CN107381549A - A kind of preparation method of graphene heat conducting film - Google Patents
A kind of preparation method of graphene heat conducting film Download PDFInfo
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- CN107381549A CN107381549A CN201710642873.6A CN201710642873A CN107381549A CN 107381549 A CN107381549 A CN 107381549A CN 201710642873 A CN201710642873 A CN 201710642873A CN 107381549 A CN107381549 A CN 107381549A
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- graphene oxide
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- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/32—Thermal properties
Abstract
The present invention is a kind of preparation method of graphene heat conducting film, belongs to heat conduction technical field of membrane.The present invention is by adding magnesium powder, diethylenetriamine, catalyst and graphene oxide hybrid reaction, graphene oxide is pre-processed, so that the group such as the epoxy radicals on graphene oxide top layer is reduced, after ultrasonic vibration and centrifugal treating, graphene oxide suspension and ethylenediamine, N, N diisopropylethylamine reacts, and further the groups such as the epoxy radicals of surface of graphene oxide is reduced, so as to effectively reduce graphene heat conduction membrane layer gap；Using ethylenediamine as reducing agent, using N, N diisopropylethylamine handles graphene oxide as reduction agent aid, effectively its surface can be reduced, ensureing to react at 100 DEG C of water bath with thermostatic control can just be carried out thoroughly.The beneficial effects of the invention are as follows：Graphene heat conducting film of the present invention has smaller piece lamellar spacing, higher thermal conductivity, is worthy to be popularized and uses.
Description
Technical field
The present invention relates to a kind of preparation method of graphene heat conducting film, belong to heat conduction field of membrane preparation.
Background technology
Graphene（Graphene）It is a kind of new material for the individual layer shape chip architecture being made up of carbon atom.It is one kind by carbon
Atom is with sp2Hybridized orbit composition hexangle type is in the flat film of honeycomb lattice, the two-dimensional material of only one carbon atom thickness.
Graphene heat conducting film not only has high coefficient of thermal conductivity, also has good stability at high temperature, can be used as efficient dissipate
Hot material.Existing heat conducting film is mostly graphite and polyimides, or graphene-graphite composite radiating film, relative to simple
Graphene heat conducting film, the preparation technology of these heat conducting films is complicated, and thermal conductivity is relatively low, and cost is high.
Application No. CN102573413A Chinese patent discloses more than a kind of graphene radiation material, including one layer
The graphene or graphene composite material of monomolecular thickness.Prepared graphene heat dissipation film, thermal conductivity 600W/mk~
1500W/m·k.Wherein, support layer material is insulating resin, metal foil, metal one-faced tapes, single-sided insulation adhesive tape or two-sided exhausted
Edge adhesive tape, thickness are 0.01~0.05mm；Adhesive layer is pressure sensitive adhesive or PUR, and thickness is 0.005~0.05mm.This method work
Skill is complicated, and condition is difficult to control.Therefore this area needs to develop that a kind of preparation technology is simple, the higher graphene heat conduction of thermal conductivity
Film.The Chinese patent of Application No. 201110002281.0 disclosed in prior art is using graphite as raw material, in 950 DEG C of expansion furnace
Interior progress thermal expansion processing, finally by calendering, obtains ultra-thin graphene paper.The thickness of graphene paper is 40 μm, thermal conductivity factor
For 300W/mK.Although the preparation method technique is simple, the graphene paper thermal conductivity factor prepared is low, and heat conductivility is poor.
But the preferable graphene heat conducting film of heat conductivility can be obtained using macromolecule pyrolysismethod, but technique is cumbersome, and every time only
The graphene film of sheet, low yield can be obtained, although graphene film lamellar spacing can be reduced to a certain extent, existing reduces journey
The problems such as degree is not high, and thermal conductivity is relatively low, it is difficult to meet requirement of the manufacturing enterprise to the capacity of heat transmission.Therefore, a kind of low lamella is researched and developed
Gap, the graphene heat conducting film of high thermal conductivity have great importance.
The content of the invention
The technical problems to be solved by the invention：Larger for current graphene oxide layer gap, thermal conductivity is relatively low
A kind of drawback, there is provided preparation method of graphene heat conducting film.
