CN109502629A - Zinc oxide nano-sheet/nano particle preparation method - Google Patents
Zinc oxide nano-sheet/nano particle preparation method Download PDFInfo
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- CN109502629A CN109502629A CN201811472821.XA CN201811472821A CN109502629A CN 109502629 A CN109502629 A CN 109502629A CN 201811472821 A CN201811472821 A CN 201811472821A CN 109502629 A CN109502629 A CN 109502629A
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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
- C01G9/03—Processes of production using dry methods, e.g. vapour phase processes
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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
- C01P2002/70—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
- 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
Abstract
The invention belongs to technical field of nano material, more particularly to a kind of preparation method of zinc oxide nano-sheet/nano particle, it the described method comprises the following steps: (1) uniformly mixing divalent zinc ion salt, NaCl, KCl by the ratio between the amount of substance 1:100x:10x, wherein 0.2 < x < 0.6 or 0.6 < x < 1.5；(2) obtained mixture is collected in crucible and is put into Muffle furnace, be warming up to 760-880 DEG C of baking mixes 4h, then cool down；(3) reaction product is impregnated into desalination, filters, obtains white solid；(4) white solid is taken out into centrifuge washing, then dried, obtain product zinc oxide nano-sheet or Zinc oxide nanoparticle.The nano material dimensional controllability of preparation is good, and pattern is uniform, good dispersion, is conducive to the photoelectric properties for improving ZnO nano material, explores its application in energy and environment.
Description
Technical field
The invention belongs to technical field of nano material, and in particular to a kind of preparation of zinc oxide nano-sheet/nano particle
Method.
Background technique
ZnO is a kind of with important direct band gap semiconductor material with wide forbidden band, and forbidden bandwidth at room temperature is
3.37eV is had a wide range of applications due to its superior photoelectric properties in many fields.With the microminiaturization and nanometer material of device
Material has the reasons such as biggish specific surface area, and the research of nano-ZnO becomes especially popular.
There are many kinds of the methods for preparing zinc oxide and doped zinc oxide material, is divided into chemical method and physics by reaction type
Method.Currently used mainly chemical method, main method has following several: sol-gal process, the precipitation method, hydro-thermal method, solid phase are anti-
Ying Fa, sputter coating method etc..In these methods, hydro-thermal method manufacturing cycle is longer, solid reaction process it is higher to temperature requirement and
And it needs to carry out continuous grinding operation；Sputter coating method the high requirements on the equipment, yield is also general, is not suitable for industrialized production；
The precipitation method and the sample of sol-gal process preparation are easy to appear reunion, and the particle diameter distribution of ZnO particle is wide, bad dispersibility.It is existing
Synthetic method is unfavorable for industrialized production, constrains performance study and the application of zinc oxide material.
Summary of the invention
Invention broadly provides a kind of preparation method of zinc oxide nano-sheet/nano particle, the nano materials of preparation
Dimensional controllability is good, and pattern is uniform, good dispersion, be conducive to improve ZnO nano material photoelectric properties, explore its energy with
Application in environment.Its technical solution is as follows:
A kind of preparation method of zinc oxide nano-sheet/nano particle, comprising the following steps:
(1) divalent zinc ion salt, NaCl, KCl are uniformly mixed by the ratio between the amount of substance 1:100x:10x, wherein 0.2 < x
< 0.6 or 0.6 < x < 1.5；
(2) obtained mixture is collected in crucible and is put into Muffle furnace, be warming up to 760-880 DEG C of baking mixes
Then 4h is cooled down；
(3) reaction product is impregnated into desalination, filters, obtains white solid；
(4) white solid is taken out into centrifuge washing, then dried, obtain product zinc oxide nano-sheet or zinc-oxide nano
Grain.
Preferably, the divalent zinc ion salt is zinc nitrate, zinc acetate, zinc oxalate or zinc carbonate.
Preferably, as 0.2 < x < 0.6, product is Zinc oxide nanoparticle, and the diameter of nano particle is 300-
900nm；As 0.6 < x < 1.5, product is zinc oxide nano-sheet, and a length of 2-5 μm of nano flake, width is 1-4 μm, thickness
For 100-500nm.
Preferably, uniform to mixture ground and mixed using agate mortar in step (1).
Preferably, mixture heating rate is 5 DEG C/min in step (2).
Preferably, the white solid in step (4) after washing is dried in vacuo between 40-80 DEG C.
Using the above scheme, the invention has the following advantages that
Using divalent zinc ion salt, NaCl, KCl, by the ratio between amount of certain substance, uniformly mixing is roasted through high temperature the present invention again
It burns, distills water retting desalination, filter, washing is dried to obtain product zinc oxide nano-sheet or nano particle.The method of the present invention ring
Border is friendly, and the reaction time is short, and low energy consumption, and reaction step is few, and simple process, equipment is simple, and raw material is cheap and easy to get, and properties of product are excellent
Different, controllability is strong, will light, electricity, in terms of possess vast market prospect.
