CN109901340A - A kind of self energizing electrochomeric films and its preparation method and application - Google Patents
A kind of self energizing electrochomeric films and its preparation method and application Download PDFInfo
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- CN109901340A CN109901340A CN201910154134.1A CN201910154134A CN109901340A CN 109901340 A CN109901340 A CN 109901340A CN 201910154134 A CN201910154134 A CN 201910154134A CN 109901340 A CN109901340 A CN 109901340A
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Abstract
The present invention provides a kind of self energizing electrochomeric films and its preparation method and application, the present invention is by by WO3Film and poly- 3,4- (2,2- dimethyl allene, two oxygroup) thiophene film overlay in the same substrate and obtain self energizing electrochomeric films；As a result, it has been found that fast by the response time of the electrochromic device of the film preparation, device required time of fading after coloring shorten to 15.5s.Not only with respect to the WO of no catalysis material3Self energizing device fading time greatly reduces, and relative to fading time 25.7s needed for the device for doing catalysis material using platinum, also there is certain advantage.And device, after 200 circulations, performance can still remain stable, and fading time only extends to 22.0s.And the device shows certain optical conversion efficiencies with the ability externally done work in addition to it can generate the charge for itself discoloration, while also under sunlight.
Description
Technical field
The present invention relates to electrochromic material fields more particularly to a kind of self energizing electrochomeric films and preparation method thereof
And application.
Background technique
Replace traditional non-renewable energy resources using new energies such as solar energy, has been always full generation since the middle of last century
Boundary's researcher effort for it direction.Classical electrochromic device can be by making material under the influence of alive outside
The optical properties of material stablize reversible variation.WO3Because it has well stable optical modulation performance, such as WO3Electrochromism
Device can obstruct a large amount of visible light and infrared light in colored state, and when bleached state, sunlight can be entered the room, band
Carry out bright and heat, and is always the electrochromic material studied the most extensively.
After the last century whole world faces serious energy crisis, researcher is dedicated to WO3With conventional dyestuff
Sensitized cells technology combines, and is desirably to obtain the WO for not depending on external energy supply3Self energizing electrochromic device.In research process
In, it has been found that WO can be accelerated using expensive noble metal platinum3Colour fading process.But high platinum seriously limits
WO3The application of self energizing electrochromic device.
Therefore it provides a kind of self energizing electroluminescent film for not needing noble metal is of great significance.
Summary of the invention
In view of this, technical problem to be solved by the present invention lies in provide a kind of self energizing electrochomeric films and its system
Your gold the electrochromic device of Preparation Method and application, self energizing electrochomeric films preparation provided by the invention does not need not only
Belong to, and fading time shortens after device coloring.
The present invention provides a kind of self energizing electrochomeric films, by by WO3Film and poly- 3,4- (2,2- dimethyl propylenes
Two oxygroup of alkene) thiophene film overlays in the same substrate and obtains.
Preferably, the WO in substrate3Area shared by film and poly- 3,4- (2,2- dimethyl allene, two oxygroup) thiophene are thin
Area ratio shared by film is 2: (0.3~1.5).
Preferably, the substrate is indium oxide tin glass.
The present invention also provides a kind of preparation methods of self energizing electrochomeric films, comprising:
1) by WO3It is deposited in substrate, obtains deposition WO3The substrate of film；
2) in deposition WO3WO is not deposited in the substrate of film3Poly- 3, the 4- of site deposition (2,2- dimethyl allene, two oxygroup)
Thiophene film obtains self energizing electrochomeric films.
The present invention also provides a kind of self energizing electrochromic devices, comprising: light anode, working electrode and electrolyte；
Wherein, the working electrode is self energizing electrochomeric films of the present invention.
Preferably, the light anode is prepared in accordance with the following methods:
1) TiO is coated in substrate2Slurry obtains coating TiO2Substrate；
2) TiO will be coated2Substrate merging photosensitive dye solution in carry out Dye Adsorption, obtain light anode.
Preferably, the photosensitive dye is ruthenium pyridine organometallic complex.
Preferably, the substrate is fluorine-doped tin oxide glass.
Preferably, the electrolyte is I-/I3 -Redox couple electrolyte.
The present invention also provides a kind of preparation methods of self energizing electrochromic device, comprising: with glue by light anode and work
It is fixed as electrodes face, and injects electrolyte between light anode and working electrode, obtain self energizing electrochromic device；Its
In, the working electrode is self energizing electrochomeric films of the present invention.
Compared with prior art, the present invention provides a kind of self energizing electrochomeric films, by by WO3Film and poly- 3,
4- (2,2- dimethyl allene, two oxygroup) thiophene film is overlayed in the same substrate and is obtained；As a result, it has been found that the film is used for electricity
The electrochromic device that the working electrode of mutagens color device obtains has been shown can compare favourably with the device prepared based on metal platinum
Optical modulation performance and photoelectric conversion performance, the experimental results showed that, the electrochromism device of film preparation provided by the invention
The response time of part is fast, and device required time of fading after coloring shorten to 15.5s.Not only with respect to no catalysis material
WO3Self energizing device fading time greatly reduces, relative to fading time needed for the device for doing catalysis material using platinum
25.7s also has certain advantage.And device, after 200 circulations, performance can still remain stable, and fading time is only
Extend to 22.0s.And the device does work in addition to it can generate the charge for itself discoloration, while also with external under sunlight
Ability, show certain optical conversion efficiencies.
Detailed description of the invention
Fig. 1 is classical electrochromic device and self energizing electrochromic device described herein；
Fig. 2 is the optical transmittance and initial cycle state outcome of three kinds of devices；
Fig. 3 is that detailed optical performance of three kinds of devices at 680nm compares data；
Fig. 4 is the cyclical stability test result for the self energizing electrochromic device that embodiment 2 obtains.
Specific embodiment
The present invention provides a kind of self energizing electrochomeric films, by by WO3Film and poly- 3,4- (2,2- dimethyl propylenes
Two oxygroup of alkene) thiophene film overlays in the same substrate and obtains；Wherein, the WO in the substrate3Area shared by film and poly-
Area ratio shared by 3,4- (2,2- dimethyl allene, two oxygroup) thiophene films is 2: (0.3~1.2), more preferably 2: (0.5~
1.2), most preferably 2: (0.8~1)；The WO3The thickness of film is preferably 150~300nm, more preferably 200~250nm.
The thickness of poly- 3,4- (2,2- dimethyl allene, the two oxygroup) thiophene film is preferably 150~300nm, more preferably 200~
250nm.The present invention is not particularly limited the source of substrate, the base material well known in the art that can be used for electrochromic device
, preferably indium oxide tin glass.
The present invention also provides a kind of preparation methods of self energizing electrochomeric films, comprising:
1) by WO3It is deposited in substrate, obtains deposition WO3The substrate of film；
2) in deposition WO3WO is not deposited in the substrate of film3Poly- 3, the 4- of site deposition (2,2- dimethyl allene, two oxygroup)
Thiophene film obtains self energizing electrochomeric films.
According to the present invention, the present invention is by WO3It is deposited in substrate, obtains deposition WO3The substrate of film；Wherein, the present invention couple
The method of deposition tungstic acid does not have particular/special requirement, and method well known in the art such as can be by with the poly- wolframic acid of polyoxy
(PPTA) precursor sol is that deposition obtains WO to raw material in substrate by way of plating3Film.
According to the present invention, the present invention is in deposition WO3WO is not deposited in the substrate of film3Poly- 3, the 4- of site deposition (2,2- bis-
Two oxygroup of metering system) thiophene film, obtain self energizing electrochomeric films；The present invention is to poly- 3,4- (2, the 2- dimethyl of deposition
Two oxygroup of propylene) method of thiophene do not have particular/special requirement, and well known to a person skilled in the art poly- 3,4- (2,2- is deposited in substrate
Two oxygroup of dimethyl allene) thiophene method；The present invention is preferably by by PProDOT-Me2Monomer utilizes electrochemical polymerization
Film build method is deposited onto exposed substrate (in the substrate not deposited by tungstic acid).
The present invention also provides a kind of self energizing electrochromic devices, comprising: light anode, working electrode and electrolyte；Its
In, the working electrode is self energizing electrochomeric films of the present invention.
In the present invention, the present invention does not have particular/special requirement to the source of light anode, well known in the art to can be used for electroluminescent change
The light anode of color device, light anode of the present invention are preferably prepared in accordance with the following methods:
1) TiO is coated in substrate2Slurry obtains coating TiO2Substrate；
2) TiO will be coated2Substrate merging photosensitive dye solution in carry out Dye Adsorption, obtain light anode.
Wherein, the present invention in substrate to coating TiO2The method of slurry does not have particular/special requirement, and those skilled in the art can
To select suitable coating method and raw material according to general knowledge known in this field；The present invention also wants the substrate without special
It asks, the substrate well known in the art that can be used as light anode, such as can be fluorine-doped tin oxide glass.The present invention will also apply
Cover TiO2Substrate merging photosensitive dye solution in carry out Dye Adsorption, obtain light anode, wherein the photosensitive dye is excellent
It is selected as ruthenium pyridine organometallic complex, more preferably N719 dyestuff；Solvent in photosensitive dye solution is preferably methanol, second
The concentration of one or more of alcohol, propylene glycol carbonate, dimethyl sulfoxide and acetonitrile, the photosensitive dye solution is preferably
0.2~0.3mM.
In the present invention, the present invention to electrolyte also without particular/special requirement, it is well known in the art for electrochromic device
Electrolyte, the present invention are preferably I-/I3 -Redox couple electrolyte.
The present invention also provides a kind of preparation methods of self energizing electrochromic device, comprising: with glue by light anode and work
It is fixed as electrodes face, and injects electrolyte between light anode and working electrode, obtain self energizing electrochromic device.Its
In, the glue is preferably ultraviolet cured adhesive；And after merging electrolyte, also need also to seal injection port with glue.
Self energizing electrochomeric films provided by the invention, by by WO3Film and poly- 3,4- (2,2- dimethyl allenes two
Oxygroup) thiophene film overlays in the same substrate and obtains；As a result, it has been found that the film to be used for the working electrode of electrochromic device
Obtained electrochromic device has shown the optical modulation performance that can be compared favourably with the device prepared based on metal platinum and light
Electric conversion performance, specifically, the response time of the electrochromic device of film preparation provided by the invention is fast, device is in coloring
Required time of fading afterwards shorten to 15.5s.Not only with respect to the WO of no catalysis material3Self energizing device fading time subtracts significantly
It is few, relative to fading time 25.7s needed for the device for doing catalysis material using platinum, also there is certain advantage.And device exists
After 200 circulations, performance can still remain stable, and fading time only extends to 22.0s.And the device is under sunlight
In addition to it can generate the charge for itself discoloration, while also there is the ability externally done work, shows certain optical transition
Efficiency.
It is clearly and completely described below in conjunction with the technical solution of the embodiment of the present invention, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
Technical staff's every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
Material requested: 3,4- (2,2- dimethyl allene, two oxygroup) thiophene (ProDOT-Me2), titanium tetraisopropylate, ice vinegar
Acid, simple substance tungsten powder, acetonitrile, hydrogen peroxide, N719 dyestuff, methanol, lithium iodide (LiI), iodine (I2), lithium perchlorate (LiClO4),
Propylene glycol carbonate (PC), tin indium oxide (ITO) glass, fluorine-doped tin oxide glass (FTO), uv-curable glue
Embodiment 1
The preparation of light anode: in clean 100ml conical flask, being first added 20mL acetic acid and 10ml titanium tetraisopropylate,
5min is stirred on magnetic stirring apparatus is uniformly mixed the two.Later, measure 10mL deionized water, with dropper by deionized water dropwise
It is added in the mixed liquor in stirring.During dropwise addition, with the addition of deionized water, white is had in solution
Titanium tetraisopropylate hydrolysate occurs, and continues to stir, finally obtains transparent clear solution.Then by this solution in ultrasonic pond
It is ultrasonically treated 10min, is transferred in hydrothermal reaction kettle, reaction kettle is put into Muffle furnace later then, from room temperature to 200
DEG C processing 4h, 3 DEG C/min of heating rate.After reaction, hydrothermal reaction kettle is taken out while hot, with tap water shower hydro-thermal reaction
Kettle shell is cooled to room temperature, just obtains the TiO of white at this time2Slurry reacts extraction raffinate with colourless.By white TiO2 slurry
It is mixed in a certain ratio with extraction raffinate is reacted, just obtains TiO required for us after stirring 12h on magnetic stirring apparatus2Scrape pasting
Material.FTO electro-conductive glass is cut into 2.5cm x 3.5cm size, is put into the beaker equipped with dehydrated alcohol, dehydrated alcohol will
FTO substrate is totally submerged, and then beaker is put into ultrasonic pond and is cleaned by ultrasonic 30min, is taken out FTO substrate later and is placed on purification work
Make natural air drying in platform.The both sides up and down that high invisible tape covers FTO substrate conducting face are thought with 3M, and exposing area is about
The region of 2.5cm x 2.5cm, the TiO that region distance FTO substrate bottom about 2mm will be stirred evenly2Slurry is coated in
On this region, then use the sheet glass of surfacing by TiO2Slurry blade coating uniformly, tears adhesive tape off later, will be coated with TiO2Slurry
FTO substrate be put into Muffle furnace and be heat-treated, program setting is 450 DEG C of processing 30min after 110 DEG C of processing 30min, liter
Warm rate is 2~6 DEG C/min.After heat treatment, furnace cooling.There to be TiO later2FTO substrate be put into containing N719 contaminate
20h is adsorbed in the methanol solution of material.Dye strength is 0.3mM, and Dye Adsorption process is in glove box (VIII20G, MBRAUN, moral
State) in carry out.After the completion of absorption, FTO substrate is taken out, washes away the dyestuff not adsorbed completely on substrate with methanol to get positive to light
Pole.
WO on working electrode3Partial preparation: WO3Film is by the poly- wolframic acid of polyoxy reported in the literature (PPTA) precursor sol
Plating is made；The wherein preparation process of PPTA are as follows: the hydrogen peroxide (H for being 30% by the concentration of the W powder of 6g and 60mL2O2) mixing,
Vigorous reaction can occur in the process and release a large amount of heat, therefore the process need to carry out in -10 DEG C of ice bath.Reaction terminates
Afterwards, the W powder that filtering removal is not reacted completely, and obtained milky filtrate is placed in ultrasonic pond ultrasound 30min, it is extra to remove
H2O2.Continuous backflow is then carried out, first flow back at 55 DEG C 6h, and then flow back at 65 DEG C 1h, finally flows back at 85 DEG C
30min, further to remove extra H2O2And make solution gelatinizing, it needs accurately to control reflux temperature and time in reflux course
Coagulation occurs to avoid solution.After reflux course, colloidal sol becomes light yellow by milky, and the ethyl alcohol of equivalent is added at this time
(60ml), and continue that the colloidal sol of yellow can be obtained in 50 DEG C of reflux 12h.By gained colloidal sol be placed in refrigerator it is aging for a week after
Transparent, bisque PPTA precursor sol can be obtained.After obtaining PPTA colloidal sol, using three-electrode system in electrochemical operation
Stand (CHI 650D) use chronoamperometry carry out electrochemical deposition WO3Film, electroplating parameter are (0.5V, 150s), can be with
Obtain the WO of blue3Film, and it is placed on air drying with washes of absolute alcohol, finally 300 DEG C of roastings in Muffle furnace
The colorless and transparent WO that thickness is about 200nm can be obtained in 30min3Film.Notice that reserving exposed area on the electrode (reserves about
Area for 1/3) it is used for PProDOT-Me2Preparation.
PProDOT-Me on working electrode2Preparation: PProDOT-Me2It is formed a film using electrochemical polymerization, was specifically prepared
Journey are as follows: suitable monomer is dissolved in 0.1mol/L LiClO4In/acetonitrile solution, obtaining monomer molar concentration is 0.01mol/L's
Precursor solution；Secondly it is using above-mentioned electrode exposed part as working electrode, filamentary silver using electrochemical workstation (CHI-650D)
Reference electrode, platinized platinum are to carry out electrochemical deposition plated film to the three-electrode system of electrode, are applied using chronoamperometry and stablize electricity
Pressure, electroplating parameter are (1.5V, 5s).Then the film that plating obtains is cleaned in acetonitrile.
The preparation of electrolyte solution: electrolyte I-/I3 -Redox couple electrolyte, in the glove box for being full of high pure nitrogen
In take iodine and lithium iodide, incorporate propylene glycol carbonate, simple substance iodine concentration is 1mM in obtained solution, and lithium iodide concentrations are
300mM。
Embodiment 2
The assembling of self energizing electrochromic device
Working electrode and light anode are fixed face-to-face with uv-curable glue, with 5mL syringe in two panels tin indium oxide glass
Electrolyte solution is injected in gap among glass, then injection port is made into completed device with ultraviolet glue package curing.The present invention mentions
The self energizing electrochromic device of confession, under illumination condition, when working electrode is connected with light anode, WO3It can spontaneously colour,
Route can spontaneously fade when disconnecting.
Wherein, as shown in FIG. 1, FIG. 1 is the classical WO without catalysis material for the device architecture of preparation3Self energizing device, benefit
The device junction composition of the device and the offer self energizing electrochromic device of embodiment 2 that are faded with metal platinum acceleration, specific volume,
It is the classical WO without catalysis material respectively from left to right in figure3Self energizing device accelerates the device to fade using metal platinum, with
And self energizing electrochromic device of the present invention.
To the WO of no catalysis material3Self energizing device, the classical device and embodiment 2 for accelerating colour fading using metal platinum
The optical performance parameter for providing self energizing electrochromic device is measured, specifically, the optical property of device is needed in illumination
Under the conditions of test, testing light source is the halogen lamp of 150w, and performance test and register instrument are USB 2000+ type Ocean Optics
The portable optical recorder of company.Optical modulation performance curve and device of three kinds of devices between 400~800nm exist
Fig. 2~Fig. 4 is shown in circulation performance at 680nm wavelength under original state, wherein recurrent state is set as shorted devices state 20s,
Then keep off state 80s.Fig. 2 is the optical transmittance and initial cycle state outcome of three kinds of devices, in more detail
Response time relatively may refer to Fig. 3, and Fig. 3 is that detailed optical performance of three kinds of devices at 680nm compares data；It can from figure
To find out, PProDOT-Me is utilized2When the device to fade being accelerated to show highest optical modulation rate and most fast colour fading
Between.Make a general survey of all WO of existing literature report3The fading time of the performance of self energizing electrochromic device, 15.5s also enables this device
Part becomes most outstanding one of the device that fades.
The cycle performance for the device that embodiment 2 obtains is tested as shown in figure 4, Fig. 4 is that the self energizing that embodiment 2 obtains is electroluminescent
The cyclical stability test result of Electrochromic device, it can be seen from the figure that this device, in 200 circulations, fading time is only
22.0s only is extended to from 15.5s, has shown comparable cyclical stability.
The above description of the embodiment is only used to help understand the method for the present invention and its core ideas.It should be pointed out that pair
For those skilled in the art, without departing from the principle of the present invention, the present invention can also be carried out
Some improvements and modifications, these improvements and modifications also fall within the scope of protection of the claims of the present invention.
Claims (10)
1. a kind of self energizing electrochomeric films, by by WO3Film and poly- 3,4- (2,2- dimethyl allene, two oxygroup) thiophene are thin
Film is overlayed in the same substrate and is obtained.
2. self energizing electrochomeric films according to claim 1, which is characterized in that the WO in substrate3Face shared by film
Area ratio shared by long-pending and poly- 3,4- (2,2- dimethyl allene, two oxygroup) thiophene film is 2: (0.3~1.5).
3. self energizing electrochomeric films according to claim 1, which is characterized in that the substrate is tin indium oxide glass
Glass.
4. a kind of preparation method of self energizing electrochomeric films, comprising:
1) by WO3It is deposited in substrate, obtains deposition WO3The substrate of film；
2) in deposition WO3WO is not deposited in the substrate of film3Poly- 3, the 4- of site deposition (2,2- dimethyl allene, two oxygroup) thiophene
Film obtains self energizing electrochomeric films.
5. a kind of self energizing electrochromic device, comprising: light anode, working electrode and electrolyte；
Wherein, the working electrode is self energizing electrochomeric films described in claims 1 to 3 any one.
6. self energizing electrochromic device according to claim 5, which is characterized in that the light anode is in accordance with the following methods
It is prepared:
1) TiO is coated in substrate2Slurry obtains coating TiO2Substrate；
2) TiO will be coated2Substrate merging photosensitive dye solution in carry out Dye Adsorption, obtain light anode.
7. self energizing electrochromic device according to claim 6, which is characterized in that the photosensitive dye is ruthenium pyridine
Organometallic complex.
8. self energizing electrochromic device according to claim 6, which is characterized in that the substrate is fluorine-doped tin oxide
Glass.
9. self energizing electrochromic device according to claim 5, which is characterized in that the electrolyte is I-/I3 -Oxidation
Reduction is to electrolyte.
10. a kind of preparation method of self energizing electrochromic device, comprising: with glue that light anode and working electrode is solid face-to-face
It is fixed, and electrolyte is injected between light anode and working electrode, obtain self energizing electrochromic device；
Wherein, the working electrode is self energizing electrochomeric films described in claims 1 to 3 any one.
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| CN110736420A (en) * | 2019-09-19 | 2020-01-31 | 北京科技大学 | Preparation method of portable self-powered hydrogel strain sensor |
| CN113322500A (en) * | 2020-07-09 | 2021-08-31 | 中国科学技术大学 | Based on WO3Non-complementary absorption type electrochromic device of thin film and preparation method thereof |
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