CN101514472A - A method for preparing electrochromic nickel oxide film - Google Patents
A method for preparing electrochromic nickel oxide film Download PDFInfo
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- CN101514472A CN101514472A CNA2009101138889A CN200910113888A CN101514472A CN 101514472 A CN101514472 A CN 101514472A CN A2009101138889 A CNA2009101138889 A CN A2009101138889A CN 200910113888 A CN200910113888 A CN 200910113888A CN 101514472 A CN101514472 A CN 101514472A
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Abstract
The invention discloses a method for preparing electrochromic nickel oxide film, comprising the steps of: preparing 0.1mol/L-8.0mol/L of water solution for analyzing pure potassium hydroxide, sodium hydroxide or lithium hydroxide, subsequently adding 0.0mol/L-0.5mol/L of inorganic complexing reagent composed of potassium chloride, sodium chloride and lithium chloride, and then adding 0.0mol/L-0.5mol/L of inorganic complexing reagent composed of citrate, oxalate, tartrate, acetate, and other carboxylic acid derivative; under the temperature of 5 DEG C-85 DEG c and tank voltage of 0.6V-12.0V, continuously electrolyting for 1 min-10h based on graphite block as cathode, metallic nickel foil as anode, switching off the power, taking out the anode strip and finally flushing with tap water, thus the nickel oxide film with electrochromic property can be obtained. The invention has advantages of simple process, and the prepared nickel oxide film is strong in matrix binding force, compact uniform in film layer, good in electrochromic reversibility, easily controllable in film thickness, and is applicable for bulk production.
Description
Technical field
The present invention relates to a kind of preparation method of electrochromic nickel oxide film.
Background technology
Nickel oxide film is a kind of p N-type semiconductorN functional materials with characteristics such as energy storage, electrochromism, catalysis, gas sensitizations, has important use in many high-tech sectors such as chemical power source, flat pannel display, organic chemical industry, environment measurings.The preparation method of nickel oxide film generally can be divided into physics method and chemical method.The physics method mainly comprises methods such as vacuum-evaporation, sputter, ion beam depositing, epitaxial film deposition, advantages such as that the film that makes has is good with matrix bond, rete density height, good uniformity.But because of physics method equipment used cost costliness, processing condition require high, be difficult for carrying out the even plated film of big area and limited its development.Chemical method mainly comprises methods such as thermolysis, chemical vapour deposition, cathodic reaction deposition, sol-gel, its advantage is employed equipment cheap and simple, can accurately controls film chemical component, easy big area manufacturing etc., its shortcoming is a film deposition process difficulty relatively, and film is relatively poor relatively to the sticking power of matrix.Comparatively speaking, chemical method prepare nickel oxide film have with low cost, controllability good, be fit to advantages such as big area and mass-producing manufacturing, thereby has bright development prospect.
Summary of the invention
The purpose of this invention is to provide a kind of have strong with basal body binding force, rete is fine and close, thickness and component is adjustable, good uniformity, good reversibility, the method for preparing electrochemical anodic oxidation of the electrochromic nickel oxide film of characteristics such as big area manufacturing easily.
Concrete steps of the present invention are: the aqueous solution of preparation 0.1mol/L～8.0mol/L analytical pure potassium hydroxide, sodium hydroxide or lithium hydroxide, add 0.0mol/L～0.5mol/L Repone K, sodium-chlor and the inorganic coordination agent of lithium chloride respectively, add 0.0mol/L～0.5mol/L Citrate trianion, oxalate, tartrate, acetate and other carboxylic acid derivative organic complexing agent again; With the graphite block is negative electrode, is anode with the metal nickel foil, under 5 ℃～85 ℃ temperature, control flume voltage is 0.6V～12.0V, deenergization and take out anode strip behind continuous electrolysis 1min～10h with the tap water flushing, promptly obtains having the nickel oxide film of electrochromic property.
The electrochromic nickel oxide film of present method preparation is a metallic nickel matrix converted in-situ film, the tightness degree of itself and matrix bond is that other method deposited film hardly matches, and this nickel oxide film has characteristics such as good reversibility, good stability, nothing come off, long lifetime.
Description of drawings
Fig. 1 is the cyclic voltammetry curve (electrolytic solution is the 1.0mol/L lithium hydroxide aqueous solution, and reference electrode is a saturated calomel electrode, and temperature is 20 ℃, and scanning speed is 5mV/s, and cycle index is 2200 times) of the embodiment of the invention 1 nickel oxide film.
Fig. 2 is 1,000 times of electron scanning micrograph of the embodiment of the invention 1 nickel oxide film.
Fig. 3 is 10,000 times of electron scanning micrographs of the embodiment of the invention 1 nickel oxide film.
Fig. 4 is the cyclic voltammetry curve (electrolytic solution is the 1.0mo1/L lithium hydroxide aqueous solution, and reference electrode is a saturated calomel electrode, and temperature is 15 ℃, and scanning speed is 5mV/s, and cycle index is 3 times) of the embodiment of the invention 2 nickel oxide films.
