CN106186047B - One kind is based on secondary nanosphere hierarchical Z nO nano materials and preparation method thereof - Google Patents
One kind is based on secondary nanosphere hierarchical Z nO nano materials and preparation method thereof Download PDFInfo
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- CN106186047B CN106186047B CN201610634822.4A CN201610634822A CN106186047B CN 106186047 B CN106186047 B CN 106186047B CN 201610634822 A CN201610634822 A CN 201610634822A CN 106186047 B CN106186047 B CN 106186047B
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- 239000002086 nanomaterial Substances 0.000 title claims abstract description 66
- 239000002077 nanosphere Substances 0.000 title claims abstract description 63
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 111
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000004202 carbamide Substances 0.000 claims abstract description 15
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims abstract description 14
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims abstract description 14
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims abstract description 14
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000005642 Oleic acid Substances 0.000 claims abstract description 14
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims abstract description 14
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims abstract description 14
- YZYKBQUWMPUVEN-UHFFFAOYSA-N zafuleptine Chemical compound OC(=O)CCCCCC(C(C)C)NCC1=CC=C(F)C=C1 YZYKBQUWMPUVEN-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000000243 solution Substances 0.000 claims description 109
- 238000003756 stirring Methods 0.000 claims description 21
- 238000011049 filling Methods 0.000 claims description 20
- 239000013049 sediment Substances 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 239000011259 mixed solution Substances 0.000 claims description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000005119 centrifugation Methods 0.000 claims description 10
- 238000010792 warming Methods 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims 1
- 238000002156 mixing Methods 0.000 claims 1
- 238000005406 washing Methods 0.000 claims 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 abstract description 85
- 239000011787 zinc oxide Substances 0.000 abstract description 42
- 230000002708 enhancing effect Effects 0.000 abstract description 7
- 239000002096 quantum dot Substances 0.000 abstract description 4
- 238000006243 chemical reaction Methods 0.000 description 20
- 239000000463 material Substances 0.000 description 19
- 238000001816 cooling Methods 0.000 description 16
- 239000002105 nanoparticle Substances 0.000 description 9
- 239000002245 particle Substances 0.000 description 7
- 238000001228 spectrum Methods 0.000 description 7
- 238000000034 method Methods 0.000 description 5
- 230000005476 size effect Effects 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 5
- 239000011701 zinc Substances 0.000 description 5
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 230000001590 oxidative effect Effects 0.000 description 4
- 230000035945 sensitivity Effects 0.000 description 4
- 229910052725 zinc Inorganic materials 0.000 description 4
- 238000000862 absorption spectrum Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 239000002073 nanorod Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- 238000004847 absorption spectroscopy Methods 0.000 description 2
- 239000010405 anode material Substances 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000001413 cellular effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 238000004020 luminiscence type Methods 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- 101100136092 Drosophila melanogaster peng gene Proteins 0.000 description 1
- 241000257465 Echinoidea Species 0.000 description 1
- 244000283207 Indigofera tinctoria Species 0.000 description 1
- 244000131316 Panax pseudoginseng Species 0.000 description 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000008358 core component Substances 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
- 238000009792 diffusion process Methods 0.000 description 1
- JRBPAEWTRLWTQC-UHFFFAOYSA-N dodecylamine Chemical compound CCCCCCCCCCCCN JRBPAEWTRLWTQC-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 235000008434 ginseng Nutrition 0.000 description 1
- 230000009931 harmful effect Effects 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000036314 physical performance Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000002123 temporal effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 229910052984 zinc sulfide Inorganic materials 0.000 description 1
- KFWJXQPJTRYYQW-UHFFFAOYSA-N zinc;carbonic acid;oxygen(2-) Chemical compound [O-2].[Zn+2].OC(O)=O KFWJXQPJTRYYQW-UHFFFAOYSA-N 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
- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/20—Light-sensitive devices
- H01G9/2027—Light-sensitive devices comprising an oxide semiconductor electrode
- H01G9/204—Light-sensitive devices comprising an oxide semiconductor electrode comprising zinc oxides, e.g. ZnO
-
- 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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- 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
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
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- 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
- C01P2002/84—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by UV- or VIS- data
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- 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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- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/542—Dye sensitized solar cells
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Abstract
The present invention relates to quantum dot solar cell field, and in particular to one kind is based on secondary nanosphere hierarchical Z nO nano materials and preparation method thereof.One kind is based on secondary nanosphere hierarchical Z nO nano materials, it is characterised in that：It is prepared by the solution comprising zinc acetate dihydrate, dimethylformamide, urea, oleic acid, dimethylformamide；Zinc acetate dihydrate, dimethylformamide, urea, oleic acid, the proportioning of solution of dimethylformamide are：0.65‑1.3g：100‑200ml：0.4g：0.1ml：30ml.Of the invention equipment requirement is not high compared with common zinc oxide, absorbs luminous intensity enhancing, the increase of photoresponse scope.
