CN114126116A - Flexible, transparent and degradable thin film heater with embedded silver nanowire annular conductive network and its preparation method and application - Google Patents
Flexible, transparent and degradable thin film heater with embedded silver nanowire annular conductive network and its preparation method and application Download PDFInfo
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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—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor
- H05B3/12—Heating 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
- H01B13/0036—Details
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Abstract
本发明涉及一种嵌入式银纳米线环状导电网络的柔性透明可降解薄膜加热器及其制备方法与应用，该方法通过调整银纳米线溶液浓度和喷涂设备的喷嘴尺寸与载运气体压强，向聚合物薄膜衬底表面喷涂银纳米线溶液，在毛细流动的作用下，银纳米线溶液中的银纳米线从中心位置被驱动到边缘位置，形成规则的银纳米线咖啡环形貌；干燥后在聚合物薄表面得到银纳米线环状导电网络薄膜，得到的薄膜加热器具有均匀的方阻，从而使薄膜加热器具有均匀的加热性能，并且具有优良的长时间稳定和循环的加热性能。并且可以通过改变喷涂银纳米线的量与施加薄膜加热器两端电压的大小来调整薄膜加热器的透明度和加热性能，更好地满足不同应用领域的需求。
The invention relates to a flexible, transparent and degradable film heater embedded with a ring-shaped conductive network of silver nanowires, and a preparation method and application thereof. The silver nanowire solution is sprayed on the surface of the polymer film substrate. Under the action of capillary flow, the silver nanowires in the silver nanowire solution are driven from the center position to the edge position, forming a regular silver nanowire coffee ring shape; after drying The silver nanowire annular conductive network film is obtained on the thin surface of the polymer, and the obtained film heater has uniform square resistance, so that the film heater has uniform heating performance and excellent long-term stability and cyclic heating performance. And the transparency and heating performance of the thin film heater can be adjusted by changing the amount of sprayed silver nanowires and the magnitude of the voltage applied across the thin film heater, so as to better meet the needs of different application fields.
Description
Technical Field
The invention relates to a flexible transparent degradable film heater with an embedded silver nanowire annular conductive network, and a preparation method and application thereof, and belongs to the field of flexible transparent degradable film heaters.
Background
In recent years, thin film heating devices have been widely used in the fields of military, medical treatment, construction, industry, agriculture, and household goods. And controlling the flexible circuit board to generate power by applying voltage to the conductive loop of the thin film heater. Part of the power is converted into a thermal effect, thereby achieving the purpose of heating the object.
In daily life, especially in severe cold and harsh environments, the flexible film heater can be used not only for defrosting and defogging, but also for warming or heating certain key parts of the body, such as knees, waist and the like. Since a general heating device is not convenient to bend and fold when in use, has low applicability, and seriously affects the use performance and effect to a certain extent, a high-performance flexible film heater is needed.
Compared with the traditional film heater, the flexible film heater has higher flexibility and can still normally work after a certain voltage is applied under the bending or folding condition of a certain degree. Therefore, various complex film heating devices can be manufactured and are suitable for different fields.
However, conventional flexible thin film heaters are constructed of two parts, a resistive layer and a flexible substrate. From the viewpoint of the used material of the resistance layer, the metal nanowire has good resistance performance and good flexibility performance required by the electrode. Among them, silver nanowires are an ideal material for manufacturing flexible heaters because of their good stability and relatively low price. From the material of the substrate, the conventional film heater uses Polydimethylsiloxane (PDMS), polyethylene terephthalate (PET), and copolyester (Ecoflex) plastic substrate, which is not easy to process and degrade after use, resulting in environmental pollution.
Chinese patent document CN110602812A discloses a degradable film heater and a method for manufacturing the same, which uses paper as a substrate, thereby greatly reducing the manufacturing cost, and making the film heater have excellent degradable characteristics and easy to be disposed and recycled. However, the silver nanowire solution is easy to be unevenly dripped in the preparation process of the heater, so that the sheet resistance is uneven, the heating performance of the film heater is uneven, the stability is poor, and the paper substrate is poor in mechanical performance and chemical performance and easy to damage under the action of external force or liquid invasion.
Therefore, a high-performance flexible degradable film heater with uniform sheet resistance, uniform heating performance and high stability is urgently needed.
