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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- Prior art keywords
- nickel oxide
- oxide film
- electrochromic
- hydroxide
- chloride
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- 229910000480 nickel oxide Inorganic materials 0.000 title claims abstract description 26
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title abstract description 16
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims abstract description 21
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 21
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 11
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 7
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 7
- 239000007864 aqueous solution Substances 0.000 claims abstract description 7
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 7
- 239000010439 graphite Substances 0.000 claims abstract description 7
- 239000008399 tap water Substances 0.000 claims abstract description 6
- 235000020679 tap water Nutrition 0.000 claims abstract description 6
- 239000008139 complexing agent Substances 0.000 claims abstract description 5
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 5
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims abstract description 5
- 229910052751 metal Inorganic materials 0.000 claims abstract description 5
- 239000002184 metal Substances 0.000 claims abstract description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims abstract description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 claims abstract description 3
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims abstract description 3
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims abstract description 3
- 229940095064 tartrate Drugs 0.000 claims abstract description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract 4
- 239000001103 potassium chloride Substances 0.000 claims abstract 2
- 235000011164 potassium chloride Nutrition 0.000 claims abstract 2
- 239000011780 sodium chloride Substances 0.000 claims abstract 2
- 238000002360 preparation method Methods 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 239000010408 film Substances 0.000 abstract 4
- 239000000758 substrate Substances 0.000 abstract 1
- 239000010409 thin film Substances 0.000 abstract 1
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 238000002484 cyclic voltammetry Methods 0.000 description 4
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 4
- 238000011010 flushing procedure Methods 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000000151 deposition Methods 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 239000008151 electrolyte solution Substances 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 235000006408 oxalic acid Nutrition 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 235000007466 Corylus avellana Nutrition 0.000 description 1
- 240000003211 Corylus maxima Species 0.000 description 1
- 206010070834 Sensitisation Diseases 0.000 description 1
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000010349 cathodic reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000010884 ion-beam technique Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000008313 sensitization Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000001149 thermolysis Methods 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
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- Electrochromic Elements, Electrophoresis, Or Variable Reflection Or Absorption Elements (AREA)
Abstract
本发明公开了一种电致变色氧化镍薄膜的制备方法。步骤为：配制0.1mol/L～8.0mol/L分析纯氢氧化钾、氢氧化钠或氢氧化锂的水溶液，分别加入0.0mol/L～0.5mol/L氯化钾、氯化钠和氯化锂无机配位剂，再加入0.0mol/L～0.5mol/L柠檬酸盐、草酸盐、酒石酸盐、乙酸盐和其它羧酸衍生物有机配位剂；以石墨块为阴极，以金属镍箔为阳极，在5℃～85℃温度下，控制槽电压为0.6V～12.0V，连续电解1min～10h后断开电源并取出阳极片，用自来水冲洗，即得到具有电致变色特性的氧化镍薄膜。本发明工序简单，制备的氧化镍薄膜与基体结合力强，膜层致密均匀，电致变色可逆性好，膜厚度容易调控，容易进行大面积制造。
The invention discloses a method for preparing an electrochromic nickel oxide film. The steps are: prepare an aqueous solution of 0.1mol/L～8.0mol/L analytically pure potassium hydroxide, sodium hydroxide or lithium hydroxide, and add 0.0mol/L～0.5mol/L potassium chloride, sodium chloride and chloride Lithium inorganic complexing agent, then add 0.0mol/L～0.5mol/L citrate, oxalate, tartrate, acetate and other organic complexing agents of carboxylic acid derivatives; graphite block as cathode, metal Nickel foil is used as the anode. At a temperature of 5°C to 85°C, the voltage of the control cell is 0.6V to 12.0V. After continuous electrolysis for 1min to 10h, the power supply is disconnected and the anode piece is taken out and washed with tap water to obtain electrochromic. nickel oxide film. The process of the invention is simple, the prepared nickel oxide thin film has strong binding force with the substrate, the film layer is dense and uniform, the electrochromic reversibility is good, the film thickness is easy to control, and it is easy to manufacture in a large area.
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)
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2009101138889A CN101514472A (en) | 2009-02-23 | 2009-02-23 | A method for preparing electrochromic nickel oxide film |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2009101138889A CN101514472A (en) | 2009-02-23 | 2009-02-23 | A method for preparing electrochromic nickel oxide film |
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| Publication Number | Publication Date |
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| CN101514472A true CN101514472A (en) | 2009-08-26 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNA2009101138889A Pending 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-shaped nanometer 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 | A kind of 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-shaped nanometer 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 | A kind of quantitative lithiated nickel oxide electrochromic film and preparation method thereof |
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Open date: 20090826 |