CN106219616A - 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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- CN106219616A CN106219616A CN201610566399.9A CN201610566399A CN106219616A CN 106219616 A CN106219616 A CN 106219616A CN 201610566399 A CN201610566399 A CN 201610566399A CN 106219616 A CN106219616 A CN 106219616A
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Abstract
The invention discloses a kind of use hydro-thermal method in molybdenum dioxide nano wire, nanometer sheet substrate compound cobalt acid nickel nano film array thus obtain molybdenum dioxide/cobalt acid nickel classification hybrid nanostructure array and preparation method thereof.Concrete step is: the method that (1) deposits by chemical gaseous phase prepares molybdenum dioxide nano wire or molybdenum dioxide nano-chip arrays on sprayed molybdenum carbon paper；(2) nano wire of above-mentioned preparation, nano-chip arrays are placed in the mixed solution containing cobalt nitrate, nickel nitrate, ammonium fluoride and carbamide, use hydro-thermal reaction method to carry out reaction under different temperature, different time, variable concentrations precursor solution and prepare composite precursor；(3) presoma of above-mentioned preparation is placed in tube furnace, and in atmosphere it is made annealing treatment, thus 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 nanostructured field, is specifically related to a kind of molybdenum dioxide/cobalt acid nickel classification hybrid nanostructure
Array and preparation method thereof.
Background technology
At the second eleventh century along with the progress of science and technology, our modern society is faced with the energy and environmental correclation
Problem, as polluted, the shortage of Fossil fuel and global warming.In order to overcome these complication, cleaning and renewable energy source material,
And an urgent demand of their equipment.Fortunately, use regenerative resource, such as solar energy and wind energy, be effectively improved
In our daily life, but the disperse properties of regenerative resource requires have high performance energy storage device.In this respect, electrification
Learn energy-storage system and the efficient storage of solar energy and wind energy is played vital effect.At present, battery and ultracapacitor by
The most promising and the successful energy storage system that can commercially obtain is become in its low cost and high-performance.
Recent years, transition metal oxide receives substantial amounts of research due to its higher theoretical specific capacity.Molybdenum
Oxide presents multiple special appearance, structure and character because of its valence state mutability, photocatalysis, gas sensing, lithium ion battery,
Image shows, information stores, variable reflectivity lens and the first-class aspect of high energy efficiency smart windows have important application.Titanium dioxide
Molybdenum is a typical stratiform transition group metallic oxide, and it has the highest theoretical capacity (838mAh/g), low cost, low
Resistivity and good electro-chemical activity.But the change of volume causes that cycle life is the highest to be limited during discharge and recharge
Its development.Ternary spinel-type cobalt acid nickel due to its low cost, high conductivity, nontoxic, environmental friendliness, ABUNDANT NATUREAL RESOURSES and
High theoretical capacity has also attracted to pay close attention to widely, and cobalt acid nickel nano film array, it is interconnected to form net between sheet and sheet
Network shape structure, mutually supports between sheet and sheet to make structure more stable, material can be helped to slow down in cyclic process because volume is swollen
Swollen and the structural failure that causes, thus improve stability.In recent years, two kinds are shown to the material of the chemical property of improvement
It is combined forming advanced hierarchy and has 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, makes the evolving path of electronics and ion shorten, cause high power capacity and times
Rate performance.
Summary of the invention
It is an object of the invention to: overcome weak point of the prior art, it is provided that a kind of preparation method is simple, and structure is closed
Reason, the preparation method of the molybdenum dioxide/cobalt acid nickel classification hybrid nanostructure array of size rule.
In order to realize foregoing invention purpose, the present invention provides 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
Row are grown in the substrate of molybdenum dioxide nano wire or molybdenum dioxide nanometer sheet respectively, and the thickness of compound cobalt acid nickel nano film is
10-20nm。
Preferably, described cobalt acid nickel nano film size rule, it is evenly distributed.
