CN113684464A - A coiling formula equipment for preparation of graphite alkene composite film - Google Patents
A coiling formula equipment for preparation of graphite alkene composite film Download PDFInfo
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- CN113684464A CN113684464A CN202110992659.XA CN202110992659A CN113684464A CN 113684464 A CN113684464 A CN 113684464A CN 202110992659 A CN202110992659 A CN 202110992659A CN 113684464 A CN113684464 A CN 113684464A
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/56—Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/54—Controlling or regulating the coating process
- C23C14/542—Controlling the film thickness or evaporation rate
- C23C14/545—Controlling the film thickness or evaporation rate using measurement on deposited material
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/56—Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks
- C23C14/564—Means for minimising impurities in the coating chamber such as dust, moisture, residual gases
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
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Abstract
The invention discloses winding equipment for preparing a graphene composite film, which mainly comprises a cavity, an evaporation module, a coating module and a pattern generating roller, wherein the evaporation module is arranged in the cavity; the evaporation module deposits a catalyst film layer on the surface of the flexible base film through vacuum evaporation coating. The coating module coats the graphene composite material on the catalyst film layer to form a coating layer; the coating layer is catalyzed and grown into a graphene composite wet film layer under the action of a catalyst below the coating layer. The pattern generation roller partially removes the unformed wet film layer on the flexible base film passing through the pattern generation roller through negative pressure absorption, so that the graphene composite film with the specific pattern is formed on the flexible base film. The pattern generating roller comprises an inner roller and an outer roller; the outer roller is provided with a mesh array; the inner roller is provided with an absorption hole array, and the absorption holes are connected with the meshes through absorption pipelines; the interior roller is inside to be the cavity structure, and the tip of interior roller links to each other with the low vacuum pump, and the low vacuum pump is with inside the taking out of interior roller become for the negative pressure of cavity internal gas pressure.
Description
Technical Field
The invention belongs to the technical field of graphene composite film preparation, and particularly relates to a winding type device for preparing a graphene composite film.
Background
The graphene serving as a novel nano material has higher specific surface area, strength, heat conduction and electric conduction performance than the traditional material. At present, adding graphene into the existing material to prepare a graphene composite material so as to improve the performance of the raw material becomes a hot spot of current research and application. Among a plurality of graphene composite materials, the graphene-silicon rubber composite material has excellent mechanical, thermal and electrical properties and has a good application prospect in the field of aerospace. The silicon rubber is an elastic polymer which takes Si-O-Si bonds as a main chain and organic groups as side chains and has inorganic and organic properties, free moving electrons are difficult to generate due to weak interaction force of molecular chains, the silicon rubber can be aged and decomposed at high temperature, the silicon rubber is low in strength and almost non-conductive, the tensile strength of the silicon rubber without reinforcement is only 0.3MPa, the common silicon rubber material can only be safely used within 260 ℃, and the application value is limited. In order to overcome the defects of the silicon rubber in strength and conductivity and further improve the high temperature resistance, a plurality of scientific researchers dope various graphene into the silicon rubber so as to improve the strength, heat resistance and conductivity of the silicon rubber and meet the harsh requirements of space exploration on the performance of the silicon rubber material.
However, the existing preparation process of the graphene-silicon rubber composite material is complex, still stays in a laboratory stage, and is difficult to realize industrialization. Particularly, the graphene-silicon rubber composite flexible film material proposed recently can be widely applied to more fields due to the characteristics of lightness, thinness, flexibility, changeability in shape and the like, but the popularization and application of the material are limited due to the fact that the industrialization technology of the graphene-silicon rubber composite flexible film material is blank.
Disclosure of Invention
The invention provides roll-to-roll graphene composite film preparation equipment, which meets the requirements of large-scale production equipment and technology of flexible graphene composite film materials represented by flexible graphene-silicon rubber composite films.
The invention provides winding equipment for preparing a graphene composite film, which mainly comprises a cavity, an evaporation module, a coating module, a shaping module and a winding system, wherein the evaporation module is arranged in the cavity; the winding system comprises an unwinding roller, a winding roller, an evaporation main roller and a pattern generation roller; the chamber is divided into an evaporation working area and a non-evaporation working area by a partition plate, and the evaporation module is arranged in the evaporation working area; the pattern generating roller is arranged between the coating module and the shaping module; the pattern generation roller partially removes the unformed wet film layer on the flexible base film passing through the pattern generation roller through negative pressure absorption, so that the graphene composite film with the specific pattern is formed on the flexible base film.
