CN112804775A - Method for preparing electrothermal film by adopting transparent graphene - Google Patents
Method for preparing electrothermal film by adopting transparent graphene Download PDFInfo
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- CN112804775A CN112804775A CN202110060717.5A CN202110060717A CN112804775A CN 112804775 A CN112804775 A CN 112804775A CN 202110060717 A CN202110060717 A CN 202110060717A CN 112804775 A CN112804775 A CN 112804775A
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/20—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater
- H05B3/34—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater flexible, e.g. heating nets or webs
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B1/00—Details of electric heating devices
- H05B1/02—Automatic switching arrangements specially adapted to apparatus ; Control of heating devices
- H05B1/0202—Switches
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B1/00—Details of electric heating devices
- H05B1/02—Automatic switching arrangements specially adapted to apparatus ; Control of heating devices
- H05B1/0227—Applications
- H05B1/0288—Applications for non specified applications
- H05B1/0294—Planar elements
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/0019—Circuit arrangements
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/02—Details
- H05B3/03—Electrodes
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Abstract
The invention discloses a method for preparing an electrothermal film by adopting transparent graphene, which comprises the following steps: s1: transferring a graphene film on the surface of a flexible substrate; s2: printing a silver paste electrode on the surface of the graphene film to obtain a composite structural member of a flexible substrate, the graphene film and the electrode; s3: taking a flexible packaging film, forming a PTC or NTC thermosensitive film monitoring circuit on the surface of the packaging film by adopting a vacuum coating process, and covering a layer of OCA glue on the surface of the PTC or NTC thermosensitive film monitoring circuit to obtain a PI-PTC/NTC layer-OCA glue structural component; s4: and (3) attaching and baking the composite structural member of the flexible substrate-graphene film-electrode prepared by S2 and the PI-PTC/NTC layer-OCA adhesive structural component prepared by S3 to obtain the flexible substrate-graphene film-electrode-OCA adhesive-PTC/NTC layer-flexible packaging film structure.
Description
Technical Field
The invention relates to the field of electrothermal film preparation, in particular to a preparation method for obtaining a flexible electrothermal film with a thermal protection function by arranging a thermal resistance layer.
Background
In recent years, with the development of consumer upgrading and health industry, various flexible heating application products (such as heating clothes, heating protective clothing and the like) are continuously pushed out in the market, and particularly, graphene far infrared health physiotherapy products are rapidly developed and accepted by consumers. The graphene far infrared health physiotherapy product can emit far infrared light waves, the wavelength range mainly falls in a range of 6-14 microns, far infrared rays in the range are easily absorbed by a human body, and the far infrared light waves are called life light waves and are particularly valued by consumers. In addition, various graphene flexible electric heating film products for floor heating are also greatly developed.
Currently, the flexible graphene far infrared health physiotherapy product adopts a graphene flexible electric heating film as an electric heating element. However, current graphene flexible conductive films, such as PU-based graphene polymeric (self-supporting) conductive films, CVD graphene conductive films, generally do not have a self-limiting temperature (PTC) effect. The self-limiting temperature PTC effect means that after the temperature of the electric heating film exceeds a certain temperature, the resistance of the electric heating film is sharply increased, so that the heating power is reduced, the heating temperature automatically falls back, and after the temperature is lower than the certain temperature, the electric heating film can restore to normally work, so that the working safety of the electric heating film is greatly improved. At present, a common flexible electric heating film temperature control system generally adopts a thermistor (temperature sensor) adhered to the surface of an electric heating film to monitor the temperature of the electric heating film and realize temperature control. However, the thermistor (temperature sensor, using PTC or NTC effect) has a small size, only a small area can be monitored, the temperature of the surface of the electrothermal film cannot be monitored in a large range, and once the temperature of the electrothermal film is out of control, potential safety hazards and defects exist.
The statements in the background section are merely prior art as they are known to the inventors and do not, of course, represent prior art in the field.
