CN107352533B - Utilize the flexible heat conducting film and preparation method thereof of more partial size graphenes synergistic effect - Google Patents
Utilize the flexible heat conducting film and preparation method thereof of more partial size graphenes synergistic effect Download PDFInfo
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- CN107352533B CN107352533B CN201710555360.1A CN201710555360A CN107352533B CN 107352533 B CN107352533 B CN 107352533B CN 201710555360 A CN201710555360 A CN 201710555360A CN 107352533 B CN107352533 B CN 107352533B
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- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/24—Thermal properties
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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
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- C01B2204/32—Size or surface area
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Abstract
The present invention provides a kind of flexible heat conducting film and preparation method thereof using more partial size graphenes synergistic effect, heat conducting film of the invention is uniformly mixed with by the graphene powder of different-grain diameter, preparation method includes: by big partial size graphene powder, middle partial size graphene powder, small particle graphene powder, it is scattered in deionized water, mixes；It will be prepared into graphene film containing the dispersion solution there are many partial size graphene powder, obtains the heat conducting film.The present invention is uniformly mixed with heat conducting film using the graphene powder of a variety of different-grain diameters, and the graphene powder of various different-grain diameters produces apparent synergistic effect, greatly improves the thermal coefficient of film.Meanwhile prepared heat conducting film has good flexibility, can be used for solving the heat dissipation problem of flexible circuit etc..
Description
Technical field
The present invention relates to a kind of flexible heat conducting films and preparation method thereof, specifically, being to utilize more partial sizes about a kind of
The flexible heat conducting film and preparation method thereof of graphene synergistic effect.
Background technique
With the rapid development of electronics technology industry, electronic product increasingly lighting, while functional requirement also gradually increases
Add.The integrated level and packing density of electronic component are continuously improved so that calorific value increased dramatically when product is run.Power consumption increases
Caused heat dissipation problem is urgently to be resolved, and the production preparation of all kinds of heat-conducting interface materials and heat conducting film has attracted extensive concern.
But heat conducting film at present on the market generallys use the graphene raw material of single particle size or metal material simply rolls
Processing preparation, the usual thermal conductivity of the heat conducting film of preparation is lower, and application is restricted.
Summary of the invention
It is an object of the present invention to provide a kind of heat conducting films with higher heat-conductivity.
Another object of the present invention is to provide a kind of preparation methods of heat conducting film with higher heat-conductivity.
The present invention is uniformly mixed with heat conducting film, the stone of various different-grain diameters using the graphene powder of a variety of different-grain diameters
Black alkene powder produces apparent synergistic effect, greatly improves the thermal coefficient of film.Meanwhile method preparation of the invention
Heat conducting film have good flexibility, can be used for solving the heat dissipation problem of flexible circuit etc..
It on the one hand, the present invention provides a kind of heat conducting film, is uniformly mixed with by the graphene powder of different-grain diameter
It forms.
Specific embodiment according to the present invention, heat conducting film of the invention, raw material composition in include big partial size graphene
Powder, middle partial size graphene powder and small particle graphene powder, the big partial size graphene powder, middle partial size Graphene powder
The mass ratio of body and small particle graphene powder is 2~4:5~6:1~2.
In some specific embodiments of the invention, heat conducting film of the invention, raw material composition in include big partial size stone
Black alkene powder, middle partial size graphene powder and small particle graphene powder, big partial size graphene powder account for heat conducting film gross mass
20%~40%, middle partial size graphene powder accounts for the 50%~60% of heat conducting film gross mass, and small particle graphene powder, which accounts for, leads
The 10%~20% of hotting mask gross mass.
The partial size of specific embodiment according to the present invention, heat conducting film of the invention, the big partial size graphene powder is
30 μm~40 μm.
The partial size of specific embodiment according to the present invention, heat conducting film of the invention, the middle partial size graphene powder is
15 μm~25 μm.
Specific embodiment according to the present invention, heat conducting film of the invention, the partial size of the small particle graphene powder are 1
μm~2 μm.
Heat conducting film of the invention, lateral thermal coefficient are 50~400W/ (mK), and longitudinal thermal coefficient is 0.7~4W/
(mK), with a thickness of 20~107 μm, 0.25~1.3g/cm of density3.Meanwhile the heat conducting film of method preparation of the invention is with good
Good flexibility, can bend 51~70 times or higher without fractureing, can be used to solve the heat dissipation problem of flexible circuit etc..
On the other hand, the present invention also provides a kind of methods for preparing the heat conducting film, this method comprises:
By the graphene powder of different-grain diameter (such as big partial size graphene powder, middle partial size graphene powder and granule
Diameter graphene powder) it is scattered in deionized water, obtain a variety of partial size graphene powder dispersion solution；
A variety of partial size graphene powder dispersion solution are prepared into graphene film, obtain the heat conducting film.
Specific embodiment according to the present invention, in the preparation method of heat conducting film of the invention, the graphene powder is
The processed graphene powder of acid.
Specific embodiment according to the present invention, in the preparation method of heat conducting film of the invention, at the acid of graphene powder
Reason method includes:
Graphene powder and acid are mixed, in conjunction with ultrasonic treatment, obtain the processed graphene powder of acid.
Specific embodiment according to the present invention, the preparation method of heat conducting film of the invention, it is described acid treatment process in, it is excellent
Selection of land, the acid are selected from one of sulfuric acid, nitric acid or a variety of.It is highly preferred that the acid is the mixed acid of sulfuric acid and nitric acid,
The volume ratio of middle sulfuric acid and nitric acid is 3~5:1~2.
Specific embodiment according to the present invention, the preparation method of heat conducting film of the invention, it is described acid treatment process in, together
When combine ultrasonic treatment, the ultrasonic treatment condition is preferred are as follows: 400W~800W handles 3~12h.
The present invention shows to be used to prepare of the invention lead by the graphene powder of the above acid processing by experimental study
Hotting mask is beneficial to the formation of heat conducting film, particularly suitable for a variety of partial size graphene powders are dispersed solution to filter into
Embrane method prepares the process of heat conducting film.
Specific embodiment according to the present invention is to take the processed stone of acid in the preparation method of heat conducting film of the invention
Black alkene powder is scattered in deionized water together with the dispersion liquid of acid, is used to prepare heat conducting film.The processed Graphene powder of acid
For body together in the dispersion liquid of acid, the concentration of graphene powder is about 3mg/ml~5mg/ml.
Specific embodiment according to the present invention, in the preparation method of heat conducting film of the invention, the use of the deionized water
Amount and the weight ratio of big partial size graphene are 1:0.00001~0.00005.
Specific embodiment according to the present invention, in the preparation method of heat conducting film of the invention, can be used filter membrane formation process,
A variety of partial size graphene powder dispersion solution are prepared into graphene film by vacuum drying method, roll-in film forming etc..These tools
The method of body is referred to the preparation method of uniform particle size graphene film in the prior art.In the present invention, formed a film using filtering
When method, it is preferred to use intermittence filters (dispersion liquid is added several times).Using vacuum drying method, preferably control drying condition is 60
℃12h.Using roll-in membrane formation process, preferably control condition is 4Mpa, 1min.
Beneficial effects of the present invention:
The present invention is uniformly mixed with heat conducting film using the graphene powder of a variety of different-grain diameters, and heating conduction is better than single
The graphene film of partial size produces apparent synergistic effect, greatly improves the thermal coefficient of film.Meanwhile it is of the invention
The heat conducting film of method preparation has good flexibility, can be used for solving the heat dissipation problem of flexible circuit etc..
Detailed description of the invention
Fig. 1 is the graphene film that a specific embodiment of the invention is prepared.
Fig. 2 is to test schematic diagram to the flexible test of graphene film in the specific embodiment of the invention.
Specific embodiment
The present invention will be further described with reference to embodiments, these embodiments are not intended to restrict the invention, for
For those skilled in the art, the invention may be variously modified and varied.All within the spirits and principles of the present invention, institute
Any modification, equivalent substitution, improvement and etc. of work, should all be included in the protection scope of the present invention.
Embodiment 1
The heat conducting film of the present embodiment is prepared according to the following steps:
1. taking big partial size graphene powder (35~37 μm of particle size distribution range), medium grain size graphene powder (partial size point
18~20 μm of cloth range), small particle graphene powder (1~2 μm of particle size distribution range), respectively carry out the following conditions acid at
Reason:
The graphene powder is added in the acid solution that sulfuric acid and nitric acid are mixed according to volume ratio 3:1, is subject to ultrasonic place
Reason, the ultrasonic treatment condition are as follows: 600W handles 6h, obtains graphene dispersing solution；In each graphene dispersing solution, graphene powder
Concentration be 4mg/ml；
2. taking processed big partial size graphene (35~37 μm) dispersion liquid of 0.03g acid, (0.03g is with the stone in dispersion liquid
Black alkene poidometer, that is, take 7.5mL Graphene powder dispersion liquid herein；Below in relation to the graphene dispersing solution for taking specified weight
Expression way is identical), it is scattered in 1L deionized water, is dispersed with stirring uniformly；
3. taking processed medium grain size graphene (18~20 μm) dispersion liquid of 0.05g acid, it is scattered in prepared by step 2
In solution；
4. taking processed small particle graphene (1~2 μm) dispersion liquid of 0.02g acid, it is scattered in solution prepared by step 3
In；
5. the solution that above-mentioned steps 4 obtain is uniformly mixed under high velocity agitation；
6. prepare flexible heat conducting film using the mixture that membrane formation process obtains step 5 is filtered, and carry out 60 DEG C 12 hours
Then vacuum drying processing keeps carrying out pressurized treatments to film in one minute, obtains the stone of the present embodiment using the pressure of 4MPa
Black alkene film, appearance is referring to Fig. 1.
After tested, the graphene film that the present embodiment is prepared, 68 μm of thickness, density: 1.06g/cm3, laterally lead
Hot coefficient is 275W/ (mK), and longitudinal thermal coefficient is 3.1W/ (mK).It is tested using flexible test as shown in Figure 2, it can
62 times resistant to bending.Flexibility decreases after bending 62 times.
Embodiment 2
The heat conducting film of the present embodiment is prepared according to the following steps:
1. taking big partial size graphene powder (particle size distribution range (30~31 μm), medium grain size graphene powder (partial size point
(particle size distribution range (1~2 μm) carries out sour processing, the acid respectively for cloth range (21~23 μm), small particle graphene powder
Treatment conditions are as follows:
Big partial size graphene powder (30~31 μm): the graphene powder is immersed in sulfuric acid and nitric acid according to volume ratio
It in the acid solution of 2:1 mixing, is ultrasonically treated, the ultrasonic treatment condition are as follows: 400W handles 10h, obtains graphene dispersing solution；
In the graphene dispersing solution, the concentration of graphite olefin(e) acid powder is 3.5mg/ml；
Middle partial size graphene powder (21~23 μm): the graphene powder is immersed in sulfuric acid and nitric acid according to volume ratio
It in the acid solution of 3:1 mixing, is ultrasonically treated, the ultrasonic treatment condition are as follows: 400W handles 8h, obtains graphene dispersing solution；
In the graphene dispersing solution, the concentration of graphite olefin(e) acid powder is 3.5mg/ml；
Small particle graphene powder (1~2 μm): the graphene powder is immersed in sulfuric acid and nitric acid according to volume ratio 5:
It in 1 mixed acid solution, is ultrasonically treated, the ultrasonic treatment condition are as follows: 800W handles 3h, obtains graphene dispersing solution；It should
In graphene dispersing solution, the concentration of graphite olefin(e) acid powder is 3.5mg/ml；
2. taking processed big partial size graphene (30~31 μm) dispersion liquid of 0.04g acid, it is scattered in 1L deionized water, stirs
It mixes and is uniformly dispersed；
3. taking processed small particle graphene (1~2 μm) dispersion liquid of 0.01g acid, it is scattered in solution prepared by step 2
In；
4. taking processed medium grain size graphene (21~23 μm) dispersion liquid of 0.05g acid, it is scattered in prepared by step 3
In solution；
5. the solution that above-mentioned steps 4 obtain is uniformly mixed under high velocity agitation；
6. preparing flexible heat conducting film using the mixture that membrane formation process obtains step 5 is filtered, and carry out about 60 DEG C 12 hours
Vacuum drying processing, then using 4MPa pressure keep one minute to film carry out pressurized treatments, obtain the present embodiment
Graphene film, appearance with it is essentially identical shown in Fig. 1.
After tested, the graphene film that the present embodiment is prepared, 75 μm of thickness, density: 0.96g/cm3, laterally lead
Hot coefficient is 201W/ (mK), and longitudinal thermal coefficient is 2.5W/ (mK).Flexible test experiment display can be 59 times resistant to bending.It is curved
Flexibility decreases after folding 59 times.
Comparative example 1
The heat conducting film of this comparative example is prepared according to the following steps:
1. the sour treatment process of big partial size graphene powder, medium grain size graphene powder, small particle graphene powder is same
Embodiment 1；
2. taking processed big partial size graphene (35~37 μm) dispersion liquid of 0.01g acid, it is scattered in 1L deionized water, stirs
It mixes and is uniformly dispersed；
3. taking processed medium grain size graphene (18~20 μm) dispersion liquid of 0.02g acid, it is scattered in prepared by step 2
In solution；
4. taking processed small particle graphene (1~2 μm) dispersion liquid of 0.07g acid.It is scattered in solution prepared by step 3
In；
5. the solution that above-mentioned steps 4 obtain is uniformly mixed under high velocity agitation；
6. prepare flexible heat conducting film using the mixture that membrane formation process obtains step 5 is filtered, and carry out 60 DEG C 12 hours
Then vacuum drying processing keeps carrying out pressurized treatments to film in one minute, obtains the stone of this comparative example using the pressure of 4MPa
Black alkene film, appearance with it is essentially identical shown in Fig. 1.
After tested, the graphene film that this comparative example is prepared, 56 μm of thickness, density: 1.29g/cm3, flexibility survey
Examination experiment bending 56 times, lateral thermal coefficient is 89W/ (mK), and longitudinal thermal coefficient is 0.92W/ (mK).
Comparative example 2
The heat conducting film of the present embodiment is prepared according to the following steps:
1. 0.01g is taken to be scattered in 1L deionized water without the processed big partial size graphene (35~37 μm) of peracid, stir
It mixes and is uniformly dispersed；
2. 0.02g is taken to be scattered in prepared by step 1 without the processed medium grain size graphene of peracid (18~20 μm)
In solution；
3. 0.07g is taken to be scattered in solution prepared by step 2 without the processed small particle graphene of peracid (1~2 μm)
In；
4. the solution that above-mentioned steps 3 obtain is uniformly mixed under high velocity agitation；
5. prepare flexible heat conducting film using the mixture that membrane formation process obtains step 4 is filtered, and carry out 60 DEG C 12 hours
Then vacuum drying processing keeps carrying out pressurized treatments to film in one minute using the pressure of 4MPa.As a result, it has been found that, it is difficult to it is made
Flexible graphene film.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (8)
1. a kind of heat conducting film is uniformly mixed with by the graphene powder of different-grain diameter, lateral thermal coefficient is
50~400W/ (mK), longitudinal thermal coefficient is 0.7~4W/ (mK), with a thickness of 20~107 μm, 0.25~1.3g/ of density
cm3；
It also, include big partial size graphene powder, middle partial size graphene powder and granule in the raw material composition of the heat conducting film
Diameter graphene powder, the partial size of the big partial size graphene powder are 30 μm~40 μm, the grain of the middle partial size graphene powder
Diameter is 15 μm~25 μm, and the partial size of the small particle graphene powder is 1 μm~2 μm, the big partial size graphene powder, middle grain
The mass ratio of diameter graphene powder and small particle graphene powder is 2~4:5~6:1~2.
It include big partial size graphene powder, middle partial size graphene in raw material composition 2. heat conducting film according to claim 1
Powder and small particle graphene powder, big partial size graphene powder account for the 20%~40% of heat conducting film gross mass, middle partial size stone
Black alkene powder accounts for the 50%~60% of heat conducting film gross mass, small particle graphene powder account for heat conducting film gross mass 10%~
20%.
3. a kind of method for preparing heat conducting film of any of claims 1 or 2, this method comprises:
It disperses the processed graphene powder of acid of different-grain diameter in deionized water, obtains a variety of partial size graphene powder dispersions
Solution；The sour processing method of graphene powder includes: that graphene powder and acid are mixed, and in conjunction with ultrasonic treatment, obtains acid
Processed graphene powder；
A variety of partial size graphene powder dispersion solution are prepared into graphene film, obtain the heat conducting film.
4. according to the method described in claim 3, wherein, the acid is selected from one of sulfuric acid, nitric acid or a variety of.
5. according to the method described in claim 4, wherein, the acid is the mixed acid of sulfuric acid and nitric acid, wherein sulfuric acid and nitric acid
Volume ratio be 3~5:1~2.
6. according to the method described in claim 4, wherein, the ultrasonic treatment condition are as follows: 400W~800W handles 3~12h.
7. according to the method described in claim 3, wherein, the dosage of the deionized water and the weight ratio of big partial size graphene are
1:0.00001~.00005.
8. according to the method described in claim 3, wherein, being formed a film using suction filtration membrane formation process, vacuum drying method or roll-in will be described
A variety of partial size graphene powder dispersion solution are prepared into graphene film.
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| EP3875430A4 (en) * | 2018-10-31 | 2022-11-23 | Toray Industries, Inc. | Graphene dispersion, method for producing same, and electrode for secondary battery |
| CN113357571B (en) * | 2021-06-24 | 2022-11-01 | 四川依菲兰科技有限公司 | Graphite alkene heat dissipation lamps and lanterns for education |
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| JP2006165155A (en) * | 2004-12-06 | 2006-06-22 | Matsushita Electric Ind Co Ltd | Thermally conductive sheet |
| JP2006165153A (en) * | 2004-12-06 | 2006-06-22 | Matsushita Electric Ind Co Ltd | Thermally conductive sheet |
| JP5116082B2 (en) * | 2007-04-17 | 2013-01-09 | 住友精密工業株式会社 | High thermal conductivity composite material |
| JP2012104628A (en) * | 2010-11-10 | 2012-05-31 | Panasonic Corp | Heat conductive sheet |
| CN103146198A (en) * | 2013-03-12 | 2013-06-12 | 深圳市博恩实业有限公司 | Heat conducting composite material and heat conducting composite sheet prepared by applying same |
| CN103449423B (en) * | 2013-08-27 | 2016-03-16 | 常州第六元素材料科技股份有限公司 | A kind of Graphene heat conducting film and preparation method thereof |
| CN104817071B (en) * | 2015-03-17 | 2017-07-18 | 清华大学 | A kind of size classification method of grapheme material |
| CN105722375B (en) * | 2016-01-29 | 2018-03-06 | 白德旭 | A kind of graphene heat abstractor and preparation method thereof |
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