CN106145693A - A kind of porous WO3the preparation method of electrochomeric films - Google Patents
A kind of porous WO3the preparation method of electrochomeric films Download PDFInfo
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- CN106145693A CN106145693A CN201510186245.2A CN201510186245A CN106145693A CN 106145693 A CN106145693 A CN 106145693A CN 201510186245 A CN201510186245 A CN 201510186245A CN 106145693 A CN106145693 A CN 106145693A
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Abstract
The invention provides a kind of porous WO3The preparation method of electrochomeric films, including: after peroxide tungstic acid and the solution containing pore creating material template uniformly being mixed, being spun on substrate, heat treatment at 350-500 DEG C, obtains described porous WO the most again3Electrochomeric films, wherein, pore creating material template includes poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide).This preparation technology is simple, and process equipment is simple, and the Tungstic anhydride. loose structure pattern of composition thin film can conveniently control, and manufacturing cost is relatively low, it is easy to accomplish large-scale production.
Description
Technical field
The invention belongs to WO3Electrochomeric films technology of preparing, is specifically related to use sol-gal process, spin coating technique to prepare
Porous WO3Thin film.
Background technology
The world has come into low-carbon (LC), energy-conserving and environment-protective, new forms of energy, life sciences, intelligent things network technology etc. and has been at present
The leading fourth industrial revolution epoch.The flourishing emergence of these new industries promotes the mankind to enter a Green Sustainable
New stage.The most effectively economize on resources and protect environment to realize the important topic that sustainable development is current sciemtifec and technical sphere.
Along with global warming, day by day exhausted and mankind's excessive influence to environment of earth resource, environmental protection, energy-saving low-carbon material become
For the focus of research, intelligent color-changing thin film is exactly the new function material grown up under these circumstances.Electrochromism refers to thing
Reversible color change is there is in matter under the effect of extra electric field or electric current；In numerous electrochromic materials, oxo transition metal
Compound WO3Obtain the favor of people, and be considered as the electrochromic material having most using value.
WO3The main electrochromic reaction occurred is as follows:
Chinese patent 201310324918.7 discloses one and prepares WO3The method of nano-array.Its main preparation process is such as
Under: wolframic acid is dissolved in aqueous hydrogen peroxide solution, adds water and be configured to the tungstic add peroxide solution that tungstenic concentration is 1～5mol/L；Will
Tungstic add peroxide solution is coated on the conducting surface of the clean conductive substrates of cleaning, obtains being coated with the conductive substrates of crystal seed layer；By tungsten
Salt is dissolved in alcohol, forms precursor solution, and the conductive substrates that will be covered with crystal seed layer is fixed in reactor, by precursor solution
Add in reactor, react 8～16h at 150～250 DEG C, again at 350～450 DEG C of heat treatments 1～3h after taking-up.
Chinese patent (200910059118.0) discloses a kind of lifting technology that uses, and utilization sol-gal process prepares three oxidations
The method of tungsten electrochomeric films.This invention preparation process includes, reacts, react 5-7 hour in tungsten powder and hydrogen peroxide ice-water bath
Rear filtration, adds dehydrated alcohol and glacial acetic acid in filtrate, stirs.Little at 50-60 DEG C of backflow 5-6 by reflux
Time, obtain the WO of homogeneous transparent3Colloidal sol, is immersed in WO by cleaned substrate3In colloidal sol, with 2-3cm/min speed to
Upper lifting substrate, is repeated several times rear natural air drying, and substrate after heat treatment obtains WO3Thin film.
Chinese patent 201310174818.0 discloses a kind of employing magnetron sputtering method and prepares WO3The side of electrochomeric films
Method.It uses radiofrequency magnetron sputtering technology, with WO3Pottery is cathode targets, deposits WO on ITO substrate3Thin film.Main
Process is wanted to include: ito glass substrate is carried out；Target and substrate are installed, and regulate target-substrate distance；It is filled with argon, and
Carry out pre-sputtering；Heating substrate, makes substrate reach temperature required；Sputter by the technological parameter set；Close magnetron sputtering
Equipment also takes out sample.
