CN211352478U - High-temperature-resistant transparent flexible electrothermal film - Google Patents
High-temperature-resistant transparent flexible electrothermal film Download PDFInfo
- Publication number
- CN211352478U CN211352478U CN202020131603.6U CN202020131603U CN211352478U CN 211352478 U CN211352478 U CN 211352478U CN 202020131603 U CN202020131603 U CN 202020131603U CN 211352478 U CN211352478 U CN 211352478U
- Authority
- CN
- China
- Prior art keywords
- electrode
- transparent flexible
- graphene
- film
- mica sheet
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Abstract
The application discloses high temperature resistant transparent flexible electric heat membrane. The high-temperature-resistant transparent flexible electrothermal film comprises a mica sheet substrate (1), a transparent flexible heating layer (2), a flexible electrode (3) and a mica sheet protective layer (4), wherein the flexible electrode (3) is positioned on the surface of the transparent flexible heating layer (2), and the mica sheet substrate (1) and the mica sheet protective layer (4) clamp the flexible electrode (3) and the transparent flexible heating layer (2) in the middle. The preparation method of the high-temperature resistant transparent flexible electrothermal film comprises the step of growing a transparent flexible heating layer (2) on the surface of a mica sheet substrate (1). The high-temperature-resistant transparent flexible electrothermal film can resist high temperature, and has flexibility and high light transmission.
Description
Technical Field
The disclosure relates to the field of electric heating, in particular to a high-temperature-resistant transparent flexible electrothermal film.
Background
With the trend of changing coal into electricity in China, the mode of heating by using the electric heating film becomes a main development trend for replacing the traditional heating mode. At present, electric heating film heating devices in the market mainly take carbon materials or carbon-containing materials as core heating materials. The carbon material may be in various forms, such as carbon fiber, carbon slurry, carbon crystal, graphene slurry (containing graphene nanoplatelets), graphene transparent film, and the like.
The carbon material in the electric heating film can tolerate higher temperature, but most of the existing electric heating films use epoxy resin, PET, PEN, PI and other insulator substrates which can only be used below 200 ℃, so the temperature characteristic of the current electric heating film is limited by the temperature characteristic of the substrate, the heating temperature of the carbon material is further improved, the substrate can be damaged, and the electric heating film is further damaged. Although glass as a substrate material can resist high temperature, a hard electric heating plate obtained by using glass as a substrate cannot be applied to a flexible scene.
Disclosure of Invention
The technical problem that this disclosure will solve lies in, as far as the heating effect is concerned, the electric heat membrane can be comparable with traditional coal heating mode or resistance wire heating mode just can reach higher temperature, but under the high temperature condition, present electric heat membrane damages easily.
The present disclosure provides an electrothermal film, which is wholly flexible and transparent and can resist high temperature of more than 400 ℃.
Specifically, the present disclosure proposes the following technical solutions:
some embodiments of the present disclosure provide a high temperature resistant transparent flexible electrothermal film, including a mica sheet substrate, a transparent flexible heating layer, a flexible electrode and a mica sheet protective layer, wherein the flexible electrode is located on the surface of the transparent flexible heating layer, and the mica sheet substrate and the mica sheet protective layer sandwich the flexible electrode and the transparent flexible heating layer.
In the electrothermal film provided by some embodiments of the present disclosure, the thickness of the mica sheet substrate is 0.1 to 200 μm, preferably 4 to 80 μm, and more preferably 10 to 50 μm.
In the electrothermal film provided by some embodiments of the present disclosure, the thickness of the mica sheet protective layer is 0.1 to 200 μm, preferably 4 to 50 μm, and more preferably 10 to 30 μm.
In the electric heating film provided by some embodiments of the present disclosure, the transparent flexible heating layer is 1-10 layers of single-layer carbon atom graphene films, preferably, the transparent flexible heating layer is 1-5 layers of single-layer carbon atom graphene films, and more preferably, the transparent flexible heating layer is 1-2 layers of single-layer carbon atom graphene films.