In order to solve the above technical problems, the present invention is using technical scheme as described below：
（1）Graphene oxide is ground, sieves, graphene oxide, magnesium powder, diethylenetriamine, catalyst is well mixed, is added
In beaker equipped with deionized water, reaction, reaction solution A is obtained, by reaction solution A stand at low temperature, filters to obtain solid phase filtrate；
（2）Solid phase filtrate is taken, is added in the beaker equipped with NaOH solution, after stirring, is placed in ultrasonic oscillation device and surpasses
Acoustic shock is swung, and obtains the suspension of graphene oxide；
（3）The suspension of graphene oxide is subjected to centrifugal treating, normal temperature stands to obtain solidliquid mixture, filtered off except in centrifuge tube
Lower floor's solid formation, collect the graphene oxide colloidal suspensions of upper strata isotropic stable；
（4）The graphene oxide colloidal suspensions of collection are added in the beaker equipped with ethanol solution, by ethylenediamine and N, N- bis-
Wopropyl ethyl amine is added in beaker, stirring while adding, water bath with thermostatic control heating response, and standing cools down to obtain reaction solution B, and by reaction solution
B is washed to neutrality；
（5）, will in microporous membrane surface formation thin film after filtering by the reaction solution B after washing by filtering with microporous membrane
Film is placed in baking oven together with filter membrane, and normal temperature stands cooling after drying, and film is taken off from filter membrane, that is, obtains graphene and leads
Hotting mask.
The step（1）The graphene oxide powder of middle screening is 200~400 mesh.
The step（1）Middle graphene oxide, magnesium powder, diethylenetriamine, catalyst, the mass ratio of deionized water are 1:1
~3:1~3:0.1:100.
The step（1）Middle catalyst is any one in Pt/C catalyst, Pd/C catalyst, Fe-N/C catalyst.
The step（2）The quality of middle NaOH solution is 20~30 times of solid phase filtrate.
The step（4）The mass ratio of middle ethylenediamine and DIPEA is 1~4:1.
Compared with other method, advantageous effects are the present invention：
（1）The present invention by add magnesium powder, diethylenetriamine, catalyst and with graphene oxide hybrid reaction, to graphite oxide
Alkene is pre-processed so that and the group such as the epoxy radicals on graphene oxide top layer is reduced, after ultrasonic vibration and centrifugal treating,
Graphene oxide suspension and ethylenediamine, DIPEA reaction, further to the epoxy radicals of surface of graphene oxide
Reduced Deng group, so as to effectively reduce graphene heat conduction membrane layer gap；
（2）The present invention is using ethylenediamine as reducing agent, using DIPEA as reduction agent aid, to graphite oxide
Alkene is handled, and effectively its surface can be reduced, and ensureing to react at 100 DEG C of water bath with thermostatic control can just be carried out thoroughly.
Embodiment
Miillpore filter：Material：Composite fibre film；Specification：D=100mm；Aperture：0.22μm.
The preparation method of graphene heat conducting film of the present invention, comprises the following steps：
（1）Graphene oxide is ground, filters out the graphene oxide particle of 200~400 mesh, in mass ratio 1:1~3:1~3:
0.1:100, graphene oxide, magnesium powder, diethylenetriamine, catalyst, deionized water are well mixed, are placed in beaker, 50~
1~2h is reacted at 60 DEG C, obtains reaction solution A, reaction solution is stood into 30~50min at 0~10 DEG C, filters to obtain solid phase filtrate；
（2）Solid phase filtrate is taken, adds in the beaker of the NaOH solution equipped with 1.8mol/L, after stirring, is placed in ultrasonic wave
In oscillator, 30~40min of ultrasonic vibration under 200~300W power, the suspension of graphene oxide is obtained；
（3）The suspension of graphene oxide is introduced into centrifuge tube, under 600~1200r/min rotating speed centrifugal treating 1~
2min, normal temperature stand 1~3h, filter off the graphene oxide glue that upper strata isotropic stable is collected except lower floor's solid formation in centrifuge tube
Shape suspension；
（4）The graphene oxide suspension of collection is added in the beaker equipped with ethanol solution, in mass ratio 1~4:1 by second two
Amine and DIPEA, add in beaker, it is stirring while adding, 100 DEG C of water bath with thermostatic control heating, 8~10h is reacted, is stood
0.5~1h of cooling obtains reaction solution B, and reaction solution B is washed 2~3 times, in neutrality；
（5）, will in microporous membrane surface formation thin film after filtering by the reaction solution B after washing by filtering with microporous membrane
Film is placed in baking oven together with filter membrane, 60 DEG C of 4~5h of baking, is stood 0.5~1h of cooling, is taken off film from filter membrane after cooling
Under, that is, obtain graphene heat conducting film.
Example 1
Miillpore filter：Material：Composite fibre film；Specification：D=100mm；Aperture：0.22μm.