Description
Technical field
The present invention relates to quantum dot solar cell field, and in particular to a kind of hierarchy based on secondary nanosphere
ZnO nano material and preparation method thereof.
Background technology
It is well known that the energy is the key point for supporting rapid economic development.In recent years along with economy prosperity and development,
The whole world is faced with increasingly serious environmental pollution and energy shortage problem.How rich reserves, green safe are developed
Novel energy is increasingly becoming the effective way of the current energy problem of solution of people's common concern.As it is a kind of it is pollution-free, can be again
Raw new energy, effective utilize of solar energy are expected to alleviate human society and environmental problem.Solar cell can realize photoelectric direct
Conversion is connect, is the maximally effective new device using solar energy.
Light anode is the core component of battery, and key effect is played in terms of the charge-trapping and transmission in photoelectric process.
At present, effect it is best, be TiO using more light anode material2.With the further investigation to photo-anode film, scholars
Start to be directed to developing to remove TiO2Outer other potential semi-conducting materials.By contrasting ZnO and TiO2Related physical performance ginseng
Number is found, in the conductor oxidate of numerous broad-band gaps, the energy gaps of ZnO at room temperature are 3.2e V or so and TiO2The most
It is close.Also, ZnO electron mobility and electron diffusion coefficient are above TiO2, it is the light anode material for having very much application potential
Material.The nano zinc oxide material of current research is mostly zero dimension, one-dimensional and two-dimentional structure, but its development is by specific surface area
It is less than normal and capture visible ray it is indifferent wait limit.Therefore, the material of simple to operate, function admirable graded structure is researched and developed
Material has important prospect.In recent years, scientists propose the concept of the three-dimensional hierarchical structure of zinc oxide, not only effective comprehensive
Advantage in zero dimension, one-dimensional, each self-structure of two-dimensional structure, and its unique space structure, make it remain nano material
Nano-particle can also be overcome the harmful effect such as easily to assemble outside the physicochemical property of script.Cellular construction assemble simultaneously after can cause
Synergy and coupling, can be improved the performance of original material.
In recent years, three-dimensional or level structure nano material increasingly attracts people's attention.Current scholars are directed to
The three-dimensional hierarchical structure nano material of zinc oxide has carried out a series of research, and makes some progress.Jin Li
Et al. reacted by adjusting hydrothermal in urea content, obtain stratiform bicarbonate zinc oxide material, by calcining.Divided
The porous ZnO material of grade, and the material has higher sensitivity characteristic to acetone gas.Peng Sun et al. are successfully synthesized
The graduation SnO that is made up of the porous nanometer sheet of monocrystalline2Material, and the experiment of hydro-thermal temporal evolution is combined, infer this material
Expect self assembly growth course, and to material carry out vapor sensitivity test, find its have preferable gas-sensitive property relative to
Alcohol gas.Chong Wang et al. obtain flower-shaped graduate WO using acidic treatment3Material, and detect it to NO2Gas
With sensitivity characteristic.Yuxiang Qin et al. are using Seed Layer induction hydrothermal synthesis method, by flower-shaped and cellular graduation
V2O5Material growth, by performance test, finds this material in room temperature and work temperature in the alumina substrate with platinum electrode
Spend for 250 DEG C when alcohol gas are shown with higher sensitivity.Liu etc. adds small of spherical Zn powder in reaction solution
Grain and in this, as nuclearing centre, the three-dimensional ball formed by ZnO nanorod cluster is prepared for using hydro-thermal method in alkali system
Shape body, research finds about 4 μm of the chondritic diameter, and has good optical property.Xie etc. is using lauryl amine as additive
It is prepared for the three-dimensional hierarchy of sea urchin shape ZnO nanorod base, the One-Dimensional ZnO nanorod diameter in products therefrom is 50-80nm,
About 2 μm of length, there is strong ultraviolet excitation performance at room temperature.
