CN115231565A - Fluorinated graphene heat-conducting film and preparation method thereof - Google Patents
Fluorinated graphene heat-conducting film and preparation method thereof Download PDFInfo
- Publication number
- CN115231565A CN115231565A CN202210751384.5A CN202210751384A CN115231565A CN 115231565 A CN115231565 A CN 115231565A CN 202210751384 A CN202210751384 A CN 202210751384A CN 115231565 A CN115231565 A CN 115231565A
- Authority
- CN
- China
- Prior art keywords
- fluorinated graphene
- graphene
- heat
- fluorinated
- film
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 143
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000006185 dispersion Substances 0.000 claims abstract description 28
- 239000007788 liquid Substances 0.000 claims abstract description 25
- 238000003825 pressing Methods 0.000 claims abstract description 15
- 239000003960 organic solvent Substances 0.000 claims abstract description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 22
- 229910021389 graphene Inorganic materials 0.000 claims description 21
- 238000005485 electric heating Methods 0.000 claims description 18
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 14
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 13
- 229910052731 fluorine Inorganic materials 0.000 claims description 13
- 239000011737 fluorine Substances 0.000 claims description 13
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 12
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims description 9
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- 239000012528 membrane Substances 0.000 abstract description 9
- 239000002994 raw material Substances 0.000 abstract description 9
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000010408 film Substances 0.000 description 63
- 229910001220 stainless steel Inorganic materials 0.000 description 9
- 239000010935 stainless steel Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 230000017525 heat dissipation Effects 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000000465 moulding Methods 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- 239000004372 Polyvinyl alcohol Substances 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 description 4
- 238000009210 therapy by ultrasound Methods 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 2
- 229910021383 artificial graphite Inorganic materials 0.000 description 2
- 229920002301 cellulose acetate Polymers 0.000 description 2
- 230000006837 decompression Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 239000002135 nanosheet Substances 0.000 description 2
- 229920001721 polyimide Polymers 0.000 description 2
- 238000011085 pressure filtration Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000003490 calendering Methods 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 238000005087 graphitization Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
Images
Classifications
-
- 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
- C01B32/194—After-treatment
-
- 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
- C01B32/10—Carbon fluorides, e.g. [CF]nor [C2F]n
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K7/00—Constructional details common to different types of electric apparatus
- H05K7/20—Modifications to facilitate cooling, ventilating, or heating
- H05K7/2039—Modifications to facilitate cooling, ventilating, or heating characterised by the heat transfer by conduction from the heat generating element to a dissipating body
-
- 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
- C01B2204/04—Specific amount of layers or specific thickness
-
- 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
- C01B2204/32—Size or surface area
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Geology (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Materials Engineering (AREA)
- Nanotechnology (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention relates to a preparation method of a fluorinated graphene heat-conducting film, which comprises the following steps: dispersing fluorinated graphene in an organic solvent to prepare a fluorinated graphene dispersion liquid; placing the fluorinated graphene dispersion liquid in a magnetic field, carrying out orientation treatment in the horizontal direction, and removing the organic solvent to prepare a fluffy fluorinated graphene film; and clamping the fluffy fluorinated graphene film between templates with smooth mirror surfaces, and performing vacuum pressing to prepare the fluorinated graphene heat-conducting film. According to the preparation method of the fluorinated graphene heat-conducting membrane, fluorinated graphene is used as a raw material, and is matched with the action of an organic solvent and a magnetic field, so that the obtained fluorinated graphene is in oriented arrangement, and the prepared fluorinated graphene heat-conducting membrane has a high heat conductivity coefficient. In addition, the preparation method of the fluorinated graphene heat-conducting film is high in production efficiency and feasible in large-scale production.
Description
Technical Field
The invention relates to the technical field of functional thin film materials, in particular to a fluorinated graphene heat-conducting film and a preparation method thereof.
Background
With the development of mobile phones towards high performance and miniaturization, the heat productivity of chips is larger and is limited by narrow space, and heat is easy to gather to form hot spots, so that the chips cannot normally work, and therefore materials with higher transverse heat conductivity need to be adopted for carrying out uniform heating. For 4G mobile phones, the material is usually an artificial graphite heat dissipation film, which is prepared from a polyimide film as a raw material through carbonization, graphitization and calendaring processes. The artificial graphite heat dissipation film is limited by polyimide film raw materials, has limited thickness (less than 100 micrometers), and cannot cope with higher heat productivity of a 5G mobile phone chip. The graphene heat dissipation film can break through the limitation of thickness and meet the requirement of even heating of a 5G mobile phone chip, so that the graphene heat dissipation film is widely applied.