Although presently disclosed relevant WO3The Chinese patent of method for manufacturing thin film is more, but technique is simple, lower-cost
The WO of preparation porous3The patent of thin film but rarely has disclosure.
Summary of the invention
Present invention seek to address that cannot easy preparation WO3The technical problem of thin film, the invention provides a kind of porous WO3Electricity
Cause the preparation method of optically variable films.
The invention provides a kind of porous WO3The preparation method of electrochomeric films, including:
After peroxide tungstic acid and the solution containing pore creating material template are uniformly mixed, it is spun on substrate, the most again at 350-500
Heat treatment at DEG C, obtains described porous WO3Electrochomeric films, wherein, pore creating material template includes poly(ethylene oxide)-polycyclic oxygen
Propane-poly(ethylene oxide).
It is preferred that the preparation method of peroxide tungstic acid includes:
To H2WO4Middle addition H2O2, dissolve H2WO4And form transparent mixed liquor, then stand 0.5-2 days.
It is preferred that the preparation method of the solution containing pore creating material template includes:
Pore creating material template is dissolved in dehydrated alcohol, and stirs to mixed liquor transparent, thus obtain the solution containing pore creating material template.
It is preferred that poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide) concentration in dehydrated alcohol is 0.2-0.4g/mL.
It is preferred that described substrate includes pretreated ITO electro-conductive glass substrate.
It is preferred that described pretreatment includes immersing substrate successively ultrasonic cleaning in acetone, dehydrated alcohol and deionized water,
The time that per stage cleans is 10-20 minute, is dried afterwards.
It is preferred that the technological parameter of spin coating masking includes: rotating speed 3000-5000rpm, spin coating 1～2 minutes.
It is preferred that be dried 14-20 hour at 40 DEG C-60 DEG C.
It is preferred that at 350 DEG C-500 DEG C heat treatment 3-8 hour.
Beneficial effects of the present invention:
Porous Tungsten Trioxide Electrochromic Films in the present invention, takes sol-gel process for preparing, and this preparation technology is simple, process equipment
Simply, the Tungstic anhydride. loose structure pattern of composition thin film can conveniently control, and manufacturing cost is relatively low, it is easy to accomplish give birth on a large scale
Produce.The porous Tungsten Trioxide Electrochromic Films of preparation has that spectrum range of accommodation is big, coloration efficiency is high, fast response time etc. is excellent
Point, may not only be applied to electrochromism field, it is also possible to for gas-discoloration device, NO2Gas sensing device and photovoltaic etc. are led
Territory, has broad application prospects.
Accompanying drawing explanation
Fig. 1 is electrochromic device operation principle schematic diagram；
Fig. 2 shows in the case of being not added with P123, the WO of spin coating on ito glass substrate3The XRD figure spectrum of thin film；
Fig. 3 shows the WO prepared in the case of not adding P1233Film surface SEM pattern；
Fig. 4 shows the WO prepared in the case of not adding P1233Thin-membrane section SEM pattern；
Fig. 5 shows addition P in embodiment 1123The WO of preparation3Film surface SEM pattern (low multiple)；
Fig. 6 shows addition P in embodiment 1123The WO of preparation3Film surface SEM pattern (high multiple)；
Fig. 7 shows addition P in embodiment 1123The WO of preparation3Thin-membrane section SEM pattern；
Fig. 8 shows addition P in embodiment 1123The WO of preparation3Thin-membrane section SEM pattern；
Fig. 9 shows addition P in embodiment 2123The WO of preparation3Thin-membrane section SEM pattern；
Figure 10 shows WO in embodiment 1310 cyclic voltammetry curves of thin film are (with 1MLiClO4/ PC is electrolyte, and Pt is
To electrode, saturated silver chloride is reference electrode, and scanning speed is 60mv/s)；
Figure 11 shows WO in embodiment 2310 cyclic voltammetry curves of thin film are (with 1MLiClO4/ PC is electrolyte, and Pt is
To electrode, saturated silver chloride is reference electrode, and scanning speed is 60mv/s)；
Figure 12 shows WO in embodiment 13The spectral transmittance curve of thin film；
Figure 13 shows WO in embodiment 23The spectral transmittance curve of thin film；
Figure 14 shows WO in embodiment 13Thin film coloring before and after facing to pictorial diagram, (left side is coloured state, and the right is for fading
State)；
Figure 15 shows WO in embodiment 23Thin film coloring before and after facing to pictorial diagram, (left side is coloured state, and the right is for fading
State).
