CN113582166A - Heat conduction membrane manufacture equipment - Google Patents
Heat conduction membrane manufacture equipment Download PDFInfo
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- CN113582166A CN113582166A CN202110966848.XA CN202110966848A CN113582166A CN 113582166 A CN113582166 A CN 113582166A CN 202110966848 A CN202110966848 A CN 202110966848A CN 113582166 A CN113582166 A CN 113582166A
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
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- C01B32/182—Graphene
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B65H23/00—Registering, tensioning, smoothing or guiding webs
- B65H23/04—Registering, tensioning, smoothing or guiding webs longitudinally
- B65H23/26—Registering, tensioning, smoothing or guiding webs longitudinally by transverse stationary or adjustable bars or rollers
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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
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- C01B32/205—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
- C01B32/20—Graphite
- C01B32/21—After-treatment
Abstract
The invention provides heat-conducting film manufacturing equipment which comprises reeling and unreeling equipment, a thermal reduction furnace, a graphitization furnace and calendaring equipment, wherein the reeling and unreeling equipment is used for carrying out substrate stripping and reeling on a graphene oxide film, the thermal reduction furnace is used for carrying out thermal reduction treatment on the graphene oxide film reeled by the reeling and unreeling equipment to obtain the graphene film, the reeling and unreeling equipment is used for reeling the graphene film obtained by the thermal reduction furnace and unreeling the reeled graphene film to the graphitization furnace, and the graphitization furnace is used for carrying out joule thermal graphitization treatment on the graphene film; the rolling equipment is used for rolling the graphene film subjected to the thermal graphitization treatment by the coke ear of the graphitization furnace; the winding and unwinding equipment winds the graphene film subjected to calendering treatment by the calendering equipment to obtain the rolled heat-conducting film. The invention realizes the roll-to-roll production of the heat-conducting film, 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 heat-conducting film manufacturing equipment.
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
The invention provides heat-conducting film manufacturing equipment which comprises winding and unwinding equipment, a thermal reduction furnace, a graphitization furnace and calendaring equipment, wherein the winding and unwinding equipment is used for stripping and winding a base material of a graphene oxide film, the thermal reduction furnace is used for carrying out thermal reduction treatment on the graphene oxide film wound by the winding and unwinding equipment to obtain the graphene film, the winding and unwinding equipment is used for winding the graphene film obtained by the thermal reduction furnace and unwinding the wound graphene film to the graphitization furnace, and the graphitization furnace is used for carrying out joule heating graphitization treatment on the graphene film; the rolling equipment is used for rolling the graphene film subjected to the thermal graphitization treatment by the coke ear of the graphitization furnace; the winding and unwinding equipment winds the graphene film subjected to calendering treatment by the calendering equipment to obtain the rolled heat-conducting film.
Optionally, the manufacturing apparatus further comprises a coater and an IR tunnel furnace, wherein the coater is used for manufacturing a graphene oxide thin film, graphene oxide slurry is coated on the surface of the substrate by using the coater, and the IR tunnel furnace is used for baking the graphene oxide slurry coated on the surface of the substrate to form a film, preferably, the baking temperature of the IR tunnel furnace is 50-150 ℃, the baking time is 1-60 minutes, and further preferably, the baking temperature of the IR tunnel furnace 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 thermal reduction furnace includes a sealed gas feeding port region, a sealed gas discharging port region and a transmission device, the sealed gas discharging port region is arranged between the sealed gas feeding port region and the sealed gas discharging port region, protective gas is introduced into the sealed region, the transmission device sets an operation speed, the graphene oxide film unreeled by the reeling and unreeling device is transmitted to the sealed gas feeding port region and then transmitted to the sealed gas discharging port region, the heated reduction region includes a plurality of temperature intervals, thermal reduction is performed in the temperature intervals to obtain the graphene film, the graphene film passes through the sealed gas discharging port region by transmission of the transmission device, and the graphene film is reeled by the reeling and unreeling device.
Optionally, the rolling device further performs rolling treatment on the graphene film obtained by the thermal reduction furnace, and then transmits the graphene film to the winding and unwinding device, and preferably, the pressure of the rolling device is 2-20 MPa.
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.