However, since the graphene material has excellent electrical conductivity, the graphene thermal conductive film has poor electrical insulation, which limits the application of the graphene thermal conductive film in more application scenarios. Some technologies involve introducing insulating nanomaterials such as boron nitride into a graphene heat-conducting film, and improving the insulating property by blocking the formation of a graphene conductive network, but the mechanical property and the heat-conducting property of the graphene heat-conducting film are obviously reduced.
The fluorinated graphene is a graphene derivative, and compared with graphene, the fluorinated graphene has better insulativity and stability, is more suitable for serving as a heat conduction material, and has a wider application scene. However, the conventional fluorinated graphene heat-conducting film has the defect of low heat conductivity coefficient. If the technology relates to the technical field of preparing the fluorinated graphene heat-conducting film by using fluorinated graphene as a raw material and adopting a reduced-pressure suction filtration method, the preparation method has no feasibility of large-scale production, and the prepared fluorinated graphene heat-conducting film has a low heat conductivity coefficient and is difficult to meet the heat dissipation requirement of electronic equipment.
Disclosure of Invention
Based on the above, one of the purposes of the present invention is to provide a preparation method of a fluorinated graphene thermal conductive film with high thermal conductivity.
The preparation method of the fluorinated graphene heat-conducting film comprises the following steps:
dispersing fluorinated graphene in an organic solvent to prepare a fluorinated graphene dispersion liquid;
placing the fluorinated graphene dispersion liquid in a magnetic field, carrying out orientation treatment in the horizontal direction, and removing the organic solvent to prepare a fluffy fluorinated graphene film;
and clamping the fluorinated fluffy graphene film between templates with smooth mirror surfaces for vacuum pressing to prepare the fluorinated graphene heat-conducting film.
In one embodiment, the fluorine content of the fluorinated graphene is 45wt% to 65wt%.
In one embodiment, the fluorinated graphene has a lamellar structure with 5-20 layers; and/or the flake diameter of the fluorinated graphene is 5-20 microns.
In one embodiment, the organic solvent comprises one or more of ethanol, diethyl ether, isopropanol, and acetone.
In one embodiment, the solid content of the fluorinated graphene dispersion liquid is 0.5wt% to 2wt%.
In one embodiment, the magnetic field has a strength of 5 tesla to 20 tesla.
In one embodiment, the vacuum pressing pressure is 20 tons to 1000 tons for 2 minutes to 30 minutes.
In one embodiment, the magnetic field is applied by a magnetic field orienting device, and the magnetic field orienting device comprises a power supply (1), two coils (2) and (3) which are connected with the power supply and distributed at intervals, an electric heating plate (4) positioned between the two coils (2) and (3), and a mold (5) placed on the electric heating plate (4); the two coils (2) and (3) have the same radius and are arranged oppositely; the central connecting line of the two coils (2) and (3) is superposed with the central axis of the mould (5);
and during pressing, placing the fluorinated fluffy graphene film and the template into a forming groove of the mold (5).
The invention further provides a fluorinated graphene heat-conducting film, which is prepared by adopting the preparation method of the fluorinated graphene heat-conducting film.
In one embodiment, the thickness of the fluorinated graphene heat-conducting film is 60-300 microns; and/or
The thermal conductivity of the fluorinated graphene heat-conducting film is more than or equal to 250W/m.degree.
Compared with the prior art, the invention has the following advantages and beneficial effects:
according to the preparation method of the fluorinated graphene heat-conducting film, fluorinated graphene is used as a raw material, the fluorinated graphene is arranged in an oriented manner under the action of a magnetic field, and the solvent is heated and evaporated, so that the prepared fluorinated graphene heat-conducting film has a high heat conductivity coefficient, and the method is high in production efficiency and feasible in large-scale production.
Drawings
FIG. 1 is a schematic view of a magnetic field aligning apparatus.
Reference numerals:
1: a power source; 2 and 3: a coil; 4: an electric hot plate; 5: and (5) molding.
