CN106082186A - A kind of heat conduction thin film of graphene nano carbon/carbon-copper composite material and preparation method thereof - Google Patents
A kind of heat conduction thin film of graphene nano carbon/carbon-copper composite material and preparation method thereof Download PDFInfo
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- CN106082186A CN106082186A CN201610404290.5A CN201610404290A CN106082186A CN 106082186 A CN106082186 A CN 106082186A CN 201610404290 A CN201610404290 A CN 201610404290A CN 106082186 A CN106082186 A CN 106082186A
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Abstract
The invention discloses heat conduction thin film of a kind of graphene nano carbon/carbon-copper composite material and preparation method thereof, this heat conduction thin film is composited with multi-layer graphene by copper nano particles, described copper particle diameter is at Nano grade, it is evenly distributed between graphene layer, fill up the fault location at Graphene, and be connected upper and lower two layer graphenes.This heat conduction thin film while keeping horizontal high heat conductance characteristic, can effectively increase the thermal conductivity of its longitudinal direction, can be used for dissipation from electronic devices.
Description
Technical field
The invention belongs to technical field of heat transfer, be specifically related to a kind of Graphene-Nanometer Copper composite heat conduction thin film and
Its preparation method.
Background technology
Along with the improving constantly of integrated level, packaging density and operating frequency of electronic chip, chip heat flow density is rapid
Increasing, bring great challenge to chip cooling, heat dissipation problem has had influence on electronic product, high-power electrical, aviation boat
It etc. the development in field.For solving problem above, people, except being optimized Thermal Design of Electronic Equipments, find performance more excellent
Good heat radiation thin film also becomes an important breakthrough mouth.
Graphene is have now been found that the thinnest, the hardest, and the novel nano-material that conductive and heat-conductive ability is the strongest, Graphene is sent out
The most so far, the performance such as its calorifics, mechanics and electricity obtains the research of more and more scholar.Scientist estimates mono-layer graphite under room temperature
The transverse thermal conductivity of alkene is up to 5300W/ (mK), but single-layer graphene thickness only has about 0.335nm.Multi-layer graphene interlayer
Be easily generated sliding because only existing Van der Waals force so that it is longitudinal thermal conductivity is the highest, due to its transverse thermal conductivity of phon scattering with
The increase of the number of plies and reduce rapidly, limit its application at heat radiation film applications.Scientists has been carried out graphite in recent years
Alkene composite makes and the multinomial research of various performance, utilizes the heat conductivility that Graphene is excellent, develops heat conductivility
Good graphene composite material, has important realistic meaning.
Summary of the invention
Goal of the invention: in order to overcome the deficiencies in the prior art, the present invention provides a kind of Graphene-Nanometer Copper to be combined
Heat conduction thin film of material and preparation method thereof, can be applicable to the high thermal conductivity graphite alkene membrane structure of dissipation from electronic devices.
Technical scheme: for achieving the above object, the technical solution used in the present invention is:
The heat conduction thin film of a kind of Graphene-Nanometer Copper composite, is composited with multi-layer graphene by copper granule, described
Copper particle diameter, at Nano grade, is evenly distributed between adjacent two graphene layer.Copper granule fills up the defect at Graphene
Place, and it is connected upper and lower two layer graphenes.
Further, the thickness of the heat conduction thin film of gained is 50 μm-100 μm, and under room temperature, transverse thermal conductivity is at 600W/m K
Above.
Further, a diameter of 35nm-120nm of described copper granule.
The preparation method of the heat conduction thin film of above-mentioned Graphene-Nanometer Copper composite, comprises the following steps:
1) graphene oxide film is prepared；
2) electroplating technology is used to prepare electro deposition oxidation graphene film on described graphene oxide film；
3) being vacuum dried, anneal, the described electro deposition oxidation graphene film that reduces forms Graphene-Nanometer Copper THIN COMPOSITE
Film；
4) hot pressing annealing.