Optionally, the graphitization furnace comprises a feeding port sealing gas mu area, a joule heating graphitization area, a discharging port sealing gas mu area and a conveying device, the graphitization area is arranged in a sealing area between the feeding port sealing gas mu area and the discharging port sealing gas mu area, protective gas is introduced into the sealing area, the graphitization area is provided with a multi-joule heating graphite electrode, the multi-joule heating graphite electrode is synchronously driven with the driving device, the joule heating graphite electrode adopts a double-roller form of an upper roller and a lower roller, the conveying device sets an operation speed, the graphene film unreeled by the reeling and unreeling device is conveyed to the feeding port sealing gas mu area and then conveyed to the joule heating graphitization area, the multi-joule heating graphite electrode performs continuous joule heating graphitization treatment on the graphene film passing through the discharging port sealing gas mu area through the conveying device, and (4) winding by using winding and unwinding equipment, wherein preferably, the temperature of the Joule thermal graphitization zone is 2400-3100 ℃, and the running speed of the transmission equipment is 0.05-1 m/min.
Optionally, the graphitization furnace comprises a feeding port sealing gas mu area, a joule heating graphitization area, a discharging port sealing gas mu area and a conveying device, the graphitization area is arranged in a sealing area between the feeding port sealing gas mu area and the discharging port sealing gas mu area, protective gas is introduced into the sealing area, the graphitization area is provided with a multi-joule heating graphite electrode, the multi-joule heating graphite electrode and the conveying device synchronously transmit, the joule heating graphite electrode adopts a compression electrode, the conveying device sets an operation speed, a graphene film unreeled by the reeling and unreeling device is transmitted to the feeding port sealing gas mu area and then transmitted to the joule heating graphitization area, the multi-joule heating graphite electrode performs semi-continuous joule heating graphitization treatment on the graphene film passing through the graphene film, the multi-joule heating graphite electrode passes through the discharging port sealing gas mu area through the conveying device transmission, and is reeled by the reeling and unreeling device, preferably, the temperature of the joule heat graphitization zone is 2400-3100 ℃, and the time of the single joule heat graphitization treatment is 1-60 s.
Optionally, the protective gas is high-purity nitrogen or high-purity argon, and preferably, the oxygen content of the protective gas is controlled below 60 ppm.
Optionally, the rolling device is a vacuum rolling machine and/or a pair-roll rolling machine, and preferably, the rolling device rolls the graphene film subjected to the joule heat graphitization treatment by the graphitization furnace at a pressure of 50-200 MPa.
Optionally, when the rolling device is a vacuum rolling machine, the manufacturing device further includes a sheet cutting machine, the sheet cutting machine cuts the rolled graphene film subjected to the joule heat graphitization treatment into a sheet graphene film, and the vacuum rolling machine rolls the sheet graphene film.
Optionally, the thermal reduction furnace and the graphitization furnace are thermal reduction zones and graphitization zones of one atmosphere furnace, and preferably, the atmosphere furnace is a push plate furnace.
The heat-conducting film manufacturing equipment provided by the invention is used for carrying out roll-to-roll reduction on the graphene oxide film, carrying out graphitization treatment by adopting a joule heat graphitization mode after rolling, and finally carrying out roll-to-roll rolling by adopting rolling equipment, so that roll-to-roll production of the heat-conducting film can be realized in the whole process after optimization, the production efficiency can be obviously improved, and the production cost can be reduced.
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 an embodiment of a thermal reduction furnace of the apparatus for producing a thermally conductive film according to the present invention;
FIG. 2 is a schematic view of an embodiment of a graphitization furnace of the heat conductive film production apparatus according to the present invention;
FIG. 3 is a schematic view of one embodiment of a Joule heated graphite electrode of the present invention;
FIG. 4 is a schematic view of another embodiment of a Joule heated graphite electrode of 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.
