CN109574515A - A kind of electrochromism windshield and preparation method thereof - Google Patents
A kind of electrochromism windshield and preparation method thereof Download PDFInfo
- Publication number
- CN109574515A CN109574515A CN201811529766.3A CN201811529766A CN109574515A CN 109574515 A CN109574515 A CN 109574515A CN 201811529766 A CN201811529766 A CN 201811529766A CN 109574515 A CN109574515 A CN 109574515A
- Authority
- CN
- China
- Prior art keywords
- preparation
- electrochromism
- glass substrate
- windshield
- inkjet printing
- 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.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/3411—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials
- C03C17/3417—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials all coatings being oxide coatings
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
- B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B33/00—Layered products characterised by particular properties or particular surface features, e.g. particular surface coatings; Layered products designed for particular purposes not covered by another single class
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/12—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by using adhesives
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/21—Oxides
- C03C2217/217—FeOx, CoOx, NiOx
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/21—Oxides
- C03C2217/219—CrOx, MoOx, WOx
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/21—Oxides
- C03C2217/24—Doped oxides
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/21—Oxides
- C03C2217/24—Doped oxides
- C03C2217/241—Doped oxides with halides
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/11—Deposition methods from solutions or suspensions
- C03C2218/119—Deposition methods from solutions or suspensions by printing
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/30—Aspects of methods for coating glass not covered above
- C03C2218/32—After-treatment
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Electrochromic Elements, Electrophoresis, Or Variable Reflection Or Absorption Elements (AREA)
Abstract
The present invention relates to a kind of electrochromism windshields and preparation method thereof.The windshield is successively made of glass substrate, transparent patterned cathode, electrochromic layer, polymer Li-ion electrolyte layer, ion storage layer, transparent public anode and glass substrate.The preparation method comprises the following steps: (1) being sequentially prepared transparent patterned cathode, electrochromic layer using inkjet printing methods on the 1st glass substrate；(2) transparent public anode, ion storage layer are sequentially prepared using inkjet printing methods in the 2nd glass substrate；(3) by two pieces of glass substrates polymer Li-ion electrolyte layer pipe sensitive adhesion.The present invention has the advantages that preparation method of the present invention is by electrochromism technical application on shield glass, using patterned electrode, windshield compartmentalization discoloration is realized, while using the electrode spacing lower than resolution of eye, visual effect, transmission performance are more preferably.
Description
Technical field
The invention belongs to electrochromism technical fields, and in particular to a kind of electrochromism windshield and its preparation side
Method.
Background technique
Electrochromism phenomenon (Electrochromics, EC) refers to material color, transmissivity, reflection under electric field action
Inverible transform occurs for rate.It is prepared into difference on a special substrate by can either physically or chemically coat electrochromic material
The electrochromic device of application.The electrochromic device of Successful commercial application has electrochromic intelligent window, electricity at present
Mutagens color automobile rearview mirror etc..
Currently, application of the electrochromism technology on automobile is the hot spot direction that the technical market is promoted.In hot summer,
To avoid light dazzling, driver generally requires to wear sunglasses or puts down barn door, though the shading facility of these auxiliary can be with
It effectively avoids dazzling the eyes problem, but experience decline of driving, and be easy to cause driving during wearing sunglasses or putting down barn door
Member is absent minded, increases driving risk.
Conventional electrochromism windshield be it is a kind of by transparency conducting layer, cathodic electrochromic layer, transparent electrolyte layer,
The laminated glass of anode electrochromic layer composition, usual this glass can actively or automatically be cut in colourless, coloured two states
It changes.However, this conventional electrochromism windshield cannot achieve the progressive discoloration in part on demand, it can not still meet very well and drive
It sails requirement, promote driving experience.
Summary of the invention
In place of the above shortcoming and defect of the existing technology, primary and foremost purpose of the present invention there is provided one kind can be actively
Adjust the electrochromism windshield of color change interval and discoloration.
Another object of the present invention is to provide the preparation method of above-mentioned electrochromism windshield.
