CN108545961A - A kind of preparation method of nickel oxide nano pipe - Google Patents
A kind of preparation method of nickel oxide nano pipe Download PDFInfo
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- CN108545961A CN108545961A CN201810736675.0A CN201810736675A CN108545961A CN 108545961 A CN108545961 A CN 108545961A CN 201810736675 A CN201810736675 A CN 201810736675A CN 108545961 A CN108545961 A CN 108545961A
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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
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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
- C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
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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
- C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
- C03C17/23—Oxides
- C03C17/25—Oxides by deposition from the liquid phase
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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
- C03C2217/00—Coatings on glass
- C03C2217/40—Coatings comprising at least one inhomogeneous layer
- C03C2217/425—Coatings comprising at least one inhomogeneous layer consisting of a porous layer
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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
- C03C2217/00—Coatings on glass
- C03C2217/70—Properties of coatings
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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
- C03C2217/00—Coatings on glass
- C03C2217/90—Other aspects of coatings
- C03C2217/94—Transparent conductive oxide layers [TCO] being part of a multilayer coating
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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
- 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
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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
- C03C2218/00—Methods for coating glass
- C03C2218/30—Aspects of methods for coating glass not covered above
- C03C2218/32—After-treatment
- C03C2218/328—Partly or completely removing a coating
Abstract
The invention discloses a kind of preparation methods of nickel oxide nano pipe, zinc oxide seed layer is prepared by spin-coating method first, then high-sequential, the zinc oxide nano rod template perpendicular to FTO conductive substrates are prepared by hydro-thermal method, the length of zinc oxide nano rod is controlled by controlling the hydro-thermal reaction time；Then the method for passing through chemical bath prepares the sheet nickel oxide of one layer of coating zinc oxide nanometer rods, then pass through alkaline corrosion and remove zinc oxide template, finally annealing obtains the nickel oxide nano pipe perpendicular to conductive substrates, and nickel oxide nano pipe is perpendicular to FTO conductive substrates.The present invention is of low cost, and operation is simple, and reaction condition is controllable, and obtained nickel oxide nano pipe structure has higher specific surface area, is conducive to quick transmission of the electrolyte ion in nickel oxide nano structure, improves the electrochromic property of nickel oxide material.
Description
Technical field
The invention belongs to anode electrochromic material preparing technical field, be related to it is a kind of can be as electrochromic material
The preparation method of nickel oxide nano pipe.
Background technology
Electrochromic material has as a kind of novel energy-saving material in display, smart window, stealth material etc.
The continuous of immeasurable potentiality, especially smart window is popularized, and has prodigious effect to improving life comfort level.Due to electroluminescent
These features of off-color material have huge effect to energy conservation and environmental protection.Nickel oxide material due to resourceful,
Preparation method is simple, therefore receives significant attention.Traditional dense oxide nickel film is unfavorable for electricity since specific surface area is small
The diffusion for solving liquid causes the discoloration response time long, and contrast is low, and coloration efficiency is low；Due to the electrochemistry that nanostructure is excellent
Can, thus can preparation structure is orderly, nanostructure nickel oxide photochromic layer perpendicular to substrate, to improve the ratio table of nickel oxide
Area expands ion channel, reduces the diffusional resistance of charge or ion between electrolyte and electrode material, to improve oxidation
Nickel shortens the response time to the modulation amplitude and coloration efficiency of light.
Invention content
It is an object of the invention to：A kind of preparation method of nickel oxide nano pipe is provided, current nickel oxide conduct is improved
The response speed of electrochromic material and visible optical modulation amplitude.
To achieve the goals above, the present invention provides the following technical solutions：
A kind of preparation method of nickel oxide nano pipe, includes the following steps：
(1) Zinc diacetate dihydrate is dissolved in alcohol, ultrasonic disperse obtains solution I；By zinc nitrate hexahydrate and hexa-methylene
Tetramine is dissolved in ultra-pure water and obtains solution II；Six hydration nickel sulfate and potassium peroxydisulfate are dissolved in ultra-pure water, ultrasonic disperse obtains molten
Liquid III；
(2) solution I is spun on FTO electro-conductive glass, the FTO electro-conductive glass that spin coating finishes is placed in Muffle furnace and is carried out
Annealing；FTO electro-conductive glass after annealing is put into solution II progress hydro-thermal reaction and stirs to get zinc oxide nano rod；
(3) the FTO electro-conductive glass of zinc oxide nano rod is placed in solution III load, electromagnetic agitation, and ammonium hydroxide is added
Carry out chemical bath deposition；FTO electro-conductive glass is then taken out, is immersed in NaOH solution after being rinsed with water and obtains the oxidation of hollow shape
Nickel；It is put into make annealing treatment under argon atmosphere in tube furnace after the nickel oxide of hollow shape is rinsed with water and be received up to nickel oxide
Mitron.