The chamber is provided with a vacuum system and an inflation system; the vacuum system is used for creating a clean vacuum environment in the chamber, and the inflation system is used for inflating the working gas. Before the graphene composite film is prepared, gas in the cavity is firstly pumped out through a vacuum system to enable the vacuum degree in the cavity to reach more than 10Pa (namely, the pressure reaches below 10 Pa), then working gas required for preparing the graphene composite film is introduced into a non-evaporation working area in the cavity through an inflation system, and the gas pressure of the non-evaporation working area in the cavity is controlled within the range of 0.01 MPa-0.1 MPa. The evaporation main roller is arranged across the evaporation working area and the non-evaporation working area, and the gap between the partition plate and the roller surface of the evaporation main roller is within the range of 1-5 mm. The chamber is also provided with a pressure gauge, a hygrometer and a thermometer for measuring environmental parameters.
The evaporation main roller is positioned at the downstream of the unwinding roller and at the upstream of the coating module; the evaporation module is positioned below the evaporation main roller and used for depositing a catalyst film layer on the surface of the flexible base film through vacuum evaporation coating.
The pattern generating roller is disposed downstream of the coating module. The pattern generating roller is a double-layer mechanism and comprises an inner roller and an outer roller; the surface of the outer roller is of a net structure, and a mesh array is arranged on the surface of the outer roller; the roller wall of the inner roller is provided with an absorption hole array, absorption holes in the absorption hole array are connected with meshes in the mesh array through absorption pipelines, and the absorption holes are in one-to-one correspondence with the meshes; the interior roller is inside to be the cavity structure, and the tip of interior roller links to each other with the low vacuum pump, and the low vacuum pump is with inside the taking out of interior roller become for the negative pressure of cavity internal gas pressure.
The inner side of the roller wall of the inner roller is provided with a covering cylinder slot; the shielding cylinder can be inserted into the slot of the shielding cylinder, and the unfolding shape of the shielding cylinder corresponds to a specific pattern of the graphene composite film to be formed on the flexible base film; the shielding cylinder shields and seals some absorption holes in the absorption hole array on the roller wall from the inner side of the roller wall of the inner roller; when the pattern generating roller works, the constant and stable negative pressure of the inner roller can generate negative pressure absorption on the wet film layer covered on the meshes from the uncovered absorption holes through the absorption pipelines and the meshes connected with the absorption holes, thereby removing the part of the wet film layer on the flexible base film wound by the pattern generating roller.
By controlling the exhaust speed of the roughing pump, the negative pressure absorption strength of the pattern generation roller to the wet film layer can be adjusted, and the part of the wet film layer covering the mesh is completely or partially removed.
In one embodiment, the pattern generating roll further comprises a controller; an electric control valve is arranged on the absorption pipeline; after the controller receives the pattern generation command, the electrically controlled valves on some absorption pipelines are opened according to a preset pattern generation program, and the negative pressure of the inner roller can generate negative pressure absorption on the wet film layer covered on the meshes from the absorption pipelines through the absorption holes and the meshes connected with the absorption pipelines, so that the part of the wet film layer on the flexible base film wound on the pattern generation roller is removed. The controller can independently adjust the opening of the electric control valves on some absorption pipelines to independently control the negative pressure absorption strength of the controlled meshes connected with the absorption pipelines to the wet film layer, so that the wet film layer covered on the controlled meshes is completely or partially removed. The controller respectively controls the negative pressure absorption strength of the wet film layer by the adjacent meshes, so that the trend of gradual change is formed between the negative pressure absorption strengths of the adjacent meshes, and the wet film layer covering the adjacent meshes forms a groove pattern with continuously and gradually changed depth. In addition, the controller can form patterns with different depths on a plurality of areas of the wet film layer by respectively controlling the negative pressure absorption strength of the meshes of the plurality of areas to the wet film layer.
The coating module coats the graphene composite material on a catalyst film layer on the surface of the flexible base film to form a coating layer; a growth roller is arranged at the downstream of the coating module; when the flexible base film winds the growth roller, the coating layer is catalyzed and grown into the graphene composite wet film layer under the action of the catalyst below the coating layer.