In the electrothermal film provided by some embodiments of the present disclosure, the thickness of the flexible electrode is 0.01 to 200 μm, preferably 0.1 to 50 μm, and more preferably 10 to 20 μm; optionally, the flexible electrodes are selected from parallel electrodes comprising parallel bus bars or interdigitated electrodes comprising bus bars and a plurality of inner electrodes; optionally, the shape of the bus bar is selected from linear and/or curvilinear; optionally, the shape of the inner electrode is selected from rectangular, wavy line and/or zigzag.
Some embodiments of the present disclosure provide an electrothermal film, wherein the compliant electrode comprises a transparent compliant electrode and/or a non-transparent compliant electrode; optionally, the inner electrode is a transparent flexible electrode, and the bus bar is a non-transparent flexible electrode;
optionally, the flexible electrode internally comprises a nanowire structure; optionally, the flexible electrode comprises a regular or irregular nano-grid structure formed by interweaving nano-wires, optionally, the nano-wires are selected from nano-metal wires, optionally, the metal is selected from silver, nickel, copper or an alloy thereof; optionally, the flexible electrode further comprises graphene micro-sheets inside, and the length and the width of each graphene micro-sheet are 20 nm-1 μm.
On the other hand, some embodiments of the present disclosure provide a method for preparing a high temperature resistant transparent flexible electrothermal film, comprising the steps of: growing a transparent flexible heating layer on the surface of the mica flake substrate, or transferring the transparent flexible heating layer to the surface of the mica flake substrate;
optionally, the transparent flexible heating layer is grown on the surface of the mica flake substrate by a plasma chemical vapor deposition method, and optionally, the growth temperature is 400-600 ℃.
Some embodiments of the present disclosure provide methods of making wherein the mica flake substrate is obtained by mechanically exfoliating natural mica or synthetic mica, optionally wherein the natural mica comprises muscovite mica and the mica flake substrate is obtained by mechanically exfoliating muscovite mica.
Some embodiments of the present disclosure provide methods of preparation, comprising the steps of: manufacturing a flexible electrode on the transparent flexible heating layer by screen printing or ink-jet printing, optionally manufacturing a mask according to the electrode structure, coating the nano metal wire dispersion liquid or the metal conductive slurry on the transparent flexible heating layer by screen printing or ink-jet printing by using the mask, and drying under a reducing atmosphere to obtain the transparent flexible electrode;
or transferring the prepared metal grid electrode to the surface of graphene, optionally manufacturing a metal network template according to the electrode structure, then carrying out chemical modification on the metal network template and carrying out electrochemical deposition on a metal material to prepare a flexible electrode, and then transferring the flexible electrode to the surface of the transparent flexible heating layer.
Some embodiments of the present disclosure provide a high temperature resistant transparent flexible electrothermal film obtained by the above preparation method.
The beneficial effect of this application includes:
1. the present disclosure uses transparent flexible mica as an electrothermal film substrate, has a low thermal expansion coefficient, a small surface roughness, and a high light transmittance, and has excellent mechanical flexibility.
2. The high-temperature-resistant transparent flexible electrothermal film disclosed by the invention can quickly generate heat, can bear 400 ℃ at least, and can be widely applied to the fields of electric heating, high-temperature sterilization and the like.
3. According to the electric heating film, the transparent flexible mica is used as the electric heating film substrate, the graphene film can be directly grown on the substrate, and the obtained electric heating film is stronger in binding force between the graphene film and the substrate; in addition, the method for directly growing the graphene film can greatly reduce the production cost, better control the production qualification rate, ensure the high quality of the graphene film, and better meet the requirements of low power consumption, high energy, safety and stability and the like.
4. The transparent flexible electrode prepared by the method can enable the electric heating film to be in a light-transmitting state integrally, and the bending resistance is better.
Drawings
FIG. 1 is an exploded view of a high temperature resistant transparent flexible electrothermal film according to embodiments 6-9 of the present disclosure;
FIG. 2 is a schematic top view of a high temperature resistant transparent flexible electrothermal film according to embodiments 6-9 of the present disclosure;
FIG. 3 is an enlarged view of the electric heating film prepared in example 8 corresponding to portion A in FIG. 2;
in the figure, 1 is a mica flake substrate, 2 is a transparent flexible heating layer, 3 is a flexible electrode, 31 is a bus bar, 32 is an internal electrode, and 4 is a mica flake protective layer.
