CN104492675A - Low-temperature electrochromic NiO film preparation method - Google Patents
Low-temperature electrochromic NiO film preparation method Download PDFInfo
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Abstract
The invention discloses a low-temperature electrochromic NiO film preparation method. The method includes the steps: S1, preparing precursor solution, namely solving a nickelic solute material in a cosolvent, and stirring at the room temperature; S2, depositing the precursor solution onto the surface of a transparent conductive substrate to form a precursor film by means of spin coating or the Czochralski method, and putting the deposited precursor film on a roasting table for roasting treatment at the temperature of 100-120 DEG C; S3, adopting an ultraviolet lamp for photochemical treatment, wherein the ultrasonic lamp emits 90% of ultraviolet light 254 nanometers in wavelength and 10% of ultraviolet light 185 nanometers in wavelength. The low-temperature electrochromic NiO film preparation method is simple in preparation process and low in preparation temperature and can be used for preparing electrochromic NiO films not only on transparent hard conductive substrates but also on transparent flexible conductive substrates.
Description
Technical field
The present invention relates to the preparation field of functional material, more specifically, relate to a kind of method of low-temperature growth electrochromism NiO film.
Background technology
Electrochromism refer to device for Optical Properties of Materials can occur under the effect of extra electric field or electric current optical property (as transmission, reflection and absorption etc.) stable, the phenomenon of reversible shock color change, present the reversible transition of transparency and color in appearance.It is reversible with features such as memory storage abilities that electrochromic material generally possesses discoloration continuously adjustabe, colourshifting process.Electrochromic correlative study is from the thirties in 20th century, and so far, electrochromism causes as a kind of phenomenon of uniqueness and pays close attention to widely and achieve larger progress.At present, electrochromic material has been applied to electrochromic intelligent window, the field such as automobile rearview mirror and road sign display.
The technique preparing electrochomeric films at present mainly adopts sol-gel process, chemical vapour deposition technique, physical vaporous deposition, chemical bath deposition method and electrochemical deposition method etc., but technics comparing is complicated, is unfavorable for large-scale application.
Summary of the invention
An object of the present invention is to provide a kind of method of low-temperature growth electrochromism NiO film, comprises the following steps:
S1. precursor liquid is configured:
Nickeliferous solute material is dissolved in cosolvent, stirring at room temperature, obtains final product;
S2. adopt spin coating method or czochralski method deposition precursor liquid to form precursor film in transparent conductive substrates surface, then the precursor film of deposition is placed in baking table and carries out baking and process, the temperature of described baking process is 100 ~ 120
oc;
S3. adopt uviol lamp to carry out photochemical treatment, described uviol lamp is made up of the ultraviolet light of 254 nano wave lengths of 90% and the ultraviolet light of 185 nano wave lengths of 10%.
The photochemical treatment time described in S3 flow process is 0.5 ~ 12 hour.
Described spin coating method is for adopting spin coating equipment spin coating NiO precursor liquid in electrically conducting transparent substrate.
NiO precursor liquid is deposited on electrically conducting transparent substrate for adopting Best-Effort request equipment by described czochralski method.
Described nickeliferous solute material is nickel acetate or nickel nitrate; Described cosolvent is EGME and glacial acetic acid.
Described transparent conductive substrates is clear hard conductive substrates or transparent flexible conductive substrates.
A kind of above-mentioned preparation method is provided to prepare the application in intelligent window in addition.
A kind of above-mentioned preparation method is provided to prepare the application in automobile rearview mirror or road sign display in addition.
A kind of above-mentioned preparation method is provided application in preparation preparation large area electrochomeric films and/or flexible electrochomeric films in addition.
The maximum temperature of the preparation flow of described electrochromism NiO film is not more than 120 above
oc, in preparation flow, temperature is lower, therefore Low Temperature Photochemistry solwution method not only can deposit NiO film in clear hard glass conductive substrates, is also applicable to deposit NiO film in the conductive substrates such as transparent flexible PET simultaneously.
Core technology scheme of the present invention is the Low Temperature Photochemistry solution manufacturing method providing a kind of electrochromism NiO film.This preparation method is simple, and cost is low, and temperature is low, can be used for large area film forming, and can prepare electrochromism NiO film on transparent flexible conducting substrate.The method is with a wide range of applications in the preparation field such as large area electrochomeric films and flexible electrochomeric films.
Accompanying drawing explanation
Fig. 1. take Low Temperature Photochemistry solwution method to be prepared in electrically conducting transparent suprabasil electrochromism NiO film.