A film thickness monitoring device is arranged between the pattern generating roller and the shaping module and used for monitoring the thickness of the wet film layer on line; and the coating module performs dynamic feedback control on the supply amount of the graphene composite material according to the received film thickness monitoring signal, so that the film thickness of the graphene composite film is adjusted on line.
The coating module comprises a plurality of coating units arranged in the width direction of the flexible base film; the film thickness monitoring device carries out multi-point online film thickness monitoring on the wet film layer in the width direction of the flexible base film; the coating unit can carry out dynamic feedback control according to the film thickness monitoring signal on the region corresponding to the coating unit, and the film thickness of the graphene composite film on the region is adjusted on line.
The sizing module is located downstream of the pattern generating roll; the shaping module adopts illumination heating or drying box heating to dry and shape the wet film layer, so that the graphene composite film is formed on the wet film layer. The heating temperature range of the shaping module is 100-150 ℃. And a cooling roller is arranged at the downstream of the shaping module and used for cooling the graphene composite film subjected to heating and shaping.
A temperature control roller is arranged at the downstream of the evaporation main roller; the temperature control interval of the temperature control roller is 40-100 ℃; the temperature control roller adjusts the temperature of the flexible base film wound by the temperature control roller to be within the temperature range of catalytic reaction.
The downstream of the shaping module is provided with 2 laminating rollers which are oppositely arranged; a protective film roller is arranged in the cavity. The laminating roller is used for pressing the protective film from the protective film roller to cover the surface of the shaped graphene composite film, so as to protect the surface of the graphene composite film on the flexible base film and prevent the graphene composite film from being damaged in the rolling and transporting processes; the protective film is preferably a thermal release tape. Destaticizing devices are provided both upstream and downstream of the laminating roller. Preferably, the laminating rollers are provided with a pressure sensor and a pressure controller for measuring the pressure between the laminating rollers, the pressure between the laminating rollers can be monitored and adjusted in real time through the feedback of the pressure sensor, and the protective film is prevented from being damaged when being pressed on the surface of the graphene composite film.
The working process of the winding type equipment for preparing the graphene composite film mainly comprises the following steps:
(1) starting an evaporation module to perform vacuum evaporation coating, and depositing a catalyst film layer on the surface of the flexible base film wound by the evaporation main roller; starting a coating module at the downstream of the evaporation module, and coating the graphene composite material on a catalyst film layer on the surface of the flexible base film by the coating module to form a coating layer; a growth roller is arranged at the downstream of the coating module; when the flexible base film passes through the growth roller, the coating layer is catalyzed and grown into a graphene composite wet film layer under the action of a catalyst below the coating layer;
(2) the pattern generating roller arranged at the downstream of the growth roller partially removes the unformed wet film layer on the flexible base film wound on the roller body through a negative pressure absorption process, so that the wet film layer generates a set pattern;
(3) heating, drying and shaping the wet film layer through a shaping module arranged at the downstream of the pattern generating roller to form a graphene composite film on the wet film layer; the shaping module adopts illumination heating or drying box heating; the formed graphene composite film has a specific pattern.
Before the evaporation module is started, the chamber is vacuumized through a vacuum system, when the vacuum degree in the chamber reaches a set value, working gas is filled into the non-evaporation working area through an inflation system, and the gas pressure of the non-evaporation working area is controlled within the range of 0.01 MPa-0.1 MPa.
A film thickness monitoring device is arranged at the downstream of the pattern generating roller and used for carrying out online film thickness monitoring on the wet film layer; and the coating module performs dynamic feedback control on the supply amount of the graphene composite material according to the received film thickness monitoring signal, so that the film thickness of the graphene composite film is adjusted on line. The film thickness monitoring device carries out multi-point online film thickness monitoring on the wet film layer in the width direction of the flexible base film; the coating unit can carry out dynamic feedback control according to the film thickness monitoring signal on the region corresponding to the coating unit, and the film thickness of the graphene composite film on the region is adjusted on line.