Preferably, the preparation method of a kind of molybdenum dioxide/cobalt acid nickel classification hybrid nanostructure array, concrete steps are such as
Under:
(1) carbon fiber paper is put into the vacuum chamber of magnetron sputtering deposition system, and the method using d.c. sputtering, by controlling
Sputtering power and sputtering time, obtain the metal molybdenum thin film that thickness is controlled on the surface of carbon fiber paper；
(2) weigh the powder containing molybdenum element and pour burning boat into, and paved；By the splash-proofing sputtering metal molybdenum of acquisition in step (1)
It is 1cm that carbon fiber paper cuts into area2-6cm2Thin 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, makes annealing treatment in high-purity argon gas atmosphere,
Molybdenum dioxide nano wire or the carbon fiber paper of molybdenum dioxide nanometer sheet is had to growth；
(4) weigh in nickel nitrate, cobalt nitrate, ammonium fluoride, carbamide addition deionized water and be configured to solution, and stir 30min
Mixed solution derived above；
(5) mixed solution that step (4) configures is poured in polytetrafluoroethyllining lining, and growth prepared by step (3)
The carbon fiber paper having molybdenum dioxide nano wire or molybdenum dioxide nanometer sheet is that substrate is put in mixed solution, then by politef
Liner is put into and is carried out 2-5h hydro-thermal reaction in rustless steel water heating kettle at a temperature of 100-150 DEG C；
(6), after hydro-thermal reaction terminates, carbon fiber paper taken out and constantly rinses with deionized water, then drying；
(7) carbon fiber paper that step (6) is dried is put in tube furnace, make annealing treatment in atmosphere, obtain dioxy
Change molybdenum/cobalt acid nickel classification hybrid nanostructure array.
Preferably, the sputtering power in step (1) is 40-80W, and sputtering time is 20-60min.
Preferably, every 1cm2-6cm2Thin slice add 1-3g containing molybdenum element powder.
Preferably, the annealing described in step (3) includes a liter process for gentle insulation, described liter gentleness insulating process
All reacting in the high-purity argon gas atmosphere that purity is 99.999%, centre need not change gas circuit, and annealing temperature is 400-800
DEG C, programming rate is 5～25 DEG C/min, and temperature retention time is 20～90min.
Preferably, in step (4), the amount of the material of nickel nitrate is 0.5-2mmol, and the amount of the material of cobalt nitrate is 1-
4mmol, the amount of the material of ammonium fluoride is 2-10mmol, and the amount of the material of carbamide is 5-20mmol, the deionization water body added
Amass as 50-100ml.
Preferably, the annealing described in step (7) is carried out in atmosphere, and annealing temperature is 200-400 DEG C, annealing time
For 1.8-2.2h.
The beneficial effects of the present invention is: the present invention mainly utilizes hydro-thermal method to prepare molybdenum dioxide/cobalt acid nickel classification hydridization
Nano-structure array, cobalt surface acid nickel nano film array sizes is little, sheet thickness ultrathin, and specific surface area is big, and beneficially electrolyte expands
It is scattered to electrode interior, makes all active materials can participate in electrochemical charge thermal energy storage process, raising stock utilization, and dioxy
Change molybdenum nanometer linear structure and be conducive to electronics transmission between electrolyte and electrode, improve electrical conductivity；And cobalt acid nickel nanometer
In chip arrays, sheet and sheet are directly coupled to each other, mutually support, are formed network-like, and the structure making material is more stable.Hydro-thermal reaction
Having technique simple, cost is relatively low, and safe and reliable free of contamination feature is suitable for large-scale production, therefore has bigger business
Prospect.