Detailed description of the invention
The present invention is further illustrated, it should be appreciated that accompanying drawing and following embodiment are only below in conjunction with accompanying drawing and following embodiment
For the present invention is described, and the unrestricted present invention.
WO3Thin film is that a kind of being it is believed that most is expected to practical a kind of inorganic electrochromic material, and it is in smart window, aobvious
Show that the fields such as device, automobile rearview mirror, sensor, Electronic Paper have great application prospect.The invention provides one and prepare many
The method of hole Tungsten Trioxide Electrochromic Films, its thin film prepared has even structure, defect is few, porous density is high and electroluminescent
The advantage that discoloration is good, and preparation cost is low, is easily controlled, reproducible, practical.
Described method specifically includes following steps:
(1) electro-conductive glass substrate (such as ITO electro-conductive glass substrate) is cleaned；
With acetone, dehydrated alcohol, deionized water ultrasonic 10～20 minutes ITO electro-conductive glass substrates respectively, then at 60 DEG C～80 DEG C
Dry glass substrate in baking oven；
(2)WO3The preparation of colloidal sol；
With H2WO4For presoma, add H2O2Dissolve H2WO4, form transparent peroxide tungstic acid, stand 0.5～2 day；
For more specifically, by 6-8g Na2WO4·2H2O joins the dense HNO of 30～50ml 68%3In, at 50 DEG C of heating in water bath
2 hours, it is centrifuged processing under rotating speed is 3000～5000rpm, it is thus achieved that H2WO4Yellow mercury oxide, then by H2WO4Yellow
Color precipitation joins 10～20ml 30%H2O2In, then magnetic agitation 1～3 hours, it is thus achieved that the peroxide wolframic acid of homogeneous transparent, and
With oxygen O2Generation, i.e. form WO3Colloidal sol；
(3) preparation of pore creating material masterplate；
Poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide) P123 is dissolved in dehydrated alcohol, and stirs, is formed transparent homogeneous
Solution；
For more specifically, 1～5g P123 is dissolved in 10ml dehydrated alcohol, and stirs, form transparent homogeneous phase solution；
(4) porous WO3The preparation of thin film；
(2) and (3) are mixed together, form mixed solution, use spin coating masking technique, under rotating speed is 3000～5000rpm
Spin coating 1～2min, obtains the thin film of homogeneous transparent；
(5)WO3Being dried of thin film；
The thin film obtained in (4) is dried 14～20 hours at 40 DEG C～60 DEG C；
(6)WO3The high-temperature heat treatment of thin film；
By the thin film that obtains in (5) heat treatment 3～8 hours at 350 DEG C～500 DEG C.
Ito glass substrate is carried out by step 1, particularly as follows: substrate is immersed successively acetone, dehydrated alcohol and go from
Ultrasonic cleaning in sub-water, the time that per stage cleans is 10-20 minute, and cold wind dries up afterwards.
The preparation of step 3 pore creating material masterplate, particularly as follows: be dissolved in nothing by poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide)
In water-ethanol, form 0.2～0.4g/ml solution.
Compared with prior art, present invention have the advantage that
Porous Tungsten Trioxide Electrochromic Films of the present invention and preparation method thereof, takes sol-gel process for preparing, this preparation technology letter
Single, process equipment is simple, and the Tungstic anhydride. loose structure pattern of composition thin film can conveniently control, and manufacturing cost is relatively low, it is easy to real
Existing large-scale production.There is the advantages such as spectrum range of accommodation is big, coloration efficiency is high, fast response time, may not only be applied to electroluminescent change
Color field, it is also possible to for gas-discoloration device, NO2The field such as gas sensing device and photovoltaic, before having wide application
Scape.