Detailed Description
The technical scheme of the disclosure is clearly and completely described in the following with reference to the accompanying drawings. Obviously, all other embodiments obtained by a person of ordinary skill in the art without making creative efforts based on the specific embodiments in the present disclosure belong to the protection scope of the present disclosure.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments according to the present disclosure.
In the description herein, unless otherwise expressly specified or limited, the term "graphene" is one consisting of carbon atoms in sp2The hybrid tracks form a hexagonal honeycomb lattice two-dimensional carbon nanomaterial. The graphene can be divided into a graphene film and graphene nanoplatelets according to the size of the graphene, the length and the width of each graphene nanoplatelet are 20 nm-1 mu m, and the graphene nanoplatelets are in a powder state in a macroscopic view and can be prepared into a graphene dispersion liquid; the graphene film has a large size, the length or width of the graphene film is 10 mm-1 m, the length can even reach 200m, and the graphene film is macroscopically viewedA thin film state.
The term "mica flakes" refers to soft, resilient mica platelets having a thickness of less than 300 μm.
Some embodiments of the present disclosure provide a high temperature resistant transparent flexible electrothermal film, including a mica sheet substrate, a transparent flexible heating layer, a flexible electrode, and a mica sheet protective layer. The transparent flexible heating layer is located on the mica sheet substrate, the flexible electrode is located on one side surface of the transparent flexible heating layer, and the mica sheet protective layer and the mica sheet substrate clamp the heating layer and the electrode in the middle to jointly protect the heating layer and the electrode.
Optionally, the mica flake substrate and the mica flake protective layer have a thickness of 0.1 to 200 μm, such as 4 to 50 μm, or any value therebetween. The mica flakes of different thickness have different mechanical properties and light transmittance, and the inventors have tested that the mica flakes of 200 μm thickness have a light transmittance of about 70%, and the thinner the mica flakes, the higher the light transmittance and the higher the flexibility, but the thinner the mica flakes, the smaller the width or length thereof.
Alternatively, mica platelets 0.1 to 200 microns thick are obtained by peeling apart mica platelets, which can withstand high temperatures up to 600 ℃, have a low coefficient of thermal expansion, a small surface roughness and a high light transmission (more than 80% can be achieved), and have good mechanical flexibility. The mica sheet can be selected from natural mica sheet or fluorine crystal mica sheet.
Optionally, the transparent flexible heating layer is a graphene film. Optionally, the transparent flexible heating layer is a single-layer carbon atom graphene film with 1-10 layers. Optionally, the transparent flexible heating layer is a single-layer carbon atom graphene film with 1-5 layers. Optionally, the transparent flexible heating layer is a single-layer carbon atom graphene film with 1-2 layers. The resistance of the heating layer can be changed by adjusting the number of the graphene film layers, so that the heating power can be adjusted. The graphene film can be prepared by a chemical vapor deposition method, and the prepared graphene forms a film with larger size and more complete structure.
Some embodiments of the present disclosure provide a preparation method of a high temperature resistant transparent flexible electrothermal film, taking a graphene film as a transparent flexible heating layer as an example, comprising the following steps:
(1) growing a graphene film on a metal substrate by a chemical vapor deposition method (or a plasma enhanced chemical vapor deposition method, PECVD),
(2) the method comprises the steps of transferring a graphene film grown on a metal substrate to the surface of a mica sheet substrate after metal etching, optionally coating a polymethyl methacrylate (PMMA) solution on one side of the graphene film grown on the metal substrate, then etching away the metal to leave a graphene film and a PMMA layer, attaching one side of the graphene film and the PMMA layer to the mica sheet substrate, and dissolving and removing PMMA on the surface of the graphene film by using a solvent, so that the graphene film is transferred to the surface of the mica sheet substrate;
(3) by utilizing a mask plate with a designed structure, printing an electrode on the surface of the graphene film through silk screen patterning or ink-jet printing, or transferring a prepared metal grid electrode to the surface of the graphene film;
(4) and covering a mica flake protective layer on the surface of the prepared graphene film of the electrode.
