CN110255538A - A kind of preparation method of graphene cooling fin - Google Patents
A kind of preparation method of graphene cooling fin Download PDFInfo
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- CN110255538A CN110255538A CN201910562588.2A CN201910562588A CN110255538A CN 110255538 A CN110255538 A CN 110255538A CN 201910562588 A CN201910562588 A CN 201910562588A CN 110255538 A CN110255538 A CN 110255538A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/24—Thermal properties
Abstract
The invention discloses a kind of preparation methods of graphene cooling fin, comprising: is add to deionized water graphite oxide, adds dispersing agent, agitated, oscillation or ultrasound, aqueous graphene oxide solution is prepared；The aqueous graphene oxide solution is coated on substrate, and is made it dry, graphene oxide membrane is obtained, the graphene oxide membrane is stripped down from the substrate；The graphene oxide membrane stripped down using laser irradiation obtains graphene film so that graphene oxide restores；The graphene film is placed in retort, charing process is carried out；Graphene film after charing process is subjected to roll-in, graphene cooling fin is made.By the present invention in that carbonizing with laser reduction graphene oxide and to it, the graphene cooling fin with excellent heat dissipation property can be made, technique is easily controllable, and purity is high.
Description
Technical field
The present invention relates to the technical fields of electronic product radiating material, and in particular to a kind of high thermal conductivity graphene cooling fin
Preparation method.
Background technique
With the rapid development of modern science and technology, the micromation of electronic device, chip dominant frequency are continuously improved, and function increasingly increases
By force, the power consumption of one single chip is gradually increased, these result in heat flow density and sharply increase.For example, the electricity such as current mobile phone, computer
Sub- product has become the necessity of people's life.With the continuous upgrading of hardware, the calculating of performed task is more complicated
Cumbersome, the core components such as CPU, GPU will face the puzzlement of heat, and the dominant frequency of chip improves, and power increase generates amount of heat,
If heat is unable to disperse in time, the reduction of frequency will cause, while heat source position thermal sensation becomes stronger.Actual use process
In, electronic component and battery can all generate a large amount of heat.And studies have shown that being more than the failure mode of 55% electronic equipment
Be by temperature it is excessively high caused by, in order to not influence normal operation, good cooling system is particularly important, therefore electronic component
Heat dissipation problem plays the role of very important in the development of electronic component.How above-mentioned heat is shed in time, guarantees electricity
Sub- component and normal battery operation have to consider when being a good thermal solution design.
Existing market portioned product carries out heat conduction and heat radiation, especially copper and aluminium by metal group material, although copper is thermally conductive
Coefficient is 398W/mK, but weight is big, oxidizable etc. to limit its application, and the thermal coefficient of aluminium is 237W/mK,
It is difficult meet the needs of existing product is to heat conduction and heat radiation.
Heat dissipation film made of the natural graphite material and artificial synthesized graphite material used at present is to electronic product
Heat dissipation have certain improvement.In the case where using graphite radiating film in the heat sink conception of electronic product, graphite radiating film
Thermal coefficient be only capable of reaching about 1500W/mK, be not able to satisfy part height heat dissipation product demand.Therefore a height is researched and developed
The heat dissipation film of heat dissipation is imperative.
Graphene (Graphenes) is a kind of two-dimentional carbon nanomaterial being made of carbon atom with sp2 hybridized orbit, is single
The general designation of layer graphene, bilayer graphene and multi-layer graphene.Graphene is the nanometer material that known world is most thin, most hard
Material, it is almost fully transparent, the light of absorption 2.3%；With excellent heat-conductive characteristic, wherein flawless single layer stone
The thermal coefficient of black alkene is higher than carbon nanotube and diamond, is the highest carbon material of thermal coefficient so far, but its preparation is tired
It is difficult, at high cost.
It is then desired to develop the new fin material with high-termal conductivity, especially prepare the material and be easy to control
The method of system and purity is high meets market for the demand of the heat dissipation problem of electronic component and battery etc., solves the prior art
Deficiency.