Enumerate embodiment further below to describe the present invention in detail.It will similarly be understood that following example are served only for this
Bright it is further described, it is impossible to being interpreted as limiting the scope of the invention, those skilled in the art is according to the present invention's
Some nonessential improvement and adjustment that foregoing is made belong to protection scope of the present invention.The technique ginseng that following example is concrete
Number etc. is the most only an example in OK range, in the range of i.e. those skilled in the art can be done suitably by explanation herein
Select, and do not really want to be defined in the concrete numerical value of hereafter example.
Comparative example 1
(1) electro-conductive glass substrate is cleaned；
With acetone, dehydrated alcohol, deionized water ultrasonic 20 minutes ITO electro-conductive glass substrates respectively, then dry in the baking oven of 60 DEG C
Dry glass substrate；
(2)WO3The preparation of colloidal sol；
By 6g Na2WO4·2H2O joins the dense HNO of 30ml 68% volume ratio3In, 50 DEG C of heating in water bath 2 hours, turning
Speed is for being centrifuged under 9500rpm processing, it is thus achieved that H2WO4Yellow mercury oxide, then by H2WO4Yellow mercury oxide joins 10ml
30%H2O2In, and magnetic agitation 2 hours, it is thus achieved that the peroxide tungstic acid of homogeneous transparent, and with oxygen O2Generation,
I.e. form WO3Colloidal sol；
(3) fine and close WO3The preparation of thin film；
Colloidal sol prepared by (2), spin coating 2min under rotating speed is 3000rpm, obtain the thin film of homogeneous transparent；
(4)WO3Being dried of thin film；
The thin film obtained in (3) is dried 16 hours at 40 DEG C；
(5)WO3The high-temperature heat treatment of thin film；
Thin film heat treatment 5 hours at 420 DEG C that will obtain in (4).
Experiments verify that, in the membrane-film preparation process of comparative example 1, in the case of being not added with P123, heavy on ito glass
Amass the WO of monocline3Thin film, the XRD figure of thin film is composed as shown in Figure 2.Its surface topography is as it is shown on figure 3, the section of thin film
Pattern is as shown in Figure 4.WO3Film surface is smooth, and thickness is uniform, and thin film is the finest and close, and thin film variable color response time is slow.
Embodiment 1
(1) electro-conductive glass substrate is cleaned；
With acetone, dehydrated alcohol, deionized water ultrasonic 20 minutes ITO electro-conductive glass substrates respectively, then dry in the baking oven of 60 DEG C
Dry glass substrate；
(2)WO3The preparation of colloidal sol；
By 6g Na2WO4·2H2O joins the dense HNO of 30ml 68% volume ratio3In, 50 DEG C of heating in water bath 2 hours, turning
Speed is for being centrifuged under 9500rpm processing, it is thus achieved that H2WO4Yellow mercury oxide, then by H2WO4Yellow mercury oxide joins 10ml
30%H2O2In, and magnetic agitation 2 hours, it is thus achieved that the peroxide tungstic acid of homogeneous transparent, and with oxygen O2Generation,
I.e. form WO3Colloidal sol；
(3) preparation of pore creating material masterplate；
3.5g P123 is dissolved in 10ml dehydrated alcohol, and stirs, form transparent homogeneous phase solution；
(4) porous WO3The preparation of thin film；
(2) and (3) are mixed together solution, spin coating 2min under rotating speed is 3000rpm, obtain the thin film of homogeneous transparent；
(5)WO3Being dried of thin film；
The thin film obtained in (4) is dried 16 hours at 40 DEG C；
(6)WO3The high-temperature heat treatment of thin film；
Thin film heat treatment 5 hours at 420 DEG C that will obtain in (5).
