CN103172273B - A kind of hydro-thermal method prepares the method for electro-allochromatic nickel oxide film - Google Patents
A kind of hydro-thermal method prepares the method for electro-allochromatic nickel oxide film Download PDFInfo
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- CN103172273B CN103172273B CN201310128228.4A CN201310128228A CN103172273B CN 103172273 B CN103172273 B CN 103172273B CN 201310128228 A CN201310128228 A CN 201310128228A CN 103172273 B CN103172273 B CN 103172273B
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- 229910000480 nickel oxide Inorganic materials 0.000 title claims abstract description 46
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 238000001027 hydrothermal synthesis Methods 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 48
- 239000011521 glass Substances 0.000 claims abstract description 37
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims abstract description 27
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000000243 solution Substances 0.000 claims abstract description 19
- 239000013078 crystal Substances 0.000 claims abstract description 18
- SPIFDSWFDKNERT-UHFFFAOYSA-N nickel;hydrate Chemical compound O.[Ni] SPIFDSWFDKNERT-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000004202 carbamide Substances 0.000 claims abstract description 10
- 235000013877 carbamide Nutrition 0.000 claims abstract description 10
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 7
- 239000011259 mixed solution Substances 0.000 claims abstract description 7
- 239000002904 solvent Substances 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 239000002086 nanomaterial Substances 0.000 claims description 14
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 8
- 238000001354 calcination Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 239000002070 nanowire Substances 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 2
- 239000002135 nanosheet Substances 0.000 claims description 2
- 239000010408 film Substances 0.000 abstract description 26
- 238000002360 preparation method Methods 0.000 abstract description 20
- 239000010409 thin film Substances 0.000 abstract description 17
- 239000000758 substrate Substances 0.000 abstract description 8
- 230000000873 masking effect Effects 0.000 abstract description 4
- 239000012467 final product Substances 0.000 abstract 1
- 239000012528 membrane Substances 0.000 description 10
- 230000008859 change Effects 0.000 description 9
- 239000000463 material Substances 0.000 description 8
- 229940078494 nickel acetate Drugs 0.000 description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 description 4
- 238000002834 transmittance Methods 0.000 description 4
- 238000004506 ultrasonic cleaning Methods 0.000 description 4
- 238000001291 vacuum drying Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- 230000004044 response Effects 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 230000002441 reversible effect Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 230000018199 S phase Effects 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000005562 fading Methods 0.000 description 1
- 239000005357 flat glass Substances 0.000 description 1
- MHCFAGZWMAWTNR-UHFFFAOYSA-M lithium perchlorate Chemical compound [Li+].[O-]Cl(=O)(=O)=O MHCFAGZWMAWTNR-UHFFFAOYSA-M 0.000 description 1
- 229910001486 lithium perchlorate Inorganic materials 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 238000004549 pulsed laser deposition Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 239000004984 smart glass Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
Abstract
The present invention relates to a kind of method that hydro-thermal method prepares electro-allochromatic nickel oxide film, including: four water nickel acetates are dissolved in the mixed solution of ethanol and n-butyl alcohol, drip ammonia after dissolving, obtain colloidal sol；Above-mentioned colloidal sol is spun on FTO conductive glass surface, is dried, obtains the FTO electro-conductive glass with crystal seed layer；Four water nickel acetates, carbamide and solvent mixing, obtain reaction solution, is then immersed in reaction solution by the above-mentioned FTO electro-conductive glass with crystal seed layer, carries out hydro-thermal reaction, under the conditions of 160 180 DEG C, keep 6 12h, be cooled to room temperature, clean, dry, calcine, to obtain final product.The preparation method of the present invention is simple, and low cost has the industry application possibility in glass surface masking；The nanostructured nickel oxide film of the present invention is the surface being grown directly upon FTO electro-conductive glass by hydro-thermal method, and nickel oxide and substrate have preferable adhesion, beneficially electronics conduction, also improve the electrochemical stability of thin film simultaneously.
Description
Technical field
The invention belongs to the preparation field of electrochomeric films, prepare electro-allochromatic nickel oxide particularly to a kind of hydro-thermal method
The method of thin film.
Background technology
Electrochromism refers to that material produces under electric field action and stablizes reversible change phenomenon.When material is in electrochemical action
The injection of lower generation electronics and ion and extraction so that it is valence state and chemical constituent change so that the reflection of material with thoroughly
Penetrate performance change, it is achieved the selectivity of heat radiation and visible ray passes through or reflection to external world, also can stop internal energy (such as heat)
Diffusion so that the facility such as building, the vehicles keeps nice and cool in summer and keeps winter warm, reduce a large amount of of the energy
Consume.Therefore, electrochomeric glass or device can be widely applied to each side such as building, space flight, traffic, for energy-conservation,
The aspects such as environmental protection are significant.