Further, described step 1) prepare graphene oxide film method particularly includes:
1-1) natural flaky graphite powder is joined in the mixture containing concentrated nitric acid sodium and freezing concentrated sulphuric acid；
1-2) add potassium permanganate, and stir mixture；
1-3) it is gradually added into hydrogen peroxide solution and removes remaining potassium permanganate；
1-4) mixture diluted and be centrifuged, obtaining graphene oxide；
1-5) clean described graphene oxide with hydrochloric acid solution and deionized water；
1-6) filtered under vacuum dehydration obtains graphene oxide film.
Further, described step 2) use electroplating technology to prepare electro deposition oxidation stone on described graphene oxide film
Ink alkene thin film, specifically comprises the processes of: add graphene oxide into and deionized water carries out ultrasonic disperse, electroplating bath carries out electrophoresis
Deposition, is specially electro-deposition 180s under conditions of 20V constant voltage, and during electrolysis, the copper sheet as anode loses electronics
Form bivalent cupric ion, form the dark film of gel i.e. electro deposition oxidation graphene film at anode surface.
Further, described step 3) method particularly includes: described electro deposition oxidation graphene film is put into atmosphere furnace
In be dried, put into atmosphere furnace afterwards, be passed through nitrogen, be heated to 300 DEG C with the speed of 6 DEG C/min, logical after constant temperature 10 minutes
Enter hydrogen, then with the ramp of 8 DEG C/min to corresponding temperature, by hydrogen annealing heat treatment, the defect of Graphene be repaired,
Step 2) electroplating process in formed bivalent cupric ion be reduced into nano copper particle and move to graphene oxide
Interlayer is formed Graphene-Nanometer Copper laminated film.
Further, the technique of described hydrogen annealing is for being separately heated to 400 DEG C, 500 DEG C, 650 DEG C and 700 DEG C.Annealing
Temperature is formed relevant with the thermal polymerization of copper ion and copper nano particles, and copper particle diameter size raises with annealing temperature and increases,
But the too conference of copper granule causes the decline of thermal conductivity, therefore annealing temperature interval is scheduled on 400 DEG C-700 DEG C.
Further, described step 4) use hot-pressing technique, specially pressure 30MPa, with the ramp of 10 DEG C/min
To 800 DEG C, constant temperature 30min, then natural cooling.Hot pressing makes to contact between copper nano particles with Graphene tightr, makes simultaneously
The distance of the composite interlayer must with multiple structure reduces, and contacts tightr.
Further, described step 4) use annealing technology, in the atmosphere of nitrogen with the ramp of 10 DEG C/min extremely
300 DEG C, constant temperature 1h, then natural cooling.The heat treatment mode using annealing is the thermal stress in order to eliminate thin film, reduces and lacks
Fall into.
Beneficial effect: heat conduction thin film of Graphene-Nanometer Copper composite that the present invention provides and preparation method thereof, permissible
Keeping while horizontal high heat conductance characteristic, effectively increasing the thermal conductivity of its longitudinal direction, the small-sized electronic device that can be used for
Heat radiation.
Accompanying drawing explanation
Fig. 1 is the preparation method schematic flow sheet of the present invention.
Detailed description of the invention
Below in conjunction with the accompanying drawings the present invention is further described.
It is illustrated in figure 1 the preparation method of the heat conduction thin film of a kind of Graphene-Nanometer Copper composite, utilizes physics or change
Method prepares graphene oxide, then utilizes electroplating technology to prepare electro deposition oxidation Graphene on graphene oxide film
Thin film, forms Graphene-Nanometer Copper laminated film with hydrogen annealing redox graphene, and utilizes annealing temperature control copper to receive
The diameter of rice grain.Use hot-pressing technique to make to contact between copper nano particles with Graphene tightr, make to have simultaneously
The distance of the composite interlayer of multiple structure reduces, and contacts tightr.The heat treatment mode finally using annealing eliminates thin film
Thermal stress, reduce defect.