Disclosure of Invention
Aiming at the defects of the prior art, particularly the problem of poor stability caused by non-uniform heating performance of the film heater due to non-uniform sheet resistance, the invention provides a flexible transparent degradable film heater with an embedded silver nanowire annular conductive network, and a preparation method and application thereof.
The film heater has uniform sheet resistance, so that the film heater has uniform heating performance; the film heater provided by the invention has excellent long-time stable and circulating heating performance; the film heater provided by the invention can meet the requirements of most application fields within the heating temperature range, and is particularly suitable for the medical field; compared with the traditional film heater, the film heater provided by the invention has the advantages of simple process, low cost, excellent performance, good degradability, biocompatibility and antibacterial property, and is beneficial to application to human bodies.
In order to achieve the purpose, the invention is realized by the following technical scheme:
the preparation method of the flexible transparent degradable film heater of the embedded silver nanowire annular conductive network comprises the following steps:
(1) preparing a silver nanowire mother solution and a polylactic acid (PLA) solution, wherein the solvent of the silver nanowire solution is an organic solution or a mixed solution of water and the organic solution;
(2) taking a silver nanowire mother solution level solvent to adjust the concentration of a silver nanowire solution, adjusting the nozzle size and the carrier gas pressure of spraying equipment, spraying the silver nanowire solution on the surface of a polymer film substrate, driving the silver nanowires in the silver nanowire solution from the central position to the edge position under the action of capillary flow to form a regular silver nanowire coffee ring shape, obtaining a silver nanowire annular conductive network, and drying to form a silver nanowire annular conductive network film on the polymer film;
(3) spin-coating a PLA solution on the surface of the dried conductive network film by using a spin coater;
(4) and heating to solidify the liquid flexible substrate, and cooling and peeling the film to obtain the flexible transparent degradable film heater of the embedded silver nanowire annular conductive network.
Preferably, in the step (1), the diameter of the silver nanowire is 10-200nm, the length of the silver nanowire is 10-200 μm, and the concentration of the silver nanowire in the silver nanowire mother liquor is 10-15 mg/ml.
Preferably, in step (1), the organic solution is isopropanol, ethanol or methanol, and the concentration of the organic solution in the mixed solution of water and the organic solution is: 0.1-5 mg/ml.
The organic solvent has the advantages of low boiling point, easy evaporation and the like, is beneficial to the generation of coffee ring effect of silver nanowire solution, and then self-assembly is carried out under the action of capillary flow to obtain the silver nanowire annular conductive network.
Preferably, in step (1), the PLA solution is prepared by the following method:
according to the mass ratio of 1: (5-40) mixing and stirring polylactic acid (PLA) and an organic solvent for 1-12 hours to obtain a polylactic acid (PLA) solution.
More preferably, the polylactic acid (PLA) is one or a mixture of two or more of levorotatory polylactic acid, dextrorotatory polylactic acid, and racemic polylactic acid.
Most preferably, the polylactic acid (PLA) is l-polylactic acid.
Further preferably, the organic solvent is dichloromethane (CH)2Cl2) Or trichloromethane (CHCl)3)。
Most preferably, the organic solvent is methylene Chloride (CH)2Cl2)。
Preferably, in step (2), the concentration of the silver nanowire solution after adjustment is 0.1-9 mg/ml.
Preferably, in step (2), the diameter of the nozzle of the spray device is 0.1-5mm and the distance from the nozzle to the polymer film is 1-50 cm.
Preferably, in step (2), the carrier gas is high purity air, nitrogen or argon, and the pressure of the carrier gas is 0.1-1 MPa.
Preferably, according to the invention, in step (2), the spray thickness is 0.001 to 0.1 mm.
Preferably, according to the invention, in step (2), every 4-36cm22-30mL of silver nanowire solution is sprayed on the substrate.
According to the invention, in the step (2), the spraying equipment is preferably a manual spraying gun and an automatic spraying gun.
Both manual and automated spray gun devices are conventional in the art.
Preferably, in step (2), the polymer film substrate is a flexible substrate, and preferably, the polymer film substrate is Polytetrafluoroethylene (PTFE), polyethylene terephthalate (PET), Polycarbonate (PC) or polyvinyl chloride (PVC).