Accompanying drawing explanation
Fig. 1 is that the molybdenum dioxide prepared by embodiment 1/cobalt acid nickel classification hybrid nanostructure array is in different amplification
Under scanning electron photo；
Fig. 2 is that the molybdenum dioxide prepared by embodiment 2/cobalt acid nickel classification hybrid nanostructure array is in different amplification
Under scanning electron photo；
Fig. 3 is the X-ray diffraction photo of the molybdenum dioxide/cobalt acid nickel classification hybrid nanostructure array of the present invention, shows
Spinel-type cobalt acid nickel the most successfully synthesizes；
Fig. 4 is the x-ray photoelectron power spectrum of the molybdenum dioxide/cobalt acid nickel classification hybrid nanostructure array of the present invention, table
Bright molybdenum dioxide sample surfaces successfully mixes Ni and Co element；
Fig. 5 is the high-resolution-ration transmission electric-lens figure of the molybdenum dioxide/cobalt acid nickel classification hybrid nanostructure array of the present invention
Sheet, by Mapping spectrogram, we can clearly see that cobalt acid nickel is successfully compound to the surface of molybdenum dioxide nano wire.
Detailed description of the invention
The invention will be further described for 1-5 pin below in conjunction with the accompanying drawings.
Embodiment 1:
The preparation method of a kind of molybdenum dioxide/cobalt acid nickel classification hybrid nanostructure array, specifically comprises the following steps that
(1) carbon fiber paper of purchase is put into the vacuum chamber of magnetron sputtering deposition system, sputters 30min with the power of 40W,
Obtain the carbon fiber paper of splash-proofing sputtering metal molybdenum；
(2) weigh 1.2g powder Han molybdenum element with electronic balance and pour burning boat into, and paved；Step (1) will be obtained
The carbon fiber paper of splash-proofing sputtering metal molybdenum to 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, anneals with 600 DEG C in high-purity argon gas atmosphere
Processing, wherein, programming rate is 20 DEG C/min, and temperature retention time is 60min, obtains growing the carbon having molybdenum dioxide nano-wire array
Fibrous paper；
(4) 1mmol nickel nitrate, 2mmol cobalt nitrate, 6mmol ammonium fluoride, 15mmol carbamide addition 70ml deionized water are weighed
In be configured to solution, and stir 30min mixed solution derived above；
(5) mixed solution that step (4) configures is poured in polytetrafluoroethyllining lining, and growth prepared by step (3)
The carbon fiber paper having molybdenum dioxide nano wire is that substrate is put in mixed solution, then polytetrafluoroethyllining lining is put into stainless steel water
Hot still carries out at a temperature of 120 DEG C 3h hydro-thermal reaction；
(6), after hydro-thermal reaction terminates, carbon fiber paper taken out and constantly rinses with deionized water, then drying；
(7) putting in tube furnace by the carbon paper that step (6) is dried, 350 DEG C make annealing treatment 2 hours in atmosphere, obtain two
Molybdenum oxide/cobalt acid nickel classification hybrid nanostructure array.
Molybdenum dioxide prepared by this example/cobalt acid nickel classification hybrid nanostructure array structure is reasonable, size uniform, cobalt
Acid nickel nano film thickness 10nm, prepared molybdenum dioxide/cobalt acid nickel classification hybrid nanostructure array pattern is as shown in Figure 1.
Embodiment 2:
The preparation method of a kind of molybdenum dioxide/cobalt acid nickel classification hybrid nanostructure array, specifically comprises the following steps that
(1) carbon fiber paper of purchase is put into the vacuum chamber of magnetron sputtering deposition system, sputters 30min with the power of 40W,
Obtain the carbon fiber paper of splash-proofing sputtering metal molybdenum；
(2) weigh 1.2g powder Han molybdenum element with electronic balance and pour burning boat into, and paved；Step (1) will be obtained
The carbon fiber paper of splash-proofing sputtering metal molybdenum to 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, anneals with 500 DEG C in high-purity argon gas atmosphere
Processing, wherein, programming rate is 20 DEG C/min, and temperature retention time is 80min, obtains growing the carbon having molybdenum dioxide nano-chip arrays
Fibrous paper；
(4) 1mmol nickel nitrate, 2mmol cobalt nitrate, 6mmol ammonium fluoride, 15mmol carbamide addition 70ml deionized water are weighed
In be configured to solution, and stir 30min mixed solution derived above；
(5) mixed solution that step (4) configures is poured in polytetrafluoroethyllining lining, and growth prepared by step (3)
The carbon fiber paper having molybdenum dioxide nanometer sheet is that substrate is put in mixed solution, then polytetrafluoroethyllining lining is put into stainless steel water
Hot still carries out at a temperature of 120 DEG C 3h hydro-thermal reaction；
(6), after hydro-thermal reaction terminates, carbon fiber paper taken out and constantly rinses with deionized water, then drying；
(7) putting in tube furnace by the carbon paper that step (6) is dried, 350 DEG C make annealing treatment 2 hours in atmosphere, obtain two
Molybdenum oxide/cobalt acid nickel classification 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, and specific surface area is big, cobalt acid nickel nano film thickness 20nm, prepared molybdenum dioxide/cobalt acid nickel classification hybridized nanometer knot
Structure array pattern is as shown in Figure 2.
