CN108996557A - A kind of hollow ball structure nickel oxide/copper oxide composite nano materials and preparation method thereof - Google Patents
A kind of hollow ball structure nickel oxide/copper oxide composite nano materials and preparation method thereof Download PDFInfo
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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- C01P2004/00—Particle morphology
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
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- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
Abstract
The invention discloses a kind of hollow ball structure nickel oxide/copper oxide composite nano materials and preparation method thereof, the preparation method comprises the following steps: nickel salt and cupric salt dissolution are obtained mixed solution in a solvent, polymer-supported reagents and urea are sequentially added into this mixed solution again, stirring to the two is completely dissolved, then hydro-thermal reaction is carried out, products therefrom further progress calcining, up to hollow ball structure nickel oxide/copper oxide composite nano materials after calcining.Compared with prior art, raw material of the present invention is cheap and easy to get, and the acquisition of hollow structure without being additionally added template in the reaction system, and synthesis technology is simple, and the structure snd size of products therefrom are controllable, product yield high.
Description
Technical field
The invention belongs to the fabricating technology fields of inorganic micro Nano material, and in particular to a kind of hollow ball structure oxidation
Nickel/copper oxide composite nano materials and preparation method thereof.
Background technique
The characteristics of hollow micro Nano material of inorganic oxide is because of its hollow structure, make it have low-density, high-specific surface area,
The advantages that high osmosis, high thermal stability and high thermodynamic stability, in recent years catalysis, absorption with air-sensitive, energy and the energy,
Drug storage illustrates wide application prospect with fields such as releases, can be used for light material additive, acoustical and thermal material, medicine
The fields such as object slow-released carrier, catalyst carrier；Oxide hollow sphere makes due to excellent properties such as high yield, high-specific surface areas
It has great application prospect in the physics such as electricity, magnetic, absorption and catalysis and chemical field.
From the angle of material intrinsic property, the performance of single metal oxide mostly can be insufficient, and such as CuO makees
For a kind of P-type semiconductor, conductive capability is weaker, influences its application as electrochemical material.Therefore by various metals oxygen
Compound combines, and the deficiency in single composition oxide material performance can be made up, to make material in electricity such as electro-catalysis, battery electrodes
Chemical field has more good application effect.
By the way that inorganic oxide material is prepared as hollow micro nano structure, and to hollow micro nano structure oxide material
Composition, pattern, size etc. carry out a series of regulations, the specific function of material and attribute can be assigned, thus in mechanics, electricity
The different aspects such as, optics show the characteristic better than conventional oxide material powder particle.
Therefore some different inorganic oxides are be combined with each other, and is further prepared into the compound of hollow micro nano structure
Nano material is the effective means for improving material property, such as improves the catalytic performance of photoelectric, improve gas sensor
Sensitivity and recovery capability improve the chemical property etc. of electrode material.Currently, template is to prepare the micro-nano material of hollow structure
Expect most common method.This method comprises: first with synthesis template, then template surface deposit or coat target product, then
Template inside removal obtains hollow structure material；Or the template first to prepare reacts as reactant in template surface,
Hollow structure is formed inside template based on Kinkendal Effect.Template prepares hollow structure micro Nano material, because of its process
Relatively complicated, production cost is higher, limits its practical application and popularization.
So finding simple process, low-cost method, hollow structure micro Nano material is prepared, sky is especially prepared
Core structure composite micro-nano rice material be it is very necessary, will for micro Nano material apply with development provide more scientific basis and
Technical support.
Summary of the invention
The object of the present invention is to provide a kind of hollow ball structure nickel oxide/copper oxide composite nano materials and its preparations
Method, the raw material of use and simple process, equipment is simple, preparation cost is low, easily accomplishes scale production.
