CN110681553A - Flexible transparent heater based on AgNWs and preparation method thereof - Google Patents
Flexible transparent heater based on AgNWs and preparation method thereof Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/02—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to macromolecular substances, e.g. rubber
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
- B05D1/40—Distributing applied liquids or other fluent materials by members moving relatively to surface
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
- B05D5/12—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain a coating with specific electrical properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/24—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials for applying particular liquids or other fluent materials
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/50—Multilayers
- B05D7/56—Three layers or more
- B05D7/58—No clear coat specified
- B05D7/584—No clear coat specified at least some layers being let to dry, at least partially, before applying the next layer
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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
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2201/00—Polymeric substrate or laminate
- B05D2201/02—Polymeric substrate
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2451/00—Type of carrier, type of coating (Multilayers)
Abstract
The AgNWs-based flexible transparent heater prepared by using a spin-coating method has the advantages of excellent performance, low cost, simple process and high repeatability. The transmittance of the AgNWs-based flexible transparent heater on the PET substrate prepared by the invention is about 88% when the wavelength is 550nm, the square resistance is about 12 omega/sq, and the steady-state temperature is 170 ℃ when 5V voltage is applied.
Description
Technical Field
The invention belongs to the field of functional thin film materials, and particularly relates to a flexible transparent heater based on AgNWs and a preparation method thereof.
Background
The transparent conductive film is one of electronic devices commonly used in life of people, and can be used for flexible solar cells, touch displays, electronic skins, nano generators, intelligent windows and the like. Meanwhile, the flexible conductive film is also an important temperature regulator as a resistance type heater. As an emerging application technology, the flexible transparent resistance heater is expected to become a wearable thermal therapy device combined with a human body. At present, the transparent conductive thin film material mainly used is Indium Tin Oxide (ITO), but indium element is expensive, so that the material cost is increased, and secondly, the brittleness of the ITO causes that the material cannot meet the requirement on flexibility under many conditions.
Silver nanowires have excellent electrical conductivity and mechanical strength, while silver is stored in a large amount. Conductive films containing silver nanowires have many advantages: the preparation process is simple, low in cost, good in repeatability and the like. These advantages have led to extensive research into conductive films comprising silver nanowires, which are the most promising materials for replacing ITO conductive films, and also have led to the possibility of applying silver nanowire conductive films to flexible transparent heaters. However, the transparent conductive film prepared by using silver nanowires has the defects of poor adhesion with a substrate, large sheet resistance and the like, which greatly limits the application of the transparent conductive film.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a flexible transparent heater based on AgNWs and a preparation method thereof, and solves the problems in the prior art that the cost of an ITO film is high, the adhesion of a silver nanowire transparent conductive film to a substrate is poor, the sheet resistance is high and the like.
The technical scheme of the invention is as follows:
a preparation method of a flexible transparent heater based on AgNWs comprises the following steps:
(1) preparing a silver nanowire solution, PEDOT (PSS solution), PVA (polyvinyl acetate) solution and a substrate;
(2) after the step (1) is finished, spin-coating AgNWs/absolute ethyl alcohol mixed solution on the substrate by using a spin coater, and naturally drying;
(3) after the step (2) is finished, spin-coating PEDOT (PSS) mixed solution on the substrate by using a spin coater, and drying by using an oven;
(4) and (4) after the step (3) is finished, spin-coating the PVA mixed solution by using a spin coater, and drying.
The silver nanowire solution in the step (1) is prepared by uniformly mixing silver nanowires and absolute ethyl alcohol to prepare a solution with the concentration of 1.5-1.8 mg/ml.
The step (1) of the PEDOT: PSS (poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid) solution refers to that the PEDOT: PSS is uniformly mixed with deionized water, absolute ethyl alcohol and ethylene glycol according to a proportion and is subjected to ultrasonic treatment, wherein the weight ratio of the PEDOT: PSS: the optimal ratio of the deionized water to the absolute ethyl alcohol to the ethylene glycol is 1:0.5:0.3:0.2, and the optimal ultrasonic treatment time is 10-30 minutes.
