CN114774087A - Method for preparing graphene heat-conducting film - Google Patents
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- CN114774087A CN114774087A CN202210372307.9A CN202210372307A CN114774087A CN 114774087 A CN114774087 A CN 114774087A CN 202210372307 A CN202210372307 A CN 202210372307A CN 114774087 A CN114774087 A CN 114774087A
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Abstract
The invention discloses a method for preparing a graphene heat-conducting film, which comprises the following steps: conveying the filter membrane from outside to a vacuum box; spraying the graphene slurry onto the surface of the filter membrane before the filter membrane enters the vacuum box; leveling graphene slurry on the surface of the filter membrane; downwards filtering a filter membrane in a vacuum box to form a graphene heat-conducting membrane; introducing the graphene heat-conducting film into a plurality of rolling shaft assemblies for rolling, wherein the roller spacing of the rolling shaft assemblies is gradually reduced along the transmission direction of the graphene heat-conducting film; heating the graphene heat conduction film in the process of rolling the graphene heat conduction film; and rolling the graphene heat conduction film. According to the technical scheme, the method for preparing the graphene heat conduction film can quickly discharge moisture and bubbles in the graphene heat conduction film, can improve the heat conduction performance of the graphene heat conduction film, and can be used for continuous mass production of the graphene heat conduction film.
Description
Technical Field
The invention belongs to the technical field of graphene heat-conducting films, and particularly relates to a method for preparing a graphene heat-conducting film.
Background
The graphene heat-conducting film plays an important role in electronic components, aerospace and the field with high heat dissipation requirements. The graphene heat-conducting film prepared in the current market is mainly obtained by a doping method (graphene is doped with other raw materials such as carbon nano tubes, polyimide resin and the like), a polyimide film carbonization method, a graphitization method and the like, wherein other impurities are easily introduced in the doping process to influence the heat conductivity of the graphene film, and the graphene heat-conducting film prepared by the polyimide film graphitization method can obtain the graphene film with better heat conductivity, but defects appear in a graphene structure after multiple high-temperature treatments to influence the heat conductivity and the electric conductivity of the graphene structure, so that the graphene heat-conducting film with high heat conductivity and excellent performance cannot be obtained.
Disclosure of Invention
The invention aims to solve at least one of the technical problems in the prior art, and provides a method for preparing a graphene heat-conducting film, which can quickly discharge moisture and bubbles in the graphene heat-conducting film, can improve the heat-conducting property of the graphene heat-conducting film, and can be used for continuous mass production of the graphene heat-conducting film.
The technical scheme adopted by the invention for solving the technical problem is as follows:
a method of making a graphene thermal conductive film, comprising:
conveying the filter membrane from outside to a vacuum box;
before the filter membrane enters the vacuum box, spraying graphene slurry onto the surface of the filter membrane;
leveling graphene slurry on the surface of the filter membrane;
and downwards filtering the filter membrane in the vacuum box to form the graphene heat-conducting membrane.
Introducing the graphene heat-conducting film into a plurality of roller press shaft assemblies for rolling, wherein the roller spacing of the roller press shaft assemblies is gradually reduced along the transmission direction of the graphene heat-conducting film;
heating the graphene heat conduction film in the process of rolling the graphene heat conduction film;
and rolling the graphene heat conduction film.
With reference to the foregoing implementation manners, in some implementation manners of the present invention, the graphene thermal conductive film is introduced into three roller press shaft assemblies for rolling, and the roller spacing of the three roller press shaft assemblies along the transmission direction of the graphene thermal conductive film is sequentially: 100-200 μm, 80-100 μm, 50-80 μm.
With reference to the foregoing implementation manners, in some implementation manners of the present invention, the roller axle assembly is disposed in a drying room, and the drying room is provided with a drying system, and the drying system is configured to heat the graphene thermal conductive film.
With reference to the foregoing implementation manners, in some implementation manners of the present invention, the temperature of heating the graphene thermal conductive film by the drying system is 100 ℃ to 200 ℃.
In combination with the above implementations, in certain implementations of the invention, the vacuum level in the vacuum box is-0.1 MPa.
In some implementations of the invention, the graphene slurry is sprayed onto the surface of the filter membrane by a sprayer, and the graphene slurry is mixed and then conveyed to the sprayer before being sprayed.