Disclosure of Invention
Aiming at one or more problems in the prior art, the invention provides a method for preparing an electrothermal film by adopting transparent graphene, which comprises the following steps:
s1: transferring a graphene film on the surface of a flexible substrate;
s2: printing a silver paste electrode on the surface of the graphene film to obtain a composite structural member of a flexible substrate, the graphene film and the electrode;
s3: taking a flexible packaging film, forming a PTC or NTC thermosensitive film monitoring circuit on the surface of the packaging film by adopting a vacuum coating process, and covering a layer of OCA glue on the surface of the PTC or NTC thermosensitive film monitoring circuit to obtain a PI-PTC/NTC layer-OCA glue structural component;
s4: and (3) attaching and baking the composite structural member of the flexible substrate-graphene film-electrode prepared by S2 and the PI-PTC/NTC layer-OCA adhesive structural component prepared by S3 to obtain the flexible substrate-graphene film-electrode-OCA adhesive-PTC/NTC layer-flexible packaging film structure.
According to an aspect of the present invention, in S1, the flexible substrate surface is transferred with 1-10 graphene thin films.
According to an aspect of the present invention, in S1, the flexible substrate surface is transferred with 2 graphene films.
According to an aspect of the present invention, in S3, the specific method for forming the PTC or NTC thermosensitive thin film monitoring circuit on the surface of the flexible packaging film by using the vacuum coating process is:
a) coating photoresist on the surface of the flexible packaging film, or pressing a photosensitive dry film, and then obtaining patterned photoresist or dry film through exposure and development processes;
b) obtaining a PTC or NTC heat-sensitive film layer on the surface of a flexible packaging substrate with a patterned photoresist or dry film on the surface by a sputtering method or a vacuum evaporation method;
c) removing the photoresist or the dry film to obtain a PTC or NTC heat-sensitive film patterned electrode;
d) one side of the flexible packaging substrate PTC circuit is provided with a layer of optical transparent adhesive, and the transparent adhesive can adopt a mode of coating liquid optical transparent adhesive (LOCA) or directly attaching semi-cured optical transparent adhesive (OCA).
According to one aspect of the invention, the PTC or NTC circuit is of U-shaped configuration.
According to one aspect of the invention, the U-shaped configuration PTC or NTC circuit is a porous continuous wire.
According to one aspect of the invention, the layer of OCA glue is applied in the form of Liquid Optical Clear Adhesive (LOCA) or directly attached to semi-cured Optical Clear Adhesive (OCA).
According to an aspect of the present invention, in the step S4, the baking temperature is 120-180 ℃, and the baking time is 10-50 minutes.
According to an aspect of the present invention, in the S4, the baking temperature is 140 ℃ and the baking time is 30 minutes.
According to an aspect of the present invention, in S4, before the flexible substrate-graphene film-electrode composite structure prepared in S2 is attached to the PI-PTC layer-OCA paste structure assembly prepared in S3, an electrothermal film heating layer connection terminal and a PTC connection terminal exposure hole are previously provided.
In the step c), in order to ensure that the CVD graphene electrothermal film has higher optical transmittance and reduce the shielding of the PTC or NTC thermosensitive film pattern on far infrared light of the heating layer, the PTC or NTC thermosensitive film pattern can adopt a high-transmittance design.
According to the preparation method of the graphene electrothermal film, the PTC/NTC circuit is implanted into the surface of the flexible electrothermal film packaging material to monitor the surface temperature of the electrothermal film in a large range, so that the temperature of the electrothermal film can be effectively prevented from being out of control, and the use safety of the electrothermal film is improved; in addition, the PTC/NTC circuit pattern is prepared on the surface of the packaging material, the PTC/NTC material has good adhesion with the base material, the PTC/NTC and the heating layer material can be isolated, and the defects that the PTC/NTC circuit is directly arranged on the surface of the heating layer, the PTC/NTC circuit is easy to fall off, the bending resistance is poor and the like are avoided.
