CN113613474A - Preparation method of heat-conducting film - Google Patents
Preparation method of heat-conducting film Download PDFInfo
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- CN113613474A CN113613474A CN202110967267.8A CN202110967267A CN113613474A CN 113613474 A CN113613474 A CN 113613474A CN 202110967267 A CN202110967267 A CN 202110967267A CN 113613474 A CN113613474 A CN 113613474A
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- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
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- 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
- H05K7/20436—Inner thermal coupling elements in heat dissipating housings, e.g. protrusions or depressions integrally formed in the housing
- H05K7/20445—Inner thermal coupling elements in heat dissipating housings, e.g. protrusions or depressions integrally formed in the housing the coupling element being an additional piece, e.g. thermal standoff
- H05K7/20472—Sheet interfaces
- H05K7/20481—Sheet interfaces characterised by the material composition exhibiting specific 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
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/194—After-treatment
Abstract
The invention provides a preparation method of a heat-conducting film, which comprises the following steps: coating graphene oxide slurry on the surface of a base material, baking the graphene oxide slurry into a graphene oxide film, and stripping and rolling the base material of the graphene oxide film; carrying out thermal reduction treatment on the rolled graphene oxide film to obtain a graphene film; carrying out joule heat graphitization treatment on the graphene film; and carrying out rolling treatment on the graphene film subjected to the thermal graphitization treatment of the focusing lug to obtain the heat-conducting film. The invention realizes roll-to-roll production, and can obviously improve the production efficiency and reduce the production cost.
Description
Technical Field
The invention belongs to the technical field of heat-conducting films, and particularly relates to a preparation method of a heat-conducting film.
Background
In recent years, with the development of 5G mobile phone terminal equipment, the core SOC chip has higher and higher integration level, the chip has more and more serious heating, and the requirements for heat conduction and heat dissipation in the mobile phone design process are higher and higher. Traditional metal foil heat dissipation, natural graphite heat dissipation, even artificial graphite heat dissipation schemes have not been able to meet the demand for high heat flux. The graphene heat-conducting film is a novel heat-conducting and heat-dissipating material developed in recent years, has the characteristics of high heat-conducting coefficient and high heat flux, is well applied to various flagship mobile phones, and is expected to solve the problem of heat management of mobile phone terminal equipment.
At present, in the graphite alkene heat conduction membrane production process, still there is the yields not high, need the problem of piece formula production. And traditional artifical graphite heat conduction membrane has realized roll-type production in process of production basically, and production efficiency is high, the yield is high, and the cost has the advantage than graphite alkene heat conduction membrane. One of the major limiting factors for realizing roll-to-roll production of the graphene heat-conducting film is the problems of severe expansion of materials and reduction of mechanical properties of the materials in the heat treatment process. The reason is that the graphene thermal conductive film is generally made of graphene oxide, and severe oxygen loss reaction causes severe material expansion in the thermal treatment process. In addition, at present, the roll-to-roll production cannot be realized no matter the artificial graphite heat-conducting film or the graphene heat-conducting film is, and the important factor that the heat-conducting film production cost cannot be continuously explored is the same.
Disclosure of Invention
In view of one or more of the problems of the prior art, the present invention provides a method for preparing a thermally conductive film, comprising:
step S1, coating graphene oxide slurry on the surface of a base material, baking the graphene oxide slurry into a graphene oxide film, and stripping and rolling the base material of the graphene oxide film;
step S2, carrying out thermal reduction treatment on the rolled graphene oxide film to obtain a graphene film;
step S3, carrying out Joule thermal graphitization treatment on the graphene film;
and step S4, performing rolling treatment on the graphene film subjected to the thermal graphitization treatment of the lugs to obtain the heat-conducting film.
Optionally, the step S1 includes:
coating the graphene oxide slurry on the surface of the base material by using a coating machine;
baking the graphene oxide slurry coated on the surface of the substrate to form a film, peeling the film from the substrate and rolling the film, preferably, baking the film after coating at 50-150 ℃ for 1-60 minutes, wherein the baking temperature of the graphene oxide film cannot be too high, so that the film has certain moisture while the surface of the film is dried, and the film can keep good flexibility, peelability and rolling characteristics, preferably, the baking temperature is 60-80 ℃ and the baking time is 20-40 minutes.
Optionally, the solid content of the graphene oxide slurry is 1-30 wt%, and the viscosity is 1000-100000 cps.
Optionally, the substrate is a PE (polyethylene) mesh, a PP (polypropylene) filter cloth, or a silica gel protective film.