Some embodiments of the present disclosure provide another preparation method of a high temperature resistant transparent flexible electrothermal film, taking a graphene film as a transparent flexible heating layer as an example, including the following steps:
(1) growing a graphene film on a mica flake substrate by a Plasma Enhanced Chemical Vapor Deposition (PECVD) method,
(2) by utilizing a mask plate with a designed structure, printing an electrode on the surface of the graphene film through silk screen patterning or ink-jet printing, or transferring a prepared metal grid electrode to the surface of the graphene film;
(3) and covering a mica flake protective layer on the surface of the prepared graphene film of the electrode.
In some embodiments of the present disclosure, a mica flake substrate with a thickness of 50 μm (20, 30, 70, 100, 150, 180, 200 μm, etc.) is obtained by mechanical peeling, the mica flake substrate is transferred into a central region of a quartz tube in a plasma chemical vapor deposition device, the quartz tube is sealed and evacuated, a plasma generator is started and hydrogen is introduced, the quartz tube is heated to 400 to 600 ℃, carbon source gas (for example, methane, ethane, propane, butane, ethylene, propylene or acetylene) and hydrogen are introduced, and graphene nucleation growth is maintained for 60 to 200 min. In the growth process, the high-temperature plasma fills the whole quartz tube, and high-efficiency plasma etching or graphene growth can be formed. Nitrogen atom doping can be carried out by introducing ammonia gas or nitrogen gas in the PECVD growth process.
In some embodiments of the present disclosure, methane and hydrogen are introduced at 550-600 ℃ to keep the graphene nucleated and grow for 60-120 min; or introducing ethylene and hydrogen plasmas at the temperature of 450-500 ℃ and growing for 80-200 min.
In some embodiments of the present disclosure, after the growth is completed, the introduction of the carbon source gas is stopped, the quartz tube starts to cool to room temperature, the gas is closed, and the device is opened to take out the sample, so as to obtain the graphene film grown on the mica substrate.
Most of the insulator substrates such as epoxy resin, PET, PEN, PI and the like adopted by the traditional graphene transparent electrothermal film can only be used below 200 ℃, so that a graphene film cannot be grown on the substrates by adopting a chemical vapor deposition method, but the metal substrate is etched and removed after the graphene film is grown on a high-temperature-resistant metal substrate, and then the graphene film is transferred to the substrate. Because the mica flake substrate can resist higher temperature, the graphene film can be directly grown on the substrate by using a plasma enhanced chemical vapor deposition method, so that the production cost is greatly reduced, and the combination firmness between the graphene film and the substrate is better. In addition, the graphene film directly grows on the mica sheet substrate, so that the problem that the integrity of the graphene film is damaged possibly in the process of etching metal and transferring the graphene film is solved, the production yield can be better controlled, the high quality of the graphene film is ensured, and the low power consumption can be better realized to meet the requirements of high energy, safety and stability and the like.
Embodiments of the present disclosure are further illustrated by the following specific examples.
Example 1 preparation of graphene/mica flake composite layer by transfer method
The copper foil with the single-layer carbon atom graphene film is attached to flat glass, then the flat glass is placed on a spin coating machine, a layer of polymethyl methacrylate (PMMA) is coated on one surface of the graphene film in a spin coating mode, and the flat glass is baked for 5min at the temperature of 105 ℃. And then removing the sample from the glass to obtain a copper foil/graphene/PMMA composite layer, etching the copper foil in the copper foil/graphene/PMMA composite layer by using an ammonium persulfate solution to obtain a PMMA/graphene sample floating on the surface of the etching solution, and then repeatedly cleaning the PMMA/graphene sample by using deionized water to remove residual ammonium persulfate. And transferring the cleaned PMMA/graphene sample to a mica sheet substrate with the thickness of 50 microns, baking for 1h at 180 ℃ to enhance the bonding force between the mica sheet and the graphene film, dissolving the PMMA by using acetone to obtain a graphene/mica sheet composite layer, and measuring the sheet resistance of the film to be 180 omega/□ by using a four-probe sheet resistance tester.
The transfer process is repeated by using a clean PMMA/graphene sample, a multi-layer graphene film can be transferred on the mica sheet, and the sheet resistance of the two-layer graphene film obtained by twice transfer is detected to be 150 omega/□.
