CN106186045A - A kind of preparation method of flower shape zinc oxide nano-particle cluster - Google Patents
A kind of preparation method of flower shape zinc oxide nano-particle cluster Download PDFInfo
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- CN106186045A CN106186045A CN201610596102.3A CN201610596102A CN106186045A CN 106186045 A CN106186045 A CN 106186045A CN 201610596102 A CN201610596102 A CN 201610596102A CN 106186045 A CN106186045 A CN 106186045A
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- C01G9/02—Oxides; Hydroxides
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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- 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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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/50—Agglomerated particles
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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Abstract
A kind of method preparing flower shape zinc oxide nano-particle cluster, comprises the following steps: 1) precipitant is joined in zinc solution, stir 0.5 1h；Wherein, the molar concentration of zinc solution is 0.001 0.004mol/L, and precipitant is 1:10 with the mol ratio of zinc salt；2) by step 1) gained solution is heated to 90 100 DEG C, and it is down to room temperature after stirring 4 6h, washs, be dried, obtain flower shape zinc oxide nano-particle cluster.Present invention process flow process is simple, easy to operate, additive-free in course of reaction, template, it is ensured that product purity, and reaction temperature is low, and the response time is short, and cost and energy consumption are low, environmental friendliness, can be with large-scale industrial production.
Description
Technical field
The present invention relates to the preparation method of a kind of nano zine oxide, a kind of flower shape zinc oxide nano-particle cluster
Preparation method.
Background technology
Zinc oxide energy gap at room temperature is about 3.37eV, has good heat conduction, conduction, piezoelectricity, photoelectric characteristic,
And stable chemical nature, therefore at solaode, lithium ion battery, ultraviolet lasing device, gas sensor, Flied emission
It is used widely in multiple field such as device.Enrich additionally, zinc oxide has raw material resources, cheap, environmental protection etc.
Advantage, can carry out large-scale production.The performance of nano zinc oxide material depends on its pattern and size, therefore synthesizes not similar shape
The nano zinc oxide material of looks and size is studied its new performance and finds corresponding application to become new research side
To.Lot of documents reports the nano zine oxide preparing various different-shape by different methods, such as nano-particle, nanometer
Line, nanometer rods, nano belt, nanotube, nanometer sheet etc., conventional preparation method have hydro-thermal method, sol-gal process, microemulsion method and
The sedimentation method etc..
Document " preparation of Zhang Xianli .ZnO nano material and performance study [D]. Anhui: University of Anhui, 2009. " report
The preparation method of a kind of petal-shaped zinc oxide, i.e. using direct precipitation method is 1:2, temperature at zinc acetate and sodium hydroxide mol ratio
Be 80 DEG C to 100 DEG C, solvent be to react 24h under conditions of glycerol.The method response time is longer, and makes molten of glycerol
Agent, cost is high, has certain limitation in actual production.
Document " Xie Zhiqiang. the hydro-thermal method preparation of zinc oxide nano rod and the research [D] of photocatalysis performance thereof. Nanning: Guangxi
University, 2012. " use analytical pure zinc oxide as zinc source, sodium hydroxide is mineralizer, with the alkali of hydrochloric acid regulation and control reaction solution
Degree, with hydrothermal synthesis method at 60 DEG C, has prepared many nanoparticle aggregates flower-shaped oxygen together under the reaction condition of 18h
Change zinc.This hydrothermal synthesis method is high to equipment requirements, and danger coefficient is big, has certain operation easier.
Summary of the invention
It is an object of the invention to overcome above-mentioned the deficiencies in the prior art, it is provided that a kind of flower shape zinc oxide nano-particle cluster
Preparation method, technological process is simple, easy to operate, additive-free in course of reaction, template, it is ensured that product purity, and instead
Answering temperature low, the response time is short, and cost and energy consumption are low, can be with large-scale industrial production
In order to achieve the above object, the technical scheme that the present invention takes is:
A kind of method preparing flower shape zinc oxide nano-particle cluster, comprises the following steps:
1) precipitant is joined in zinc solution, stir 0.5-1h；Wherein, the molar concentration of zinc solution is 0.001-
0.004mol/L, precipitant is 1:10 with the mol ratio of zinc salt；
2) by step 1) stirring after solution be heated to 90-100 DEG C, stirring 4-6h after be down to room temperature, wash, be dried,
To flower shape zinc oxide nano-particle cluster.