With reference to the foregoing implementation manners, in some implementation manners of the present invention, the sprayer is connected to a slurry mixing mechanism, the slurry mixing mechanism includes a dispersion machine and a homogenizer, the dispersion machine is communicated with the homogenizer through a first pipeline, an outlet of the homogenizer is connected to the sprayer through a second pipeline, and an outlet of the homogenizer is provided with a control valve.
In combination with the above implementations, in some implementations of the invention, a graphene slurry on a surface of the filter membrane is leveled by a slurry leveling machine, the slurry leveling machine includes a first leveling machine and a second leveling machine, the second leveling machine is disposed between the first leveling machine and the vacuum box, the first leveling machine includes a first translation driving assembly and a first leveling rod extending in a left-right direction, the first translation driving assembly is configured to drive the first leveling rod to move in a front-rear direction, the second leveling machine includes a lifting driving assembly, a second translation driving assembly and a second leveling rod extending in a left-right direction, the lifting driving assembly is configured to drive the second leveling rod to move in an up-down direction, and the second translation driving assembly is configured to drive the second leveling rod to move in a front-rear direction.
With reference to the foregoing implementation manners, in some implementation manners of the present invention, the vacuum box includes an air pump and a belt conveyor, a belt of the belt conveyor is provided with a plurality of spaced filtering holes, the filter membrane is laid on a surface of the belt conveyor, and the air pump is connected to a bottom of the vacuum box.
With reference to the foregoing implementation manners, in some implementation manners of the present invention, the graphene thermal conductive film further includes a motor and a winding roller, an output shaft of the motor extends in a left-right direction and is in transmission connection with the winding roller, and the winding roller is used for winding the graphene thermal conductive film.
One of the above technical solutions has at least one of the following advantages or beneficial effects: according to the technical scheme, the graphene thermal conductive film preparation method adopts a downward suction filtration mode, can enable graphene slurry to quickly form a film and be separated from a filter membrane, achieves continuous and large-scale production of the graphene thermal conductive film, and solves the problem that the width of graphene is limited. In addition, according to the method for preparing the graphene heat conduction film, the graphene heat conduction film is dried in the rolling process, so that moisture and bubbles in the graphene heat conduction film are rapidly discharged, the heat conductivity of the graphene heat conduction film can be improved, and the product quality of the graphene heat conduction film is ensured.
Drawings
The invention will be further described with reference to the accompanying drawings in which:
FIG. 1 is a schematic diagram of the connection of one embodiment of the present invention.
Detailed Description
Reference will now be made in detail to the present preferred embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like reference numerals refer to like elements throughout.
In the present invention, if directions (up, down, left, right, front, and rear) are described, it is only for convenience of describing the technical solution of the present invention, and it is not intended or implied that the technical features referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus, it is not construed as limiting the present invention.
In the invention, the meaning of "a plurality of" is one or more, the meaning of "a plurality of" is more than two, and the meaning of "more than", "less than", "more than" and the like is understood to not include the number; the terms "above", "below", "within" and the like are understood to include the instant numbers. In the description of the present invention, if there are descriptions of "first" and "second" for the purpose of distinguishing technical features only, they are not interpreted as indicating or implying relative importance or implicitly indicating the number of the technical features indicated or implicitly indicating the precedence of the technical features indicated.
In the present invention, unless otherwise specifically limited, the terms "disposed," "mounted," "connected," and the like are to be understood in a broad sense, and for example, may be directly connected or indirectly connected through an intermediate; can be fixedly connected, can also be detachably connected and can also be integrally formed; may be mechanically connected, may be electrically connected or may be capable of communicating with each other; either internal to the two elements or in an interactive relationship of the two elements. The technical field can reasonably determine the specific meaning of the words in the invention by combining the specific contents of the technical scheme.
Referring to fig. 1, an embodiment of the present invention provides a method for preparing a graphene thermal conductive film, including:
the filter membrane (not shown) is transported from the outside into the vacuum chamber 1, i.e. the filter membrane is transported from the front to the back into the vacuum chamber 1. It will be appreciated that the filter membrane may be conveyed into the vacuum box 1 by a conveyor assembly 2 such as a belt conveyor or a caterpillar conveyor.