In an embodiment, as shown in fig. 1 and 2, the apparatus for manufacturing a heat-conducting film of the present invention includes a winding and unwinding apparatus 1, a thermal reduction furnace 2, a graphitization furnace 3, and a calendaring apparatus 4, where the winding and unwinding apparatus peels and winds a graphene oxide film, the thermal reduction furnace performs thermal reduction processing on the graphene oxide film wound by the winding and unwinding apparatus to obtain a graphene film, the winding and unwinding apparatus winds the graphene film obtained by the thermal reduction furnace and unwinds the wound graphene film to the graphitization furnace, and the graphitization furnace performs joule heating graphitization processing on the graphene film; the rolling equipment is used for rolling the graphene film subjected to the thermal graphitization treatment by the coke ear of the graphitization furnace; the winding and unwinding equipment winds the graphene film subjected to calendering treatment by the calendering equipment to obtain the rolled heat-conducting film.
In an embodiment, as shown in fig. 1, the thermal reduction furnace 2 includes a feeding port sealed gas admiring region 5, a thermal reduction region 21, a discharging port sealed gas admiring region 6, and a conveying device 7, the thermal reduction region is disposed in a sealing region between the feeding port sealed gas admiring region and the discharging port sealed gas admiring region, a protective gas is introduced into the sealing region, the conveying device sets an operation speed, the graphene oxide film unreeled by the winding and unwinding device is conveyed to the feeding port sealed gas admiring region and then conveyed to the thermal reduction region, the thermal reduction region includes a plurality of temperature intervals, thermal reduction is performed in the plurality of temperature intervals to obtain a graphene film, the graphene film is conveyed by the conveying device through the discharging port sealed gas admiring region, and the graphene film is reeled by the winding and unwinding device.
In the thermal reduction process, the graphene film expands seriously, so that the tensile resistance of the graphene film is reduced, the tensile resistance of the graphene film is improved through calendering, the rolling and subsequent graphitization treatment are facilitated, preferably, the calendering equipment is used for further calendering the graphene film obtained by the thermal reduction furnace and then transmitting the calendered graphene film to the winding and unwinding equipment, and preferably, the pressure of the calendering equipment is 2-20 MPa.
Preferably, 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 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.
In one embodiment, as shown in FIG. 2, the graphitization furnace 3 includes a feed port sealed aeroponic section 5, a Joule heated graphitization section 31, a feed port sealed aeroponic section 6 and a transfer apparatus 7, the graphitizing region is arranged in a sealing region between the feed inlet sealing air mousse region and the discharge outlet sealing air mousse region, protective gas is introduced into the sealing area, the graphitizing area is provided with a multi-focusing-lug thermal graphite electrode 10, the multi-lug heat graphite electrode is synchronously driven with the transmission device, the transmission device sets the running speed, the graphene film unreeled by the winding and unwinding device is transmitted to the sealed gas-admiring area of the feeding port and then transmitted to the joule heat graphitization area, the multi-lug heat graphite electrode carries out joule heat graphitization treatment on the passing graphene film, the multi-lug heat graphite electrode passes through the sealed gas-admiring area of the discharging port through transmission of the transmission device, and the multi-lug heat graphite electrode is wound by the winding and unwinding device.
In one embodiment, as shown in fig. 3, the joule heating graphite electrode 10 is in the form of a pair of rollers including an upper roller 101 and a lower roller 102, and the multi-joule heating graphite electrode 10 performs a continuous joule heating graphitization process on the passing graphene thin film 12.
Preferably, the temperature of the joule heat graphitization area is 2400-3100 ℃, the operating speed of the transmission equipment is 0.05-1m/min, the operating 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 operating speed is, the graphitization time is controlled, and the slower the speed is, the better the graphitization effect is.
In one embodiment, as shown in fig. 4, the joule heating graphite electrode 10 employs a compression type electrode (an upper graphite electrode 103 and a lower graphite electrode 104), and the multi-joule heating graphite electrode 10 performs a semi-continuous joule heating graphitization process on the passing graphene film 12.
Preferably, the temperature of the joule heat graphitization area is 2400-3100 ℃, the time of single joule heat graphitization treatment is 1-60s, and the graphitization effect can be ensured at 2400-3100 ℃, and the higher the temperature is, the better the graphitization effect is; the single treatment time controls the graphitization time, with slower rates being better.
In the above embodiments, the protective gas is high purity nitrogen or argon, preferably, the oxygen content of the protective gas is controlled below 60ppm, and the oxygen content is low, so as to ensure that the graphite oxide film is not oxidized during the thermal reduction process.