Under the parameter of embodiment 1, in membrane-film preparation process, in the case of adding 3.5g P123, on ito glass
Deposited the WO of monocline3Thin film.Its surface topography (different amplifications), the cross-section morphology of thin film as illustrated in Figures 5 and 6
As shown in FIG. 7 and 8.WO3Film surface is smooth, and thickness is uniform, and thin film presents loose structure, thin film variable color response time
Hurry up.Figure 10 is WO in embodiment 1310 cyclic voltammetry curve figures of thin film；Figure 12 is WO in embodiment 13Thin film
Light transmittance curve；WO in Figure 14 embodiment 13Thin film coloring before and after facing to pictorial diagram, (left side is coloured state, the right
For state of fading)；Therefore WO3Porous membrane variable color response time is short, and uniform coloring, color contrast big.
Embodiment 2
(1) electro-conductive glass substrate is cleaned；
With acetone, dehydrated alcohol, deionized water ultrasonic 20 minutes ITO electro-conductive glass substrates respectively, then dry in the baking oven of 60 DEG C
Dry glass substrate；
(2)WO3The preparation of colloidal sol；
By 6g Na2WO4·2H2O joins the dense HNO of 30ml 68% volume ratio3In, 50 DEG C of heating in water bath 2 hours, turning
Speed is for being centrifuged under 9500rpm processing, it is thus achieved that H2WO4Yellow mercury oxide, then by H2WO4Yellow mercury oxide joins 10ml
30%H2O2In, then magnetic agitation 2 hours, it is thus achieved that the peroxide wolframic acid of homogeneous transparent, and with oxygen O2Generation, i.e. shape
Become WO3Colloidal sol；
(3) preparation of pore creating material masterplate；
2g P123 is dissolved in 10ml dehydrated alcohol, and stirs, form transparent homogeneous phase solution；
(4) porous WO3The preparation of thin film；
(2) and (3) are mixed together solution, spin coating 2min under rotating speed is 3000rpm, obtain the thin film of homogeneous transparent；
(5)WO3Being dried of thin film；
The thin film obtained in (4) is dried 16 hours at 40 DEG C；
(6)WO3The high-temperature heat treatment of thin film；
Thin film heat treatment 5 hours at 420 DEG C that will obtain in (5).
Under the parameter of embodiment 2, in the case of adding 2g P123, WO3Thin-membrane section SEM pattern such as Fig. 9；
Thin film is to be connected with each other by the nanoparticle of 20～30nm to pile up, and defines a lot of nano-pore knots during accumulation
Structure.WO in Figure 11 embodiment 2310 cyclic voltammetry curves of thin film；Figure 13 is WO in embodiment 23Thin film saturating
Light rate curve；WO in Figure 15 embodiment 23Thin film coloring before and after facing to pictorial diagram, (left side is coloured state, and the right is
Fade state)；Therefore WO3Porous membrane variable color response time is short, and uniform coloring, color contrast bigger.
From the foregoing, it will be observed that the present invention can in ITO Conducting Glass the WO of depositing homogeneous3Porous membrane；The present invention is made
Standby WO3The process of porous membrane is simple, and equipment is very simple, and preparation cost is low, dives in the market with extensive extension
Power.WO prepared by the present invention3Porous membrane variable color response time is short, and uniform coloring, color contrast big.
Claims (9)
1. porous WO3The preparation method of electrochomeric films, it is characterised in that including:
After peroxide tungstic acid and the solution containing pore creating material template uniformly being mixed, being spun on substrate, heat treatment at 350-500 DEG C, obtains described porous WO the most again3Electrochomeric films, wherein, pore creating material template includes poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide).
Preparation method the most according to claim 1, it is characterised in that the preparation method of peroxide tungstic acid includes:
To H2WO4Middle addition H2O2, dissolve H2WO4And form transparent mixed liquor, then stand 0.5-2 days.
Preparation method the most according to claim 1 and 2, it is characterised in that the preparation method of the solution containing pore creating material template includes:
By pore creating material template in dehydrated alcohol, and stir to mixed liquor transparent, thus obtain the solution containing pore creating material template.
4. according to the preparation method described in claim 1-3, it is characterised in that poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide) concentration in dehydrated alcohol is 0.2-0.4g/mL.
