CN102191526B - Preparation method of optical device - Google Patents
Preparation method of optical device Download PDFInfo
- Publication number
- CN102191526B CN102191526B CN 201010127932 CN201010127932A CN102191526B CN 102191526 B CN102191526 B CN 102191526B CN 201010127932 CN201010127932 CN 201010127932 CN 201010127932 A CN201010127932 A CN 201010127932A CN 102191526 B CN102191526 B CN 102191526B
- Authority
- CN
- China
- Prior art keywords
- nickel oxide
- electrode
- oxide film
- membrane electrode
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Images
Landscapes
- Electrochromic Elements, Electrophoresis, Or Variable Reflection Or Absorption Elements (AREA)
Abstract
The invention discloses a preparation method of an optical device. The preparation method comprises the steps of: preparing a 0.01-1MOL/L nickel nitrate solution; forming an electroplating solution; adding a nitric acid solution in the electroplating solution, and adjusting the pH value of the electroplating solution to be 3-4; forming a nickel oxide film on a conductive substrate in a cathode electroplating manner, preparing a nickel oxide film electrode with a transparent conductive glass substrate and the nickel oxide film, wherein the nickel oxide film electrode has an optical modulation capability range; and thermally treating the nickel oxide film electrode at the temperature of 200-300 DEG C instead of activating the nickel oxide film electrode with an electrochemical method, so that the nickel oxide film electrode achieves a favorable lithium ion implanting/emigrating property and an optical modulation capability range is enlarged. The preparation method disclosed by the invention is suitable to various occasions in need of the preparation method of the optical device.
Description
Technical field
The present invention relates to a kind of preparation method of Optical devices, particularly relate to a kind of have that good lithium ion embeds and the electrochromism electrode of the nickel oxide layer of moving out with and preparation method thereof, wherein this electrode can be used for the heat-tinting electrode in a kind of electrochromism device.
Background technology
The characteristic of electrochromism membrane electrode generally is to change over colored state or be varied to vitreous state from colored state from vitreous state for changing its optical property when the embedding of positively charged ion and electronics or when moving out membrane structure, and its colour-change is reversing process.This kind electrochromic material has many industrial application, for example: intelligent type energy saving window, sun roof, glareproof mirror, indicating meter and sensor etc.
The coloring mode of electrochromic material can be divided into two kinds: first kind is called negative electrode painted (cathodiccoloration), painted when being positively charged ion and electronics embedding membrane electrode, and when positively charged ion and electronics are moved out membrane electrode, discolor, with this kind/thin-film material of the mode of discoloring has Tungsten oxide 99.999, molybdenum oxide, titanium oxide, Viology and PEDOT etc.; Second kind is called anode painted (anodic coloration), discolor when being positively charged ion and electronics embedding membrane electrode, and painted when positively charged ion and electronics are moved out membrane electrode, with this kind/thin-film material of the mode of discoloring has nickel oxide, iridium oxide and Prussian blue etc.
Nickel oxide film is the common painted electrochromic material of anode, presents vitreous state when positively charged ion and electronics embed film, and presents chocolate when positively charged ion and electronics are moved out film.The preparation method of nickel oxide film electrode has hot evaporation, sputter, sol-gel method and electrochemical deposition etc.In these preparation methods, electrochemical deposition method is most convenient and cheap, and easily by adjusting size of current, solution composition and depositing temperature are controlled the thickness of nickel oxide film.