Do not retrieve based on secondary nanosphere hierarchical Z nO nano materials and preparation method thereof identical patent document.
The content of the invention
It is an object of the invention to provide one kind to be based on secondary nanosphere hierarchical Z nO nano materials and preparation method thereof,
Equipment requirement is not high, absorbs luminous intensity enhancing, the increase of photoresponse scope.
To achieve the above object, the technical solution adopted in the present invention is a kind of hierarchy based on secondary nanosphere
ZnO nano material, it is characterised in that：It is by comprising zinc acetate dihydrate, dimethylformamide, urea, oleic acid, dimethyl formyl
The solution of amine is prepared；Zinc acetate dihydrate, dimethylformamide, urea, oleic acid, dimethylformamide solution proportioning
For：0.65-1.3g：100-200ml：0.4g：0.1ml：30ml.
The diameter of described secondary nanometer ball particle is about 6-15nm.
A kind of above-mentioned preparation method based on secondary nanosphere hierarchical Z nO nano materials, it is characterised in that including with
Lower step：
1) 0.65-1.3g zinc acetate dihydrate is weighed, is added in 100-200ml dimethylformamide and stirs to abundant
Dissolving, solution A is labeled as by the mixed solution；
2) weigh 0.4g urea and measure 0.1ml oleic acid, both then are added into 30ml concentration respectively is
In the solution of 99.5wt% dimethylformamide, the solution is labeled as B solution；
3) first the beaker for filling solution A is placed in water-bath, under the conditions of 65-95 DEG C of keeping temperature, water-bath 3-7h；It
Afterwards, solution A (above-mentioned reaction system) is cooled down with frozen water, it is cooled down rapidly；
4) under rapid stirring (150 revs/min of rotating speed), the B solution in step 2) is added dropwise to
In the solution A { reaction system of step 3) } of cooling, the mixed solution is labeled as C solution；
5) beaker for filling C solution is again placed in water-bath, is warming up to 50 DEG C and keeps 1h；
6) C solution after water-bath is cooled down with frozen water, is placed in centrifuge tube centrifuges afterwards；
7) first washed 3 times with dimethylformamide, and take out the sediment after centrifugation, then by the sediment with anhydrous second
Alcohol fully washs final white product；
8) above-mentioned white product is dried, and produces the hierarchical Z nO nano materials based on secondary nanosphere.
The absorption luminous intensity enhancing of hierarchical Z nO nano materials based on secondary nanosphere, the increase of photoresponse scope, and
And compared with common commercial ZnO, it is launched and Absorption edge is also changed.
One kind is further prepared using solvent-thermal method and is based on secondary nanosphere hierarchical Z nO nano materials, the classification knot
Structure is made up of multiple nano granular of zinc oxide, and its diameter is about 200-350nm, and the diameter of wherein individual particle is about 4-
15nm。
The present invention has advantages below：1) present invention prepares a kind of classification knot based on secondary nanosphere using solvent-thermal method
Structure ZnO nano material, it is simple and easy, cost is relatively low (equipment requirement is not high)；2) the hierarchical Z nO nanometer materials that the present invention synthesizes
Expect clear in structure, wherein hierarchy zinc oxide is made up of multiple spherical nanoparticles；3) what the present invention synthesized is received based on secondary
The hierarchical Z nO nano materials fluorescence intensity enhancing of rice ball, the increase of photoresponse scope, and due to nanometer size effect, its
Absorption edge also there occurs blue shift (characteristic of transmitting and absorption band blue shift), shows that the material is more easy to be optically excited, so as to reach
To the purpose for improving quantum dot solar cell efficiency.It can be applied to quantum dot solar cell, Aero-Space and material
Deng field.