Summary of the invention
In order to solve above-mentioned the deficiencies in the prior art, by the present invention in that being carried out with laser reduction graphene oxide and to it
Charing process provides a kind of preparation method of graphene cooling fin.It can be made by means of the present invention with excellent heat dissipation
The graphene cooling fin of performance, technique is easily controllable, and product purity is high, wherein the thermal coefficient of graphene cooling fin obtained
Up to 2103W/mK.
The present invention adopts the following technical scheme that:
A kind of preparation method of graphene cooling fin, wherein itself the following steps are included:
Graphite oxide is add to deionized water, dispersing agent, agitated, oscillation or ultrasound is added, water is prepared
Property graphene oxide solution；
The aqueous graphene oxide solution is coated on substrate, and is made it dry, graphene oxide membrane is obtained, by institute
Graphene oxide membrane is stated to strip down from the substrate；
The graphene oxide membrane stripped down using laser irradiation obtains graphene film so that graphene oxide restores；
The graphene film is placed in retort, charing process is carried out；
Graphene film after charing process is subjected to roll-in, graphene cooling fin is made.
Preferably, the piece diameter D50 of the graphene oxide is 20~100 μm, preferably 50~80 μm.
Preferably, the concentration of the aqueous graphene oxide solution is 0.5~10mg/mL, preferably 1~5mg/mL.
Preferably, the coating is transfer coated, intaglio printing, spraying or other coating methods.
Preferably, the laser is the superlaser that wavelength is 400~800nm, and optimal wavelength is the height of 400~750nm
It can laser.
Preferably, the temperature of the charing process is 600~1500 DEG C, preferably 850~1250 DEG C.
Preferably, graphene cooling fin obtained with a thickness of 5~50 μm, preferably 10~30 μm.
The effect of invention
Graphene cooling fin obtained can reduce interface resistance, optimization lattice structure, realize and lead by the method for the invention
Heat leak.For example, the heat dissipation performance of graphene cooling fin obtained is obvious by the method for the invention in the identical situation of thickness
Better than graphite heat radiation fin.The graphene cooling fin prepared by the present invention with a thickness of 10 μm when, the graphene cooling fin
Horizontal direction thermal coefficient may be up to 2103W/mK.The method of the invention graphene cooling fin obtained with a thickness of 25 μm
Horizontal thermal conductivity factor is 2025W/mK, hence it is evident that higher than the horizontal thermal conductivity factor of the commercially available graphite heat radiation fin with a thickness of 25 μm
1500W/m·K.Method process operation of the invention is simple, easily controllable, and product purity is high, can be met with lower cost
Requirement of the market to cooling fin.
Detailed description of the invention
Fig. 1 is the flow chart for the method that the present invention prepares graphene cooling fin.
The graphene cooling fin of Fig. 2 one specific embodiment of the present invention and the horizontal direction of commercially available graphite heat radiation fin are thermally conductive
The comparison result (graphene fin thickness and graphite heat radiation fin thickness be 25 μm) of coefficient.
Comparison result (the graphene of the horizontal direction thermal coefficient of the graphene cooling fin of different-thickness Fig. 3 of the invention
Fin thickness is respectively 25 μm and 10 μm).
The heat dissipation effect comparison of the graphene cooling fin and commercially available graphite heat radiation fin of Fig. 4 one specific embodiment of the present invention
Figure.
Specific embodiment
The present invention will be described in detail below with reference to the drawings of preferred embodiments, whereby to the present invention how applied technology method
Technical problem is solved, and the realization process for reaching technical effect can fully understand and implement.
It makes an explanation below in conjunction with attached drawing to exemplary embodiment of the invention, including each of embodiment of the present invention
Kind details should think them only exemplary to help understanding.Therefore, those of ordinary skill in the art should recognize
It arrives, embodiment described herein can be made various changes and modifications, without departing from scope and spirit of the present invention.
Although there is used herein specific term, they are only used for general and descriptive meaning, rather than in order to
The purpose of limitation.Unless otherwise defined, all technical and scientific terms used herein has the master described with the disclosure
Inscribe the normally understood identical meaning of those of ordinary skill in the art.