During the electrochromism characteristic of most of research nickel oxide film electrode, all with the basic metal aqueous solution as ionogen, and the painted reaction of nickel oxide film can be expressed as follows:
Ni(OH)
2+OH
-→NiOOH+H
2O+e
-
Transparent (transparent) dark (darken)
The nickel oxide of divalence is oxidized to the nickel oxide of trivalent in the following formula, and film becomes chocolate by transparent transition.When above-mentioned reaction reversed, nickel oxide film was transformed into clear, colorless.Yet in complementary type electrochromism assembly (tungsten oxide film is that the working electrode nickel oxide film is counter electrode), the basic metal aqueous solution is not suitable for as the ionogen in the assembly, because aqueous alkaline electrolyte can cause the dissolving of tungsten oxide film electrode.Therefore, based on the non-aqueous electrolyte of lithium ion, as lithium perchlorate (LiClO
4) be dissolved in the ionogen that propylene carbonate (propylene carbonate) forms and then select for the ionogen of complementary assembly the best, this kind ionogen can make assembly have long-term operational stability.Therefore, the lithium ion character that embeds/move out nickel oxide film just seems suitable important.In order to make lithium ion can carry out quick and reversible embedding and the process of moving out in the nickel oxide film, traditional nickel oxide film need utilize electrochemical method to carry out the program of so-called initial activation.One of method of initial activation nickel oxide is exactly to apply repeatedly Eo+ to being immersed in the membrane electrode that contains in the lithium-ion electrolyte, makes lithium ion partly embed and form the lithium nickel oxide film in the nickel oxide film that its chemical equation is as follows:
NiO
x+yLi
++ye
-→Li
yNiO
x
Wherein, the initial lithium ion that embeds has activated the agent structure of nickel oxide film, makes this film can subsequently carry out the process that reversible lithium ion embeds/moves out.Yet, the redox potential that applies how many cycle indexes just can make it to have the process that good lithium ion embeds/moves out in the nickel oxide membrane electrode, main according to script nickel oxide depositing of thin film condition, need to carry out tens of inferior film reactivation processs usually at least.But, if needing to carry out activation treatment earlier in electrolytic solution before use, could use membrane electrode, can increase the programstep of extra cleaning film electrode like this, and cause the complexity on the processing procedure, and increase manufacturing cost.
In view of this, people such as M.Rubin uses LiNiO
2As target, directly deposit the lithium nickel oxide membrane electrode in the mode of sputter, the cycle index that reduces the required activation of film is for once.But, use the sputtering method deposit film to need expensive vacuum apparatus, can't effectively reduce manufacturing cost.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of preparation method of Optical devices, can solve high nickel oxide film electrode and similar electrode making equipment costliness, problem that cost of manufacture is high.
The present invention has disclosed an electrode with bigger electrochromism scope, the membrane electrode that electrochemical method deposits, only need through suitable thermal treatment, namely have good lithium ion and embed/move out characteristic, directly can use the electrochromism electrode as complementary electrochromism assembly.
One of purpose of the present invention, for improving in the past the nickel oxide membrane electrode when using lithium-ion electrolyte to drive cation source as variable color, the not convenient property of the reactivation process that need circulate through an electrochemical redox.
The invention provides a kind of preparation method of Optical devices, the technical scheme that adopts is: a kind of preparation method of Optical devices comprises: configuration 0.01-1MOL/L nickel nitrate solution; Form electroplate liquid; Add salpeter solution in this electroplating solution, its pH value is adjusted between the 3-4; Utilize the negative electrode plating mode to form a nickel oxide film at a conductive base, finish a nickel oxide membrane electrode and have this transparent conducting glass base material and this nickel oxide film, wherein this nickel oxide membrane electrode has an optical modulation limit of power; And do not activate this nickel oxide membrane electrode with electrochemical method, and heat-treat for about 200 ℃-300 ℃ with temperature, so that this nickel oxide membrane electrode has the character that good lithium ion embeds/moves out, and this optical modulation limit of power of augmentation.
Preferably, in order to keep the concentration of nitrate ion in the electroplate liquid, can add saltpetre, SODIUMNITRATE or the lithium nitrate solution of 0.1MOL/L-1MOL/L in electroplate liquid.
Also comprise the electrical capacity of measuring this nickel oxide membrane electrode with following method, whether good to learn the character that this lithium ion embeds/move out: as to be working electrode with this nickel oxide film thin electrodes, be counter electrode with a platinum titanium mesh, being reference electrode with silver/silver chloride, is lithium perchlorate (LiClO with 1MOL/L
4) to be dissolved in propylene carbonate be electrolyte solution, this working electrode is carried out cyclic voltammetric scan analysis.