A kind of preparation method of hollow ball structure nickel oxide/copper oxide composite nano materials provided by the invention, including with
Lower step:
A, in a solvent by nickel salt and cupric salt dissolution, solution a is obtained；
B, polymer-supported reagents and urea are sequentially added in the solution a formed to step A, stirring is completely molten to the two
Solution, obtains solution b；
C, solution b is subjected to hydro-thermal reaction, solution and product will be separated after reaction, separating obtained product is further
Cleaning, drying；
D, the product further progress after will be dry obtained by step C is calcined, and is aoxidized after calcining up to hollow ball structure
Nickel/copper oxide composite nano materials.
In step A, the nickel salt is nitrate, sulfate, chlorate, the acetic acid of the nickel containing the crystallization water or without the crystallization water
One of salt is a variety of；The cupric salt is cupric nitrate, sulfate, the chlorine containing the crystallization water or without the crystallization water
One of salt dissolving, acetate are a variety of.
Further, in step A, the nickel salt, cupric salt are respectively preferably Nickelous nitrate hexahydrate, three nitric hydrates
Copper.
Ni in step A, in the nickel salt and cupric salt2+、Cu2+The ratio between the amount of substance be 1:1~1.5, Ni2+?
Concentration in solvent is 20-27mmol/L.
In step A, the solvent is that deionized water or deionized water and ethylene glycol are mixed according to what 1~2:1 of volume ratio was formed
Close liquid.
In step B, the polymer-supported reagents, urea, solvent described in step A ratio be 13~40g:16~
25g:1L.
In step B, the polymer-supported reagents are polyvinylpyrrolidone；It is preferred that the polyvinylpyrrolidine that K value is 30
Ketone.
In step C, the temperature and time of the hydro-thermal reaction is respectively 80~140 DEG C, 8~12 hours；Preferably 90 DEG C,
10 hours.
In step D, the calcining is referred under air atmosphere, by room temperature to after 700~800 DEG C, calcining 3~5
Hour.
The present invention also provides the hollow ball structure being prepared according to preparation method nickel oxide/copper oxide is compound
Nano material, by adjusting the composition proportion of solvent, can hollow ball structure nickel oxide/copper oxide prepared by Effective Regulation it is compound
Nano material size.
It is provided by the present invention to prepare in hollow ball structure nickel oxide/copper oxide composite nano materials method, macromolecule
The presence of auxiliary reagent polyvinylpyrrolidone increases the viscosity of reaction solution, therefore reacts urea in heating process and decompose generation
Gas forms bubble in reaction solution.Polyvinylpyrrolidonemolecules molecules are gathered in bubble surface, so that bubble is steady in reaction solution
It is fixed to exist.Since the non-bonding electrons on polyvinylpyrrolidone chain on O and N can form coordinate bond with metal ion, this makes
Metal ion is obtained also to assemble in bubble surface.Under hydrothermal conditions metal ion further with the OH in water-Reaction, in bubble table
Hydrate of looking unfamiliar precipitating, to form hollow ball structure.By calcining thereafter, so that hydroxide is converted into oxidation
Object finally obtains hollow ball structure nickel oxide/copper oxide composite nano materials.The addition of dihydric alcohol can further increase in solvent
The viscosity of reaction system, so that the bubble that the gas after urea decomposition is formed is not easy to assemble, to obtain smaller size
Bubble.Therefore pass through proportion shared by dihydric alcohol in adjustment solvent, and then hollow ball structure nickel oxide prepared by Effective Regulation/
Copper oxide composite nano materials size.
The present invention prepares hollow ball structure nickel oxide/copper oxide composite nano materials method, and hard mold is added without additional
Plate obtains hollow micro nano structure, and prepared scantling is uniform, and structure is uniform, concise in technology, favorable reproducibility, reaction dress
Set it is simple, with reaction mass and it is honest and clean be easy to get, preparation cost is low, is easy to amplify and accomplish scale production.And the material of preparation is two
The composite material that kind metal oxide is constituted, performance compare single metal oxidation nano material and will get a promotion；And the sky having
Bulbus cordis structure makes it have the advantages that large specific surface area, density are small.Therefore the hollow ball structure oxidation that preparation method of the present invention provides
It is more that nickel/copper oxide composite nano materials can be applicable to electro-catalysis, electrode material for super capacitor, Li ion battery electrode materials etc.