5. according to described preparation method arbitrary in claim 1-4, it is characterised in that described substrate includes pretreated ITO electro-conductive glass substrate.
Preparation method the most according to claim 5, it is characterised in that described pretreatment includes immersing substrate successively ultrasonic cleaning in acetone, dehydrated alcohol and deionized water, the time that per stage cleans is 10-20 minute, is dried afterwards.
7. according to described preparation method arbitrary in claim 1-6, it is characterised in that the technological parameter of spin coating masking includes: rotating speed 3000-5000
Rpm, spin coating 1-2 minute.
8. according to described preparation method arbitrary in claim 1-7, it is characterised in that be dried 14-20 hour at 40 DEG C-60 DEG C.
9. according to described preparation method arbitrary in claim 1-8, it is characterised in that heat treatment 3-8 hour at 350 DEG C-500 DEG C.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108663868A (en) * | 2018-07-05 | 2018-10-16 | 东华大学 | A kind of preparation method of tungsten oxide electrochromic electrode |
| CN108863101A (en) * | 2018-06-20 | 2018-11-23 | 华南理工大学 | A kind of high modulation ability crystallization Tungsten Trioxide Electrochromic Films and preparation method thereof |
| CN110255620A (en) * | 2019-05-09 | 2019-09-20 | 哈尔滨工业大学 | A kind of preparation method of two dimension tungsten base nanometer sheet liquid crystal and the method for preparing tungsten base nanometer sheet electrochomeric films material using it |
| CN110467357A (en) * | 2019-08-01 | 2019-11-19 | 西安理工大学 | A kind of tungsten oxide film and preparation method thereof with horn-like pore structure |
| CN110590180A (en) * | 2019-10-18 | 2019-12-20 | 西安交通大学 | Preparation method of low-cost environment-friendly tungsten oxide electrochromic film suitable for large-area production |
| CN111039573A (en) * | 2019-12-23 | 2020-04-21 | 华南理工大学 | WO (WO)3Electrochromic film and preparation method thereof |
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| CN103395842A (en) * | 2013-07-30 | 2013-11-20 | 浙江大学 | Tungsten trioxide nanometer array electrochromic film and preparation method thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108863101A (en) * | 2018-06-20 | 2018-11-23 | 华南理工大学 | A kind of high modulation ability crystallization Tungsten Trioxide Electrochromic Films and preparation method thereof |
| CN108863101B (en) * | 2018-06-20 | 2020-09-22 | 华南理工大学 | High-modulation-capacity crystalline tungsten trioxide electrochromic film and preparation method thereof |
| CN108663868A (en) * | 2018-07-05 | 2018-10-16 | 东华大学 | A kind of preparation method of tungsten oxide electrochromic electrode |
| CN108663868B (en) * | 2018-07-05 | 2021-01-05 | 东华大学 | Preparation method of tungsten oxide electrochromic electrode |
| CN110255620A (en) * | 2019-05-09 | 2019-09-20 | 哈尔滨工业大学 | A kind of preparation method of two dimension tungsten base nanometer sheet liquid crystal and the method for preparing tungsten base nanometer sheet electrochomeric films material using it |
| CN110255620B (en) * | 2019-05-09 | 2022-04-01 | 哈尔滨工业大学 | Preparation method of two-dimensional tungsten-based nanosheet liquid crystal and method for preparing tungsten-based nanosheet electrochromic film material by using same |
| CN110467357A (en) * | 2019-08-01 | 2019-11-19 | 西安理工大学 | A kind of tungsten oxide film and preparation method thereof with horn-like pore structure |
| CN110467357B (en) * | 2019-08-01 | 2021-10-22 | 西安理工大学 | Tungsten oxide film with horn-shaped pore structure and preparation method thereof |
| CN110590180A (en) * | 2019-10-18 | 2019-12-20 | 西安交通大学 | Preparation method of low-cost environment-friendly tungsten oxide electrochromic film suitable for large-area production |
| CN111039573A (en) * | 2019-12-23 | 2020-04-21 | 华南理工大学 | WO (WO)3Electrochromic film and preparation method thereof |
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Application publication date: 20161123 |