Electrochromic material generally can be divided into anodic coloration and cathodic coloration two class.NiO is that great representational anode causes
The electrochromic material of color, the adjustable extent of NiO film transmission rate is mainly in visible region, and adjustable extent is relatively big, has stable
Electrochromic property and long service life, and can and WO3Use Deng negative electrode coloring material fit, form complementary electroluminescent
Electrochromic device, is the focus of current electrochromic material research.The most frequently used preparation method of NiO electrochomeric films have sputtering,
Vacuum evaporation, pulsed laser deposition, sol-gel technique, chemistry and electrochemical deposition etc..But said method or depend on multiple
Miscellaneous equipment and Technology, it is difficult to prepare large area uniform NiO thin film；Or prepare thin film weak with the adhesion of substrate,
Cyclical stability is poor, it is difficult to meet practical application request.The hydro-thermal method using crystal seed auxiliary is directly raw in electro-conductive glass substrate
The electro-allochromatic nickel oxide film of long nanostructured is possible not only to improve the adhesion between thin film and substrate, and can pass through
Regulation hydrothermal process parameter realizes the controlled preparation to nickel oxide microstructure, and the method preparation technology is simple, and low cost has
At the industry application possibility of glass surface masking, it is expected to break through the technical bottleneck of existing electrochomeric films material, in solution
State the problem mentioned, lay a solid foundation for realizing the extensive industrialization of electrochomeric glass.
Summary of the invention
The technical problem to be solved is to provide a kind of method that hydro-thermal method prepares electro-allochromatic nickel oxide film,
The method preparation method is simple, and low cost has the industry application possibility in glass surface masking；The present invention is auxiliary by crystal seed
The hydro-thermal method helped achieves the controlled preparation in conductive substrates of nickel oxide nano structural membrane, and by regulation hydrothermal process parameter
Achieve the regulation and control to film surface appearance, thus be effectively improved the response speed of thin film, coloration efficiency；The present invention receives
Rice structure nickel oxide film is the surface being grown directly upon FTO electro-conductive glass by hydro-thermal method, and nickel oxide and substrate have preferably
Adhesion, beneficially electronics conduction, also improve the electrochemical stability of thin film simultaneously.
The method that a kind of hydro-thermal method of the present invention prepares electro-allochromatic nickel oxide film, including:
(1) four water nickel acetates are dissolved in the mixed solution of ethanol and n-butyl alcohol, drip ammonia after dissolving, obtain colloidal sol；
Wherein the mol ratio of four water nickel acetates and ammonia is 1:1；
(2) above-mentioned colloidal sol is spun on FTO conductive glass surface, is dried, obtains the FTO electro-conductive glass with crystal seed layer；
(3) four water nickel acetates, carbamide and solvent mixing, obtain reaction solution, is then conducted electricity by the above-mentioned FTO with crystal seed layer
Glass immerses in reaction solution, carries out hydro-thermal reaction, under the conditions of 160-180 DEG C, keeps 6-12h, is cooled to room temperature, clean,
Drying, calcine, obtain nickel oxide nano structure electrochomeric films, wherein the mol ratio of four water nickel acetates and carbamide is 1:2.1-
4.2。
In described step (1), the concentration of four water nickel acetates is 0.2～0.4mol/L, and ammonia concn used is 14.8mol/L
(supplementing).
N-butyl alcohol and the volume ratio of ethanol in described step (1) are 1:2-5.
In described step (2), FTO electro-conductive glass is through supersound washing.
Described supersound washing is to wash through deionized water, acetone and EtOH Sonicate successively, and the supersound washing time is 20～30
Minute.
Being dried in described step (2) as being vacuum dried, baking temperature is 40-60 DEG C, and drying time is 6-12h.
In described step (3), the concentration of four water nickel acetates is 0.02～0.04mol/L, and solvent is water, ethanol or volume ratio
Water and alcohol mixeding liquid for 1:1.
In described step (3), hydro-thermal reaction is carried out in a kettle., and reaction solution amount accounts for the 80% of reactor volume.
In described step (3), calcining heat is 400-600 DEG C, and calcination time is 2-6h.
Described step (3) nickel oxide nano structure is nano wire, nanometer sheet or nano-sheet floral structure.