The preparation method of graphene heat conducting film of the present invention, comprises the following steps：
（1）Graphene oxide is ground, filters out the graphene oxide particle of 200 mesh, in mass ratio 1: 3:1:0.1:100 will
Graphene oxide, magnesium powder, diethylenetriamine, catalyst, deionized water are well mixed, and are placed in beaker, react 2h at 60 DEG C,
Reaction solution A is obtained, reaction solution is stood into 30min at 0 DEG C, filters to obtain solid phase filtrate；
（2）Solid phase filtrate is taken, adds in the beaker of the NaOH solution equipped with 1.8mol/L, after stirring, is placed in ultrasonic wave
In oscillator, the ultrasonic vibration 30min under 300W power, the suspension of graphene oxide is obtained；
（3）The suspension of graphene oxide is introduced into centrifuge tube, centrifugal treating 1min, normal temperature under 1200r/min rotating speed
1h is stood, filters off the graphene oxide colloidal suspensions that upper strata isotropic stable is collected except lower floor's solid formation in centrifuge tube；
（4）The graphene oxide suspension of collection is added in the beaker equipped with ethanol solution, in mass ratio 4:1 by ethylenediamine and
DIPEA, add in beaker, it is stirring while adding, 100 DEG C of water bath with thermostatic control heating, 10h is reacted, stands cooling 0.5h
Reaction solution B is obtained, reaction solution B is washed 3 times, in neutrality；
（5）, will in microporous membrane surface formation thin film after filtering by the reaction solution B after washing by filtering with microporous membrane
Film is placed in baking oven together with filter membrane, 60 DEG C of baking 4h, is stood cooling 0.5h, is taken film off from filter membrane after cooling, produce
To graphene heat conducting film.
Example 2
Miillpore filter：Material：Composite fibre film；Specification：D=100mm；Aperture：0.22μm.
The preparation method of graphene heat conducting film of the present invention, comprises the following steps：
（1）Graphene oxide is ground, filters out the graphene oxide particle of 300 mesh, in mass ratio 1: 2:2:0.1:100 will
Graphene oxide, magnesium powder, diethylenetriamine, catalyst, deionized water are well mixed, and are placed in beaker, react 1.5h at 55 DEG C,
Reaction solution A is obtained, reaction solution is stood into 40min at 5 DEG C, filters to obtain solid phase filtrate；
（2）Solid phase filtrate is taken, adds in the beaker of the NaOH solution equipped with 1.8mol/L, after stirring, is placed in ultrasonic wave
In oscillator, the ultrasonic vibration 30min under 300W power, the suspension of graphene oxide is obtained；
（3）The suspension of graphene oxide is introduced into centrifuge tube, centrifugal treating 2min, normal temperature are quiet under 800r/min rotating speed
2h is put, filters off the graphene oxide colloidal suspensions that upper strata isotropic stable is collected except lower floor's solid formation in centrifuge tube；
（4）The graphene oxide suspension of collection is added in the beaker equipped with ethanol solution, in mass ratio 2:1 by ethylenediamine and
DIPEA, add in beaker, it is stirring while adding, 100 DEG C of water bath with thermostatic control heating, 9h is reacted, stand cooling 1h and obtain
Reaction solution B, reaction solution is washed 3 times, in neutrality；
（5）, will in microporous membrane surface formation thin film after filtering by the reaction solution B after washing by filtering with microporous membrane
Film is placed in baking oven together with filter membrane, 60 DEG C of baking 5h, is stood cooling 1h, is taken film off from filter membrane after cooling, that is, obtain
Graphene heat conducting film.
Example 3
Miillpore filter：Material：Composite fibre film；Specification：D=100mm；Aperture：0.22μm.
The preparation method of graphene heat conducting film of the present invention, comprises the following steps：
（1）Graphene oxide is ground, filters out the graphene oxide particle of 400 mesh, in mass ratio 1: 1:3:0.1:100 will
Graphene oxide, magnesium powder, diethylenetriamine, sodium borohydride, deionized water are well mixed, and are placed in beaker, react 1h at 50 DEG C,
Reaction solution A is obtained, reaction solution is stood into 50min at 10 DEG C, filters to obtain solid phase filtrate；
（2）Solid phase filtrate is taken, adds in the beaker of the NaOH solution equipped with 1.8mol/L, after stirring, is placed in ultrasonic wave
In oscillator, the ultrasonic vibration 40min under 300W power, the suspension of graphene oxide is obtained；
（3）The suspension of graphene oxide is introduced into centrifuge tube under 600r/min rotating speed to centrifugal treating 2min, normal temperature are quiet
3h is put, filters off the graphene oxide colloidal suspensions that upper strata isotropic stable is collected except lower floor's solid formation in centrifuge tube；
（4）The graphene oxide suspension of collection is added in the beaker equipped with ethanol solution, in mass ratio 1:1 by ethylenediamine and
DIPEA, add in beaker, it is stirring while adding, 100 DEG C of water bath with thermostatic control heating, 8h is reacted, stand cooling 1h and obtain
Reaction solution B, reaction solution B is washed 3 times, in neutrality；
（5）, will in microporous membrane surface formation thin film after filtering by the reaction solution B after washing by filtering with microporous membrane
Film is placed in baking oven together with filter membrane, 60 DEG C of baking 5h, is stood cooling 1h, is taken film off from filter membrane after cooling, that is, obtain
Graphene heat conducting film.