Brief description of the drawings
Fig. 1 is to scheme (the b in figure based on secondary nanosphere hierarchical Z nO nano materials SEM in the embodiment of the present invention 1,7
It is the enlarged drawing of a in figure).
Fig. 2 is to scheme (the b in figure based on secondary nanosphere hierarchical Z nO nano materials SEM in the embodiment of the present invention 2,8
It is the enlarged drawing of a in figure).
Fig. 3 is the XRD based on secondary nanosphere hierarchical Z nO nano materials and ZnO in the embodiment of the present invention 3.
Fig. 4 is the infared spectrum based on secondary nanosphere hierarchical Z nO nano materials and ZnO in the embodiment of the present invention 3.
Fig. 5 is to be based on secondary nanosphere hierarchical Z nO nano material SEM and TEM collection of illustrative plates in the embodiment of the present invention 3.
Fig. 6 is the UV, visible light based on secondary nanosphere hierarchical Z nO nano materials and ZnO in the embodiment of the present invention 3
Absorption spectrum.
Fig. 7 is the luminescence generated by light based on secondary nanosphere hierarchical Z nO nano materials and ZnO in the embodiment of the present invention 3
Spectrum.
Fig. 8 is to be schemed in the embodiment of the present invention 5 based on secondary nanosphere hierarchical Z nO nano materials SEM.
Embodiment
In order that this area researcher is better understood by the present invention, spy provides specific implementation case and further deeply explained
It is bright, but the invention is not limited in following embodiment.
Embodiment 1：
A kind of preparation method based on secondary nanosphere hierarchical Z nO nano materials, comprises the following steps：
1) 0.65g zinc acetate dihydrate is weighed, being added to stirring in 100ml dimethylformamide, will to abundant dissolving
The mixed solution is labeled as solution A；
2) weigh 0.4g urea and measure 0.1ml oleic acid, both then are added into 30ml concentration respectively is
In the solution of 99.5wt% dimethylformamide, the solution is labeled as B solution；
3) first the beaker for filling solution A is placed in water-bath, under the conditions of 70 DEG C of keeping temperature, water-bath 5h；Afterwards, ice is used
Water cooling solution A (above-mentioned reaction system), makes it cool down rapidly；
4) under rapid stirring (150 revs/min of rotating speed), the B solution in step 2) is added dropwise to
In the solution A { reaction system of step 3) } of cooling, the mixed solution is labeled as C solution；
5) beaker for filling C solution is again placed in water-bath, is warming up to 50 DEG C and keeps 1h；
6) C solution after water-bath is cooled down with frozen water, is placed in centrifuge tube centrifuges afterwards；
9) first washed 3 times with dimethylformamide, and take out the sediment after centrifugation, then by the sediment with anhydrous second
Alcohol fully washs final white product；
8) above-mentioned white product is dried, and produces the hierarchical Z nO nano materials based on secondary nanosphere.
The hierarchical Z nO nano materials based on secondary nanosphere in embodiment 1, wherein Fig. 1 are the embodiment of the present invention 1
The SEM figures of middle gained nano material, primary structure zinc oxide is the nanometer rods of secondary oxidative zinc nanoparticles composition as seen from the figure,
The length of wherein nanometer rods is about 100nm, and diameter is about 20nm, and the diameter of secondary structure nanosphere individual particle is about 6nm.
