CN109661043B - Color-changeable flexible heating composite film - Google Patents
Color-changeable flexible heating composite film Download PDFInfo
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- CN109661043B CN109661043B CN201811339790.0A CN201811339790A CN109661043B CN 109661043 B CN109661043 B CN 109661043B CN 201811339790 A CN201811339790 A CN 201811339790A CN 109661043 B CN109661043 B CN 109661043B
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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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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/50—Sympathetic, colour changing or similar inks
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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
- H05B3/02—Details
-
- 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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- 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
- H05B3/10—Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor
- H05B3/12—Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material
-
- 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
- H05B2203/00—Aspects relating to Ohmic resistive heating covered by group H05B3/00
- H05B2203/013—Heaters using resistive films or coatings
-
- 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
- H05B2203/00—Aspects relating to Ohmic resistive heating covered by group H05B3/00
- H05B2203/017—Manufacturing methods or apparatus for heaters
Abstract
The invention discloses a color-changeable flexible heating composite film which comprises a thermochromic first flexible polymer film layer, a conductive layer, a second flexible polymer film layer and conductive electrodes, wherein the conductive layer is superposed on the first flexible polymer film layer, the second flexible polymer film layer is superposed on the conductive layer, and the conductive electrodes are superposed on the conductive layer and positioned on two sides of the second flexible polymer film layer. The color-changeable flexible heating composite film adopts commercialized thermochromic ink and the like as raw materials, has simple preparation process and low cost, is beneficial to large-scale production, and has great application prospect in the aspects of improving the adhesion, scratch resistance and environmental stability of a conductive layer of a conductive material used in the field of thermochromic. The color-changeable flexible heating composite film can be used and stored for a long time, has good insulativity and safety, and can be used for cup heat preservation and temperature indication thereof, thermochromism display devices, thermotherapy pads and other thermochromism devices.
Description
Technical Field
The invention relates to the technical field of thermotropic heating films, in particular to a color-changeable flexible heating composite film which can be used for cup heat preservation and temperature indication thereof, a thermotropic color-changing display device, a thermotherapy pad and other thermotropic color-changing devices.
Background
In recent years, the electric heating film has been receiving more and more attention due to its wide application prospect, such as defrosting and defogging of heating sensors, car windows, mirrors and display devices, thermotherapy pads for human body treatment, thermochromic display devices, and the like. The traditional conductive material Indium Tin Oxide (ITO) has been widely used in electrical heating films, but its further development and application in the next generation of intelligent flexible electronic devices are limited due to the shortcomings of scarce raw materials, complex preparation process, high cost, high brittleness and the like. In order to solve these problems, researchers have developed many alternative materials for ITO such as graphene, carbon nanotubes, metal grids, metal nanowires, etc. The materials can be simply compounded with a flexible substrate by using methods such as roller coating, spin coating, spray coating and the like to form a flexible heating film, and the flexible heating film is used in various flexible electronic fields such as thermochromic display devices, vehicle window defrosting and defogging, thermotherapy pads and the like. When the flexible heating film is applied to the thermochromic field, the surface of the flexible heating film is required to be coated with color-changing ink and provided with a conductive layer, the adhesion of the ink is low, the ink is not scratch-resistant, and the conductive layer is directly exposed in the air and is easily oxidized and corroded, so that the flexible heating film cannot be used for a long time.
Disclosure of Invention
The invention aims to solve the technical problem of providing a color-changeable flexible heating composite film aiming at the defects of the prior art, the composite film has good scratch resistance and environmental stability, can be used and stored for a long time, has good insulativity and safety, is beneficial to large-scale production, has huge application prospect in the aspects of improving the adhesive force, scratch resistance and environmental stability of a conductive layer of a conductive material used in the thermochromic field, and can be used for cup heat preservation and temperature indication thereof, thermochromic display devices, thermotherapeutic pads and other thermochromic devices.
The technical scheme adopted by the invention for solving the technical problems is as follows: a color-changeable flexible heating composite film comprises a thermochromic first flexible polymer film layer, a conductive layer, a second flexible polymer film layer and conductive electrodes, wherein the conductive layer is superposed on the first flexible polymer film layer, the second flexible polymer film layer is superposed on the conductive layer, and the conductive electrodes are superposed on the conductive layer and positioned on two sides of the second flexible polymer film layer.
