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 PDFInfo
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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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- 239000011258 core-shell material Substances 0.000 title claims abstract description 46
- 239000002121 nanofiber Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 239000000243 solution Substances 0.000 claims abstract description 17
- 239000006185 dispersion Substances 0.000 claims abstract description 16
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 239000013049 sediment Substances 0.000 claims abstract description 16
- 239000002244 precipitate Substances 0.000 claims abstract description 14
- LHQLJMJLROMYRN-UHFFFAOYSA-L cadmium acetate Chemical compound [Cd+2].CC([O-])=O.CC([O-])=O LHQLJMJLROMYRN-UHFFFAOYSA-L 0.000 claims abstract description 10
- 230000005291 magnetic effect Effects 0.000 claims abstract description 9
- 238000013019 agitation Methods 0.000 claims abstract description 8
- VBIXEXWLHSRNKB-UHFFFAOYSA-N ammonium oxalate Chemical compound [NH4+].[NH4+].[O-]C(=O)C([O-])=O VBIXEXWLHSRNKB-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000007864 aqueous solution Substances 0.000 claims abstract description 8
- 150000002171 ethylene diamines Chemical class 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 239000011858 nanopowder Substances 0.000 claims abstract description 8
- 239000003643 water by type Substances 0.000 claims abstract description 8
- 239000002159 nanocrystal Substances 0.000 claims abstract description 4
- 238000005516 engineering process Methods 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 15
- 239000011541 reaction mixture Substances 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 14
- 238000005406 washing Methods 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 13
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 239000004567 concrete Substances 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims description 7
- AIYYMMQIMJOTBM-UHFFFAOYSA-L nickel(ii) acetate Chemical class [Ni+2].CC([O-])=O.CC([O-])=O AIYYMMQIMJOTBM-UHFFFAOYSA-L 0.000 claims description 7
- 238000000967 suction filtration Methods 0.000 claims description 7
- 238000001291 vacuum drying Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 241000549556 Nanos Species 0.000 claims description 6
- 239000013078 crystal Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 abstract description 2
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 abstract 1
- 238000001354 calcination Methods 0.000 abstract 1
- 229940078494 nickel acetate Drugs 0.000 abstract 1
- 229910052980 cadmium sulfide Inorganic materials 0.000 description 44
- 239000000126 substance Substances 0.000 description 8
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 239000004065 semiconductor Substances 0.000 description 6
- 239000002131 composite material Substances 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000002114 nanocomposite Substances 0.000 description 3
- 229910000480 nickel oxide Inorganic materials 0.000 description 3
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000005693 optoelectronics Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 description 1
- 235000006506 Brasenia schreberi Nutrition 0.000 description 1
- 244000267222 Brasenia schreberi Species 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 229910052729 chemical element Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/04—Oxides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G11/00—Compounds of cadmium
- C01G11/02—Sulfides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Organic Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Composite Materials (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Catalysts (AREA)
- Powder Metallurgy (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
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
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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