The present invention is further improved by, and described zinc solution is by preparing soluble in water for zinc nitrate hexahydrate.
The present invention is further improved by, and described precipitant is sodium hydroxide.
The present invention is further improved by, described step 1) in stirring at room temperature carry out.
The present invention is further improved by, and cooling uses nature to be down to room temperature.
The present invention is further improved by, washing use distilled water clean to pH value be 7, then with washes of absolute alcohol 3
Secondary.
The present invention is further improved by, and being dried is to carry out in thermostatic drying chamber.
The present invention is further improved by, and the temperature being dried is 60-80 DEG C, and the time is 10-12h.
Compared with prior art, the invention have the benefit that the present invention, with zinc salt and precipitant as raw material, uses straight
Connect the sedimentation method at 90-100 DEG C, react 4-6h, synthesize the flower shape zinc oxide nano-particle cluster of morphology controllable.Zinc oxide nano
Rice grain is evenly distributed, a size of 20-40 nanometer, can be widely applied to catalysis, biological medicine, sensor, electromagnetic absorption, photic
The fields such as luminescence, air-sensitive and varistor.The present invention compared with prior art, has method easy, the advantage of low cost, only
Can be prepared by flower shape zinc oxide nano-particle cluster by the sedimentation method, technological process is simple, easy to operate, without adding in course of reaction
Adding agent, template, and ensure that product purity, and reaction temperature is low, the response time is short, and cost and energy consumption are low, and environmental friendliness can
With large-scale industrial production.
Further, precipitant is sodium hydroxide, is because sodium hydroxide and has stronger alkalescence, can be as alkali source.
Accompanying drawing explanation
Fig. 1 is the XRD figure of zinc oxide in the embodiment of the present invention 1；
Fig. 2 is the SEM figure of zinc oxide under different amplification in the embodiment of the present invention 1.Wherein, Fig. 2 (a) amplification is
30000, Fig. 2 (b) method multiple is 110000.
Detailed description of the invention
With embodiment, the present invention is described in further details below in conjunction with the accompanying drawings.
Embodiment 1
Weigh 0.1188g zinc nitrate hexahydrate to be dissolved in 400mL distilled water, add 0.1600g sodium hydroxide to above-mentioned
In zinc solution, mix and blend 0.5h under room temperature.Then heating said solution is to 95 DEG C, reacts 5h.Reaction end treats that nature drops
To room temperature, product distilled water clean to pH value be 7, then with washes of absolute alcohol 3 times, dry in the thermostatic drying chamber of 60 DEG C
10h, i.e. can get white zinc oxide powder body.
Seeing Fig. 1, the nano zine oxide prepared as can be seen from Figure 1 is wurtzite-type, and purity is high, free from admixture peak.
See Fig. 2, can be seen that from Fig. 2 (a) Zinc oxide nanoparticle prepared has been self-assembled into a kind of flower-shaped cluster,
Can be seen that Zinc oxide nanoparticle is evenly distributed from Fig. 2 (b), a size of 20-40 nanometer.
Embodiment 2
Weigh 0.2380g zinc nitrate hexahydrate to be dissolved in 400mL distilled water, add 0.3200g sodium hydroxide to above-mentioned
In zinc solution, mix and blend 0.8h under room temperature.Then heating said solution is to 95 DEG C, reacts 6h.Reaction end treats that nature drops
To room temperature, product distilled water clean to pH value be 7, then with washes of absolute alcohol 3 times, dry in the thermostatic drying chamber of 70 DEG C
11h, i.e. can get white zinc oxide powder body.