Preferably, a concentration of 30-50mM of zinc acetate in solution I in step (1)；A concentration of 20- of zinc nitrate in solution II
The molar ratio of 30mM, zinc nitrate and hexa is 1：1；Concentration of nickel sulfate is 0.1M-0.12M, nickel sulfate in solution III
Molar ratio with potassium peroxydisulfate is 5:1.
Preferably, rotating speed is 500-1000 circles/second, spin-coating time 1-2min when spin coating in step (2).
Preferably, annealing temperature is 350-420 DEG C in step (2), annealing time 25-35min.
Preferably, the condition of hydro-thermal reaction is that 1-2h is carried out at 75-85 DEG C in step (2).
Preferably, the chemical bath deposition time is 1-2min in step (3).
Preferably, NaOH concentration is 1-2M in NaOH solution in step (3), and FTO electro-conductive glass immerses in NaOH solution
Time is 0.8-1.2h.
Preferably, annealing condition is the 300-400 DEG C of heat preservation 1.5-2h under argon atmosphere in step (3).
Preferably, the zinc oxide nano rod obtained in step (2) is perpendicular to FTO electro-conductive glass, and the length of nanometer rods
Degree can be controlled by the aqua-solution method reaction time.
Preferably, the nickel oxide nano pipe obtained in step (3) can be used as electrochromic material, in nickel oxide nano pipe
Nickel oxide be hollow tubular and perpendicular to FTO electro-conductive glass, nickel oxide nano pipe is made of uniform nickel oxide nano piece,
The thickness of nickel oxide nano piece is less than 5nm, width 18-22nm.
The beneficial effects of the present invention are：
1, the chemistry such as raw material such as zinc nitrate, zinc acetate, nickel sulfate, hexa and ammonium hydroxide that the present invention uses examination
Agent, it is of low cost, resource is extensive；
2, the present invention is synthesized using solwution method with chemical bath deposition, and reaction condition will not destroy conductive substrates, reaction product
It is contacted with substrate tightly；Pattern is controlled by regulating and controlling solwution method reaction with the chemical bath deposition time, easy to operate, process can
Control.
3, it is suitble in the substrate for being deposited on different complicated shapes from the method for this wet-chemical of chemical bath using solwution method, and
Product morphology and size uniform；
4, product morphology of the invention is orderly, the hollow nanotube be made of tiny nickel oxide nano piece and traditional densification
Structure, which is compared, possesses the specific surface area of bigger, conducive to coming into full contact with for electrolyte and active material, improves nickel oxide as electroluminescent
The discoloration response speed and visible optical modulation amplitude of off-color material.
Description of the drawings
Fig. 1 is scanning electron microscope (SEM) photograph of the zinc oxide nano rod (ZnO) of embodiment 1 under different amplification；
Fig. 2 is scanning electron microscope (SEM) photograph of the nickel oxide nano pipe (NiO) of embodiment 1 under different amplification, and nickel oxide is received
The diameter of mitron is in 100nm or so；
Fig. 3 is the section surface sweeping electron microscope of the nickel oxide nano pipe of embodiment 1, and the length of nickel oxide nano pipe is about
800nm, and nanotube is to be in close contact with conductive substrates；
Fig. 4 is the transmission electron micrograph of the nickel oxide nano pipe (NiO) of embodiment 1, tiny nickel oxide nano piece
Thickness in 5nm hereinafter, width is in 20nm or so；
Fig. 5 is the XRD diagram of the nickel oxide nano pipe (NiO) of embodiment 1；
Fig. 6 is the electrochromic optical modulation amplitude performance map of nickel oxide nano pipe (NiO) of embodiment 1, is in wavelength
Modulation amplitude at 550nm is 72%；
Fig. 7 is the kinetics figure of nickel oxide nano pipe (NiO) electrochromic property of embodiment 1, dyeing time 5.2
Second, fading time is 5.4 seconds.