Before the filter membrane enters the vacuum box 1, spraying graphene slurry onto the surface of the filter membrane;
and leveling the graphene slurry on the surface of the filter membrane to preliminarily adjust the thickness of the graphene slurry.
And (3) filtering the filter membrane in the vacuum box 1 downwards to form a graphene heat conducting membrane 3. Under the suction filtration effect, on one hand, the graphene slurry can quickly discharge excessive moisture and bubbles, so that a film is quickly formed; on the other hand, the filter membrane can be clung to the conveying assembly 2 under the suction filtration effect, so that the filter membrane is separated from the formed graphene heat-conducting membrane 3, and the graphene heat-conducting membrane 3 is continuously conveyed forwards.
The graphene heat conducting film 3 is introduced into a plurality of rolling shaft assemblies 4 for rolling, and the transmission of the rolling shaft assemblies 4 is the prior art, so that the further detailed description is omitted. The roller spindle assembly 4 includes a first driving roller 41 and a second driving roller 42 extending in the left-right direction, and a roller gap 43 is formed between the first driving roller 41 and the second driving roller 42. Roll gap 43 of roll shaft assembly 4 reduces along graphene heat conduction membrane 3's direction of transfer gradually to suppress graphene heat conduction membrane 3 step by step, thereby regulate and control the thickness size of graphene heat conduction membrane 3 step by step, graphene heat conduction membrane 3's thickness control is more accurate. Simultaneously, also do benefit to moisture and bubble in quick and the graphene thermal film 3 of just discharging effectively, ensure that graphene thermal film 3's heat conductivility is more excellent.
In the process of rolling the graphene thermal conductive film 3, the graphene thermal conductive film 3 is heated. Combine together through roll-in and drying, when the moisture in the quick discharge graphite alkene heat conduction membrane 3, can further compact graphite alkene heat conduction membrane 3 to obtain the graphite alkene heat conduction membrane 3 that the thermal conductivity is more excellent, graphite alkene heat conduction membrane 3's drying and compaction effect are better, and its each item performance is better. Specifically, the heat conductivity coefficient of the prepared graphene heat-conducting film 3 is 800-; the tensile strength is 20-50 MPa; the width of the graphene heat conduction film 3 is 500-800 mm; length 100-1000 m; bending test 20000 times or more (R5/180 °); the conductivity is 5 to 20 multiplied by 105S/cm.
And finally, rolling the graphene heat-conducting film 3 to continuously roll the graphene heat-conducting film 3.
According to the technical scheme, the method for preparing the graphene heat-conducting membrane 3 adopts a downward suction filtration mode, so that the graphene slurry can be quickly formed into a membrane and separated from the filter membrane, continuous and mass production of the graphene heat-conducting membrane 3 is realized, and the problem of limited width of graphene is solved. In addition, according to the method for preparing the graphene heat conduction film 3, the graphene heat conduction film 3 is dried in the rolling process, so that moisture and bubbles in the graphene heat conduction film 3 can be rapidly discharged, the heat conductivity of the graphene heat conduction film 3 can be improved, and the product quality of the graphene heat conduction film 3 is guaranteed.
Referring to fig. 1, in some embodiments, an air extractor 11 is connected to the bottom of the vacuum box 1, and the conveying assembly 2 includes a belt conveyor, a belt of the belt conveyor is provided with a plurality of spaced filtering holes (not shown), and a filter membrane is laid on the surface of the belt conveyor, so as to ensure that the air extractor 11 can act on the filter membrane when extracting air downwards, so as to realize a filtering function.
Further, graphite alkene thick liquids pass through 5 sprays to the surface of filter membrane of sprayer, before spraying graphite alkene thick liquids, mix graphite alkene thick liquids after, carry to 5 in the sprayer to the structure homogeneity when fully dispersing graphite alkene thick liquids not only improves graphite alkene thick liquids film-forming still does benefit to 5 sprayers and sprays, improve equipment's work efficiency and life.
Further, referring to fig. 1, the sprayer 5 is connected with a slurry mixing mechanism, the slurry mixing mechanism includes a disperser 61 and a homogenizer 62, the disperser 61 is communicated with the homogenizer 62 through a first pipeline 631, an outlet of the homogenizer 62 is connected to the sprayer 5 through a second pipeline 632, and a control valve 64 is disposed at the outlet of the homogenizer 62 so as to control the graphene slurry to flow into the sprayer 5. Through dispenser 61 and the cooperation work of isotropic symmetry 62, can carry out abundant dispersion work to graphite alkene thick liquids, do benefit to the quality that improves graphite alkene filming.