In order to ensure the permeability of the CVD graphene electrothermal film and reduce the shielding of the PTC/NTC circuit patterns on far infrared light of the heating layer, the U-shaped PTC/NTC circuit can be arranged into a porous continuous wire structure. The product manufactured by the method is connected with a temperature controller outside the electric heating film by monitoring the PTC/NTC circuit resistor as a temperature sensor, when local temperature is overhigh, the resistance of the port of the PTC/NTC circuit is changed violently, and the temperature controller executes an instruction of cutting off the power supply of the heating layer, so that the heating film is ensured to be cut off rapidly, and the use safety is ensured. After the PTC/NTC circuit resistor recovers to the original value, the temperature controller executes an instruction of switching on the graphene heating layer power supply, so that the monitoring and the safety control of the abnormal temperature of the electric heating film can be effectively realized.
According to the invention, the PTC/NTC monitoring circuit with the U-shaped curve layout is obtained on the inner surface of the flexible electric heating film packaging substrate by a vacuum coating method, so that the heating surface of the graphene electric heating film can be monitored in a large area, the problem of thermal runaway is prevented, and the use safety of the electric heating film is favorably improved. The PTC/NTC circuit is isolated from the conductive film of the heating layer by OCA glue, so that the generation of crosstalk between the resistors of the PTC/NTC circuit and the conductive film of the heating layer and the damage to the conductive film in the preparation process of the PTC/NTC circuit can be prevented.
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 description is to be regarded as illustrative in nature and not as restrictive.
In the description of the present invention, it is to be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "straight", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", and the like, indicate orientations and positional relationships based on those shown, and are used merely for convenience of description and simplicity of description, but do not indicate or imply that the device or element so referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus should not be construed as limiting the present invention. Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, features defined as "first", "second", may explicitly or implicitly include one or more of the described features. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
In the description of the present invention, it should be noted that unless otherwise explicitly stated or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection, either mechanically, electrically, or in communication with each other; either directly or indirectly through intervening media, either internally or in any other relationship. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
In the present invention, unless otherwise expressly stated or limited, "above" or "below" a first feature means that the first and second features are in direct contact, or that the first and second features are not in direct contact but are in contact with each other via another feature therebetween. Also, the first feature being "on," "above" and "over" the second feature includes the first feature being directly on and obliquely above the second feature, or merely indicating that the first feature is at a higher level than the second feature. A first feature being "under," "below," and "beneath" a second feature includes the first feature being directly above and obliquely above the second feature, or simply meaning that the first feature is at a lesser level than the second feature.
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.
While the preferred embodiments of the present invention will be described below, it should be understood that the preferred embodiments described herein are merely illustrative and explanatory of the invention and are not restrictive thereof.
Example 1:
a method for preparing an electrothermal film by adopting transparent graphene specifically comprises the following steps:
1) selecting a transparent PET film with the thickness of 50 microns, transferring 2 layers of graphene films on the surface of the transparent PET film, wherein the sheet resistance of the film is 150 ohm/sq; in addition, preparing an NTC circuit wiring terminal exposure hole on the edge of the PET by adopting a laser cutting process;
2) printing conductive silver paste on the surface of the graphene to form an electric heating film heating layer electrode;
3) selecting a 50-micron-thick PET packaging substrate, and laminating and covering a 20-micron-thick photosensitive dry film on the surface of the PET packaging substrate. Subsequently, a U-shaped pattern having a trench width of 150 μm was obtained by exposure and development processes.
4) Preparing a layer of NTC thermosensitive film on the surface of the PET-U type photosensitive resist pattern by adopting a vacuum magnetron sputtering method, wherein the thickness of the film is 2 microns, and the NTC material is a MnCoNiO thermosensitive film. Then, the photosensitive film was cleaned off to obtain a U-shaped MnCoNiO-based thermosensitive thin film circuit having a thickness of 2 μm and a width of 150. mu.m. In addition, on the edge of the PET packaging substrate, an electric heating membrane electrode terminal exposure hole is prepared through a laser cutting process;
5) coating a layer of thermosetting liquid OCA optical transparent adhesive (LOCA) on the surface of the PET-U type NTC circuit formed in the step 4);
6) and (3) attaching the PET packaging substrate-NTC circuit-LOCA structure containing LOCA glue with the PET substrate-graphene-silver electrode structure formed in the step 2), and then baking in an oven at the baking temperature of 140 ℃ for 30 minutes to form the complete PET flexible graphene electrothermal film with the NTC circuit.