The invention is realized by the following technical scheme:
A kind of preparation method of electrochromism windshield, including following preparation step:
(1) method of inkjet printing is used to prepare a layer thickness as the patterned of 100nm~200nm on the glass substrate
Transparent conductive film, the then annealed solidification of film, as cathode, the glass substrate is known as the first glass substrate；
(2) inkjet printing prepares the WO that a layer thickness is 200nm~300nm on cathode3Electrochromic layer, then film
Solidify by annealing；
(3) method of inkjet printing is used to prepare a layer thickness as the patterned of 100nm~200nm on the glass substrate
Transparent conductive film, the then annealed solidification of film, as public anode, the glass substrate is known as the second glass substrate；
(4) inkjet printing prepares the NiO electrochromic layer that a layer thickness is 200nm~300nm on public anode, then
Film mainly plays ion storage by annealing solidification, NiO；
(5) the first glass substrate and the second glass substrate are pressed by cementing medium of polymer lithium salt electrolyte, obtained
The electrochromism windshield.
Preferably, step (1) and step (3) transparent conductive film are fluorine-doped tin oxide film (SnO2: F) or mix tungsten
SnO 2 thin film (SnO2:W)。
Preferably, the fluorine-doped tin oxide film (SnO2: F) preparation process are as follows: by NH4F and SnCl2Example in molar ratio
It is dissolved in organic solvent for 0.1:5~2:5 and mixed solution is made, SnCl2Concentration in mixed solution be 0.3mol/L~
0.6mol/L, by the mixed solution 40 DEG C~70 DEG C stirring in water bath agings for 24 hours, obtain precursor liquid, then sprayed again
Ink printing, it is furthermore preferred that the organic solvent is ethyl alcohol.
Preferably, the tungsten-doped tin oxide film (SnO2: W) preparation process are as follows: by WCl6And SnCl2Example in molar ratio
It is dissolved in organic solvent for 0.5:100~2:100 and mixed solution is made, SnCl2Concentration in mixed solution is 0.3mol/L
~0.6mol/L, by the mixed solution 40 DEG C~70 DEG C stirring in water bath agings for 24 hours, obtain precursor liquid, then carry out again
Inkjet printing, it is furthermore preferred that the organic solvent is ethyl alcohol.
Preferably, step (1) and step (3) described glass substrate with a thickness of 2mm~3mm, the glass substrate is silicon
Or quartz glass.
Preferably, the technological parameter of step (1) and step (3) described inkjet printing are as follows: 30 DEG C~50 DEG C of substrate temperature, spray
Head temperature is 25 DEG C~35 DEG C.
Preferably, step (1) and step (3) are described is annealed into first in 120 DEG C~150 DEG C preannealing 10min~15min,
Later again in 400 DEG C~550 DEG C annealing 1h~1.5h.
Preferably, the figure of step (1) the patterned transparent conductive film be horizontal stripe, width of fringe be 1~
2mm, the interval of striped is less than 73 μm；Each stripe electrode can individually be gated by data-interface, not electric with other stripeds
Extremely it is connected, striped number is 130~160.
To avoid fringe spacing from influencing traffic safety, fringe spacing must satisfy the requirement of resolution of eye.Human eye is minimum
Resolution angle is 1 ', and minimum resolution distance is 73 μm under the corresponding human eye distance of distinct vision (25cm), therefore the interval of striped needs
73 μm hereinafter, be continuous in transparency conducting layer visual effect entire in this way.
Preferably, step (3) the patterned transparent conductive film figure is continuous whole, without fringe spacing.
Preferably, step (2) WO3The preparation process of electrochromic layer are as follows: by wolframic acid or WCl6It is dissolved in organic solvent
Tungstic acid or WCl is made6Solution, tungstic acid or WCl6The concentration of solution is 0.8~1.2mol/L, by tungstic acid or
WCl6Precursor solution is prepared after 40 DEG C~80 DEG C stirred in water bath 3h in solution, then carries out inkjet printing again, more excellent
Choosing, the organic solvent is that ethyl alcohol and ethylene glycol are made by the volume ratio blending of 10:1.