Specific implementation mode
Embodiment 1：
FTO electro-conductive glass is sequentially placed into acetone, ethyl alcohol, alcohol first and is cleaned by ultrasonic 15min, then uses 30mM's
Zinc acetate/ethyl alcohol (Zn (Ac)2/C2H5OH) solution is spun on for 500 revolutions per seconds on electro-conductive glass in rotating speed, is subsequently placed at Muffle furnace
In 400 DEG C of annealing, obtain the electro-conductive glass with zinc oxide seed layer；Electro-conductive glass with zinc oxide seed layer is placed in
20mM methenamines (C6H12N4, 99.5%) and 20mM zinc nitrates (Zn (NO3)2·6H2O, 99.5%) in aqueous solution, 75-85
Hydro-thermal 1-2 hours under the conditions of DEG C, entire reaction carries out in Petri dish, obtains the conductive glass of zinc oxide nano rod load
Glass；4g six hydration nickel sulfates (NiSO4·6H2O, 99%), 0.8g potassium peroxydisulfates (K2S2O8, 99.5%) and it is dissolved in 40mL deionized waters
(18.25MΩ·cm-3) in, there is the electro-conductive glass of zinc oxide nano rod to be placed in solution load, ammonium hydroxide is added at room temperature
(NH3H2O, 25%~28%) and continue at the uniform velocity to stir, chemical bath deposition 2min, a large amount of water flushings are placed on 1-2M
0.8-1.2 hours in sodium hydroxide (NaOH 99.54%) solution, it is therefore an objective to erode the zinc oxide nano rod as template, stay
The nickel oxide of lower hollow shape, last a large amount of water are dried after rinsing and anneal 2 in 300-400 DEG C under argon atmosphere in tube furnace
Hour, the middle empty nanotube being made of nickel oxide nano piece is obtained, and nanotube is perpendicular to substrate.Had using Hitachi, Japan
Limit company SU8020 scanning electron microscopic observation samples, zinc oxide nano rod and empty nanotube pattern in nickel oxide are as shown in Figure 1, 2, 3.
Gained sample is analyzed using Dutch Panaco D/max-2500 types X-ray diffraction analysis instrument, acquired results are as shown in Figure 4.Oxidation
The electrochromic property of nickel film is tested using Shimadzu UV-3600 optics protractors, optical modulation and optical modulation kinetics
It can as shown in Figure 5,6, wherein the optical contrast in wavelength 550nm is 72%；In terms of dynamics, fading time is 5.4 seconds,
The color time is 5.2 seconds.
Claims (10)
1. a kind of preparation method of nickel oxide nano pipe, it is characterised in that：Include the following steps：
(1) Zinc diacetate dihydrate is dissolved in alcohol, ultrasonic disperse obtains solution I；By zinc nitrate hexahydrate and hexa
It is dissolved in ultra-pure water and obtains solution II；Six hydration nickel sulfate and potassium peroxydisulfate are dissolved in ultra-pure water, ultrasonic disperse obtains solution
III；
(2) solution I is spun on FTO electro-conductive glass, the FTO electro-conductive glass that spin coating finishes is placed in Muffle furnace and is annealed
Processing；FTO electro-conductive glass after annealing is put into solution II progress hydro-thermal reaction and stirs to get zinc oxide nano rod；
(3) the FTO electro-conductive glass of zinc oxide nano rod is placed in solution III load, electromagnetic agitation, and ammonium hydroxide progress is added
Chemical bath deposition；FTO electro-conductive glass is then taken out, is immersed in NaOH solution after being rinsed with water and obtains the nickel oxide of hollow shape；It will
The nickel oxide of hollow shape, which is put into after being rinsed with water in tube furnace, to be carried out making annealing treatment under argon atmosphere up to nickel oxide nano pipe.
2. a kind of preparation method of nickel oxide nano pipe according to claim 1, it is characterised in that：Solution I in step (1)
Middle a concentration of 30-50mM of zinc acetate；A concentration of 20-30mM of zinc nitrate in solution II, mole of zinc nitrate and hexa
Than being 1：1；Concentration of nickel sulfate is 0.1M-0.12M in solution III, and the molar ratio of nickel sulfate and potassium peroxydisulfate is 5:1.