Kind neighborhood.
Detailed description of the invention
Fig. 1 is that hollow ball structure nickel oxide/copper oxide composite nano materials X- that the embodiment of the present invention 1 is prepared is penetrated
Line powder diffraction pattern；
Fig. 2 is hollow ball structure nickel oxide/copper oxide composite nano materials scanning that the embodiment of the present invention 1 is prepared
Electron microscope (SEM) photo；
Fig. 3 is hollow ball structure nickel oxide/copper oxide composite nano materials scanning that the embodiment of the present invention 2 is prepared
Electron microscope (SEM) photo；
Fig. 4 is hollow ball structure nickel oxide/copper oxide composite nano materials scanning that the embodiment of the present invention 3 is prepared
Electron microscope (SEM) photo；
Fig. 5 is hollow ball structure nickel oxide/copper oxide composite nano materials scanning that the embodiment of the present invention 4 is prepared
Electron microscope (SEM) photo；
Fig. 6 is hollow ball structure nickel oxide/copper oxide composite nano materials scanning that the embodiment of the present invention 5 is prepared
Electron microscope (SEM) photo；
Fig. 7 is hollow ball structure nickel oxide/copper oxide composite nano materials scanning that the embodiment of the present invention 6 is prepared
Electron microscope (SEM) photo.
Specific embodiment
Below with reference to embodiment and Figure of description, the present invention is described in detail.
Embodiment 1
A kind of preparation method of hollow ball structure nickel oxide/copper oxide composite nano materials, comprising the following steps:
A, 0.8mmol Nickelous nitrate hexahydrate, 0.8mmol Gerhardite are weighed, Nickelous nitrate hexahydrate and three are hydrated
30mL deionized water is added in copper nitrate and ethylene glycol is to stir to being completely dissolved, obtain in the mixed solution of 2:1 composition by volume
To clarification, transparent solution；
B, 0.48g urea, 1.2g polyvinylpyrrolidone are added in the solution obtained to step A, stirring to being completely dissolved,
It is clarified, transparent mixed solution；
C, the mixed solution for obtaining step B is transferred in the reaction kettle of polytetrafluoroethyllining lining, by reaction kettle it is closed after
As in insulating box, isothermal reaction 10h hours at 90 DEG C, it is cooled to room temperature.Liquid after cooling in reaction kettle is passed through into centrifugation
Isolate solid product, after product is washed centrifugation with alcohol, then be centrifuged with milli-Q water, after repeating above operation 2 times will
To solid product be placed in drying box, dry 6 hours at 90 DEG C；
D, the solid product by step C after dry, is placed in Muffle furnace, under air atmosphere, is warming up to 700 at room temperature
After DEG C, calcine 3 hours, last cooled to room temperature obtains hollow ball structure nickel oxide/copper oxide composite nano materials.
Fig. 1 is hollow ball structure nickel oxide/copper oxide composite nano materials X-ray diffraction pattern that embodiment 1 obtains.
As shown in Figure 1, the nickel oxide card of each diffraction maximum position of resulting materials and JCPDS (Joint Committee on Powder Diffraction Standards)
47-1049 and copper oxide card 45-0937 match, and show that product is the composite material being made of nickel oxide and copper oxide.
Fig. 2 is hollow ball structure nickel oxide/copper oxide composite nano materials scanning electron microscope that embodiment 1 obtains
Photo, display material are the chondritic being made of particle, sphere diameter average out to 600nm.Pass through opening for gained spheroidal material surface
Mouthful, it can be observed that material internal is hollow design feature.