Detailed Description
In order that the invention may be more fully understood, reference will now be made to the following description. The following is a description of preferred embodiments of the invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
Reference herein to numerical intervals is deemed to be continuous, unless otherwise stated, and includes both the minimum and maximum values of that range, as well as each value between such minimum and maximum values. Further, when a range refers to an integer, each integer between the minimum and maximum values of the range is included. Further, when multiple range-describing features or characteristics are provided, the ranges may be combined. In other words, unless otherwise indicated, all ranges disclosed herein are to be understood to encompass any and all subranges subsumed therein.
The temperature parameter herein is not particularly limited, and is allowed to be either constant temperature treatment or treatment within a certain temperature range. The constant temperature process allows the temperature to fluctuate within the accuracy of the instrument control.
An embodiment provides a preparation method of a fluorinated graphene heat-conducting film, which includes the following steps:
s110: dispersing fluorinated graphene in an organic solvent to prepare a fluorinated graphene dispersion liquid.
In one example, the fluorinated graphene has a fluorine content of 45wt% to 65wt%. In some specific examples, the fluorinated graphene described above may have a fluorine content of 45wt%, 46wt%, 47wt%, 48wt%, 50wt%, 52wt%, 54wt%, 56wt%, 58wt%, 60wt%, 62wt%, 63wt%, 64wt%, or 65wt%.
In one example, the fluorinated graphene has a lamellar structure with 5 to 20 layers. In some specific examples, the number of layers of the fluorinated graphene may be 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, or 20, and preferably, the number of layers of the fluorinated graphene is between 7 and 15, and more preferably between 9 and 11.
In one example, the sheet diameter of the fluorinated graphene is 5 to 20 micrometers, and specifically, the sheet diameter of the fluorinated graphene may be 5 to 6 micrometers, 7 to 8 micrometers, 9 to 10 micrometers, 11 to 12 micrometers, 13 to 14 micrometers, 15 to 16 micrometers, 17 to 18 micrometers, 19 to 20 micrometers.
In one example, the organic solvent includes one or more of ethanol, diethyl ether, isopropanol, and acetone.
In one example, the solid content of the fluorinated graphene dispersion is 0.5wt% to 2wt%, for example, the solid content of the fluorinated graphene dispersion may be 0.5wt%, 0.6wt%, 0.7wt%, 0.8wt%, 0.9wt%, 1wt%, 1.1wt%, 1.2wt%, 1.3wt%, 1.4wt%, 1.5wt%, 1.6wt%, 1.7wt%, 1.8wt%, 1.9wt%, or 2wt%, and preferably, the solid content of the fluorinated graphene dispersion is between 1wt% and 1.5 wt%.
S120: placing the fluorinated graphene dispersion liquid in a magnetic field, carrying out orientation treatment in the horizontal direction, and removing the organic solvent to prepare a fluffy fluorinated graphene film;
in one example, the strength of the magnetic field is 5 tesla to 20 tesla, and specifically, the strength of the magnetic field may be 5 tesla, 6 tesla, 7 tesla, 8 tesla, 9 tesla, 10 tesla, 11 tesla, 12 tesla, 13 tesla, 14 tesla, 15 tesla, 16 tesla, 17 tesla, 18 tesla, 19 tesla, or 20 tesla, and preferably, the strength of the magnetic field is between 10 tesla to 15 tesla.
In one example, the vacuum pressing is performed at a pressure of 20 tons to 1000 tons for 2 minutes to 30 minutes. Specifically, the pressure of the above vacuum pressing may be 20 tons, 50 tons, 100 tons, 150 tons, 200 tons, 300 tons, 400 tons, 500 tons, 600 tons, 700 tons, 800 tons, 900 tons, or 1000 tons, and the time may be 30 minutes, 25 minutes, 20 minutes, 15 minutes, 10 minutes, 5 minutes, or 2 minutes.
In one example, the magnetic field is applied by a magnetic field orienting device, which comprises a power supply 1, two coils 2 and 3 connected with the power supply and distributed at intervals, an electric heating plate 4 positioned between the two coils 2 and 3, and a mold 5 placed on the electric heating plate 4; the two coils 2 and 3 have the same radius and are arranged oppositely; the central connecting line of the two coils 2 and 3 is superposed with the central axis of the mould 5.
In one example, the two sides of the electric heating plate 4 are provided with fixing brackets, and the fixing brackets are provided with fixing grooves which are electrically connected with a power supply.