The invention has the beneficial effects that:
the winding type equipment provided by the invention provides a clean environment for preparing the graphene composite film by vacuumizing the closed chamber and then charging working gas. The method comprises the steps of firstly depositing a catalyst layer required by growth of a graphene composite material on a flexible substrate through vacuum evaporation coating, enabling the graphene composite material coated on the catalyst layer to grow into a wet film layer, enabling the wet film layer to generate a set pattern through a negative pressure absorption process of a pattern generation roller, and heating, drying and shaping the wet film layer through a shaping module to finally obtain the graphene composite flexible film with the specific pattern. The device can realize large-scale batch production of the graphene composite flexible film represented by the graphene-silicon rubber composite film. The flexible film has excellent heat resistance, high strength, excellent electromagnetic shielding property and specific patterns, so that the product can meet the application requirements of certain special occasions.
Drawings
FIG. 1 is a schematic diagram of the construction of one embodiment of the roll-to-roll apparatus of the present invention;
FIG. 2 is a schematic structural view of one embodiment of a pattern generating roll in the present invention;
fig. 3 is a schematic structural view of another embodiment of the pattern generating roller in the present invention.
Detailed Description
The following further describes the embodiments of the present invention with reference to the drawings. It should be understood that the detailed description and specific examples, while indicating the present invention, are intended for purposes of illustration and explanation only and are not intended to limit the scope of the invention.
Fig. 1 is a schematic structural diagram of an embodiment of a roll-to-roll apparatus according to the present invention, and as shown in the drawing, the present invention provides a roll-to-roll apparatus for graphene composite film preparation, which mainly includes a chamber 1, an evaporation module 2, a coating module 3, a shaping module 4, and a roll-to-roll system; the winding system comprises an unwinding roller 5, a winding roller 6, an evaporation main roller 7 and a pattern generating roller 8; the chamber 1 is divided into an evaporation working area 10 and a non-evaporation working area 11 by a partition plate 9, and the evaporation module 2 is arranged in the evaporation working area 10; the pattern generating roller 8 is disposed between the coating module 3 and the sizing module 4; the pattern generating roller 8 partially removes an unformed wet film layer on the flexible base film passing around the pattern generating roller 8 by negative pressure absorption, thereby forming a graphene composite film having a specific pattern on the flexible base film.
The chamber 1 is provided with a vacuum system 12 and an inflation system 13; the vacuum system 12 is used to create a clean vacuum environment within the chamber 1 and the inflation system is used to inflate the working gas. Before the graphene composite film is prepared, gas in the chamber 1 is firstly pumped out through the vacuum system 12 to enable the vacuum degree in the chamber to reach more than 10Pa (namely, the pressure reaches below 10 Pa), then working gas required for preparing the graphene composite film is introduced into the non-evaporation working area 11 in the chamber through the inflation system 13, and the gas pressure of the non-evaporation working area 11 in the chamber is controlled within the range of 0.01 MPa-0.1 MPa. The evaporation main roller 7 spans the evaporation working area and the non-evaporation working area, and the gap between the partition plate 9 and the roller surface of the evaporation main roller 7 is within the range of 1-5 mm. The chamber 1 is also provided with a pressure gauge, a hygrometer and a thermometer for measuring environmental parameters.
The evaporation main roller 7 is located downstream of the unwinding roller 5 and upstream of the coating module 3; the evaporation module 2 is positioned below the evaporation main roller 7 and used for depositing a catalyst film layer on the surface of the flexible base film through vacuum evaporation coating.
The coating module 3 coats the graphene composite material on the catalyst film layer on the surface of the flexible base film to form a coating layer; a growth roller 22 is arranged downstream of the coating module 3; when the flexible base film passes around the growth roller 22, the coating layer is catalytically grown into a graphene composite wet film layer under the action of the catalyst below the coating layer.
A film thickness monitoring device 23 is arranged between the pattern generating roller 8 and the shaping module 4, and the film thickness monitoring device 23 carries out online film thickness monitoring on the wet film layer; and the coating module 3 performs dynamic feedback control on the supply amount of the graphene composite material according to the received film thickness monitoring signal, so that the film thickness of the graphene composite film is adjusted on line.
The coating module 3 includes a plurality of coating units arranged in the width direction of the flexible base film; the film thickness monitoring device 23 carries out multi-point online film thickness monitoring on the wet film layer in the width direction of the flexible base film; the coating unit can carry out dynamic feedback control according to the film thickness monitoring signal on the region corresponding to the coating unit, and the film thickness of the graphene composite film on the region is adjusted on line.