Embodiment 3
Weigh 0.2975g zinc nitrate hexahydrate to be dissolved in 400mL distilled water, add 0.3999g sodium hydroxide to above-mentioned
In zinc solution, mix and blend 1h under room temperature.Then heating said solution is to 90 DEG C, reacts 6h.Reaction end treats that nature is down to
Room temperature, product distilled water clean to pH value be 7, then with washes of absolute alcohol 3 times, dry 12h in the thermostatic drying chamber of 70 DEG C,
I.e. can get white zinc oxide powder body.
Embodiment 4
Weigh 0.3572g zinc nitrate hexahydrate to be dissolved in 400mL distilled water, add 0.4800g sodium hydroxide to above-mentioned
In zinc solution, mix and blend 0.8h under room temperature.Then heating said solution is to 100 DEG C, reacts 5h.Reaction end treats that nature drops
To room temperature, product distilled water clean to pH value be 7, then with washes of absolute alcohol 3 times, dry in the thermostatic drying chamber of 80 DEG C
10h, i.e. can get white zinc oxide powder body.
Embodiment 5
Weigh 0.4760g zinc nitrate hexahydrate to be dissolved in 400mL distilled water, add 0.6400g sodium hydroxide to above-mentioned
In zinc solution, mix and blend 1h under room temperature.Then heating said solution is to 100 DEG C, reacts 4h.Reaction end treats that nature is down to
Room temperature, product distilled water clean to pH value be 7, then with washes of absolute alcohol 3 times, dry 12h in the thermostatic drying chamber of 80 DEG C,
I.e. can get white zinc oxide powder body.
Embodiment 6
1) by prepared zinc solution soluble in water for zinc nitrate hexahydrate, sodium hydroxide is joined in zinc solution, room temperature
Lower stirring 0.5h, obtains water-soluble zinc salt solution；Wherein, the molar concentration of zinc solution is 0.001mol/L, sodium hydroxide with
The mol ratio of zinc nitrate hexahydrate is 1:10；
2) by step 1) gained solution is heated to 100 DEG C, after stirring 4h, is naturally cooling to room temperature, uses distilled water to clean
It is 7 to pH value, then with washes of absolute alcohol 3 times, in thermostatic drying chamber, at 60 DEG C of dry 12h, obtains flower shape zinc oxide nanometer
Particle clusters.
Embodiment 7
1) by prepared zinc solution soluble in water for zinc nitrate hexahydrate, sodium hydroxide is joined in zinc solution, room temperature
Lower stirring 1h, obtains water-soluble zinc salt solution；Wherein, the molar concentration of zinc solution is 0.004mol/L, sodium hydroxide and six
The mol ratio of nitric hydrate zinc is 1:10；
2) by step 1) gained solution is heated to 90 DEG C, after stirring 6h, is naturally cooling to room temperature, uses distilled water to clean extremely
PH value is 7, then with washes of absolute alcohol 3 times, in thermostatic drying chamber, at 80 DEG C of dry 10h, obtains flower shape zinc oxide nanometer
Grain cluster.
Claims (8)
1. the method preparing flower shape zinc oxide nano-particle cluster, it is characterised in that comprise the following steps:
1) precipitant is joined in zinc solution, stir 0.5-1h；Wherein, the molar concentration of zinc solution is 0.001-
0.004mol/L, precipitant is 1:10 with the mol ratio of zinc salt；
2) by step 1) stirring after solution be heated to 90-100 DEG C, stirring 4-6h after be down to room temperature, wash, be dried, spent
Shape Zinc oxide nanoparticle cluster.
A kind of method preparing flower shape zinc oxide nano-particle cluster the most according to claim 1, it is characterised in that described
Zinc solution is by preparing soluble in water for zinc nitrate hexahydrate.
A kind of method preparing flower shape zinc oxide nano-particle cluster the most according to claim 1, it is characterised in that described
Precipitant is sodium hydroxide.
A kind of method preparing flower shape zinc oxide nano-particle cluster the most according to claim 1, it is characterised in that described
Step 1) in stirring at room temperature carry out.
A kind of method preparing flower shape zinc oxide nano-particle cluster the most according to claim 1, it is characterised in that cooling
Nature is used to be down to room temperature.
A kind of method preparing flower shape zinc oxide nano-particle cluster the most according to claim 1, it is characterised in that washing
Use distilled water clean to pH value be 7, then with washes of absolute alcohol 3 times.
A kind of method preparing flower shape zinc oxide nano-particle cluster the most according to claim 1, it is characterised in that be dried
It is to carry out in thermostatic drying chamber.
A kind of method preparing flower shape zinc oxide nano-particle cluster the most according to claim 1, it is characterised in that be dried
Temperature be 60-80 DEG C, the time is 10-12h.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107089677A (en) * | 2017-06-07 | 2017-08-25 | 首都医科大学宣武医院 | Preparation method of zinc oxide nanoparticles based on silk fibroin biological template regulation |
| CN109928421A (en) * | 2019-02-28 | 2019-06-25 | 江苏赛清科技有限公司 | With flower-like micro/nano structure Zinc oxide powder and its preparation method and application |
| CN111170356A (en) * | 2020-02-11 | 2020-05-19 | 江南大学 | Preparation method of shape-controllable nano zinc oxide |
| US20220113270A1 (en) * | 2020-10-08 | 2022-04-14 | City University Of Hong Kong | Method for fabricating zinc oxide nanostructures and gas sensors |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101613121A (en) * | 2009-07-16 | 2009-12-30 | 聊城大学 | A kind of preparation method of ellipsoid-shaped zinc oxide |
| CN102101693A (en) * | 2010-12-29 | 2011-06-22 | 安徽理工大学 | Preparation method and application of double-function micro-nano hierarchical structural zinc oxide power |
-
2016
- 2016-07-26 CN CN201610596102.3A patent/CN106186045A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101613121A (en) * | 2009-07-16 | 2009-12-30 | 聊城大学 | A kind of preparation method of ellipsoid-shaped zinc oxide |
| CN102101693A (en) * | 2010-12-29 | 2011-06-22 | 安徽理工大学 | Preparation method and application of double-function micro-nano hierarchical structural zinc oxide power |
Non-Patent Citations (2)
| Title |
|---|
| YONGJIANG SUN ET AL.: "Facile synthesis of flower-like 3D ZnO superstructures via solution route", 《CRYSTENGCOMM》 * |
| 汪苇等: "片状纳米氧化锌的合成和形貌控制", 《大连工业大学学报》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107089677A (en) * | 2017-06-07 | 2017-08-25 | 首都医科大学宣武医院 | Preparation method of zinc oxide nanoparticles based on silk fibroin biological template regulation |
| CN107089677B (en) * | 2017-06-07 | 2018-07-10 | 首都医科大学宣武医院 | Preparation method of zinc oxide nanoparticles based on silk fibroin biological template regulation |
| CN109928421A (en) * | 2019-02-28 | 2019-06-25 | 江苏赛清科技有限公司 | With flower-like micro/nano structure Zinc oxide powder and its preparation method and application |
| CN111170356A (en) * | 2020-02-11 | 2020-05-19 | 江南大学 | Preparation method of shape-controllable nano zinc oxide |
| CN111170356B (en) * | 2020-02-11 | 2021-04-20 | 江南大学 | Preparation method of shape-controllable nano zinc oxide |
| US20220113270A1 (en) * | 2020-10-08 | 2022-04-14 | City University Of Hong Kong | Method for fabricating zinc oxide nanostructures and gas sensors |
| US11639910B2 (en) * | 2020-10-08 | 2023-05-02 | City University Of Hong Kong | Method for fabricating zinc oxide nanostructures and gas sensors |
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