In one example, when the two coils 2 and 3 are energized, a magnetic field is formed along the direction of the central line of the two coils, and the magnetic field passes through a die 5 which is arranged on an electric heating plate 4 and is provided with fluorinated graphene dispersion liquid.
In one example, under the action of a magnetic field, the fluorinated graphene is arranged along the direction of the magnetic field, i.e. in the horizontal direction.
In one example, when the electric heating plate is electrified and heated, and the solvent is volatilized, the fluffy fluorinated graphene film in the horizontal orientation arrangement is obtained. The fluffy appearance is caused by the existence of voids left after more solvent is volatilized.
In one example, the mold 5 is made of stainless steel and has a molding groove, and the surface of the molding groove is plated with fluorine.
In one example, the depth of the molding groove is set according to a target thickness of the prepared fluorinated graphene thermal conductive film.
In one example, the forming groove has a depth of 1.5 cm to 10 cm.
S130: and clamping the fluffy fluorinated graphene film between templates with smooth mirror surfaces, and performing vacuum pressing to prepare the fluorinated graphene heat-conducting film.
In one example, the fluffy graphene fluoride film and the template are placed in a forming groove of the mold 5 during pressing.
In one example, the fluffy fluorinated graphene membrane has a density of 1.9 g/cc to 2.2 g/cc after vacuum pressing. Due to the fact that the horizontal orientation degree and the density of the fluorinated graphene are high, the prepared fluorinated graphene heat-conducting film has high heat conductivity in the horizontal direction.
In one example, the preparation method of the fluorinated graphene heat conduction film comprises the following steps:
1. dispersing the fluorinated graphene with the lamellar structure, the number of which is between 5 and 20, in one or more organic solvents of ethanol, diethyl ether, isopropanol and acetone, and ultrasonically treating to obtain a fluorinated graphene dispersion liquid with the solid content of 0.5 to 2 weight percent;
the fluorine content of the fluorinated graphene is 45wt% -65 wt%.
The sheet diameter of the fluorinated graphene is 5-20 micrometers.
2. And transferring the fluorinated graphene dispersion liquid into a magnetic field orientation device, carrying out orientation treatment in the horizontal direction, carrying out orientation arrangement on the fluorinated graphene along the horizontal direction under the action of a magnetic field with the strength of 5-20 Tesla, and heating to completely volatilize the solvent to obtain the fluffy fluorinated graphene film.
The magnetic field is applied by a magnetic field orienting device shown in fig. 1, which comprises a power supply 1, two coils 2 and 3 connected with the power supply and distributed at intervals, an electric heating plate 4 positioned between the two coils 2 and 3, and a mold 5 placed on the electric heating plate 4; the two coils 2 and 3 have the same radius and are arranged oppositely; the central connecting line of the two coils 2 and 3 is superposed with the central axis of the mould 5. After the two coils 2 and 3 are electrified, a magnetic field is formed along the central connection line direction of the two coils, and the magnetic field passes through a die 5 which is positioned on an electric hot plate 4 and is provided with fluorinated graphene dispersion liquid. The two sides of the electric heating plate 4 are provided with fixing supports, fixing grooves are arranged on the fixing supports, and the fixing grooves are electrically connected with a power supply. The die 5 is made of stainless steel and is provided with a forming groove, and the surface of the forming groove is plated with fluorine. The depth of the forming groove is set according to the target thickness of the prepared fluorinated graphene heat-conducting film, and is specifically 1.5-10 cm.
3. And (3) clamping the fluffy fluorinated graphene film between stainless steel sheets with smooth mirror surfaces, stacking the fluffy fluorinated graphene film in a mould, and performing vacuum pressing for 2-30 minutes under the pressure of 20-1000 tons through a vacuum flat press to obtain the fluorinated graphene heat-conducting film.
An embodiment also provides a fluorinated graphene heat-conducting film prepared by the preparation method of the fluorinated graphene heat-conducting film.
In one example, the thickness of the fluorinated graphene thermal conductive film is 60-300 micrometers. In some specific examples, the thickness of the fluorinated graphene thermal conductive film may be 60 micrometers, 80 micrometers, 100 micrometers, 120 micrometers, 150 micrometers, 180 micrometers, 200 micrometers, 220 micrometers, 250 micrometers, 280 micrometers, or 300 micrometers.