Fig. 2. be deposited on the cyclic voltammetry scan curve of the electrochromism NiO film of clear glass/FTO substrate.
Fig. 3. the electrochromism NiO film being deposited on clear glass/FTO substrate fades the transmitance collection of illustrative plates of state and coloured state.
Fig. 4. be deposited on the cyclic voltammetry scan curve of the electrochromism NiO film of transparent flexible PET/ITO substrate.
Fig. 5. the electrochromism NiO film being deposited on transparent flexible PET/ITO substrate fades the transmitance collection of illustrative plates of state and coloured state.
Detailed description of the invention
The present invention is further described below in conjunction with the drawings and specific embodiments.Unless stated otherwise, the present invention adopts reagent, equipment and method are reagent, the Apparatus and operation method of the art routine.
Embodiment 1
Electrochromism NiO thin film deposition in clear glass/FTO conductive substrates schematic diagram as shown in Figure 1, the method of testing that its Low Temperature Photochemistry method prepares electrochromism NiO film flow process and electrochromism phenomenon is as follows: the preparation of NiO precursor liquid: solute is nickel acetate, solvent is EGME and glacial acetic acid, and EGME and glacial acetic acid ratio are 2:1.Stirring at room temperature is to dissolving completely.
The preparation of NiO precursor thin film: take chemical solution spin coating method, is spun and coated at NiO precursor liquid in transparent glass/FTO substrate, then 120
othe baking table of C carries out baking process.
The photochemical treatment of NiO precursor thin film: the precursor thin film after baking to be placed under ultraviolet lamp room temperature photo-irradiation treatment 4 hours.Ultraviolet light equiwavelength is mainly 254 nanometers (90%) and 184 nanometers (10%).
The testing and analyzing of electrochromic property: adopt electrochemical workstation CHI 660E, adopts the Cyclic voltamogram of three-electrode system test electrochromism NiO film.Three-electrode system: saturated calomel is reference electrode, platinized platinum is to electrode, and electrochromism NiO film is working electrode, and the potassium hydroxide solution of 1 mol/L is electrolyte.Be deposited on the cyclic voltammetry curve of the electrochromism NiO film of clear glass/FTO substrate as shown in Figure 2.In addition, adopt ultraviolet-visible-near infrared spectrometer (UV 3150) test electrochromism NiO film painted with fade after transmitance, the electrochromism NiO film being deposited on clear glass/FTO substrate fade state and coloured state transmitance collection of illustrative plates as shown in Figure 3.
Embodiment 2
Electrochromism NiO thin film deposition in transparent flexible PET/ ITO conductive substrates schematic diagram as shown in Figure 1, the method of testing that its Low Temperature Photochemistry method prepares electrochromism NiO film flow process and electrochromism phenomenon is as follows: the preparation of NiO precursor liquid: solute is nickel nitrate, solvent is EGME and glacial acetic acid, and EGME and glacial acetic acid ratio are 2:1.Stirring at room temperature is to dissolving completely.
The preparation of NiO precursor thin film: take chemical solution spin coating method, is spun and coated in transparent flexible PET/ITO substrate, then 120 by NiO precursor liquid
obaking process is carried out in the baking box of C.
The photochemical treatment of NiO precursor thin film: the precursor thin film after baking to be placed under ultraviolet lamp room temperature photo-irradiation treatment 6 hours.Ultraviolet light equiwavelength is mainly 254 nanometers (90%) and 184 nanometers (10%).
The testing and analyzing of electrochromic property: adopt electrochemical workstation CHI 660E, adopt the Cyclic voltamogram of the test electrochromism NiO film of three-electrode system.Three-electrode system: saturated calomel is reference electrode, platinized platinum is to electrode, and NiO film is working electrode, and the potassium hydroxide solution of 1 mol/L is electrolyte.Be deposited on the cyclic voltammetry curve of the electrochromism NiO film of transparent flexible PET/ITO substrate as shown in Figure 4.In addition, adopt ultraviolet-visible-near infrared spectrometer (UV 3150) test electrochromism NiO film painted with fade after transmitance, the electrochromism NiO film being deposited on flexible PET/ITO substrate fade state and coloured state transmitance collection of illustrative plates as shown in Figure 5.