Detailed description of the invention
Fig. 1 is the x-ray diffraction pattern of the nano zinc oxide material of the method for the present invention preparation；
Fig. 2 is the scanning electron microscope (SEM) photograph of zinc oxide nano-sheet prepared by the embodiment of the present invention 1；
Fig. 3 is the scanning electron microscope (SEM) photograph of zinc oxide nano-sheet prepared by the embodiment of the present invention 2；
Fig. 4 is the scanning electron microscope (SEM) photograph of Zinc oxide nanoparticle prepared by the embodiment of the present invention 3.
Specific embodiment
Experimental method in following embodiment is conventional method unless otherwise required, related experiment reagent and material
Material is conventional biochemical reagent and material unless otherwise required.
The method of crystal growth from flux zinc oxide nano-sheet/nano particle of the present invention, using divalent zinc ion salt, NaCl, KCl
The ratio between amount by certain substance uniformly distill water retting desalination again through high-temperature roasting, filter by mixing, and washing is dried to obtain product
Zinc oxide nano-sheet or nano particle, are specifically implemented according to the following steps:
Step 1: in this example, by divalent zinc ion salt, NaCl, KCl, by the ratio between amount of substance 1: 100x: 10x, 0.2
< x < 0.6 or 0.6 < x < 1.5, are ground using agate mortar, are uniformly mixed, are obtained solid mixture；
Step 2: the mixture obtained in step 1 being collected in alumina crucible and is placed into Muffle furnace, by 5 DEG C/min
Rate be warming up to 760-880 DEG C, roast 4 hours, natural cooling；
Step 3: by the product ion water retting desalination after step 2 reaction, filtering, obtain white solid；
Step 4: white solid will be obtained in step 3 to be taken out to centrifuge tube, for several times with deionized water centrifuge washing, 40 DEG C-
It is dried in vacuo between 80 DEG C, is made a length of 2-5 μm of zinc oxide nano-sheet of the present invention, width is 1-4 μm, with a thickness of 100-500nm
Hexagon sheet or diameter 300~900nm or so nano particle regular shape.
If the ratio between amount of reactant species 1: 100x: 10x in step 1,0.2 < x < 0.6, then solid mixture can be converted
For Zinc oxide nanoparticle；If the ratio between amount of reactant species 1: 100x: 10x in step 1,0.6 < x < 1.5, then solid is mixed
Object can be converted into zinc oxide nano-sheet；If the reaction temperature in step 2 is lower than 760 DEG C or the reaction time is lower than 4h,
Solid mixture cannot be fully converted to zinc oxide nano-sheet；Solid is mixed if the reaction temperature in step 2 is higher than 880 DEG C
Closing object can be converted to that micron particles are larger and non-uniform Zinc oxide particles.
Specific embodiment
Embodiment 1
By Zn (CH3COO)2, NaCl, KCl, ground by the ratio between amount of substance 1: 100: 10 using agate mortar, it is uniformly mixed
It closes, obtains solid mixture, obtained mixture is collected in alumina crucible and is placed into Muffle furnace, by 5 DEG C/min's
Rate is warming up to 820 DEG C, roasts 4 hours, natural cooling, by the ion water retting desalination of the product after reaction, filters, obtains white
Color solid will obtain white solid and take out to centrifuge tube, and for several times with deionized water centrifuge washing, 60 DEG C of vacuum drying obtain this hair
Bright zinc oxide nano-sheet material.
X-ray diffraction test shows that product is pure zinc oxide, and electron scanning electromicroscopic photograph shows (Fig. 2), the oxidation of acquisition
Zinc nano flake regular shape, length are 3-4 μm, and width is 2-3 μm, with a thickness of 200-300nm.With other preparation method phases
Than the present invention is environmental-friendly, and the time is short, and low energy consumption, and reaction step is few, and simple process, equipment is simple, and raw material is cheap and easy to get, produces
Product are had excellent performance, and controllability is strong.
Embodiment 2
By Zn (CH3COO)2, NaCl, KCl, ground by the ratio between amount of substance 1: 120: 12 using agate mortar, it is uniformly mixed
It closes, obtains solid mixture, obtained mixture is collected in alumina crucible and is placed into Muffle furnace, by 5 DEG C/min's
Rate is warming up to 780 DEG C, roasts 4 hours, natural cooling, by the ion water retting desalination of the product after reaction, filters, obtains white
Color solid will obtain white solid and take out to centrifuge tube, and for several times with deionized water centrifuge washing, 60 DEG C of vacuum drying obtain this hair
Bright zinc oxide nano-sheet material.Electron scanning Electronic Speculum detection photo (Fig. 3) shows to obtain the zinc-oxide nano nanometer that product is
Thin slice.
Embodiment 3
By Zn (NO3)2, NaCl, KCl, ground by the ratio between amount of substance 1: 40: 4 using agate mortar, uniformly mix, obtain
Obtained mixture is collected in alumina crucible and places into Muffle furnace by solid mixture, heats up by the rate of 5 DEG C/min
It to 800 DEG C, roasts 4 hours, natural cooling, by the ion water retting desalination of the product after reaction, filters, obtain white solid,
It will obtain white solid to take out to centrifuge tube, for several times with deionized water centrifuge washing, sky is dried to obtain oxygen of the present invention between 60 DEG C
Change zinc nanoparticles.