In one example, the thermal conductivity of the fluorinated graphene thermal conductive film is more than or equal to 250W/m.degree. In some specific examples, the thermal conductivity of the fluorinated graphene thermal conductive film may be 250 w/m.degree, 280 w/m.degree, 300 w/m.degree, 350 w/Midu, 400 w/m.degree, 450 w/m.degree, or 500 w/m.degree.
In one example, the density of the fluorinated graphene thermal conductive film is 1.9 to 2.2 g/cc. In some specific examples, the density of the fluorinated graphene thermal conductive film may be 1.9 g/cc, 2.0 g/cc, 2.1 g/cc, or 2.2 g/cc.
According to the preparation method of the fluorinated graphene heat-conducting film, fluorinated graphene is used as a raw material, the fluorinated graphene is arranged in an oriented manner under the action of a magnetic field, and the solvent is heated and evaporated.
The following are specific examples.
Example 1: preparation of fluorinated graphene heat-conducting film
The preparation method of the fluorinated graphene heat-conducting film comprises the following steps:
1. dispersing fluorinated graphene with the fluorine content of 45wt%, 20 layers and the sheet diameter of 20 micrometers in ethanol, and performing ultrasonic treatment to obtain a fluorinated graphene dispersion liquid with the solid content of 2wt%.
2. And transferring the fluorinated graphene dispersion liquid into a magnetic field orientation device, carrying out orientation treatment in the horizontal direction, enabling the fluorinated graphene to be arranged in an oriented manner along the horizontal direction under the action of a magnetic field with the strength of 5 Tesla, and heating to completely volatilize ethanol to obtain the fluffy fluorinated graphene film.
The magnetic field is applied by a magnetic field orientation device shown in fig. 1, which comprises a power supply 1, two coils 2 and 3 connected with the power supply and distributed at intervals, an electric heating plate 4 positioned between the two coils 2 and 3, and a mold 5 placed on the electric heating plate 4; the two coils 2 and 3 have the same radius and are arranged oppositely; the central connecting line of the two coils 2 and 3 is superposed with the central axis of the mould 5. After the two coils 2 and 3 are electrified, a magnetic field is formed along the central connection line direction of the two coils, and the magnetic field passes through a die 5 which is positioned on an electric hot plate 4 and is provided with fluorinated graphene dispersion liquid. The two sides of the electric heating plate 4 are provided with fixing supports, fixing grooves are arranged on the fixing supports, and the fixing grooves are electrically connected with a power supply. The die 5 is made of stainless steel and is provided with a forming groove, and the surface of the forming groove is plated with fluorine. The depth of the molding groove was 1.5 cm.
3. Placing a smooth-mirror-surface stainless steel sheet between every two fluffy fluorinated graphene films, stacking the stainless steel sheets in a grinding tool, and performing vacuum pressing for 10 minutes under the pressure of 50 tons through a vacuum flat press to obtain the fluorinated graphene heat-conducting film.
Example 2: preparation of fluorinated graphene heat-conducting film
The preparation method of the fluorinated graphene heat-conducting film comprises the following steps:
1. dispersing fluorinated graphene with 65wt% of fluorine element, 5 layers and 5-micron sheet diameter in acetone, and performing ultrasonic treatment to obtain a fluorinated graphene dispersion liquid with 0.5wt% of solid content.
2. And transferring the fluorinated graphene dispersion liquid into a magnetic field orientation device, carrying out orientation treatment in the horizontal direction, enabling the fluorinated graphene to be arranged in an oriented manner along the horizontal direction under the action of a magnetic field with the strength of 20 Tesla, and heating to completely volatilize acetone to obtain the fluffy fluorinated graphene film.
The magnetic field is applied by a magnetic field orientation device shown in fig. 1, which comprises a power supply 1, two coils 2 and 3 connected with the power supply and distributed at intervals, an electric heating plate 4 positioned between the two coils 2 and 3, and a mold 5 placed on the electric heating plate 4; the two coils 2 and 3 have the same radius and are arranged oppositely; the central connecting line of the two coils 2 and 3 is superposed with the central axis of the mould 5. After the two coils 2 and 3 are electrified, a magnetic field is formed along the central connection line direction of the two coils, and the magnetic field passes through a die 5 which is positioned on an electric hot plate 4 and is provided with fluorinated graphene dispersion liquid. The two sides of the electric heating plate 4 are provided with fixing supports, fixing grooves are arranged on the fixing supports, and the fixing grooves are electrically connected with a power supply. The die 5 is made of stainless steel and is provided with a forming groove, and the surface of the forming groove is plated with fluorine. The depth of the forming groove is 10 cm.