In the present invention, first by crystal seed assisting alcohol-hydrothermal method growth predecessor Ni (OH) on cleaned FTO sheet glass2
Nano structure membrane, then obtains NiO nano structure membrane by calcining.By regulation reaction solution in carbamide addition with
And the composition of solvent, it is possible to achieve the controlled preparation of nickel oxide nano structure.
The nickel oxide nano structural membrane of the present invention has bigger specific surface area, and the hole between nanostructured has been
Full-open, can reduce ion and electronics injects/extract out the path of electrode material, shorten ion and electronics at electrode material
Internal migration time.Therefore, the NiO nanostructured electrochomeric films of the present invention has that color change is fast, coloration efficiency is high
The advantage such as excellent with cyclical stability, can be assembled into all kinds of electrochromic device, have in the field such as smart window, large screen display
It is widely applied prospect.
Beneficial effect
(1) preparation method of the present invention is simple, and low cost has the industry application possibility in glass surface masking；
(2) present invention by the hydro-thermal method that crystal seed assists achieve nickel oxide nano structural membrane in conductive substrates controlled
Preparation, and achieve the regulation and control to film surface appearance by regulation hydrothermal process parameter, thus it is effectively improved thin film
Response speed, coloration efficiency；
(3) the nanostructured nickel oxide film of the present invention is the surface being grown directly upon FTO electro-conductive glass by hydro-thermal method,
Nickel oxide and substrate have preferable adhesion, beneficially electronics conduction, also improve the electrochemical stability of thin film simultaneously.
Accompanying drawing explanation
The X-ray diffractogram of the nickel oxide nano structure electrochomeric films of Fig. 1 embodiment 1 preparation；
The stereoscan photograph of the nickel oxide nano structure electrochomeric films of Fig. 2 embodiment 1 preparation；
The stereoscan photograph of the nickel oxide nano structure electrochomeric films of Fig. 3 embodiment 2 preparation；
The stereoscan photograph of the nickel oxide nano structure electrochomeric films of Fig. 4 embodiment 3 preparation；
The stereoscan photograph of the nickel oxide nano structure electrochomeric films of Fig. 5 embodiment 4 preparation.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is expanded on further.Should be understood that these embodiments are merely to illustrate the present invention
Rather than restriction the scope of the present invention.In addition, it is to be understood that after having read the content that the present invention lectures, people in the art
The present invention can be made various changes or modifications by member, and these equivalent form of values fall within the application appended claims equally and limited
Scope.
Embodiment 1
FTO electro-conductive glass is immersed successively respective supersound washing post-drying in deionized water, acetone and ethanol standby.Weigh
0.45g tetra-water nickel acetate is dissolved in the mixed solution of 6mL ethanol and 3mL n-butyl alcohol, drips after four water nickel acetates are completely dissolved
0.12mL strong aqua ammonia obtains vitreosol；Then vitreosol is spun on the FTO conductive glass surface of ultrasonic cleaning, 40
At DEG C, vacuum drying obtains nickel hydroxide crystal seed layer in 12 hours.Preparation is containing 0.6g tetra-water nickel acetate, 0.6g carbamide, 56mL water
Reaction solution, then invades the FTO electro-conductive glass with crystal seed layer obtained above in the water heating kettle filling reaction solution, in
180 DEG C are incubated 6 hours, finally naturally cool to room temperature, take out FTO electro-conductive glass, after cleaning successively with water and ethanol, dry,
Calcine 3 hours at 500 DEG C.
Fig. 1 is the X-ray diffractogram of obtained thin film, and reference standard X ray diffracting spectrum is it can be seen that this thin film is vertical
The nickel oxide of side's phase is corresponding with standard card JCPDS 04-0835.Fig. 2 is the stereoscan photograph of obtained nickel oxide film,
Can be seen that this thin film is made up of NiO nanowire network structure.
Embodiment 2
FTO electro-conductive glass is immersed successively respective supersound washing post-drying in deionized water, acetone and ethanol standby.Weigh
0.9g tetra-water nickel acetate is dissolved in the mixed solution of 7.5mL ethanol and 2.5mL n-butyl alcohol, drips after four water nickel acetates are completely dissolved
Add 0.24mL strong aqua ammonia and obtain vitreosol；Then vitreosol is spun on the FTO conductive glass surface of ultrasonic cleaning,
At 60 DEG C, vacuum drying obtains nickel hydroxide crystal seed layer in 6 hours.Preparation is containing 0.6g tetra-water nickel acetate, 0.3g carbamide, 56mL water
Reaction solution, then the FTO electro-conductive glass with crystal seed layer obtained above is invaded in the water heating kettle filling reaction solution,
It is incubated 12 hours in 160 DEG C, finally naturally cools to room temperature, take out FTO electro-conductive glass, clean successively with water and ethanol, dry
After, calcine 6 hours at 400 DEG C.