Electron scanning Electronic Speculum detection photo (Fig. 4) shows the Zinc oxide nanoparticle that acquisition product is, diameter is in 500-
800nm or so.
Embodiment 4
By ZnCO3, NaCl, KCl, ground by the ratio between amount of substance 1: 80: 8 using agate mortar, uniformly mix, consolidate
Obtained mixture is collected in alumina crucible and places into Muffle furnace by body mixture, is warming up to by the rate of 5 DEG C/min
It 800 DEG C, roasts 4 hours, natural cooling, by the ion water retting desalination of the product after reaction, filters, obtain white solid, it will
It obtains white solid to take out to centrifuge tube, for several times with deionized water centrifuge washing, sky is dried to obtain oxidation of the present invention between 60 DEG C
Zinc nano-flake material.
Embodiment 5
It by zinc oxalate, NaCl, KCl, is ground by the ratio between amount of substance 1: 150: 15 using agate mortar, uniformly mixes, obtain
To solid mixture, obtained mixture is collected in alumina crucible and is placed into Muffle furnace, by the rate liter of 5 DEG C/min
Temperature roasts 4 hours, natural cooling to 880 DEG C, and the ion water retting desalination of the product after reaction filters, it is solid to obtain white
Body will obtain white solid and take out to centrifuge tube, and for several times with deionized water centrifuge washing, sky is dried to obtain the present invention between 80 DEG C
Zinc oxide nano-sheet material.
It will be apparent to those skilled in the art that can make various other according to the above description of the technical scheme and ideas
Corresponding change and deformation, and all these changes and deformation all should belong to the protection scope of the claims in the present invention
Within.
Claims (6)
1. a kind of preparation method of zinc oxide nano-sheet/nano particle, it is characterised in that: the following steps are included:
(1) divalent zinc ion salt, NaCl, KCl are uniformly mixed by the ratio between the amount of substance 1:100x:10x, wherein 0.2 < x <
0.6 or 0.6 < x < 1.5；
(2) obtained mixture is collected in crucible and is put into Muffle furnace, be warming up to 760-880 DEG C of baking mixes, so
After cool down；
(3) reaction product is impregnated into desalination, filters, obtains white solid；
(4) white solid is taken out into centrifuge washing, then dried, obtain product zinc oxide nano-sheet or Zinc oxide nanoparticle.
2. the preparation method of zinc oxide nano-sheet/nano particle according to claim 1, it is characterised in that: described two
Valence zinc ion salt is zinc nitrate, zinc acetate, zinc oxalate or zinc carbonate.
3. the preparation method of zinc oxide nano-sheet/nano particle according to claim 1, it is characterised in that: as 0.2 <
When x < 0.6, product is Zinc oxide nanoparticle, and the diameter of nano particle is 300-900nm；As 0.6 < x < 1.5, product
For zinc oxide nano-sheet, a length of 2-5 μm of nano flake, width is 1-4 μm, with a thickness of 100-500nm.
4. the preparation method of zinc oxide nano-sheet/nano particle according to claim 1, it is characterised in that: step (1)
It is middle uniform to mixture ground and mixed using agate mortar.
5. the preparation method of zinc oxide nano-sheet/nano particle according to claim 1, it is characterised in that: step (2)
Middle mixture heating rate is 5 DEG C/min.
6. the preparation method of zinc oxide nano-sheet/nano particle according to claim 1, it is characterised in that: step (4)
White solid after middle washing is dried in vacuo between 40-80 DEG C.
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| CN201811472821.XA CN109502629A (en) | 2018-12-04 | 2018-12-04 | Zinc oxide nano-sheet/nano particle preparation method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111233025A (en) * | 2020-01-21 | 2020-06-05 | 江苏理工学院 | Zinc oxide doped nano-sheet and molten salt method preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108793231A (en) * | 2018-08-13 | 2018-11-13 | 江苏理工学院 | The method that molten-salt growth method synthesizes fusiform germanic acid zinc nanoparticles |
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2018
- 2018-12-04 CN CN201811472821.XA patent/CN109502629A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108793231A (en) * | 2018-08-13 | 2018-11-13 | 江苏理工学院 | The method that molten-salt growth method synthesizes fusiform germanic acid zinc nanoparticles |
Non-Patent Citations (2)
| Title |
|---|
| 王文宝等: ""NaCl熔盐法制备ZnO 片状纳米晶及其光学性能研究"", 《化工新型材料》 * |
| 苏海林等: ""熔盐法生长 ZnO 单晶颗粒的微结构与形貌研究"", 《合肥工业大学学报(自然科学版)》 * |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111233025A (en) * | 2020-01-21 | 2020-06-05 | 江苏理工学院 | Zinc oxide doped nano-sheet and molten salt method preparation method thereof |
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