Above content is only the design example to the present invention and explanation, affiliated those skilled in the art
Described specific embodiment is made various amendment or supplements or use similar mode to substitute, without departing from invention
Design or surmount scope defined in the claims, protection scope of the present invention all should be belonged to.
Claims (8)
1. molybdenum dioxide/cobalt acid nickel classification hybrid nanostructure array, it is characterised in that: make cobalt acid nickel by hydro-thermal reaction
Nano-chip arrays is grown in the substrate of molybdenum dioxide nano wire or molybdenum dioxide nanometer sheet respectively, compound cobalt acid nickel nano film
Thickness be 10-20nm.
Molybdenum dioxide the most according to claim 1/cobalt acid nickel classification hybrid nanostructure array, it is characterised in that: described
Cobalt acid nickel nano film size rule, be evenly distributed.
3. the preparation method of molybdenum dioxide/cobalt acid nickel classification hybrid nanostructure array, it is characterised in that: concrete steps are such as
Under:
(1) carbon fiber paper is put into the vacuum chamber of magnetron sputtering deposition system, the method using d.c. sputtering, sputtered by control
Power and sputtering time, obtain the metal molybdenum thin film that thickness is controlled on the surface of carbon fiber paper；
(2) weigh the powder containing molybdenum element and pour burning boat into, and paved；By fine for the carbon of the splash-proofing sputtering metal molybdenum obtained in step (1)
It is 1cm that dimension paper cuts into area2-6cm2Thin 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, makes annealing treatment in high-purity argon gas atmosphere, given birth to
Long have molybdenum dioxide nano wire or the carbon fiber paper of molybdenum dioxide nanometer sheet；
(4) weigh in nickel nitrate, cobalt nitrate, ammonium fluoride, carbamide addition deionized water and be configured to solution, and stir more than 30min
Obtain mixed solution；
(5) mixed solution that step (4) configures is poured in polytetrafluoroethyllining lining, and growth prepared by step (3) is had two
The carbon fiber paper of molybdenum oxide nanowires or molybdenum dioxide nanometer sheet is that substrate is put in mixed solution, then by polytetrafluoroethyllining lining
Put into and rustless steel water heating kettle carries out at a temperature of 100-150 DEG C 2-5h hydro-thermal reaction；
(6), after hydro-thermal reaction terminates, carbon fiber paper taken out and constantly rinses with deionized water, then drying；
(7) carbon fiber paper that step (6) is dried is put in tube furnace, makes annealing treatment in atmosphere, obtain molybdenum dioxide/
Cobalt acid nickel classification hybrid nanostructure array.
The preparation method of molybdenum dioxide the most according to claim 3/cobalt acid nickel classification hybrid nanostructure array, its feature
Being: the sputtering power in step (1) is 40-80W, sputtering time is 20-60min.
The preparation method of molybdenum dioxide the most according to claim 3/cobalt acid nickel classification hybrid nanostructure array, its feature
It is: every 1cm2-6cm2Thin slice add 1-3g containing molybdenum element powder.