Embodiment 2
A kind of preparation method of hollow ball structure nickel oxide/copper oxide composite nano materials, comprising the following steps:
A, 0.8mmol Nickelous nitrate hexahydrate, 0.8mmol Gerhardite are weighed, Nickelous nitrate hexahydrate and three are hydrated
Copper nitrate is added in 30mL deionized water, stirs to being completely dissolved, is clarified, transparent solution；
B, 0.48g urea, 1.2g polyvinylpyrrolidone are added in the solution obtained to step A, stirring to being completely dissolved,
It is clarified, transparent mixed solution；
C, the mixed solution for obtaining step B is transferred in the reaction kettle of polytetrafluoroethyllining lining, by reaction kettle it is closed after
As in insulating box, isothermal reaction 8h hours at 120 DEG C, it is cooled to room temperature.Liquid after cooling in reaction kettle is passed through into centrifugation
Isolate solid product, after product is washed centrifugation with alcohol, then be centrifuged with milli-Q water, after repeating above operation 2 times will
To solid product be placed in drying box, dry 6 hours at 90 DEG C；
D, the solid product by step C after dry, is placed in Muffle furnace, under air atmosphere, is warming up to 700 at room temperature
After DEG C, calcine 4 hours, last cooled to room temperature obtains hollow ball structure nickel oxide/copper oxide composite nano materials.
Fig. 3 is hollow ball structure nickel oxide/copper oxide composite nano materials scanning electron microscope that embodiment 2 obtains
Photo, display material are the chondritic being made of particle, sphere diameter average out to 900nm.Pass through opening for gained spheroidal material surface
Mouthful, it can be observed that material internal is hollow design feature.
Embodiment 3
A kind of preparation method of hollow ball structure nickel oxide/copper oxide composite nano materials, comprising the following steps:
A, 0.8mmol Nickelous nitrate hexahydrate, 0.8mmol Gerhardite are weighed, Nickelous nitrate hexahydrate and three are hydrated
40mL deionized water is added in copper nitrate and ethylene glycol volume ratio is to stir to being completely dissolved, obtain in the mixed solution of 1:1 composition
Clarification, transparent solution；
B, 1.0g urea, 0.8g polyvinylpyrrolidone are added in the solution obtained to step A, stirring to being completely dissolved,
It is clarified, transparent mixed solution；
C, the mixed solution for obtaining step B is transferred in the reaction kettle of polytetrafluoroethyllining lining, by reaction kettle it is closed after
As in insulating box, isothermal reaction 12h hours at 70 DEG C, it is cooled to room temperature.Liquid after cooling in reaction kettle is passed through into centrifugation
Isolate solid product, after product is washed centrifugation with alcohol, then be centrifuged with milli-Q water, after repeating above operation 2 times will
To solid product be placed in drying box, dry 6 hours at 80 DEG C；
D, the solid product by step C after dry, is placed in Muffle furnace, under air atmosphere, is warming up to 700 at room temperature
After DEG C, calcine 4 hours, last cooled to room temperature obtains hollow ball structure nickel oxide/copper oxide composite nano materials.
Fig. 4 is hollow ball structure nickel oxide/copper oxide composite nano materials scanning electron microscope that embodiment 3 obtains
Photo, display material are the chondritic being made of particle, sphere diameter average out to 1200nm.Pass through opening for gained spheroidal material surface
Mouthful, it can be observed that material internal is hollow design feature.
Embodiment 4
A kind of preparation method of hollow ball structure nickel oxide/copper oxide composite nano materials, comprising the following steps:
A, 0.8mmol Nickelous nitrate hexahydrate, 1.2mmol Gerhardite are weighed, Nickelous nitrate hexahydrate and three are hydrated
35mL deionized water and ethylene glycol volume ratio is added in copper nitrate, stirring to being completely dissolved,
It is clarified, transparent solution；
B, 0.6g urea, 1.2g polyvinylpyrrolidone are added in the solution obtained to step A, stirring to being completely dissolved,
It is clarified, transparent mixed solution；
C, the mixed solution for obtaining step B is transferred in the reaction kettle of polytetrafluoroethyllining lining, by reaction kettle it is closed after
It as in insulating box, isothermal reaction 6h hours at 140 DEG C, is cooled to room temperature, liquid after cooling in reaction kettle is passed through into centrifugation
Isolate solid product, after product is washed centrifugation with alcohol, then be centrifuged with milli-Q water, after repeating above operation 2 times will
To solid product be placed in drying box, dry 6 hours at 90 DEG C；
D, the solid product by step C after dry, is placed in Muffle furnace, under air atmosphere, is warming up to 700 at room temperature
After DEG C, calcine 5 hours, last cooled to room temperature obtains hollow ball structure nickel oxide/copper oxide composite nano materials.