Embodiment 2：
A kind of preparation method based on secondary nanosphere hierarchical Z nO nano materials, comprises the following steps：
1) 0.65g zinc acetate dihydrate is weighed, being added to stirring in 100ml dimethylformamide, will to abundant dissolving
The mixed solution is labeled as solution A；
2) weigh 0.4g urea and measure 0.1ml oleic acid, both then are added into 30ml concentration respectively is
In the solution of 99.5wt% dimethylformamide, the solution is labeled as B solution；
3) first the beaker for filling solution A is placed in water-bath, under the conditions of 80 DEG C of keeping temperature, water-bath 5h；Afterwards, ice is used
The above-mentioned reaction system of water cooling, makes it cool down rapidly；
4) under rapid stirring (150 revs/min of rotating speed), the B solution in step 2) is added dropwise to
In the solution A { reaction system of step 3) } of cooling, the mixed solution is labeled as C solution；
5) beaker for filling C solution is again placed in water-bath, is warming up to 50 DEG C and keeps 1h；
6) C solution after water-bath is cooled down with frozen water, is placed in centrifuge tube centrifuges afterwards；
7) first washed 3 times with dimethylformamide, and take out the sediment after centrifugation, then by the sediment with anhydrous second
Alcohol fully washs final white product；
8) above-mentioned white product is dried, and produces the hierarchical Z nO nano materials based on secondary nanosphere.
Fig. 2 is the SEM figures of the hierarchical Z nO nano materials based on secondary nanosphere in the embodiment 2, as seen from the figure should
Primary structure zinc oxide is the ellipsoid structure of secondary oxidative zinc nanoparticles composition, and the length of wherein ellipsoid is about 300nm, straight
Footpath is about 200nm, and the diameter of the individual particle of secondary structure nanosphere is about 8nm.
Embodiment 3：
A kind of preparation method based on secondary nanosphere hierarchical Z nO nano materials, comprises the following steps：
1) 0.65g zinc acetate dihydrate is weighed, being added to stirring in 100ml dimethylformamide, will to abundant dissolving
The mixed solution is labeled as solution A；
2) weigh 0.4g urea and measure 0.1ml oleic acid, both then are added into 30ml concentration respectively is
In the solution of 99.5wt% dimethylformamide, the solution is labeled as B solution；
3) first the beaker for filling solution A is placed in water-bath, under the conditions of 90 DEG C of keeping temperature, water-bath 5h；Afterwards, ice is used
The above-mentioned reaction system of water cooling, makes it cool down rapidly；
4) under rapid stirring (150 revs/min of rotating speed), the B solution in step 2) is added dropwise to
The mixed solution { in the reaction system of step 3), is labeled as C solution by the solution A of cooling；
5) beaker for filling C solution is again placed in water-bath, is warming up to 50 DEG C and keeps 1h；
6) C solution after water-bath is cooled down with frozen water, is placed in centrifuge tube centrifuges afterwards；
7) first washed 3 times with dimethylformamide, and take out the sediment after centrifugation, then by the sediment with anhydrous second
Alcohol fully washs final white product；
8) above-mentioned white product is dried, and produces the hierarchical Z nO nano materials based on secondary nanosphere.
Obtained by embodiment 3 is white powder based on secondary nanosphere hierarchical Z nO nano materials, wherein one
Level structure zinc oxide sphere diameter about 350nm, the diameter of the individual particle of secondary structure nanosphere is about 8nm.
The XRD of hierarchical Z nO nano materials and common ZnO in the embodiment of the present invention 3 based on secondary nanosphere is such as
Shown in Fig. 3, know that sample XRD spectrum and pure ZnO have consistent diffraction maximum, and the hexagonal wurtzite structure of ZnO standard spectral peaks by figure
(JCPDS card 36-1451) coincide.However, compared with common ZnO XRD diffraction patterns, the hierarchy of secondary nanosphere
The obvious widthization of the diffraction maximum of ZnO nano material XRD, this exists mainly due to caused by quantum size effect with its surface
Nano ZnO particles are relevant.
Infared spectrum based on secondary nanosphere hierarchical Z nO nano materials and common ZnO in the embodiment of the present invention is such as
Shown in Fig. 4, both show uniformity, and obvious ZnO characteristic peak is shown in figure；465cm-1The peak at place is ZnO's
Characteristic peak, 1415cm-1And 1560cm-1It is due to that the vibration peaks of C=C and C=O groups causes respectively, these groups are probably system
What standby process introduced, in addition, 3440cm-1The peak at place belongs to-OH vibration peaks；Infared spectrum shows that both almost do not have difference, enter
One step shows that hierarchical Z nO nano materials based on secondary nanosphere and common ZnO structures are identicals.