Term in invention
" graphene oxide " herein, is product of the powdered graphite after chemical oxidation and removing, and color is pale brown
Color can be via various and oxygen-containing function because after aoxidizing, oxygen-containing functional group increases and keeps property more active compared with graphene thereon
Group reaction and improve nature.After aoxidizing, graphene oxide still maintains the layer structure of graphite, graphene oxide sheet
The diameter of layer is graphene oxide sheet diameter.
" aqueous graphene oxide solution " herein, refers to and is add to deionized water graphite oxide, adds point
Powder, agitated, oscillation or ultrasound, are made aqueous graphene oxide solution.
" D50 " herein refers to that the cumulative particle sizes percentile an of sample reaches partial size corresponding when 50%.
Its physical significance is that partial size is greater than its particle and accounts for 50%, also accounts for 50%, D50 less than its particle and is also meso-position radius or intermediate value
Partial size.Graphene oxide sheet diameter D50 is that the accumulative flake diameter distribution percentage of graphene oxide sample reaches corresponding when 50%
Piece diameter.
" charing " herein refers to that solid phase carbonizes, i.e., solid carbonization reaction object without gas phase or liquid phase and directly in
Solid-state is decomposed reacts with thermal polycondensation, becomes the process of solid-state charing product.
" thermal coefficient " herein, refers under the conditions of steady heat transfer, the material of 1m thickness, and the temperature difference of both side surface is 1
Degree (K, DEG C), in 1 second, the heat transmitted by 1 square metre of area, unit is watt/ meter Du (W/mK, it is available for K herein
DEG C replace).For anisotropic material, horizontal direction thermal coefficient and vertical direction thermal coefficient have difference.
In a specific embodiment, referring to Fig.1, the preparation method of graphene cooling fin of the invention includes following five
A step: the first step prepares aqueous graphene oxide solution using graphene oxide and aqueous solvent；Second step, by the water
Property graphene oxide solution is coated on substrate, and is made it dry, and graphene oxide membrane is obtained, by the graphene oxide membrane from
It is stripped down on the substrate；Third step, the graphene oxide membrane stripped down using laser irradiation, so that graphene oxide is also
Original obtains graphene film；The graphene film is placed in retort by the 4th step, carries out charing process；5th step will carbonize
Treated, and graphene film carries out roll-in, and graphene cooling fin is made.
In a specific embodiment, aqueous graphene oxide solution preparation process are as follows: refer to and be added to graphite oxide
In deionized water, dispersing agent, agitated, oscillation or ultrasound are added, aqueous graphene oxide solution is made.
In a specific embodiment, the piece diameter D50 of the graphene oxide is 20~100 μm, the aqueous oxidation
The concentration of graphene solution is 0.5~10mg/mL.
In a specific embodiment, the piece diameter D50 of the graphene oxide is 50~80 μm, the aqueous oxidation stone
The concentration of black alkene solution is 1~5mg/mL.
In a specific embodiment, the laser is the superlaser that wavelength is 400~800nm, at the charing
The temperature of reason is 600~1500 DEG C.
In a specific embodiment, the laser is the superlaser that wavelength is 400~750nm, at the charing
The temperature of reason is 850~1250 DEG C.
In a specific embodiment, the coating is transfer coated, intaglio printing, spraying or other coating methods,
Obtained graphene cooling fin with a thickness of 5~50 μm, preferably 10~30 μm.
In a specific embodiment, the piece diameter D50 of the graphene oxide is 20~100 μm, the aqueous oxidation
The concentration of graphene solution is 0.5~10mg/mL, and the laser is the superlaser that wavelength is 400~800nm, the charing
The temperature of processing is 600~1500 DEG C, and the coating is transfer coated, intaglio printing, spraying or other coating methods, obtained
Graphene cooling fin with a thickness of 5~50 μm.
