CN107382092A - TiO with Nanoparticles Embedded structure2 /WO3Compound electrochromic membrane and preparation method thereof - Google Patents

TiO with Nanoparticles Embedded structure2 /WO3Compound electrochromic membrane and preparation method thereof Download PDF

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Publication number
CN107382092A
CN107382092A CN201710704288.4A CN201710704288A CN107382092A CN 107382092 A CN107382092 A CN 107382092A CN 201710704288 A CN201710704288 A CN 201710704288A CN 107382092 A CN107382092 A CN 107382092A
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tio
preparation
solution
nanocrystalline
nanoparticles embedded
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Inventor
刘涌
韩高荣
袁广中
滑晨铮
姜珊珊
宋晨路
汪建勋
沈鸽
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Zhejiang University ZJU
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Zhejiang University ZJU
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Priority to CN201710704288.4A priority Critical patent/CN107382092A/en
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    • 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
    • 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
    • C03C2217/40—Coatings comprising at least one inhomogeneous layer
    • C03C2217/43—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase
    • C03C2217/44—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the composition of the continuous phase
    • C03C2217/45—Inorganic continuous phases
    • 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
    • C03C2217/40—Coatings comprising at least one inhomogeneous layer
    • C03C2217/43—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase
    • C03C2217/46—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the dispersed phase
    • C03C2217/47—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the dispersed phase consisting of a specific material
    • C03C2217/475—Inorganic materials
    • C03C2217/477—Titanium oxide
    • 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
    • C03C2217/70—Properties of coatings
    • 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
    • C03C2218/111—Deposition methods from solutions or suspensions by dipping, immersion
    • 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
    • C03C2218/112—Deposition methods from solutions or suspensions by spraying
    • 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
    • C03C2218/116—Deposition methods from solutions or suspensions by spin-coating, centrifugation

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  • 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 discloses a kind of TiO with Nanoparticles Embedded structure2/WO3The preparation method of compound electrochromic membrane, including step：1) by TiO2Manocrystalline powders are dissolved in water, form TiO2The nanocrystalline aqueous solution；2) to TiO2Ammonium metatungstate is added in the nanocrystalline aqueous solution, supersound process forms presoma composite solution；3) ethanol and polyethylene glycol are added into forerunner's bluk recombination solution and is ultrasonically treated to adjust the viscosity of solution and surface tension；4) prepare wet film on electrically-conductive backing plate using spin-coating method or czochralski method or spraying process, 5) wet film is thermally treated resulting in TiO in atmosphere2/WO3Compound electrochromic membrane.Invention additionally discloses the TiO obtained using above-mentioned preparation method2/WO3Compound electrochromic membrane.Preparation method of the present invention is simple, easily on various substrates of different shapes film forming, materials are few, cost is low, are suitable for industrialized production.