SEM figures and TEM figures based on secondary nanosphere hierarchical Z nO nano materials in the embodiment of the present invention 3, such as Fig. 5 a
It is shown；Prepared ZnO primary structures are spherical in shape, and than more uniform, a diameter of 240nm or so, Fig. 5 b-c show this
Primary structure is made up of smaller nanosphere, has an obvious hierarchy feature, transmission electron microscope picture 5d show this two
A diameter of 8nm of nanometer bead of level structure or so.
Inhaled in the embodiment of the present invention based on secondary nanosphere hierarchical Z nO nano materials and common ZnO UV, visible light
It is as shown in Figure 6 to receive spectrum；It can be seen from the figure that ZnO samples and there is larger area with the absorption spectrum of hierarchical Z nO nano materials
Not.Hierarchical Z nO nano materials based on secondary nanosphere absorb luminous intensity enhancing, and photoresponse scope also increases, Er Qieqi
Ultraviolet-ray visible absorbing sideband also there occurs blue shift, this mainly due to occurring in secondary nanoparticle caused by quantum size effect,
It is consistent with characterization result before.
Luminescence generated by light light based on secondary nanosphere hierarchical Z nO nano materials and common ZnO in the embodiment of the present invention 3
Spectrum is as shown in Figure 7；The fluorescence intensity of the hierarchical Z nO nano materials based on secondary nanosphere is substantially higher than common ZnO in figure
Some, illustrate under the irradiation of identical light, and the material of the hierarchical Z nO containing nanostructured is easier to be generated more
Carrier, photo-generated carrier is compound again to make its fluorescence intensity higher；In addition, compared with common ZnO fluorescent emissions peak position,
Also there is blue shift in fluorescence emission peak based on secondary nanosphere hierarchical Z nO nano materials, this absorption spectrum with them
It is almost consistent.
Embodiment 4：
A kind of preparation method based on secondary nanosphere hierarchical Z nO nano materials, comprises the following steps：
1) 0.65g zinc acetate dihydrate is weighed, being added to stirring in 200ml dimethylformamide, will to abundant dissolving
The mixed solution is labeled as solution A；
2) weigh 0.4g urea and measure 0.1ml oleic acid, both then are added into 30ml concentration respectively is
In the solution of 99.5wt% dimethylformamide, the solution is labeled as B solution；
3) first the beaker for filling solution A is placed in water-bath, under the conditions of 90 DEG C of keeping temperature, water-bath 5h；Afterwards, ice is used
The above-mentioned reaction system of water cooling, makes it cool down rapidly；
4) under rapid stirring (150 revs/min of rotating speed), the B solution in step 2) is added dropwise to
In the solution A { reaction system of step 3) } of cooling, the mixed solution is labeled as C solution；
5) beaker for filling C solution is again placed in water-bath, is warming up to 50 DEG C and keeps 1h；
6) C solution after water-bath is cooled down with frozen water, is placed in centrifuge tube centrifuges afterwards；
7) first washed 3 times with dimethylformamide, and take out the sediment after centrifugation, then by the sediment with anhydrous second
Alcohol fully washs final white product；
8) above-mentioned white product is dried, and produces the hierarchical Z nO nano materials based on secondary nanosphere.