Embodiment
The preparation method of the heat conduction thin film of a kind of Graphene-Nanometer Copper composite, preparation process flow chart is as follows, specifically
For: natural for 2.0g flaky graphite powder is joined the mixture of the concentrated sulphuric acid freezing containing 1.0g concentrated nitric acid sodium and 92ml
In.Add 9.0g potassium permanganate, and stir mixture.Then it is gradually added into hydrogen peroxide solution and removes remaining potassium permanganate,
Again mixture diluted and be centrifuged, graphene oxide hydrochloric acid solution and the deionized water of gained are cleaned.Put in atmosphere furnace
Filtered under vacuum is dehydrated.
Add graphene oxide into and deionized water carries out ultrasonic disperse, electroplating bath carries out electrophoretic deposition.Permanent at 20V
Electro-deposition 180s under conditions of pressure, anode surface forms the dark film of gel (GO-EPD), is then vacuum dried in atmosphere furnace.
GO-EPD film carries out high-temperature hydrogen annealing process in atmosphere furnace, is separately heated to 400, and 500,650, and 700 DEG C,
Copper particle diameter size raises with annealing temperature and increases.The thin film of preparation is put into hot press hot pressing, and pressure 30MPa, with 10
DEG C/ramp of min to 800 DEG C, constant temperature 30min, then natural cooling.Put in atmosphere furnace afterwards in the atmosphere of nitrogen
With the ramp of 10 DEG C/min to 300 DEG C, constant temperature 1h, then natural cooling.
Owing to only existing weak interaction force Van der Waals force between graphene layer, leveraging longitudinal heat conduction, this implements
The heat conduction thin film of Graphene-Nanometer Copper composite that example obtains, because at the many Nanometer Coppers of Intercalation reaction of Graphene
Grain, the copper nano particles that on the one hand heat conductivity is higher take part in the heat conduction of interlayer, on the other hand uses hot-pressing technique to make copper
Between nano-particle with Graphene, composite interlayer contact tightr, the most this structure can increase longitudinal thermal conductance
Rate.Meanwhile, this structure does not destroy the most highly thermally conductive characteristic that Graphene itself has, and transverse thermal conductivity can reach 600W/
More than m K, higher than the 500W/m K of existing commercial thermal conductivity thin film, thermal conductivity at least improves 20%.Film thickness is at 50-100 μ
Between m, can be used for the heat radiation of electronic device.
The above is only the preferred embodiment of the present invention, it should be pointed out that: for the ordinary skill people of the art
For Yuan, under the premise without departing from the principles of the invention, it is also possible to make some improvements and modifications, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (10)
1. the heat conduction thin film of Graphene-Nanometer Copper composite, it is characterised in that: it is combined with multi-layer graphene by copper granule
Forming, described copper particle diameter, at Nano grade, is evenly distributed between adjacent two graphene layer.
The heat conduction thin film of Graphene the most according to claim 1-Nanometer Copper composite, it is characterised in that: leading of gained
The thickness of hot thin film is 50 μm-100 μm, and under room temperature, transverse thermal conductivity is at more than 600W/m K.
The heat conduction thin film of Graphene the most according to claim 1-Nanometer Copper composite, it is characterised in that: described copper
A diameter of 35nm-120nm of grain.
The preparation method of the heat conduction thin film of Graphene the most according to claim 1-Nanometer Copper composite, its feature exists
In: comprise the following steps:
1) graphene oxide film is prepared；
2) electroplating technology is used to prepare electro deposition oxidation graphene film on described graphene oxide film；
3) being vacuum dried, anneal, the described electro deposition oxidation graphene film that reduces forms Graphene-Nanometer Copper laminated film；
4) hot pressing annealing.