Example 2 preparation of graphene/mica flake composite layer by directly growing graphene on mica flake
Peeling by a mechanical peeling method to obtain a mica flake substrate with the thickness of 50 microns, transferring the mica flake substrate to the central area of a quartz tube in plasma chemical vapor deposition equipment, sealing and vacuumizing the quartz tube, starting a plasma generator, introducing hydrogen, starting to heat after 5 minutes, heating the quartz tube to 500 ℃ at the speed of 10 ℃/min, controlling the pressure in the quartz tube to be about 33Pa, keeping the temperature at 500 ℃ for 30 minutes, and etching and cleaning the mica flake substrate. Heating the quartz tube to 600 ℃, introducing methane and hydrogen, wherein the hydrogen accounts for 40%, controlling the pressure in the quartz tube to be 6Pa, and keeping the nucleation growth of graphene for 80 min; in the growth process, the high-temperature plasma fills the whole quartz tube, and high-efficiency graphene growth can be formed. And (3) after the growth is finished, closing the methane, starting cooling the quartz tube to room temperature under hydrogen (6Pa), closing the gas, opening the equipment, taking out the sample, obtaining a graphene/mica sheet composite layer with the graphene film grown on the mica sheet substrate, and measuring the sheet resistance of the graphene film to be 150 omega/□ by using a four-probe sheet resistance tester.
Example 3 preparation of graphene/mica flake composite layer by directly growing graphene on mica flake
Peeling by a mechanical peeling method to obtain a mica flake substrate with the thickness of 30 microns, transferring the mica flake substrate to the central area of a quartz tube in plasma chemical vapor deposition equipment, sealing and vacuumizing the quartz tube, starting a plasma generator, introducing hydrogen, starting to heat after 5 minutes, heating the quartz tube to 500 ℃ at the speed of 10 ℃/min, controlling the pressure in the quartz tube to be about 33Pa, keeping the temperature at 500 ℃ for 30 minutes, and etching and cleaning the mica flake substrate. Heating the quartz tube to 600 ℃, introducing methane and hydrogen, wherein the hydrogen accounts for 40%, controlling the pressure in the quartz tube to be 6Pa, and keeping the nucleation growth of graphene for 100 min; in the growth process, the high-temperature plasma fills the whole quartz tube, and high-efficiency graphene growth can be formed. And (3) after the growth is finished, closing the methane, starting cooling the quartz tube to room temperature under hydrogen (6Pa), closing the gas, opening the equipment, taking out the sample, obtaining a graphene/mica sheet composite layer with the graphene film grown on the mica sheet substrate, and measuring the sheet resistance of the graphene film to be 151 omega/□ by using a four-probe sheet resistance tester.
Example 4 preparation of graphene/mica flake composite layer by directly growing graphene on mica flake
Peeling by a mechanical peeling method to obtain a mica flake substrate with the thickness of 10 microns, transferring the mica flake substrate to the central area of a quartz tube in plasma chemical vapor deposition equipment, sealing and vacuumizing the quartz tube, starting a plasma generator, introducing hydrogen, starting to heat after 5 minutes, heating the quartz tube to 500 ℃ at the speed of 10 ℃/min, controlling the pressure in the quartz tube to be about 33Pa, keeping the temperature at 500 ℃ for 30 minutes, and etching and cleaning the mica flake substrate. Then introducing ethylene and hydrogen plasmas, wherein the hydrogen content accounts for 50%, and the cavity is controlled under 6Pa, and growing for 120 min. After the growth is finished, closing ethylene, finally, starting cooling the quartz tube to room temperature under hydrogen (6Pa), closing gas, opening the equipment, taking out a sample to obtain a graphene/mica sheet composite layer with the graphene film grown on the mica substrate, and measuring the sheet resistance of the graphene film to be 148 omega/□ by a four-probe sheet resistance tester.
