CN113867031A - Elastic stretchable intelligent light adjusting film based on silver nanowire electrode and preparation method thereof - Google Patents
Elastic stretchable intelligent light adjusting film based on silver nanowire electrode and preparation method thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims description 18
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- 239000011159 matrix material Substances 0.000 claims abstract description 16
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 44
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- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells
- G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
- G02F1/1333—Constructional arrangements; Manufacturing methods
- G02F1/1334—Constructional arrangements; Manufacturing methods based on polymer dispersed liquid crystals, e.g. microencapsulated liquid crystals
Abstract
The invention discloses an elastic stretchable intelligent light adjusting film based on a silver nanowire electrode. The light adjusting film comprises a polymer dispersed liquid crystal layer (1) positioned in the middle layer, an enhancement layer (2), a silver nanowire layer (3) and a transparent base layer (4) which are sequentially arranged from inside to outside at two ends by taking the polymer dispersed liquid crystal layer (1) as a center, wherein the two enhancement layers (2) are respectively provided with a power supply connecting structure (5) connected with an external control switch and a driving power supply; the silver nanowire layer (3) has ductility and serves as a conductive electrode, and finally a 7-layer sandwich structure of transparent matrix layer/silver nanowire layer/reinforcing layer/polymer dispersed liquid crystal layer/reinforcing layer/silver nanowire layer/transparent matrix layer is formed. The intelligent light modulation film prepared by the invention has the characteristics of good flexibility, rich applicable scenes, stable and reliable light modulation performance, low cost, convenience in construction and long service life, and can control the intensity of transmitted light through low voltage.
Description
Technical Field
The invention relates to the technical field of intelligent light adjusting films, in particular to a design and a preparation method of an elastic stretchable intelligent light adjusting film based on a silver nanowire electrode.
Background
The intelligent light regulating film is one new kind of electronic light regulating and controlling product and has the basic structure including two transparent conducting electrodes with one polymer dispersed liquid crystal layer sandwiched between them. The working mechanism of the intelligent light adjusting film is as follows: in the electrified state, the liquid crystal molecules are regularly and orderly arranged, at the moment, light can penetrate through the liquid crystal molecules, and the light adjusting film is in a transparent state; under the power-off state, the liquid crystal molecules are irregularly arranged in a mess, light cannot pass through the liquid crystal molecules at the moment, and the light adjusting film is in an opaque state. At present, transparent electrodes adopted by intelligent light modulation films in the market are basically ITO (indium tin oxide) films. However, since indium is a rare metal and the storage amount is small, ITO is expensive. Moreover, ITO as an inorganic material has a large brittleness and a strong mechanical rigidity, which limits its application in the flexible field.
Metal nanowires, especially silver nanowires (AgNWs), have good flexibility and conductivity, and are considered as the most promising materials to replace ITO. If AgNWs-based conductive materials can be combined with liquid crystal materials, the problem of shortage of flexible light modulation films on the market at present can be solved by preparing the flexible composite film with light modulation performance. However, the problem that the traditional AgNWs is not stable for a long time in an electrolyte environment still needs to be overcome by simply adopting the traditional AgNWs as an electrode of the intelligent light modulation film, and the electrolyte can corrode the AgNWs to influence the structural stability of the AgNWs. In addition, continuous current in the electrified state can cause the temperature of partial AgNWs area to be overhigh, so that silver wires are broken to become droplet balls, and the linear structure is lost, so that the conductivity is lost.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides an elastic stretchable intelligent light adjusting film based on a silver nanowire electrode and a preparation method thereof. The product of the invention has good flexibility, stretching property, low cost, simple structure and long service life. The method of the invention is used for assembling layer by layer, and the bonding force between layer structures is improved, thereby improving the structural stability and the conductive stability of the product.