In one embodiment, the manufacturing apparatus further comprises a coater for manufacturing the graphene oxide thin film, wherein the graphene oxide slurry is coated on the surface of the substrate by using the coater, and an IR tunnel furnace for baking the graphene oxide slurry coated on the surface of the substrate to form a film.
Preferably, the baking temperature of the IR tunnel furnace is 50-150 ℃, the baking time is 1-60 minutes, the baking temperature of the graphene oxide film cannot be too high, the surface drying of the film is ensured, meanwhile, a certain amount of moisture exists in the film, and the film can keep good flexibility, stripability and rolling characteristics, and further preferably, the baking temperature of the IR tunnel furnace 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.
In one embodiment, the rolling device is a vacuum rolling machine and/or a pair-roll rolling machine, preferably, in order to ensure that the graphene thermal conductive film has a density close to that of graphite, improve mechanical properties, and control a thermal conductivity coefficient, the pressure of the rolling device in rolling the graphene film subjected to the thermal graphitization treatment by the coke lug of the graphitization furnace is 50-200 MPa.
Optionally, when the rolling device is a vacuum rolling machine, the manufacturing device further includes a sheet cutting machine, the sheet cutting machine cuts the rolled graphene film subjected to the joule heat graphitization treatment into a sheet graphene film, and the vacuum rolling machine rolls the sheet graphene film.
In one embodiment, the thermal reduction furnace and the graphitization furnace are thermal reduction zones and graphitization zones of one atmosphere furnace, preferably, the atmosphere furnace is a push plate furnace.
In one embodiment, as shown in fig. 1 and 2, the heat conductive film manufacturing apparatus further includes one or more of the following components:
the display screen 8 is used for displaying parameters in the process of preparing the heat-conducting membrane, and the parameters comprise one or more of the number of temperature intervals of the thermal reduction zone, the temperature of each temperature interval, the mode of joule heat graphitization, the temperature of the joule heat graphitization zone, the time of joule heat graphitization treatment, the oxygen content of protective gas, the pressure of the calendering equipment and the running speed of the transmission equipment;
the control panel 9 is provided with a plurality of control buttons, and the control buttons are used for inputting parameters in the process of preparing the heat-conducting film by a client;
and the control cabinet 11 is used for controlling parameters in the process of preparing the heat-conducting film.
According to the invention, the graphene oxide film is generated by coating the end of the graphene oxide material on the coating machine and then is pretreated, and the roll-to-roll production of the heat-conducting film is realized by adopting roll-to-roll heat treatment, so that the 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.
To illustrate the beneficial effects of the present invention, the following examples prepared a thermally conductive film using the thermally conductive film apparatus of the present invention, specifically:
example 1:
the method for preparing the heat-conducting film by the heat-conducting film equipment comprises the following steps:
1) coating graphene oxide slurry on the surface of a PP porous membrane substrate by using a coating machine, 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 by adopting a winding and unwinding device after baking is finished, and stripping the PP porous film substrate;
3) placing the baked graphene oxide film into a thermal reduction area of a push plate furnace, and discharging and receiving materials by using roll-to-roll winding and unwinding equipment;
4) introducing high-purity nitrogen protective gas into the push plate furnace, wherein the oxygen content is controlled to be 50ppm in a feeding port gas mousse area and a discharge port sealing gas mousse area, and is controlled to be 10ppm in a thermal reduction area;
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 by using a double-roller rolling machine, wherein the pressure of the double-roller rolling machine is 10MPa, and rolling after rolling;
7) a Joule thermal graphitization area is arranged in the push plate furnace, and a winding and unwinding device for roll-to-roll feeding and material receiving is arranged in a feeding port air mousse area and a discharging port sealing air mousse area of the push plate furnace; introducing high-purity nitrogen protective gas into the push plate furnace, wherein the oxygen content is controlled to be 50ppm in a feeding port gas mousse area and a discharging port sealing gas mousse area, and is controlled to be 10ppm in a Joule heat graphitization area;
8) and (3) carrying out continuous joule heating graphitization treatment on the reduced graphene film by adopting joule heating graphite electrodes 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 heating graphitization treatment by using a double-roll calender 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 method for preparing the heat-conducting film by the heat-conducting film equipment comprises the following steps:
1) coating graphene oxide slurry on the surface of a PP porous membrane substrate by using a coating machine, 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 a thermal reduction area of an atmosphere push plate furnace, and discharging and receiving materials by using roll-to-roll winding and unwinding equipment;
4) introducing high-purity nitrogen protective gas into the push plate furnace, wherein the oxygen content is controlled to be 50ppm in a feeding port gas mousse area and a discharge port sealing gas mousse area, and is controlled to be 10ppm in a thermal reduction area;
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 by using a double-roller rolling machine, wherein the pressure of the double-roller rolling machine is 8MPa, and rolling after rolling;
7) a joule heat graphitization area is arranged in the atmosphere push plate furnace, and a winding and unwinding device for roll-to-roll feeding and material receiving is arranged in a feed opening air mousse area and a discharge opening sealing air mousse area of the push plate furnace; introducing high-purity nitrogen protective gas into the push plate furnace, wherein the oxygen content is controlled to be 50ppm in a feeding port gas mousse area and a discharge port sealing gas mousse area, and is controlled to be 10ppm in a thermal reduction area;
8) carrying out semi-continuous joule heating graphitization treatment on the reduced graphene film by adopting a joule heating graphite 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 manufactured by the heat-conducting film manufacturing equipment and the graphene film manufactured by the high-temperature graphitization furnace is smaller, the heat-conducting film manufacturing equipment adopts the graphene oxide slurry, after coating, the graphene oxide slurry is subjected to roll-to-roll reduction in the tunnel type push plate furnace protected by inert gas, after primary rolling, the graphene oxide slurry is subjected to graphitization treatment by radiation of joule heat graphitization, and finally, rolling equipment is adopted for secondary rolling (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, the production efficiency can be obviously improved, and the production cost can be reduced. Compared with the traditional heat conducting film preparation equipment, 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) by the vacuum graphitization furnace heat treatment, and the energy consumption has obvious advantages.
The existing graphene heat-conducting film production equipment cannot perform whole-course roll-to-roll production in the production process of the graphene heat-conducting film, and is an important factor influencing the production efficiency, production yield and 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. The heat-conducting film manufacturing equipment is characterized by comprising winding and unwinding equipment, a thermal reduction furnace, a graphitization furnace and calendaring equipment, wherein the winding and unwinding equipment is used for stripping and winding a base material of a graphene oxide film, the thermal reduction furnace is used for carrying out thermal reduction treatment on the graphene oxide film wound by the winding and unwinding equipment to obtain the graphene film, the winding and unwinding equipment is used for winding the graphene film obtained by the thermal reduction furnace and unwinding the wound graphene film to the graphitization furnace, and the graphitization furnace is used for carrying out joule heat graphitization treatment on the graphene film; the rolling equipment is used for rolling the graphene film subjected to the thermal graphitization treatment by the coke ear of the graphitization furnace; the winding and unwinding equipment winds the graphene film subjected to calendering treatment by the calendering equipment to obtain the rolled heat-conducting film.
2. The apparatus of claim 1, further comprising a coater for manufacturing the graphene oxide thin film, wherein the graphene oxide slurry is coated on the surface of the substrate by using the coater, and an IR tunnel furnace for baking the graphene oxide slurry coated on the surface of the substrate to form a film, wherein the baking temperature of the IR tunnel furnace is preferably 50-150 ℃ and the baking time is 1-60 minutes, and further preferably the baking temperature of the IR tunnel furnace is 60-80 ℃ and the baking time is 20-40 minutes.
3. The apparatus for manufacturing a thermal conductive film according to claim 1 or 2, wherein the graphene oxide slurry has a solid content of 1-30 wt%, and a viscosity of 1000-; or/and
the base material is PE (polyethylene) net, PP (polypropylene) filter cloth or silica gel protective film.
4. The heat conduction film manufacturing equipment according to claim 1, wherein the thermal reduction furnace comprises a feed inlet sealing gas mu region, a thermal reduction region, a discharge outlet sealing gas mu region and a transmission device, the thermal reduction region is arranged in a sealing region between the feed inlet sealing gas mu region and the discharge outlet sealing gas mu region, protective gas is introduced into the sealing region, the transmission device sets an operation speed, the graphene oxide film unwound by the winding and unwinding device is transmitted to the feed inlet sealing gas mu region and then transmitted to the thermal reduction region, the thermal reduction region comprises a plurality of temperature intervals, thermal reduction is performed in the plurality of temperature intervals to obtain a graphene film, the graphene film passes through the discharge outlet sealing gas mu region through transmission of the transmission device, and winding is performed through the winding and unwinding device;
preferably, the rolling equipment is also used for rolling the graphene film obtained by the thermal reduction furnace and then transmitting the rolled graphene film to winding and unwinding equipment, and further preferably, the pressure of the rolling equipment is 2-20 MPa;
preferably, 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 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.
5. The heat-conducting film manufacturing equipment as claimed in claim 1, wherein the graphitization furnace comprises a feed inlet sealing air mousse region, a joule heating graphitization region, a discharge outlet sealing air mousse region and a conveying device, the graphitization region is arranged in a sealing region between the feed inlet sealing air mousse region and the discharge outlet sealing air mousse region, a protective gas is introduced into the sealing region, the graphitization region is provided with a multi-joule heating graphite electrode, the multi-joule heating graphite electrode and the conveying device synchronously drive, the joule heating graphite electrode is in a double-roller form of an upper roller and a lower roller, the conveying device sets an operation speed, the graphene film unreeled by the reeling and unreeling device is conveyed to the feed inlet sealing air mousse region and then conveyed to the joule heating graphitization region, and the multi-joule heating graphite electrode performs continuous joule heating graphitization on the passing graphene film, the conveying device is used for conveying the hot graphite and the hot graphite to pass through the discharge port sealing air mousse area, and the winding and unwinding device is used for winding, wherein preferably, the temperature of the joule heat graphitization area is 2400-.
6. The heat-conducting film manufacturing equipment as claimed in claim 1, wherein the graphitization furnace comprises a feed inlet sealing air mousse region, a joule heating graphitization region, a discharge outlet sealing air mousse region and a conveying device, the graphitization region is arranged in a sealing region between the feed inlet sealing air mousse region and the discharge outlet sealing air mousse region, protective gas is introduced into the sealing region, the graphitization region is provided with a multi-joule heating graphite electrode, the multi-joule heating graphite electrode is synchronously driven by the driving device, the joule heating graphite electrode adopts a pressing electrode, the conveying device sets an operation speed, the graphene film unreeled by the reeling and unreeling device is conveyed to the feed inlet sealing air mousse region and then conveyed to the joule heating graphitization region, and the multi-joule heating graphite electrode performs semi-continuous joule heating graphitization on the passing graphene film, the conveying device is used for driving the sealing air-mousse zone to pass through the discharge port, and the winding and unwinding device is used for winding, wherein the temperature of the joule heating graphitization zone is preferably 2400-.
7. The manufacturing apparatus of a thermally conductive film as claimed in claims 4 to 6, wherein the protective gas is a high purity nitrogen gas or a high purity argon gas, and preferably, the oxygen content of the protective gas is controlled to be 60ppm or less.
8. The manufacturing equipment of the heat conducting film according to claim 1, wherein the rolling equipment is a vacuum rolling machine and/or a pair-roll rolling machine, and preferably, the pressure of the rolling equipment in rolling the graphene thin film subjected to the thermal graphitization treatment by the coke ear of the graphitization furnace is 50-200 MPa.
9. The apparatus for manufacturing a heat conductive film according to claim 8, wherein when the rolling apparatus is a vacuum rolling machine, the apparatus further comprises a sheet cutting machine, the sheet cutting machine cuts the rolled graphene film after the joule heat graphitization treatment into a sheet graphene film, and the vacuum rolling machine rolls the sheet graphene film.
10. A thermally conductive film manufacturing apparatus according to claims 1 to 9, wherein the thermal reduction furnace and the graphitization furnace are a thermal reduction zone and a graphitization zone of one atmosphere furnace, preferably, the atmosphere furnace is a pusher furnace.
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