The sizing module 4 is located downstream of the pattern generating roller 8; the shaping module 4 adopts illumination heating or drying box heating to dry and shape the wet film layer, so that the graphene composite film is formed on the wet film layer. The heating temperature range of the shaping module 4 is 100-150 ℃. And a cooling roller 24 is arranged at the downstream of the shaping module 4, and the cooling roller 24 cools the graphene composite film after heating and shaping.
A temperature-controlled roll 25 is arranged downstream of the evaporation main roll 7; the temperature control interval of the temperature control roller 25 is 40-100 ℃; the temperature control roller 25 adjusts the temperature of the flexible base film wound around the temperature control roller to be within the catalytic reaction temperature range.
The downstream of the shaping module 4 is provided with 2 laminating rollers 26 which are oppositely arranged; a protective film roll 27 is provided in the chamber 1. The laminating roller is used for pressing the protective film from the protective film roller to cover the surface of the shaped graphene composite film, so as to protect the surface of the graphene composite film on the flexible base film and prevent the graphene composite film from being damaged in the rolling and transporting processes; the protective film is preferably a thermal release tape. Destaticizing devices are provided both upstream and downstream of the laminating roller. Preferably, the laminating rollers are provided with a pressure sensor and a pressure controller for measuring the pressure between the laminating rollers, the pressure between the laminating rollers can be monitored and adjusted in real time through the feedback of the pressure sensor, and the protective film is prevented from being damaged when being pressed on the surface of the graphene composite film.
A pattern generating roller 8 is disposed downstream of the coating module 3. FIG. 2 is a schematic structural view of one embodiment of the pattern generating roll of the present invention, and as shown, the pattern generating roll 8 is a double-layered structure including an inner roll 14 and an outer roll 15; the surface of the outer roller 15 is of a net structure, and a mesh array is arranged on the surface; an absorption hole array is arranged on the roller wall of the inner roller 14, and absorption holes 16 in the absorption hole array are connected with meshes 17 in the mesh array through absorption pipelines 18; the inner roller 14 is internally provided with a cavity structure, the end part of the inner roller 14 is connected with a low vacuum pump 19, and the low vacuum pump 19 pumps the inside of the inner roller 14 into negative pressure relative to the air pressure in the cavity.
The inner side of the roller wall of the inner roller 14 is provided with a covering cylinder slot; the shielding cylinder 20 can be inserted into the slot of the shielding cylinder, and the unfolded shape of the shielding cylinder 20 corresponds to a specific pattern of the graphene composite film to be formed on the flexible base film; the shielding cylinder 20 shields and seals some absorption holes in the absorption hole array on the roller wall from the inner side of the roller wall of the inner roller; when the pattern generating roller 8 is in operation, the constant and stable negative pressure of the inner roller can generate negative pressure absorption on the wet film layer covered on the meshes from the uncovered absorption holes through the absorption pipes and the meshes connected with the absorption holes, thereby removing the part of the wet film layer on the flexible base film wound on the pattern generating roller.
By controlling the exhaust speed of the roughing pump 19, the negative pressure absorption force of the pattern generating roller to the wet film layer can be adjusted, and the part of the wet film layer covering the mesh is completely or partially removed.
Fig. 3 is a schematic structural view of another embodiment of the pattern generating roller in the present invention. As shown, in this embodiment, the pattern generating roller 8 further comprises a controller; an electric control valve 21 is arranged on the absorption pipeline 18; after the controller receives the pattern generation instruction, the electronic control valves on some absorption pipelines are opened according to a preset pattern generation program, the negative pressure of the inner roller can generate negative pressure absorption on the wet film layer covered on the meshes from the absorption pipelines through the absorption holes and the meshes connected with the absorption pipelines, and therefore the wet film layer on the flexible base film wound on the roller body is removed. The controller can independently adjust the opening of the electric control valves on some absorption pipelines to independently control the negative pressure absorption strength of the controlled meshes connected with the absorption pipelines to the wet film layer, so that the wet film layer covered on the controlled meshes is completely or partially removed. The controller respectively controls the negative pressure absorption strength of the wet film layer by the adjacent meshes, so that the trend of gradual change is formed between the negative pressure absorption strengths of the adjacent meshes, and the wet film layer covering the adjacent meshes forms a groove pattern with continuously and gradually changed depth. In addition, the controller can form patterns with different depths on a plurality of areas of the wet film layer by respectively controlling the negative pressure absorption strength of the meshes of the plurality of areas to the wet film layer.