Example 2:
a method for preparing an electrothermal film by adopting transparent graphene specifically comprises the following steps:
1) selecting a transparent PET film with the thickness of 100 micrometers, transferring 1 layer of graphene film on the surface of the transparent PET film, wherein the sheet resistance of the film is 320 ohm/sq; in addition, on the edge of the PET, a PTC circuit wiring terminal exposure hole is prepared by adopting a laser cutting process;
2) printing conductive silver paste on the surface of the graphene to form an electric heating film heating layer electrode;
3) selecting a 50-micron-thick PET packaging substrate, and laminating and covering a 20-micron-thick photosensitive dry film on the surface of the PET packaging substrate. Subsequently, a U-shaped pattern having a trench width of 150 μm was obtained by exposure and development processes.
4) A layer of PTC thermosensitive film with the thickness of 2 microns is prepared on the surface of the PET-U type photosensitive resist pattern by adopting a vacuum magnetron sputtering method. The photosensitive film was then washed away to obtain a U-shaped PTC thermosensitive film circuit having a thickness of 2 micrometers and a width of 150 micrometers. In addition, on the edge of the PET packaging substrate, an electric heating membrane electrode terminal exposure hole is prepared through a laser cutting process;
5) at the PTC circuit port, a PTC circuit silver paste terminal (riveting type) is printed and formed, and the silver paste terminal is enabled to have good electric contact with the PTC circuit interface.
6) Coating a layer of semi-solid OCA optical transparent adhesive on the surface of the PET-U type PTC circuit formed in the step 5);
7) and (3) attaching the PET packaging substrate-PTC circuit-OCA structure containing OCA glue with the PET substrate-graphene-silver electrode structure formed in the step 2), and then baking in an oven at the baking temperature of 120 ℃ for 50 minutes to form the complete PET flexible graphene electrothermal film with the PTC circuit.
Example 3:
a method for preparing an electrothermal film by adopting transparent graphene specifically comprises the following steps:
1) selecting a transparent PET film with the thickness of 10 microns, transferring 10 layers of graphene films on the surface of the transparent PET film, wherein the sheet resistance of the film is 110 ohm/sq; in addition, on the edge of the PET, a PTC circuit wiring terminal exposure hole is prepared by adopting a laser cutting process;
2) printing conductive silver paste on the surface of the graphene to form an electric heating film heating layer electrode;
3) selecting a 10-micron-thick PET packaging substrate, and laminating and covering a 20-micron-thick photosensitive dry film on the surface of the PET packaging substrate. Subsequently, a U-shaped pattern having a trench width of 150 μm was obtained by exposure and development processes.
4) A layer of PTC thermosensitive film with the thickness of 2 microns is prepared on the surface of the PET-U type photosensitive resist pattern by adopting a vacuum magnetron sputtering method. The photosensitive film was then washed away to obtain a U-shaped PTC thermosensitive film circuit having a thickness of 2 micrometers and a width of 150 micrometers. In addition, on the edge of the PET packaging substrate, an electric heating membrane electrode terminal exposure hole is prepared through a laser cutting process;
5) at the PTC circuit port, a PTC circuit silver paste terminal (riveting type) is printed and formed, and the silver paste terminal is enabled to have good electric contact with the PTC circuit interface.