In a specific embodiment, the piece diameter D50 of the graphene oxide is 50~80 μm, the aqueous oxidation stone
The concentration of black alkene solution is 1~5 μm, and the laser is the superlaser that wavelength is 400~750nm, the temperature of the charing process
Degree is 850~1250 DEG C, and the coating is transfer coated, intaglio printing, spraying or other coating methods, obtained graphene
Cooling fin with a thickness of 10~30 μm.
The preparation method of graphene cooling fin of the invention, solves and is used to prepare electronic component and electricity currently on the market
The problem that the heat sink material in pond etc. is not easy to control or purity is lower is had by the graphene cooling fin that method of the invention is prepared
There is high thermal conductivity, meets the demand of high heat dissipation product well, substantially improve the thermal diffusivity of electronic component and battery.
By in preparation method each parameter and term restriction within the scope of the invention so that the horizontal direction of graphene cooling fin is thermally conductive
Coefficient reaches 1700W/mK or more.The preparation method simple possible is readily produced, and is had and is realized the huge latent of industrialization production
Power.
Embodiment
Embodiment 1
Graphite oxide is add to deionized water, dispersing agent, agitated, oscillation or ultrasound is added, water is prepared
Property graphene oxide solution, wherein the piece diameter of graphene oxide is 90 μm, and the concentration of graphene oxide solution is 0.5mg/mL.It adopts
Graphene oxide solution is coated on substrate with transfer coated mode, obtains graphene oxide membrane after dry, and stone will be aoxidized
Black alkene film is stripped down from substrate.Wavelength is used to be irradiated in graphene oxide membrane for the superlaser of 788nm, so that
Graphene oxide reduction, obtains graphene film.Above-mentioned graphene film is put into retort, 1250 DEG C at a temperature of carry out charcoal
Change processing.Graphene film after charing process is subjected to roll-in, obtains the graphene cooling fin with a thickness of 10 μm.After tested, it obtains
The horizontal direction thermal coefficient of the graphene cooling fin arrived is 1928W/mK.
Embodiment 2
The piece diameter of graphene oxide is set as 50 μm, the concentration of graphene oxide solution is set as 1.5mg/mL, high energy
The wavelength of laser is set as 418nm, and charing process temperature is set as 1500 DEG C, obtains graphene heat sink compound thickness and is set as
20 μm, in addition to this, graphene cooling fin is prepared in the same manner as example 1, and carry out various evaluations.After tested, it obtains
The horizontal direction thermal coefficient of the graphene cooling fin arrived is 1800W/mK.
Embodiment 3
The piece diameter of graphene oxide is set as 20 μm, the concentration of graphene oxide solution is set as 5mg/mL, and high energy swashs
The wavelength of light is set as 655nm, and charing process temperature is set as 900 DEG C, obtains graphene heat sink compound thickness and is set as 50 μ
In addition to this m prepares graphene cooling fin, and carry out various evaluations in the same manner as example 1.After tested, it obtains
The horizontal direction thermal coefficient of the graphene cooling fin is 1733W/mK.
Embodiment 4
The piece diameter of graphene oxide is set as 50 μm, the concentration of graphene oxide solution is set as 2.5mg/mL, high energy
The wavelength of laser is set as 488nm, and charing process temperature is set as 1300 DEG C, obtains graphene heat sink compound thickness and is set as
30 μm, in addition to this, graphene cooling fin is prepared in the same manner as example 1, and carry out various evaluations.After tested, it obtains
The horizontal direction thermal coefficient of the graphene cooling fin arrived is 1950W/mK.
Embodiment 5
The piece diameter of graphene oxide is set as 60 μm, the concentration of graphene oxide solution is set as 1mg/mL, and high energy swashs
The wavelength of light is set as 730nm, and charing process temperature is set as 1200 DEG C, obtains graphene heat sink compound thickness and is set as 25
μm, in addition to this, graphene cooling fin is prepared in the same manner as example 1, and carry out various evaluations.After tested, it obtains
The graphene cooling fin horizontal direction thermal coefficient be 2025W/mK.