Referring to fig. 1, in some embodiments, a graphene slurry of the surface of the filter membrane is leveled using a slurry leveler, which includes a first leveler 71 and a second leveler 72. The second screed 72 is arranged between the first screed 71 and the vacuum box 1. The first leveling machine 71 includes a first leveling rod 711 extending in the left-right direction and a first translation driving unit (not shown) for driving the first leveling rod 711 to move in the front-back direction, so as to primarily level the surface of the graphene slurry by the first leveling rod 711, thereby facilitating the subsequent pressing work.
The second leveling machine 72 includes a lifting driving assembly (not shown), a second translation driving assembly (not shown), and a second leveling rod 721 extending in the left-right direction, the lifting driving assembly is configured to drive the second leveling rod 721 to move in the up-down direction, and the second translation driving assembly is configured to drive the second leveling rod 721 to move in the front-back direction, so as to adjust the height position of the second leveling rod 721, thereby primarily adjusting the thickness of the graphene slurry. The second translation driving assembly is configured to drive the second leveling rod 721 to move in the front-back direction, and after adjusting the height of the second leveling rod 721 to a proper position, the second leveling rod 721 may be further driven to compact the graphene slurry in the front-back direction.
It is understood that the first leveling machine 71 and the second leveling machine 72 can be directly disposed on the ground, and the first leveling rod 711 and the second leveling rod 721 are correspondingly driven to move by the manipulators; it is also possible to mount the first and second levelers 71, 72 at the frame of the transport mechanism where the conveyor assembly 2 is mounted, etc. It can also be understood that the first translation driving assembly, the lifting driving assembly and the second translation driving assembly may adopt a hydraulic cylinder, a linear motor or a rotary motor to drive the rack to reciprocate through a gear, and the like, and are not limited herein.
In some embodiments, the vacuum degree in the vacuum box 1 is-0.1 MPa, so as to achieve a good suction filtration effect, ensure a rapid film formation, and achieve a smooth separation of the graphene heat-conducting film 3 from the filter membrane.
It can be understood that the thickness of the graphene thermal conductive film 3 can be adjusted according to actual requirements, the number of the roller pressing shaft assemblies 4 and the roller spacing 43 of the roller pressing shaft assemblies 4. In some embodiments, referring to fig. 1, the graphene thermal conductive film 3 is introduced into three roller press shaft assemblies 4 for rolling, and the roller spacing 43 of the three roller press shaft assemblies 4 is, in order along the conveying direction of the graphene thermal conductive film 3: 100-200 μm, 80-100 μm, 50-80 μm to control the thickness of the graphene thermal conductive film 3 to be between 50-80 μm.
Further, the roller spindle assembly 4 is disposed in a drying room 8, and a passage 9 communicating with the drying room 8 and the vacuum box 1 is formed therebetween. The drying room 8 is provided with a drying system (not shown in the figure) for heating the graphene thermal conductive film 3. Because the inside of drying chamber 8 can form a relatively inclosed space, avoid exposing graphite alkene heat conduction membrane 3 outside, do benefit to rapid heating and stoving graphite alkene heat conduction membrane 3, improve production efficiency.
In some embodiments, the temperature of the drying system for heating the graphene thermal conductive film 3 is 100 ℃ to 200 ℃, and the temperature can avoid destructive influence on the graphene structure while ensuring the drying requirement of the graphene thermal conductive film 3, ensure the integrity of the graphene structure, and ensure the thermal conductivity and electrical conductivity of the graphene thermal conductive film 3. It is to be understood that the drying system includes a heat pump drying system, a hot air furnace, an electric heating dryer, or the like, and is not particularly limited herein.
Referring to fig. 1, still including motor (not shown in the figure) and wind-up roll 91, the output shaft of motor extends along left right direction to be connected with wind-up roll 91 transmission, wind-up roll 91 is used for automatic winding graphite alkene heat conduction membrane 3, in order to accomodate the graphite alkene heat conduction membrane 3 that prepares, ensures the clean and tidy of production site, and production efficiency is higher.