6) Coating a layer of semi-solid OCA optical transparent adhesive on the surface of the PET-U type PTC circuit formed in the step 5);
6) and (3) attaching the PET packaging substrate-PTC circuit-OCA structure containing OCA glue with the PET substrate-graphene-silver electrode structure formed in the step 2), and then baking in an oven at the baking temperature of 180 ℃ for 10 minutes to form the complete PET flexible graphene electrothermal film with the PTC circuit.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method for preparing an electrothermal film by adopting transparent graphene is characterized by comprising the following steps:
s1: transferring a graphene film on the surface of a flexible substrate;
s2: printing a silver paste electrode on the surface of the graphene film to obtain a composite structural member of a flexible substrate, the graphene film and the electrode;
s3: taking a flexible packaging film, forming a PTC or NTC thermosensitive film monitoring circuit on the surface of the packaging film by adopting a vacuum coating process, and covering a layer of OCA glue on the surface of the PTC or NTC thermosensitive film monitoring circuit to obtain a PI-PTC/NTC layer-OCA glue structural component;
s4: and (3) attaching and baking the composite structural member of the flexible substrate-graphene film-electrode prepared by S2 and the PI-PTC/NTC layer-OCA adhesive structural component prepared by S3 to obtain the flexible substrate-graphene film-electrode-OCA adhesive-PTC/NTC layer-flexible packaging film structure.
2. The method for preparing the electrothermal film by using the transparent graphene as claimed in claim 1, wherein in S1, 1-10 graphene films are transferred on the surface of the flexible substrate.
3. The method for preparing the electrothermal film by using the transparent graphene as claimed in claim 2, wherein in S1, the surface of the flexible substrate is transferred with 2 graphene films.
4. The method of claim 3, wherein in the step S3, the specific method for forming the PTC or NTC thermosensitive thin film monitoring circuit on the surface of the flexible packaging film by using the vacuum coating process is as follows:
a) coating photoresist on the surface of the flexible packaging film, or pressing a photosensitive dry film, and then obtaining patterned photoresist or dry film through exposure and development processes;
b) obtaining a PTC or NTC heat-sensitive film layer on the surface of a flexible packaging substrate with a patterned photoresist or dry film on the surface by a sputtering method or a vacuum evaporation method;
c) removing the photoresist or the dry film to obtain a PTC or NTC heat-sensitive film patterned electrode;
d) one side of the flexible packaging substrate PTC circuit is provided with a layer of optical transparent adhesive, and the transparent adhesive can adopt a mode of coating liquid optical transparent adhesive (LOCA) or directly attaching semi-cured optical transparent adhesive (OCA).
5. The method for preparing the graphene electrothermal film based on the CVD method with the overheat protection function according to claim 4, wherein the PTC or NTC circuit is of a U-shaped structure.
6. The method for preparing the electrothermal film by using the transparent graphene as claimed in claim 5, wherein the U-shaped PTC or NTC circuit is a porous continuous wire.
7. The method for preparing the electrothermal film by using the transparent graphene according to claim 4, wherein the layer of OCA glue is applied in a Liquid Optical Clear Adhesive (LOCA) coating mode or directly attached to a semi-cured OCA.
8. The method for preparing the graphene electrothermal film based on the CVD method with the overheat protection function as claimed in claim 1, wherein in S4, the baking temperature is 120-180 ℃, and the baking time is 10-50 minutes.
9. The method of preparing the electrothermal film by using the transparent graphene as claimed in claim 8, wherein in the step S4, the baking temperature is 140 ℃ and the baking time is 30 minutes.
10. The method of preparing an electrothermal film using transparent graphene according to claim 1, wherein in S4, before the composite structural member of the flexible substrate-graphene film-electrode prepared in S2 is attached to the PI-PTC layer-OCA glue structural member prepared in S3, a terminal of the heating layer of the electrothermal film and a PTC terminal exposure hole are previously provided.
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| CN113421698A (en) * | 2021-06-30 | 2021-09-21 | 东莞市驭能科技有限公司 | Flexible conductive film capable of being firmly welded and preparation method and application thereof |
| CN115006110A (en) * | 2022-06-02 | 2022-09-06 | 南通国峰新材料科技有限公司 | Graphene crystal film bandage and gypsum bandage using same |
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