The technical scheme of the invention is as follows: an elastic stretchable intelligent light adjusting film based on a silver nanowire electrode comprises the following structures: the polymer dispersed liquid crystal layer is positioned in the middle layer, and the enhancement layer, the silver nanowire layer and the transparent matrix layer are respectively and sequentially arranged on two sides of the polymer dispersed liquid crystal layer from near to far; the two enhancement layers are respectively provided with a power supply connecting structure which is connected with an external control switch and a driving power supply; the silver nanowire layer is malleable and serves as a conductive electrode.
Furthermore, the diameter of the silver nanowires in the silver nanowire layer is 20-50 nm.
Furthermore, the sheet resistance of the silver nanowire layer is 20-100 omega/□.
Further, the reinforcing layer is a metal layer having a higher reducibility than metallic silver under the same reaction conditions.
Furthermore, the reinforcing layer is a metal nickel layer or a metal chromium layer.
Furthermore, the transparent substrate layer is a transparent thermoplastic elastic material layer, and the transparent thermoplastic elastic material is one or a composite of more of polyurethane thermoplastic elastic materials, styrene thermoplastic elastic materials, polyolefin thermoplastic elastic materials and polyamide thermoplastic elastic materials.
Further, the power supply connection structure is a conductive material combined with the enhancement layer, and the conductive material is copper foil or conductive cloth.
The invention also provides a preparation method of the elastic stretchable intelligent light adjusting film based on the silver nanowire electrode, which comprises the following steps:
1) pretreatment of transparent substrate layers
Sequentially carrying out ultrasonic treatment on the transparent substrate layer in acetone, ethanol and deionized water for 10-30 min to remove impurities on the surface;
2) compounding of silver nanowire layer and transparent substrate layer
Coating the silver nanowire conductive ink on the surface of the transparent matrix layer in the step by a wet coating method, drying and curing, removing the solvent to obtain a silver nanowire layer, and performing hot-pressing treatment on the transparent matrix layer coated with the silver nanowire layer to obtain a silver nanowire layer and a transparent matrix layer which are compounded, namely a transparent conductive film;
3) preparation of conductive films containing enhancement layers
Electroplating the surface of the transparent conductive film obtained in the step by adopting an electrochemical method to obtain the transparent conductive film containing the enhancement layer;
4) preparation of light-adjusting film
And (3) superposing the two transparent conductive films containing the enhancement layers obtained in the step(s) to enable the enhancement layers to face oppositely, filling polymer dispersed liquid crystal between the two enhancement layers, and sealing the edges by using light curing glue to obtain the elastic stretchable intelligent light adjusting film based on the silver nanowire electrode.
Further, the drying and curing temperature in the step 2) is 40-80 ℃, and the time is 10-60 min; the temperature of the hot pressing treatment is 100-200 ℃, and the pressure is 0.1-0.8 Mpa.
Further, in the electroplating process of the step 3): the electroplating solution is a mixed solution of 0.1-10 mol/L boric acid, 0.1-10 mol/L chloride of the metal of the enhancement layer and 0.1-10 mol/L ethylenediamine hydrochloride; the electroplating current is 0.01-0.1A, and the electroplating time is 1-10 s.
In the elastically stretchable intelligent light adjusting film based on the silver nanowire electrode, the silver nanowire layer plays a main conductive role, and the enhancement layer reduces the contact resistance among the silver nanowires to a certain extent; the diameter of the silver nanowires is a major contributor to the conductivity and transparency of the film. The thickness and the content of the enhancement layer are controlled by controlling the current and the electroplating time during electroplating, and because the adopted electroplating process has small nickel or chromium content and has small influence on the thickness of the enhancement layer on the diameter of the silver nanowire, the diameter of the silver nanowire does not include the thickness of the enhancement layer, namely the thickness of the enhancement layer can be ignored relative to the diameter of the silver nanowire.
The working principle of the invention is as follows: when the intelligent light adjusting film is electrified, liquid crystal molecules in the polymer dispersed liquid crystal layer are regularly and orderly arranged, at the moment, light can penetrate through the liquid crystal dispersed liquid crystal layer, and the light adjusting film is in a transparent state; when the power is turned off, the liquid crystal molecules in the polymer dispersed liquid crystal layer are irregularly arranged in a random mode, light cannot pass through the liquid crystal molecules at the moment, and the light adjusting film is in an opaque state. Therefore, the transmittance of the film can be intelligently regulated and controlled through the external electric field. The light control film needs to be constantly energized to maintain a transparent state. At this time, the enhancement layer covering the surface of the silver nanowire layer can protect the silver nanowire, the resistance of the transparent conductive film is reduced, and fusing failure of the silver nanowire caused by long-time electrification is avoided. Meanwhile, the reinforcing layer separates the silver nanowires from the polymer dispersed liquid crystal layer, and meanwhile, the metal material used by the reinforcing layer has stronger reducibility than silver under the same condition, so that the corrosion of the polymer dispersed liquid crystal layer to the silver nanowires can be weakened to a certain extent by a cathode protection method of a sacrificial anode, and the service life of the silver nanowire layer is prolonged.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the invention, the elastic stretchable intelligent light adjusting film is prepared by adopting the elastic stretchable transparent matrix and the silver nanowires, and the elastic stretchable light adjusting film has a simple forming mode and can be simultaneously applied to a flexible plane and a rigid plane.
2. According to the invention, the enhancement layer is adopted to protect the silver nanowires, so that the corrosion resistance of the silver nanowires is improved, and the structural stability is improved. Meanwhile, the enhancement layer can also reduce the contact resistance between the silver nanowires and improve the conductivity of the silver nanowire electrode.
Drawings
Fig. 1 is a schematic side view of an elastically stretchable intelligent light adjusting film based on a silver nanowire electrode in an embodiment of the present invention;
fig. 2 is a schematic top view of an elastically stretchable intelligent light adjusting film based on silver nanowire electrodes according to an embodiment of the present invention;
fig. 3 is a graph showing transmittance of an elastic stretchable transparent conductive film based on a silver nanowire electrode prepared by the methods provided in examples 1 to 4 of the present invention and comparative example 1;
FIG. 4 is a scanning electron micrograph and a power spectrum of an elastically stretchable transparent conductive film based on a silver nanowire electrode prepared by the methods provided in examples 1 to 3 of the present invention and comparative example 1; wherein (a1) is a scanning electron micrograph of the silver nanowire electrode-based elastically stretchable transparent conductive film obtained in comparative example 1; (a2) a spectrum of the elastically stretchable transparent conductive film based on the silver nanowire electrode obtained in comparative example 1; (b1) scanning electron micrographs of the elastically stretchable transparent conductive film based on the silver nanowire electrode obtained in example 1; (b2) is a spectrum diagram of the elastic stretchable transparent conductive film based on the silver nanowire electrode obtained in example 1; (c1) scanning electron micrographs of the elastically stretchable transparent conductive film based on the silver nanowire electrode obtained in example 2; (c2) is a spectrum of the elastically stretchable transparent conductive film based on the silver nanowire electrode obtained in example 2; (d1) scanning electron micrographs of the elastically stretchable transparent conductive film based on the silver nanowire electrode obtained in example 3; (d2) is a spectrum of the elastically stretchable transparent conductive film based on the silver nanowire electrode obtained in example 3;
fig. 5 is a graph of sheet resistance versus tensile elongation for an elastically stretchable transparent conductive film based on a silver nanowire electrode prepared by the methods provided in examples 1 to 3 of the present invention and comparative example 1;
in the figure: 1. a polymer dispersed liquid crystal layer; 2. an enhancement layer; 3. a silver nanowire layer; 4. a transparent substrate layer; 5. and a power supply connection structure.
Detailed Description
The invention is described in detail below with reference to the figures and the specific embodiments.
Example 1
A preparation method of an elastic stretchable intelligent light adjusting film based on a silver nanowire electrode comprises the following steps:
(1) pretreatment of transparent substrates
And (3) sequentially carrying out ultrasonic treatment on the transparent matrix in acetone, ethanol and deionized water for 30min to remove impurities on the surface.
(2) Preparation of transparent conductive film
The silver nanowire conductive ink is coated on the surface of a transparent substrate in a wet coating mode, and then dried and cured for 20min at the temperature of 60 ℃. And hot pressing the transparent substrate coated with the silver nanowire layer at 140 ℃ under the pressure of 0.8 Mpa.
(3) Preparation of conductive films containing enhancement layers
And (3) carrying out nickel plating on the surface of the transparent conductive film by adopting an electrochemical method, wherein the concentration of the electroplating solution is a mixed solution of 0.5mol/L boric acid, 1mol/L nickel chloride and 0.5mol/L ethylenediamine hydrochloride. The plating current used was 0.01A and the plating time was 10 s.
(4) Preparation of light-adjusting film
And filling polymer dispersed liquid crystal between the two transparent conductive films with the enhancement layers, and sealing edges by using light-curing glue to obtain the light-adjusting film.
The structure of the obtained product is shown in fig. 1 and 2, and as can be seen, the product comprises a polymer dispersed liquid crystal layer 1 positioned in the middle layer, and an enhancement layer 2, a silver nanowire layer 3 and a transparent matrix layer 4 which are arranged on two sides of the polymer dispersed liquid crystal layer 1 from near to far in sequence; the two enhancement layers 2 are respectively provided with a power supply connecting structure 5 which is connected with an external control switch and a driving power supply to form a sandwich structure of a transparent matrix layer 4/a silver nanowire layer 3/an enhancement layer 2/a polymer dispersed liquid crystal layer 1/an enhancement layer 2/a silver nanowire layer 3/a transparent matrix layer 4.
Example 2
A method for preparing an elastic stretchable intelligent light adjusting film based on a silver nanowire electrode, wherein the electroplating current is 0.02A, and the rest is the same as that in the embodiment 1.
Example 3
A method for preparing an elastic stretchable intelligent light adjusting film based on a silver nanowire electrode, wherein the electroplating current is 0.05A, and the rest is the same as that in the embodiment 1.
Example 4
A preparation method of an elastic stretchable intelligent light adjusting film based on a silver nanowire electrode comprises the following steps that electroplating current is 0.1A, and the rest is the same as that in the embodiment 1.
Comparative example 1
A preparation method of an elastic stretchable intelligent light adjusting film based on a silver nanowire electrode comprises the following steps:
(1) pretreatment of transparent substrates
And (3) sequentially carrying out ultrasonic treatment on the transparent matrix in acetone, ethanol and deionized water for 30min to remove impurities on the surface.
(2) Preparation of transparent conductive film
The silver nanowire conductive ink is coated on the surface of a transparent substrate in a wet coating mode, and then dried and cured for 20min at the temperature of 60 ℃. And hot pressing the transparent substrate coated with the silver nanowire layer at 140 ℃ under the pressure of 0.8 Mpa.
(3) Preparation of light-adjusting film
And filling polymer dispersed liquid crystal between the two transparent conductive films, and sealing the edges with light-curing glue to obtain the light-adjusting film.
Fig. 3 is a graph showing the transmittance of the elastically stretchable transparent conductive film based on the silver nanowire electrode obtained in examples 1 to 4 and comparative example 1 of the present invention and the elastically stretchable transparent conductive film based on the silver nanowire electrode without using the reinforcing layer, and it can be seen that the transmittance of the film is as high as 87.5% when the electroplating is not performed on the surface of the silver nanowire transparent conductive film, and the transmittance of the film is reduced to 80% or less when the electroplating current is 0.01A, and the transmittance of the film is gradually reduced as the electroplating current is further increased, and the transmittance of the film is reduced to 47% when the electroplating current is 0.05A. When the plating current reaches 0.1A, the transmittance of the film is greatly reduced to 11% due to the excessive content of nickel, and the dimming effect can not be achieved basically at this time, so the subsequent research is not carried out.
Fig. 4 is a scanning electron microscope image and an energy spectrum image of the elastic stretchable transparent conductive film based on the silver nanowire electrode obtained in examples 1 to 3 and comparative example 1 of the present invention, and it can be seen that the surface of the silver nanowire is smooth, uniform and fine when it is not plated with nickel; when the electroplating current is smaller (0.01A), the silver nanowires become coarse, and meanwhile, the content of nickel element on the surface also reaches 30.68%. When the electroplating current is 0.02A, the nickel plating layer on the surface of the silver nanowire shows non-uniform growth, a plurality of raised sheets appear, and the nickel content reaches 77.55 percent. When the electroplating current reaches 0.05A, the nickel plating layer on the surface of the silver nanowire becomes uniform again, and the nickel content reaches 86.55%.
Since the process of electroplating nickel is essentially a process in which redox reaction occurs, the cathode reaction equation of the reaction is formula (1), from which it can be seen that the content of reduced nickel is related to the number of electrons lost by redox reaction, and the charge amount can be obtained from formula (2), and through two formulas, the content of nickel can be related to the electroplating time and current. Therefore, with the increase of the electroplating current, the content of nickel on the surface of the conductive film is higher and higher, the silver nanowires are thicker and thicker, and the transmittance of the transparent conductive film is reduced. Similarly, the change of the electroplating time increases the content of electroplated nickel, and also reduces the transmittance of the transparent conductive film. In order to make the light modulation film have a wider light modulation range, the conductive film containing the enhancement layer should have higher transmittance under the condition that nickel has an obvious protection effect on the silver nanowires. According to experimental tests, the transmittance and the enhancement layer enhancement effect can be considered within the range of 0.08-0.12C of the electric charge amount, and the optimal light modulation film is obtained.
Ni2++2 e-＝Ni (1)
Q＝It＝ne (2)
Wherein I refers to current, the unit is A, t refers to time, the unit is s, n is an integer, and e refers to elementary charge
Selecting 6 parallel transparent conductive film samples containing the enhancement layer obtained in the step (3) in the example 1, and measuring the resistance of the transparent conductive film before and after nickel plating, wherein the initial resistance value is the resistance value of the transparent conductive film prepared by the method in the comparative example 1. The test results are shown in Table 1.
Table 1 resistance of transparent conductive film obtained in example 1 and comparative example 1
According to the data in the table, the existence of the enhancement layer can obviously reduce the resistance of the silver nanowire transparent conductive film after the silver nanowire transparent conductive film is plated with nickel, and the problem of silver nanowire conductivity failure caused by joule heat can be solved to a certain extent.
Fig. 5 is a graph of sheet resistance versus tensile elongation for the elastically stretchable transparent conductive film based on a silver nanowire electrode prepared by the methods provided in examples 1 to 3 of the present invention and comparative example 1, and it can be seen that the sheet resistance of the films is less changed when the degree of stretching is not high (< 5%) for all the films. As the degree of stretching increases, the change in sheet resistance of the film becomes greater. Comparing the sheet resistance of different film samples under the same elongation, the sheet resistance of the film sample can be effectively reduced by nickel plating, but the sheet resistance of the film tends to be stable and does not decrease as the nickel plating current increases and the nickel content increases.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. An elastic stretchable intelligent light adjusting film based on a silver nanowire electrode is characterized by comprising the following structures: the polymer dispersed liquid crystal layer (1) is positioned in the middle layer, and the two ends of the polymer dispersed liquid crystal layer (1) are respectively provided with an enhancement layer (2), a silver nanowire layer (3) and a transparent matrix layer (4) from inside to outside in sequence; the two enhancement layers (2) are respectively provided with a power supply connecting structure (5) which is connected with an external control switch and a driving power supply; the silver nanowire layer (3) has ductility and serves as a conductive electrode.
2. The elastic stretchable intelligent light adjusting film based on the silver nanowire electrodes as claimed in claim 1, wherein the diameters of the silver nanowires in the silver nanowire layer (3) are 20-50 nm, and the length-diameter ratio (the ratio of the length to the diameter) is 500-1000.
3. The elastic stretchable intelligent light adjusting film based on silver nanowire electrodes as claimed in claim 1, wherein the sheet resistance of the silver nanowire layer (3) is 20-100 Ω/□.
4. The elastic stretchable smart light adjusting film based on silver nanowire electrodes as claimed in claim 1, wherein the reinforcement layer (2) is a metal layer with stronger reducibility than metallic silver under the same reaction conditions.
5. The elastic stretchable smart membrane based on silver nanowire electrodes as claimed in claim 1, wherein the reinforcement layer (2) is a metallic nickel layer or a metallic chromium layer.
6. The elastic stretchable intelligent dimming film based on the silver nanowire electrode according to claim 1, wherein the transparent substrate layer (4) is a transparent thermoplastic elastic material layer, and the transparent thermoplastic elastic material is one or more of polyurethane thermoplastic elastic material, styrene thermoplastic elastic material, polyolefin thermoplastic elastic material and polyamide thermoplastic elastic material.
7. The elastic stretchable intelligent light adjusting film based on the silver nanowire electrode as claimed in claim 1, wherein the power supply connection structure (5) is a conductive material combined with the enhancement layer (2), and the conductive material is copper foil or conductive cloth.
8. The preparation method of the elastic stretchable intelligent light adjusting film based on the silver nanowire electrode as claimed in any one of claims 1 to 7, characterized by comprising the following steps:
(1) pretreatment of transparent substrate layers
Sequentially carrying out ultrasonic treatment on the transparent substrate layer in acetone, ethanol and deionized water for 10-30 min to remove impurities on the surface;
(2) compounding of silver nanowire layer and transparent substrate layer
Coating silver nanowire conductive ink on the surface of the transparent matrix layer in the step (1) in a wet coating mode, drying and curing, removing a solvent to obtain a silver nanowire layer, and performing hot-pressing treatment on the transparent matrix layer coated with the silver nanowire layer to obtain a silver nanowire layer and a transparent matrix layer which are compounded, namely a transparent conductive film;
(3) preparation of conductive films containing enhancement layers
Electroplating the surface of the transparent conductive film obtained in the step (2) by adopting an electrochemical method to obtain a transparent conductive film containing an enhancement layer;
(4) preparation of light-adjusting film
And (4) superposing the two transparent conductive films containing the enhancement layers obtained in the step (3) to enable the enhancement layers to face oppositely, filling polymer dispersed liquid crystal between the two enhancement layers, and sealing the edges by using light curing glue to obtain the elastic stretchable intelligent light adjusting film based on the silver nanowire electrode.
9. The method for preparing the elastic stretchable intelligent light adjusting film based on the silver nanowire electrode as claimed in claim 8, wherein the temperature for drying and curing in the step (2) is 40-80 ℃ for 10-60 min; the temperature of the hot pressing treatment is 100-200 ℃, and the pressure is 0.1-0.8 Mpa.
10. The method for preparing the elastic stretchable intelligent light adjusting film based on the silver nanowire electrode as claimed in claim 8, wherein in the electroplating process in the step (3): the electroplating solution is a mixed solution of 0.1-10 mol/L boric acid, 0.1-10 mol/L chloride of the metal of the enhancement layer and 0.1-10 mol/L ethylenediamine hydrochloride; the electroplating current is 0.01-0.1A, and the electroplating time is 1-10 s.
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Inventor after: Lv Yongsheng Inventor after: Wang Xiangwei Inventor after: Peng Ruihui Inventor after: Sha Jianjun Inventor after: Liu Lin Inventor after: Wu Wei Inventor before: Wang Xiangwei Inventor before: Peng Ruihui Inventor before: Sha Jianjun Inventor before: Lv Yongsheng Inventor before: Liu Lin Inventor before: Wu Wei |
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Application publication date: 20211231 |