Preferably, wherein after this thermal treatment of process, this nickel oxide film has good electrochromism character.
A kind of preparation method of Optical devices comprises: at the enterprising electroplating of a conductive base, to form a nickel oxide film, finish a nickel oxide membrane electrode and comprise this nickel oxide film and this conductive base; And this nickel oxide membrane electrode of thermal treatment, so that this nickel oxide membrane electrode has the character that good lithium ion embeds/moves out.
Preferably, this heat treated temperature is approximately between 150 degree Celsius, 450 degree extremely Celsius.
Preferably, this heat treated temperature is about 250 degree Celsius.
Preferably, this heat treatment period is about 30 minutes to 2 hours.
Nickel oxide film after the thermal treatment/discoloring penetrates rate variance and can reach about 50.3%.Heal when thick when film thickness, the painted volume increase of film can promote film and color depth, makes the optics penetration of film electrochromism change and becomes greatly.So the present invention's film thickness is healed when thick, it/discolors and penetrates rate variance and can further increase.
This nickel oxide membrane electrode does not need to utilize electrolytic solution to activate.
This nickel oxide membrane electrode does not need cleaning step to wash this electrolytic solution off.
The present invention can more comprise with the nickel oxide membrane electrode as the heat-tinting electrode, as the painted electrode of reduction, prepares an electrochromism assembly with the tungsten oxide film electrode.Electrochromism assembly of the present invention can comprise first electrode and second electrode that are formed on the transparent or semitransparent base material, and ionogen.And its first electrode, second electrode and ionogen or its combination can comprise an electrochromic material.
The base material of first electrode and second electrode select following selection for use: glass baseplate (glass panelsor substrate), PET (polyethylene terephthalate), PVC (polyvinyl chloride) and PE (polyethlene) etc., but not as limit.
Conductive base on first electrode, second electrode or this two electrode can be a transparency conducting layer that is formed on the transparent substrate.The material of transparency conducting layer can select that metal oxide film such as tin indium oxide (ITO), stannic oxide are mixed fluorine (FTO), stannic oxide is mixed antimony (ATO), doped zinc oxide aluminium; With and composition thereof the group that formed, but not as limit.
The material of the electrochromism thin film layer on the first electrode transparency conducting layer may be selected to be tungsten oxide, molybdenum oxide, niobium oxide and PEDOT etc., but not as limit.
Ion storage layer on the second electrode transparency conducting layer or the material of electrochromism layer may be selected to be nickel oxide, iridium oxide and Prussian blue etc., but not as limit.
Folded dielectric substrate is one to contain the material of lithium ion between two electrodes, and the source of lithium ion can for example be LiClO
4, LiSbF
6, LiAsF
6, Li (CF
3COO), Li
2C
2O
4, LiI, LiPF
6, LiBF
4, LiCF
3SO
3And LiTFSI (lithium trifluoromethanesulfonimide) etc., but be not as limit.Electrolyte solvent can be selected from propylene carbonate, NSC 11801, diethyl carbonate, methylcarbonate, carbonic acid methylethyl ester, γ-Ding Suan lactone, acetonitrile, tetrahydrofuran (THF), triethylene glycol dme, tetraethyleneglycol dimethyl ether, Triethyleneglycol di n heptanoate, Triethyleneglycol di 2 ethylhexanoate, the perhaps mixture of these compounds.In addition, can add high molecular polymer and form colloidal state or solid state electrolyte, for example be PMMA, PEO, PVB etc., but not as limit.
Adopt the present invention, have the characteristic that good reversible lithium ion embeds/moves out after the suitable thermal treatment of nickel oxide film process that utilizes the long-pending method in negative electrode Shen to electroplate, represent a wider optics electrochromism scope simultaneously.When making the electrochromism assembly, compared to using traditional nickel oxide film, use heat treated nickel oxide film of the present invention not need just have good electrochromism characteristic through electrochemical process or additive method activated ni sull, directly can be applied in the heat-tinting electrode in the electrochromism assembly.Therefore, when using heat-tinting electrode in the electrochromism assembly according to nickel oxide film according to the present invention, in the process of making the electrochromism assembly, can reduce fabrication steps, reduce manufacturing cost and increase process rate.