Description

TiO with Nanoparticles Embedded structure2/WO3Compound electrochromic membrane and its preparation Method
Technical field
The present invention relates to electrochromism energy-conservation laminated film field, and in particular to a kind of with Nanoparticles Embedded structure TiO2/WO3Compound electrochromic membrane and preparation method thereof.
Background technology
So-called electrochromism refers in the presence of applied voltage or electric field, and material color or transmitance are stablized reversible Change.The research of electrochromic effect will trace back to Deb in 1966 to amorphous state WO3The preparation of film, learn both at home and abroad since then Person has carried out deeply extensive research around electrochomeric films and its application.At present, electrochromic material is considered as most to have One of intellectual material of application prospect, in smart window (smart window), automobile anti-glazing rearview mirror, electrochromic display device (ECD) etc. Direction has huge potential using value.
In numerous electrochromic materials, WO3As most common inorganic cathode electrochromic material, there is cheap nothing The advantages that malicious superior performance is stable, is received significant attention.General WO3The preparation method of film includes chemical vapor deposition, radio frequency Sputtering and the method for some wet-chemicals, such as collosol and gel, spray pyrolysis, WO prepared by these methods3Film often by Dense in structure, chemism is relatively low, and the migration of its intermediate ion or electronics is affected, and often spectral modulation amplitude is not Height, the response time is longer, and discoloration is inefficient.TiO2It is that a kind of non-toxic inexpensive has the active material of superior chemical, small size TiO2Nanocrystalline and WO3It is compounded to form the TiO with Nanoparticles Embedded structure2/WO3Nano compound film, TiO2It is nanocrystalline in WO3 Nanoparticles Embedded structure is formed in matrix, TiO can be formed in the film2/WO3Hetero-junctions, strengthen WO3Electrochromic property, can Complementary type full-solid electrochromic device is composed of as the anode electrochromism such as negative electrode coloring material and NiO.
The content of the invention
It is an object of the invention to provide a kind of modulation amplitude is big, the response time is fast, and the efficiency high that changes colour has nanometer edge The TiO of embedding structure2/WO3Compound electrochromic membrane and preparation method thereof.
Concrete technical scheme of the present invention is as follows：
A kind of TiO with Nanoparticles Embedded structure2/WO3The preparation method of compound electrochromic membrane, comprises the following steps：
Step (1)：By TiO2Manocrystalline powders ultrasonic disperse is dissolved in water, forms TiO2The nanocrystalline aqueous solution；
Step (2)：To TiO2Ammonium metatungstate is added in the nanocrystalline aqueous solution, supersound process forms presoma composite solution；
Step (3)：Ethanol and polyethylene glycol are added into forerunner's bluk recombination solution and is ultrasonically treated to adjust the viscous of solution Degree and surface tension；
Step (4)：By composite solution made from step (2) using spin coating, czochralski method or spraying process coated on substrate into Wet film；
Step (5)：Wet film in step (4) is annealed in atmosphere, and WO is made3Film.
In the present invention, with ammonium metatungstate and TiO2It is nanocrystalline it is molten altogether form composite solution in aqueous, add ethanol and Polyethylene glycol is to adjust the viscosity of solution, by the way that composite solution is uniformly coated in into base the methods of spin coating, czochralski method or spraying On plate, then it is heat-treated under air conditionses, forms TiO2/WO3Nano-composite electrochromic film.
In step (1), by TiO2Nanocrystalline ultrasonic disperse is dissolved in water, forms TiO2The nanocrystalline aqueous solution.TiO used2Nanometer Brilliant average grain diameter has larger solubility in 3~20nm in aqueous.Preferably, TiO2Nanocrystalline concentration control exists Below 0.4g/mL, TiO2Nanocrystalline concentration is too high to be caused to dissolve insufficient, final forming thin film degradation, film transmission Rate reduces.
In step (2), the TiO completed is configured to step (1)2Ammonium metatungstate is added in the nanocrystalline aqueous solution, forms forerunner Bluk recombination solution；Preferably, the nanocrystalline mass ratio of ammonium metatungstate and TiO2 added, between 1~50, ammonium metatungstate is dense The too low meeting of degree causes to not sufficiently form TiO2/WO3Nanoparticles Embedded structure, electrochromic property are deteriorated.
In addition, to obtain optimal electrochromic property, ammonium metatungstate and TiO2Nanocrystalline quality is than optimum control 2 ~5 is proper.
In step (3), after the completion of composite solution configuration, ethanol and polyethylene glycol, ethanol and poly- second two are added into solution Alcohol can adjust solution viscosity and surface tension.Preferably, polyethylene glycol is PEG600 in the step, in the step ethanol with And the volume fraction of PEG600 and step (1) reclaimed water is 2:1:6.