Preferably, the technological parameter of step (2) described inkjet printing are as follows: 40 DEG C of substrate temperature, 30 DEG C of nozzle temperature.
Preferably, the temperature of step (2) described annealing is 200 DEG C~300 DEG C, and the time of annealing is 0.5h~1.5h.
Preferably, the preparation process of step (4) the NiO electrochromic layer are as follows: nickel acetate is dissolved in organic solvent and is made
Nickel acetate solution is obtained, the concentration of nickel acetate solution is 1.0mol/L, and stirring is made precursor solution afterwards for 24 hours, is then sprayed again
Ink printing, it is furthermore preferred that the organic solvent is that glycol monoethyl ether and ethylene glycol are made by the volume ratio blending of 10:1.
Preferably, the technological parameter of step (4) described inkjet printing are as follows: 40 DEG C of substrate temperature, 30 DEG C of nozzle temperature
Preferably, the temperature of step (4) described annealing is 300 DEG C~350 DEG C, and the time of annealing is 0.5h~1.5h.
Preferably, step (5) the polymer lithium salt electrolyte is PMMA lithium salts electrolyte, PVB lithium salts electrolyte and PEO
One of lithium salts electrolyte.
The electrochromism windshield that the preparation method of above-mentioned electrochromism windshield is prepared.
The principle of the present invention are as follows:
(1) Li under electric field driven, in electrolyte+WO is migrated into when the electron synchrotron provided with conductive layer3Electrochromism
Layer generates blue LixWO3, NiO is due to Li+Deintercalation and gray, at this time the effect of windshield entirety be dusty blue, effectively
Shielded from sunlight.After adding reversed electric field, Li+In WO3Enter NiO film through electrolyte transport after deintercalation, windshield overall effect is
Colourless, the depth of windshield discoloration depends on the voltage swing applied and conduction time.
(2) region for needing to change colour is selected by control gating patterned transparent conductive layer, by controlling in gating
The voltage value applied on transparency conducting layer changes the depth of discoloration.
Compared with prior art, the invention has the following advantages and beneficial effects:
(1) windshield production technology of the present invention can be compatible with conventional windshield production technology, is not necessarily to from root
Originally the production technology of windshield is sexually revised；
(2) it can actively regulate the color change interval of windshield, can guarantee that windshield is kept immediately ahead of vision in this way
High light transmission；
(3) discoloration of windshield can be independently adjusted according to actual environment, regulation button is mountable to conveniently touch
Position, significant increase drives experience and comfort level；
(4) color change interval for differentiating spacing lower than human eye minimum is had chosen, ensure that the continuous of windshield color changeable effect
Property and uniformity, reduce visual fatigue.
Detailed description of the invention
Fig. 1 is the first glass substrate electrode pattern schematic diagram of embodiment 1.
Fig. 2 is the second glass electrode arrangement schematic diagram of embodiment 1.
Fig. 3 is the patterned electrodes technical parameter schematic diagram of the first glass substrate of embodiment 1.
Fig. 4 is the overall structure diagram of electrochromism windshield made from embodiment 1, and wherein a is the first glass
Glass substrate, b are patterned cathode, c WO3Electrochromic layer, d are polyelectrolyte floor, e is NiO electrochromism, f is public
Common-anode, g are the second glass substrate.
Fig. 5 is electrochromism windshield transmittance graph under different power-on voltages made from embodiment 1.
Fig. 6 is electrochromism windshield transmittance graph under different power-on voltages made from embodiment 2.
Specific embodiment
Present invention will now be described in further detail with reference to the embodiments and the accompanying drawings, but embodiments of the present invention are unlimited
In this.