The preparation method of the heat conduction thin film of Graphene the most according to claim 4-Nanometer Copper composite, its feature exists
In: described step 1) prepare graphene oxide film method particularly includes:
1-1) natural flaky graphite powder is joined in the mixture containing concentrated nitric acid sodium and freezing concentrated sulphuric acid；
1-2) add potassium permanganate, and stir mixture；
1-3) it is gradually added into hydrogen peroxide solution and removes remaining potassium permanganate；
1-4) mixture diluted and be centrifuged, obtaining graphene oxide；
1-5) clean described graphene oxide with hydrochloric acid solution and deionized water；
1-6) filtered under vacuum dehydration obtains graphene oxide film.
The preparation method of the heat conduction thin film of Graphene the most according to claim 4-Nanometer Copper composite, its feature exists
In: described step 2) use electroplating technology to prepare electro deposition oxidation graphene film on described graphene oxide film, specifically
Technique is: adds graphene oxide into and carries out ultrasonic disperse in deionized water, carries out electrophoretic deposition in electroplating bath, is specially
Electro-deposition 180s under conditions of 20V constant voltage, during electrolysis, lose as the copper sheet of anode electronically form cupric from
Son, forms the dark film of gel i.e. electro deposition oxidation graphene film at anode surface.
The preparation method of the heat conduction thin film of Graphene the most according to claim 4-Nanometer Copper composite, its feature exists
In: described step 3) method particularly includes: described electro deposition oxidation graphene film is put in atmosphere furnace and be dried, put into afterwards
In atmosphere furnace, being passed through nitrogen, be heated to 300 DEG C with the speed of 6 DEG C/min, constant temperature is passed through hydrogen after 10 minutes, then with 8 DEG C/
The ramp of min is to corresponding temperature, and by hydrogen annealing heat treatment, the defect of Graphene is repaired, step 2) galvanizer
During skill formed bivalent cupric ion be reduced into nano copper particle and move to graphene oxide interlayer in formed graphite
Alkene-Nanometer Copper laminated film.
The preparation method of the heat conduction thin film of Graphene the most according to claim 7-Nanometer Copper composite, its feature exists
In: the technique of described hydrogen annealing is for being separately heated to 400 DEG C, 500 DEG C, 650 DEG C and 700 DEG C.
The preparation method of the heat conduction thin film of Graphene the most according to claim 4-Nanometer Copper composite, its feature exists
In described step 4) use hot-pressing technique, specially pressure 30MPa, with the ramp of 10 DEG C/min to 800 DEG C, constant temperature
30min, then natural cooling.
The preparation method of the heat conduction thin film of Graphene the most according to claim 4-Nanometer Copper composite, its feature exists
In described step 4) use annealing technology, with the ramp of 10 DEG C/min to 300 DEG C in the atmosphere of nitrogen, constant temperature 1h, so
Rear natural cooling.
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107313102A (en) * | 2017-07-03 | 2017-11-03 | 鄂尔多斯市紫荆创新研究院 | A kind of aluminium base graphene, the preparation method of CNT composite heat dissipation material |
| CN108486568A (en) * | 2018-02-26 | 2018-09-04 | 武汉理工大学 | A kind of flaky graphite alkene/metal hetero-junction laminated film and preparation method thereof for heat conduction |
| CN108763764A (en) * | 2018-05-29 | 2018-11-06 | 南京航空航天大学 | A kind of computational methods of graphene-flexible substrates buckling structure deformation |
| WO2019047164A1 (en) * | 2017-09-08 | 2019-03-14 | 深圳大学 | Preparation method for graphene oxide |