3. Placing a smooth-mirror-surface stainless steel sheet between every two fluffy fluorinated graphene films, stacking the stainless steel sheets in a grinding tool, and performing vacuum pressing for 30 minutes under the pressure of 1000 tons through a vacuum flat press to obtain the fluorinated graphene heat-conducting film.
Comparative example 1: preparation of fluorinated graphene heat-conducting film
Comparative example 1 differs from example 1 in that: the fluorinated graphene heat-conducting membrane is prepared by taking fluorinated graphene and polyvinyl alcohol as raw materials and adopting a reduced pressure filtration method.
The preparation method comprises the following steps:
1. 40 mg of fluorinated graphene with the fluorine content of 45wt%, 20 layers and the sheet diameter of 20 microns is weighed and dispersed in 200 ml of water, 0.05 ml of 6wt% polyvinyl alcohol (molecular weight of 145 kg/mol) aqueous solution is added, and ultrasonic treatment is carried out for 30 minutes to obtain uniformly dispersed fluorinated graphene dispersion liquid.
2. And pouring the fluorinated graphene dispersion liquid into a decompression filtering device of a mixed cellulose acetate filtering membrane to enable fluorinated graphene nanosheets to be uniformly deposited layer by layer to obtain the fluorinated graphene heat-conducting membrane.
Comparative example 2: preparation of fluorinated graphene heat-conducting film
Comparative example 2 differs from example 2 in that: the fluorinated graphene heat-conducting membrane is prepared by taking fluorinated graphene and polyvinyl alcohol as raw materials and adopting a reduced pressure filtration method.
The preparation method comprises the following steps:
1. 200 mg of fluorinated graphene with 65wt% of fluorine content, 5 layers and 5-micron sheet diameter is weighed and dispersed in 200 ml of water, 0.05 ml of 6wt% polyvinyl alcohol (molecular weight of 145 kg/mol) aqueous solution is added, and ultrasonic treatment is carried out for 30 minutes to obtain uniformly dispersed fluorinated graphene dispersion liquid.
2. And pouring the fluorinated graphene dispersion liquid into a decompression filtering device of a mixed cellulose acetate filtering membrane to enable fluorinated graphene nanosheets to be uniformly deposited layer by layer to obtain the fluorinated graphene heat-conducting membrane.
The fluorinated graphene thermal conductive films prepared in examples 1 to 2 and comparative examples 1 to 2 were subjected to density, thickness and thermal conductivity tests, and the test results are shown in table 1 below. Wherein, the test standard of the thermal conductivity test is ASTM E1461.
TABLE 1 thickness and thermal conductivity test results
As can be seen from table 1 above, the thermal conductivity of examples 1 to 2 is significantly higher than that of comparative examples 1 to 2. Specifically, it can be seen from the data of example 1 and comparative example 1, and the data of example 2 and comparative example 2 that the fluorinated graphene is used as a raw material, and the organic solvent and the magnetic field are matched to obtain a fluorinated graphene dispersion liquid in an oriented arrangement, and the prepared fluorinated graphene thermal conductive film has a high thermal conductivity coefficient. In addition, the preparation method of the fluorinated graphene heat-conducting film is high in production efficiency and feasible in large-scale production.
All possible combinations of the technical features of the above embodiments may not be described for the sake of brevity, but should be considered as within the scope of the present disclosure as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. A preparation method of a fluorinated graphene heat conduction film is characterized by comprising the following steps:
dispersing fluorinated graphene in an organic solvent to prepare a fluorinated graphene dispersion liquid;
placing the fluorinated graphene dispersion liquid in a magnetic field, carrying out orientation treatment in the horizontal direction, and removing the organic solvent to prepare a fluffy fluorinated graphene film;
and clamping the fluorinated fluffy graphene film between templates with smooth mirror surfaces for vacuum pressing to prepare the fluorinated graphene heat-conducting film.
2. The method of preparing a graphene fluoride heat conduction film according to claim 1, wherein the content of fluorine element in the graphene fluoride is 45wt% to 65wt%.