Preferably, the first flexible polymer thin film layer is obtained by curing a first solution to form a film, the first solution is obtained by mixing thermochromic ink, a polymer solute and an organic solvent, and the polymer solute is any one of polyimide, polymethyl methacrylate, polyvinyl alcohol, polyurethane and polydimethylsiloxane; in the first solution, the mass ratio of the thermochromic printing ink to the organic solvent is 1: 100-400, and the mass ratio of the polymer solute to the organic solvent is 1: 10-30.
Further, the film forming process of the first flexible polymer film layer is as follows: and dripping or spin-coating the first solution on clean glass provided with the conducting layer, heating and curing at 60-200 ℃, and naturally cooling to form a film.
Preferably, the conductive layer is formed by depositing graphene, carbon nanotubes or metal nanowires on the glass, and the first solution is dripped or spin-coated on the conductive layer.
Preferably, the film forming process of the first flexible polymer film layer is as follows: and dripping or spin-coating the first solution on clean glass, heating and curing at 60-200 ℃, naturally cooling to obtain the first flexible high polymer thin film layer, and depositing on the first flexible high polymer thin film layer by using a roller coating, spin coating, spray coating, sputtering or vacuum deposition method to obtain the conductive layer.
Preferably, the conductive layer is formed by depositing an oxide/metal/oxide or a conductive polymer on the first flexible high polymer film layer by roll coating, spin coating, spray coating, sputtering or vacuum deposition.
The conductive layer is prepared by deposition by using a roller coating, spin coating, spray coating, sputtering or vacuum deposition method, and the preparation method has the advantages that the deposition process and parameters are controllable, and the resistance of the conductive layer can be controlled by changing the coating or sputtering deposition times and deposition time, so that the thermochromic process of the composite film is controlled.
Preferably, the range of the difference between the thermal expansion coefficients of the second flexible polymer film layer and the first flexible polymer film layerIs +/-6X 10-4and/K. The first flexible polymer film layer and the second flexible polymer film layer with similar thermal expansion coefficients can ensure that the two polymer film layers can be well combined with the conductive layer together, thereby ensuring the environmental stability and the service life of the composite film.
Further, the second flexible polymer film layer is obtained by dripping the second solution on the conductive layer, heating and curing at 60-150 ℃ and naturally cooling; the second solution is prepared by dissolving polymethyl methacrylate, polyvinyl alcohol or polyurethane in an organic solvent according to a mass ratio of 1: 10-30.
Preferably, the conductive electrode is a copper tape adhered to the conductive layer, or the conductive electrode is obtained by dropping silver paste or sputtering a metal electrode on the conductive layer.
Preferably, the thicknesses of the first flexible polymer film layer and the second flexible polymer film layer are respectively 10-50 μm.
Compared with the prior art, the invention has the following advantages:
1. according to the color-changeable flexible heating composite film disclosed by the invention, the conducting layer is arranged between the first flexible polymer film layer and the second flexible polymer film layer, and the first flexible polymer film layer and the second flexible polymer film layer which are insulated can effectively protect the conducting layer and prevent the conducting layer from being exposed in the air, so that the oxidation and corrosion of the conducting layer are prevented, the environmental stability of the conducting layer is greatly improved, and the service life of the composite film is greatly prolonged;
2. according to the invention, the thermochromic ink, the polyimide and other high-molecular solutes and the organic solvent are mixed to prepare a first solution, and the first solution is cured to form a film to obtain a first flexible high-molecular film layer, so that the thermochromic ink is well cured, the bonding force between the thermochromic ink and the conductive layer can be increased, the problem of poor adhesion of the thermochromic ink in the traditional film is solved, the scratch resistance of the composite film is improved, and the application space of the composite film is enlarged;
3. according to the invention, a second solution is prepared by mixing a polymethyl methacrylate and other high molecular solutes and an organic solvent, and the second solution is solidified on the conductive layer to form a film, so that a second flexible high molecular film layer is obtained, the second flexible high molecular film layer plays a role in protecting the conductive layer, the electrical property of the composite film is not influenced while the conductive layer is prevented from being exposed in air, and the resistance of the film is ensured to be unchanged;
4. the color-changeable flexible heating composite film adopts commercialized thermochromic ink and the like as raw materials, has simple preparation process and low cost, is beneficial to large-scale production, and has great application prospect in the aspects of improving the adhesion, scratch resistance and environmental stability of a conductive layer of a conductive material used in the field of thermochromic;
5. the color-changeable flexible heating composite film can be used and stored for a long time, has good insulativity and safety, and can be used for cup heat preservation and temperature indication thereof, thermochromism display devices, thermotherapy pads and other thermochromism devices.