Embodiment 5：
A kind of preparation method based on secondary nanosphere hierarchical Z nO nano materials, comprises the following steps：
1) 1.3g zinc acetate dihydrate is weighed, stirring in 200ml dimethylformamide is added to and is dissolved to abundant, by this
Mixed solution is labeled as solution A；
2) weigh 0.4g urea and measure 0.1ml oleic acid, both then are added into 30ml concentration respectively is
In the solution of 99.5wt% dimethylformamide, the solution is labeled as B solution；
3) first the beaker for filling solution A is placed in water-bath, under the conditions of 90 DEG C of keeping temperature, water-bath 5h；Afterwards, ice is used
The above-mentioned reaction system of water cooling, makes it cool down rapidly；
4) under rapid stirring (150 revs/min of rotating speed), the B solution in step 2) is added dropwise to
In the solution A { reaction system of step 3) } of cooling, the mixed solution is labeled as C solution；
5) beaker for filling C solution is again placed in water-bath, is warming up to 50 DEG C and keeps 1h；
6) C solution after water-bath is cooled down with frozen water, is placed in centrifuge tube centrifuges afterwards；
7) first washed 3 times with dimethylformamide, and take out the sediment after centrifugation, then by the sediment with anhydrous second
Alcohol fully washs final white product；
8) above-mentioned white product is drying to obtain the hierarchical Z nO nano materials based on secondary nanosphere.
Obtained by embodiment 5 is white powder based on secondary nanosphere hierarchical Z nO nano materials, wherein scheming
8 be the SEM figures of gained nano material in the embodiment of the present invention 5, and wherein primary structure zinc oxide sphere diameter is about 200-350nm,
Skewness, and the diameter of the individual particle of secondary structure nanosphere is about 15nm.And known by ultraviolet-visible absorption spectroscopy
The nano material absorbs luminous intensity enhancing, and photoresponse scope also increases, and also there occurs indigo plant for its ultraviolet-ray visible absorbing sideband
Move, this occurs caused by quantum size effect mainly due in secondary nanoparticle.
Embodiment 6：
A kind of preparation method based on secondary nanosphere hierarchical Z nO nano materials, comprises the following steps：
1) 1.3g zinc acetate dihydrate is weighed, stirring in 100ml dimethylformamide is added to and is dissolved to abundant, by this
Mixed solution is labeled as solution A；
2) weigh 0.4g urea and measure 0.1ml oleic acid, both then are added into 30ml concentration respectively is
In the solution of 99.5wt% dimethylformamide, the solution is labeled as B solution；
3) first the beaker for filling solution A is placed in water-bath, under the conditions of 90 DEG C of keeping temperature, water-bath 5h；Afterwards, ice is used
The above-mentioned reaction system of water cooling, makes it cool down rapidly；
4) under rapid stirring (150 revs/min of rotating speed), the B solution in step 2) is added dropwise to
In the solution A { reaction system of step 3) } of cooling, the mixed solution is labeled as C solution；
5) beaker for filling C solution is again placed in water-bath, is warming up to 50 DEG C and keeps 1h；
6) C solution after water-bath is cooled down with frozen water, is placed in centrifuge tube centrifuges afterwards；
7) first washed 3 times with dimethylformamide, and take out the sediment after centrifugation, then by the sediment with anhydrous second
Alcohol fully washs final white product；
8) above-mentioned white product is dried, and produces the hierarchical Z nO nano materials based on secondary nanosphere.
Embodiment 7：
A kind of preparation method based on secondary nanosphere hierarchical Z nO nano materials, comprises the following steps：
1) 0.65g zinc acetate dihydrate is weighed, being added to stirring in 100ml dimethylformamide, will to abundant dissolving
The mixed solution is labeled as solution A；
2) weigh 0.4g urea and measure 0.1ml oleic acid, both then are added into 30ml concentration respectively is
In the solution of 99.5wt% dimethylformamide, the solution is labeled as B solution；
3) first the beaker for filling solution A is placed in water-bath, under the conditions of 90 DEG C of keeping temperature, water-bath 3h；Afterwards, ice is used
The above-mentioned reaction system of water cooling, makes it cool down rapidly；
4) under rapid stirring (150 revs/min of rotating speed), the B solution in step 2) is added dropwise to
In the solution A { reaction system of step 3) } of cooling, the mixed solution is labeled as C solution；
5) beaker for filling C solution is again placed in water-bath, is warming up to 50 DEG C and keeps 1h；
6) C solution after water-bath is cooled down with frozen water, is placed in centrifuge tube centrifuges afterwards；
7) first washed 3 times with dimethylformamide, and take out the sediment after centrifugation, then by the sediment with anhydrous second
Alcohol fully washs final white product；
8) above-mentioned white product is dried, and produces the hierarchical Z nO nano materials based on secondary nanosphere.
Obtained by embodiment 7 based on secondary nanosphere hierarchical Z nO nano materials, institute in the embodiment of the present invention 7
The nanometer rods that nano material primary structure zinc oxide is secondary oxidative zinc nanoparticles composition are obtained, the length of wherein nanometer rods is about
100nm, diameter are about 20nm, and the diameter of secondary structure nanosphere is about 12nm.And know that this is received by ultraviolet-visible absorption spectroscopy
Rice material absorbs luminous intensity enhancing, and photoresponse scope also increases, and its ultraviolet-ray visible absorbing sideband is also there occurs blue shift, this
Occur mainly due in secondary nanoparticle caused by quantum size effect.
Embodiment 8：
A kind of preparation method based on secondary nanosphere hierarchical Z nO nano materials, comprises the following steps：
1) 0.65g zinc acetate dihydrate is weighed, being added to stirring in 100ml dimethylformamide, will to abundant dissolving
The mixed solution is labeled as solution A；
2) weigh 0.4g urea and measure 0.1ml oleic acid, both then are added into 30ml concentration respectively is
In the solution of 99.5wt% dimethylformamide, the solution is labeled as B solution；
3) first the beaker for filling solution A is placed in water-bath, under the conditions of 90 DEG C of keeping temperature, water-bath 7h；
4) after, above-mentioned reaction system is cooled down with frozen water, it is cooled down rapidly；
4) under rapid stirring (150 revs/min of rotating speed), the B solution in step 2) is added dropwise to
In the solution A { reaction system of step 3) } of cooling, the mixed solution is labeled as C solution；
5) beaker for filling C solution is again placed in water-bath, is warming up to 50 DEG C and keeps 1h；
6) C solution after water-bath is cooled down with frozen water, is placed in centrifuge tube centrifuges afterwards；
7) first washed 3 times with dimethylformamide, and take out the sediment after centrifugation, then by the sediment with anhydrous second
Alcohol fully washs final white product；
8) above-mentioned white product is dried, and produces the hierarchical Z nO nano materials based on secondary nanosphere.
Obtained by embodiment 8 based on secondary nanosphere hierarchical Z nO nano materials, institute in the embodiment of the present invention 8
Obtain the ellipsoid structure that nano material primary structure zinc oxide is secondary oxidative zinc nanoparticles composition, the wherein length of ellipsoid about
It is about 200nm for 300nm, diameter, the diameter of secondary structure nanosphere is about 15nm.
Claims (2)
1. a kind of preparation method of the hierarchical Z nO nano materials based on secondary nanosphere, it is characterised in that including following step
Suddenly：
1) 0.65-1.3g zinc acetate dihydrate is weighed, is added in 100-200ml dimethylformamide and stirs to fully molten
Solution, solution A is labeled as by the mixed solution；
2) weigh 0.4g urea and measure 0.1ml oleic acid, both are then added to 30ml dimethylformamide respectively
In solution, the solution is labeled as B solution；
3) first the beaker for filling solution A is placed in water-bath, under the conditions of 65-95 DEG C of keeping temperature, water-bath 3-7h；Afterwards, use
Frozen water cools down solution A, it is cooled down rapidly；
4) under conditions of stirring, the B solution in step 2) is added dropwise in the solution A cooled down, the mixing is molten
Liquid is labeled as C solution；
5) beaker for filling C solution is again placed in water-bath, is warming up to 50 DEG C and keeps 1h；
6) C solution after water-bath is cooled down with frozen water, is placed in centrifuge tube centrifuges afterwards；
7) first washed 3 times with dimethylformamide, and take out the sediment after centrifugation, then the sediment is filled with absolute ethyl alcohol
Divide washing final white product；
8) above-mentioned white product is dried, and produces the hierarchical Z nO nano materials based on secondary nanosphere.
2. a kind of preparation method of hierarchical Z nO nano materials based on secondary nanosphere according to claim 1, its
It is characterised by, the rotating speed of the stirring in step 4) is 150 revs/min.
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