Embodiment 1
(1) it uses the method for inkjet printing to prepare a layer thickness using silica glass as substrate to mix for the patterned of 120nm
Fluorine tin oxide transparent conductive film is as cathode.The glass substrate is the first glass substrate, and the fluorine-doped tin oxide is transparent to be led
The specific preparation step of conductive film are as follows: by stannous chloride powder (production of Aladdin company) and NH4F (production of Mike woods company) with
The molar ratio of 5:1 is dissolved in alcohol solvent, SnCl2Concentration be 0.5mol/L, after being stirred for 24 hours under 60 DEG C of heating water baths
Precursor solution is prepared.It is printed using ink-jet printer Dimatix2800, sets electrode pattern parameter (horizontal stripe
Electrode, single stripe electrode width 2mm are divided into 50 μm between adjacent stripes, stripe electrode number 146), 40 DEG C of substrate temperature, spray
30 DEG C of temperature of head.130 DEG C of preannealing 10min after the completion of graphical printing, then 500 DEG C of annealing 1h, are prepared cathode.
(2) step anneal preparation on cured patterned cathode with a thickness of 200nm WO3Electrochromic layer, it is specific to walk
Suddenly are as follows: use WCl6(production of Mike woods company) is dissolved in organic solvent, and organic solvent ethyl alcohol and ethylene glycol are blended and prepare,
Ratio is 10:1, the WCl of preparation6Solution concentration is 0.8mol/L, before solution is prepared after 60 DEG C of heating water baths stir 3h
Liquid solution is driven, using ink-jet printer (Dimatix2800), 40 DEG C of substrate temperature, 30 DEG C of nozzle temperature, electrochromic layer is printed
After the completion in 300 DEG C of annealing 1.5h.
(3) method of inkjet printing is used to prepare a layer thickness as the patterned transparent of 120nm on silica glass substrate
Conductive film is as public anode, and the glass substrate is known as the second glass substrate, and the transparent conductive film preparation step is such as
Under: by stannous chloride powder (production of Aladdin company) and NH4F (production of Mike woods company) is dissolved in ethyl alcohol with the ratio of 5:1
In solvent, SnCl2Concentration be 0.5mol/L, stirred under 60 DEG C of heating water baths and precursor solution be prepared afterwards for 24 hours.Using
Ink-jet printer Dimatix2800 printing, is arranged 40 DEG C of substrate temperature, 30 DEG C of nozzle temperature.130 DEG C after the completion of graphical printing
Preannealing 10min, then 500 DEG C of annealing 1h, are prepared public anode.
(4) NiO for using the method for inkjet printing to prepare a layer thickness as 200nm on the public anode after annealing solidifies
Electrochromic layer, specific steps are as follows: be dissolved in organic solvent, organic solvent second using nickel acetate (production of Mike woods company)
Glycol monomethyl ether and ethylene glycol, which are blended, to be prepared, ratio 10:1, and the nickel acetate solution concentration of preparation is 1.0mol/L, solution stirring
Precursor solution is prepared afterwards for 24 hours, is printed using ink-jet printer Dimatix2800,40 DEG C of substrate temperature, nozzle temperature 30
℃.In 300 DEG C of annealing 1.5h after the completion of printing, nickel oxide layer is prepared.
(5) taking mass parts ratio is PVB: lithium perchlorate: propene carbonate=10:2:1 mixing and doping polymer electrolytic
Matter brushes the polymer dielectric on the first and second glass substrates after 150 DEG C of heating and meltings, vacuum condition (1 ×
10-1Pa pressing removes bubble, pressure 2MPa under), and the pressing duration is 6h, accesses automotive control circuit system after the completion of pressing
System.
Electrochromism windshield made from 1 step of embodiment (5) is accessed into automotive control circuit system, different electricity
Pressure value keeps the discoloration depth of photochromic layer different, and transmissivity is as shown in Figure 5 with voltage relationship is applied.Cathode is set to connect power cathode, it is public
Common-anode connects positive pole, the different striped cathodes of gating under driving circuit control, access different voltages value, conduction time 60s,
Then graduated colors can be realized with windshield.When cathode connects positive pole, public anode connects power cathode, and voltage value 5V leads to
The electric time is 60s, and windshield returns to colour fading state.
