CN109881198A - The preparation method of stannic oxide/vanadic anhydride core-shell structure multi-color electrochromic film - Google Patents
The preparation method of stannic oxide/vanadic anhydride core-shell structure multi-color electrochromic film Download PDFInfo
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Abstract
The present invention provides a kind of production methods of stannic oxide/vanadic anhydride core-shell structure multi-color electrochromic film, it include: that two hydrate of stannous chloride is dissolved in hydrochloric acid and the aqueous solution of thioacetic acid, it is added into the reaction kettle for being placed with conductive substrates, high-temperature heat treatment obtains homoepitaxial ground tin dioxide nanosheet array after hydro-thermal reaction；Using vanadic sulfate hydrate as vanadium source, vanadic anhydride is deposited on tin dioxide nanosheet array using potentiostatic method, finally heat treatment obtains the multi-color electrochromic film of core-shell structure in air.In the present invention tin dioxide nanosheet perpendicular to substrate and growth distribution it is uniform, vanadic anhydride uniformly fills the gap and surface for being coated on nanometer sheet.The laminated film has excellent cyclical stability and electrochromic property, and the Rapid reversible transformation between blue, green and yellow may be implemented, be expected to the adaptive camouflage field using Yu Haiyang, oasis and desert Environment.
Description
Technical field
The present invention relates to electrochomeric films technical fields, and in particular to a kind of stannic oxide/vanadic anhydride nucleocapsid knot
The preparation method of the multi-color electrochromic film of structure.
Background technique
Electrochromism is defined as the optical property of material under the effect of different applied voltages there is a phenomenon where reversible change,
This phenomenon is being embedded in and is being deviate from caused by the redox reaction in materials process as ion or electronics.Past tens
Nian Zhong never stops the research steps of electrochromic material, has been greatly developed in theory and practice.It is existing
Many fields are applied to due to its special optical modulation function in, electrochromic material, such as smart window, light-sensitive sunglasses,
Energy-saving information display and adaptive camouflage.It is a huge challenge that electrochromic material, which is applied to camouflage field,.Specifically
For, it is seen that the adaptive camouflage of optical band needs material to adjust itself color according to the color change of background, come reach with
The purpose of background fusion realizes that the perfection of vision-based detection is hidden.By previous research it is found that conducting polymer (Organic Electricity mutagens
Color material) it is normally used for camouflage field, because it is with fast switching time, polychrome variation and preferable flexibility etc. are excellent
Point.One remarkable advantage of organic electrochromic material is the color change that film can be adjusted by replacement side-chain radical.
So, the organic conductive polymer seemingly optimal selection as camouflage electrochromic material.However, due to organic monomer
Complicated synthetic route, harsh reaction condition, low-yield and thin polymer film in the natural environment stability difference etc. because
Element limits its practical application.Therefore, the application of inorganic electrochromic material in this regard is explored to be of great significance, because
With good chemical stability, preparation process is simple for it, it is easy to accomplish the advantages that all solid stateization of device.
Transition metal oxide vanadic anhydride has the dual electrochromic property of anode and cathode, and unique polychrome is electroluminescent
Color shifting properties make that it is suitable for many special dimensions.Vanadium pentoxide films can under voltage appropriate in yellow, green and
It is reversibly converted between blue, these three colors and desert, the color of oasis and ocean matches, therefore vanadic anhydride is answered
It is feasible for the adaptive camouflage of military affairs in these environment.In general, inorganic electrochromic material has excellent uvioresistant
Beta radiation performance, this further improves the application of vanadic anhydride in this area.But vanadium pentoxide films are electroluminescent
There are also disadvantage in Electrochromic device, for example, cyclic reversibility and stability it is poor, conductivity and ionic diffusion coefficient are low, coloring effect
Rate is low.Nowadays, composite material has received widespread attention, because composite construction can bring excellent synergisticing performance or multi-functional
Property.Stannic oxide is N-shaped wide band gap semiconducter, due to its high electronics transfer rate, chemical inertness and to atmospheric conditions and high temperature
Stability is widely used in lithium battery, solar battery, liquid crystal display, sensor and electrochromic device.Here, passing through
Hydro-thermal and the film technique of electro-deposition have synthesized stannic oxide/vanadic anhydride core-shell structure multi-color electrochromic film.Two
Being introduced into for tin oxide nano piece does not influence the color change of vanadic anhydride in oxidation-reduction process, and laminated film still may be used
Reversibly to change between yellow, green and blue.In addition, laminated film is in transmission modulation, response time, coloration efficiency
Excellent performance is also shown in terms of cyclical stability.
Summary of the invention
To reach this purpose, the present invention provides a kind of electroluminescent changes of stannic oxide/vanadic anhydride core-shell structure polychrome
The preparation method of color film.The inorganic composite film of preparation method preparation has and the good binding force of substrate, chemical stabilization
Property high, the advantages of optical cycle is had excellent performance.Meanwhile the electrochomeric films may be implemented between yellow, green and blue
It reversibly converts, has broad application prospects.
In order to achieve the above-mentioned object of the invention, present invention provide the technical scheme that
A kind of preparation method of the multi-color electrochromic film of stannic oxide/vanadic anhydride core-shell structure, including it is as follows
Step:
(1) conductive substrates are cleaned by ultrasonic in water, drying is stand-by；
(2) urea, hydrochloric acid, thioacetic acid and two hydrate of stannous chloride are dissolved in deionized water, form presoma
Solution；
(3) precursor solution in step (2) is added in the reaction kettle that placed conductive substrates, reacts 4 at 80~160 DEG C
~8h rinses drying, then 400~600 DEG C of 2~4h of heat treatment in tube furnace, has obtained tin dioxide nanosheet battle array after taking-up
Column；
(4) vanadic sulfate hydrate, lauryl sodium sulfate and sodium chloride are dissolved in the mixed of deionized water and dehydrated alcohol
It closes in solution, it is 1.5~2.0 that dilute sulfuric acid, which is added dropwise, and adjusts the pH value of solution, forms the electrolysis for being used to prepare vanadic anhydride
Liquid；
It (5) is reference electrode using the tin dioxide nanosheet array in step (3) as working electrode, Ag/AgCl electrode
And platinized platinum is, using the electrolyte of the vanadic anhydride of step (4) preparation, permanent electricity to be utilized on electrochemical workstation to electrode
Position method deposits vanadic anhydride, obtained laminated film is dried, finally 300~500 DEG C of 2~4h of heat treatment in air, is obtained
Stannic oxide/vanadic anhydride core-shell structure multi-color electrochromic film is arrived.
It is used as the preferred technical solution of the present invention below:
In step (1), conductive substrates are cleaned by ultrasonic in water, drying is stand-by, it specifically includes:
Conductive substrates are cleaned by ultrasonic 10~30min in the beaker equipped with deionized water, are then placed on 60 DEG C of baking oven
3~10min surface treatment is done in middle drying before carrying out hydro-thermal reaction in plasma cleaner.
The conductive substrates are FTO electro-conductive glass, conductive carbon cloth film or conductive metal film.Further preferably, the FTO
Electro-conductive glass is commercial product, and size can be customized, it is easy to accomplish the preparation of different area film.
In step (2), urea, hydrochloric acid, thioacetic acid and two hydrate of stannous chloride are dissolved in deionized water, formed
Precursor solution specifically includes: urea, thioacetic acid and hydrochloric acid being successively dissolved in deionized water, stirred to clarify, is added
Two hydrate of stannous chloride, stirring form precursor solution (having White Flocculus).
The urea, hydrochloric acid, thioacetic acid, stannous chloride dihydrate, deionized water the ratio between dosage for 0.6g~
1.2g:0.5mL~2mL:10 μ μ of L~30 L:0.1g~0.3g:60mL~100mL.
Further preferably, the mass percent of the hydrochloric acid is 20%~38%.
In step (3), conductive substrates are tilted a certain angle and are placed in reaction kettle, wherein the conduction of FTO electro-conductive glass
Placed face down.The protective gas of the tube furnace is argon gas.Further preferably, protective gas argon flow is 100sccm.
In step (4), the vanadic sulfate hydrate, lauryl sodium sulfate, sodium chloride, deionized water and anhydrous second
The amount ratio of alcohol is 1.2~2.0g:0.1~0.3g:0.1~0.8g:40mL~80mL:20~40mL；
Further preferably, the concentration of the dilute sulfuric acid is 0.3~0.6mol/L.