Example 5 preparation of graphene/mica flake composite layer by directly growing graphene on mica flake
Peeling off the mica flake substrate with the thickness of 80 microns by a mechanical peeling method, transferring the mica flake substrate to the central area of a quartz tube in plasma chemical vapor deposition equipment, sealing and vacuumizing the quartz tube, starting a plasma generator, introducing hydrogen, starting to heat after 5 minutes, heating the quartz tube to 500 ℃ at the speed of 10 ℃/min, controlling the pressure in the quartz tube to be about 33Pa, keeping the temperature at 500 ℃ for 30 minutes, and etching and cleaning the mica flake substrate. Then introducing ethylene and hydrogen plasmas, wherein the hydrogen content accounts for 50%, and the cavity is controlled under 6Pa, and growing for 80 min. After the growth is finished, closing ethylene, finally, starting cooling the quartz tube to room temperature under hydrogen (6Pa), closing gas, opening the equipment, taking out a sample to obtain a graphene/mica sheet composite layer with the graphene film grown on the mica substrate, and measuring the sheet resistance of the graphene film to be 148 omega/□ by a four-probe sheet resistance tester.
Example 6 preparation of high temperature resistant transparent flexible electrothermal film
According to the structural design of the electrode, the graphene/mica sheet composite layer prepared in the embodiment 2 is adopted, the silver nanowire dispersion liquid is coated on the film by using a mask to prepare a transparent flexible electrode, then the transparent flexible electrode is placed in a tubular furnace, reducing gas hydrogen is introduced to dry at 300 ℃, and the transparent flexible electrode is taken out after cooling. And gluing the mica sheet protective layer on the uppermost layer on the electrode and the graphene film through high-temperature-resistant transparent adhesive. Finally, the high-temperature resistant flexible full-transparent electrothermal film is obtained.
The electric heating film prepared by the process is shown in fig. 1 and fig. 2, referring to fig. 1, the electric heating film sequentially comprises a mica sheet substrate 1, a transparent flexible heating layer 2, a transparent flexible electrode 3 and a mica sheet protective layer 4 from bottom to top, the thickness of the mica sheet substrate 1 is 50 micrometers, the thickness of the transparent flexible electrode 3 is 20 micrometers, the thickness of the mica sheet protective layer 4 is 20 micrometers, the transparent flexible heating layer 2 is a double-layer carbon atom graphene film, the overall light transmittance is 82%, and after the obtained electric heating film is bent for 500 times in four directions (up, down, left and right) with the curvature radius of 55mm, the resistance change of the electric heating film is less than 5%. Referring to fig. 2, the transparent flexible electrode 3 in the electric heating film is an interdigital electrode, and includes a bus bar 31 and a plurality of inner electrodes 32, the flexible electrode 3 has a network structure formed by interweaving nano silver wires, and the transparency of the whole electrode is high.
Example 7 preparation of high temperature resistant transparent flexible electrothermal film
According to the electrode structure design, the graphene/mica sheet composite layer prepared in the embodiment 3 is adopted, a composite nano dispersion liquid formed by mixing the graphene dispersion liquid and the nano copper wire dispersion liquid is coated on a film by using a mask, a transparent flexible electrode is prepared, then the transparent flexible electrode is placed in a tubular furnace, reducing gas hydrogen is introduced to dry at 350 ℃, and the transparent flexible electrode is taken out after cooling. The mica sheet protective layer on the uppermost layer can be adhered to the graphene film and the electrode through high-temperature resistant transparent adhesive. Finally, the high-temperature resistant flexible full-transparent electrothermal film is obtained.
As shown in fig. 1, the electric heating film prepared by the above process is similar to the electric heating film prepared in example 6, and comprises a mica sheet substrate 1, a transparent flexible heating layer 2, a transparent flexible electrode 3 and a mica sheet protective layer 4 from bottom to top in sequence, wherein the mica sheet substrate 1 is 30 μm thick, the transparent flexible electrode is 10 μm thick, the mica sheet protective layer is 10 μm thick, the transparent flexible heating layer 2 is a double-layer carbon atom graphene film, the overall light transmittance is 83%, and the resistance of the electric heating film obtained is changed by less than 5% after the electric heating film is bent 500 times in four directions (up, down, left and right) with a curvature radius of 55 mm. Referring to fig. 2, the transparent flexible electrode 3 in the electric heating film is an interdigital electrode, and includes a bus bar 31 and a plurality of inner electrodes 32, the flexible electrode 3 has a network structure formed by interweaving nano silver wires and graphene micro-sheets, and the transparency of the whole electrode is high.