Description of drawings
Fig. 1 is the cyclic voltammetric collection of illustrative plates that shows through 250 ℃ of heat treated nickel oxide membrane electrodes.
Fig. 2 is the cyclic voltammetric collection of illustrative plates that shows without heat treated nickel oxide membrane electrode.
Fig. 3 be show through 250 ℃ of heat treated nickel oxide membrane electrodes painted/penetrate spectrum when discoloring.
Fig. 4 is the cyclic voltammetric collection of illustrative plates that shows through initial first three time of 250 ℃ of heat treated nickel oxide membrane electrodes.
Fig. 5 be show electrochromism assembly (the sub-PVB/ nickel oxide of Tungsten oxide 99.999/diversion) painted/penetrate spectrum when discoloring.
Fig. 6 illustrates one second preferred embodiment according to the present invention, a kind of preparation method's schematic flow sheet of Optical devices.
Element numbers
602 form step
604 heat treatment steps
Embodiment
Below in conjunction with drawings and embodiments the present invention is described in further detail.
Simultaneously, should understand in this area tool and know the knowledgeable usually, under not departing from spirit of the present invention and category, all can various modifications and modification be arranged to the present invention.
The present invention's one first preferred embodiment provides a kind of preparation method of Optical devices, can comprise that one first configuration step, one second configuration step, a mixing step, a set-up procedure, form step, a heat treatment step.
In this first configuration step, be the nickelous nitrate (Ni (NO of configuration 250mL, about 0.01MOL/L-0.1MOL/L
3)
2) solution.Wherein, be good with about 0.2MOL/L again.
In this second configuration step, be the saltpetre (KNO of configuration 250mL, 0.2MOL/L
3) solution.
In mixing step, mix the electroplate liquid system that above-mentioned two solution form 0.1MOL/L nickel nitrate solution and 0.1MOL/L potassium nitrate solution with equal-volume, wherein the mixed nitrate potassium solution is in order to keep the concentration of nitrate ion.
In this set-up procedure, for adding salpeter solution in this electroplating solution, its pH value is adjusted between the 3-4, be good with about 3.5 again.
Forming step in this, for utilizing the negative electrode plating mode, is working electrode with a transparent conducting glass base material, this transparent conducting glass base material is immersed in this electroplate liquid, and be counter electrode with a platinum titanium mesh, be 0.25mA/cm with the current density
2Decide electric current, on this transparent conducting glass base material, utilize this electroplate liquid, electroplated about 30 minutes, to form a transparent nickel hydroxide film at this transparent conducting glass base material, finish a nickel oxide membrane electrode and have this transparent conducting glass base material and this nickel oxide film, wherein this nickel oxide membrane electrode has an optical modulation limit of power.
Before this formation step is carried out, the surface cleaning of this transparent conducting glass base material is clean, use again it is immersed in and carry out anodizing in the acidic solution, take out then with deionized water and clean, with nitrogen the water on this transparent conducting glass base material is dried up again, to carry out follow-up formation step.
Above-mentioned formation step is a kind of electrochemical deposition (electrodeposition) step.Above-mentioned transparent conducting glass base material can be the stannic oxide (ITO that indium mixes; Indium tin oxide) stannic oxide (FTO of glass baseplate or fluorine doping; Fluorine doped tin oxide) glass baseplate.
In this heat treatment step, do not activate this nickel oxide membrane electrode with electrochemical method, and this nickel oxide membrane electrode is placed a baking box, heat-treat with suitable temperature, treatment time is about one to two hour, this moment the nickel oxide film present light brown so that this nickel oxide membrane electrode has the character that good lithium ion embeds/moves out, and this optical modulation limit of power of augmentation.Above-mentioned suitable temperature can be 150 degree Celsius approximately, 450 degree extremely Celsius, is good with 250 degree persons Celsius approximately again wherein.