Optionally, the step S2 includes:
the method comprises the following steps of (1) adopting an atmosphere protection push plate furnace, placing a graphene oxide film in the push plate furnace, and arranging discharging and receiving traction devices at a feeding port and a discharging port of the push plate furnace to realize roll-to-roll discharging and receiving;
introducing protective gas into the push plate furnace, wherein the protective gas is preferably high-purity nitrogen or high-purity argon, and further preferably the oxygen content of the protective gas is controlled to be below 60ppm and the oxygen content is low, so that the graphite oxide film is not oxidized in the thermal reduction process;
setting the temperatures of a plurality of temperature intervals in the pusher furnace and the operation speed of the graphene oxide film;
and carrying out thermal reduction in a plurality of temperature intervals of the push plate furnace according to the set running speed of the graphene oxide film to obtain the graphene film.
Optionally, the step S2 further includes:
the continuous rolling treatment is carried out on the graphene film, preferably, the pressure in the rolling treatment is 2-20MPa, and the graphene film is expanded seriously in the thermal reduction process, so that the tensile resistance of the graphene film is reduced, and therefore, the tensile mechanical property of the graphene film is improved through rolling, and the rolling and subsequent graphitization treatment are facilitated;
and rolling the rolled graphene film.
Optionally, the plurality of temperature intervals include a first low-temperature zone, a second medium-temperature zone, and a third high-temperature zone, the first low-temperature zone having a temperature set from room temperature to 300 ℃; a second intermediate temperature zone, the temperature is set to be from 300 ℃ to 800 ℃; a third high temperature zone, the temperature is set to be from 800 ℃ to 1200 ℃; preferably, the total length of one temperature interval is 20-100 meters; preferably, the running speed of the graphene film is 0.1-1 m/min. In different temperature ranges, the graphene oxide has different deoxidation and exhaust processes, the expansion of the graphene film is affected differently, and the graphene film may be broken into powder by the violent deoxidation and exhaust processes.
Optionally, the step S3 includes:
a joule heat graphitization area is arranged in the push plate furnace protected by atmosphere;
a roll-to-roll type feeding and receiving device is arranged in a feeding area and a discharging area of the atmosphere-protected pusher furnace;
the continuous joule heating graphitization treatment is carried out on the passing graphene film by adopting a plurality of pairs of roller pressing graphite electrodes in the form of upper rollers and lower rollers, preferably, the joule heating graphitization temperature is 2400-3100 ℃, the operation speed of the graphene film is 0.05-1m/min, 2400-3100 ℃, the graphitization effect can be ensured, the higher the temperature is, the better the operation speed is, the graphitization time is controlled, and the slower the speed is, the better the graphitization effect is.
Optionally, the step S3 includes:
a joule heat graphitization area is arranged in the push plate furnace protected by atmosphere;
a roll-to-roll type feeding and receiving device is arranged in a feeding area and a discharging area of the atmosphere-protected pusher furnace;
carrying out semi-continuous joule heating graphitization treatment on the graphene film by adopting a pressing type plurality of pairs of roller graphite pressing electrodes, preferably, the joule heating graphitization temperature is 2400-; the single treatment time controls the graphitization time, with slower rates being better.
Optionally, the step S4 includes:
and (3) rolling the graphene film subjected to the joule heat graphitization treatment by using a vacuum rolling machine or a double-roller rolling machine, preferably, the rolling pressure is 50-200MPa, so that the graphene heat-conducting film is ensured to have the density close to that of graphite, the mechanical property is improved, and the heat conductivity coefficient is controlled.
Optionally, the step S4 includes:
cutting the coiled graphene film subjected to the joule heat graphitization treatment into a sheet type graphene film;
and rolling the sheet graphene film by using a vacuum rolling machine.
According to the preparation method, the graphene oxide slurry is adopted, after being coated, roll-to-roll reduction is carried out in a tunnel type push plate furnace protected by inert gas, after rolling, graphitization treatment is carried out by a joule heat graphitization method, and finally rolling is carried out by rolling equipment.
Starting from pretreatment after coating of a graphene oxide material, roll-to-roll heat treatment technology is adopted to realize roll-to-roll production of a heat-conducting film, and a graphene film subjected to high-temperature thermal reduction is obtained; the graphene heat-conducting membrane subjected to graphitization heat treatment is efficiently obtained by adopting a Joule heat graphitization treatment process.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
fig. 1 is a schematic view of a flow chart of a method for producing a thermally conductive film according to the present invention.
Detailed Description
In the following, only certain exemplary embodiments are briefly described. As those skilled in the art will recognize, the described embodiments may be modified in various different ways, all without departing from the spirit or scope of the present invention. Accordingly, the drawings and description are to be regarded as illustrative in nature, and not as restrictive.