Example 8 preparation of high temperature resistant transparent Flexible electrothermal film
By adopting the graphene/mica sheet composite layer prepared in the embodiment 4, according to the electrode structure design, the arrangement mode of the metal network transparent electrode is firstly designed, then the transparent network template of the electrode is manufactured, then chemical modification and electrochemical deposition of metal silver are carried out on the network template, and finally the corresponding metal network transparent electrode is obtained on the graphene film in a copying and transferring mode. The mica sheet protective layer on the uppermost layer can be adhered to the graphene film and the electrode through high-temperature resistant transparent adhesive. Finally, the high-temperature resistant flexible full-transparent electrothermal film is obtained.
As shown in fig. 1, the electric heating film prepared by the above process is similar to the electric heating film prepared in example 6, the electric heating film sequentially comprises a mica sheet substrate 1, a transparent flexible heating layer 2, a transparent flexible electrode 3 and a mica sheet protective layer 4 from bottom to top, the mica sheet substrate is 10 μm thick, the transparent flexible electrode is 20 μm thick, the mica sheet protective layer is 10 μm thick, the transparent flexible heating layer is a double-layer carbon atom graphene film, the overall light transmittance is 85%, and after the obtained electric heating film is bent 500 times in four directions (up, down, left and right) with a curvature radius of 55mm, the resistance change of the electric heating film is less than 5%. Referring to fig. 2, the transparent flexible electrode 3 in the electrothermal film is an interdigital electrode, and includes a bus bar 31 and a plurality of internal electrodes 32; referring to fig. 3, the interior of the flexible electrode 3 is a metal network, and the transparency of the whole electrode is high.
Example 9 preparation of high temperature resistant partially transparent flexible electrothermal film
By adopting the graphene/mica sheet composite layer prepared in the embodiment 5, according to the electrode structure design, the silver conductive slurry is coated on the film by using the mask to prepare the non-transparent flexible electrode, then the non-transparent flexible electrode is placed in the tubular furnace, and reducing gases such as hydrogen and the like are introduced to dry at 320 ℃, and then the non-transparent flexible electrode is taken out after cooling. The mica sheet protective layer on the uppermost layer can be adhered to the graphene film and the electrode through high-temperature resistant transparent adhesive. And finally obtaining the high-temperature resistant flexible electric heating film with the opaque electrode part.
As shown in fig. 1, the electric heating film prepared by the above process sequentially comprises a mica sheet substrate 1, a transparent flexible heating layer 2, a non-transparent flexible electrode 3 and a mica sheet protective layer 4 from bottom to top, the thickness of the mica sheet substrate is 80 μm, the thickness of the flexible electrode is 50 μm, the thickness of the mica sheet protective layer is 30 μm, the transparent flexible heating layer is double-layer carbon atom graphene, the light transmittance of a non-electrode part is 80%, after the obtained electric heating film is bent 500 times in four directions (up, down, left and right) with a curvature radius of 55mm, the resistance change of the electric heating film is less than 10%, and the bending resistance of the non-transparent electrode made of the slurry is slightly worse than that of the transparent electrodes made in other embodiments, so the resistance change is slightly larger than that of the other embodiments.
Claims (10)
1. The high-temperature-resistant transparent flexible electrothermal film is characterized by comprising a mica sheet substrate (1), a transparent flexible heating layer (2), a flexible electrode (3) and a mica sheet protective layer (4), wherein the flexible electrode (3) is positioned on the surface of the transparent flexible heating layer (2), and the flexible electrode (3) and the transparent flexible heating layer (2) are clamped between the mica sheet substrate (1) and the mica sheet protective layer (4).
2. The electrothermal film according to claim 1, wherein the mica sheet substrate (1) has a thickness of 0.1 to 200 μm.
3. The electrothermal film according to claim 1, wherein the mica sheet protective layer (4) has a thickness of 0.1 to 200 μm.
4. The electrothermal film according to claim 1, wherein the transparent flexible heating layer (2) is a single-layer carbon atom graphene film with 1-10 layers.
5. The electrothermal film according to claim 1, wherein the thickness of the flexible electrode (3) is 0.01-200 μm.
6. The electrothermal film according to claim 5, wherein the flexible electrodes (3) are selected from parallel electrodes comprising parallel bus bars (31) or interdigitated electrodes comprising bus bars (31) and a plurality of inner electrodes (32).
