person skilled in the art in the field according to the present invention content to some nonessential modifications and adaptations for making of the present invention
Still belong to protection scope of the present invention, protection scope of the present invention is subject to claims.
Claims (6)
1. a kind of preparation method of high heat conducting nano copper-graphite film composite material, which is characterized in that including step in detail below：
（1）, graphite film is subjected to chemical roughening treatment：Graphite film is embathed using sodium hydroxide solution or Piranha solution, is soaked
Washing temperature is 20-90 DEG C, and embathing the time is 1-30min, then rinses graphite film using deionized water and dries；
（2）, by after roughening treatment graphite film carry out corona treatment：The corona treatment is will be after gas ionization
In film surface, processing atmosphere is at least one of air, oxygen, nitrogen, argon gas for directly bombardment, and processing speed is 1-10 m/
Min is handled 1-5 times；
（3）, the graphite film after corona treatment is subjected to plating Copper treatment：Using cyanide-free alkaline copper plating or cyanide electroplating side
Method carries out plating Copper treatment, and thickness of coating is 50-800 nm；
（4）, by electro-coppering, treated that graphite film is passivated processing, obtained after being cleaned, being dried again after Passivation Treatment high
Heat conducting nano copper-graphite film composite products.
2. the preparation method of high heat conducting nano copper-graphite film composite material according to claim 1, it is characterised in that：Institute
State step（1）Middle concentration of sodium hydroxide solution is 50-500 g/L.
3. the preparation method of high heat conducting nano copper-graphite film composite material according to claim 1, it is characterised in that：Institute
State step（1）The concentrated sulfuric acid and dioxygen water volume ratio are 3 in middle Piranha solution:1.
4. the preparation method of high heat conducting nano copper-graphite film composite material according to claim 1, it is characterised in that：Institute
Stating Passivation Treatment is that graphite film is immersed directly in copper passivator, and copper passivator concentration is 5-100 g/L, passivation temperature 0-
90 DEG C, passivation time 0.1-10min.
5. according to claim 1 to the preparation of the copper of high heat conducting nano described in any claim in 4-graphite film composite material
Method, it is characterised in that：The graphite film is with a thickness of 10-200 μm.
6. the preparation method of high heat conducting nano copper-graphite film composite material as claimed in claim 5, it is characterised in that：It is described
Graphite film is natural stone ink film or electrographite film or graphene heat dissipation film.
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| CN111923425A (en) * | 2020-07-28 | 2020-11-13 | 北京化工大学 | Preparation method of high-thermal-conductivity graphite film-carbon fiber resin matrix composite material |
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| CN114822919A (en) * | 2022-04-14 | 2022-07-29 | 广东墨睿科技有限公司 | Graphene-metal composite film and manufacturing method thereof |
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| CN114822919A (en) * | 2022-04-14 | 2022-07-29 | 广东墨睿科技有限公司 | Graphene-metal composite film and manufacturing method thereof |
| CN114822919B (en) * | 2022-04-14 | 2023-09-19 | 广东墨睿科技有限公司 | Manufacturing method of graphene-metal composite film |
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