Embodiment 2
(1) it uses the method for inkjet printing to prepare a layer thickness using silica glass as substrate to mix for the patterned of 120nm
Tungsten tin oxide transparent conductive film is as cathode.The glass substrate is the first glass substrate, and the tungsten-doped tin oxide transparent is led
The specific preparation step of conductive film are as follows: by stannous chloride powder (production of Aladdin company) and WCl6(production of Mike woods company) with
The molar ratio of 100:1 is dissolved in alcohol solvent, SnCl2Concentration be 0.5mol/L, stirred for 24 hours under 60 DEG C of heating water baths
After precursor solution is prepared.It is printed using ink-jet printer Dimatix2800, sets electrode pattern parameter (horizontal bar
Line electrode, single stripe electrode width 2mm are divided into 50 μm between adjacent stripes, stripe electrode number 146), 40 DEG C of substrate temperature,
30 DEG C of nozzle temperature.130 DEG C of preannealing 10min after the completion of graphical printing, then 500 DEG C of annealing 1h, are prepared cathode.
(2) step anneal preparation on cured patterned cathode with a thickness of 200nm WO3Electrochromic layer, it is specific to walk
Suddenly are as follows: after tungsten powder (production of Mike woods company) and hydrogen peroxide (W and hydrogen peroxide molar ratio 1:11) reaction dissolution,
120 DEG C are concentrated by evaporation 3 hours, then titrate to obtain the tungstic acid of 2mol/L；Using the tungstic acid of above-mentioned preparation and organic molten
The isometric ratio mixing of agent, organic solvent are that ethyl alcohol and ethylene glycol are blended and prepare, ratio 10:1, the alcoholic solution of the wolframic acid of preparation
Concentration is 1mol/L, and precursor solution is prepared after 75 DEG C of stirring in water bath 5h in solution.Using ink-jet printer
(Dimatix2800), 40 DEG C of substrate temperature, 30 DEG C of nozzle temperature.In 300 DEG C of annealing 1.5h after the completion of electrochromic layer printing.
(3) method of inkjet printing is used to prepare a layer thickness as the patterned transparent of 120nm on silica glass substrate
Conductive film is as public anode, and the glass substrate is known as the second glass substrate, and the transparent conductive film preparation step is such as
Under: by stannous chloride powder (production of Aladdin company) and NH4F (production of Mike woods company) is dissolved in ethyl alcohol with the ratio of 5:1
In solvent, SnCl2Concentration be 0.5mol/L, stirred under 60 DEG C of heating water baths and precursor solution be prepared afterwards for 24 hours.Using
Ink-jet printer Dimatix2800 printing, is arranged 40 DEG C of substrate temperature, 30 DEG C of nozzle temperature.130 DEG C after the completion of graphical printing
Preannealing 10min, then 500 DEG C of annealing 1h, are prepared public anode.
(4) method of inkjet printing is used to prepare a layer thickness as 200nm on the transparent conductive film after annealing solidifies
NiO electrochromic layer, specific steps are as follows: be dissolved in organic solvent, You Jirong using nickel acetate (production of Mike woods company)
Agent spent glycol monomethyl ether and ethylene glycol, which are blended, to be prepared, and ratio 10:1, the nickel acetate solution concentration of preparation is 1.0mol/L, molten
Precursor solution is prepared in liquid stirring afterwards for 24 hours, is printed using ink-jet printer Dimatix2800,40 DEG C of substrate temperature, spray head
30 DEG C of temperature.In 300 DEG C of annealing 1.5h after the completion of printing, nickel oxide layer is prepared.
(5) taking mass parts ratio is PVB: lithium perchlorate: propene carbonate=10:2:1 mixing and doping polymer electrolytic
Matter brushes the polymer dielectric on the first and second glass substrates after 150 DEG C of heating and meltings, vacuum condition (1 ×
10-1Pa pressing removes bubble, pressure 2MPa under), and the pressing duration is 6h, accesses automotive control circuit system after the completion of pressing
System.