Reference examples：The graphene heat conducting film of company of Xiamen City production
The graphene heat conducting film of graphene heat conducting film obtained by above-described embodiment and reference examples is detected, specific detection is as follows：
Thermal conductivity measuring instrument：Heat conductivity dynamic measurer；
Thickness measuring instrument：AFM, it is 25 DEG C, constant pressure 0.1MPa to set steady temperature；
As a result it is as shown in table 1.
Table 1：
| Detection project | Example 1 | Example 2 | Example 3 | Reference examples |
| Horizontal thermal conductivity W/ (mk) | 1045 | 960 | 880 | 800 |
| Vertical thermal conductivity W/ (mk) | 50 | 43 | 38 | 25 |
| Thickness/mm | 0.028 | 0.034 | 0.038 | 0.04 |
As seen from the above table, graphene heat conducting film of the present invention has higher thermal conductivity, meets requirement, is worthy to be popularized and makes
With.
Claims (6)
1. a kind of preparation method of graphene heat conducting film, it is characterised in that this method comprises the following steps：
（1）Graphene oxide is ground, sieves, graphene oxide, magnesium powder, diethylenetriamine, catalyst is well mixed, is added
In beaker equipped with deionized water, reaction, reaction solution A is obtained, by reaction solution A stand at low temperature, filters to obtain solid phase filtrate；
（2）Solid phase filtrate is taken, is added in the beaker equipped with NaOH solution, after stirring, is placed in ultrasonic oscillation device and surpasses
Acoustic shock is swung, and obtains the suspension of graphene oxide；
（3）The suspension of graphene oxide is subjected to centrifugal treating, normal temperature stands to obtain solidliquid mixture, filtered off except in centrifuge tube
Lower floor's solid formation, collect the graphene oxide colloidal suspensions of upper strata isotropic stable；
（4）The graphene oxide colloidal suspensions of collection are added in the beaker equipped with ethanol solution, by ethylenediamine and N, N- bis-
Wopropyl ethyl amine is added in beaker, stirring while adding, water bath with thermostatic control heating response, and standing cools down to obtain reaction solution B, and by reaction solution
B is washed to neutrality；
（5）, will in microporous membrane surface formation thin film after filtering by the reaction solution B after washing by filtering with microporous membrane
Film is placed in baking oven together with filter membrane, and normal temperature stands cooling after drying, and film is taken off from filter membrane, that is, obtains graphene and leads
Hotting mask.
2. the preparation method of graphene heat conducting film according to claim 1, it is characterised in that the step（1）Middle screening
Graphene oxide powder is 200~400 mesh.
3. the preparation method of graphene heat conducting film according to claim 1, it is characterised in that the step（1）Middle oxidation stone
Black alkene, magnesium powder, diethylenetriamine, catalyst, the mass ratio of deionized water are 1:1~3:1~3:0.1:100.
4. the preparation method of graphene heat conducting film according to claim 1, it is characterised in that the step（1）Middle catalyst
For any one in Pt/C catalyst, Pd/C catalyst, Fe-N/C catalyst.
5. the preparation method of graphene heat conducting film according to claim 1, it is characterised in that the step（2）
The quality of middle NaOH solution is 20~30 times of solid phase filtrate.
6. the preparation method of graphene heat conducting film according to claim 1, it is characterised in that the step（4）
The mass ratio of middle ethylenediamine and DIPEA is 1~4:1.
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| CN110240892A (en) * | 2019-07-03 | 2019-09-17 | 桂林理工大学 | A kind of bionic laminar graphene/imide derivative thermally conductive film and preparation method thereof |
| CN112898953A (en) * | 2021-01-14 | 2021-06-04 | 蒋军良 | Preparation method of graphene heat-conducting film |
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