Most preferably, the polymer film substrate is Polytetrafluoroethylene (PTFE).
Preferably, in step (2), the drying temperature is 25-150 ℃ and the drying time is 5-120 min.
Preferably, in step (3), the spin coating of PLA solution is carried out at a spin coater rotation speed of 100 and 1500rpm for 5-120 s.
According to the invention, in the step (4), the liquid flexible substrate is heated to be cured, and the spin-coated film material is placed in an oven to be heated to be cured, wherein the heating temperature is 25-150 ℃, and the heating time is 1-24 h.
Preferably, in the step (4), the PLA film is peeled from the substrate after cooling; the thickness of the film obtained after peeling is 0.01-0.2 mm.
A flexible transparent degradable film heater of an embedded silver nanowire annular conductive network is prepared by the method.
The sheet resistance of the film heater is adjusted by changing the amount of the sprayed silver nanowires, so that the film heaters with different sheet resistances of 0.1-500 omega/sq are realized, and the film heaters with different transparencies and heating performances are obtained, thereby better meeting the requirements of different application fields.
The flexible transparent degradable film heater of the embedded silver nanowire annular conductive network has the following technical advantages and characteristics:
1. according to the preparation method, the silver nanowire solution is sprayed on the surface of the polymer film substrate by adjusting the concentration of the silver nanowire solution, the size of a nozzle of spraying equipment and the pressure of carrier gas, and the silver nanowires in the silver nanowire solution are driven to the edge position from the center position under the action of capillary flow to form a regular silver nanowire coffee ring shape; and drying to obtain the silver nanowire annular conductive network film on the surface of the polymer film, wherein the obtained film heater has uniform sheet resistance, so that the film heater has uniform heating performance and excellent long-time stable and cyclic heating performance.
2. The film heater can adjust the transparency and the heating performance of the film heater by changing the amount of the sprayed silver nanowires, and better meets the requirements of different application fields.
3. The film heater is friendly to the natural environment, can be naturally degraded, is easy to treat after being used, has low cost, does not pollute the ecological environment, and is beneficial to the environmental protection and sustainable development.
4. The film heater of the invention adopts PLA as the substrate, has low manufacturing cost, and ensures that the film heater has the excellent characteristics of flexibility, transparency, degradability and easy processing and recycling.
5. The film heater can adjust the heating performance of the heater by changing the magnitude of the voltage applied to two ends of the film, thereby better meeting the requirements of different application fields.
6. The film heater can meet the requirements of most application fields within the heating temperature range, is particularly suitable for the medical field, and is compared with the traditional film heater.
7. The film heater provided by the invention has the advantages of simple process, low cost, excellent performance, good biocompatibility and antibacterial property, and is beneficial to application to human bodies.
Advantages of additional aspects of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention.
Drawings
FIG. 1 is a schematic view of the process of the present invention for preparing a novel flexible transparent degradable film heater;
FIG. 2 is an optical microscope photograph of the thin film heater prepared in example 1;
FIG. 3 is a scanning electron microscope photograph of the thin film heater prepared in example 1;
FIG. 4 is a graph showing a test pattern of sheet resistance and transparency of a thin film heater to which experimental example 1 is applied;
FIG. 5 is a graph showing a test of sheet resistance of a thin film heater to which experimental example 2 was applied;
FIG. 6 is a graph showing surface temperature rise curves at different voltages using the thin film heater of Experimental example 3;
FIG. 7 is a graph showing the continuous heating at a voltage of 2.5V using the thin film heater of Experimental example 3;
FIG. 8 is a graph showing a heating-cooling cycle at a voltage of 2.5V using the thin film heater of Experimental example 3;
FIG. 9 is a graph showing a test of sheet resistance of a large area thin film heater in application Experimental example 4;
FIG. 10 is a graph showing surface temperature rise at different voltages using the large-area thin film heater of Experimental example 4.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
Example 1:
the preparation method of the flexible transparent degradable film heater with the embedded silver nanowire annular conductive network comprises the following specific steps of:
(1) preparing silver nanowire mother liquor: adding silver nanowires into isopropanol, and uniformly stirring to obtain silver nanowire mother liquor, wherein the concentration of the silver nanowires in the silver nanowire mother liquor is 10 mg/ml;
preparing a PLA solution: according to the mass ratio of 1: 10, mixing and stirring the levorotatory polylactic acid and dichloromethane for 6 hours to obtain a polylactic acid (PLA) solution;
(2) adjusting the concentration of the silver nanowire solution to 0.2mg/ml by taking a silver nanowire mother solution grade solvent, adjusting the pressure intensity of a carrier gas and the size of a nozzle of spraying equipment, spraying the silver nanowire solution on the surface of a polytetrafluoroethylene film substrate, wherein the diameter of the nozzle of the spraying equipment is 0.5mm, the distance from the nozzle to a polymer film is 15cm, the carrier gas is high-purity nitrogen, the pressure intensity of the carrier gas is 0.3Mpa, the spraying thickness is 0.002mm, and the pressure intensity of the carrier gas is 2 x 2cm25.3mL of silver nanowire solution is sprayed on the substrate;
under the action of capillary flow, the silver nanowires in the silver nanowire solution are driven to the edge position from the central position to form a silver nanowire coffee ring shape, so that a silver nanowire annular conductive network is obtained, and a silver nanowire annular conductive network film is formed on the polymer film after drying;
(3) spin-coating a PLA solution on the surface of the dried silver nanowire by using a spin coater; the rotating speed of a spin coater is 800rpm when the PLA solution is spin-coated, and the spin coating time is 60s
(4) Heating the spin-coated film material in an oven to solidify the liquid flexible substrate, wherein the heating temperature is 60 ℃, the heating time is 15h, and peeling the PLA film and the substrate after cooling to obtain the flexible transparent degradable film heater of the embedded silver nanowire annular conductive network; the average sheet resistance of the thin film heater was 9 Ω/sq.
Through the flow schematic diagram of the film heater, the preparation process is simple, the requirements on experimental equipment, materials and environment are low, the cost is high, the controllability is high, the repeatability is high, and the large-scale batch production can be realized.
An electron microscope image and a scanning electron microscope image of the thin film heater manufactured in example 1 are respectively shown in fig. 2 and fig. 3, which illustrate that the silver nanowire conductive network is in a ring structure and is embedded in the flexible substrate, so as to obtain the flexible transparent degradable thin film heater with the embedded silver nanowire ring conductive network.
Example 2:
the preparation process is the same as that described in example 1, except that:
in the step (1), preparing a PLA solution: according to the mass ratio of 1: 15, mixing and stirring the levorotatory polylactic acid and dichloromethane for 7 hours to obtain a polylactic acid (PLA) solution. The rest was carried out as in example 1.
Example 3:
the preparation process is the same as that described in example 1, except that:
in the step (1), preparing a PLA solution: according to the mass ratio of 1: 20, mixing and stirring the levorotatory polylactic acid and dichloromethane for 8 hours to obtain a polylactic acid (PLA) solution.
In the step (2), taking a silver nanowire mother liquor-level solvent to adjust the concentration of the silver nanowire solution to 1.3 mg/ml;
the rest was carried out as in example 1.
Example 4:
the preparation process is the same as that described in example 1, except that:
in the step (1), preparing a PLA solution: according to the mass ratio of 1: 30, and mixing and stirring the levorotatory polylactic acid and dichloromethane for 9 hours to obtain a polylactic acid (PLA) solution.
In the step (2), taking a silver nanowire mother liquor-level solvent to adjust the concentration of the silver nanowire solution to 3.5 mg/ml;
the rest was carried out as in example 1.
Example 5:
the preparation process is the same as that described in example 1, except that:
in the step (1), preparing a PLA solution: according to the mass ratio of 1: 35, mixing and stirring the levorotatory polylactic acid and the dichloromethane for 12 hours to obtain a polylactic acid (PLA) solution.
In the step (2), taking a silver nanowire mother liquor-level solvent to adjust the concentration of the silver nanowire solution to 5.5 mg/ml;
the rest was carried out as in example 1.
Example 6:
the preparation process is the same as that described in example 1, except that:
in the step (2), the diameter of a nozzle of the spraying equipment is 0.8mm, the distance from the nozzle to the polymer film is 25cm, the carrier gas is high-purity nitrogen, the pressure of the carrier gas is 0.4Mpa, and the spraying thickness is 0.002 mm;
the rest was carried out as in example 1.
Example 7:
the preparation process is the same as that described in example 1, except that:
in the step (2), the diameter of a nozzle of the spraying equipment is 2mm, the distance from the nozzle to the polymer film is 40cm, the carrier gas is high-purity nitrogen, the pressure intensity of the carrier gas is 0.6Mpa, and the spraying thickness is 0.002 mm;
the rest was carried out as in example 1.
Application Experimental example 1
The spraying amount of the silver nanowires sprayed in example 1 was changed, namely, the spraying amount is 2 x 2cm2The amount of the silver nanowire solution sprayed on the substrate is respectively 2mL, 3mL, 4mL, 5mL and 6 mL; the film heaters with different transparencies and different sheet resistances are obtained respectively, and the sheet resistance of the film heater can be adjusted by adjusting the spraying amount of the sprayed silver nanowires, and the obtained film heater is shown in figure 4.
Application Experimental example 2
The method of example 1 was followed at 2 x 2cm25mL of silver nanowire solution is sprayed on the substrateThe average sheet resistance of the obtained thin film heater is 10.03 omega/sq.
The sheet resistance at different positions on the thin film heater was measured, and the sheet resistance at different positions was shown in fig. 5, and the average sheet resistance was 10.03 Ω/sq, indicating that the thin film heater had a uniform sheet resistance and thus could uniformly generate heat when a voltage was applied across the thin film heater.
Application Experimental example 3
The method of example 1 was followed at 2 x 2cm25.2mL of silver nanowire solution is sprayed on the substrate, and the average sheet resistance of the obtained thin film heater is 9.1 omega/sq.
The surface temperature rise curves under the condition of applying different voltages to the two ends of the thin film heater are shown in fig. 6, and the test results are shown in fig. 6, which illustrates that different heating effects can be obtained by applying different voltages. Therefore, different heating effects can be obtained by changing the voltage, so that the film heater can better meet the requirements of different application fields. As shown in FIG. 7, when the thin film heater is continuously heated under the condition that 2.5V voltage is applied across the two ends of the thin film heater for 2h, the heating temperature of the thin film heater is always kept at about 105 ℃, which shows that the device has excellent continuous and stable heating performance. The heating and cooling cycles (20s one cycle) were performed under the condition that 2.5V was applied across the thin film heater for 4000s, and the device still worked normally after 200 cycles, as shown in fig. 8, which illustrates that the device has excellent heating and cooling cycle performance.
Application Experimental example 4
In 5X 5cm by the method of example 1216mL of silver nanowire solution is sprayed on the substrate, and the average sheet resistance of the obtained thin film heater is 9.6 omega/sq.
The sheet resistance was measured at different positions on the thin film heater, and the results are shown in fig. 9, which shows that the thin film heater has a uniform sheet resistance, and the average sheet resistance is 9.6 Ω/sq, and thus heat can be uniformly generated when a voltage is applied across the thin film heater. The surface heating curves for different magnitudes of voltage applied across the thin film heater are shown in fig. 10. Therefore, different heating effects can be obtained by applying different voltages.
The thin film heater provided by the embodiment has the advantages of simple preparation process and excellent heating performance, and the transparency and the heating performance of the thin film heater can be adjusted by changing the amount of the sprayed silver nanowires, so that the requirements of different application fields can be better met.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. 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)
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| CN202111201278.1A CN114126116A (en) | 2021-10-15 | 2021-10-15 | Flexible, transparent and degradable thin film heater with embedded silver nanowire annular conductive network and its preparation method and application |
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| CN111403107A (en) * | 2020-03-12 | 2020-07-10 | 重庆文理学院 | A kind of degradable silver nanowire/all-stereo composite polylactic acid transparent conductive film and preparation method thereof |
| CN112053800A (en) * | 2020-07-31 | 2020-12-08 | 山东大学 | An embedded high temperature resistant transparent conductive film, its preparation method and application |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111403107A (en) * | 2020-03-12 | 2020-07-10 | 重庆文理学院 | A kind of degradable silver nanowire/all-stereo composite polylactic acid transparent conductive film and preparation method thereof |
| CN112053800A (en) * | 2020-07-31 | 2020-12-08 | 山东大学 | An embedded high temperature resistant transparent conductive film, its preparation method and application |
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