Drawings
FIG. 1 is a schematic structural view of a color-changeable flexible heat laminated film in example 1;
FIG. 2 is a schematic view of the structure of a thermochromic film in comparative example 1;
FIG. 3 is a plot of film temperature of example 1 as a function of time as recorded by an infrared thermometer;
FIG. 4 is a plot of film temperature versus time for comparative example 1 recorded using an infrared thermometer;
FIG. 5 is a graph of the rate of change of resistance of the films of example 1 and comparative example 1 during 6000 bends;
FIG. 6 is a graph showing the rate of change in resistance of the films of example 1 and comparative example 1 obtained by a conventional humid heat aging test;
fig. 7 is a graph showing the rate of change in resistance of the films of example 1 and comparative example 1 obtained by the damp heat aging test in a hydrogen sulfide atmosphere.
Detailed Description
The invention is described in further detail below with reference to the accompanying examples.
The color-changeable flexible heating composite film of embodiment 1, as shown in fig. 1, includes a thermochromic first flexible polymer film layer 1, a conductive layer 2, a second flexible polymer film layer 3, and conductive electrodes 4, the conductive layer 2 is stacked on the first flexible polymer film layer 1, the second flexible polymer film layer 3 is stacked on the conductive layer 2, and the conductive electrodes 4 are stacked on the conductive layer 2 and located on both sides of the second flexible polymer film layer 3.
In example 1, the conductive layer 2 is a conductive network obtained by depositing silver nanowires on glass, and the preparation process thereof is as follows: dropping 1mL of silver nanowire solution with the concentration of 0.5mg/L on glass with the size of 50mm multiplied by 50mm, rolling or spin-coating the silver nanowire solution to form a silver nanowire conductive network, heating the silver nanowire conductive network at 160 ℃ for 30 minutes to reduce the junction resistance of the silver nanowire conductive network, and finally obtaining the conductive layer 2 on the glass.
In example 1, the first flexible polymer thin film layer 1 was obtained by curing a first solution to form a film, and the first solution was obtained by mixing thermochromic ink, polyimide, and an organic solvent, N-dimethylacetamide; in the first solution, the mass ratio of the thermochromic ink to the polyimide was 1:300, and the mass ratio of the polyimide to the N, N-dimethylacetamide was 1: 10. The film forming process of the first flexible polymer film layer 1 is as follows: and dripping or spin-coating the first solution on the conducting layer 2 on the glass, putting the glass into an oven, heating and curing at the temperature of 80 ℃/2h in the oven, and naturally cooling to form the film.
In example 1, the conductive electrode was a copper tape attached to the conductive layer.
In example 1, the second flexible polymer thin film layer 2 was obtained by curing a second solution to form a film, and the second solution was obtained by dissolving polymethyl methacrylate in an organic solvent at a mass ratio of 1: 10. The film forming process of the second flexible polymer film layer 3 is as follows: and dripping the second solution on the exposed surface of the silver nanowire conductive network on the side provided with the conductive electrode 4, heating and curing in an oven at 60 ℃/3h, and naturally cooling to form a film.
For comparison, a thermochromic thin film in which the second flexible polymer thin film layer is not provided was used as comparative example 1.
The thermochromic thin film of comparative example 1 has the same overall structure as the composite thin film of example 1. As shown in fig. 2, the thermochromic solar cell comprises a thermochromic first flexible polymer film layer 1, a conductive layer 2 and conductive electrodes 4, wherein the conductive layer 2 is stacked on the first flexible polymer film layer 1, and the conductive electrodes 4 are stacked on the conductive layer 2 and positioned on two sides of the surface of the conductive layer 2.