The working process of the winding type equipment for preparing the graphene composite film mainly comprises the following steps:
(1) starting an evaporation module to perform vacuum evaporation coating, and depositing a catalyst film layer on the surface of the flexible base film wound by the evaporation main roller; starting a coating module at the downstream of the evaporation module, and coating the graphene composite material on a catalyst film layer on the surface of the flexible base film by the coating module to form a coating layer; a growth roller is arranged at the downstream of the coating module; when the flexible base film passes through the growth roller, the coating layer is catalyzed and grown into a graphene composite wet film layer under the action of a catalyst below the coating layer;
(2) the pattern generating roller arranged at the downstream of the growth roller partially removes the unformed wet film layer on the flexible base film wound on the roller body through a negative pressure absorption process, so that the wet film layer generates a set pattern;
(3) heating, drying and shaping the wet film layer through a shaping module arranged at the downstream of the pattern generating roller to form a graphene composite film on the wet film layer; the shaping module adopts illumination heating or drying box heating; the formed graphene composite film has a specific pattern.
Before the evaporation module is started, the chamber is vacuumized through a vacuum system, when the vacuum degree in the chamber reaches a set value, working gas is filled into the non-evaporation working area through an inflation system, and the gas pressure of the non-evaporation working area is controlled within the range of 0.01 MPa-0.1 MPa.
A film thickness monitoring device is arranged at the downstream of the pattern generating roller and used for carrying out online film thickness monitoring on the wet film layer; and the coating module performs dynamic feedback control on the supply amount of the graphene composite material according to the received film thickness monitoring signal, so that the film thickness of the graphene composite film is adjusted on line. The film thickness monitoring device carries out multi-point online film thickness monitoring on the wet film layer in the width direction of the flexible base film; the coating unit can carry out dynamic feedback control according to the film thickness monitoring signal on the region corresponding to the coating unit, and the film thickness of the graphene composite film on the region is adjusted on line.
Claims (10)
1. A winding type device for preparing a graphene composite film mainly comprises a cavity, an evaporation module, a coating module, a shaping module and a winding system; the winding system comprises an unwinding roller, a winding roller, an evaporation main roller and a pattern generation roller; the chamber is divided into an evaporation working area and a non-evaporation working area by a partition plate, and the evaporation module is arranged in the evaporation working area; the pattern generating roller is arranged between the coating module and the shaping module; the pattern generation roller partially removes the unformed wet film layer on the flexible base film passing through the pattern generation roller through negative pressure absorption, so that the graphene composite film with the specific pattern is formed on the flexible base film.
2. The roll-to-roll apparatus for graphene composite film preparation according to claim 1, wherein: the evaporation main roller is positioned at the downstream of the unwinding roller and at the upstream of the coating module; the evaporation module is positioned below the evaporation main roller and used for depositing a catalyst film layer on the surface of the flexible base film through vacuum evaporation coating.
3. The roll-to-roll apparatus for graphene composite film preparation according to claim 1, wherein: the pattern generating roller is a double-layer mechanism and comprises an inner roller and an outer roller; the surface of the outer roller is of a net structure, and a mesh array is arranged on the surface of the outer roller; the roller wall of the inner roller is provided with an absorption hole array, and absorption holes in the absorption hole array are connected with meshes in the mesh array through absorption pipelines; the interior roller is inside to be the cavity structure, and the tip of interior roller links to each other with the low vacuum pump, and the low vacuum pump is with inside the taking out of interior roller become for the negative pressure of cavity internal gas pressure.
4. The roll-to-roll apparatus for graphene composite film preparation according to claim 3, wherein: the inner side of the roller wall of the inner roller is provided with a covering cylinder slot; the shielding cylinder can be inserted into the slot of the shielding cylinder, and the unfolding shape of the shielding cylinder corresponds to a specific pattern of the graphene composite film to be formed on the flexible base film; the shielding cylinder shields and seals some absorption holes in the absorption hole array on the roller wall from the inner side of the roller wall of the inner roller; when the pattern generating roller works, the negative pressure of the inner roller can generate negative pressure absorption on the wet film layer covered on the meshes from the unblocked absorption holes through the absorption pipes and the meshes connected with the unblocked absorption holes, so that the part of the wet film layer on the flexible base film wound around the pattern generating roller is removed.