The preparation method of molybdenum dioxide the most according to claim 3/cobalt acid nickel classification hybrid nanostructure array, its feature
It is: the annealing described in step (3) includes a liter process for gentle insulation, and described liter gentleness insulating process in purity is all
Reacting in the high-purity argon gas atmosphere of 99.999%, centre need not change gas circuit, and annealing temperature is 400-800 DEG C, programming rate
Being 5～25 DEG C/min, temperature retention time is 20～90min.
The preparation method of molybdenum dioxide the most according to claim 3/cobalt acid nickel classification hybrid nanostructure array, its feature
Being: in step (4), the amount of the material of nickel nitrate is 0.5-2mmol, the amount of the material of cobalt nitrate is 1-4mmol, ammonium fluoride
The amount of material is 2-10mmol, and the amount of the material of carbamide is 5-20mmol, and the deionized water volume added is 50-100ml.
The preparation method of molybdenum dioxide the most according to claim 3/cobalt acid nickel classification hybrid nanostructure array, its feature
Being: the annealing described in step (7) is carried out in atmosphere, and annealing temperature is 200-400 DEG C, annealing time is 1.8-
2.2h。
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| CN107032414A (en) * | 2017-03-13 | 2017-08-11 | 中山大学 | A kind of preparation method of the sour zinc nano-material of flexible cobalt |
| CN107177053A (en) * | 2017-05-22 | 2017-09-19 | 陕西科技大学 | Sour nickel silicon carbide fibre multi-scale reinforcing body enhancing polyimide resin based structures absorbing material of a kind of cobalt and preparation method thereof |
| CN107591251A (en) * | 2017-07-14 | 2018-01-16 | 电子科技大学 | A kind of soap-free emulsion polymeization formulation NiCo2O4@NiMoO4Core-shell nano chip arrays material and preparation method thereof |
| CN107685150A (en) * | 2017-08-24 | 2018-02-13 | 武汉理工大学 | A kind of Ni ＆ MoO of nitrogen-doped carbon cladding2Superfine nanowire and its preparation method and application |
| CN110885100A (en) * | 2018-09-07 | 2020-03-17 | 湖北大学 | Preparation method of novel lithium nickel manganese oxide positive electrode material with hierarchical structure |
| CN111573746A (en) * | 2020-05-06 | 2020-08-25 | 电子科技大学 | Porous nickel-cobalt oxide and two-step synthesis method thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107032414A (en) * | 2017-03-13 | 2017-08-11 | 中山大学 | A kind of preparation method of the sour zinc nano-material of flexible cobalt |
| CN107032414B (en) * | 2017-03-13 | 2019-04-23 | 中山大学 | A kind of preparation method of flexibility cobalt acid zinc nano-material |
| CN107177053A (en) * | 2017-05-22 | 2017-09-19 | 陕西科技大学 | Sour nickel silicon carbide fibre multi-scale reinforcing body enhancing polyimide resin based structures absorbing material of a kind of cobalt and preparation method thereof |
| CN107591251A (en) * | 2017-07-14 | 2018-01-16 | 电子科技大学 | A kind of soap-free emulsion polymeization formulation NiCo2O4@NiMoO4Core-shell nano chip arrays material and preparation method thereof |
| CN107685150A (en) * | 2017-08-24 | 2018-02-13 | 武汉理工大学 | A kind of Ni ＆ MoO of nitrogen-doped carbon cladding2Superfine nanowire and its preparation method and application |
| CN107685150B (en) * | 2017-08-24 | 2019-08-23 | 武汉理工大学 | A kind of carbon-coated Ni & MoO of N doping2Superfine nanowire and its preparation method and application |
| CN110885100A (en) * | 2018-09-07 | 2020-03-17 | 湖北大学 | Preparation method of novel lithium nickel manganese oxide positive electrode material with hierarchical structure |
| CN111573746A (en) * | 2020-05-06 | 2020-08-25 | 电子科技大学 | Porous nickel-cobalt oxide and two-step synthesis method thereof |
| 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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