According to this first preferred embodiment, the present invention is after this thermal treatment of process, and this nickel oxide film has good electrochromism character.
Whether according to this first preferred embodiment, the present invention can more comprise the electrical capacity of measuring this nickel oxide membrane electrode with a method, good to learn the character that this lithium ion embeds/move out.This method is working electrode with this nickel oxide film thin electrodes, is counter electrode with a platinum titanium mesh, is reference electrode with silver/silver chloride (Ag/AgCl), with 1MOL/L lithium perchlorate (LiClO
4) to be dissolved in propylene carbonate be electrolyte solution, this working electrode is carried out cyclic voltammetric scan analysis.Fig. 4 is initial first three the circle cyclic voltammetry scan collection of illustrative plates through heat treated nickel oxide membrane electrode.See also Fig. 4, scan first three the circle cyclic voltammogram that analyzes according to this cyclic voltammetric, the circulation that can find out first three circle cyclic voltammogram significantly has tangible reaction electric weight, can learn that this nickel oxide film has good electrochromism character, so do not need the said reactivation process of prior art (activation).
The device of measuring the electrochemical properties of nickel oxide membrane electrode is working electrode with nickel oxide film thin electrodes, and platinum titanium mesh is counter electrode, and silver/silver chloride (Ag/AgCl) is reference electrode, and electrolyte solution is 1MOL/L lithium perchlorate (LiClO
4) be dissolved in propylene carbonate.Working electrode is carried out cyclic voltammetric scan analysis, Fig. 1 and Fig. 2 show through Overheating Treatment and without the cyclic voltammetric collection of illustrative plates of heat treated nickel oxide membrane electrode.Comparison diagram 1 and Fig. 2 scan the area that enclose in the loop, through 250 ℃ of heat treated nickel oxide film electrodes bigger electrical capacity is arranged obviously, and the electrical capacity of not passing through heat treated membrane electrode is very little, shows the character that has good lithium ion to embed/move out through heat treated plating nickel oxide film electrode.And through when heat treated nickel oxide film electrode embeds at lithium ion/move out, show significant colour-change, when lithium ion embedded film, membrane electrode presented vitreous state; When lithium ion was moved out film, membrane electrode presented dun.Fig. 3 shows the amount of spectrum mapping that embeds at lithium ion/do when moving out through heat treated nickel oxide film.When the nickel oxide film is painted, be 27.8% in the penetration coefficient of wavelength 550nm; And film is under the state of discoloring, and is 78.1% in the penetration coefficient of wavelength 550nm.So, the nickel oxide film/discoloring penetrates rate variance and reaches about 50.3%, and large-scale optical modulation ability is arranged.But its optical modulation ability is not limited to this value, and when film thickness is healed when thick, its optical modulation ability is bigger.
According to this first preferred embodiment, the present invention can more comprise with the nickel oxide membrane electrode as the heat-tinting electrode, as the painted electrode of reduction, prepares an electrochromism assembly with the tungsten oxide film electrode.For example, with sticking the spacer of fixed thickness around the electrode wherein, with 1MOL/L lithium perchlorate-propylene carbonate-polymethylmethacrylate system (LiClO
4+ PC+PMMA) colloidal electrolyte is coated on this electrode, and another electrode and aforesaid electrode pair are fitted, and the unnecessary ionogen wiped clean of extruding, gets up with epoxy resin (epoxy) involution all around, can finish electrochromism device of the present invention.
Above-mentioned electrochromism assembly preparation process can be carried out with a polyvinyl butyral acetal solid state electrolyte film making step, an applying step and a pressing step in addition.Above-mentioned electrochromism assembly preparation process can comprise having that to lead ionic polyvinyl butyral acetal be a solid state electrolyte.