In comparative example 1, the conductive layer 2 is a conductive network obtained by depositing silver nanowires on glass, and the preparation process is as follows: dropping 1mL of silver nanowire solution with the concentration of 0.5mg/L on glass with the size of 50mm multiplied by 50mm, rolling or spin-coating the silver nanowire solution to form a silver nanowire conductive network, heating the silver nanowire conductive network at 160 ℃ for 30 minutes to reduce the junction resistance of the silver nanowire conductive network, and finally obtaining the conductive layer 2 on the glass.
In the comparative example 1, the first flexible polymer thin film layer 1 was obtained by curing a first solution to form a film, and the first solution was obtained by mixing thermochromic ink, polyimide, and an organic solvent, N-dimethylacetamide; in the first solution, the mass ratio of the thermochromic ink to the polyimide was 1:300, and the mass ratio of the polyimide to the N, N-dimethylacetamide was 1: 10. The film forming process of the first flexible polymer film layer 1 is as follows: and dripping or spin-coating the first solution on the conducting layer 2 on the glass, putting the glass into an oven, heating and curing at the temperature of 80 ℃/2h in the oven, and naturally cooling to form the film.
In comparative example 1, the conductive electrode was a copper tape adhered to the conductive layer.
Metal wires were attached to the conductive electrodes 4 of the films of example 1 and comparative example 1, respectively, and the thickness, conductivity, heating performance, bending performance, and environmental stability of the films were tested.
Through detection, the thickness of the film of the embodiment 1 is 20-100 μm; the resistances of the two sides of the film are the same as those of the silver nanowire conductive network without the first flexible polymer thin film layer 1 and the second flexible polymer thin film layer 3, and are both 16.0 Ω.
Through detection, the thickness of the film of the comparative example 1 is 10-50 μm; the resistance of the two sides of the film is the same as that of the silver nanowire conductive network without the first flexible polymer film layer 1, and is 16.0 omega.
The low voltage heating test is performed on the film of example 1, a power supply is connected to the conductive electrodes 4 on both sides of the film, an infrared thermometer is used to measure the temperature and record the curve of the temperature of the film changing with time, as shown in fig. 3, the heating result proves that the working voltage of the film is low, which indicates that the heating performance of the conductive layer 2 is not affected after the second flexible polymer film layer 3 is covered, and the temperature of the film can be roughly determined from the color-changing temperature, and the color-changing film can be selected from the existing known different color-changing temperature inks to be suitable for different low power consumption devices.
The film of comparative example 1 was subjected to a low voltage heating test, a power supply was connected to the conductive electrodes 4 on both sides of the film, and the temperature was measured with an infrared thermometer and the change curve of the film temperature with time was recorded, as shown in fig. 4, the heating results demonstrated that the working voltage of the film was low and the film temperature could be roughly determined from the discoloration temperature, and the discoloration film here could be adapted to different low power consumption devices by using different known discoloration temperature inks.
The films of example 1 and comparative example 1 were bent 6000 times, each with a bending radius of 2mm, respectively, and the resistances of both sides of the films were measured and recorded with a multimeter during the bending, and the test results are shown in fig. 5, in which PI/AgNW represents comparative example 1 and PI/AgNW/PMMA represents example 1. FIG. 5 shows that the film of example 1 has a resistance change rate of only 7%, demonstrating that the film of example 1 has good bending properties and can be applied to flexible devices; FIG. 5 shows that the film of comparative example 1 has a resistance change rate of less than 12%, demonstrating that the thermochromic film of comparative example 1 has a lower bending property than that of comparative example 1, although it has a better bending property
Example 1.
The film of example 1 and the film of comparative example 1 were subjected to a conventional damp heat aging test and a damp heat aging test in a hydrogen sulfide atmosphere, respectively. The test conditions for both damp heat aging tests were 105 ℃/100% RH (humidity). The results of the conventional damp-heat aging test are shown in fig. 6, and the results of the damp-heat aging test in a hydrogen sulfide atmosphere are shown in fig. 7. In FIGS. 6 and 7, PI/AgNW represents comparative example 1, and PI/AgNW/PMMA represents example 1. As can be seen from fig. 6, the film of example 1 had a resistance change rate of only 16%, whereas the film of comparative example 1 had a resistance change rate as high as 49%. As can be seen from fig. 7, the film of example 1 had a resistance change rate of only 25%, whereas the film of comparative example 1 had a resistance change rate as high as 60%. Therefore, the resistance of the film of comparative example 1 is greatly changed, which indicates that the environmental stability of the thermochromic film of comparative example 1 needs to be improved, and the second flexible polymer thin film layer provided in the composite film of the present invention can effectively improve the environmental stability of the film.