The PVA solution in the step (1) is prepared by mixing PVA and deionized water according to the proportion of 1:10, stirring by using magnetic force and heating to 90 ℃ to completely dissolve the PVA.
The substrate in the step (1) is a PET, PC or PVC flexible transparent substrate, and is ultrasonically washed by absolute ethyl alcohol and deionized water before use and is dried by high-purity nitrogen.
And (3) uniformly coating the AgNWs/absolute ethyl alcohol mixed solution in the step (2) on the surface of the substrate, wherein the rotating speed of the spin coater is 650-1500 rpm, and the time is 10-30 s.
And (3) uniformly coating the mixed solution of PEDOT and PSS on the surface of the AgNWs layer, wherein the rotating speed of a glue homogenizing machine is 2000-4000 rpm, the time is 40-120 s, the temperature of an oven is 120-150 ℃, and the time is 30-60 min.
The PVA mixed solution in the step (4) needs to be uniformly coated on the surface of the PEDOT-PSS layer; the rotating speed of the spin coater is 2000 rpm-4000 rpm, and the time is 40 s-120 s. And after the spin coating is finished, drying by using a heating plate, wherein the temperature of the heating plate is 100 ℃.
The AgNWs flexible transparent heater prepared by the preparation method is used for preparing the AgNWs flexible transparent heater.
The invention has the beneficial effects that: the AgNWs-based flexible transparent heater prepared by the spin-coating method has the advantages of excellent performance, low cost, simple process and high repeatability. The transmittance of the prepared AgNWs-based flexible transparent heater is about 88% when the wavelength is 550nm, the square resistance is about 12 omega/sq, and the steady-state temperature is 170 ℃ when 5V voltage is applied.
Drawings
FIG. 1 is a schematic diagram of an AgNWs-based flexible transparent heater on a PET substrate; wherein: 1-a PVA layer; 2-PEDOT: a PSS layer; 3-AgNWs layer; 4-a substrate;
FIG. 2 is a graph of the optical transmission performance (UV-Vis) at a square resistance of 14 Ω/sq for a sample based on an AgNWs flexible transparent heater on a PET substrate.
Detailed Description
The present invention is further illustrated below with reference to specific examples, which are intended to be illustrative only and not to limit the scope of the invention.
Example 1
1. Tearing off the protective films on the two sides of the PC substrate, then ultrasonically cleaning the PC substrate and the quartz plate by using absolute ethyl alcohol and deionized water in sequence, and drying by using high-purity nitrogen for later use.
2. Preparing a mixed solution of silver nanowires and absolute ethyl alcohol. The self-made silver nanowires are uniformly mixed with absolute ethyl alcohol to prepare a mixed solution with the concentration of 1.7 mg/ml.
3. Preparing PEDOT, PSS mixed solution and silver nanowire solution. PSS, PEDOT: deionized water: anhydrous ethanol: the ethylene glycol was mixed uniformly in a ratio of 1:0.5:0.3:0.2 and sonicated for 20 minutes.
4. A PVA mixed solution was prepared. PVA and deionized water were mixed in a ratio of 1:10 and dissolved completely by magnetic stirring. Wherein the magnetic stirring setting speed is 400rpm, and the temperature is 90 ℃.
5. And adsorbing the PC substrate on a spin coater, setting the parameters to be 750rpm and the time to be 15s, spin-coating the AgNWs mixed solution, and naturally drying after the spin coating is finished.
6. And 5, after the step 5 is finished, setting parameters of a spin coater at 2000rpm for 60s, spin-coating the PEDOT-PSS mixed solution, putting the spin-coated PEDOT-PSS mixed solution into an oven to be dried for 50min at 150 ℃, taking out the spin-coated PEDOT-PSS mixed solution, and naturally cooling the spin-coated PEDOT-PSS mixed solution to room temperature.
7. And 6, after the spin coating is finished, setting parameters of the spin coater to be 2000rpm, setting the time to be 60s, spin-coating the PVA mixed solution, heating the mixture by using a heating plate to dry the mixture at 100 ℃ after the spin coating is finished, taking down the mixture after the drying, and naturally cooling the mixture to room temperature.