3. a kind of preparation method of nickel oxide nano pipe according to claim 1, it is characterised in that：Spin coating in step (2)
When rotating speed be 500-1000 circles/second, spin-coating time 1-2min.
4. a kind of preparation method of nickel oxide nano pipe according to claim 1, it is characterised in that：Annealing in step (2)
Temperature is 350-420 DEG C, annealing time 25-35min.
5. a kind of preparation method of nickel oxide nano pipe according to claim 1, it is characterised in that：Hydro-thermal in step (2)
The condition of reaction is that 1-2h is carried out at 75-85 DEG C.
6. a kind of preparation method of nickel oxide nano pipe according to claim 1, it is characterised in that：It is chemical in step (3)
Bath sedimentation time is 1-2min.
7. a kind of preparation method of nickel oxide nano pipe according to claim 1, it is characterised in that：NaOH in step (3)
NaOH concentration is 1-2M in solution, and the time that FTO electro-conductive glass immerses in NaOH solution is 0.8-1.2h.
8. a kind of preparation method of nickel oxide nano pipe according to claim 1, it is characterised in that：Annealing in step (3)
Treatment conditions are the 300-400 DEG C of heat preservation 1.5-2h under argon atmosphere.
9. a kind of preparation method of nickel oxide nano pipe according to claim 1, it is characterised in that：Step obtains in (2)
Zinc oxide nano rod be perpendicular to FTO electro-conductive glass, and the length of nanometer rods can be controlled by the aqua-solution method reaction time
System.
10. a kind of preparation method of nickel oxide nano pipe according to claim 1, it is characterised in that：Step obtains in (3)
Nickel oxide nano pipe can be used as electrochromic material, the nickel oxide in nickel oxide nano pipe be hollow tubular and perpendicular to
FTO electro-conductive glass, nickel oxide nano pipe are made of uniform nickel oxide nano piece, and the thickness of nickel oxide nano piece is less than 5nm,
Width is 18-22nm.
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Cited By (5)
| 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 |
| CN110729137A (en) * | 2019-10-23 | 2020-01-24 | 湖北大学 | Foamed nickel self-supporting nickel nanotube supercapacitor electrode material and preparation method thereof |
| CN112992551A (en) * | 2021-03-17 | 2021-06-18 | 华南理工大学 | Self-charging super capacitor and preparation method thereof |
| CN113026072A (en) * | 2019-12-25 | 2021-06-25 | 南京理工大学 | Method for preparing metal oxide nanotube array by combining template and pulse method |
| CN113433171A (en) * | 2021-06-24 | 2021-09-24 | 兰州大学 | Gas-sensitive material, gas-sensitive sensor, and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102583504A (en) * | 2012-01-18 | 2012-07-18 | 山东大学 | Method for preparation and regulation of surface-roughness ZnO nano-cone or nanorod array |
| CN102616730A (en) * | 2011-02-01 | 2012-08-01 | 成功大学 | Manufacturing method of hollow nanotube structure |
-
2018
- 2018-07-06 CN CN201810736675.0A patent/CN108545961A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102616730A (en) * | 2011-02-01 | 2012-08-01 | 成功大学 | Manufacturing method of hollow nanotube structure |
| CN102583504A (en) * | 2012-01-18 | 2012-07-18 | 山东大学 | Method for preparation and regulation of surface-roughness ZnO nano-cone or nanorod array |
Cited By (6)
| 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 |
| CN110729137A (en) * | 2019-10-23 | 2020-01-24 | 湖北大学 | Foamed nickel self-supporting nickel nanotube supercapacitor electrode material and preparation method thereof |
| CN113026072A (en) * | 2019-12-25 | 2021-06-25 | 南京理工大学 | Method for preparing metal oxide nanotube array by combining template and pulse method |
| CN113026072B (en) * | 2019-12-25 | 2022-12-13 | 南京理工大学 | Method for preparing metal oxide nanotube array by combining template and pulse method |
| CN112992551A (en) * | 2021-03-17 | 2021-06-18 | 华南理工大学 | Self-charging super capacitor and preparation method thereof |
| CN113433171A (en) * | 2021-06-24 | 2021-09-24 | 兰州大学 | Gas-sensitive material, gas-sensitive sensor, and preparation method and application thereof |
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