3. The method for preparing a graphene fluoride heat-conducting film according to claim 2, wherein the graphene fluoride has a lamellar structure with 5 to 20 layers; and/or the flake diameter of the fluorinated graphene is 5-20 microns.
4. The method according to claim 1, wherein the organic solvent comprises one or more of ethanol, diethyl ether, isopropanol, and acetone.
5. The method for preparing a graphene fluoride heat-conducting film according to claim 1, wherein the solid content of the graphene fluoride dispersion liquid is 0.5wt% to 2wt%.
6. The method of claim 1, wherein the magnetic field has a strength of 5 tesla to 20 tesla.
7. The method for preparing the fluorinated graphene thermal conductive film according to claim 1, wherein the pressure of the vacuum pressing is 20 tons to 1000 tons, and the time is 2 minutes to 30 minutes.
8. The method for preparing a fluorinated graphene thermal conductive film according to any one of claims 1 to 7, wherein the magnetic field is applied by a magnetic field orienting device, the magnetic field orienting device comprises a power supply (1), two coils (2) and (3) connected with the power supply and distributed at intervals, an electric heating plate (4) positioned between the two coils (2) and (3), and a mold (5) placed on the electric heating plate (4); the two coils (2) and (3) have the same radius and are arranged oppositely; the central connecting line of the two coils (2) and (3) is superposed with the central axis of the mould (5);
and during pressing, placing the fluffy fluorinated graphene film and the template into a forming groove of the mold (5).
9. A fluorinated graphene heat-conducting film, which is prepared by the method for preparing a fluorinated graphene heat-conducting film according to any one of claims 1 to 8.
10. The graphene fluoride thermally conductive film of claim 9, wherein the graphene fluoride thermally conductive film has a thickness of 60 to 300 μm; and/or
The density of the fluorinated graphene heat-conducting film is 1.9-2.2 g/cc; and/or
The thermal conductivity of the fluorinated graphene heat-conducting film is more than or equal to 250W/m.degree.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202210751384.5A CN115231565A (en) | 2022-06-29 | 2022-06-29 | Fluorinated graphene heat-conducting film and preparation method thereof |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202210751384.5A CN115231565A (en) | 2022-06-29 | 2022-06-29 | Fluorinated graphene heat-conducting film and preparation method thereof |
Publications (1)
Publication Number | Publication Date |
---|---|
CN115231565A true CN115231565A (en) | 2022-10-25 |
Family
ID=83671876
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202210751384.5A Pending CN115231565A (en) | 2022-06-29 | 2022-06-29 | Fluorinated graphene heat-conducting film and preparation method thereof |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN115231565A (en) |
Citations (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101474897A (en) * | 2009-01-16 | 2009-07-08 | 南开大学 | Grapheme-organic material layered assembling film and preparation method thereof |
CN206262795U (en) * | 2016-12-02 | 2017-06-20 | 深圳八六三计划材料表面技术研发中心 | A kind of Uniform Electromagnetic Field apparatus for coating for Graphene oriented alignment in coating |
CN109912912A (en) * | 2019-03-06 | 2019-06-21 | 东华大学 | A kind of flexible, electrical isolation fluorinated graphene heat conduction composite membrane and its preparation and application |
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 |
CN112852077A (en) * | 2021-01-13 | 2021-05-28 | 业成科技(成都)有限公司 | Piezoelectric composite material film, manufacturing method thereof and piezoelectric loudspeaker |
CN113321444A (en) * | 2021-07-08 | 2021-08-31 | 南方科技大学 | Fluorinated graphene heat-conducting film and preparation method and application thereof |
CN113416420A (en) * | 2021-06-25 | 2021-09-21 | 厦门大学 | Preparation method of high-orientation-arrangement graphene sheet thermal interface material |
CN114436251A (en) * | 2022-03-24 | 2022-05-06 | 四川大学 | Preparation method and application of fluorinated graphene with high thermal stability, high insulation and high thermal conductivity |
CN114956066A (en) * | 2022-06-30 | 2022-08-30 | 安徽宇航派蒙健康科技股份有限公司 | Graphene composite heat-conducting film and preparation method thereof |
-
2022
- 2022-06-29 CN CN202210751384.5A patent/CN115231565A/en active Pending