The optical transmittance of the sample based on the AgNWs flexible transparent heater on the PC substrate is 87% at the wavelength of 550nm, the square resistance is 13 omega/sq, and the steady-state temperature is 130 ℃ when 4V voltage is applied.
Example 2
1. Tearing off the protective films on the two sides of the PET substrate, then ultrasonically cleaning the PET substrate and the quartz plate by using absolute ethyl alcohol and deionized water in sequence, and blow-drying by using high-purity nitrogen for later use.
2. Preparing a mixed solution of silver nanowires and absolute ethyl alcohol. The self-made silver nanowires are uniformly mixed with absolute ethyl alcohol to prepare a mixed solution with the concentration of 1.6 mg/ml.
3. Preparing PEDOT, PSS mixed solution and silver nanowire solution. PSS, PEDOT: deionized water: anhydrous ethanol: the ethylene glycol was mixed uniformly in a ratio of 1:0.5:0.3:0.2 and sonicated for 30 minutes.
4. A PVA mixed solution was prepared. PVA and deionized water were mixed in a ratio of 1:10 and dissolved completely by magnetic stirring. Wherein the magnetic stirring setting speed is 400rpm, and the temperature is 90 ℃.
5. And adsorbing the PET substrate on a spin coater, setting the parameters at 800rpm for 10s, spin-coating the AgNWs mixed solution, and naturally drying after the spin coating is finished.
6. And 5, after the step 5 is finished, setting parameters of a spin coater at 2000rpm for 60s, spin-coating the PEDOT-PSS mixed solution, putting the spin-coated PEDOT-PSS mixed solution into an oven to be dried for 50min at 150 ℃, taking out the spin-coated PEDOT-PSS mixed solution, and naturally cooling the spin-coated PEDOT-PSS mixed solution to room temperature.
7. And 6, after the spin coating is finished, setting parameters of a spin coater to be 2000rpm, carrying out spin coating on the PVA mixed solution for 30s, heating the PVA mixed solution by using a heating plate to 100 ℃ for drying after the spin coating is finished, taking down the PVA mixed solution after the drying, and naturally cooling the PVA mixed solution to room temperature.
The optical transmittance of a sample based on an AgNWs flexible transparent heater on the PET substrate is 89% at the wavelength of 550nm, the square resistance is 14 omega/sq, and the steady-state temperature is 150 ℃ when 5V voltage is applied.
Example 3
1. Tearing off the protective films on the two sides of the PET substrate, then ultrasonically cleaning the PET substrate and the quartz plate by using absolute ethyl alcohol and deionized water in sequence, and blow-drying by using high-purity nitrogen for later use.
2. Preparing a mixed solution of silver nanowires and absolute ethyl alcohol. The self-made silver nanowires are uniformly mixed with absolute ethyl alcohol to prepare a mixed solution with the concentration of 1.8 mg/ml.
3. Preparing PEDOT, PSS mixed solution and silver nanowire solution. PSS, PEDOT: deionized water: anhydrous ethanol: the ethylene glycol was mixed uniformly in a ratio of 1:0.5:0.3:0.2 and sonicated for 20 minutes.
4. A PVA mixed solution was prepared. PVA and deionized water were mixed in a ratio of 1:10 and dissolved completely by magnetic stirring. Wherein the magnetic stirring setting speed is 400rpm, and the temperature is 90 ℃.
5. And adsorbing the PET substrate on a spin coater, setting the parameters to be 1000rpm and the time to be 20s, spin-coating the AgNWs mixed solution, and naturally drying after the spin coating is finished.
6. And 5, after the step 5 is finished, setting parameters of a spin coater at 2000rpm for 60s, spin-coating the PEDOT-PSS mixed solution, putting the spin-coated PEDOT-PSS mixed solution into an oven to be dried for 50min at 150 ℃, taking out the spin-coated PEDOT-PSS mixed solution, and naturally cooling the spin-coated PEDOT-PSS mixed solution to room temperature.
7. And 6, after the spin coating is finished, setting parameters of the spin coater to be 2000rpm, setting the time to be 60s, spin-coating the PVA mixed solution, heating the mixture by using a heating plate to dry the mixture at 100 ℃ after the spin coating is finished, taking down the mixture after the drying, and naturally cooling the mixture to room temperature.
The optical transmittance of a sample based on an AgNWs flexible transparent heater on the PET substrate is 85% at the wavelength of 550nm, the square resistance is 11 omega/sq, and the steady-state temperature is 170 ℃ when 5V voltage is applied.
Example 4
1. Tearing off the protective films on the two sides of the PET substrate, then ultrasonically cleaning the PET substrate and the quartz plate by using absolute ethyl alcohol and deionized water in sequence, and blow-drying by using high-purity nitrogen for later use.
2. Preparing a mixed solution of silver nanowires and absolute ethyl alcohol. The self-made silver nanowires are uniformly mixed with absolute ethyl alcohol to prepare a mixed solution with the concentration of 1.7 mg/ml.
3. Preparing PEDOT, PSS mixed solution and silver nanowire solution. PSS, PEDOT: deionized water: anhydrous ethanol: the ethylene glycol was mixed uniformly in a ratio of 1:0.5:0.3:0.2 and sonicated for 20 minutes.
4. A PVA mixed solution was prepared. PVA and deionized water were mixed in a ratio of 1:10 and dissolved completely by magnetic stirring. Wherein the magnetic stirring setting speed is 400rpm, and the temperature is 90 ℃.
5. And adsorbing the PET substrate on a spin coater, setting the parameters to be 750rpm and the time to be 20s, spin-coating the AgNWs mixed solution, and naturally drying after the spin coating is finished.
6. And 5, after the step 5 is finished, setting parameters of a spin coater at 2000rpm for 60s, spin-coating the PEDOT-PSS mixed solution, putting the spin-coated PEDOT-PSS mixed solution into an oven to be dried for 50min at 150 ℃, taking out the spin-coated PEDOT-PSS mixed solution, and naturally cooling the spin-coated PEDOT-PSS mixed solution to room temperature.
7. And 6, after the spin coating is finished, setting parameters of the spin coater to be 2000rpm, setting the time to be 60s, spin-coating the PVA mixed solution, heating the mixture by using a heating plate to dry the mixture at 100 ℃ after the spin coating is finished, taking down the mixture after the drying, and naturally cooling the mixture to room temperature.
The optical transmittance of a sample based on an AgNWs flexible transparent heater on the PET substrate is 88 percent at the wavelength of 550nm, the square resistance is 12 omega/sq, and the steady-state temperature is 165 ℃ when 5V voltage is applied.
Example 5
8. Tearing off the protective films on the two sides of the PVC substrate, then ultrasonically cleaning the PVC substrate and the quartz plate by using absolute ethyl alcohol and deionized water in sequence, and blow-drying by using high-purity nitrogen for later use.
9. Preparing a mixed solution of silver nanowires and absolute ethyl alcohol. The self-made silver nanowires are uniformly mixed with absolute ethyl alcohol to prepare a mixed solution with the concentration of 1.7 mg/ml.
10. Preparing PEDOT, PSS mixed solution and silver nanowire solution. PSS, PEDOT: deionized water: anhydrous ethanol: the ethylene glycol was mixed uniformly in a ratio of 1:0.5:0.3:0.2 and sonicated for 20 minutes.
11. A PVA mixed solution was prepared. PVA and deionized water were mixed in a ratio of 1:10 and dissolved completely by magnetic stirring. Wherein the magnetic stirring setting speed is 400rpm, and the temperature is 90 ℃.
12. And adsorbing the PVC substrate on a spin coater, setting the parameter at 750rpm for 15s, spin-coating the AgNWs mixed solution, and naturally drying after the spin coating is finished.
13. And 5, after the step 5 is finished, setting parameters of a spin coater at 2000rpm for 60s, spin-coating the PEDOT-PSS mixed solution, putting the spin-coated PEDOT-PSS mixed solution into an oven to be dried for 50min at 150 ℃, taking out the spin-coated PEDOT-PSS mixed solution, and naturally cooling the spin-coated PEDOT-PSS mixed solution to room temperature.