Fig. 3 is the stereoscan photograph of obtained nickel oxide film, it can be seen that this thin film is by NiO nanowire group
Become.
Embodiment 3
FTO electro-conductive glass is immersed successively respective supersound washing post-drying in deionized water, acetone and ethanol standby.Weigh
0.6g tetra-water nickel acetate is dissolved in the mixed solution of 7mL ethanol and 2mL n-butyl alcohol, drips after four water nickel acetates are completely dissolved
0.16mL strong aqua ammonia obtains vitreosol；Then vitreosol is spun on the FTO conductive glass surface of ultrasonic cleaning, 50
At DEG C, vacuum drying obtains nickel hydroxide crystal seed layer in 8 hours.Preparation is containing 0.3g tetra-water nickel acetate, 0.3g carbamide, 56mL ethanol
Reaction solution, then the FTO electro-conductive glass with crystal seed layer obtained above is invaded in the water heating kettle filling reaction solution,
It is incubated 8 hours in 170 DEG C, finally naturally cools to room temperature, take out FTO electro-conductive glass, clean successively with water and ethanol, dry
After, calcine 2 hours at 600 DEG C.
Fig. 4 is the stereoscan photograph of obtained nickel oxide film, it can be seen that this thin film is by NiO nanometer sheet group
Becoming, these nanometer sheet define the structure of a porous, and this structure not only increases the specific surface area active of electrochemical reaction,
And beneficially ion and the injection/extraction of electronics.
Embodiment 4
FTO electro-conductive glass is immersed successively respective supersound washing post-drying in deionized water, acetone and ethanol standby.Weigh
0.6g tetra-water nickel acetate is dissolved in the mixed solution of 7mL ethanol and 2mL n-butyl alcohol, drips after four water nickel acetates are completely dissolved
0.16mL strong aqua ammonia obtains vitreosol；Then vitreosol is spun on the FTO conductive glass surface of ultrasonic cleaning, 50
At DEG C, vacuum drying obtains nickel hydroxide crystal seed layer in 8 hours.Preparation is containing 0.3g tetra-water nickel acetate, 0.3g carbamide, 28mL ethanol
With the reaction solution of 28mL water, then the FTO electro-conductive glass with crystal seed layer obtained above is invaded and fill reaction solution
In water heating kettle, it is incubated 8 hours in 170 DEG C, finally naturally cools to room temperature, take out FTO electro-conductive glass, the most clear with water and ethanol
After washing, drying, calcine 2 hours at 600 DEG C.Fig. 5 is the stereoscan photograph of obtained nickel oxide film, can see
Go out the flower-like structure that the surface topography of this thin film is made up of NiO nanometer sheet.
In order to understand the electrochromic property of the nickel oxide nano structural membrane obtained by the various embodiments described above, we are with three
It is thin that electrode system combined with electrochemical work station and solid ultraviolet-uisible spectrophotometer measure prepared nickel oxide nano structure
The light transmission rate change of film and electrochromism response speed, and calculate coloration efficiency.Wherein three-electrode system is: with the oxygen of preparation
Change nickel nano structure membrane electrode as working electrode, with Ag/AgCl as reference electrode, with platinum filament for electrode, with 1mol/L
The polycarbonate solution of lithium perchlorate be electrolyte.
Result shows: when applying side's pressure of-1V and 1V, nickel oxide nano structural membrane is reversible between transparent and brown
Change；The light transmittance of this thin film has significantly change at 400～900nm wave bands, has reached maximum at λ=550nm；Cause
This, record nickel oxide nano structural membrane light transmittance changing value at λ=550nm, rings with the light transmittance at λ=550nm simultaneously
Should change to detect its electrochromic effect speed, and calculate its coloration efficiency, test and result of calculation are as shown in table 1.By with
Upper result understands, and the nickel oxide nano structural membrane obtained by embodiment 1 and embodiment 3 has good electrochromic property.
Table 1
| Thin film | Light transmittance changing value | Coloration time | Fading time | Coloration efficiency |
| Embodiment 1 | 60% | 6s | 8s | 69.6cm2/C |
| Embodiment 2 | 53% | 9s | 12s | 56.4cm2/C |
| Embodiment 3 | 66% | 4s | 8s | 73.2cm2/C |
| Embodiment 4 | 52% | 18s | 16s | 46.2cm2/C |
Claims (9)
1. the method that hydro-thermal method prepares electro-allochromatic nickel oxide film, including:
(1) four water nickel acetates are dissolved in the mixed solution of ethanol and n-butyl alcohol, drip ammonia after dissolving, obtain colloidal sol；Wherein
The mol ratio of four water nickel acetates and ammonia is 1:1；Wherein the concentration of four water nickel acetates is 0.2～0.4mol/L, and ammonia used is dense
Degree is 14.8mol/L；
(2) above-mentioned colloidal sol is spun on FTO conductive glass surface, is dried, obtains the FTO electro-conductive glass with crystal seed layer；
(3) four water nickel acetates, carbamide and solvent mixing, obtain reaction solution, then by the above-mentioned FTO electro-conductive glass with crystal seed layer
Immerse in reaction solution, carry out hydro-thermal reaction, under the conditions of 160-180 DEG C, keep 6-12h, be cooled to room temperature, clean, dry,
Calcining, obtains nickel oxide nano structure electrochomeric films, and wherein the mol ratio of four water nickel acetates and carbamide is 1:2.1-4.2；
Wherein the concentration of four water nickel acetates is 0.02～0.04mol/L.
The method that a kind of hydro-thermal method the most according to claim 1 prepares electro-allochromatic nickel oxide film, it is characterised in that: institute
The volume ratio stating the n-butyl alcohol in step (1) and ethanol is 1:2-5.
The method that a kind of hydro-thermal method the most according to claim 1 prepares electro-allochromatic nickel oxide film, it is characterised in that: institute
State in step (2) FTO electro-conductive glass through supersound washing.
The method that a kind of hydro-thermal method the most according to claim 3 prepares electro-allochromatic nickel oxide film, it is characterised in that: institute
Stating supersound washing is to wash through deionized water, acetone and EtOH Sonicate successively, and the supersound washing time is 20～30 minutes.
The method that a kind of hydro-thermal method the most according to claim 1 prepares electro-allochromatic nickel oxide film, it is characterised in that: institute
Stating and be dried in step (2) as being vacuum dried, baking temperature is 40-60 DEG C, and drying time is 6-12h.
The method that a kind of hydro-thermal method the most according to claim 1 prepares electro-allochromatic nickel oxide film, it is characterised in that: institute
State solvent in step (3) be water, ethanol or volume ratio be water and the alcohol mixeding liquid of 1:1.
The method that a kind of hydro-thermal method the most according to claim 1 prepares electro-allochromatic nickel oxide film, it is characterised in that: institute
Stating hydro-thermal reaction in step (3) to carry out in a kettle., reaction solution amount accounts for the 80% of reactor volume.
The method that a kind of hydro-thermal method the most according to claim 1 prepares electro-allochromatic nickel oxide film, it is characterised in that: institute
Stating calcining heat in step (3) and be 400-600 DEG C, calcination time is 2-6h.
The method that a kind of hydro-thermal method the most according to claim 1 prepares electro-allochromatic nickel oxide film, it is characterised in that: institute
Stating step (3) nickel oxide nano structure is nano wire, nanometer sheet or nano-sheet floral structure.
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| CN110987822B (en) * | 2019-11-19 | 2022-07-05 | 广西大学 | Method for detecting volatile organic compound |
| CN112062170B (en) * | 2020-09-09 | 2021-09-21 | 中国海洋大学 | Hydrothermal preparation method of nickel oxide electrochromic film with graded porous morphology and structure |
| CN114477789B (en) * | 2022-02-11 | 2022-11-22 | 中国海洋大学 | Solvothermal preparation method of titanium-doped nickel oxide electrochromic film |
| CN114933420A (en) * | 2022-05-31 | 2022-08-23 | 中国人民解放军火箭军工程大学 | Gradient temperature-based hydrothermal preparation method of multilayer nano-sheet NiO electrochromic film |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1224700A (en) * | 1998-12-31 | 1999-08-04 | 冶金工业部钢铁研究总院 | Preparation of electro-allochromatic nickel oxide film |
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2013
- 2013-04-12 CN CN201310128228.4A patent/CN103172273B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1224700A (en) * | 1998-12-31 | 1999-08-04 | 冶金工业部钢铁研究总院 | Preparation of electro-allochromatic nickel oxide film |
Non-Patent Citations (1)
| Title |
|---|
| "Hierarchical NiO microflake films with high coloration efficiency, cyclic stability and low power consumption for applications in a complementary electrochromic device";Dongyun Ma et al.;《Nanoscale》;20130328;第5卷;第4808-4815页 * |
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