Embodiment 6
The piece diameter of graphene oxide is set as 60 μm, the concentration of graphene oxide solution is set as 1mg/mL, and high energy swashs
The wavelength of light is set as 730nm, and charing process temperature is set as 1200 DEG C, obtains graphene heat sink compound thickness and is set as 10
μm, in addition to this, graphene cooling fin is prepared in the same manner as example 1, and carry out various evaluations.After tested, it obtains
The graphene cooling fin horizontal direction thermal coefficient be 2103W/mK.
Embodiment 7
The piece diameter of graphene oxide is set as 55 μm, the concentration of graphene oxide solution is set as 2mg/mL, and high energy swashs
The wavelength of light is set as 650nm, and charing process temperature is set as 1150 DEG C, obtains graphene heat sink compound thickness and is set as 20
μm, in addition to this, graphene cooling fin is prepared in the same manner as example 1, and carry out various evaluations.After tested, it obtains
The graphene cooling fin horizontal direction thermal coefficient be 2008W/mK.
Embodiment 8
The piece diameter of graphene oxide is set as 35 μm, the concentration of graphene oxide solution is set as 6mg/mL.Using spray
Graphene oxide solution is coated on substrate by painting mode, obtains graphene oxide membrane after dry, and by graphene oxide membrane from
It is stripped down on substrate.600nm is set as using the wavelength of superlaser, charing process temperature is set as 1000 DEG C, obtains stone
Black alkene heat sink compound thickness is set as 35 μm, in addition to this, prepares graphene cooling fin in the same manner as example 1,
And carry out various evaluations.After tested, the horizontal direction thermal coefficient of the graphene cooling fin obtained is 1850W/mK.
Embodiment 9
The piece diameter of graphene oxide is set as 70 μm, the concentration of graphene oxide solution is set as 5.5mg/mL, high energy
The wavelength of laser is set as 788nm, and charing process temperature is set as 1450 DEG C, obtains graphene heat sink compound thickness and is set as
28 μm, in addition to this, graphene cooling fin is prepared in the same manner as example 1, and carry out various evaluations.After tested, it obtains
The horizontal direction thermal coefficient of the graphene cooling fin arrived is 1980W/mK.
Embodiment 10
The piece diameter of graphene oxide is set as 85 μm, the concentration of graphene oxide solution is set as 0.8mg/mL.Using
Graphene oxide solution is coated on substrate by intaglio printing mode, obtains graphene oxide membrane after dry, and by graphite oxide
Alkene film is stripped down from substrate.430nm is set as using the wavelength of superlaser, charing process temperature is set as 1300 DEG C,
It obtains graphene heat sink compound thickness and is set as 8 μm, in addition to this, prepare graphene in the same manner as example 1 and dissipate
Backing, and carry out various evaluations.After tested, the horizontal direction thermal coefficient of the graphene cooling fin obtained is 1655W/m
K。
Embodiment 11
The piece diameter of graphene oxide is set as 15 μm, the concentration of graphene oxide solution is set as 0.3mg/mL.Using
Graphene oxide solution is coated on substrate by transfer coated mode, obtains graphene oxide membrane after dry, and by graphite oxide
Alkene film is stripped down from substrate.380nm is set as using the wavelength of superlaser, charing process temperature is set as 1550 DEG C,
It obtains graphene heat sink compound thickness and is set as 55 μm, in addition to this, prepare graphene in the same manner as example 1 and dissipate
Backing, and carry out various evaluations.After tested, the horizontal direction thermal coefficient of the graphene cooling fin obtained is 1625W/m
K。
Comparative example
The comparative example used in the present invention is the commercially available graphite heat radiation fin with a thickness of 25 μm.
Following table 1 lists the preparation condition and acquired results of above-described embodiment and reference material.