Embodiment
Embodiment 1:
Taking by weighing commercially available analytical pure potassium hydroxide (purity 95%) 44.8g is dissolved in the 100ml distilled water, add 2.0g analytical pure oxalic acid (purity 99.5%), 1.0g analytical pure citric acid (purity 99.0%), 2.0g analytical pure potassium hydroxide, 0.4g analytical pure Repone K (purity 99.8%) successively, stirring and dissolving.With the graphite block is negative electrode, (0.1mm * 10mm * 30mm) is an anode with the metal nickel foil, be connected to the negative pole and the positive pole of LZ-I hull trough test instrument (Wuhan Long Ze Electronics Co., Ltd.) respectively, time is set to 240min, opening power, regulating voltage are 4.0V, and continuous electrolysis is to finishing, take out the nickel foil anode and with the tap water flushing, oven dry promptly gets nickel oxide film in 80 ℃ of loft drier.In 1.0mol/L analytical pure lithium hydroxide (purity 90%) aqueous solution, with the graphite block is supporting electrode, nickel oxide film with preparation is the research electrode, with 232 type saturated calomel electrode (production of Shanghai thunder magnetic instrument plant) is reference electrode, (Shanghai occasion China instrument company) goes up and measures cyclic voltammetry curve at the CHI660C electrochemical workstation, and the result as shown in Figure 1.In the forward and reverse scan round process of current potential, nickel oxide film transforms between black-and-blue and filbert repeatedly.When electric potential scanning stops experiment during to 5.5V, with this nickel oxide film electrode with the tap water flushing and place 80 ℃ of loft drier to dry.It is carried out x-ray diffraction pattern (XRD) measure, in the XRD figure spectrum metallic nickel diffraction peak is only arranged, and non-oxidation nickel diffraction peak.It is carried out scanning electron microscope (SEM) measure, its photo is shown in accompanying drawing 2, accompanying drawing 3.
Embodiment 2:
Taking by weighing commercially available analytical pure potassium hydroxide (purity 95%) 5.6g is dissolved in the 100ml distilled water, add 2.0g analytical pure oxalic acid (purity 99.5%), 1.0g analytical pure citric acid (purity 99.0%), 4.0g analytical pure potassium hydroxide, 0.4g analytical pure Repone K (purity 99.8%) successively, stirring and dissolving.With the graphite block is negative electrode, (0.1mm * 10mm * 30mm) is an anode with the metal nickel foil, be connected to the negative pole and the positive pole of LZ-I hull trough test instrument (Wuhan Long Ze Electronics Co., Ltd.) respectively, time is set to 30min, opening power, regulating voltage are 4.0V, and continuous electrolysis is to finishing, take out the nickel foil anode and with the tap water flushing, oven dry promptly gets nickel oxide film in 80 ℃ of loft drier.In 1.0mol/L analytical pure lithium hydroxide (purity 90%) aqueous solution, with the graphite block is supporting electrode, with the nickel oxide film is the research electrode, with 232 type saturated calomel electrode (production of Shanghai thunder magnetic instrument plant) is reference electrode, (Shanghai occasion China instrument company) goes up and measures cyclic voltammetry curve at the CHI660C electrochemical workstation, and the result as shown in Figure 4.In the forward and reverse scan round process of current potential, nickel oxide film puce and colourless between transform repeatedly.
Claims (1)
1. the preparation method of an electrochromic nickel oxide film, it is characterized in that concrete steps are: the aqueous solution of preparation 0.1mol/L～8.0mol/L analytical pure potassium hydroxide, sodium hydroxide or lithium hydroxide, add 0.0mol/L～0.5mol/L Repone K, sodium-chlor and the inorganic coordination agent of lithium chloride respectively, add 0.0mol/L～0.5mol/L Citrate trianion, oxalate, tartrate, acetate and other carboxylic acid derivative organic complexing agent again; With the graphite block is negative electrode, is anode with the metal nickel foil, under 5 ℃～85 ℃ temperature, control flume voltage is 0.6V～12.0V, deenergization and take out anode strip behind continuous electrolysis 1min～10h with the tap water flushing, promptly obtains having the nickel oxide film of electrochromic property.
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| Application Number | Priority Date | Filing Date | Title |
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| CNA2009101138889A CN101514472A (en) | 2009-02-23 | 2009-02-23 | A method for preparing electrochromic nickel oxide film |
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| CNA2009101138889A CN101514472A (en) | 2009-02-23 | 2009-02-23 | A method for preparing electrochromic nickel oxide film |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109755029A (en) * | 2019-01-31 | 2019-05-14 | 燕山大学 | A kind of preparation method of flower piece shape nano-nickel oxide |
| CN109841810A (en) * | 2019-01-07 | 2019-06-04 | 浙江工业大学 | A kind of preparation method and application of Ni-NiO/C composite material |
| CN112736199A (en) * | 2019-10-28 | 2021-04-30 | 天津大学 | C8-BTBT single crystal film, preparation method thereof and organic field effect transistor based on C8-BTBT single crystal film |
| CN115259245A (en) * | 2022-06-24 | 2022-11-01 | 玻璃新材料创新中心(安徽)有限公司 | Quantitative lithiated nickel oxide electrochromic film and preparation method thereof |
-
2009
- 2009-02-23 CN CNA2009101138889A patent/CN101514472A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109841810A (en) * | 2019-01-07 | 2019-06-04 | 浙江工业大学 | A kind of preparation method and application of Ni-NiO/C composite material |
| CN109755029A (en) * | 2019-01-31 | 2019-05-14 | 燕山大学 | A kind of preparation method of flower piece shape nano-nickel oxide |
| CN109755029B (en) * | 2019-01-31 | 2020-04-03 | 燕山大学 | Preparation method of flower-like nano nickel oxide |
| CN112736199A (en) * | 2019-10-28 | 2021-04-30 | 天津大学 | C8-BTBT single crystal film, preparation method thereof and organic field effect transistor based on C8-BTBT single crystal film |
| CN112736199B (en) * | 2019-10-28 | 2023-03-24 | 天津大学 | C8-BTBT (British Bittery-based) single crystal film, preparation method thereof and organic field effect transistor based on C8-BTBT single crystal film |
| CN115259245A (en) * | 2022-06-24 | 2022-11-01 | 玻璃新材料创新中心(安徽)有限公司 | Quantitative lithiated nickel oxide electrochromic film and preparation method thereof |
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Open date: 20090826 |