5. The roll-to-roll apparatus for graphene composite film preparation according to claim 4, wherein: by controlling the exhaust speed of the roughing pump, the negative pressure absorption strength of the pattern generation roller to the wet film layer can be adjusted, and the part of the wet film layer covering the mesh is completely or partially removed.
6. The roll-to-roll apparatus for graphene composite film preparation according to claim 2, wherein: the coating module coats the graphene composite material on a catalyst film layer on the surface of the flexible base film to form a coating layer; a growth roller is arranged at the downstream of the coating module; when the flexible base film winds the growth roller, the coating layer is catalyzed and grown into the graphene composite wet film layer under the action of the catalyst below the coating layer.
7. The roll-to-roll apparatus for graphene composite film preparation according to claim 6, wherein: a film thickness monitoring device is arranged between the pattern generating roller and the shaping module and used for monitoring the thickness of the wet film layer on line; and the coating module performs dynamic feedback control on the supply amount of the graphene composite material according to the received film thickness monitoring signal, so that the film thickness of the graphene composite film is adjusted on line.
8. The roll-to-roll apparatus for graphene composite film preparation according to claim 7, wherein: the coating module comprises a plurality of coating units arranged in the width direction of the flexible base film; the film thickness monitoring device carries out multi-point online film thickness monitoring on the wet film layer in the width direction of the flexible base film; the coating unit can carry out dynamic feedback control according to the film thickness monitoring signal on the region corresponding to the coating unit, and the film thickness of the graphene composite film on the region is adjusted on line.
9. The roll-to-roll apparatus for graphene composite film preparation according to claim 1, wherein: the sizing module is located downstream of the pattern generating roll; the shaping module adopts illumination heating or drying box heating to dry and shape the wet film layer, so that the graphene composite film is formed on the wet film layer.
10. The roll-to-roll apparatus for graphene composite film preparation according to claim 2, wherein: a temperature control roller is arranged at the downstream of the evaporation main roller; the temperature control interval of the temperature control roller is 40-100 ℃; the temperature control roller adjusts the temperature of the flexible base film wound by the temperature control roller to be within the temperature range of catalytic reaction.
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Citations (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1148099A (en) * | 1995-07-28 | 1997-04-23 | 莱博德股份公司 | Method and equipment for mfg. belt contg. no metal during film-making process of metal evaporation |
| CN1732284A (en) * | 2002-12-26 | 2006-02-08 | 凸版印刷株式会社 | Vacuum deposition apparatus and method of producing vapor-deposited film |
| CN101484608A (en) * | 2006-06-23 | 2009-07-15 | 株式会社爱发科 | Take up type vacuum vapor deposition device |
| CN101501239A (en) * | 2006-10-06 | 2009-08-05 | 株式会社爱发科 | Takeup type vacuum filming apparatus |
| CN101542008A (en) * | 2007-03-09 | 2009-09-23 | 松下电器产业株式会社 | Deposition apparatus and method for manufacturing film by using deposition apparatus |
| CN201495277U (en) * | 2009-06-22 | 2010-06-02 | 杭州晶鑫镀膜包装有限公司 | Vacuum winding type aluminum film coating device |
| RU2449050C1 (en) * | 2008-04-14 | 2012-04-27 | Улвак, Инк. | Winding-type vacuum deposition plant |
| EP2508646A1 (en) * | 2011-04-05 | 2012-10-10 | Bayer Material Science AG | A process for multi-layer continuous roll-to-roll coating |
| JP5058396B1 (en) * | 2011-03-11 | 2012-10-24 | パナソニック株式会社 | Thin film manufacturing method and manufacturing apparatus |
| CN102976318A (en) * | 2012-12-21 | 2013-03-20 | 重庆绿色智能技术研究院 | Reel-to-reel graphene preparation apparatus |
| CN203080288U (en) * | 2012-12-18 | 2013-07-24 | 连云港春江机械有限公司 | Negative pressure pattern cutting device |
| KR20150041377A (en) * | 2013-10-08 | 2015-04-16 | 송보경 | a chemical vapor deposition for flexible film |
| CN104608370A (en) * | 2015-02-09 | 2015-05-13 | 上海交通大学 | Roll-to-roll based UV cured polymer film surface microstructure processing system and method |
| CN105970158A (en) * | 2016-06-27 | 2016-09-28 | 安徽赛福电子有限公司 | Evaporation technology of metalized safety thin film of capacitor |
| CN107415329A (en) * | 2017-09-25 | 2017-12-01 | 绥阳县双龙纸业有限公司 | A kind of embossing method for papermaking |
| CN108933048A (en) * | 2018-07-18 | 2018-12-04 | 广东迈特斐薄膜科技有限公司 | The manufacturing equipment and its manufacturing process of low-power consumption capacitor metalized film |
| CN110904426A (en) * | 2019-12-24 | 2020-03-24 | 苏州昆岭薄膜工业有限公司 | Production equipment and production method of aluminized 8-micron nylon film |
| CN112725760A (en) * | 2021-02-07 | 2021-04-30 | 厦门海辰新材料科技有限公司 | Evaporation coating equipment and coating method of substrate |
| CN112813400A (en) * | 2021-03-31 | 2021-05-18 | 辽宁分子流科技有限公司 | Double-sided multi-station winding type vacuum coating machine |
-
2021
- 2021-08-27 CN CN202110992659.XA patent/CN113684464B/en active Active
Patent Citations (20)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1148099A (en) * | 1995-07-28 | 1997-04-23 | 莱博德股份公司 | Method and equipment for mfg. belt contg. no metal during film-making process of metal evaporation |
| CN1732284A (en) * | 2002-12-26 | 2006-02-08 | 凸版印刷株式会社 | Vacuum deposition apparatus and method of producing vapor-deposited film |
| CN101484608A (en) * | 2006-06-23 | 2009-07-15 | 株式会社爱发科 | Take up type vacuum vapor deposition device |
| CN101501239A (en) * | 2006-10-06 | 2009-08-05 | 株式会社爱发科 | Takeup type vacuum filming apparatus |
| CN101542008A (en) * | 2007-03-09 | 2009-09-23 | 松下电器产业株式会社 | Deposition apparatus and method for manufacturing film by using deposition apparatus |
| RU2449050C1 (en) * | 2008-04-14 | 2012-04-27 | Улвак, Инк. | Winding-type vacuum deposition plant |
| CN201495277U (en) * | 2009-06-22 | 2010-06-02 | 杭州晶鑫镀膜包装有限公司 | Vacuum winding type aluminum film coating device |
| JP5058396B1 (en) * | 2011-03-11 | 2012-10-24 | パナソニック株式会社 | Thin film manufacturing method and manufacturing apparatus |
| CN103392025A (en) * | 2011-03-11 | 2013-11-13 | 松下电器产业株式会社 | Thin-film production method and production device |
| EP2508646A1 (en) * | 2011-04-05 | 2012-10-10 | Bayer Material Science AG | A process for multi-layer continuous roll-to-roll coating |
| CN203080288U (en) * | 2012-12-18 | 2013-07-24 | 连云港春江机械有限公司 | Negative pressure pattern cutting device |
| CN102976318A (en) * | 2012-12-21 | 2013-03-20 | 重庆绿色智能技术研究院 | Reel-to-reel graphene preparation apparatus |
| KR20150041377A (en) * | 2013-10-08 | 2015-04-16 | 송보경 | a chemical vapor deposition for flexible film |
| CN104608370A (en) * | 2015-02-09 | 2015-05-13 | 上海交通大学 | Roll-to-roll based UV cured polymer film surface microstructure processing system and method |
| CN105970158A (en) * | 2016-06-27 | 2016-09-28 | 安徽赛福电子有限公司 | Evaporation technology of metalized safety thin film of capacitor |
| CN107415329A (en) * | 2017-09-25 | 2017-12-01 | 绥阳县双龙纸业有限公司 | A kind of embossing method for papermaking |
| CN108933048A (en) * | 2018-07-18 | 2018-12-04 | 广东迈特斐薄膜科技有限公司 | The manufacturing equipment and its manufacturing process of low-power consumption capacitor metalized film |
| CN110904426A (en) * | 2019-12-24 | 2020-03-24 | 苏州昆岭薄膜工业有限公司 | Production equipment and production method of aluminized 8-micron nylon film |
| CN112725760A (en) * | 2021-02-07 | 2021-04-30 | 厦门海辰新材料科技有限公司 | Evaporation coating equipment and coating method of substrate |
| CN112813400A (en) * | 2021-03-31 | 2021-05-18 | 辽宁分子流科技有限公司 | Double-sided multi-station winding type vacuum coating machine |
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