CN106590618A - Coated-structure NiO/rGO composite thin film and preparation method thereof - Google Patents
Coated-structure NiO/rGO composite thin film and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a coated-structure NiO/rGO composite thin film, which includes a substrate and a NiO/rGO composite film layer coating the substrate. In the NiO/rGO composite film layer, the surface of metal nickel is uniformly coated by a NiO layer, so that the NiO, as well as the metal nickel, is adhered to the graphene layer together. The invention also discloses a preparation method of the coated-structure NiO/rGO composite thin film. The method includes the steps of: (1) uniformly mixing nonionic water-soluble high-molecular polymer, graphene oxide and a solvent, adding the mixture to a nickel salt precursor liquid, and stirring the mixture uniformly to produce a nickel precursor solution; (2) adding ammonia water to the nickel precursor solution to produce nickel sol; (3) coating the substrate with the nickel sol and drying the sol to form the NiO/rGO composite thin film. The NiO/rGO composite thin film has the specificities that graphene has high electronic conductivity and large specific surface area. Compared with a NiO composite thin film in the prior art, the NiO/rGO composite thin film has higher response speed and has better industrial development prospect.
Description
Technical field
The present invention relates to electrochromism energy-conservation laminated film field, and in particular to a kind of NiO/rGO with clad structure
Laminated film and preparation method thereof.
Background technology
The research of electrochromic effect will trace back to Deb in 1966 to amorphous state WO3The preparation of thin film, learns both at home and abroad since then
Person has carried out deeply extensive research around electrochomeric films and its application.At present, electrochromic material is considered as most have
One of intellectual material of application prospect, is widely studied for the anti-glazing on smart windows, Variable reflectance device such as automobile and truck
Light rearview mirror, display screen and variable emissivity thermal suite etc..
In numerous electrochromic materials, the WO of negative electrode coloring3It is well studied, part achievement is in practical device
Applied on part.And nickel oxide is used as excellent anode coloring material, because of its good circulation discoloration life-span, big coloring/
Colour killing scope, can be with WO3It is composed of complementary type full-solid electrochromic device of great interest.In recent years, perhaps
Many scholars are dissolved into Graphene in the research of nano compound film.Graphene is that carbon atom is tightly packed into monolayer bi-dimensional cellular
A kind of carbonaceous new material of shape lattice structure, its electron mobility is up to 1.5 × 104cm2/ (Vs), with excellent electric conductivity.
Also, Graphene has enrichment to metal ion because of its high-specific surface area, and have good cycle performance and quickly fill/
Discharge characteristicses.Therefore, nickel oxide and Graphene can be prepared into the excellent thin film of electrochromic property as composite.
Research shows that preparing electrochomeric films can adopt chemical vapor deposition, radio-frequency sputtering, sol-gel, electrification
The methods such as deposition and thermal evaporation are learned, wherein sol-gel process (Sol-gel method) is generally used containing high chemical active ingredient
Compound makees presoma (such as metal organic alkoxide), is hydrolyzed, is condensed chemical reaction, forms stable transparent molten in the solution
Colloid, imposes on the substrate surface after cleaned process, finally certain by dip coating, spin coating or spraying process afterwards
At a temperature of heat treatment be obtained metal-oxide film.The method easily controls the stoichiometric proportion and knot of thin film than additive method
Structure, requires base shape and can prepare large-area film, low cost with short production cycle is controlled easily in combination with additive method very low
The structure and performance of system and regulation thin film, is more suitable for preparing the electrochromic layer in electrochromic device, therefore becomes preparation
The important method of thin-film material.
The content of the invention
It is an object of the invention to provide it is a kind of it is with low cost, simple to operate, be easy to industrialization large area production have
NiO/rGO laminated films of clad structure and preparation method thereof.
Concrete technical scheme of the present invention is as follows：
A kind of NiO/rGO laminated films with clad structure, described NiO/rGO laminated films include substrate and painting
Overlay on the NiO/rGO composite films on substrate；
In described NiO/rGO composite films, metal nickel surface uniformly wraps up layer of Ni O, and the two is attached to jointly
On graphene layer.
A kind of preparation method of the NiO/rGO laminated films with clad structure, comprises the following steps：
Step (1)：By polyethylene glycol oxide (PEO), graphene oxide and solvent mix homogeneously, it is added to nickel salt precursor liquid and stirs
Even prepared nickel precursor solution；
Described nickel salt precursor liquid can be nickel acetate, nickel nitrate or Nickel dichloride., further preferably using nickel acetate, acetic acid
Can decompose, it is to avoid using the nitrate anion and the chloride ion that are difficult to decompose.
Step (2)：Simultaneously condensing reflux is changed into transparent equal to Deca ammonia up to solution from emerald green in nickel precursor solution
Even blue nickel sol, using condensation reflux unit as colloidal sol main body generating meanss, and is carried out under condition of water bath heating；
Step (3)：Nickel sol obtained in step (2) is coated on substrate using spin coating or czochralski method, is dried to obtain dry
Film；
Step (4)：" double annealing " heat treatment mode that the dry film is combined using vacuum annealing and air anneal, is obtained
NiO/rGO laminated films.
In the present invention, nickel sol is set uniformly to be coated on substrate by colloidal sol-gel spin-coating method, then in vacuum bar
Heat treatment is carried out under part makes the organic moiety in nickel sol or carbonization, and heat treatment removes carbon residue in air, and preparation is provided
There are the NiO/rGO compound electrochromic membranes of nanometer clad structure, the shortcoming of bad dispersibility when overcoming doped graphene is improved
The performances such as electrical conductivity, the chemical stability of electrochomeric films.Metal nickel surface is uniformly wrapped up in obtained membrane structure
Layer of Ni O, the two is attached on graphene layer jointly, and the flexibility and electric conductivity of Graphene can effectively buffer colourshifting process
In stereomutation, stress is reduced, while the also problem of effective active substance aggregation.Preparation method of the present invention is simple, easily
On various substrates of different shapes film forming, few materials, low cost, be suitable for industrialized production.
In step (1), nonionic water soluble polymer is added in solvent, stirring and dissolving uniformly obtains solution A；Will
Graphene oxide ultrasonic disperse in a solvent, obtains solution B；Nickel acetate is added in solvent, stirring and dissolving uniformly obtains molten
Liquid C；After by solution A, B mix homogeneously, in being added to solution C, prepared nickel precursor solution is stirred evenly；
The concentration range of the nickel precursor solution is the mol ratio model of 0.1-0.5mol/L, graphene oxide and nickel acetate
Enclose for 0-5%, graphene oxide is related to its dispersibility, when graphene oxide exceeds 5% in the present invention, it is difficult to be uniformly dispersed.
Preferably, in step (1), the solvent that solution A, B, C choose is the same.Described solvent is ethanol and n-butyl alcohol.
Further preferably, ethanol and n-butyl alcohol volume ratio are 2 in described solvent:1.
In the nickel precursor solution, the non-ionic water-soluble macromolecule of the inventory can be by bonding action and oxygen
Change the crosslinking of nickel network structure, its presence can to a certain extent improve the stability of colloidal sol, while also increasing colloidal sol
Viscosity.Preferably, described non-ionic water-soluble macromolecule be polyvinylpyrrolidone (PVP), Polyethylene Glycol (PEG) or
Polyethylene glycol oxide (PEO), more preferably polyethylene glycol oxide (PEO), be improve colloidal sol stability, the concentration range of PEO
It is between 2%-5%.
In step (2), after the completion of the configuration of nickel precursor solution, ammonia is added in solution, the presence of ammonia is except can be with
H necessary to hydrolysis of alkoxide is provided2O, NH therein3The speed for reducing hydrolysis of alkoxide and polycondensation reaction can be coordinated with nickel again, from
And improve the stability of colloidal sol.
Test finds that adding the mass fraction W of ammonia should be strict controlled between 2%-6%, and water can cause very little alcohol
Not exclusively, film-forming type can be poor for salt hydrolysiss, and water is too many to cause sol surface tension force to increase again, and colloidal sol becomes with the wellability of substrate
Difference, film forming is uneven.Preferably, colloidal sol has higher stability as PH=10, it is calculated, it is molten per 100ml presomas
The dosage of 3.5ml ammonia is 3.5ml in liquid.
Step (3) process is carried out after the completion of step (2) process, obtained nickel sol is coated on substrate, preferably,
Described substrate is ito glass or FTO glass.
Substrate needs to be cleaned before coating nickel sol, is favorably improved coating effect of the nickel sol on substrate, improves
The performance of laminated film.Concrete cleaning is as follows：In acetone ito glass is cleaned by ultrasonic into 30min, deionized water rinsing 3
Ultrasound 30min in deionized water is put into after secondary, then ultrasonic 30min operations are carried out in ethanol after deionized water rinses 3 times, to fill
Divide oils and fatss, dust of clean ito glass surface attachment etc..
Nickel sol is coated into method to substrate a lot, in the present invention, nickel sol is coated in by substrate using spin-coating method
On, it is the uniformity for ensureing film thickness and film forming, spin coating rotating speed should be controlled in 500-3000r/min, spin-coating time scope 2-
60sec；It is spun slow, coating can be caused uneven；Spin coating is too fast, can cause coated thin；Before this spin coating rotating speed is the present invention
500r/min spin coating time 9s, are then spin coated onto rotating speed 2000r/min spin coating time 20s.The obtained NiO/ under the spincoating conditions
The thickness of rGO laminated films is moderate, and uniformity of film is good.
After the completion of nickel sol coating, drying carrying out precipitation treatment is obtained dry film；Preferably, the temperature for being dried precipitation is 80
DEG C, drying time is 20min.
Xerogel thin film obtained in step (3) is thermally treated, will remove after organic carbon in thin film, and graphene oxide is also
Original is obtained described NiO/rGO laminated films into Graphene.Preferably, the vacuum of step (4) is 10-4-10-5Pa；Very
The temperature range annealed in empty and air is 250-500 DEG C.Temperature is less than 250 DEG C, and Organic substance is unable to carbonization, has a large amount of
Organic substance residues, affect performance, and nickel oxide is presented amorphous state；Temperature is too high, and ITO substrate resistance can increase, and be unfavorable for optics
Performance.
There is very big optical modulation scope by NiO/rGO laminated films obtained in the inventive method；And preparation method
Simply, easily on various substrates of different shapes film forming, few materials, low cost, be suitable for industrialized production.It is prepared by the present invention
NiO/rGO laminated films combine the features such as Graphene electronic conductivity is high, and specific surface area is big, it is compound with existing NiO
Thin film is compared with faster response speed, it may have more preferable industry development prospect.
Description of the drawings
Fig. 1 is the TEM photos of NiO/rGO laminated films obtained in embodiment 1；
Fig. 2 is the SEM surface pictures of NiO/rGO laminated films obtained in embodiment 1；
Fig. 3 is the SEM cross-section photographs of NiO/rGO laminated films obtained in embodiment 1；
Fig. 4 is 300 degree of heat treatments of NiO/rGO laminated films Jing obtained in embodiment 1, after activating 50 times on an ito substrate
Transmitted spectrum.
Fig. 5 is the TEM photos of NiO/rGO laminated films obtained in embodiment 2；
Fig. 6 is the SEM surface pictures of NiO/rGO laminated films obtained in embodiment 2；
Fig. 7 is the SEM cross-section photographs of NiO/rGO laminated films obtained in embodiment 2；
Fig. 8 is 300 degree of heat treatments of NiO/rGO laminated films Jing obtained in embodiment 2, after activating 50 times on an ito substrate
Transmitted spectrum.
Specific embodiment
Following examples press the enforcement of aforesaid operations method：
Embodiment 1
The present embodiment, as substrate, carries out before coating following cleaning step using ito glass (30mm × 30mm)：Third
Ito glass is cleaned by ultrasonic after 30min → deionized water rinsing 3 times in ketone is put into ultrasonic 30min → deionization in deionized water
Carry out ultrasonic 30min → drying, standby after rinsing 3 times in water in ethanol.
Step (1)：3g PEO are added to into 25mL solvent (ethanol:N-butyl alcohol is 2:1) in, stirring and dissolving uniformly obtains molten
Liquid A；
By 35.214mg graphene oxides ultrasonic disperse in 25mL solvent (ethanol:N-butyl alcohol is 2:1) in, solution B is obtained；
The four hydration nickel acetates of 4.9738g are added to into 50ml solvent (ethanol:N-butyl alcohol is 2:1) in, stirring and dissolving is equal
It is even, obtain solution C；
After by solution A, B mix homogeneously, in being added to solution C, prepared nickel precursor solution is stirred evenly；
Step (2)：Simultaneously condensing reflux is changed into Deca 3.5mL ammonia up to solution from emerald green in nickel precursor solution
Bright uniform blue nickel sol；
Step (3)：Using spin coating instrument by nickel sol spin coating quartz base plate after cleaning；Before this spin coating rotating speed was
500r/min spin coating time 9s, are then spin coated onto rotating speed 2000r/min spin coating time 20s.After the completion of nickel sol coating, 80 DEG C of dryings
20min obtains dry film.
Step (4)：Dry film obtained in step (3) is first annealed under vacuo, annealing temperature is 300 DEG C, then in air
Middle annealing, annealing temperature is 300 DEG C, and vacuum is 10-4Pa, temperature retention time is 10min, and NiO/rGO laminated films are obtained.
As shown in figure 1, the TEM photos of the NiO/rGO laminated films for preparing show, it is brilliant that nickel oxide is evenly coated at metallic nickel
Grain surface；The SEM surface pictures of NiO/rGO laminated films are as shown in Fig. 2 its surface is grain structure of uniform size；NiO/
RGO laminated films cross-section photographs are as shown in figure 3, film thickness is 80nm；300 degree of heat treatments of thin film Jing, activation 50 times after
Transmitted spectrum on ito substrate is as shown in figure 4, transmitance changing value of the thin film at 550nm is 66.1%；Above-mentioned test result shows
Show, NiO/rGO laminated films are obtained there is preferable spectral characteristic.
Embodiment 2
Compare with embodiment 1, difference is that the graphene oxide in step (1) adds quality for 23.476mg；Other ginsengs
Number is constant, and the TEM photos (Fig. 5) of the NiO/rGO laminated films of preparation show that nickel oxide is evenly coated at metal nickel crystallite table
Face；The SEM surface pictures of the laminated film are as shown in fig. 6, its surface is grain structure of uniform size；NiO/rGO THIN COMPOSITEs
Film cross-section photographs are as shown in fig. 7, film thickness is 80nm；300 degree of heat treatments of thin film Jing, after activating 50 times on an ito substrate
Transmitted spectrum is as shown in figure 8, transmitance changing value of the thin film at 550nm is 54.1%.
The foregoing is only the preferable implementation example of the present invention, be not limited to the present invention, it is all in spirit of the invention and
Within principle, any modification, equivalent substitution and improvements made etc. should be included within the scope of the present invention.
Claims (10)
1. a kind of NiO/rGO laminated films with clad structure, it is characterised in that described NiO/rGO laminated films include
Substrate and the NiO/rGO composite films being coated on substrate；
In described NiO/rGO composite films, metal nickel surface uniformly wraps up layer of Ni O, and the two is attached to graphite jointly
On alkene layer.
2. a kind of preparation method of NiO/rGO laminated films as claimed in claim 1, it is characterised in that comprise the following steps：
1) by nonionic water soluble polymer, graphene oxide and solvent mix homogeneously, it is added to nickel salt precursor liquid and stirs evenly system
Obtain nickel precursor solution；
2) ammonia is added in nickel precursor solution, nickel sol is obtained；
3) obtained nickel sol is coated on substrate, is dried prepared NiO/rGO laminated films.
3. preparation method according to claim 2, it is characterised in that described non-ionic water-soluble macromolecule is poly- second
One kind in alkene pyrrolidone, Polyethylene Glycol and polyethylene glycol oxide.
4. preparation method according to claim 3, it is characterised in that polyethylene glycol oxide is dense in the nickel precursor solution
Degree scope is 2%～5%.
5. preparation method according to claim 4, it is characterised in that the concentration range of the nickel precursor solution is 0.1
The molar ratio range of～0.5mol/L, graphene oxide and nickel salt is 0～5%.
6. preparation method according to claim 1, it is characterised in that the mass fraction for adding ammonia is 2%-6%.
7. preparation method according to claim 5, it is characterised in that in the PH=10 of the nickel precursor solution, ammonia
The dosage of water is 3.5%.
8. preparation method according to claim 2, it is characterised in that the solvent is the mixed liquor of ethanol and n-butyl alcohol,
Wherein ethanol and n-butyl alcohol volume ratio are 2:1.
9. preparation method according to claim 2, it is characterised in that described substrate is ito glass or FTO glass, system
The nickel sol for obtaining is coated on substrate using spin coating or czochralski method.
10. preparation method according to claim 2, it is characterised in that heat treatment is carried out to dried xerogel thin film,
Including vacuum annealing and air anneal, the vacuum of vacuum annealing is 10-4-10-5The temperature model annealed in Pa, vacuum and air
Enclose for 250-500 DEG C.
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Cited By (3)
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| CN107693946A (en) * | 2017-10-25 | 2018-02-16 | 陈襄国 | A kind of moving link with health role |
| CN108574096A (en) * | 2018-05-11 | 2018-09-25 | 皖西学院 | NiO/rGO composite nano materials and preparation method thereof and lithium cell cathode material |
| CN110739155A (en) * | 2019-09-24 | 2020-01-31 | 广东工业大学 | nickel sulfide/graphene composite film and preparation method and application thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107693946A (en) * | 2017-10-25 | 2018-02-16 | 陈襄国 | A kind of moving link with health role |
| CN108574096A (en) * | 2018-05-11 | 2018-09-25 | 皖西学院 | NiO/rGO composite nano materials and preparation method thereof and lithium cell cathode material |
| CN108574096B (en) * | 2018-05-11 | 2020-06-16 | 皖西学院 | NiO/rGO composite nano material, preparation method thereof and lithium battery anode material |
| CN110739155A (en) * | 2019-09-24 | 2020-01-31 | 广东工业大学 | nickel sulfide/graphene composite film and preparation method and application thereof |
| CN110739155B (en) * | 2019-09-24 | 2021-10-19 | 广东工业大学 | Nickel sulfide/graphene composite film and preparation method and application thereof |
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