Step (4) processing is carried out after the completion of step (3) processing, obtained composite solution is coated on substrate, it is described Substrate is ITO electro-conductive glass or FTO electro-conductive glass, and substrate needs to be cleaned before coating solution, is favorably improved ammonium metatungstate Coating effect of the solution on substrate, improve the performance of laminated film.Specific cleaning is as follows：It is in acetone that ITO is conductive Glass or FTO electro-conductive glass are cleaned by ultrasonic 30min, are put into ultrasonic 30min in deionized water after deionized water rinsing 3 times, then use Ultrasonic 30min operations are carried out in ethanol after deionized water rinsing 3 times, fully to clean ITO electro-conductive glass or FTO electro-conductive glass tables Grease, the dust etc. of face attachment.It is many that composite solution is coated into method to substrate, spin coating, czochralski method or spray can be used Coating coats.
Described TiO is made through high-temperature heat treatment in wet film made from step (4) in step (5)2/WO3It is nano combined thin Film.The atmosphere of heat treatment is air.The temperature range of heat treatment is 300-400 DEG C, and temperature is too high, and substrate resistance per square can increase, It is unfavorable for optical property.
Present invention also offers a kind of TiO with Nanoparticles Embedded structure2/WO3Compound electrochromic membrane, utilization are above-mentioned Preparation method obtain；Wherein, TiO2Nanocrystalline Nanoparticles Embedded is in WO3Among matrix material.
By having the TiO of Nanoparticles Embedded structure made from the inventive method2/WO3Nano-composite electrochromic film, TiO2It is nanocrystalline in WO3Nanoparticles Embedded structure is formed in film substrate, improves WO3Electrochromic property, compared to existing WO3Electrochomeric films, there is the characteristics of electrochromism modulation amplitude is big, and the response time is fast, becomes colour efficiency, there is production well Industry development prospect.And preparation method is simple, easily on various substrates of different shapes film forming, materials are few, cost is low, suitable In industrialized production.
Brief description of the drawings
Fig. 1 is the TiO with Nanoparticles Embedded structure prepared by case study on implementation 12/WO3The SEM surface pictures of laminated film；
Fig. 2 is the TiO with Nanoparticles Embedded structure prepared by case study on implementation 12/WO3The SEM cross-section photographs of laminated film；
Fig. 3 is the TiO with Nanoparticles Embedded structure prepared by case study on implementation 12/WO3The TEM photos of laminated film；
Fig. 4 is the TiO with Nanoparticles Embedded structure prepared by case study on implementation 12/WO3The electrochromism light modulation of laminated film Performance；
Fig. 5 is the TTiO with Nanoparticles Embedded structure prepared by case study on implementation 12/WO3The electrochromism response of laminated film Time.
Embodiment
The present invention is described in detail with reference to embodiment and accompanying drawing, but the present invention is not limited to this.
Case study on implementation 1：
The implementation case is used as substrate using ito glass (30mm × 30mm), carries out following cleaning step before coating： In acetone by ito glass be cleaned by ultrasonic 30min → deionized water rinsing 3 times then be put into ultrasonic 30min in deionized water → go from Ultrasonic 30min → drying, standby is carried out after being rinsed 3 times in sub- water in ethanol.
Step (1)：By 0.6g TiO2Manocrystalline powders ultrasonic disperse is dissolved in 6mL water, forms TiO2The nanocrystalline aqueous solution；
Step (2)：1.5g ammonium metatungstates are added in the foregoing nanocrystalline aqueous solution of gained TiO2, supersound process obtains compound Solution；
Step (3)：Before state to sequentially add 2mL ethanol and 1mL PEG600 in composite solution, be ultrasonically treated；
Step (4)：Using spin coating instrument by composite solution spin coating ito substrate after cleaning；Spin coating rotating speed is 500r/ Min spin coating time 5s, then rotating speed 3000r/min spin coating times 20s；
Step (5)：Wet film made from step (4) is first heat-treated in air atmosphere, heat treatment temperature is 350 DEG C, is protected The warm time is 60min, and TiO is made2/WO3Nano compound film.
As shown in figure 1, the TiO with Nanoparticles Embedded structure prepared by case study on implementation 12/WO3The SEM tables of nano compound film Face photo, film surface are uniform；As shown in Fig. 2 the TiO with Nanoparticles Embedded structure prepared by case study on implementation 12/WO3Nanometer is multiple Close the SEM cross-section photographs of film, film thickness 160nm；As shown in figure 3, the preparation of case study on implementation 1 has Nanoparticles Embedded structure TiO2/WO3The TEM photos of nano compound film, TiO2It is nanocrystalline in WO3Nanoparticles Embedded structure is formed in film substrate；Such as figure Shown in 4, the TiO with Nanoparticles Embedded structure of the preparation of case study on implementation 12/WO3The electrochromism light modulation of nano compound film Can, film visible light wave range average optical modulation amplitude up to 56%；As shown in figure 5, the preparation of case study on implementation 1 has nanometer edge The TiO of embedding structure2/WO3The electrochromism response time of nano compound film, coloring during electrochromism spectrum change rate 90% The response time is respectively 8.1s and 2.7s with fading.
The foregoing is only the preferable implementation example of the present invention, be not intended to limit the invention, it is all in spirit of the invention and Within principle, any modification, equivalent substitution and improvements made etc., it should be included in the scope of the protection.