Patent Citations (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101474897A (en) * | 2009-01-16 | 2009-07-08 | 南开大学 | Grapheme-organic material layered assembling film and preparation method thereof |
CN206262795U (en) * | 2016-12-02 | 2017-06-20 | 深圳八六三计划材料表面技术研发中心 | A kind of Uniform Electromagnetic Field apparatus for coating for Graphene oriented alignment in coating |
CN109912912A (en) * | 2019-03-06 | 2019-06-21 | 东华大学 | A kind of flexible, electrical isolation fluorinated graphene heat conduction composite membrane and its preparation and application |
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 |
CN112852077A (en) * | 2021-01-13 | 2021-05-28 | 业成科技(成都)有限公司 | Piezoelectric composite material film, manufacturing method thereof and piezoelectric loudspeaker |
CN113416420A (en) * | 2021-06-25 | 2021-09-21 | 厦门大学 | Preparation method of high-orientation-arrangement graphene sheet thermal interface material |
CN113321444A (en) * | 2021-07-08 | 2021-08-31 | 南方科技大学 | Fluorinated graphene heat-conducting film and preparation method and application thereof |
CN114436251A (en) * | 2022-03-24 | 2022-05-06 | 四川大学 | Preparation method and application of fluorinated graphene with high thermal stability, high insulation and high thermal conductivity |
CN114956066A (en) * | 2022-06-30 | 2022-08-30 | 安徽宇航派蒙健康科技股份有限公司 | Graphene composite heat-conducting film and preparation method thereof |
Non-Patent Citations (2)
Title |
---|
姚方元等: "《石墨烯与轨道交通》", 哈尔滨工业大学出版社, pages: 307 * |
闫云飞;高伟;杨仲卿;张力;冉景煜;: "煤基新材料――煤基石墨烯的制备及石墨烯在导热领域应用研究进展", 煤炭学报, no. 01, pages 449 - 460 * |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
JP5541401B2 (en) | Manufacturing method of heat conductive sheet | |
CN107043538B (en) | Thermal conductive sheet | |
CN114573358B (en) | Graphene heat conducting film, graphene heat conducting sheet, preparation method and mold | |
CN113150544A (en) | Oriented boron nitride @ polydopamine @ silver hybrid nanosheet flexible thermal interface material and preparation method thereof | |
JP2007172956A (en) | Separator member for polymer electrolyte fuel cell and its manufacturing method | |
CN113321208B (en) | Preparation method of high-compactness graphene film | |
CN110451964A (en) | A kind of preparation method of high orientation Graphite block material | |
CN113939167A (en) | Graphite film with high heat conductivity in thickness direction and preparation method thereof | |
CN108219757B (en) | Preparation method of high-in-plane heat-conducting insulating composite film | |
CN115231565A (en) | Fluorinated graphene heat-conducting film and preparation method thereof | |
CN114873587A (en) | Graphene heat-conducting film and preparation method thereof | |
CN111548586B (en) | Polymer-based composite heat conduction material and preparation method and application thereof | |
CN109228549B (en) | Preparation method of high-thermal-conductivity nanocellulose-based electrical insulation film material | |
CN114684796A (en) | Boron nitride nanosheet based on large length-diameter ratio, high-thermal-conductivity insulating composite material and preparation method thereof | |
CN115029110A (en) | Graphene composite heat-conducting film and preparation method thereof | |
CN114921233A (en) | Graphene phase-change heat-conducting film and preparation method thereof | |
CN111004461A (en) | Heat-conducting polytetrafluoroethylene sheet with stable size and preparation method thereof | |
CN114536923B (en) | Fluorine-containing resin-based high-heat-conductivity high-frequency copper-clad plate with high dielectric constant | |
CN114574122B (en) | Fluorine-containing resin-based high-frequency copper-clad plate high-heat-conductivity bonding sheet | |
CN112724445B (en) | PI/graphene oxide/graphene composite membrane and preparation method and application thereof | |
CN112759869B (en) | Light fluororesin/h-BN composite dielectric material with high heat conductivity and low dielectric loss and preparation method thereof | |
CN116606144B (en) | Method for preparing graphene heat-conducting thick film through chemical pre-reduction | |
CN116426251A (en) | Fluorinated graphene composite heat conducting film and preparation method thereof | |
CN115215330A (en) | Preparation method of graphene foam column, graphene heat dissipation material and preparation method thereof | |
CN116313338A (en) | PTC based on vertically oriented graphene as conductive material and preparation method thereof |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination |