CN107200363A - Core shell structure NiO CdS Coaxial Nanofibers and preparation method thereof - Google Patents

Core shell structure NiO CdS Coaxial Nanofibers and preparation method thereof Download PDF

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CN107200363A
CN107200363A CN201710364978.XA CN201710364978A CN107200363A CN 107200363 A CN107200363 A CN 107200363A CN 201710364978 A CN201710364978 A CN 201710364978A CN 107200363 A CN107200363 A CN 107200363A
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胡寒梅
王曼
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Anhui University of Architecture
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    • C01G53/04Oxides
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Abstract

The invention discloses core shell structure NiO CdS Coaxial Nanofibers and preparation method thereof.Using nickel acetate, ammonium oxalate and triethylamine as reaction raw materials, after water-bath, nickeliferous sediment is collected, calcining obtains NiO nano powders.0.1g NiO are weighed, 30mL are added to containing in a certain amount of cadmium acetate aqueous solution, ultrasonic disperse 10~20 minutes obtains dispersion liquid A;1mmol thiocarbamides are weighed, 30mL deionized waters are added, 0.1mL ethylenediamines are added dropwise, solution B is dissolved to obtain;Solution B is added in dispersion liquid A, magnetic agitation is placed in household microwave oven after 12 hours, low fire heating 30 minutes;After reaction terminates, filtering precipitate, produces the core shell structure NiO CdS Coaxial Nanofibers of the present invention while hot.A diameter of 130~the 280nm of core shell structure NiO CdS Coaxial Nanofibers, a length of 0.8~2 μm, centronucleus is NiO nanofibers, and external shell is CdS nanocrystals, CdS nanocrystals are closely coated on the outside of NiO nanofibers, form coaxial cable formula core shell structure.The present invention is easy to operate, reproducible.

Description

Core shell structure NiO-CdS Coaxial Nanofibers and preparation method thereof
Technical field
It is to be related to core shell structure NiO- specifically the present invention relates to complex nano material preparing technical field is belonged to CdS Coaxial Nanofibers and preparation method thereof.
Background technology
With the development of nanometer composite technology, nuclear-shell structured nano-composite material turns into the new heat of field of compound material research Point.The nano composite material of core shell structure refers to the clad structure that core-shell formula is formed with two kinds of different materials, center Core and be coated on outside shell between by physics, chemical action be connected with each other.Due to unique structure and physical chemistry Characteristic, nuclear-shell structured nano-composite material all has in fields such as materialogy, chemistry, magnetics, electricity, optics, biomedicine, catalysis Have wide practical use, as study hotspot in recent years.
Nickel oxide is typical p-type semiconductor, is a kind of up-and-coming functional material, due to good chemistry and Heat endurance, it is environment-friendly the features such as, as focus of attention, be widely used in magnetic material, gas sensor, electrode material, The fields such as catalyst, electrochemical capacitor, function ceramics, adsorbent, photoelectric device, electrochromic material and sapecial coating.Just For photochemical catalyst, NiO energy gap is 3.6~4.0eV, is wide band gap semiconducter, can only absorb UV light region Photon, but ultraviolet light only accounts for the energy of sunshine 4%, to the effective using being greatly limited of solar energy.To NiO materials Carry out functionalization compound or modified, the utilization rate of sunshine can be greatly improved.CdS is intrinsic/n-type semiconductor, category IIB-VIA races Compound, is a kind of important semi-conducting material, is had a wide range of applications in opto-electronic conversion and photocatalysis field.It is excellent as one kind Good photochemical catalyst, CdS can effectively degrade most of organic matters in wastewater from chemical industry, the guarantor of processing and environment to waste water Shield serves good effect, but photoetch easily occurs for CdS to lose activity, and scientist proposes to be modified it, with Overcome its defect.In addition, CdS band gap is 2.4eV, it is to belong to by the narrow bandgap semiconductor material of excited by visible light.Research recently It was found that CdS photoetch effect can effectively be reduced to extend its service life by forming NiO/CdS p-n composite constructions, it has been found that The n-type CdS that composite visible light is responded on the p-type NiO semi-conducting materials of ultraviolet light response, can greatly improve the profit of solar energy With rate.
In recent years, control synthesis of the researchers to NiO/CdS p-n composite constructions has done some and has explored sex work, but The work that makes substantial progress is simultaneously few.It is heterogeneous that Mohammad Qureshi etc. are prepared for three-dimensional NiO-CdS using hydro-thermal method Knot classification bouquet structure, shows as NiO nanometer particle loads (Journal of Materials on CdS microballoons Chemistry,2012,22(24):12090-12095)。
It can be seen from literature survey, the work of the NiO-CdS composites of core shell structure almost blank, and use easy Ways for education footpath prepares core shell structure NiO-CdS Coaxial Nanofibers there is not yet report.
The content of the invention
It is an object of the invention to provide core shell structure NiO-CdS Coaxial Nanofibers and preparation method thereof, to fill up existing There is the blank of technology.
The purpose of the present invention is achieved by the following technical solution.
The technical scheme is that core shell structure NiO-CdS Coaxial Nanofibers are prepared using chemical synthesising technology, its Concrete technology flow process is as follows:
(1) 1mmol nickel acetates (Ni (CH are weighed3COO)2·H2) and 2mmol ammonium oxalate ((NH O4)2C2O4·H2O) arrive The high pin beakers of 100mL, add 50mL H2O, stirring and dissolving adds a certain amount of triethylamine, continues to stir 20 minutes;
(2) above-mentioned reaction mixture is placed in water-bath, temperature setting is 80, DEG C isothermal reaction 3 hours, natural cooling, Suction filtration, washing, dry nickeliferous sediment, nickeliferous sediment is put into resistance furnace, sets certain temperature, and heat treatment 1 is small When, collect NiO nano powders;
(3) 0.1g NiO are weighed, 30mL (Cd (CH containing a certain amount of cadmium acetate are added to3COO)2·2H2O) in the aqueous solution, surpass Sound is scattered 10~20 minutes, obtains dispersion liquid A;
(4) 1mmol thiocarbamides are weighed, 30mL deionized waters are added, 0.1mL ethylenediamines are added dropwise, solution B is dissolved to obtain;
(5) solution B is added in dispersion liquid A, magnetic agitation 12 hours, reaction mixture is placed in household microwave oven, Low fire screen is set to heat 30 minutes;
(6) after reaction terminates, filtering precipitate, uses absolute ethyl alcohol and distills water washing 3~5 times, will precipitate respectively while hot Thing is placed in vacuum drying chamber and dried 4~8 hours, and temperature is 40~60 DEG C, produces core shell structure NiO-CdS co-axial nanos fine Dimension.
In above-mentioned technical proposal, the amount of triethylamine is 0.6~1.0mL in step (1).
Resistance furnace described in step (2) sets temperature to be 400~600 DEG C.
The amount of cadmium acetate material described in step (3) is 0.4~1.0mmol.
The microwave power of low fire screen is 144W in step (5).
The core shell structure NiO-CdS Coaxial Nanofibers that the present invention is obtained are a kind of novel semiconductors coupling metal oxidations Thing, all has huge application prospect in terms of optoelectronic pole material, production hydrogen, air-sensitive, catalysis, photoelectric device.Raw material is easy to get, into This cheap, suitable industrialized production.
Brief description of the drawings
Fig. 1 is X-ray diffraction (XRD) figure of core shell structure NiO-CdS Coaxial Nanofibers of the present invention.
Fig. 2 is power spectrum (EDS) constituent analysis figure of core shell structure NiO-CdS Coaxial Nanofibers of the present invention.
Fig. 3 is low power SEM (SEM) photo of core shell structure NiO-CdS Coaxial Nanofibers of the present invention.
Fig. 4 is high power SEM (SEM) photo of core shell structure NiO-CdS Coaxial Nanofibers of the present invention.
Embodiment
Make further detailed complete description to technical scheme below by way of specific embodiment.Following reality It is that the present invention is further illustrated to apply example, and is not limited the scope of the invention.
Embodiment 1
The technical scheme is that core shell structure NiO-CdS Coaxial Nanofibers are prepared using chemical synthesising technology, its Concrete technology flow process is as follows:
(1) 1mmol nickel acetates (Ni (CH are weighed3COO)2·4H2) and 2mmol ammonium oxalate ((NH O4)2C2O4·H2O) arrive The high pin beakers of 100mL, add 50mL H2O, stirring and dissolving adds 0.8mL triethylamines, continues to stir 20 minutes;
(2) above-mentioned reaction mixture is placed in water-bath, temperature setting is 80, DEG C isothermal reaction 3 hours, natural cooling, Suction filtration, washing, dry nickeliferous sediment, nickeliferous sediment is put into resistance furnace, and it is 500 DEG C to set temperature, heat treatment 1 Hour, collect NiO nano powders;
(3) 0.1g NiO are weighed, 30mL cadmium acetates containing 0.6mmol (Cd (CH are added to3COO)2·2H2O) in the aqueous solution, Ultrasonic disperse 10 minutes, obtains dispersion liquid A;
(4) 1mmol thiocarbamides are weighed, 30mL deionized waters are added, 0.1mL ethylenediamines are added dropwise, solution B is dissolved to obtain;
(5) solution B is added in dispersion liquid A, magnetic agitation 12 hours, reaction mixture is placed in household microwave oven, Low fire screen is set to heat 30 minutes;
(6) after reaction terminates, filtering precipitate, uses absolute ethyl alcohol and distills water washing 3~5 times, will precipitate respectively while hot Thing is placed in vacuum drying chamber and dried 6 hours, and temperature is 50 DEG C, produces core shell structure NiO-CdS Coaxial Nanofibers.
Referring to accompanying drawing 1, the X-ray of core shell structure NiO-CdS Coaxial Nanofibers is spread out as made from the methods described of embodiment 1 Penetrate 37.25 in (XRD) collection of illustrative plates, figureo、43.27oWith 62.86oLocate three peaks occurring can index for Emission in Cubic nickel oxide (111), the diffraction maximum of (200) and (220) three crystal faces, it is consistent with the diffraction maximum of JCPDS cards (47-1049) nickel oxide.Figure In remaining spectral line peak correspond to the cadmium sulfide of hexagonal phase, it is consistent with JCPDS cards (41-1049).Show prepared product For NiO-CdS compounds.
Referring to accompanying drawing 2, the power spectrum of core shell structure NiO-CdS Coaxial Nanofibers as made from the methods described of embodiment 1 (EDS) tetra- kinds of chemical elements of O, Ni, Cd and S are detected in constituent analysis figure, spectrogram.
Referring to accompanying drawing 3, the low power of core shell structure NiO-CdS Coaxial Nanofibers is swept as made from the methods described of embodiment 1 Electron microscope (SEM) photo is retouched, as illustrated, product is filamentary structure, a diameter of 130~280nm, a length of 0.8~2 μ m。
Referring to accompanying drawing 4, the high power of core shell structure NiO-CdS Coaxial Nanofibers is swept as made from the methods described of embodiment 1 Electron microscope (SEM) photo is retouched, as illustrated, centronucleus is NiO nanofibers, external shell is CdS nanocrystals, and CdS receives Rice crystal grain is closely coated on the outside of NiO nanofibers, forms coaxial cable formula core shell structure.
Embodiment 2
The technical scheme is that core shell structure NiO-CdS Coaxial Nanofibers are prepared using chemical synthesising technology, its Concrete technology flow process is as follows:
(1) 1mmol nickel acetates (Ni (CH are weighed3COO)2·4H2) and 2mmol ammonium oxalate ((NH O4)2C2O4·H2O) arrive The high pin beakers of 100mL, add 50mL H2O, stirring and dissolving adds 1.0mL triethylamines, continues to stir 20 minutes;
(2) above-mentioned reaction mixture is placed in water-bath, temperature setting is 80 DEG C, isothermal reaction 3 hours, natural cooling, Suction filtration, washing, dry nickeliferous sediment, nickeliferous sediment is put into resistance furnace, and it is 450 DEG C to set temperature, heat treatment 1 Hour, collect NiO nano powders;
(3) 0.1g NiO are weighed, 30mL cadmium acetates containing 0.8mmol (Cd (CH are added to3COO)2·2H2O) in the aqueous solution, Ultrasonic disperse 15 minutes, obtains dispersion liquid A;
(4) 1mmol thiocarbamides are weighed, 30mL deionized waters are added, 0.1mL ethylenediamines are added dropwise, solution B is dissolved to obtain;
(5) solution B is added in dispersion liquid A, magnetic agitation 12 hours, reaction mixture is placed in household microwave oven, Low fire screen is set to heat 30 minutes;
(6) after reaction terminates, filtering precipitate, uses absolute ethyl alcohol and distills water washing 3~5 times, will precipitate respectively while hot Thing is placed in vacuum drying chamber and dried 6 hours, and temperature is 60 DEG C, produces core shell structure NiO-CdS Coaxial Nanofibers.
Detected through XRD, EDS and SEM, it is fine for core shell structure NiO-CdS co-axial nanos as made from the methods described of embodiment 2 Dimension.
Embodiment 3
The technical scheme is that core shell structure NiO-CdS Coaxial Nanofibers are prepared using chemical synthesising technology, its Concrete technology flow process is as follows:
(1) 1mmol nickel acetates (Ni (CH are weighed3COO)2·4H2) and 2mmol ammonium oxalate ((NH O4)2C2O4·H2O) arrive The high pin beakers of 100mL, add 50mL H2O, stirring and dissolving adds 0.6mL triethylamines, continues to stir 20 minutes;
(2) above-mentioned reaction mixture is placed in water-bath, temperature setting is 80 DEG C, isothermal reaction 3 hours, natural cooling, Suction filtration, washing, dry nickeliferous sediment, nickeliferous sediment is put into resistance furnace, and it is 550 DEG C to set temperature, heat treatment 1 Hour, collect NiO nano powders;
(3) 0.1g NiO are weighed, 30mL cadmium acetates containing 0.4mmol (Cd (CH are added to3COO)2·2H2O) in the aqueous solution, Ultrasonic disperse 15 minutes, obtains dispersion liquid A;
(4) 1mmol thiocarbamides are weighed, 30mL deionized waters are added, 0.1mL ethylenediamines are added dropwise, solution B is dissolved to obtain;
(5) solution B is added in dispersion liquid A, magnetic agitation 12 hours, reaction mixture is placed in household microwave oven, Low fire screen is set to heat 30 minutes;
(6) after reaction terminates, filtering precipitate, uses absolute ethyl alcohol and distills water washing 3~5 times, will precipitate respectively while hot Thing is placed in vacuum drying chamber and dried 8 hours, and temperature is 40 DEG C, produces core shell structure NiO-CdS Coaxial Nanofibers.
Detected through XRD, EDS and SEM, it is fine for core shell structure NiO-CdS co-axial nanos as made from the methods described of embodiment 3 Dimension.
Embodiment 4
The technical scheme is that core shell structure NiO-CdS Coaxial Nanofibers are prepared using chemical synthesising technology, its Concrete technology flow process is as follows:
(1) 1mmol nickel acetates (Ni (CH are weighed3COO)2·4H2) and 2mmol ammonium oxalate ((NH O4)2C2O4·H2O) arrive The high pin beakers of 100mL, add 50mL H2O, stirring and dissolving adds 0.8mL triethylamines, continues to stir 20 minutes;
(2) above-mentioned reaction mixture is placed in water-bath, temperature setting is 80 DEG C, isothermal reaction 3 hours, natural cooling, Suction filtration, washing, dry nickeliferous sediment, nickeliferous sediment is put into resistance furnace, and it is 600 DEG C to set temperature, heat treatment 1 Hour, collect NiO nano powders;
(3) 0.1g NiO are weighed, 30mL cadmium acetates containing 1.0mmol (Cd (CH are added to3COO)2·2H2O) in the aqueous solution, Ultrasonic disperse 20 minutes, obtains dispersion liquid A;
(4) 1mmol thiocarbamides are weighed, 30mL deionized waters are added, 0.1mL ethylenediamines are added dropwise, solution B is dissolved to obtain;
(5) solution B is added in dispersion liquid A, magnetic agitation 12 hours, reaction mixture is placed in household microwave oven, Low fire screen is set to heat 30 minutes;
(6) after reaction terminates, filtering precipitate, uses absolute ethyl alcohol and distills water washing 3~5 times, will precipitate respectively while hot Thing is placed in vacuum drying chamber and dried 6 hours, and temperature is 50 DEG C, produces core shell structure NiO-CdS Coaxial Nanofibers.
Detected through XRD, EDS and SEM, it is fine for core shell structure NiO-CdS co-axial nanos as made from the methods described of embodiment 4 Dimension.