7. The electrothermal film according to claim 6, wherein the shape of the bus bar (31) is selected from linear and/or curvilinear; the shape of the inner electrode (32) is selected from rectangular, wavy line and/or zigzag.
8. The electrothermal film according to any one of claims 1 to 7, wherein the compliant electrode (3) comprises a transparent compliant electrode and/or a non-transparent compliant electrode.
9. The electrothermal film according to claim 6 or 7, wherein the inner electrode (32) is a transparent flexible electrode and the bus bar (31) is a non-transparent flexible electrode.
10. The electric heating film according to any one of claims 1-7, wherein the flexible electrode (3) comprises a regular or irregular nano-grid structure of interwoven nano-wires inside.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202020131603.6U CN211352478U (en) | 2020-01-20 | 2020-01-20 | High-temperature-resistant transparent flexible electrothermal film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202020131603.6U CN211352478U (en) | 2020-01-20 | 2020-01-20 | High-temperature-resistant transparent flexible electrothermal film |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN211352478U true CN211352478U (en) | 2020-08-25 |
Family
ID=72099896
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202020131603.6U Active CN211352478U (en) | 2020-01-20 | 2020-01-20 | High-temperature-resistant transparent flexible electrothermal film |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN211352478U (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111148294A (en) * | 2020-01-20 | 2020-05-12 | 烯旺新材料科技股份有限公司 | High-temperature-resistant transparent flexible electrothermal film and preparation method thereof |
-
2020
- 2020-01-20 CN CN202020131603.6U patent/CN211352478U/en active Active
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111148294A (en) * | 2020-01-20 | 2020-05-12 | 烯旺新材料科技股份有限公司 | High-temperature-resistant transparent flexible electrothermal film and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102597336B (en) | Graphene extensive deposition and doping techniques and use its product | |
| US20140166496A1 (en) | Method for producing shaped graphene sheets | |
| Xu et al. | Graphene–silver nanowire hybrid films as electrodes for transparent and flexible loudspeakers | |
| CN106744820B (en) | Laminated metal chalcogenide/carbon nano tube flexible composite film material of higher order structures and preparation | |
| US20130266729A1 (en) | Method for making strip shaped graphene layer | |
| CN114735941A (en) | Metal-free graphene CVD coatings on glass and other dielectric substrates | |
| JP2013501695A (en) | Wide area deposition of graphene and products containing it by heteroepitaxial growth | |
| US20130264193A1 (en) | Method for making strip shaped graphene layer | |
| CN108565130B (en) | Graphene film electrode, preparation method thereof, graphene composite film interdigital electrode with conductive circuit on surface and capacitor | |
| KR101093657B1 (en) | Fabrication method of graphene film by using joule heating | |
| US9393767B2 (en) | Method for making strip shaped graphene layer | |
| CN104882297B (en) | Process for preparing stretchable supercapacitor based on highly conductive graphene/nickel particle mixed structure | |
| CN107910383B (en) | Preparation method of metal mesh conductive film | |
| US9216908B2 (en) | Method for making strip shaped graphene layer | |
| CN104505147B (en) | The preparation method of graphene nano wall flexible conductive film | |
| CN211352478U (en) | High-temperature-resistant transparent flexible electrothermal film | |
| CN101990326A (en) | Thin-film type CNT (carbon nano tube) demister | |
| KR101500192B1 (en) | Transparent conductive films including graphene layer and mathod for manufacturing the same | |
| CN108622879B (en) | Dry contact transfer method of carbon nano tube vertical array | |
| CN111148294A (en) | High-temperature-resistant transparent flexible electrothermal film and preparation method thereof | |
| KR101505471B1 (en) | Transfer and adhesion technology of nano thin film | |
| CN108529605A (en) | A kind of preparation method of large area pattern graphite alkene | |
| CN110267372B (en) | Graphene electric heating composite part and manufacturing method thereof | |
| Zhang et al. | High weight-specific power density of thin-film amorphous silicon solar cells on graphene papers | |
| CN108910868A (en) | A method of preparing graphene dendrite on an insulating substrate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| GR01 | Patent grant | ||
| GR01 | Patent grant |