Table 1
Fig. 2 is the comparison of the graphene cooling fin of embodiment 5 and the horizontal direction thermal coefficient of commercially available graphite heat radiation fin
As a result, the two thickness is 25 μm, the horizontal direction thermal coefficient of the cooling fin of graphene made from the method for the present invention is
2025W/mK, and the horizontal direction thermal coefficient of commercially available graphite heat radiation fin is 1500W/mK.From upper table 1 and the number of Fig. 2
According to can be seen that by the method for the invention all graphene cooling fins obtained with commercially available graphite heat radiation fin compared with higher
Heat point source preferably can be diffused into plane heat source and distributed heat is uniform by thermal coefficient.And the method for the present invention
Technological operation is simple, easily controllable, and product purity is high.Graphene cooling fin obtained is as electronics by the method for the invention
The ideal material of equipment package heat dissipation purposes.
Fig. 3 be thickness be respectively 25 μm and 10 μm graphene cooling fin of the invention horizontal direction thermal coefficient ratio
Relatively result.It can be seen that graphene cooling fin of the invention from the data of Fig. 3, within the scope of certain thickness, thickness is smaller, leads
Hot coefficient is higher, and heating conduction is better.
Experimental example
5 gained graphene cooling fin of embodiment and the graphite heat radiation fin of comparative example are packed into money mobile phone test, mobile phone fortune
After row 2 hours, tested with infrared thermal imaging equipment, as a result as shown in Figure 4.It can be seen from the figure that using graphite radiating
After piece, temperature is high, and superheating phenomenon is locally present；And after using graphene cooling fin, without obvious hot spot, temperature is lower, and temperature
Degree is uniformly distributed, with the obvious advantage.
Although being described and illustrated in the present invention to some specific embodiments, it should be appreciated that, the present invention
In specific embodiment be for further explaining the intent of the present invention and content, be not for being constituted to the present invention
Certain limitation, without departing from spirit of the invention and be intended to and claims in limit range under the premise of, can be right
The present invention carries out certain modification.
Claims (10)
1. a kind of preparation method of graphene cooling fin, wherein itself the following steps are included:
Graphite oxide is add to deionized water, dispersing agent, agitated, oscillation or ultrasound is added, aqueous oxygen is prepared
Graphite alkene solution；
The aqueous graphene oxide solution is coated on substrate, and is made it dry, graphene oxide membrane is obtained, by the oxygen
Graphite alkene film is stripped down from the substrate；
The graphene oxide membrane stripped down using laser irradiation obtains graphene film so that graphene oxide restores；
The graphene film is placed in retort, charing process is carried out；
Graphene film after charing process is subjected to roll-in, graphene cooling fin is made.
2. preparation method according to claim 1, wherein the piece diameter D50 of the graphene oxide is 20~100 μm.
3. preparation method according to claim 1 or 2, wherein the piece diameter D50 of the graphene oxide is 50~80 μm.
4. preparation method described in any one of claim 1 to 3, wherein the aqueous graphene oxide solution it is dense
Degree is 0.5~10mg/mL.
5. preparation method according to any one of claims 1 to 4, wherein the aqueous graphene oxide solution it is dense
Degree is 1~5mg/mL.
6. preparation method according to any one of claims 1 to 5, wherein the coating is transfer coated, intaglio process
Brush, spraying or other coating methods.
7. preparation method described according to claim 1~any one of 6, wherein the laser is that wavelength is 400~800nm
Superlaser.
8. preparation method according to any one of claims 1 to 7, wherein the laser is that wavelength is 400~750nm
Superlaser.
9. preparation method described according to claim 1~any one of 8, wherein the temperature of the charing process be 600~
1500 DEG C, preferably 850~1250 DEG C.
10. preparation method described according to claim 1~any one of 9, wherein graphene cooling fin obtained with a thickness of
5~50 μm, preferably 10~30 μm.
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| CN110723725A (en) * | 2019-11-04 | 2020-01-24 | 中国科学院福建物质结构研究所 | Low-power laser reduction graphene film and preparation method thereof |
| CN111003706A (en) * | 2019-11-25 | 2020-04-14 | 苏州盈顺绝缘材料有限公司 | Preparation method of graphene heat conduction and dissipation material |
| CN111137878A (en) * | 2020-01-07 | 2020-05-12 | 上海烯望材料科技有限公司 | Graphene heat dissipation film and preparation method thereof |
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Application publication date: 20190920 |