In the description herein, references to "an example," "an embodiment," or "some embodiments," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The invention is not limited to the above embodiments, and those skilled in the art can make equivalent modifications or substitutions without departing from the spirit of the invention, and such equivalent modifications or substitutions are included in the scope defined by the claims of the present application.
Claims (10)
1. A method for preparing a graphene thermal conductive film, comprising:
conveying the filter membrane from outside to a vacuum box;
before the filter membrane enters the vacuum box, spraying graphene slurry onto the surface of the filter membrane;
leveling graphene slurry on the surface of the filter membrane;
downwards pumping and filtering the filter membrane in the vacuum box to form a graphene heat conducting membrane;
introducing the graphene heat conduction film into a plurality of roller press shaft assemblies for rolling, wherein the roller spacing of the roller press shaft assemblies is gradually reduced along the transmission direction of the graphene heat conduction film;
heating the graphene heat conduction film in the process of rolling the graphene heat conduction film; and rolling the graphene heat conduction film.
2. The method for preparing the graphene thermal conductive film according to claim 1, wherein the graphene thermal conductive film is introduced into three roller press shaft assemblies for rolling, and the roller spacing of the three roller press shaft assemblies is sequentially as follows along the conveying direction of the graphene thermal conductive film: 100-200 μm, 80-100 μm, 50-80 μm.
3. The method for preparing the graphene thermal conductive film according to claim 1, wherein the roller shaft assembly is arranged in a drying room, and the drying room is provided with a drying system, and the drying system is used for heating the graphene thermal conductive film.
4. The method for preparing the graphene thermal conductive film according to claim 3, wherein the temperature of the drying system for heating the graphene thermal conductive film is 100-200 ℃.
5. The method for preparing the graphene thermal conductive film according to claim 1, wherein a degree of vacuum in the vacuum chamber is-0.1 MPa.
6. The method for preparing the graphene thermal conductive film according to claim 1, wherein the graphene slurry is sprayed onto the surface of the filter membrane through a sprayer, and before the graphene slurry is sprayed, the graphene slurry is mixed and then conveyed to the sprayer.
7. The method according to claim 6, wherein a slurry mixing mechanism is connected to the sprayer, the slurry mixing mechanism comprises a disperser and a homogenizer, the disperser is communicated with the homogenizer through a first pipeline, an outlet of the homogenizer is connected to the sprayer through a second pipeline, and a control valve is arranged at an outlet of the homogenizer.
8. The method of manufacturing a graphene thermal conductive film according to claim 1, wherein the graphene slurry on the surface of the filter membrane is leveled using a slurry leveling machine, the slurry leveling machine includes a first leveling machine and a second leveling machine, the second leveling machine is disposed between the first leveling machine and the vacuum box, the first leveling machine includes a first translation driving assembly and a first leveling rod extending in a left-right direction, the first translation driving assembly is configured to drive the first leveling rod to move in a front-rear direction, the second leveling machine includes a lift driving assembly, a second translation driving assembly, and a second leveling rod extending in a left-right direction, the lift driving assembly is configured to drive the second leveling rod to move in an up-down direction, and the second translation driving assembly is configured to drive the second leveling rod to move in a front-rear direction.
9. The method for preparing the graphene thermal conductive film according to claim 1, wherein the method comprises an air extractor and a belt conveyer, a belt of the belt conveyer is provided with a plurality of spaced filtering holes, the filter membrane is laid on the surface of the belt conveyer, and the air extractor is connected to the bottom of the vacuum box.
10. The method for preparing the graphene thermal conductive film according to claim 1, further comprising a motor and a winding roller, wherein an output shaft of the motor extends in a left-right direction and is in transmission connection with the winding roller, and the winding roller is used for winding the graphene thermal conductive film.
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|---|---|---|---|---|
| CN116969449A (en) * | 2023-09-22 | 2023-10-31 | 云南欣城防水科技有限公司 | Graphene calendaring equipment |
| CN116969449B (en) * | 2023-09-22 | 2023-12-08 | 云南欣城防水科技有限公司 | Graphene calendaring equipment |
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| Publication number | Publication date |
|---|---|
| CN114774087B (en) | 2023-07-04 |
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