Claims (8)

  1. A kind of 1. TiO with Nanoparticles Embedded structure2/WO3The preparation method of compound electrochromic membrane, it is characterised in that including Following steps：
    1) by TiO2Manocrystalline powders are dissolved in water, form TiO2The nanocrystalline aqueous solution；
    2) to TiO2Ammonium metatungstate is added in the nanocrystalline aqueous solution, supersound process forms presoma composite solution；
    3) ethanol and polyethylene glycol are added into forerunner's bluk recombination solution and is ultrasonically treated to adjust the viscosity of solution and surface Power；
    4) wet film is prepared on electrically-conductive backing plate using spin-coating method or czochralski method or spraying process,
    5) wet film is thermally treated resulting in TiO in atmosphere2/WO3Compound electrochromic membrane.
  2. 2. preparation method as claimed in claim 1, it is characterised in that in step 1), TiO used2Nanocrystalline average grain diameter is 3~20nm, TiO2Nanocrystalline concentration is controlled in below 0.4g/mL.
  3. 3. preparation method as claimed in claim 1, it is characterised in that in step 2), the ammonium metatungstate and TiO of addition2Nanometer Brilliant mass ratio is between 1~50.
  4. 4. preparation method as claimed in claim 1, it is characterised in that in step 3), polyethylene glycol PEG600, ethanol and PEG600 is 2 relative to the volume fraction of water:1:6.
  5. 5. preparation method as claimed in claim 1, it is characterised in that described electrically-conductive backing plate is ito substrate or FTO bases Plate.
  6. 6. preparation method as claimed in claim 1, it is characterised in that in step 5), the temperature range of heat treatment for 300~ 400℃。
  7. A kind of 7. TiO with Nanoparticles Embedded structure2/WO3Compound electrochromic membrane, it is characterised in that using such as claim Preparation method described in 1~6 any one obtains.
  8. 8. TiO as claimed in claim 72/WO3Compound electrochromic membrane, it is characterised in that TiO2Nanocrystalline Nanoparticles Embedded In WO3Among matrix material.
CN201710704288.4A 2017-08-17 2017-08-17 TiO with Nanoparticles Embedded structure2 /WO3Compound electrochromic membrane and preparation method thereof Pending CN107382092A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110255923A (en) * 2019-06-17 2019-09-20 浙江工业大学 A kind of TiO2Nano particle adsorbs imide derivative film and its application as electrochromic material
CN113800781A (en) * 2021-09-14 2021-12-17 浙江大学 Tungsten trioxide-titanium dioxide electrochromic film and preparation method thereof
CN113913898A (en) * 2021-09-16 2022-01-11 浙江大学 TiO 22Reflection type electrochromic film and preparation method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110255923A (en) * 2019-06-17 2019-09-20 浙江工业大学 A kind of TiO2Nano particle adsorbs imide derivative film and its application as electrochromic material
CN110255923B (en) * 2019-06-17 2021-12-21 浙江工业大学 TiO 22Nanoparticle adsorption perylene bisimide derivative film and application thereof as electrochromic material
CN113800781A (en) * 2021-09-14 2021-12-17 浙江大学 Tungsten trioxide-titanium dioxide electrochromic film and preparation method thereof
CN113913898A (en) * 2021-09-16 2022-01-11 浙江大学 TiO 22Reflection type electrochromic film and preparation method thereof

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Application publication date: 20171124