CN110794633A - Manganese dioxide nanowire-based electrochromic device and preparation method thereof - Google Patents
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- 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
- G02F1/15—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 an electrochromic effect
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Abstract
The invention discloses an electrochromic device based on manganese dioxide nanowires and a preparation method thereof. The electrochromic device comprises a manganese dioxide nanowire structure film electrode; the manganese dioxide nanowire structure film electrode is composed of FTO conductive glass and a manganese dioxide nanowire structure film. Compared with the prior art, the manganese dioxide nanowire structure thin film electrode is prepared by adopting a seed-crystal-layer-free auxiliary one-step hydrothermal method and assembled into an electrochromic device, the preparation process is simple, the operation is easy, the required reagents are few, the cost is low, the electrochromic performance of the device formed by the prepared manganese dioxide nanowire structure thin film electrode is good, and the application of nano manganese dioxide in the electrochromic field is promoted.
Description
Technical Field
The invention belongs to the technical field of electrochromic film preparation, and particularly relates to an electrochromic device based on manganese dioxide nanowires and a preparation method thereof.
Background
The electrochromic material generates the injection and extraction of electrons and ions under the electrochemical action, and the valence state and chemical components are changed, so that the reflection and transmission properties of the material are changed, and the appearance of the material is represented as reversible change of color and transparency. According to the difference of electrochromic materials, the electrochromic materials can be divided into inorganic electrochromic materials and organic electrochromic materials. A complete electrochromic device is a sandwich type structure and is composed of a transparent substrate, a transparent conducting layer, an electrochromic layer, an electrolyte layer and an ion storage layer, wherein the electrochromic material mainly serves as the electrochromic layer in the electrochromic device.
Manganese dioxide is an oxide with important industrial application, is also an important transition metal oxide, has a complex crystal structure, and has various crystal forms of α, β, gamma, delta, epsilon, rho, lambda and the like, the manganese dioxide is divided into an oxidation state and a reduction state, the oxidation state is yellow or light yellow, the reduction state is brown or dark brown, and the manganese dioxide has different properties and is widely applied to the aspects of novel metal composite materials, environmental purification, battery materials and the like.
In recent years, with the continuous development of electrochromic technology and nanotechnology, more and more researchers hope to combine the two technologies, namely, improve the electrochromic performance of the material by framing the nanostructure, so as to obtain better results. Hydrothermal method is one of the common methods for preparing metal oxides. He et al (Nano Energy, 2017, 35: 242- & 250) reported that multilayer porous polypyrrole nanowires and manganese dioxide nanosheets are used as electrodes of flexible high Energy density asymmetric supercapacitors in the form of core/shell conducting polymers. Chen et al (ACS Applied Materials & Interfaces,2017, 9(40): 35040) report that the prepared manganese dioxide nanosheets similar to graphene are assembled with hollow cobalt sulfide nanometer arrays to be used as electrode Materials of supercapacitors. Chae et al (ACS Applied Materials & Interfaces,2016, 8(18): 11499) reported the preparation of manganese dioxide nanorods using microwave-assisted hydrothermal methods. The manganese dioxide nano structure is mainly applied to the field of electrode materials and capacitors, and is less applied to the field of electrochromism; and because of the defects of complex preparation process, high equipment requirement, harsh operation conditions and the like, the manganese dioxide nanowire and nanorod structures are less applied to the field of electrochromism at present. Therefore, the method for directly growing a layer of manganese dioxide film with a nanowire structure on the conductive glass substrate by adopting a crystal-seed-free assisted hydrothermal method and assembling the manganese dioxide film into the electrochromic device is expected to break through the bottleneck of the existing electrochromic film material preparation technology, solve the problems mentioned above and lay a solid foundation for realizing large-scale industrialization of electrochromic glass.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide an electrochromic device based on manganese dioxide nanowires and a preparation method thereof. According to the invention, the manganese dioxide nanowire structure film is prepared by a one-step hydrothermal method without the assistance of a seed crystal layer and assembled into an electrochromic device, the preparation process is simple, the operation is easy, the types of required reagents are few, the cost is low, the electrochromic performance of the device formed by the prepared manganese dioxide nanowire structure film electrode is good, and the application of nano manganese dioxide in the electrochromic field is promoted.
The technical scheme of the invention is specifically introduced as follows.
The invention provides an electrochromic device based on manganese dioxide nanowires, which comprises manganese dioxide nanowire structure film electrodes; the manganese dioxide nanowire structure film electrode is composed of FTO conductive glass and a manganese dioxide nanowire structure film, and the manganese dioxide nanowire structure film is of a nanowire structure or a net structure formed by self-weaving of nanowires.
In the invention, the method also comprises a counter electrode, a packaging material and an electrolyte; the counter electrode is made of blank FTO conductive glass; the packaging material is used for packaging the peripheries of the film electrode and the counter electrode, and electrolyte is filled between the film electrode and the counter electrode in the manganese dioxide nanowire structure and in a space defined by the packaging material.
In the invention, the packaging material is selected from any one of silica gel or acrylic gel, and the thickness of the packaging material is 0.1-2 mm; the electrolyte is selected from any one of potassium chloride aqueous solution, sodium chloride aqueous solution or lithium perchlorate aqueous solution, and the concentration is 0.5-5 mol/L. Preferably, the thickness of the packaging material is 0.5-1 mm; the concentration of the electrolyte is 1-3 mol/L.
The preparation method of the manganese dioxide nanowire structure film electrode comprises the following steps:
(1) dissolving potassium permanganate and manganese sulfate monohydrate in water, and performing ultrasonic oscillation to obtain a reaction solution; the molar concentration of potassium permanganate in the reaction solution is 0.06-0.08 mol/L, and the molar ratio of potassium permanganate to manganese sulfate monohydrate is 2: 1-3: 1;
(2) and (3) immersing FTO conductive glass into a hydrothermal kettle containing the reaction solution for hydrothermal reaction, naturally cooling to room temperature after the hydrothermal reaction is finished, and drying after washing with water and ethanol in sequence to obtain the manganese dioxide nanowire structure film electrode.
In the invention, in the step (2), the hydrothermal reaction temperature is 150-180 ℃, and the heat preservation time is 10-15 h.
The invention further provides a preparation method of the electrochromic device based on the manganese dioxide nanowires, which comprises the following specific steps:
firstly, preparing a manganese dioxide nanowire structure film on a conductive surface of FTO conductive glass by a hydrothermal method to obtain a manganese dioxide nanowire structure film electrode; then packaging the peripheries of the manganese dioxide nanowire structure film electrode and the counter electrode by using a packaging material; and finally, injecting electrolyte into the space defined by the manganese dioxide nanowire structure film electrode, the space defined by the counter electrode and the packaging material by using an injection needle, and assembling to obtain the electrochromic device.
Compared with the prior art, the invention has the beneficial effects that:
(1) the preparation method is simple, easy to operate, few in required reagent types, low in cost and capable of being applied to the industry of film making on the surface of glass.
(2) According to the invention, the manganese dioxide nanowire structure thin film is prepared on the FTO conductive glass without the seed crystal by adjusting the parameters such as the composition, the reaction temperature and the time of the reaction solution and is assembled into the electrochromic device, and the manganese dioxide nanowire structure can effectively improve the electrochromic properties such as the color change speed, the cycling stability and the like, and promote the development of the nano manganese dioxide in the electrochromic field.
(3) The manganese dioxide nanowire structure film electrode is prepared by a one-step hydrothermal method without a seed crystal layer, and is assembled into an electrochromic device, so that the electrochromic performance is good, and the application of nano manganese dioxide in the electrochromic field is promoted.
Drawings
Fig. 1 is a schematic structural diagram of an electrochromic device based on manganese dioxide nanowires according to the present invention.
Reference numerals: 1-electrolyte, 2-packaging material, 3-manganese dioxide nanowire structure film electrode and 4-counter electrode.
Fig. 2 is a digital photograph of the discoloration effect of the manganese dioxide nanowire-based electrochromic device according to the present invention, wherein a is a colored state and b is a faded state.
FIG. 3X-ray diffraction pattern of manganese dioxide nanowire structured electrochromic film prepared in example 1.
Fig. 4 a scanning electron micrograph of the manganese dioxide nanowire-structured electrochromic film prepared in example 1.
Fig. 5 light transmission curves of manganese dioxide nanowire-based electrochromic devices prepared in example 1 in colored and discolored states, respectively.
FIG. 6 SEM of manganese dioxide nanowire structural electrochromic film prepared in example 2.
Fig. 7 a scanning electron micrograph of the manganese dioxide nanowire-structured electrochromic film prepared in example 3.
FIG. 8 SEM of manganese dioxide nanowire structural electrochromic film prepared in example 4.
Detailed Description
The present invention is further described below in conjunction with the following figures and examples, which should be understood to be illustrative of the present invention only and not limiting.
The invention aims to apply the manganese dioxide nanowire structure film to an electrochromic device, and the device is simple in manufacturing method and low in cost.
Referring to fig. 1, which shows a schematic structural diagram of an electrochromic device based on manganese dioxide nanowires provided by the present invention, the bottom end and the top end of the device are respectively transparent FTO conductive glass as a working electrode and a counter electrode support;
the manganese dioxide nanowire structure film electrode 3 is used as an electrochromic layer and is composed of transparent FTO conductive glass and a manganese dioxide nanowire structure film thereon; the counter electrode 4 is made of blank FTO conductive glass;
the packaging material 2 is packaged around the electrodes, and the electrolyte 1 is placed in a closed space between the manganese dioxide nanowire structure film electrode 3 and the counter electrode 4 and the packaging material 2. The electrolyte 1 is selected from 0.5-5 mol/L, preferably 1-3 mol/L potassium chloride aqueous solution, sodium chloride aqueous solution, and lithium perchlorate aqueous solution. The thickness of the electrolyte 1 is determined by the thickness of the sealing material 2, and is 0.1 to 2 mm, preferably 0.5 to 1 mm.
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Furthermore, it should be understood that various changes and modifications can be made by one skilled in the art after reading the teachings of the present invention, and equivalents may fall within the scope of the invention as defined by the appended claims.
Example 1
Respectively weighing 0.3516 g of potassium permanganate and 0.1477 g of manganese sulfate monohydrate, dissolving in 30 ml of ultrapure water, and performing ultrasonic oscillation to obtain a reaction solution; and then transferring the reaction solution to a hydrothermal reaction kettle, immersing cleaned FTO conductive glass into the hydrothermal kettle filled with the reaction solution, wherein the FTO conductive glass is obliquely arranged and the conductive surface faces downwards, preserving the heat at 160 ℃ for 12 hours, naturally cooling to room temperature, taking out the FTO conductive glass, sequentially cleaning with water and ethanol, and drying to obtain the manganese dioxide nanowire structure film. FIG. 3 shows the film obtainedThe X-ray diffraction pattern is compared with the standard X-ray diffraction pattern, and the film is β -MnO2Corresponding to the standard card JCPDS No. 24-0735. FIG. 4 is a SEM photograph of the manganese dioxide thin film obtained, and it can be seen that the thin film is a network structure formed by self-braiding manganese dioxide nanowires.
Packaging the prepared manganese dioxide nanowire structural film and the periphery of a blank FTO conductive glass counter electrode by using acrylic double-sided adhesive tape with the thickness of 1 mm, and pumping 1mol/L potassium chloride aqueous solution into a space defined by a manganese dioxide nanowire structural film electrode 3, a counter electrode 4 and a packaging material 2 by using a needle tube to obtain the manganese dioxide nanowire-based electrochromic device. The electrochromic performance of the manganese dioxide nanowire-based electrochromic device prepared in the embodiment is characterized by combining an electrochemical workstation and an ultraviolet-visible spectrophotometer, wherein the electrochemical test adopts a two-electrode system, namely a working electrode is connected with a prepared reticular manganese dioxide nanowire structure film, a counter electrode and a reference electrode are connected with blank FTO conductive glass, and 1mol/L potassium chloride aqueous solution is used as an electrolyte. The results show that: when voltages of-1.5V and 1.5V are applied, the manganese dioxide nanowire-based electrochromic device reversibly changes between brown and yellowish colors, see fig. 2; as shown in FIG. 5, the transmittance of the device is obviously changed in the wavelength band of 300-800 nm, and reaches 38.7% at the position of lambda =539 nm; the results of the response time calculation of the electrochromic device based on manganese dioxide nanowires are shown in table 1. From the above results, it can be seen that the electrochromic device based on manganese dioxide nanowires prepared in example 1 has good electrochromic properties.
Example 2
Respectively weighing 0.3516 g of potassium permanganate and 0.1477 g of manganese sulfate monohydrate, dissolving in 30 ml of ultrapure water, and performing ultrasonic oscillation to obtain a reaction solution; and then transferring the reaction solution into a hydrothermal reaction kettle, immersing cleaned FTO conductive glass into the hydrothermal kettle filled with the reaction solution, wherein the FTO conductive glass is obliquely arranged and the conductive surface faces downwards, preserving the heat at 160 ℃ for 10 hours, finally naturally cooling to room temperature, taking out the FTO conductive glass, sequentially cleaning with water and ethanol, and drying to obtain the manganese dioxide nanowire-structured electrochromic film, wherein FIG. 6 is a scanning electron microscope photograph of the prepared manganese dioxide film, and the surface appearance of the film can be seen to be a nanowire self-woven mesh structure and a partial nanosheet structure. Packaging the prepared manganese dioxide nanowire structural film and the periphery of a blank FTO conductive glass counter electrode by using acrylic double-sided adhesive tape with the thickness of 1 mm, and pumping 1mol/L potassium chloride aqueous solution into a space defined by the manganese dioxide nanowire structural film electrode, the counter electrode and a packaging material by using a needle tube to obtain the manganese dioxide nanowire structural film electrochromic device. The prepared nano manganese dioxide thin film device was subjected to an electrochromic property test, and the results are shown in table 1.
Example 3
Respectively weighing 0.3516 g of potassium permanganate and 0.1880 g of manganese sulfate monohydrate, dissolving in 30 ml of ultrapure water, and performing ultrasonic oscillation to obtain a reaction solution; and then transferring the reaction solution into a hydrothermal reaction kettle, immersing cleaned FTO conductive glass into the hydrothermal kettle filled with the reaction solution, wherein the FTO conductive glass is obliquely arranged and the conductive surface faces downwards, preserving the heat at 160 ℃ for 15 hours, finally naturally cooling to room temperature, taking out the FTO conductive glass, and sequentially cleaning the FTO conductive glass with water and ethanol to obtain the manganese dioxide nanowire structure electrochromic film, wherein FIG. 7 is a scanning electron microscope photo of the prepared manganese dioxide film, and the surface appearance of the film is a nanowire structure and the nanowires are distributed unevenly. Packaging the prepared manganese dioxide nanowire structural film and the periphery of a blank FTO conductive glass counter electrode by using acrylic double-sided adhesive tape with the thickness of 1 mm, and pumping 1mol/L potassium chloride aqueous solution into a space defined by the manganese dioxide nanowire structural film electrode, the counter electrode and a packaging material by using a needle tube to obtain the manganese dioxide nanowire-based electrochromic device. The prepared nano manganese dioxide thin film device was subjected to an electrochromic property test, and the results are shown in table 1.
Example 4
Respectively weighing 0.37928 g of potassium permanganate and 0.1352 g of manganese sulfate monohydrate, dissolving in 30 ml of ultrapure water, and performing ultrasonic oscillation to obtain a reaction solution; and then transferring the reaction solution to a hydrothermal reaction kettle, immersing cleaned FTO conductive glass into the hydrothermal kettle filled with the reaction solution, wherein the FTO conductive glass is obliquely arranged and the conductive surface faces downwards, keeping the temperature at 160 ℃ for 13 hours, finally naturally cooling to room temperature, taking out the FTO conductive glass, and sequentially cleaning with water and ethanol to obtain the manganese dioxide nanowire structure electrochromic film, wherein FIG. 8 is a scanning electron microscope picture of the prepared manganese dioxide film, and the surface appearance of the film is a nanowire structure, but most of nanowires are agglomerated in a self-woven mesh structure. Packaging the prepared manganese dioxide nanowire structural film and the periphery of a blank FTO conductive glass counter electrode by using acrylic double-sided adhesive tape with the thickness of 1 mm, and pumping 1mol/L potassium chloride aqueous solution into a space defined by the manganese dioxide nanowire structural film electrode, the counter electrode and a packaging material by using a needle tube to obtain the manganese dioxide nanowire structural film electrochromic device. The prepared nano manganese dioxide thin film device was subjected to an electrochromic property test, and the results are shown in table 1.
Table 1 transmittance change value, coloring time and fading time of electrochromic device in example
Claims (8)
1. An electrochromic device based on manganese dioxide nanowires is characterized by comprising manganese dioxide nanowire structure film electrodes; the manganese dioxide nanowire structure film electrode is composed of FTO conductive glass and a manganese dioxide nanowire structure film, and the manganese dioxide nanowire structure film is of a nanowire structure or a net structure formed by self-weaving of nanowires.
2. The manganese dioxide nanowire-based electrochromic device according to claim 1, further comprising a counter electrode, an encapsulating material and an electrolyte; the counter electrode is made of blank FTO conductive glass; the packaging material is used for packaging the peripheries of the film electrode and the symmetrical electrode, and electrolyte is filled between the film electrode and the counter electrode in the manganese dioxide nanowire structure and in a space defined by the packaging material.
3. The manganese dioxide nanowire-based electrochromic device according to claim 1, wherein the packaging material is selected from any one of silica gel and acrylic gel, and the thickness of the packaging material is 0.1-2 mm; the electrolyte is selected from any one of potassium chloride aqueous solution, sodium chloride aqueous solution and lithium perchlorate aqueous solution, and the concentration of the electrolyte is 0.5-5 mol/L.
4. The manganese dioxide nanowire-based electrochromic device according to claim 1, wherein the thickness of the packaging material is 0.5-1 mm; the concentration of the electrolyte solution is 1-3 mol/L.
5. The manganese dioxide nanowire-based electrochromic device according to claim 1, wherein the preparation method of the manganese dioxide nanowire-structured thin film electrode is as follows:
(1) dissolving potassium permanganate and manganese sulfate monohydrate in water, and performing ultrasonic oscillation to obtain a reaction solution; the molar concentration of potassium permanganate in the reaction solution is 0.06-0.08 mol/L, and the molar ratio of potassium permanganate to manganese sulfate monohydrate is 2: 1-3: 1;
(2) and (3) immersing FTO conductive glass into a hydrothermal kettle containing the reaction solution for hydrothermal reaction, naturally cooling to room temperature after the hydrothermal reaction is finished, and drying after washing with water and ethanol in sequence to obtain the manganese dioxide nanowire structure film electrode.
6. The manganese dioxide nanowire-based electrochromic device according to claim 5, wherein in the step (2), the hydrothermal reaction temperature is 150-180 ℃ and the holding time is 10-15 h.
7. The preparation method of the manganese dioxide nanowire-based electrochromic device according to any one of claims 1 to 6, which comprises the following specific steps:
firstly, preparing a manganese dioxide nanowire structure film on a conductive surface of FTO conductive glass by a hydrothermal method to obtain a manganese dioxide nanowire structure film electrode; then packaging the peripheries of the manganese dioxide nanowire structure film electrode and the counter electrode by using a packaging material; and finally, injecting electrolyte into the space defined by the manganese dioxide nanowire structure film electrode, the space defined by the counter electrode and the packaging material by using an injection needle, and assembling to obtain the electrochromic device.
8. The preparation method of claim 7, wherein the preparation steps of the manganese dioxide nanowire structure thin film electrode are as follows:
(1) dissolving potassium permanganate and manganese sulfate monohydrate in water, and performing ultrasonic oscillation to obtain a reaction solution; the molar concentration of potassium permanganate in the reaction solution is 0.06-0.08 mol/L, and the molar ratio of potassium permanganate to manganese sulfate monohydrate is 2: 1-3: 1;
(2) and (3) immersing FTO conductive glass into a hydrothermal kettle containing the reaction solution for hydrothermal reaction, naturally cooling to room temperature after the hydrothermal reaction is finished, and drying after washing with water and ethanol in sequence to obtain the manganese dioxide nanowire structure film electrode.
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| JP2005181578A (en) * | 2003-12-18 | 2005-07-07 | National Institute For Materials Science | Electrochromic device |
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