Fig. 5 is hollow ball structure nickel oxide/copper oxide composite nano materials scanning electron microscope that embodiment 4 obtains
Photo, display material are the chondritic being made of particle, sphere diameter average out to 900nm.Pass through opening for gained spheroidal material surface
Mouthful, it can be observed that material internal is hollow design feature.
Embodiment 5
A kind of preparation method of hollow ball structure nickel oxide/copper oxide composite nano materials, comprising the following steps:
A, 0.8mmol Nickelous nitrate hexahydrate, 0.96mmol Gerhardite are weighed, Nickelous nitrate hexahydrate and three are hydrated
30mL deionized water is added in copper nitrate and ethylene glycol volume ratio is to stir to being completely dissolved, obtain in the mixed solution of 2:1 composition
Clarification, transparent solution.The amount of the substance of Ni ion and the volume ratio of solvent are 26.7mol/L in acquired solution；
B, 0.6g urea, 0.4g K polyvinylpyrrolidone are added in the solution obtained to step A, stirs to completely molten
Solution, is clarified, transparent mixed solution；
C, the mixed solution for obtaining step B is transferred in the reaction kettle of polytetrafluoroethyllining lining, by reaction kettle it is closed after
As in insulating box, isothermal reaction 12h hours at 60 DEG C, it is cooled to room temperature.Liquid after cooling in reaction kettle is passed through into centrifugation
Isolate solid product, after product is washed centrifugation with alcohol, then be centrifuged with milli-Q water, after repeating above operation 2 times will
To solid product be placed in drying box, dry 6 hours at 90 DEG C；
D, the solid product by step C after dry, is placed in Muffle furnace, under air atmosphere, is warming up to 800 at room temperature
After DEG C, calcine 3 hours, last cooled to room temperature obtains hollow ball structure nickel oxide/copper oxide composite nano materials.
Fig. 6 is hollow ball structure nickel oxide/copper oxide composite nano materials scanning electron microscope that embodiment 5 obtains
Photo, display material are the chondritic being made of particle, sphere diameter average out to 800nm.Pass through opening for gained spheroidal material surface
Mouthful, it can be observed that material internal is hollow design feature.
Embodiment 6
A kind of preparation method of hollow ball structure nickel oxide/copper oxide composite nano materials, comprising the following steps:
A, 0.8mmol nickel acetate tetrahydrate, 0.8mmol copper acetate dihydrate are weighed, nickel acetate tetrahydrate and one are hydrated
30mL deionized water is added in copper acetate and ethylene glycol volume ratio is to stir to being completely dissolved, obtain in the mixed solution of 2:1 composition
Clarification, transparent solution；
B, 0.6g urea, 0.8g polyvinylpyrrolidone are added in the solution obtained to step A, stirring to being completely dissolved,
It is clarified, transparent mixed solution；
C, the solution for obtaining step B is transferred in the reaction kettle of polytetrafluoroethyllining lining, by reaction kettle it is closed after as
In insulating box, isothermal reaction 10h hours at 90 DEG C, it is cooled to room temperature.Liquid after cooling in reaction kettle is passed through into centrifuge separation
Solid product out after product is washed centrifugation with alcohol, then is centrifuged with milli-Q water, will obtain after repeating above operation 2 times
Solid product is placed in drying box, 6 hours dry at 90 DEG C；
D, the solid product by step C after dry, is placed in Muffle furnace, under air atmosphere, is warming up to 700 at room temperature
After DEG C, calcine 5 hours, last cooled to room temperature obtains hollow ball structure nickel oxide/copper oxide composite nano materials.