Claims (9)
1. A color-changeable flexible heating composite film is characterized in that: the thermochromic conductive film comprises a thermochromic first flexible polymer film layer, a conductive layer, a second flexible polymer film layer and conductive electrodes, wherein the conductive layer is superposed on the first flexible polymer film layer, the second flexible polymer film layer is superposed on the conductive layer, and the conductive electrodes are superposed on the conductive layer and positioned on two sides of the second flexible polymer film layer; the first flexible high-molecular film layer is obtained by curing a first solution to form a film, the first solution is obtained by mixing thermochromic ink, a high-molecular solute and an organic solvent, and the high-molecular solute is any one of polyimide, polymethyl methacrylate, polyvinyl alcohol, polyurethane and polydimethylsiloxane; in the first solution, the mass ratio of the thermochromic printing ink to the organic solvent is 1: 100-400, and the mass ratio of the polymer solute to the organic solvent is 1: 10-30.
2. A variable color flexible heat stake film as defined in claim 1, wherein: the film forming process of the first flexible high polymer film layer is as follows: and dripping or spin-coating the first solution on clean glass provided with the conducting layer, heating and curing at 60-200 ℃, and naturally cooling to form a film.
3. A variable color flexible heat stake film as defined in claim 2, wherein: the conducting layer is obtained by depositing graphene, carbon nanotubes or metal nanowires on the glass, and the first solution is dripped or spin-coated on the conducting layer.
4. A variable color flexible heat stake film as defined in claim 1, wherein: the film forming process of the first flexible high polymer film layer is as follows: and dripping or spin-coating the first solution on clean glass, heating and curing at 60-200 ℃, naturally cooling to obtain the first flexible high polymer thin film layer, and depositing on the first flexible high polymer thin film layer by using a roller coating, spin coating, spray coating, sputtering or vacuum deposition method to obtain the conductive layer.
5. A variable color flexible heat stake film according to claim 4, wherein: the conducting layer is obtained by depositing oxide/metal/oxide or conducting polymer on the first flexible high-molecular film layer by using a roller coating, spin coating, spray coating, sputtering or vacuum deposition method.
6. A variable color flexible heat stake film as defined in claim 1, wherein: the difference range of the thermal expansion coefficients of the second flexible polymer film layer and the first flexible polymer film layer is +/-6 multiplied by 10-4/K。
7. A variable color flexible heat stake film according to claim 6, wherein: the second flexible high polymer film layer is formed by dripping a second solution on the conductive layer, heating and curing at 60-150 ℃ and naturally cooling; the second solution is prepared by dissolving polymethyl methacrylate, polyvinyl alcohol or polyurethane in an organic solvent according to a mass ratio of 1: 10-30.
8. A variable color flexible heat stake film as defined in claim 1, wherein: the conductive electrode is a copper tape adhered on the conductive layer, or is obtained by dripping silver paste or sputtering a metal electrode on the conductive layer.
9. A variable color flexible heat stake film as defined in claim 1, wherein: the thickness of the first flexible polymer film layer and the thickness of the second flexible polymer film layer are respectively 10-50 mu m.
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CN110109265A (en) * | 2019-05-21 | 2019-08-09 | 南京银纳新材料科技有限公司 | A kind of foldable thermochromism device preparation method based on nano wire film |
CN110403751B (en) * | 2019-07-19 | 2021-08-24 | 东南大学 | Flexible thermochromic interactive wearable thermotherapeutic pad and preparation method thereof |
CN113741110A (en) * | 2021-08-16 | 2021-12-03 | 河北工业大学 | Thermosensitive color-changing bistable display |
CN114059348B (en) * | 2021-11-18 | 2023-03-14 | 兰州大学 | Flexible transparent heating film, flexible transparent thermotherapy sheet and preparation method |
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