Embodiment 5
The technical scheme is that core shell structure NiO-CdS Coaxial Nanofibers are prepared using chemical synthesising technology, its Concrete technology flow process is as follows:
(1) 1mmol nickel acetates (Ni (CH are weighed3COO)2·4H2) and 2mmol ammonium oxalate ((NH O4)2C2O4·H2O) arrive The high pin beakers of 100mL, add 50mL H2O, stirring and dissolving adds 0.9mL triethylamines, continues to stir 20 minutes;
(2) above-mentioned reaction mixture is placed in water-bath, temperature setting is 80 DEG C, isothermal reaction 3 hours, natural cooling, Suction filtration, washing, dry nickeliferous sediment, nickeliferous sediment is put into resistance furnace, and it is 500 DEG C to set temperature, heat treatment 1 Hour, collect NiO nano powders;
(3) 0.1g NiO are weighed, 30mL cadmium acetates containing 0.7mmol (Cd (CH are added to3COO)2·2H2O) in the aqueous solution, Ultrasonic disperse 10 minutes, obtains dispersion liquid A;
(4) 1mmol thiocarbamides are weighed, 30mL deionized waters are added, 0.1mL ethylenediamines are added dropwise, solution B is dissolved to obtain;
(5) solution B is added in dispersion liquid A, magnetic agitation 12 hours, reaction mixture is placed in household microwave oven, Low fire screen is set to heat 30 minutes;
(6) after reaction terminates, filtering precipitate, uses absolute ethyl alcohol and distills water washing 3~5 times, will precipitate respectively while hot Thing is placed in vacuum drying chamber and dried 7 hours, and temperature is 55 DEG C, produces core shell structure NiO-CdS Coaxial Nanofibers.
Detected through XRD, EDS and SEM, it is fine for core shell structure NiO-CdS co-axial nanos as made from the methods described of embodiment 5 Dimension.

Claims (5)

1. core shell structure NiO-CdS Coaxial Nanofibers, it is characterised in that described core shell structure NiO-CdS co-axial nanos are fine Tie up as threadiness, a diameter of 130~280nm, a length of 0.8~2 μm, centronucleus is NiO nanofibers, and external shell is CdS nanometers Crystal grain, CdS nanocrystals are closely coated on the outside of NiO nanofibers, form coaxial cable formula core shell structure.
2. the preparation method of the core shell structure NiO-CdS Coaxial Nanofibers described in claim 1, it is characterised in that the side The concrete technology step of method is as follows:
(1) 1mmol nickel acetates (Ni (CH are weighed3COO)2·4H2) and 2mmol ammonium oxalate ((NH O4)2C2O4·H2O it is) high to 100mL Pin beaker, adds 50mL H2O, stirring and dissolving adds 0.6~1.0mL triethylamines, continues to stir 20 minutes;
(2) above-mentioned reaction mixture is placed in water-bath, temperature setting is 80 DEG C, isothermal reaction 3 hours, natural cooling, suction filtration, Washing, dry nickeliferous sediment, nickeliferous sediment is put into resistance furnace, and it is 400~600 DEG C to set temperature, heat treatment 1 Hour, collect NiO nano powders;
(3) 0.1g NiO are weighed, 30mL (Cd (CH containing 0.4~1.0mmol cadmium acetates are added to3COO)2·2H2O) in the aqueous solution, Ultrasonic disperse 10~20 minutes, obtains dispersion liquid A;
(4) 1mmol thiocarbamides are weighed, 30mL deionized waters are added, 0.1mL ethylenediamines are added dropwise, solution B is dissolved to obtain;
(5) solution B is added in dispersion liquid A, magnetic agitation 12 hours, reaction mixture is placed in household microwave oven, set Low fire screen is heated 30 minutes;
(6) after reaction terminates, filtering precipitate, uses absolute ethyl alcohol and distills water washing 3~5 times, sediment is put respectively while hot Dried 4~8 hours in vacuum drying chamber, temperature is 40~60 DEG C, produces core shell structure NiO-CdS Coaxial Nanofibers.
3. the preparation method of core shell structure NiO-CdS Coaxial Nanofibers according to claim 2, it is characterised in that step Suddenly in (1), the amount of triethylamine is 0.8mL.
4. the preparation method of core shell structure NiO-CdS Coaxial Nanofibers according to claim 2, it is characterised in that step Suddenly in (2), resistance furnace sets temperature to be 500 DEG C.
5. the preparation method of core shell structure NiO-CdS Coaxial Nanofibers according to claim 2, it is characterised in that step Suddenly in (3), the amount of cadmium acetate material is 0.6mmol.
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