Electrochromism windshield made from 2 step of embodiment (5) is accessed into automotive control circuit system, different electricity
Pressure value keeps the discoloration depth of photochromic layer different, and transmissivity is as shown in Figure 6 with voltage relationship is applied.Cathode is set to connect power cathode, it is public
Common-anode connects positive pole, the different striped cathodes of gating under driving circuit control, access different voltages value, conduction time 60s,
Then graduated colors can be realized with windshield.When cathode connects positive pole, public anode connects power cathode, and voltage value 5V leads to
The electric time is 60s, and windshield returns to colour fading state.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. a kind of preparation method of electrochromism windshield, which is characterized in that including following preparation step:
(1) method of inkjet printing is used to prepare a layer thickness as the patterned transparent of 100nm~200nm on the glass substrate
Conductive film, the then annealed solidification of film, as cathode, the glass substrate is known as the first glass substrate；
(2) inkjet printing prepares the WO that a layer thickness is 200nm~300nm on cathode3Electrochromic layer, then film passes through
Annealing solidification；
(3) method of inkjet printing is used to prepare a layer thickness as the patterned transparent of 100nm~200nm on the glass substrate
Conductive film, the then annealed solidification of film, as public anode, the glass substrate is known as the second glass substrate；
(4) inkjet printing prepares the NiO electrochromic layer that a layer thickness is 200nm~300nm on public anode, then film
Solidify by annealing；
(5) the first glass substrate and the second glass substrate are pressed by cementing medium of polymer lithium salt electrolyte, obtained described
Electrochromism windshield.
2. the preparation method of electrochromism windshield according to claim 1, which is characterized in that step (1) and step
Suddenly (3) described transparent conductive film is fluorine-doped tin oxide film or tungsten-doped tin oxide film.
3. the preparation method of electrochromism windshield according to claim 2, which is characterized in that the fluorine doped oxidation
The preparation process of tin thin film are as follows: by NH4F and SnCl2In molar ratio example be 0.1:5~2:5 be dissolved in organic solvent be made mixing it is molten
Liquid, SnCl2Concentration in mixed solution is 0.3mol/L~0.6mol/L, by the mixed solution in 40 DEG C~70 DEG C water-baths
It stirs aging for 24 hours, obtains precursor liquid, then carry out inkjet printing again；
The preparation process of the tungsten-doped tin oxide film are as follows: by WCl6And SnCl2Example is that 0.5:100~2:100 is dissolved in molar ratio
Mixed solution, SnCl are made in organic solvent2Concentration in mixed solution is 0.3mol/L~0.6mol/L, by the mixing
Solution 40 DEG C~70 DEG C stirring in water bath agings for 24 hours, obtain precursor liquid, then carry out inkjet printing again.
4. the preparation method of electrochromism windshield according to claim 1, which is characterized in that step (2) is described
WO3The preparation process of electrochromic layer are as follows: by wolframic acid or WCl6It is dissolved in organic solvent and tungstic acid or WCl is made6Solution, tungsten
Acid solution or WCl6The concentration of solution is 0.8~1.2mol/L, by tungstic acid or WCl6Solution stirs in 40 DEG C~80 DEG C water-baths
Precursor solution is prepared after mixing 3h, then carries out inkjet printing again.
5. the preparation method of electrochromism windshield according to claim 1, which is characterized in that step (4) is described
The preparation process of NiO electrochromic layer are as follows: by nickel acetate be dissolved in organic solvent be made nickel acetate solution, nickel acetate solution it is dense
Degree is 1.0mol/L, and stirring is made precursor solution afterwards for 24 hours, then carries out inkjet printing again.
6. the preparation method of any one electrochromism windshield according to claim 1~5, which is characterized in that step
Suddenly the technological parameter of (1) and step (3) described inkjet printing are as follows: 30 DEG C~50 DEG C of substrate temperature, nozzle temperature is 25 DEG C~35
℃；It is annealed into described in step (1) and step (3) first in 120 DEG C~150 DEG C preannealing 10min~15min, later again at 400 DEG C
~550 DEG C of annealing 1h~1.5h；Step (1) and step (3) described glass substrate with a thickness of 2mm~3mm, the glass substrate
For silicon or quartz glass.