14. And 6, after the spin coating is finished, setting parameters of the spin coater to be 2000rpm, setting the time to be 60s, spin-coating the PVA mixed solution, heating the mixture by using a heating plate to dry the mixture at 100 ℃ after the spin coating is finished, taking down the mixture after the drying, and naturally cooling the mixture to room temperature.
The optical transmittance of a sample based on an AgNWs flexible transparent heater on the PVC substrate is 87% at the wavelength of 550nm, the square resistance is 13 omega/sq, and the steady-state temperature is 105 ℃ when 2V voltage is applied.
The performance of the AgNWs-based flexible transparent heater obtained by detection is shown in Table 1.
Table 1:
the invention is not limited to the embodiments described above, many variations in detail are possible without departing from the scope and spirit of the invention.
Claims (10)
1. A preparation method of a flexible transparent heater based on AgNWs is characterized by comprising the following steps:
(1) preparing a silver nanowire solution, PEDOT (PSS solution), PVA (polyvinyl acetate) solution and a substrate;
(2) after the step (1) is finished, spin-coating AgNWs/absolute ethyl alcohol mixed solution on the substrate by using a spin coater, and naturally drying;
(3) after the step (2) is finished, spin-coating PEDOT (PSS) mixed solution on the substrate by using a spin coater, and drying by using an oven;
(4) and (4) after the step (3) is finished, spin-coating the PVA mixed solution by using a spin coater, and drying.
2. The preparation method of the AgNWs-based flexible transparent heater according to claim 1, wherein the silver nanowire solution in the step (1) is prepared by uniformly mixing silver nanowires and absolute ethyl alcohol to prepare a solution with the concentration of 1.5-1.8 mg/ml.
3. The preparation method of the AgNWs-based flexible transparent heater according to claim 1, wherein the step (1) of the PEDOT: PSS solution is that the PEDOT: PSS solution is uniformly mixed with deionized water, absolute ethyl alcohol and ethylene glycol according to a certain proportion and is subjected to ultrasonic treatment, wherein the weight ratio of the PEDOT: PSS: (deionized water + absolute ethanol + ethylene glycol) is 1: 1-3: 1, and the ultrasonic treatment time is preferably 10-30 minutes.
4. The method for preparing an AgNWs-based flexible transparent heater according to claim 1, wherein the PVA solution in step (1) is prepared by mixing PVA and deionized water in a ratio of 1:10, and stirring and heating to 90 ℃ by using magnetic force to dissolve the PVA completely.
5. The preparation method of the AgNWs-based flexible transparent heater according to claim 1, wherein the substrate in the step (1) is a PET, PC or PVC flexible transparent substrate, and is ultrasonically washed by absolute ethyl alcohol and deionized water before use and is dried by high-purity nitrogen.
6. The preparation method of the AgNWs-based flexible transparent heater according to claim 1, wherein the AgNWs/absolute ethyl alcohol mixed solution in the step (2) needs to be uniformly coated on the surface of the substrate, the rotation speed of the spin coater is 650-1500 rpm, and the time is 10-30 s.
7. The preparation method of the AgNWs-based flexible transparent heater according to claim 1, wherein the PEDOT/PSS mixed solution in the step (3) is required to be uniformly coated on the surface of the AgNWs layer, the rotating speed of a spin coater is 2000-4000 rpm, the time is 40-120 s, the temperature of an oven is 120-150 ℃, and the time is 30-60 min.
8. The preparation method of the AgNWs-based flexible transparent heater according to claim 1, wherein the PVA mixed solution in the step (4) is required to be uniformly coated on the surface of the PEDOT PSS layer; the rotating speed of the spin coater is 2000 rpm-4000 rpm, and the time is 40 s-120 s.
9. The method for preparing the AgNWs-based flexible transparent heater according to claim 8, wherein the heating plate is used for drying after the spin coating is finished, and the temperature of the heating plate is 100 ℃.
10. The AgNWs flexible transparent heater prepared by the AgNWs flexible transparent heater-based preparation method according to any one of claims 1 to 9.
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| CN113963844A (en) * | 2021-10-12 | 2022-01-21 | 浙江大学 | Flexible silver nanowire-based composite transparent film heater and preparation method thereof |
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Application publication date: 20200114 |