Fig. 7 is hollow ball structure nickel oxide/copper oxide composite nano materials scanning electron microscope that embodiment 6 obtains
Photo, display material are the chondritic being made of particle, sphere diameter average out to 600nm.Pass through opening for gained spheroidal material surface
Mouthful, it can be observed that material internal is hollow design feature.
It is above-mentioned referring to embodiment to a kind of hollow ball structure nickel oxide/copper oxide composite nano materials and preparation method thereof into
Capable detailed description is illustrative without being restrictive, and can enumerate several embodiments according to limited range, therefore
Change and modification in the case where not departing from present general inventive concept should belong within protection scope of the present invention.
Claims (10)
1. a kind of preparation method of hollow ball structure nickel oxide/copper oxide composite nano materials, which is characterized in that including following step
It is rapid:
A, in a solvent by nickel salt and cupric salt dissolution, solution a is obtained；
B, polymer-supported reagents and urea are sequentially added in the solution a formed to step A, stirring is completely dissolved to the two, obtains
To solution b；
C, solution b is subjected to hydro-thermal reaction, solution and product will be separated after reaction, separating obtained product is further clear
It washes, dry；
D, the product further progress after will be dry obtained by step C is calcined, up to hollow ball structure nickel oxide/oxygen after calcining
Change copper composite nano materials.
2. preparation method according to claim 1, which is characterized in that in step A, the nickel salt is containing the crystallization water or to be free of
One of the nitrate of the nickel of the crystallization water, sulfate, chlorate, acetate are a variety of；The cupric salt is containing the crystallization water
Or one of cupric nitrate without the crystallization water, sulfate, chlorate, acetate or a variety of.
3. preparation method according to claim 1 or 2, which is characterized in that in step A, the nickel salt, cupric salt difference
For Nickelous nitrate hexahydrate, Gerhardite.
4. preparation method according to claim 1, which is characterized in that the Ni in step A, in the nickel salt and cupric salt2 +、Cu2+The ratio between the amount of substance be 1:1~1.5, Ni2+Concentration in a solvent is 20-27mmol/L.
5. preparation method according to claim 1 or 4, which is characterized in that in step A, the solvent is deionized water, or
The mixed liquor that deionized water and ethylene glycol are formed according to 1~2:1 of volume ratio.
6. preparation method according to claim 1, which is characterized in that in step B, the polymer-supported reagents, urea
Ratio with solvent described in step A is 13~40g:16~25g:1L.
7. preparation method according to claim 1 or 6, which is characterized in that in step B, the polymer-supported reagents are
Polyvinylpyrrolidone.
8. preparation method according to claim 1, which is characterized in that in step C, the temperature and time of the hydro-thermal reaction
Respectively 80~140 DEG C, 8~12 hours.
9. preparation method according to claim 1, which is characterized in that in step D, the calcining is referred to by room temperature
To after 700~800 DEG C, calcine 3~5 hours.
10. hollow ball structure nickel oxide/copper oxide that preparation method described in -9 any one is prepared according to claim 1
Composite nano materials.
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| CN115634693A (en) * | 2022-09-30 | 2023-01-24 | 惠州学院 | Preparation method of nano composite material with hollow tube structure and application of nano composite material in catalysis of ammonia borane alcoholysis for hydrogen production |
| CN115634693B (en) * | 2022-09-30 | 2024-01-26 | 惠州学院 | Preparation method of nanocomposite with hollow tube structure and application of nanocomposite in catalyzing aminoborane alcoholysis to produce hydrogen |
| CN115888718A (en) * | 2022-10-26 | 2023-04-04 | 福州大学 | Preparation and application of Chinese chestnut-shaped hollow NiCu composite material |
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