In step (5), the condition of the potentiostatic method are as follows: potentiostatic electrodeposition voltage is 1V~3V, sedimentation time 70
~170s.Further preferably, the condition of the potentiostatic method are as follows: potentiostatic electrodeposition voltage be 2V, sedimentation time be 90~
150s。
The heating rate of last heat treatment process is 1 DEG C of min-1, the type of cooling is furnace cooling.
Preferably, the electrochromic material has core-shell structure, using the tin dioxide nanosheet of vertical arrangement as core, five
V 2 O is the shell of filling and cladding, and being formed has rough surface, the good laminated film of chemical stability.
Preferably, by the tin dioxide nanosheet of hydro-thermal method homoepitaxial, there is strong binding force with substrate, formed and stablized
Grade gridding structure, tin dioxide nanosheet thickness is about 20nm.
Preferably, the thickness of laminated film is about 500nm, and using tin dioxide nanosheet as skeleton, vanadic anhydride is to fill out
The laminated film for filling the core-shell structure of covering material shows excellent electrochromic property, has stable optical cycle
Can, thirdly color electrochromic property is especially attracted attention, it can be applied to the adaptive camouflage of military affairs in a variety of environment.
Compared with prior art, the invention has the following advantages that
1, electrochomeric films prepared in the present invention have core-shell structure, the tin dioxide nanosheet of Hydrothermal Growth
There is strong binding force with substrate, improves the stability of laminated film.The grade gridding structure of nanometer sheet is to vanadic anhydride crystalline substance
Grain has refining effect, and obtained film has the rough surface of thorn-like protrusion, increases the contact area with electrolyte, improves
Electron-transport speed and ion diffusion rates, accelerate kinetics process, improve the response time of electrochomeric films
And coloration efficiency.
2, stannic oxide does not influence the performance of vanadic anhydride inverible transform between yellow, green and blue, and five
The color diversity of V 2 O has obtained continuing application.
3, the excellent properties of inorganic electrochromic material are applied, and provide the exploration of organic multi-color electrochromic material
Supplement proposes to obtain may be implemented the new approaches of the electrochromic material of yellowish green blue three-color variation.
4, preparation method of the invention has fabulous exploitativeness, and it is thin that hydro-thermal with electro-deposition method is easily achieved large area
The large-scale industrial production of film.
Detailed description of the invention
Fig. 1 is that tin dioxide nanosheet and stannic oxide/vanadic anhydride prepared in embodiment 2 in the present invention are compound
Scanning electron photo of the surface of film under different amplification；
Fig. 2 is for FTO electro-conductive glass substrate and by single layer stannic oxide vanadic anhydride prepared by the method in embodiment 2
And stannic oxide/vanadic anhydride electrochromic material X ray diffracting spectrum comparison diagram；
Fig. 3 is stannic oxide/vanadic anhydride compound electrochromic membrane prepared by embodiment 2 in the present invention in difference
UV-Vis spectra transmission plot under voltage；
Fig. 4 is that stannic oxide/vanadic anhydride compound electrochromic membrane prepared by embodiment 2 is applying in the present invention
Voltage spaces are the chronoa mperometric plot and the corresponding transmissivity in situ song under 450nm wavelength of -1V (30s) and 1V (30s)
Line；
Fig. 5 is stannic oxide/vanadic anhydride compound electrochromic membrane optics prepared by embodiment 2 in the present invention
Cyclical stability test result figure.
Specific embodiment
The present invention is described further with reference to the accompanying drawings and examples.
Embodiment 1
The preparation of stannic oxide/vanadic anhydride core-shell structure multi-color electrochromic film:
(1) FTO electro-conductive glass (production of Shenzhen south China Xiang Cheng scientific & technical corporation) is successively cleaned by ultrasonic 20 in deionized water
Minute, it is subsequently placed in 60 DEG C of baking ovens and dries, handled 5 minutes in plasma cleaner before use；
(2) 1g urea, 1mL (37wt%) hydrochloric acid, 20 μ L thioacetic acid are successively dissolved in 80mL deionized water, stirring 5
After minute, then two hydrate of 0.2g stannous chloride is added thereto, stirring forms uniform precursor solution after ten minutes；
(3) precursor solution in step (2) is added in autoclave, before conductive substrates slant setting is immersed in
It drives in liquid solution, wherein FTO is conductive down.The hydro-thermal reaction 6h in 120 DEG C of baking oven, water cooling is to room temperature 25 after fully reacting
DEG C, it takes out sample wash and completely dries a night afterwards, 500 DEG C of heat treatment 3h, have obtained uniform life in the tube furnace for being connected with argon gas
Long tin dioxide nanosheet array；
(4) 1.63g vanadic sulfate hydrate, 0.2g lauryl sodium sulfate and 0.6g sodium chloride are dissolved in 60mL deionization
It in the mixed solution of water and 30mL dehydrated alcohol, stirs evenly, the dilute sulfuric acid that 0.5mol/L is then added dropwise adjusts solution
PH to 1.8 forms the electrolyte for being used to prepare vanadic anhydride；
It (5) is reference electrode using the tin dioxide nanosheet array in step (3) as working electrode, Ag/AgCl electrode
And platinized platinum is, using the electrolyte of the vanadic anhydride of step (4) preparation, permanent electricity to be utilized on electrochemical workstation to electrode
Position method deposits vanadic anhydride, design parameter are as follows: deposition voltage 2V, sedimentation time 90s.By obtained laminated film at 60 DEG C
12h is dried in baking oven, is then heat-treated 3h at 400 DEG C in air, and the heating rate of Muffle furnace used is 1 DEG C of min-1, with furnace
After cooling, stannic oxide/vanadic anhydride core-shell structure multi-color electrochromic film has been finally obtained.
Stannic oxide prepared by the present embodiment/vanadic anhydride compound electrochromic membrane has core-shell structure, dioxy
Change tin nanometer sheet is core, and vanadic anhydride is shell, and tin dioxide nanosheet thickness is about in 20nm or so, film thickness
300nm is uniformly grown in conductive substrates at classification network, has strong binding force with substrate.Vanadic anhydride deposition
Cladding is filled in the air gap periphery that tin dioxide nanosheet is constituted, and since sedimentation time is relatively short, laminated film is in difference
Shallower color is shown under operating voltage, thickness is about 400nm, occurs maximum transmitance modulation at 450nm and is about
40%.
Embodiment 2
The preparation of stannic oxide/vanadic anhydride core-shell structure multi-color electrochromic film:
(1) FTO electro-conductive glass (production of Shenzhen south China Xiang Cheng scientific & technical corporation) is successively cleaned by ultrasonic 20 in deionized water
Minute, it is subsequently placed in 60 DEG C of baking ovens and dries, handled 5 minutes in plasma cleaner before use:
(2) 1g urea, 1mL (37wt%) hydrochloric acid, 20 μ L thioacetic acid are successively dissolved in 80mL deionized water, stirring 5
After minute, then two hydrate of 0.2g stannous chloride is added thereto, stirring forms uniform precursor solution after ten minutes；
(3) precursor solution in step (2) is added in autoclave, before conductive substrates slant setting is immersed in
It drives in liquid solution, wherein FTO is conductive down.The hydro-thermal reaction 6h in 120 DEG C of baking oven, water cooling is to room temperature 25 after fully reacting
DEG C, it takes out sample wash and completely dries a night afterwards, 500 DEG C of heat treatment 3h, have obtained uniform life in the tube furnace for being connected with argon gas
Long tin dioxide nanosheet array；
(4) 1.63g vanadic sulfate hydrate, 0.2g lauryl sodium sulfate and 0.6g sodium chloride are dissolved in 60mL deionization
It in the mixed solution of water and 30mL dehydrated alcohol, stirs evenly, the dilute sulfuric acid that 0.5mol/L is then added dropwise adjusts solution
PH to 1.8 forms the electrolyte for being used to prepare vanadic anhydride；
It (5) is reference electrode using the tin dioxide nanosheet array in step (3) as working electrode, Ag/AgCl electrode
And platinized platinum is to electrode, the electrolyte prepared using step (4) deposits five oxygen using potentiostatic method on electrochemical workstation
Change two vanadium, design parameter are as follows: deposition voltage 2V, sedimentation time 120s.Obtained laminated film is dried in 60 DEG C of baking ovens
12h, 3h is then heat-treated at 400 DEG C in air, and the heating rate of Muffle furnace used is 1 DEG C of min-1, after furnace cooling, most
Stannic oxide/vanadic anhydride core-shell structure multi-color electrochromic film has been obtained eventually.
Stannic oxide prepared by the present embodiment/vanadic anhydride compound electrochromic membrane has core-shell structure, dioxy
Change tin nanometer sheet is core, and vanadic anhydride is shell, it can be seen that, tin dioxide nanosheet thickness is thin in 20nm or so in Fig. 1
Film thickness is about 300nm, is uniformly grown in conductive substrates at classification network, has strong binding force with substrate.Five oxygen
Change two vanadium deposition cladding and be filled in the air gap periphery that tin dioxide nanosheet is constituted, forms the THIN COMPOSITE with rough surface
Film, thickness are about 500nm.The XRD diagram of Fig. 2 shows that synthesized film is crystalline state, as can be seen from the figure obtains
Composite electrochromic material is crystalline state.As shown in figure 3, can by transmittance curve of the film under three kinds of different working conditions
Know occur maximum transmitance at 450nm and be modulated to 47%, the shape of transmittance curve is not both by under film different conditions
Different colors determines.Compound electrochromic membrane fades as shown in Figure 4 and the coloring response time is respectively 8s and 5s.In Fig. 5
Shown cyclic curve show laminated film by 2000 times continuously fade after still maintain have initial optical transmittance tune
The 85% of system.It can be seen from the above, stannic oxide prepared by the present invention/vanadic anhydride compound electrochromic membrane has response
Speed is fast, good cycling stability and the advantages of multi-color electrochromic.
Embodiment 3
The preparation of stannic oxide/vanadic anhydride core-shell structure multi-color electrochromic film:
(1) conductive carbon cloth film is successively cleaned by ultrasonic 20 minutes in deionized water, is subsequently placed in 60 DEG C of baking ovens and dries,
It is handled 5 minutes in plasma cleaner before use:
(2) 1g urea, 1mL (37wt%) hydrochloric acid, 20 μ L thioacetic acid are successively dissolved in 80mL deionized water, stirring 5
After minute, then two hydrate of 0.2g stannous chloride is added thereto, stirring forms uniform precursor solution after ten minutes；
(3) precursor solution in step (2) is added in autoclave, before conductive substrates slant setting is immersed in
It drives in liquid solution, wherein FTO is conductive down.The hydro-thermal reaction 6h in 120 DEG C of baking oven, water cooling is to room temperature 25 after fully reacting
DEG C, it takes out sample wash and completely dries a night afterwards, 500 DEG C of heat treatment 3h, have obtained uniform life in the tube furnace for being connected with argon gas
Long tin dioxide nanosheet array；
(4) 1.63g vanadic sulfate hydrate, 0.2g lauryl sodium sulfate and 0.6g sodium chloride are dissolved in 60mL deionization
It in the mixed solution of water and 30mL dehydrated alcohol, stirs evenly, the dilute sulfuric acid that 0.5mol/L is then added dropwise adjusts solution
PH to 1.8 forms the electrolyte for being used to prepare vanadic anhydride；
It (5) is reference electrode using the tin dioxide nanosheet array in step (3) as working electrode, Ag/AgCl electrode
And platinized platinum is, using the electrolyte of the vanadic anhydride of step (4) preparation, permanent electricity to be utilized on electrochemical workstation to electrode
Position method deposits vanadic anhydride, design parameter are as follows: deposition voltage 2V, sedimentation time 150s.By obtained laminated film 60
12h is dried in DEG C baking oven, is then heat-treated 3h at 400 DEG C in air, the heating rate of Muffle furnace used is 1 DEG C of min-1, with
After furnace is cooling, stannic oxide/vanadic anhydride core-shell structure multi-color electrochromic film has been finally obtained.
Stannic oxide prepared by the present embodiment/vanadic anhydride compound electrochromic membrane has core-shell structure, dioxy
Change tin nanometer sheet is core, and vanadic anhydride is shell, and tin dioxide nanosheet is uniformly grown in conductive base at classification network
On bottom, there is strong binding force with substrate.Vanadic anhydride deposition cladding is filled in the gap week that tin dioxide nanosheet is constituted
It encloses, forms the laminated film with rough surface.Stannic oxide prepared by the present embodiment/vanadic anhydride composite electrochromic
Film shows different colors when applying different voltages, as shown in the following table 1 and Figure of abstract, is displayed in blue in -1V, 0.4V
Display green, 1V show that inverible transform may be implemented in yellow, three kinds of colors, and the color that the Lab value of each color demonstrates film becomes
Change, the results are shown in Table 1.
Table 1
The embodiment of invention described above, for those skilled in the art, in the present invention
Spirit and principle within made modification, improvements and modifications, these modification, improvements and modifications also should be regarded as protection of the invention
Range.
Claims (10)
1. a kind of preparation method of stannic oxide/vanadic anhydride core-shell structure multi-color electrochromic film, which is characterized in that
Include the following steps:
(1) conductive substrates are cleaned by ultrasonic in water, drying is stand-by；
(2) urea, hydrochloric acid, thioacetic acid and two hydrate of stannous chloride are dissolved in deionized water, form precursor solution；
(3) precursor solution in step (2) is added placed in the reaction kettles of conductive substrates, react 4 at 80~160 DEG C~
8h rinses drying, then 400~600 DEG C of 2~4h of heat treatment in tube furnace, has obtained tin dioxide nanosheet array after taking-up；
(4) mixing for vanadic sulfate hydrate, lauryl sodium sulfate and sodium chloride being dissolved in deionized water and dehydrated alcohol is molten
In liquid, it is 1.5~2.0 that dilute sulfuric acid, which is added dropwise, and adjusts the pH value of solution, forms the electrolyte for being used to prepare vanadic anhydride；
(5) using the tin dioxide nanosheet array in step (3) as working electrode, Ag/AgCl electrode be reference electrode and
Platinized platinum is, using the electrolyte of the vanadic anhydride of step (4) preparation, potentiostatic method to be utilized on electrochemical workstation to electrode
Vanadic anhydride is deposited, obtained laminated film is dried, finally 300~500 DEG C of 2~4h of heat treatment in air, is obtained
Stannic oxide/vanadic anhydride core-shell structure multi-color electrochromic film.
2. preparation method according to claim 1, which is characterized in that in step (1), by conductive substrates, ultrasound is clear in water
It washes, drying is stand-by, it specifically includes:
Conductive substrates are cleaned by ultrasonic 10~30min in the beaker equipped with deionized water, is then placed in 60 DEG C of baking oven and dries
It is dry, 3~10min surface treatment is done in plasma cleaner before carrying out hydro-thermal reaction.
3. preparation method according to claim 1, which is characterized in that in step (1), the conductive substrates are led for FTO
Electric glass, conductive carbon cloth film or conductive metal film.
4. preparation method according to claim 1, which is characterized in that in step (2), by urea, hydrochloric acid, thioacetic acid and
Two hydrate of stannous chloride is dissolved in deionized water, is formed precursor solution, is specifically included: by urea, thioacetic acid and salt
Acid is successively dissolved in deionized water, is stirred to clarify, and two hydrate of stannous chloride is added, and stirring forms precursor solution.
5. the preparation method according to claim 4, which is characterized in that in step (2), the urea, hydrochloric acid, sulfydryl second
The ratio between acid, stannous chloride dihydrate, dosage of deionized water are the 0.6g~1.2g:0.5mL~2mL:10 μ μ of L~30 L:0.1g
~0.3g:60mL~100mL.
6. preparation method according to claim 5, which is characterized in that the mass percent of the hydrochloric acid be 20%~
38%.
7. preparation method according to claim 1, which is characterized in that in step (4), the vanadic sulfate hydrate,
Lauryl sodium sulfate, sodium chloride, deionized water and dehydrated alcohol amount ratio be 1.2~2.0g:0.1~0.3g:0.1~
0.8g:40mL~80mL:20~40mL.
8. preparation method according to claim 1, which is characterized in that in step (4), the concentration of the dilute sulfuric acid is
0.3~0.6mol/L.
9. preparation method according to claim 1, which is characterized in that in step (5), the condition of the potentiostatic method
Are as follows: potentiostatic electrodeposition voltage is 1V~3V, and sedimentation time is 70~170s.
10. preparation method according to claim 9, which is characterized in that in step (5), the condition of the potentiostatic method
Are as follows: potentiostatic electrodeposition voltage is 2V, and sedimentation time is 90~150s.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111679455A (en) * | 2020-06-29 | 2020-09-18 | 绍兴迪飞新材料有限公司 | Multicolor color-changing thin film device and preparation method thereof |
| CN112415826A (en) * | 2020-11-18 | 2021-02-26 | 浙江大学 | Method for simply and efficiently preparing multicolor all-solid-state electrochromic device |
| CN112490414A (en) * | 2019-09-11 | 2021-03-12 | 南京工业大学 | Tin dioxide and vanadium pentoxide composite electrode material and preparation method and application thereof |
Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61103981A (en) * | 1984-10-29 | 1986-05-22 | Canon Inc | Electrochromic element |
| WO2005116293A1 (en) * | 2004-05-28 | 2005-12-08 | Konica Minolta Holdings, Inc. | Thin film forming equipment and thin film forming method |
| CN1739057A (en) * | 2003-01-31 | 2006-02-22 | 内拉有限公司 | Electrochromic display device |
| CN1776013A (en) * | 2005-11-25 | 2006-05-24 | 湖南师范大学 | Supersonic spraying method for preparing vanadium pentoxide thin film |
| US20130168595A1 (en) * | 2011-12-29 | 2013-07-04 | Keith Chang | Nanometer thermal insulation coating and method of manufacturing the same |
| CN103469272A (en) * | 2013-09-04 | 2013-12-25 | 浙江大学 | Tungsten trioxide/polyaniline core-shell nanowire array radiochromic film and preparation method thereof |
| CN103966638A (en) * | 2014-05-07 | 2014-08-06 | 哈尔滨工业大学 | Preparation method for vanadium pentoxide nanowires of large-area crystalline/amorphous core-shell structures |
| CN104118904A (en) * | 2014-07-01 | 2014-10-29 | 济南大学 | Preparation method and application of three-dimensional hollow multilevel-structured stannic oxide gas-sensitive material |
| CN106612618A (en) * | 2014-07-31 | 2017-05-03 | Sage电致变色显示有限公司 | Controlled heating for electrochromic devices |
| CN107163928A (en) * | 2017-06-09 | 2017-09-15 | 合肥工业大学 | A kind of tungstic acid/vanadic anhydride core-shell nano linear array electrochromic material and preparation method thereof |
| US9977262B2 (en) * | 2014-03-12 | 2018-05-22 | Honeywell International, Inc. | Electrochromic lenses and methods of fabricating the same |
-
2019
- 2019-04-10 CN CN201910285964.8A patent/CN109881198B/en active Active
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61103981A (en) * | 1984-10-29 | 1986-05-22 | Canon Inc | Electrochromic element |
| CN1739057A (en) * | 2003-01-31 | 2006-02-22 | 内拉有限公司 | Electrochromic display device |
| WO2005116293A1 (en) * | 2004-05-28 | 2005-12-08 | Konica Minolta Holdings, Inc. | Thin film forming equipment and thin film forming method |
| CN1776013A (en) * | 2005-11-25 | 2006-05-24 | 湖南师范大学 | Supersonic spraying method for preparing vanadium pentoxide thin film |
| US20130168595A1 (en) * | 2011-12-29 | 2013-07-04 | Keith Chang | Nanometer thermal insulation coating and method of manufacturing the same |
| CN103469272A (en) * | 2013-09-04 | 2013-12-25 | 浙江大学 | Tungsten trioxide/polyaniline core-shell nanowire array radiochromic film and preparation method thereof |
| US9977262B2 (en) * | 2014-03-12 | 2018-05-22 | Honeywell International, Inc. | Electrochromic lenses and methods of fabricating the same |
| CN103966638A (en) * | 2014-05-07 | 2014-08-06 | 哈尔滨工业大学 | Preparation method for vanadium pentoxide nanowires of large-area crystalline/amorphous core-shell structures |
| CN104118904A (en) * | 2014-07-01 | 2014-10-29 | 济南大学 | Preparation method and application of three-dimensional hollow multilevel-structured stannic oxide gas-sensitive material |
| CN106612618A (en) * | 2014-07-31 | 2017-05-03 | Sage电致变色显示有限公司 | Controlled heating for electrochromic devices |
| CN107163928A (en) * | 2017-06-09 | 2017-09-15 | 合肥工业大学 | A kind of tungstic acid/vanadic anhydride core-shell nano linear array electrochromic material and preparation method thereof |
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