The following disclosure provides many different embodiments or examples for implementing different features of the invention. To simplify the disclosure of the present invention, the components and arrangements of specific examples are described below. Of course, they are merely examples and are not intended to limit the present invention. Furthermore, the present invention may repeat reference numerals and/or letters in the various examples, such repetition is for the purpose of simplicity and clarity and does not in itself dictate a relationship between the various embodiments and/or configurations discussed. In addition, the present invention provides examples of various specific processes and materials, but one of ordinary skill in the art may recognize applications of other processes and/or uses of other materials.
The preferred embodiments of the present invention will be described in conjunction with the accompanying drawings, and it will be understood that they are described herein for the purpose of illustration and explanation and not limitation.
Example 1:
the preparation method of the heat-conducting film comprises the following steps:
1) coating graphene oxide slurry on the surface of a PP porous membrane substrate, wherein the solid content of the graphene oxide slurry is 4%, the coating thickness is 1.8mm, and the viscosity of the graphene oxide slurry is 18000 cps;
2) baking the coated graphene oxide film in an IR tunnel furnace at the baking temperature of 80 ℃ for 30 minutes, rolling after baking, and stripping the PP porous film substrate;
3) placing the baked graphene oxide film into an atmosphere push plate furnace, and adopting a roll-to-roll discharging and receiving device;
4) introducing high-purity nitrogen protective gas into the push plate furnace, wherein the oxygen content is controlled to be 50ppm at the discharge port and the receiving port and to be 10ppm at the heating zone;
5) a plurality of temperature intervals are arranged in the push plate furnace, a first low-temperature area has the total length of 100 meters, and the temperature is set to be from 30 to 300 ℃; a second intermediate temperature zone, having a total length of 80 meters and a temperature set from 300 ℃ to 800 ℃; a third high temperature zone having a total length of 60 meters and a temperature set from 800 ℃ to 1200 ℃; the running speed of the graphene oxide film is 0.5 m/min;
6) before rolling, carrying out continuous rolling treatment on the graphene film, wherein the pressure of a rolling process is 10MPa, and rolling after rolling to finish thermal reduction treatment;
7) a joule heat graphitization area is arranged in the atmosphere push plate furnace, and a roll-to-roll type feeding and receiving device is arranged in the feeding area and the discharging area of the atmosphere push plate furnace; introducing high-purity nitrogen protective gas into the push plate furnace, wherein the oxygen content is controlled to be 50ppm at the discharge port and the receiving port and to be 10ppm at the heating zone;
8) and (3) carrying out continuous joule heating graphitization treatment on the reduced graphene film by adopting a rolling graphite electrode in the form of an upper roller and a lower roller, wherein the joule heating graphitization temperature is 2800 ℃. When the continuous joule heat graphitization treatment is carried out, the running speed of the graphene film is 0.3 m/min;
9) rolling the graphene film subjected to the joule heat graphitization treatment by using a double-roller rolling machine to obtain a heat conducting film; the rolling pressure was 70 MPa.
In the embodiment, after the graphitization treatment is finished, the treatment by the sheet cutting machine is not adopted, so that the defect that the joule heat temperature of the graphite electrode contact area is not enough to reach the graphitization temperature by the treatment by the sheet cutting machine is overcome.
Example 2:
the preparation method of the heat-conducting film comprises the following steps:
1) coating graphene oxide slurry on the surface of a PP porous membrane substrate, wherein the solid content of the graphene oxide slurry is 4%, the coating thickness is 1.8mm, and the viscosity of the graphene oxide slurry is 18000 cps;
2) baking the coated graphene oxide film in an IR tunnel furnace at the baking temperature of 80 ℃ for 30 minutes, rolling after baking, and stripping the PP porous film substrate;
3) placing the baked graphene oxide film into an atmosphere push plate furnace, and adopting a roll-to-roll discharging and receiving device;
4) introducing high-purity nitrogen protective gas into the push plate furnace, wherein the oxygen content is controlled to be 50ppm at the discharge port and the receiving port and to be 10ppm at the heating zone;
5) a plurality of temperature intervals are arranged in the push plate furnace, a first low-temperature area has the total length of 100 meters, and the temperature is set to be from 30 to 300 ℃; a second intermediate temperature zone, having a total length of 80 meters and a temperature set from 300 ℃ to 800 ℃; a third high temperature zone having a total length of 60 meters and a temperature set from 800 ℃ to 1200 ℃; the running speed of the graphene oxide film is 0.3 m/min;
6) before rolling, carrying out continuous rolling treatment on the graphene film, wherein the pressure of a rolling process is 8MPa, and rolling after rolling to finish thermal reduction treatment;
7) a joule heat graphitization area is arranged in the atmosphere push plate furnace, and a roll-to-roll type feeding and receiving device is arranged in the feeding area and the discharging area of the atmosphere push plate furnace; introducing high-purity nitrogen protective gas into the push plate furnace, wherein the oxygen content is controlled to be 50ppm at the discharge port and the receiving port and to be 10ppm at the heating zone;
8) carrying out semi-continuous joule heating graphitization treatment on the reduced graphene film by adopting a compression type upper electrode and a compression type lower electrode, wherein the joule heating graphitization temperature is 2800 ℃, and the single treatment time is 15 seconds; the graphene film moves in a semi-continuous mode, and semi-continuous graphitization is performed on the surface of the film by adopting an optical recognition device, wherein a graphite electrode is in a contact area with the graphene film.
9) Rolling the graphene sheet type thin film subjected to the joule heat graphitization treatment by using a vacuum rolling machine to obtain a heat conducting film; the rolling pressure was 65 MPa.
Taking the heat-conducting films of the embodiments 1 and 2 of the present invention as sample 1 and sample 2, and taking the graphene heat-conducting film prepared by a high-temperature graphitization furnace at 2850 ℃ in the prior art as sample 3 (carrying out graphitization treatment by a traditional high-temperature graphitization furnace at 2850 ℃ for 10 hours), the in-plane heat conductivity coefficient of the heat-conducting film is tested, as shown in the following table 1:
TABLE 1
| Sample number | Thickness (μm) | Density (g/cm)3) | Coefficient of thermal conductivity (W/m.K) |
| 1 | 25 | 1.82 | 1180 |
| 2 | 24 | 1.80 | 1165 |
| 3 | 25 | 1.84 | 1210 |
The difference between the heat-conducting performance of the heat-conducting film obtained by the preparation method of the heat-conducting film and the graphene film prepared by the high-temperature graphitization furnace is smaller, the graphene oxide slurry is adopted, after coating, roll-to-roll reduction is carried out in a tunnel type push plate furnace protected by inert gas, after primary rolling, graphitization treatment is carried out by a joule heat graphitization method, and finally rolling secondary rolling is carried out by rolling equipment (the primary rolling is used for improving the mechanical property and the heat-conducting performance of the graphene film, and the secondary rolling needs to improve the density besides the mechanical property and the heat-conducting performance, so that the pressure of the secondary rolling is larger than that of the primary rolling), the roll-to-roll production can be realized in the whole process after optimization, and the production efficiency can be obviously improved and the production cost can be reduced. Compared with the traditional preparation process of the heat conducting film, in the high-temperature graphitization stage, the energy consumed by the joule heat graphitization treatment is only 1/4-1/2 of the energy consumed (electric power) consumed by the vacuum graphitization furnace heat treatment, and the energy consumption has obvious advantages.
According to the existing production process of the graphene heat-conducting film, the whole-process roll-to-roll production of the graphene heat-conducting film in the production process cannot be carried out, and the production process is an important factor influencing the production efficiency, the production yield and the production cost of the graphene heat-conducting film. According to the invention, based on pretreatment after coating of the end of the graphene material, a reel-to-reel processing mode is adopted in the thermal reduction processing stage of the graphene film, so that the preparation with high efficiency, low cost and high yield can be realized, the traditional carbonization furnace equipment and a sheet processing mode are abandoned, and the reel-to-reel production of the heat-conducting film is realized.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method for preparing a heat-conducting film is characterized by comprising the following steps:
step S1, coating graphene oxide slurry on the surface of a base material, baking the graphene oxide slurry into a graphene oxide film, and stripping and rolling the base material of the graphene oxide film;
step S2, carrying out thermal reduction treatment on the rolled graphene oxide film to obtain a graphene film;
step S3, carrying out Joule thermal graphitization treatment on the graphene film;
and step S4, performing rolling treatment on the graphene film subjected to the thermal graphitization treatment of the lugs to obtain the heat-conducting film.
2. The method for producing a heat conductive film according to claim 1, wherein the step S1 includes:
coating the graphene oxide slurry on the surface of the base material by using a coating machine;
baking the graphene oxide slurry coated on the surface of the base material to form a film, peeling the film from the base material, and rolling the film, wherein the baking temperature after coating is preferably 50-150 ℃, the baking time is preferably 1-60 minutes, and the baking temperature is preferably 60-80 ℃, and the baking time is 20-40 minutes.