In this polyvinyl butyral acetal (PVB) solid state electrolyte film making step, the polyvinyl butyral acetal solid film is immersed in the 1MOL/L lithium perchlorate (LiClO of low temperature
4)/γ-Ding Suan lactone electrolytic solution, or with the mixing and hot pressing or extrude with suitable proportion of polyvinyl butyral powder end, lithium salts and plasticizer, lead ionic polyvinyl butyral acetal solid state electrolyte film to be made into to contain.
In this applying step, this polyvinyl butyral acetal solid state electrolyte is film adhered between this nickel oxide membrane electrode and a tungsten oxide film electrode, and envrionment temperature is about 23 ℃, and relative humidity is about 50%.
In this pressing step, according to the glyglass pressing process of standard, pressing should the applying thing, to finish this electrochromism assembly.Wherein, this electrochromism assembly in oxidation (+1.5V)-reduction (applying under voltage 2.0V), painted with discolor therebetween, between about 12%-62%, as shown in Figure 5, this assembly has good operational stability in the penetration coefficient of wavelength 550nm.
Fig. 6 illustrates one second preferred embodiment according to the present invention, a kind of preparation method's schematic flow sheet of Optical devices.See also Fig. 6, this method can comprise that one forms step 602 and a heat treatment step 604.
Form step 602 in this, at the enterprising electroplating of a conductive base, to form a nickel oxide film, finish a nickel oxide membrane electrode and comprise this nickel oxide film and this conductive base.This conductive base can be metal or the non-conductive base material that is coated with conductive membrane.
In this heat treatment step 604, this nickel oxide membrane electrode of thermal treatment is so that this nickel oxide membrane electrode has the character that good lithium ion embeds/moves out.This heat treated temperature is good with 250 degree Celsius approximately again wherein approximately between 150 degree Celsius, 450 degree extremely Celsius.This heat treated step 604 can place a baking box to carry out this nickel oxide membrane electrode, and the time is about 1 hour.This nickel oxide membrane electrode has an optical modulation limit of power.Wherein, this heat treatment step 604 is able to this optical modulation limit of power of augmentation.This nickel oxide film have more one/discoloring penetrates rate variance and can reach about 50.3%.Heal when thick when film thickness, the painted volume increase of film can promote film and color depth, makes the optics penetration of film electrochromism change and becomes greatly.So film thickness of the present invention is healed when thick, it/discolors and penetrates rate variance and can further increase.
Above-mentioned formation step 602, preferable way is carried out for utilizing the negative electrode plating mode, and is able to decide electric current or decides modes such as voltage and carry out.The current density of deciding electric current can be about 0.25mA/cm
2In addition, this forms step 602, can utilize an electroplate liquid to carry out.Wherein, this electroplate liquid is nickelous nitrate, moisture nickelous nitrate, nickelous chloride, moisture nickelous chloride, crosses the compound of chloric acid nickel or other nickel, is dissolved in formed solution in the liquid.As for the pH value of electroplate liquid, between about 3-4, be good with about 3.5 again preferably.
According to this second preferred embodiment, above-mentioned nickel oxide membrane electrode does not need to utilize electrolytic solution or other electrochemical methods to activate, thereby does not need cleaning step to wash this electrolytic solution off yet.The present invention can more comprise with the nickel oxide membrane electrode as the heat-tinting electrode, as the painted electrode of reduction, prepares an electrochromism assembly with the tungsten oxide film electrode.
According to the present invention, have the characteristic that good reversible lithium ion embeds/moves out after the suitable thermal treatment of nickel oxide film process that utilizes the long-pending method in negative electrode Shen to electroplate, represent a wider optics electrochromism scope simultaneously.When making the electrochromism assembly, compared to using traditional nickel oxide film, use heat treated nickel oxide film of the present invention not need just have good electrochromism characteristic through electrochemical process or additive method activated ni sull, directly can be applied in the heat-tinting electrode in the electrochromism assembly.Therefore, when using heat-tinting electrode in the electrochromism assembly according to nickel oxide film according to the present invention, in the process of making the electrochromism assembly, can reduce fabrication steps, reduce manufacturing cost and increase process rate.
