CN106219616B - A kind of molybdenum dioxide/cobalt acid nickel classification hybrid nanostructure array and preparation method thereof - Google Patents
A kind of molybdenum dioxide/cobalt acid nickel classification hybrid nanostructure array and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of using hydro-thermal method in molybdenum dioxide nano wire, nanometer sheet substrate compound cobalt acid nickel nano film array is to obtain molybdenum dioxide/cobalt acid nickel classification hybrid nanostructure array and preparation method thereof.Specific step is: (1) preparing molybdenum dioxide nano wire or molybdenum dioxide nano-chip arrays on sprayed molybdenum carbon paper with the method for chemical vapor deposition；(2) nano wire of above-mentioned preparation, nano-chip arrays are placed in the mixed solution containing cobalt nitrate, nickel nitrate, ammonium fluoride and urea, reaction is carried out using hydro-thermal reaction method under different temperature, different time, various concentration precursor solution and prepares composite precursor；(3) presoma by above-mentioned preparation is placed in tube furnace, and is made annealing treatment in air to it, to obtain molybdenum dioxide/cobalt acid nickel classification hybrid nanostructure array.Wherein the thickness of cobalt acid nickel nano film is 10-20nm.
Description
Technical field
The present invention relates to a kind of nanostructure field, and in particular to a kind of molybdenum dioxide/cobalt acid nickel classification hybrid nanostructure
Array and preparation method thereof.
Background technique
In the second eleventh century with the progress of science and technology, our modern society is faced with the energy and environmental correclation
Problem such as pollutes, the shortage and global warming of fossil fuel.In order to overcome these complication, cleaning and renewable energy source material,
And an urgent demand of their equipment.Fortunately, it is effectively improved using renewable energy such as solar energy and wind energy
In our daily life, but the disperse properties of renewable energy require high performance energy storage device.In this respect, electrochemical
Energy-storage system is learned to play a crucial role the efficient storage of solar energy and wind energy.Currently, battery and supercapacitor by
Become the most promising and successful energy storage system that can be obtained on the market in its low cost and high-performance.
Recent years, transition metal oxide receive a large amount of research due to its higher theoretical specific capacity.Molybdenum
Oxide because its valence state mutability shows a variety of special appearances, structure and property, photocatalysis, gas sensing, lithium ion battery,
Image is shown, information stores, is had important application in variable reflectivity lens and high energy efficiency smart windows etc..Titanium dioxide
Molybdenum is a typical stratiform transition group metallic oxide, it have very high theoretical capacity (838mAh/g), low cost, it is low
Resistivity and good electro-chemical activity.But the variation of volume causes cycle life is not high to limit during charge and discharge
It develops.Ternary spinel-type cobalt acid nickel due to its low cost, high conductivity, nontoxic, environmental-friendly, ABUNDANT NATUREAL RESOURSES and
High theoretical capacity has also attracted extensive concern, and cobalt acid nickel nano film array, and net is interconnected to form between piece and piece
Network shape structure is mutually supported to keep structure more stable between piece and piece, material can be helped to slow down in cyclic process because volume is swollen
It is swollen and caused by structural failure, to improve stability.In recent years, two kinds are shown with the material of improved chemical property
It is combined and to form advanced hierarchical structure and put into huge effort, and the development of nano structural material can be with maximum limit
Degree ground improves the contact area between electrode and electrolyte, and the diffusion path of electronics and ion is made to shorten, cause high capacity and times
Rate performance.
Summary of the invention
It is an object of the invention to: overcome shortcoming in the prior art, it is simple to provide a kind of preparation method, and structure is closed
Reason, molybdenum dioxide/cobalt acid nickel classification hybrid nanostructure array preparation method of size rule.
In order to achieve the above-mentioned object of the invention, the invention provides the following technical scheme:
A kind of molybdenum dioxide/cobalt acid nickel classification hybrid nanostructure array, makes cobalt acid nickel nano film battle array by hydro-thermal reaction
Column are grown in respectively in the substrate of molybdenum dioxide nano wire or molybdenum dioxide nanometer sheet, and the thickness of compound cobalt acid nickel nano film is
10-20nm。
Preferably, the cobalt acid nickel nano film size is regular, is evenly distributed.
Preferably, a kind of molybdenum dioxide/cobalt acid nickel classification hybrid nanostructure array preparation method, specific steps are such as
Under:
(1) carbon fiber paper is put into the vacuum chamber of magnetron sputtering depositing system, using the method for d.c. sputtering, passes through control
Sputtering power and sputtering time obtain the controllable metal molybdenum film of thickness on the surface of carbon fiber paper；
(2) it weighs powder containing molybdenum element and pours into burning boat, and paved；By the splash-proofing sputtering metal molybdenum obtained in step (1)
It is 1cm that carbon fiber paper, which cuts into area,2-6cm2Thin slice, on the burning boat being positioned ready for；
(3) the burning boat of step (2) is placed in the tube furnace of three-temperature-zone, is made annealing treatment, is obtained in high-purity argon gas atmosphere
There is the carbon fiber paper of molybdenum dioxide nano wire or molybdenum dioxide nanometer sheet to growth；
(4) it nickel nitrate, cobalt nitrate, ammonium fluoride, urea is weighed is added in deionized water and be configured to solution, and stir 30min
Mixed solution derived above；
(5) growth mixed solution that step (4) configure poured into polytetrafluoroethyllining lining, and is prepared by step (3)
There are molybdenum dioxide nano wire or the carbon fiber paper of molybdenum dioxide nanometer sheet to be that substrate is put into mixed solution, then by polytetrafluoroethylene (PTFE)
Liner is put into stainless steel water heating kettle in 100-150 DEG C of at a temperature of progress 2-5h hydro-thermal reaction；
(6) after hydro-thermal reaction, carbon fiber paper is taken out and is constantly rinsed with deionized water, is then dried；
(7) carbon fiber paper that step (6) are dried is put into tube furnace, is made annealing treatment in air, obtains dioxy
Change molybdenum/cobalt acid nickel and is classified hybrid nanostructure array.
Preferably, the sputtering power in step (1) is 40-80W, sputtering time 20-60min.
Preferably, every 1cm2-6cm2Thin slice addition 1-3g powder containing molybdenum element.
Preferably, annealing described in step (3) includes the process of heating and heat preservation, the heating and insulating process
It is reacted in the high-purity argon gas atmosphere that purity is 99.999%, centre haves no need to change gas circuit, annealing temperature 400-800
DEG C, heating rate is 5~25 DEG C/min, and soaking time is 20~90min.
Preferably, the amount of the substance of nickel nitrate is 0.5-2mmol in step (4), and the amount of the substance of cobalt nitrate is 1-
4mmol, the amount of the substance of ammonium fluoride are 2-10mmol, and the amount of the substance of urea is 5-20mmol, the deionization water body being added
Product is 50-100ml.
Preferably, annealing described in step (7) carries out in air, and annealing temperature is 200-400 DEG C, annealing time
For 1.8-2.2h.
The beneficial effects of the present invention are: the present invention mainly prepares molybdenum dioxide/cobalt acid nickel using hydro-thermal method and is classified hydridization
Nano-structure array, cobalt surface acid nickel nano film array sizes are small, piece thickness ultrathin, large specific surface area, are conducive to electrolyte expansion
It is scattered to electrode interior, makes all active materials that can participate in electrochemical charge thermal energy storage process, improves stock utilization, and dioxy
Change molybdenum nanometer linear structure and be conducive to transmission of the electronics between electrolyte and electrode, improves conductivity；And cobalt acid nickel nanometer
Piece is directly coupled to each other with piece, mutually supports in chip arrays, and formation is network-like, keeps the structure of material more stable.Hydro-thermal reaction
With simple process, cost is relatively low, and safe and reliable free of contamination feature is suitable for being mass produced, therefore has biggish business
Prospect.
Detailed description of the invention
Fig. 1 is that molybdenum dioxide prepared by embodiment 1/cobalt acid nickel is classified hybrid nanostructure array in different amplification
Under scanning electron photo；
Fig. 2 is that molybdenum dioxide prepared by embodiment 2/cobalt acid nickel is classified hybrid nanostructure array in different amplification
Under scanning electron photo；
Fig. 3 is the X-ray diffraction photo that molybdenum dioxide of the invention/cobalt acid nickel is classified hybrid nanostructure array, is shown
Spinel-type cobalt acid nickel mutually successfully synthesizes；
Fig. 4 is the x-ray photoelectron spectroscopy that molybdenum dioxide of the invention/cobalt acid nickel is classified hybrid nanostructure array, table
Bright molybdenum dioxide sample surfaces successfully mix Ni and Co element；
Fig. 5 is the high-resolution-ration transmission electric-lens figure that molybdenum dioxide of the invention/cobalt acid nickel is classified hybrid nanostructure array
Piece, what by Mapping spectrogram, we can be apparent sees that cobalt acid nickel is successfully combined to the surface of molybdenum dioxide nano wire.
Specific embodiment
The invention will be further described for 1-5 needle with reference to the accompanying drawing.
Embodiment 1:
A kind of preparation method of molybdenum dioxide/cobalt acid nickel classification hybrid nanostructure array, the specific steps are as follows:
(1) carbon fiber paper of purchase is put into the vacuum chamber of magnetron sputtering depositing system, 30min is sputtered with the power of 40W,
Obtain the carbon fiber paper of splash-proofing sputtering metal molybdenum；
(2) 1.2g powder containing molybdenum element is weighed with electronic balance and pour into burning boat, and paved；It will be obtained in step (1)
Splash-proofing sputtering metal molybdenum carbon fiber paper cut into area be 1cm2-6cm2Thin slice, on the burning boat being positioned ready for；
(3) the burning boat of step (2) is placed in the tube furnace of three-temperature-zone, is annealed in high-purity argon gas atmosphere with 600 DEG C
Processing, wherein heating rate is 20 DEG C/min, soaking time 60min, obtains the carbon that growth has molybdenum dioxide nano-wire array
Fibrous paper；
(4) 1mmol nickel nitrate, 2mmol cobalt nitrate, 6mmol ammonium fluoride, 15mmol urea are weighed, 70ml deionized water is added
In be configured to solution, and stir 30min mixed solution derived above；
(5) growth mixed solution that step (4) configure poured into polytetrafluoroethyllining lining, and is prepared by step (3)
The carbon fiber paper for having molybdenum dioxide nano wire is that substrate is put into mixed solution, then polytetrafluoroethyllining lining is put into stainless steel water
In hot kettle 120 DEG C at a temperature of carry out 3h hydro-thermal reaction；
(6) after hydro-thermal reaction, carbon fiber paper is taken out and is constantly rinsed with deionized water, is then dried；
(7) carbon paper that step (6) are dried is put into tube furnace, makes annealing treatment 2 hours for 350 DEG C in air, obtains two
Molybdenum oxide/cobalt acid nickel is classified hybrid nanostructure array.
Molybdenum dioxide prepared by this example/cobalt acid nickel classification hybrid nanostructure array structure is reasonable, of uniform size, cobalt
Sour nickel nano film thickness 10nm, prepared molybdenum dioxide/cobalt acid nickel classification hybrid nanostructure array pattern are as shown in Figure 1.
Embodiment 2:
A kind of preparation method of molybdenum dioxide/cobalt acid nickel classification hybrid nanostructure array, the specific steps are as follows:
(1) carbon fiber paper of purchase is put into the vacuum chamber of magnetron sputtering depositing system, 30min is sputtered with the power of 40W,
Obtain the carbon fiber paper of splash-proofing sputtering metal molybdenum；
(2) 1.2g powder containing molybdenum element is weighed with electronic balance and pour into burning boat, and paved；It will be obtained in step (1)
Splash-proofing sputtering metal molybdenum carbon fiber paper cut into area be 1cm2-6cm2Thin slice, on the burning boat being positioned ready for；
(3) the burning boat of step (2) is placed in the tube furnace of three-temperature-zone, is annealed in high-purity argon gas atmosphere with 500 DEG C
Processing, wherein heating rate is 20 DEG C/min, soaking time 80min, obtains the carbon that growth has molybdenum dioxide nano-chip arrays
Fibrous paper；
(4) 1mmol nickel nitrate, 2mmol cobalt nitrate, 6mmol ammonium fluoride, 15mmol urea are weighed, 70ml deionized water is added
In be configured to solution, and stir 30min mixed solution derived above；
(5) growth mixed solution that step (4) configure poured into polytetrafluoroethyllining lining, and is prepared by step (3)
The carbon fiber paper for having molybdenum dioxide nanometer sheet is that substrate is put into mixed solution, then polytetrafluoroethyllining lining is put into stainless steel water
In hot kettle 120 DEG C at a temperature of carry out 3h hydro-thermal reaction；
(6) after hydro-thermal reaction, carbon fiber paper is taken out and is constantly rinsed with deionized water, is then dried；
(7) carbon paper that step (6) are dried is put into tube furnace, makes annealing treatment 2 hours for 350 DEG C in air, obtains two
Molybdenum oxide/cobalt acid nickel is classified hybrid nanostructure array.
Molybdenum dioxide prepared by this example/cobalt acid nickel classification hybrid nanostructure array structure rule, is evenly distributed, causes
Density is high, large specific surface area, cobalt acid nickel nano film thickness 20nm, and prepared molybdenum dioxide/cobalt acid nickel is classified hybridized nanometer knot
Structure array pattern is as shown in Figure 2.
The above content is just an example and description of the concept of the present invention, affiliated those skilled in the art
It makes various modifications or additions to the described embodiments or is substituted in a similar manner, without departing from invention
Design or beyond the scope defined by this claim, be within the scope of protection of the invention.
Claims (8)
1. a kind of molybdenum dioxide/cobalt acid nickel is classified hybrid nanostructure array, it is characterised in that: make cobalt acid nickel by hydro-thermal reaction
Nano-chip arrays are grown in respectively in the substrate of molybdenum dioxide nano wire or molybdenum dioxide nanometer sheet, compound cobalt acid nickel nano film
Thickness be 10-20nm；
Molybdenum dioxide/cobalt acid nickel classification hybrid nanostructure array preparation method, the specific steps are as follows:
(1) carbon fiber paper is put into the vacuum chamber of magnetron sputtering depositing system, using the method for d.c. sputtering, is sputtered by control
Power and sputtering time obtain the controllable metal molybdenum film of thickness on the surface of carbon fiber paper；
(2) it weighs powder containing molybdenum element and pours into burning boat, and paved；By the carbon fiber of the splash-proofing sputtering metal molybdenum obtained in step (1)
It is 1cm that dimension paper, which cuts into area,2-6cm2Thin slice, on the burning boat being positioned ready for, every 1cm2-6cm2Thin slice add 1.2g
Powder containing molybdenum element；
(3) the burning boat of step (2) is placed in the tube furnace of three-temperature-zone, is made annealing treatment, is given birth in high-purity argon gas atmosphere
Carbon fiber paper with molybdenum dioxide nano wire or molybdenum dioxide nanometer sheet；
(4) it nickel nitrate, cobalt nitrate, ammonium fluoride, urea is weighed is added in deionized water and be configured to solution, and stir 30min or more
Obtain mixed solution；
(5) mixed solution that step (4) configure is poured into polytetrafluoroethyllining lining, and growth prepared by step (3) is had two
Molybdenum oxide nanowires or the carbon fiber paper of molybdenum dioxide nanometer sheet are that substrate is put into mixed solution, then by polytetrafluoroethyllining lining
It is put into stainless steel water heating kettle in 100-150 DEG C of at a temperature of progress 2-5h hydro-thermal reaction, the amount of the substance of nickel nitrate is
1mmol, the amount of the substance of cobalt nitrate are 2mmol, and the amount of the substance of ammonium fluoride is 6mmol, and the amount of the substance of urea is 15mmol,
The deionized water volume being added is 70ml；
(6) after hydro-thermal reaction, carbon fiber paper is taken out and is constantly rinsed with deionized water, is then dried；
(7) by step (6) dry carbon fiber paper be put into tube furnace, made annealing treatment in air, obtain molybdenum dioxide/
Cobalt acid nickel is classified hybrid nanostructure array, and annealing temperature is 350 DEG C, annealing time 2h.
2. molybdenum dioxide according to claim 1/cobalt acid nickel is classified hybrid nanostructure array, it is characterised in that: described
Cobalt acid nickel nano film size rule, be evenly distributed.
3. a kind of molybdenum dioxide/cobalt acid nickel classification hybrid nanostructure array preparation method, it is characterised in that: specific steps are such as
Under:
(1) carbon fiber paper is put into the vacuum chamber of magnetron sputtering depositing system, using the method for d.c. sputtering, is sputtered by control
Power and sputtering time obtain the controllable metal molybdenum film of thickness on the surface of carbon fiber paper；
(2) it weighs powder containing molybdenum element and pours into burning boat, and paved；By the carbon fiber of the splash-proofing sputtering metal molybdenum obtained in step (1)
It is 1cm that dimension paper, which cuts into area,2-6cm2Thin slice, on the burning boat being positioned ready for；
(3) the burning boat of step (2) is placed in the tube furnace of three-temperature-zone, is made annealing treatment, is given birth in high-purity argon gas atmosphere
Carbon fiber paper with molybdenum dioxide nano wire or molybdenum dioxide nanometer sheet；
(4) it nickel nitrate, cobalt nitrate, ammonium fluoride, urea is weighed is added in deionized water and be configured to solution, and stir 30min or more
Obtain mixed solution；
(5) mixed solution that step (4) configure is poured into polytetrafluoroethyllining lining, and growth prepared by step (3) is had two
Molybdenum oxide nanowires or the carbon fiber paper of molybdenum dioxide nanometer sheet are that substrate is put into mixed solution, then by polytetrafluoroethyllining lining
It is put into stainless steel water heating kettle in 100-150 DEG C of at a temperature of progress 2-5h hydro-thermal reaction；
(6) after hydro-thermal reaction, carbon fiber paper is taken out and is constantly rinsed with deionized water, is then dried；
(7) by step (6) dry carbon fiber paper be put into tube furnace, made annealing treatment in air, obtain molybdenum dioxide/
Cobalt acid nickel is classified hybrid nanostructure array.
4. molybdenum dioxide according to claim 3/cobalt acid nickel classification hybrid nanostructure array preparation method, feature
Be: the sputtering power in step (1) is 40-80W, sputtering time 20-60min.
5. molybdenum dioxide according to claim 3/cobalt acid nickel classification hybrid nanostructure array preparation method, feature
It is: every 1cm2-6cm2Thin slice addition 1-3g powder containing molybdenum element.
6. molybdenum dioxide according to claim 3/cobalt acid nickel classification hybrid nanostructure array preparation method, feature
Be: annealing described in step (3) includes the process of heating and heat preservation, and the heating and insulating process are in purity
It is reacted in 99.999% high-purity argon gas atmosphere, centre haves no need to change gas circuit, and annealing temperature is 400-800 DEG C, heating rate
For 5~25 DEG C/min, soaking time is 20~90min.
7. molybdenum dioxide according to claim 3/cobalt acid nickel classification hybrid nanostructure array preparation method, feature
Be: the amount of the substance of nickel nitrate is 1mmol in step (4), and the amount of the substance of cobalt nitrate is 2mmol, the substance of ammonium fluoride
Amount is 6mmol, and the amount of the substance of urea is 15mmol, and the deionized water volume being added is 70ml.
8. molybdenum dioxide according to claim 3/cobalt acid nickel classification hybrid nanostructure array preparation method, feature
Be: annealing described in step (7) carries out in air, and annealing temperature is 350 DEG C, annealing time 2h.
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| CN107032414B (en) * | 2017-03-13 | 2019-04-23 | 中山大学 | A kind of preparation method of flexibility cobalt acid zinc nano-material |
| CN107177053B (en) * | 2017-05-22 | 2019-04-02 | 陕西科技大学 | A kind of cobalt acid nickel-silicon carbide fiber multi-dimension reinforcement body enhancing polyimide resin based structures absorbing material and preparation method thereof |
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| CN110885100B (en) * | 2018-09-07 | 2023-04-14 | 湖北大学 | Preparation method of nickel lithium manganate cathode material with hierarchical structure |
| CN111573746B (en) * | 2020-05-06 | 2021-06-01 | 电子科技大学 | Porous nickel-cobalt oxide and two-step synthesis method thereof |
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