Claims (9)
1. a method for low-temperature growth electrochromism NiO film, is characterized in that, comprise the following steps,
S1. precursor liquid is configured: be dissolved in cosolvent by nickeliferous solute material, stirring at room temperature, obtain final product;
S2. adopt spin coating method or czochralski method deposition precursor liquid to form precursor film in transparent conductive substrates surface, then the precursor film of deposition is placed in baking table and carries out baking and process, the temperature of described baking process is 100 ~ 120
oc;
S3. adopt uviol lamp to carry out photochemical treatment, described uviol lamp is made up of the ultraviolet light of 254 nano wave lengths of 90% and the ultraviolet light of 185 nano wave lengths of 10%.
2. the method for low-temperature growth electrochromism NiO film according to claim 1, it is characterized in that, described nickeliferous solute material is nickel acetate or nickel nitrate; Described cosolvent is EGME and glacial acetic acid.
3. the method for low-temperature growth electrochromism NiO film according to claim 1, it is characterized in that, the photochemical treatment time described in S3 is 0.5 ~ 12 hour.
4. the method for low-temperature growth electrochromism NiO film according to claim 1, is characterized in that, described spin coating method is for adopting spin coating equipment spin coating NiO precursor liquid in electrically conducting transparent substrate.
5. the method for low-temperature growth electrochromism NiO film according to claim 1, is characterized in that, NiO precursor liquid is deposited on electrically conducting transparent substrate for adopting Best-Effort request equipment by described czochralski method.
6. the method for low-temperature growth electrochromism NiO film according to claim 1, is characterized in that, described transparent conductive substrates is clear hard conductive substrates or transparent flexible conductive substrates.
7. a preparation method according to claim 1 is preparing the application in intelligent window.
8. a preparation method according to claim 1 is preparing the application in automobile rearview mirror or road sign display.
9. the application of preparation method according to claim 1 in preparation preparation large area electrochomeric films and/or flexible electrochomeric films.
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Cited By (8)
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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 |
| CN108996918A (en) * | 2018-07-26 | 2018-12-14 | 暨南大学 | A kind of nano NiOxElectrochomeric films and its preparation method and application |
| CN109240014A (en) * | 2018-10-23 | 2019-01-18 | 南京邮电大学 | A kind of flexible electrochromic film and its preparation method and application based on tungsten oxide |
| CN110102457A (en) * | 2019-04-19 | 2019-08-09 | 东北大学秦皇岛分校 | A method of preparing nickel oxide nano-crystal electrochomeric films at low temperature |
| CN110109311A (en) * | 2019-04-19 | 2019-08-09 | 东北大学秦皇岛分校 | A kind of full-solid electrochromic device and preparation method thereof |
| CN110488551A (en) * | 2019-08-23 | 2019-11-22 | 南京邮电大学 | A kind of flexibility electrochromism sull, device and preparation method thereof |
| CN113185138A (en) * | 2021-06-18 | 2021-07-30 | 南京大学 | Preparation method of high-activity nanocrystalline NiO film |
| CN117263526A (en) * | 2023-10-25 | 2023-12-22 | 苏州光昛智能科技有限公司 | Post-treatment method for improving electrochromic film performance |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108663868A (en) * | 2018-07-05 | 2018-10-16 | 东华大学 | A kind of preparation method of tungsten oxide electrochromic electrode |
| CN108996918A (en) * | 2018-07-26 | 2018-12-14 | 暨南大学 | A kind of nano NiOxElectrochomeric films and its preparation method and application |
| CN109240014A (en) * | 2018-10-23 | 2019-01-18 | 南京邮电大学 | A kind of flexible electrochromic film and its preparation method and application based on tungsten oxide |
| CN110102457A (en) * | 2019-04-19 | 2019-08-09 | 东北大学秦皇岛分校 | A method of preparing nickel oxide nano-crystal electrochomeric films at low temperature |
| CN110109311A (en) * | 2019-04-19 | 2019-08-09 | 东北大学秦皇岛分校 | A kind of full-solid electrochromic device and preparation method thereof |
| CN110488551A (en) * | 2019-08-23 | 2019-11-22 | 南京邮电大学 | A kind of flexibility electrochromism sull, device and preparation method thereof |
| CN113185138A (en) * | 2021-06-18 | 2021-07-30 | 南京大学 | Preparation method of high-activity nanocrystalline NiO film |
| CN113185138B (en) * | 2021-06-18 | 2022-04-22 | 南京大学 | Preparation method of high-activity nanocrystalline NiO film |
| CN117263526A (en) * | 2023-10-25 | 2023-12-22 | 苏州光昛智能科技有限公司 | Post-treatment method for improving electrochromic film performance |
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Application publication date: 20150408 |