The above; only be the specific embodiment of the present invention, but protection scope of the present invention is not limited thereto, any those of ordinary skill in the art are in the disclosed technical scope of the present invention; the variation that can expect easily or replacement all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain that claims were limited.
Claims (9)
1. the preparation method of Optical devices, it is characterized in that: described method comprises:
Configuration 0.01-1mol/L nickel nitrate solution;
Form electroplate liquid;
Add salpeter solution in this electroplating solution, its pH value is adjusted between the 3-4;
Utilize the negative electrode plating mode to form a nickel oxide film at an electrically conducting transparent base material;
Finish a nickel oxide membrane electrode, wherein this nickel oxide membrane electrode has this electrically conducting transparent base material and this nickel oxide film, and wherein this nickel oxide membrane electrode has an optical modulation limit of power; And
Do not activate this nickel oxide membrane electrode with electrochemical method, and heat-treat for 200 ℃-300 ℃ with temperature, so that this nickel oxide membrane electrode has the character that good lithium ion embeds/moves out, and this optical modulation limit of power of augmentation.
2. the preparation method of Optical devices according to claim 1 is characterized in that: in order to keep the concentration of nitrate ion in the electroplate liquid, add saltpetre, SODIUMNITRATE or the lithium nitrate solution of 0.1-1mol/L in electroplate liquid.
3. the preparation method of Optical devices according to claim 1 is characterized in that: also comprise the electrical capacity of measuring this nickel oxide membrane electrode with following method, whether good to learn the character that this lithium ion embeds/move out:
Being working electrode with this nickel oxide membrane electrode, is counter electrode with a platinum titanium mesh, is reference electrode with silver/silver chloride, is lithium perchlorate LiClO with 1mol/L
4Being dissolved in propylene carbonate is electrolyte solution, and this working electrode is carried out the cyclic voltammetry scan analysis.
4. the preparation method of Optical devices according to claim 1 is characterized in that: wherein through after this thermal treatment, this nickel oxide film has electrochromism character.
5. the preparation method of Optical devices, it is characterized in that: described method comprises:
At the enterprising electroplating of a conductive base, to form a nickel oxide film;
Finish a nickel oxide membrane electrode, wherein this nickel oxide membrane electrode has this nickel oxide film and this conductive base; And
This nickel oxide membrane electrode of thermal treatment, so that this nickel oxide membrane electrode has the character that good lithium ion embeds/moves out, wherein this heat treated temperature is between 150 degree Celsius, 450 degree extremely Celsius.
6. the preparation method of Optical devices according to claim 5 is characterized in that: this heat treated temperature is 250 degree Celsius.
7. the preparation method of Optical devices according to claim 5, it is characterized in that: this heat treatment period is 30 minutes-2 hours.
8. the preparation method of Optical devices according to claim 5, it is characterized in that: this nickel oxide membrane electrode does not need to utilize electrolytic solution to activate.
9. the preparation method of Optical devices according to claim 8, it is characterized in that: also comprise with this nickel oxide membrane electrode as a heat-tinting electrode, and with the tungsten oxide film electrode as one the reduction painted electrode, and to have to lead ionic polyvinyl butyral acetal be a solid state electrolyte, prepare an electrochromism assembly.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010127932 CN102191526B (en) | 2010-03-19 | 2010-03-19 | Preparation method of optical device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010127932 CN102191526B (en) | 2010-03-19 | 2010-03-19 | Preparation method of optical device |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102191526A CN102191526A (en) | 2011-09-21 |
| CN102191526B true CN102191526B (en) | 2013-07-10 |
Family
ID=44600365
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201010127932 Expired - Fee Related CN102191526B (en) | 2010-03-19 | 2010-03-19 | Preparation method of optical device |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102191526B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108986955A (en) * | 2018-06-22 | 2018-12-11 | 无锡众创未来科技应用有限公司 | Transparent conductive film and its manufacturing method |
| CN110987822B (en) * | 2019-11-19 | 2022-07-05 | 广西大学 | Method for detecting volatile organic compound |
| CN113740800A (en) * | 2020-05-28 | 2021-12-03 | 南宁富桂精密工业有限公司 | Driving positioning system and driving positioning method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TW200801759A (en) * | 2006-06-30 | 2008-01-01 | Nat Univ Tsing Hua | Electrochromic structure and manufacture method thereof |
| CN101188886A (en) * | 2007-12-14 | 2008-05-28 | 北京航空航天大学 | An inorganic full-solid electric driven color-changing part and its making method |
| CN101377599A (en) * | 2007-08-28 | 2009-03-04 | 逢甲大学 | Electrochromism reflecting device |
-
2010
- 2010-03-19 CN CN 201010127932 patent/CN102191526B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TW200801759A (en) * | 2006-06-30 | 2008-01-01 | Nat Univ Tsing Hua | Electrochromic structure and manufacture method thereof |
| CN101377599A (en) * | 2007-08-28 | 2009-03-04 | 逢甲大学 | Electrochromism reflecting device |
| CN101188886A (en) * | 2007-12-14 | 2008-05-28 | 北京航空航天大学 | An inorganic full-solid electric driven color-changing part and its making method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102191526A (en) | 2011-09-21 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| ES2733281T3 (en) | Multilayer electrochromatic device with lithium oxide nickel based anode | |
| US10545387B2 (en) | Electrochromic device for applying voltage to electrodes | |
| KR101731301B1 (en) | Microporous polymer membrane for electrochromic device and smart window including the same | |
| CN103135306A (en) | Electrochromism assembly provided with composite electrochromism materials | |
| Avellaneda et al. | Solid-state electrochromic devices with Nb2O5: Mo thin film and gelatin-based electrolyte | |
| WO2007081121A1 (en) | Electrode comprising lithium nickel oxide layer, method for preparing the same, and electrochromic device comprising the same | |
| CN104216192A (en) | Preparation method of novel fast-response high-contrast electrochromic device | |
| CN112764285A (en) | Electrochromic device based on polyvinyl alcohol-polyacrylic acid hydrogel electrolyte and preparation method and application thereof | |
| KR20120064315A (en) | Electrochromic device and method of manufacturing the same | |
| CN102191526B (en) | Preparation method of optical device | |
| Liu et al. | Preparation of WO3 gel electrochromic device by simple two-step method | |
| Xie et al. | Proton and redox couple synergized strategy for aqueous low voltage-driven WO3 electrochromic devices | |
| CN108089388B (en) | Method for selectively controlling working voltage of electric dimming device | |
| Macedo et al. | Sol-gel electrochromic device: Code: F8 | |
| CN103688216A (en) | Infrared-modulating electroactive devices with visible region transparency | |
| Sorar et al. | Durability and rejuvenation of electrochromic tungsten oxide thin films in LiClO4–propylene carbonate viscous electrolyte: Effect of Ti doping of the film and polyethylene oxide addition to the electrolyte | |
| US12117708B2 (en) | Thermo-responsive dual band electrochromic device | |
| KR102429821B1 (en) | High-performance and reliable electrochromic device and method for preparing the same | |
| TWI450009B (en) | Electrochromic device and method of manufacturing the same | |
| CN112666770B (en) | Electrochromic flexible device based on P (SPMA-MMA) hydrogel electrolyte and preparation method and application thereof | |
| Collomb-Dunand-Sauthier et al. | Spectroelectrochemical behaviour of poly (3-octylthiophene): application to electrochromic windows with polyaniline and iridium oxide | |
| CN103135305A (en) | Electrochromism device provided with porous structure and manufacture procedure method thereof | |
| CN208872988U (en) | Electrochromic device component and electrochromic device | |
| Bhoumik et al. | Electrolyte design for zinc dynamic windows with fast switching that cycle more than 11,000 times with high optical contrast | |
| Cui et al. | All‐solid‐state complementary electrochromic windows based on the oxymethylene‐linked polyoxyethylene complexed with LiClO4 |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20130710 Termination date: 20150319 |
|
| EXPY | Termination of patent right or utility model |