3. The method for preparing the thermal conductive film according to claim 1 or 2, wherein the graphene oxide slurry has a solid content of 1-30 wt%, a viscosity of 1000-; or/and
the base material is PE (polyethylene) net, PP (polypropylene) filter cloth or silica gel protective film.
4. The method for producing a heat conductive film according to claim 1, wherein the step S2 includes:
the method comprises the following steps of (1) adopting an atmosphere protection push plate furnace, placing a graphene oxide film in the push plate furnace, and arranging discharging and receiving traction devices at a feeding port and a discharging port of the push plate furnace to realize roll-to-roll discharging and receiving;
introducing a protective gas into the push plate furnace, wherein the protective gas is preferably high-purity nitrogen or high-purity argon, and further preferably, the oxygen content of the protective gas is controlled to be below 60 ppm;
setting the temperatures of a plurality of temperature intervals in the pusher furnace and the operation speed of the graphene oxide film;
and carrying out thermal reduction in a plurality of temperature intervals of the push plate furnace according to the set running speed of the graphene oxide film to obtain the graphene film.
5. The method for preparing a heat conductive film according to claim 4, wherein the step S2 further comprises:
carrying out continuous rolling treatment on the graphene film, wherein the pressure in the rolling treatment is preferably 2-20 MPa;
and rolling the rolled graphene film.
6. The method according to claim 4 or 5, wherein the plurality of temperature zones include a first low-temperature zone, a second medium-temperature zone, and a third high-temperature zone, the first low-temperature zone being set at a temperature of from room temperature to 300 ℃; a second intermediate temperature zone, the temperature is set to be from 300 ℃ to 800 ℃; a third high temperature zone, the temperature is set to be from 800 ℃ to 1200 ℃; preferably, the total length of one temperature interval is 20-100 meters; preferably, the running speed of the graphene film is 0.1-1 m/min.
7. The method for producing a heat conductive film according to claim 1, wherein the step S3 includes:
a joule heat graphitization area is arranged in the push plate furnace protected by atmosphere;
a roll-to-roll type feeding and receiving device is arranged in a feeding area and a discharging area of the atmosphere-protected pusher furnace;
and (3) carrying out continuous joule heating graphitization treatment on the passing graphene film by adopting a plurality of pairs of roller pressing graphite electrodes in the form of upper rollers and lower rollers, wherein preferably, the joule heating graphitization temperature is 2400-3100 ℃, and the running speed of the graphene film is 0.05-1 m/min.
8. The method for producing a heat conductive film according to claim 1, wherein the step S3 includes:
a joule heat graphitization area is arranged in the push plate furnace protected by atmosphere;
a roll-to-roll type feeding and receiving device is arranged in a feeding area and a discharging area of the atmosphere-protected pusher furnace;
and (3) performing semi-continuous joule heating graphitization treatment on the graphene film by adopting a pressing type plurality of pairs of roller graphite pressing electrodes, wherein preferably, the joule heating graphitization temperature is 2400-3100 ℃, and the single treatment time is 1-60 s.
9. The method for producing a heat conductive film according to claim 1, wherein the step S4 includes:
and rolling the graphene film subjected to the joule heat graphitization treatment by using a vacuum calendar or a double-roller calendar, wherein the rolling pressure is preferably 50-200 MPa.
10. The method for producing a heat conductive film according to claim 9, wherein the step S4 includes:
cutting the coiled graphene film subjected to the joule heat graphitization treatment into a sheet type graphene film;
and rolling the sheet graphene film by using a vacuum rolling machine.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114349000A (en) * | 2021-12-06 | 2022-04-15 | 开封时代新能源科技有限公司 | Graphene heat-conducting film graphitization method |
| CN114368744A (en) * | 2021-12-27 | 2022-04-19 | 广东墨睿科技有限公司 | Graphene mixed material and preparation method thereof, and graphene temperature-uniforming plate and preparation method thereof |
| CN114803607A (en) * | 2022-04-15 | 2022-07-29 | 常州富烯科技股份有限公司 | Coiled material winding device, placing device, graphene heat-conducting film coiled material and preparation method |
| CN115379605A (en) * | 2022-08-10 | 2022-11-22 | 温州众合绿材科技有限公司 | Graphene heating film, assembly, system and temperature control method |
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| CN114803607A (en) * | 2022-04-15 | 2022-07-29 | 常州富烯科技股份有限公司 | Coiled material winding device, placing device, graphene heat-conducting film coiled material and preparation method |
| CN115379605A (en) * | 2022-08-10 | 2022-11-22 | 温州众合绿材科技有限公司 | Graphene heating film, assembly, system and temperature control method |
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