CN115849349A - Method for preparing high-thermal-conductivity graphene heat dissipation film - Google Patents
Method for preparing high-thermal-conductivity graphene heat dissipation film Download PDFInfo
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- CN115849349A CN115849349A CN202211617594.1A CN202211617594A CN115849349A CN 115849349 A CN115849349 A CN 115849349A CN 202211617594 A CN202211617594 A CN 202211617594A CN 115849349 A CN115849349 A CN 115849349A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 53
- 230000017525 heat dissipation Effects 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 32
- 238000012545 processing Methods 0.000 claims abstract description 15
- 239000011261 inert gas Substances 0.000 claims abstract description 13
- 230000008569 process Effects 0.000 claims abstract description 13
- 238000007540 photo-reduction reaction Methods 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 238000002360 preparation method Methods 0.000 claims abstract description 6
- 230000009467 reduction Effects 0.000 claims abstract description 6
- 238000006722 reduction reaction Methods 0.000 claims abstract description 6
- 238000002407 reforming Methods 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 229920001721 polyimide Polymers 0.000 description 6
- 238000005087 graphitization Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 229910021383 artificial graphite Inorganic materials 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000011946 reduction process Methods 0.000 description 3
- 238000003763 carbonization Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000004642 Polyimide Substances 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical group [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000003490 calendering Methods 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
Abstract
The invention discloses a method for preparing a high-thermal-conductivity graphene heat dissipation film, which is prepared by adopting a continuous microwave treatment and photo-reduction process and comprises the following specific steps: (1) Placing a graphene oxide film to be treated into a cavity of continuous microwave treatment equipment; (2) Vacuumizing the cavity, introducing inert gas, and adjusting the microwave power to 800-1000W to perform pretreatment reaction on the film at 1000-1500 ℃ to obtain a pretreated film; (3) And (3) putting the pretreated film into excimer laser processing equipment, and carrying out photoreduction and high-temperature structure reforming processing operations on the pretreated film by adopting laser waves to obtain the high-thermal-conductivity graphene heat dissipation film. The preparation method provided by the invention has the advantages that the high-efficiency and accurate reduction effects of the two processes are cooperated, the preparation efficiency of the high-thermal-conductivity graphene film can be greatly improved, the required energy consumption is reduced, and the large-scale production of the large-size graphene heat dissipation film is promoted and realized.
Description
Technical Field
The invention belongs to the technical field of heat dissipation films, relates to a method for preparing a high-thermal-conductivity graphene heat dissipation film, and more particularly relates to a method for preparing a high-thermal-conductivity graphene heat dissipation film by adopting a continuous microwave treatment and photo-reduction process.
Background
The heat dissipation film serving as a novel, rapid and effective heat dissipation material can meet the operation and development requirements of the fields of new-generation industry, electronic communication, aerospace and the like on integration of functionalization, miniaturization and lightness and thinness of micro-nano electronic components, and has important strategic significance on high-tech development.
The production of the existing artificial graphite heat dissipation film product generally adopts a polyimide film as a raw material, and sintering is carried out at 1400 ℃ to carbonize the polyimide film; after carbonization and cooling, transferring the product to a high-temperature graphitization furnace, vacuumizing the graphitization furnace, and sintering at 2900 ℃ to graphitize the product at high temperature; cooling and taking out after graphitization, and finally forming a graphite heat radiating fin product after calendering by using a calender.
The above process has the following defects: (1) The process is limited by the thickness and the size of the polyimide film material, so that the final thickness of the product is limited, when the required thickness of the product is more than 100 micrometers, an adhesive laminating and bonding form is usually adopted, the final heat conductivity coefficient is greatly reduced, and the heat dissipation performance is seriously influenced; (2) The polyimide film is difficult to modify or compound as a raw material, and the heat conductivity coefficient of the prepared graphite heat dissipation film is narrow in lifting space; (3) Carbonization and graphitization equipment usually adopts a high-frequency heating mode, the temperature rise energy consumption is extremely high, and large and medium-sized graphite heat dissipation film manufacturers need to be equipped with small power plants, so that the processing cost is increased sharply, and a certain burden is brought to local power grids.
Disclosure of Invention
The invention aims at the technical problems and provides a method for preparing a high-thermal-conductivity graphene heat dissipation film by adopting a continuous microwave treatment and photoinduced reduction process, which comprises the following steps: local ultrahigh-temperature structure reforming is carried out on the graphene oxide film through a microwave and laser two-way reduction process, the graphene oxide is self-assembled to form a film, and the preparation efficiency of the graphene heat dissipation film is effectively improved under the condition of low energy consumption. In addition, because the graphene oxide contains a large number of oxygen groups on the surface and the edge of the sheet layer, a nano phase can be introduced for material compounding to prepare the graphene composite heat dissipation film, the effective transfer of heat among graphene layers can be realized, and the interlayer heat conductivity of the graphene heat dissipation film has wide promotion space.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the invention provides a method for preparing a high-thermal-conductivity graphene heat dissipation film, which is characterized by adopting a continuous microwave treatment and photoinduced reduction process for preparation, and the method comprises the following specific steps:
step 1, placing a graphene oxide film to be treated into a cavity of continuous microwave treatment equipment;
step 2, introducing inert gas after vacuumizing the cavity, and adjusting the microwave power to 800-1000W to perform pretreatment reaction on the film at 1000-1500 ℃ to obtain a pretreated film;
and 3, putting the pretreated film prepared in the step 2 into excimer laser processing equipment, and carrying out photoinduced reduction and high-temperature structure reforming processing operation on the pretreated film by adopting laser waves to obtain the high-thermal-conductivity graphene heat dissipation film.
Preferably, the graphene oxide film has a thickness of 20 to 500 μm. Experimental results show that the method can be used for processing the graphene oxide film with the thickness of 20-500 mu m and obtaining the high-thermal-conductivity graphene heat dissipation film.
Preferably, in step 1, the continuous microwave treatment device is configured as a segmented continuous microwave heating segment. When the pretreatment reaction is carried out, the vacuum degree of the cavity of the continuous microwave treatment equipment is kept between 0.1 Pa and 10Pa, and the pretreatment reaction time is 5 min to 30min.
Preferably, in step 3, an excimer laser is used for carrying out the photoreduction reaction, the laser wavelength is 193nm or 248nm, the pulse repetition frequency is 200-1000 Hz, and the pulse energy is 5-10 mJ.
Verification experiment results show that the graphene heat dissipation film with the thickness ranging from 20 to 500 micrometers can be prepared by the method. The heat conductivity test result shows that the heat diffusion coefficient is basically between 800 and 950mm 2 S; compared with the artificial graphite heat dissipation film with the same thickness and using the polyimide film as the raw material, the heat conduction performance is greatly improved.
Therefore, in a second aspect of the present invention, a high thermal conductivity graphene heat dissipation film prepared by the above method is provided.
The invention has the following beneficial effects: the lattice of the graphene vibrates violently through interaction of microwave energy and carbon atoms in the graphene, so that the microwave energy is converted into heat energy, and the thermal reduction efficiency is realized; in addition, deep ultraviolet (wavelength is 193nm or 248 nm) photons can be strongly coupled with the graphene crystal structure, a non-thermal desorption effect is generated, and efficient and lossless photoinduced reduction is realized. By cooperating with the efficient and accurate reduction effects of the two processes, the preparation efficiency of the graphene film with high thermal conductivity can be greatly improved, the required energy consumption is reduced, and the large-scale production of the graphene heat dissipation film with large size is promoted and realized.
Detailed Description
The invention will now be described in detail with reference to specific embodiments, but it should be understood that the following detailed description is illustrative and not restrictive, and should not be taken to limit the scope of the invention.
Example 1
Placing a graphene oxide film with the thickness of 20 mu m into a cavity of continuous microwave treatment equipment; vacuumizing the cavity, introducing inert gas, and adjusting the microwave power to 800W to ensure that the film is pretreated at 1000 ℃ for reaction, thereby completing the pretreatment process and obtaining the pretreated film; vacuumizing the cavity and introducing inert gas N 2 And carrying out photoreduction deep processing on the pretreated film by adopting an excimer laser with the laser wavelength of 248nm, setting the pulse repetition frequency to be 200Hz and the pulse energy to be 10mJ, and then obtaining the high-thermal-conductivity graphene heat dissipation film.
Example 2
Placing a graphene oxide film with the thickness of 500 mu m into a cavity of continuous microwave treatment equipment; vacuumizing the cavity, introducing inert gas, and adjusting the microwave power to 800W to ensure that the film is pretreated at 1000 ℃ for reaction, thereby completing the pretreatment process and obtaining the pretreated film; vacuumizing the cavity and introducing inert gas N 2 And carrying out photoreduction deep processing on the pretreated film by adopting an excimer laser with the laser wavelength of 248nm, setting the pulse repetition frequency to be 1000Hz and the pulse energy to be 5mJ, and then obtaining the high-thermal-conductivity graphene heat dissipation film.
Example 3
Thickness of the steel sheetPutting a graphene oxide film with the thickness of 200 mu m into a cavity of continuous microwave treatment equipment; vacuumizing the cavity, introducing inert gas, and adjusting the microwave power to 1000W to ensure that the film is pretreated at 1500 ℃ for reaction, thereby completing the pretreatment process and obtaining the pretreated film; vacuumizing the cavity and introducing inert gas N 2 And carrying out photoreduction deep processing operation on the pretreated film by adopting an excimer laser with the laser wavelength of 193nm, setting the pulse repetition frequency to be 1000Hz and the pulse energy to be 10mJ, and then obtaining the high-thermal-conductivity graphene heat dissipation film.
Example 4
Placing a graphene oxide film with the thickness of 200 mu m into a cavity of continuous microwave treatment equipment; vacuumizing the cavity, introducing inert gas, and adjusting the microwave power to 1000W to ensure that the film is pretreated at 1500 ℃ for reaction, thereby completing the pretreatment process and obtaining the pretreated film; vacuumizing the cavity and introducing inert gas N 2 And carrying out photoreduction deep processing on the pretreated film by adopting an excimer laser with the laser wavelength of 193nm, setting the pulse repetition frequency to be 200Hz and the pulse energy to be 10mJ, and processing to obtain the high-thermal-conductivity graphene heat dissipation film.
Example 5
Placing a graphene oxide film with the thickness of 500 mu m into a cavity of continuous microwave treatment equipment; vacuumizing the cavity, introducing inert gas, and adjusting the microwave power to 1000W to ensure that the film is pretreated at 1500 ℃ for reaction, thereby completing the pretreatment process and obtaining the pretreated film; vacuumizing the cavity and introducing inert gas N 2 And carrying out photoreduction deep processing operation on the preprocessed film by adopting an excimer laser with the laser wavelength of 248nm, setting the pulse repetition frequency to be 1000Hz, and processing the preprocessed film by the pulse energy to be 10mJ to obtain the high-thermal-conductivity graphene heat dissipation film.
Results and analysis
The parameters of the above embodiments are combined, and the prepared graphene heat dissipation film is subjected to a heat conductivity test, and the results are shown in table 1 below:
TABLE 1 summary of the treatment conditions and results of examples 1 to 5
The result shows that the thermal diffusion coefficient of the graphene heat dissipation film prepared by the method is 780mm at least 2 The thermal diffusion coefficient of the artificial graphite film is far higher than that of the polyimide material (500-700 mm) 2 /s)。
By adopting the method disclosed by the invention, the pretreatment temperature can be effectively adjusted by controlling the continuous microwave treatment system, and the controllability of the microscopic laminated structure of the graphene film and the ordered arrangement of crystal grains and the high efficiency of the pretreatment process are realized; furthermore, the power, the light dose precision control and the scanning speed of the excimer laser system are adjusted to realize the large-size precision photoreduction and the high-temperature structure reformation of the film, so that the graphene heat dissipation film with high heat conduction efficiency is prepared.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are given by way of illustration of the principles of the present invention, and that various changes and modifications may be made without departing from the spirit and scope of the invention as defined by the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (6)
1. The method for preparing the high-thermal-conductivity graphene heat dissipation film is characterized by adopting a continuous microwave treatment and photo-reduction process for preparation, and comprises the following specific steps:
step 1, placing a graphene oxide film to be treated into a cavity of continuous microwave treatment equipment;
step 2, introducing inert gas after vacuumizing the cavity, and adjusting the microwave power to 800-1000W to perform pretreatment reaction on the film at 1000-1500 ℃ to obtain a pretreated film;
and 3, putting the pretreated film prepared in the step 2 into excimer laser processing equipment, and carrying out photoinduced reduction and high-temperature structure reforming processing operation on the pretreated film by adopting laser waves to obtain the high-thermal-conductivity graphene heat dissipation film.
2. The method for preparing the high thermal conductivity graphene heat dissipation film according to claim 1, wherein:
wherein the graphene oxide film has a thickness of 20 to 500 [ mu ] m.
3. The method for preparing the high thermal conductivity graphene heat dissipation film according to claim 1, wherein:
wherein, in the step 1, the continuous microwave treatment equipment is constructed into a segmented continuous microwave heating segment.
4. The method for preparing the high thermal conductivity graphene heat dissipation film according to claim 1, wherein:
in the step 2, the vacuum degree of the cavity of the continuous microwave treatment equipment is kept between 0.1 Pa and 10Pa, and the pretreatment reaction time is 5 min to 30min.
5. The method for preparing the high thermal conductivity graphene heat dissipation film according to claim 1, wherein:
in the step 3, an excimer laser is adopted for carrying out photoreduction reaction, the laser wavelength is 193nm or 248nm, the pulse repetition frequency is 200-1000 Hz, and the pulse energy is 5-10 mJ.
6. The high-thermal-conductivity graphene heat dissipation film prepared by the method of any one of claims 1 to 5.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103224227A (en) * | 2012-01-30 | 2013-07-31 | 深圳市润麒麟科技发展有限公司 | Microwave preparation method of graphene sheet and carbon nanotube/graphene sheet composite material |
| CN106517174A (en) * | 2016-11-25 | 2017-03-22 | 西安交通大学 | Quick heating method for graphene and deep processing method based on same |
| WO2019220903A1 (en) * | 2018-05-16 | 2019-11-21 | 国立研究開発法人産業技術総合研究所 | Graphite thin film, graphite thin film laminate, and production methods for graphite thin film and graphite thin film laminate |
| 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 |
| CN111515524A (en) * | 2019-09-12 | 2020-08-11 | 中国科学院长春光学精密机械与物理研究所 | Laser processing system and graphene oxide microstructuring and reducing treatment method |
| CN113096973A (en) * | 2021-04-12 | 2021-07-09 | 王晓京 | Method for preparing porous graphene membrane, porous graphene membrane and electrode |
-
2022
- 2022-12-15 CN CN202211617594.1A patent/CN115849349A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103224227A (en) * | 2012-01-30 | 2013-07-31 | 深圳市润麒麟科技发展有限公司 | Microwave preparation method of graphene sheet and carbon nanotube/graphene sheet composite material |
| CN106517174A (en) * | 2016-11-25 | 2017-03-22 | 西安交通大学 | Quick heating method for graphene and deep processing method based on same |
| WO2019220903A1 (en) * | 2018-05-16 | 2019-11-21 | 国立研究開発法人産業技術総合研究所 | Graphite thin film, graphite thin film laminate, and production methods for graphite thin film and graphite thin film laminate |
| CN111515524A (en) * | 2019-09-12 | 2020-08-11 | 中国科学院长春光学精密机械与物理研究所 | Laser processing system and graphene oxide microstructuring and reducing treatment method |
| 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 |
| CN113096973A (en) * | 2021-04-12 | 2021-07-09 | 王晓京 | Method for preparing porous graphene membrane, porous graphene membrane and electrode |
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