7. the preparation method of any one electrochromism windshield according to claim 1~5, which is characterized in that step
Suddenly the figure of (1) described patterned transparent conductive film is horizontal stripe, and width of fringe is 1~2mm, and the interval of striped is less than
73 μm, each stripe electrode can individually be gated by data-interface, be not connected with other stripe electrodes, and striped number is
130~160；Step (3) the patterned transparent conductive film figure is continuous entirety, without fringe spacing.
8. the preparation method of any one electrochromism windshield according to claim 1~5, which is characterized in that step
Suddenly the technological parameter of (2) described inkjet printing are as follows: 40 DEG C of substrate temperature, 30 DEG C of nozzle temperature；The temperature of step (2) described annealing
It is 200 DEG C~300 DEG C, the time of annealing is 0.5h~1.5h；The technological parameter of step (4) described inkjet printing are as follows: substrate temperature
40 DEG C, 30 DEG C of nozzle temperature of degree；The temperature of step (4) described annealing is 300 DEG C~350 DEG C, time of annealing be 0.5h~
1.5h。
9. the preparation method of electrochromism windshield according to claim 1, which is characterized in that step (5) is described
Polymer lithium salt electrolyte is one of PMMA lithium salts electrolyte, PVB lithium salts electrolyte and PEO lithium salts electrolyte.
10. the electrochromism that the preparation method of any one of the claim 1~9 electrochromism windshield is prepared
Windshield.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811529766.3A CN109574515B (en) | 2018-12-14 | 2018-12-14 | Electrochromic automobile windshield and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811529766.3A CN109574515B (en) | 2018-12-14 | 2018-12-14 | Electrochromic automobile windshield and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109574515A true CN109574515A (en) | 2019-04-05 |
| CN109574515B CN109574515B (en) | 2020-12-22 |
Family
ID=65929645
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811529766.3A Active CN109574515B (en) | 2018-12-14 | 2018-12-14 | Electrochromic automobile windshield and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109574515B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112289963A (en) * | 2020-10-23 | 2021-01-29 | Tcl华星光电技术有限公司 | OLED display panel and manufacturing method thereof |
| CN112961539A (en) * | 2021-02-07 | 2021-06-15 | 上海大学 | Nano tungsten oxide printing ink suitable for ink-jet printing film forming process, and preparation method and application thereof |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101971086A (en) * | 2007-12-12 | 2011-02-09 | 魁北克水电公司 | Electrochromic optical lens |
| CN103345097A (en) * | 2013-06-17 | 2013-10-09 | 张�林 | EC-type electrochromism laminated glass and intelligent dimming system based on same |
| CN104698715A (en) * | 2013-12-04 | 2015-06-10 | 珠海兴业绿色建筑科技有限公司 | All-solid electrochromic device |
| CN105807450A (en) * | 2014-12-30 | 2016-07-27 | 北京生美鸿业科技有限公司 | Novel transparent conducting electrode and intelligent light dimming film comprising same |
| CN108109723A (en) * | 2017-12-14 | 2018-06-01 | 湖南兴威新材料有限公司 | The method that ITO nesa coating is prepared using inkjet printing |
| CN108519710A (en) * | 2018-06-11 | 2018-09-11 | 赫得纳米科技(昆山)有限公司 | A kind of full-solid electrochromic plate and its manufacturing method |
| CN108983527A (en) * | 2018-08-28 | 2018-12-11 | 上海幂方电子科技有限公司 | A kind of self-powered type electrochromic device and preparation process |
-
2018
- 2018-12-14 CN CN201811529766.3A patent/CN109574515B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101971086A (en) * | 2007-12-12 | 2011-02-09 | 魁北克水电公司 | Electrochromic optical lens |