| CN109811175A (en) * | 2019-03-26 | 2019-05-28 | 重庆大学 | A kind of graphene-method of manufacturing carbon/carbon-copper composite material |
| CN110117810A (en) * | 2019-06-10 | 2019-08-13 | 广西师范大学 | A kind of method that electrophoresis prepares modified graphene oxide aluminium composite heat conducting material |
| CN110344099A (en) * | 2019-07-18 | 2019-10-18 | 桂林电子科技大学 | A kind of preparation method of high thermal conductivity graphene composite thin film material |
| CN110437652A (en) * | 2019-08-07 | 2019-11-12 | 山东烯泰天工节能科技有限公司 | A kind of graphene heat radiation coating and preparation method thereof |
| CN110564376A (en) * | 2019-08-27 | 2019-12-13 | 华进半导体封装先导技术研发中心有限公司 | Composite material for thermal management and preparation method thereof |
| CN111114041A (en) * | 2020-01-07 | 2020-05-08 | 中国电子科技集团公司第十六研究所 | Composite material with high-thermal-conductivity graphite-copper interpenetrating structure and preparation method thereof |
| CN111151587A (en) * | 2020-03-10 | 2020-05-15 | 广东禾木科技有限公司 | Wire drawing die and manufacturing method and application thereof |
| CN111548516A (en) * | 2020-04-21 | 2020-08-18 | 苏州锦富技术股份有限公司 | Nitrogen-doped graphene copper composite heat dissipation film and preparation method thereof |
| CN112853432A (en) * | 2021-02-05 | 2021-05-28 | 南京大学 | Preparation method of graphene/aluminum composite material heat dissipation film |
| CN113860888A (en) * | 2021-11-04 | 2021-12-31 | 四川恒力盛泰石墨烯科技有限公司 | Preparation method of graphene heat dissipation film for electronic equipment |
| CN114096118A (en) * | 2021-11-03 | 2022-02-25 | 武汉华星光电半导体显示技术有限公司 | Heat radiating fin, preparation method thereof and electronic device |
| CN114523102A (en) * | 2022-02-28 | 2022-05-24 | 常州烯雷新材料科技有限公司 | Preparation method of powder graphene coated metal particles |
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| CN107313102B (en) * | 2017-07-03 | 2019-02-26 | 鄂尔多斯市紫荆创新研究院 | A kind of preparation method of aluminium base graphene, carbon nanotube composite heat dissipation material |
| CN107313102A (en) * | 2017-07-03 | 2017-11-03 | 鄂尔多斯市紫荆创新研究院 | A kind of aluminium base graphene, the preparation method of CNT composite heat dissipation material |
| WO2019047164A1 (en) * | 2017-09-08 | 2019-03-14 | 深圳大学 | Preparation method for graphene oxide |
| CN108486568A (en) * | 2018-02-26 | 2018-09-04 | 武汉理工大学 | A kind of flaky graphite alkene/metal hetero-junction laminated film and preparation method thereof for heat conduction |
| CN108763764A (en) * | 2018-05-29 | 2018-11-06 | 南京航空航天大学 | A kind of computational methods of graphene-flexible substrates buckling structure deformation |
| CN108763764B (en) * | 2018-05-29 | 2022-04-15 | 南京航空航天大学 | Calculation method for buckling deformation of graphene-flexible substrate structure |
| CN109811175A (en) * | 2019-03-26 | 2019-05-28 | 重庆大学 | A kind of graphene-method of manufacturing carbon/carbon-copper composite material |
| CN110117810B (en) * | 2019-06-10 | 2021-03-30 | 广西师范大学 | Method for preparing modified graphene oxide aluminum composite heat conduction material through electrophoresis |
| CN110117810A (en) * | 2019-06-10 | 2019-08-13 | 广西师范大学 | A kind of method that electrophoresis prepares modified graphene oxide aluminium composite heat conducting material |
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| CN111548516A (en) * | 2020-04-21 | 2020-08-18 | 苏州锦富技术股份有限公司 | Nitrogen-doped graphene copper composite heat dissipation film and preparation method thereof |
| CN111548516B (en) * | 2020-04-21 | 2022-10-21 | 苏州锦富技术股份有限公司 | Nitrogen-doped graphene copper composite heat dissipation film and preparation method thereof |
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| CN114523102A (en) * | 2022-02-28 | 2022-05-24 | 常州烯雷新材料科技有限公司 | Preparation method of powder graphene coated metal particles |
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