CN114563895A - Porous conductive polymer-based electrochromic film and preparation method thereof - Google Patents
Porous conductive polymer-based electrochromic film and preparation method thereof Download PDFInfo
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- CN114563895A CN114563895A CN202210230368.1A CN202210230368A CN114563895A CN 114563895 A CN114563895 A CN 114563895A CN 202210230368 A CN202210230368 A CN 202210230368A CN 114563895 A CN114563895 A CN 114563895A
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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
- G02F1/15—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
- G02F1/1514—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 characterised by the electrochromic material, e.g. by the electrodeposited material
- G02F1/1516—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 characterised by the electrochromic material, e.g. by the electrodeposited material comprising organic material
- G02F1/15165—Polymers
Abstract
The invention provides a porous conductive polymer-based electrochromic film and a preparation method thereof, wherein the preparation method comprises the following steps: preparing a porous conducting polymer nano material suspension, namely preparing a conducting polymer colloidal particle dispersion liquid by a hydrothermal method, and then preparing the porous conducting polymer nano material suspension by an oxidative polymerization method; s2, preparing the porous conductive polymer-based electrochromic film. The electrochromic film is prepared by adopting the method. Compared with the electrochromic material with the porous nano structure constructed by the template method, the invention avoids the influence on the electrochemical performance of the electrochromic film due to the use of inorganic template materials such as silicon dioxide and the like which are nearly insulated, and the porous nano structure can be obtained only by assembling single conductive polymer colloid particles. The preparation of the porous conductive polymer-based electrochromic film with high contrast and stability is realized, and the process flow is greatly simplified.
Description
Technical Field
The invention relates to the technical field of functional materials, in particular to a porous conductive polymer-based electrochromic film and a preparation method thereof.
Background
According to statistics, the building energy consumption accounts for 30% of the total social energy consumption, wherein the energy consumption caused by the glass doors and windows accounts for about 50% of the total building energy consumption. The electrochromic glass is an important energy-saving material, and the color and the transmittance of the glass are reversibly changed by utilizing the change of the polarity and the strength of the electrochromic glass under an external electric field to cause the oxidation or reduction reaction of the electrochromic material, so that the active dynamic control of sunlight and solar radiation heat is realized. Therefore, intelligent windows based on electrochromic glass have important applications in the field of energy-saving buildings. As a key component of an electrochromic device, an electrochromic material mainly comprises an inorganic electrochromic material taking a transition metal oxide as a main component and an organic electrochromic material taking a conductive polymer as a main component. Compared with inorganic electrochromic materials, electrochromic conductive polymers such as polyaniline and derivatives thereof, polythiophene and derivatives thereof have the advantages of high response speed, rich colors, low raw material cost, easiness in large-scale preparation and the like.
A large number of studies show that the microstructure of the electrochromic film has a significant influence on the electrochromic performance. The dense structure tends to hinder ion transport in the electrochemical process, resulting in electrochromic films exhibiting low optical contrast and poor cycling stability. And the appropriate porous structure is helpful to increase the contact area of the film with the electrolyte, and provides more active sites for charge transfer reaction. The traditional preparation of conductive polymers based on chemical oxidative polymerization has compact structure and poor electrochromic performance, so that the optical contrast is low. Therefore, it is a hot spot of research to obtain a nano porous structure by controlling the process so as to improve the cycle stability and optical contrast of the electrochromic film. At present, a template method is mostly adopted for preparing the porous electrochromic film. Patent CN201910908676.3 proposes a template method, i.e. a method of compounding a conductive polymer with a porous inorganic nano-material with high specific surface area, to improve the problem of dense structure of the conductive polymer. In patent CN110803707A, titanium-doped hierarchical porous silica is introduced into a nano tungsten oxide film to prepare a titanium-doped hierarchical porous silica/nano tungsten oxide composite electrochromic film. Compared with a pure nano tungsten oxide film, the composite film shows an effectively enhanced optical modulation range and cycle stability. However, the existing method for preparing the porous electrochromic material by the template method has complex process and high cost, and because the template material is usually inorganic materials with poor conductivity such as silicon dioxide, halloysite nanotubes and the like, excessive use of the template material can generate negative influence on the electrochromic performance of the electrochromic film and is not beneficial to the large-scale production of the electrochromic material.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a porous conductive polymer-based electrochromic film and a preparation method thereof.
The purpose of the invention is realized by the following technical scheme: a preparation method of a porous conductive polymer-based electrochromic film comprises the following steps:
s1, preparing porous conductive polymer nano material suspension
S11, preparing conductive polymer colloid particle dispersion liquid by hydrothermal method
Adding a conductive polymer monomer into deionized water for ultrasonic treatment, then adding a copper acetate solid, and stirring and mixing; transferring the mixture into a hydrothermal reaction kettle for reaction, then carrying out high-speed centrifugation, and taking supernatant fluid to obtain the conductive polymer colloidal particle dispersion liquid.
S12, preparing conductive polymer suspension by oxidative polymerization
Adding an initiator into an acid solution to prepare an initiator solution, adding the initiator solution into the conductive polymer colloid particle dispersion liquid, continuously stirring in a low-temperature water bath, and polymerizing excessive monomers in the mixed solution under the action of the initiator and further assembling the excessive monomers and colloid particles to form a porous nano structure. After centrifugal washing, obtaining a conductive polymer nano material suspension with a porous nano structure assembled by conductive polymer colloid particles;
s2, preparing the porous conductive polymer-based electrochromic film
Adding a conductive agent, and/or a dispersing agent, and/or a film-forming agent into the conductive polymer nano-material suspension, and stirring to obtain a film-forming solution; connecting the porous conductive polymer base electrochromic composite membrane on a conductive base, and pouring the porous conductive polymer base electrochromic composite membrane into a film, or adding the film-forming solution into a spray gun, and spraying the film on the conductive base on a hot table at the temperature of 60-150 ℃ to form the porous conductive polymer base electrochromic composite membrane.
Further, in S11, the conductive polymer monomer is one of pyrrole and its derivatives, thiophene and its derivatives, and aniline and its derivatives.
In the S12, the initiator is one or more of ammonium persulfate, potassium persulfate, ferric trichloride and hydrogen peroxide; the acid solution is selected from one or more of hydrochloric acid, sulfuric acid, nitric acid or dodecylbenzene sulfonic acid.
Further, in the S12, the low-temperature water bath temperature is 0 ℃ to 5 ℃. Is beneficial to slowing down the polymerization reaction rate.
The porous conductive polymer-based electrochromic film is prepared by the method.
The invention has the beneficial effects that:
1. compared with the porous conductive polymer-based electrochromic material with the porous nano structure constructed by the template method, the invention can obtain the porous nano structure only by assembling conductive polymer colloid particles without using a template. Therefore, a template does not need to be removed in the subsequent process, and the process flow is greatly simplified.
2. When the porous conductive polymer-based electrochromic material with the porous nano structure is constructed by the template method, a large amount of organic reagents are often used in the template removing process, and a template partially based on inorganic materials (such as silicon dioxide) is also required to be removed by hydrofluoric acid, so that certain potential safety hazards and risks of environmental pollution are easily caused in the large-scale preparation process. The invention effectively avoids these risks without the use of templates, thus facilitating the mass production thereof.
3. Compared with electrochromic materials prepared by a direct chemical oxidative polymerization method and even other electrochromic films based on conductive polymers, the porous nanostructured conductive polymer-based electrochromic material prepared by combining a hydrothermal method and a chemical oxidative polymerization method has obviously enhanced optical contrast and good stability, avoids influencing the electrochromic performance of the electrochromic film due to the fact that template materials with poor conductivity such as silicon dioxide are not needed, simplifies the types of raw materials, and is beneficial to large-scale production.
Drawings
FIG. 1 is a scanning electron microscope image of PDMA-HC (porous poly 2, 5-dimethoxyaniline electrochromic nanomaterial);
FIG. 2 is a scanning electron microscope image of PDMA-C (poly-2, 5-dimethoxyaniline electrochromic nanomaterial);
FIG. 3 shows the spectroelectrochemical curves of PDMA-C (a) and PDMA-HC (b) and the cyclic stability test curves of PDMA-C (c) and PDMA-HC (d).
FIG. 4 is a schematic diagram of ion diffusion of electrochromic film based on chemical oxidative polymerization (PDMA-C film) and electrochromic film based on combination of hydrothermal method and chemical oxidative polymerization (PDMA-HC) in electrolyte.
Detailed Description
The technical solutions of the present invention are further described in detail below with reference to the accompanying drawings, but the scope of the present invention is not limited to the following.
The conductive polymer monomer is selected from aniline and its derivatives, such as 2, 5-Dimethoxyaniline (DMA).
Example 1
A preparation method of a porous conductive polymer-based electrochromic film comprises the following steps:
s1, preparing porous conductive polymer nano material suspension
S11, preparing conductive polymer colloid particle dispersion liquid by hydrothermal method
Adding 0.08-0.24g of 2, 5-Dimethoxyaniline (DMA) into 60-80 ml of deionized water, carrying out ultrasonic treatment for 30-60 minutes to obtain a dispersion liquid, adding 0.01-0.2g of copper acetate solid into 20 ml of water to obtain an oxidant, adding the oxidant into the dispersion liquid, and stirring for 15min at 60 ℃ for full mixing. The mixture was transferred to a 200 ml hydrothermal reaction kettle and held at 150 ℃ for 3 h. And centrifuging the obtained product at 10000r/min for 10 minutes at a high speed, and taking supernatant to obtain the conductive polymer colloidal particle dispersion liquid.
S12, preparing conductive polymer suspension by oxidative polymerization
Adding 0.05-0.3g of initiator into 20 ml of 1mol/L acid solution to prepare initiator solution, adding the initiator solution into the colloid dispersion liquid, continuously stirring for 3-12 hours in a low-temperature water bath at-1-15 ℃, and centrifugally washing to obtain the conductive polymer suspension with the porous nano structure assembled by conductive polymer colloid particles.
S2, preparing the porous conductive polymer-based electrochromic film
Adding 0-10 wt% of conductive agent, 0-5 wt% of dispersing agent and/or 0-5 wt% of film forming agent into the prepared conductive polymer nano material suspension, stirring for 30 minutes to obtain uniformly dispersed film forming solution, directly casting the film forming solution on a conductive base, or adding 1-5ml of film forming solution into a spray gun, and spraying the film forming solution on the conductive base on a hot table at 60-150 ℃ to form a film, thus obtaining the porous conductive polymer base electrochromic composite film.
The conductive polymer colloid particles prepared by the hydrothermal method have good dispersibility, and the average diameter of the conductive polymer colloid particles is 200 nm. The ultrafine diameter of the conductive polymer colloid nanoparticles makes them advantageous for forming porous structures during subsequent assembly.
As shown in figures 1 and 2, a hydrothermal method is combined with a chemical oxidative polymerization method to prepare the porous poly 2, 5-dimethoxyaniline electrochromic nano material (PDMA-HC). For comparison, the poly 2, 5-dimethoxyaniline electrochromic nano material (PDMA-C) is prepared by adopting a conventional chemical polymerization method. It can be found that PDMA-HC shows a significant porous structure compared to the dense structure of PDMA-C.
As shown in fig. 3, wherein (a) shows the spectroelectrochemical curves of the PDMA-C electrochromic film at different voltages; (b) represents the spectroelectrochemical curve of PDMA-HC under different voltages; (c) represents the cycling stability test of PDMA-C at 800 nm; (d) the cycle stability test of PDMA-HC at 800nm is shown, and the result shows that the electrochromic film based on PDMA-HC has significantly enhanced optical contrast in the wavelength range of 550nm-850nm compared with PDMA-C. It was also tested for its cycling stability at 800nm for switching the electrochromic film between the colored and bleached states at voltages of 0.6V and-0.4V. As can be seen from the graph, the contrast ratio of PDMA-HC in the initial condition was 75%, which is increased by 60% compared to PDMA-C. And can still be kept at 72.3% after 500 cycles, which shows that the composite material has better cycle stability.
As shown in fig. 4, the conductive polymer-based electrochromic material with a porous nano structure prepared by combining the hydrothermal method and the chemical oxidative polymerization method has better stability compared with the electrochromic material prepared by the direct chemical oxidative polymerization method and even compared with other conductive polymer-based electrochromic films.
The foregoing is illustrative of the preferred embodiments of this invention, and it is to be understood that the invention is not limited to the precise form disclosed herein and that various other combinations, modifications, and environments may be resorted to, falling within the scope of the concept as disclosed herein, either as described above or as apparent to those skilled in the relevant art. And that modifications and variations may be effected by those skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (5)
1. A preparation method of a porous conductive polymer-based electrochromic film is characterized by comprising the following steps: the method comprises the following steps:
s1, preparing porous conductive polymer nano material suspension
S11, preparing conductive polymer colloid particle dispersion liquid by hydrothermal method
Adding a conductive polymer monomer into deionized water for ultrasonic treatment, then adding a copper acetate solid, and stirring and mixing; transferring the mixture into a hydrothermal reaction kettle for reaction, then carrying out high-speed centrifugation, and taking supernatant to obtain conductive polymer colloidal particle dispersion liquid;
s12, preparing conductive polymer suspension by oxidative polymerization
Adding an initiator into an acid solution to prepare an initiator solution, adding the initiator solution into the conductive polymer colloidal particle dispersion solution, continuously stirring in a low-temperature water bath, and centrifugally washing to obtain a conductive polymer nano material suspension with a porous nano structure assembled by conductive polymer colloidal particles;
s2, preparing the porous conductive polymer-based electrochromic film
Adding a conductive agent, and/or a dispersing agent, and/or a film-forming agent into the porous conductive polymer nano material suspension, and stirring to obtain a film-forming solution; connecting the porous conductive polymer base electrochromic composite membrane on a conductive base, and pouring the porous conductive polymer base electrochromic composite membrane into a film, or adding the film-forming solution into a spray gun, and spraying the film on the conductive base on a hot table at the temperature of 60-150 ℃ to form the porous conductive polymer base electrochromic composite membrane.
2. The method for preparing a porous conducting polymer-based electrochromic film according to claim 1, wherein: in S11, the conductive polymer monomer is selected from one of pyrrole and its derivatives, thiophene and its derivatives, aniline and its derivatives.
3. The method for preparing a porous conducting polymer-based electrochromic film according to claim 1, wherein: in the S12, the initiator is one or more of ammonium persulfate, potassium persulfate, ferric trichloride and hydrogen peroxide; the acid solution is selected from one or more of hydrochloric acid, sulfuric acid, nitric acid or dodecylbenzene sulfonic acid.
4. The preparation method of the porous conductive polymer-based electrochromic film according to claim 1, wherein: in the S12, the temperature of the low-temperature water bath is 0-5 ℃.
5. A porous conductive polymer-based electrochromic film is characterized in that: the porous conductive polymer-based electrochromic film is obtained by the preparation method of any one of claims 1 to 4.
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