| CN103345097A (en) * | 2013-06-17 | 2013-10-09 | 张�林 | EC-type electrochromism laminated glass and intelligent dimming system based on same |
| CN104698715A (en) * | 2013-12-04 | 2015-06-10 | 珠海兴业绿色建筑科技有限公司 | All-solid electrochromic device |
| CN105807450A (en) * | 2014-12-30 | 2016-07-27 | 北京生美鸿业科技有限公司 | Novel transparent conducting electrode and intelligent light dimming film comprising same |
| CN108109723A (en) * | 2017-12-14 | 2018-06-01 | 湖南兴威新材料有限公司 | The method that ITO nesa coating is prepared using inkjet printing |
| CN108519710A (en) * | 2018-06-11 | 2018-09-11 | 赫得纳米科技(昆山)有限公司 | A kind of full-solid electrochromic plate and its manufacturing method |
| CN108983527A (en) * | 2018-08-28 | 2018-12-11 | 上海幂方电子科技有限公司 | A kind of self-powered type electrochromic device and preparation process |
Non-Patent Citations (1)
| Title |
|---|
| 张巡天: "全固态WO3薄膜电致变色器件研究进展", 《光电子技术》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112289963A (en) * | 2020-10-23 | 2021-01-29 | Tcl华星光电技术有限公司 | OLED display panel and manufacturing method thereof |
| CN112961539A (en) * | 2021-02-07 | 2021-06-15 | 上海大学 | Nano tungsten oxide printing ink suitable for ink-jet printing film forming process, and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109574515B (en) | 2020-12-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CA2340083C (en) | Reversible electrochemical mirror (rem) with improved electrolytic solution | |
| EP1977284B1 (en) | Electrode comprising lithium nickel oxide layer, method for preparing the same, and electrochromic device comprising the same | |
| JP6323154B2 (en) | ELECTROCHROMIC DISPLAY ELEMENT AND METHOD FOR MANUFACTURING THE SAME, DISPLAY DEVICE, INFORMATION DEVICE, AND ELECTROCHROMIC Dimmer | |
| US11221533B2 (en) | Electrochromic device | |
| KR20030040361A (en) | Fast-switching reversible electrochemical mirror(rem) | |
| KR100629190B1 (en) | A method and device for determining the thickness of a mirror metal deposition on a mirror electrode of a reversible electrochemical mirror device | |
| US6552843B1 (en) | Reversible electrodeposition device with ionic liquid electrolyte | |
| KR20010033196A (en) | Reversible electrochemical mirror | |
| CN109574515A (en) | A kind of electrochromism windshield and preparation method thereof | |
| JP5550094B2 (en) | Electrochromic compound, electrochromic composition, and display element | |
| CN110304836A (en) | Deposit the chemical baths of electrochomeric films | |
| US20010008458A1 (en) | Electrochromic mirror | |
| TW576938B (en) | Electrochromic assembly based on poly(3,4-ethylenedioxythiophene) derivatives in combination with a counterelectrode containing metal oxides from transition group VI or VIII | |
| JP3480002B2 (en) | Electrochromic dimming window | |
| US20190324339A1 (en) | Hybrid electrochromic devices and methods | |
| JP2011227248A (en) | Electrochromic display device and manufacturing method of electrochromic display device | |
| JP6776510B2 (en) | Electrochromic display elements, display devices, information equipment, manufacturing methods for electrochromic display elements, electrochromic dimming lenses | |
| JP2011039282A (en) | Light control element | |
| JP4506171B2 (en) | Electrochemical light control device and method for manufacturing the same | |
| JPS63106732A (en) | Electrochromic element | |
| JP2010243632A (en) | Method of driving display element and display element | |
| JP2017203843A (en) | Electrochromic device and method for manufacturing the same | |
| JP5530692B2 (en) | Electrochromic composition | |
| JP2005189384A (en) | Electrochemical light controlling device and its driving method | |
| TWI578076B (en) | Electrochromic sticker and method of manufacturing thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |