CN104118903A - Method for preparing three-dimensional flower-shaped zinc oxide nano material - Google Patents
Method for preparing three-dimensional flower-shaped zinc oxide nano material Download PDFInfo
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- CN104118903A CN104118903A CN201410372178.9A CN201410372178A CN104118903A CN 104118903 A CN104118903 A CN 104118903A CN 201410372178 A CN201410372178 A CN 201410372178A CN 104118903 A CN104118903 A CN 104118903A
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Abstract
The invention relates to a method for preparing a three-dimensional flower-shaped zinc oxide nano material by using a hydrothermal method and belongs to the technical field of inorganic chemical and material synthesis. The method comprises the following steps: firstly, dissolving zinc acetate in ultra-pure water, sufficiently stirring the obtained mixed solution, adding 8.0molL<-1> sodium hydroxide solution into the solution, and heating in a high-pressure kettle to grow flower-shaped zinc oxide. The three-dimensional flower-shaped zinc oxide prepared by using the method is uniform in size, and the structure is composed of nano needles which are assembled together. The method has the advantages that the operation is simple, the cost is low, and the preparation process does not use toxic reagent or surfactant, thus being friendly to the environment. The prepared zinc oxide has a large surface area and a wide application prospect in the fields such as photocatalysis and sensors.
Description
Technical field
The present invention relates to a kind of preparation method of three-dimensional flower-shaped nano zinc oxide material.
Background technology
Zinc oxide is a kind of novel II-VI family semiconductor material, its energy gap is 3.37 eV, there is very large exciton bind energy (60 meV), there is high electroconductibility, good uv absorption property and strong chemical stability simultaneously, be widely used in air-sensitive, photoelectricity, solar cell, sensor field.In the past decades, about the synthetic report of zinc oxide, have a lot, comprise aluminum oxide masterplate method, thermal evaporation, hydrothermal method, electrochemical deposition method etc., successfully prepared the zinc oxide of different structure and pattern.Wherein hydrothermal method has simple to operately, and cost is low, and the advantage such as the zinc oxide size pattern controllability of preparation is good, is to prepare the method that zinc oxide is conventional.
The performance of zinc oxide and its pattern, size, degree of crystallinity are closely related, in the zinc oxide of different-shape, three-dimensional flower-shaped structure has large surface-area, and electric transmission is easy, show excellent optics, electricity and catalysis characteristics, caused everybody increasing concern and research.In flower shape zinc oxide preparation process, conventionally need to add tensio-active agent and masterplate agent, be unfavorable for the cleaning of product, improved preparation cost, sometimes also can use toxic reagent, cause environmental pollution, cannot realize the object of using nontoxic reagent to prepare zinc oxide.The invention provides a kind of method of preparing three-dimensional flower-shaped nano zinc oxide material, in preparation process, use nontoxic reagent, and do not need to add tensio-active agent and masterplate agent, and can the three-dimensional flower-shaped nano zinc oxide material of preparation simple, cheap, environmental protection, be suitable for batch production.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of three-dimensional flower-shaped nano zinc oxide material.
The present invention realizes by following experimental program:
A method of preparing three-dimensional flower-shaped nano zinc oxide material, is characterized in that the method comprises the following steps:
A. zinc acetate is dissolved in ultrapure water and obtains mixing solutions, the mixing solutions obtaining at room temperature stirs 20 min;
B. 0.6 mL aqueous sodium hydroxide solution joined in the mixing solutions of step a gained and stir 10 min;
C. the mixing solutions of step b gained is joined in the autoclave of inner liner polytetrafluoroethylene, reactor, isothermal reaction 1 h in 120 ° of C baking ovens of preheating are tightened in sealing;
D. after completion of the reaction, autoclave is naturally cooled to room temperature, in the still that obtains, product, through centrifugation, and with ultrapure water washing, is then put into vacuum drying oven and is obtained three-dimensional flower-shaped zinc oxide at dry 15 h of 60 ° of C.
Preferably, the quality of the zinc acetate in step a is 0.0658 g, is dissolved in 20 mL ultrapure waters and obtains mixing solutions.
Preferably, in step b, the concentration of aqueous sodium hydroxide solution is 8.0 mol L
-1.
Preferably, the product obtaining in steps d is 5 with the number of times of ultrapure water washing.
The present invention is simple to operate, and cost is low, does not use toxic reagent and tensio-active agent in preparation process, environmentally friendly.The three-dimensional flower-shaped nano zinc oxide material of preparation has large surface-area, in photochemical catalysis, solar cell, sensor field, is with a wide range of applications.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope diagram (SEM) of the three-dimensional flower-shaped nano zinc oxide material of the present invention.
Fig. 2 is the X-ray diffractogram (XRD) of the three-dimensional flower-shaped nano zinc oxide material of the present invention.
Embodiment
In order to further illustrate the method for the three-dimensional flower-shaped nano zinc oxide material of preparation, the present embodiment is implemented according to technical solution of the present invention, provide concrete embodiment: take 0.0658 g zinc acetate, be dissolved in 20 mL ultrapure waters, the mixing solutions obtaining at room temperature stirs 20 min; Take 0.32 g sodium hydroxide, be dissolved in 1 mL ultrapure water, obtaining concentration is 8.0 mol L
-1aqueous sodium hydroxide solution, get the aqueous sodium hydroxide solution that 0.6 mL makes and join in appeal zinc acetate mixing solutions and at room temperature stir 10 min; Mixing solutions after appeal is stirred joins in the autoclave of inner liner polytetrafluoroethylene, and reactor is tightened in sealing, autoclave is put into baking oven, isothermal reaction 1 h under 120 ° of C; After reaction finishes, take out autoclave, naturally cool to room temperature, in the still obtaining, product, through centrifugation, with after ultrapure water washing 5 times, is put into loft drier at dry 12 h of 60 ° of C.
Prepared sample is carried out to SEM and XRD analysis, and result is referring to accompanying drawing.
Sem analysis: with the pattern of QUANTA FEG 250 thermal field emission scan electron microscope observation zinc oxide.As can be seen from Figure 1 the three-dimensional flower-shaped zinc oxide of preparation is comprised of nanoneedle, and the length of nanoneedle is 500 nm.
XRD analysis: XRD analysis advances on diffractometer and carries out at D8, is used Cu K
adiffraction.From the X diffracting spectrum of Fig. 2, can know, the XRD figure spectrum of product is consistent with zinc oxide standard diagram, and does not have other impurity peaks to occur, proves the nano zinc oxide material of successfully having prepared pure phase by the method.
Claims (4)
1. a preparation method for three-dimensional flower-shaped nano zinc oxide material, is characterized in that this preparation method comprises the following steps:
A. zinc acetate is dissolved in ultrapure water and obtains mixing solutions, the mixing solutions obtaining at room temperature stirs 20 min;
B. 0.6 mL aqueous sodium hydroxide solution joined in the mixing solutions of step a gained and stir 10 min;
C. the mixing solutions of step b gained is joined in the autoclave of inner liner polytetrafluoroethylene, reactor, isothermal reaction 1 h in 120 ° of C baking ovens of preheating are tightened in sealing;
D. after completion of the reaction, autoclave is naturally cooled to room temperature, in the still that obtains, product, through centrifugation, and with ultrapure water washing, is then put into vacuum drying oven and is obtained three-dimensional flower-shaped zinc oxide at dry 15 h of 60 ° of C.
2. preparation method according to claim 1, is characterized in that in step a, the blending ratio of zinc acetate and ultrapure water is: 0.0658 g is joined in the ultrapure water of 20 mL.
3. preparation method according to claim 1, the concentration that it is characterized in that aqueous sodium hydroxide solution in step b is 8.0 mol L
-1.
4. preparation method according to claim 1, is characterized in that the product obtaining in steps d is 5 with the number of times of ultrapure water washing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410372178.9A CN104118903A (en) | 2014-07-31 | 2014-07-31 | Method for preparing three-dimensional flower-shaped zinc oxide nano material |
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| CN201410372178.9A CN104118903A (en) | 2014-07-31 | 2014-07-31 | Method for preparing three-dimensional flower-shaped zinc oxide nano material |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104445367A (en) * | 2014-11-13 | 2015-03-25 | 华侨大学 | Preparation method of nanoflower-shaped zinc oxide |
| CN105215347A (en) * | 2015-09-07 | 2016-01-06 | 济南大学 | A kind of zinc oxide and gold nano grain composite and preparation method thereof |
| CN105540640A (en) * | 2016-01-26 | 2016-05-04 | 东北林业大学 | Preparation method of flower-shaped nanometer zinc oxide |
| CN108249474A (en) * | 2018-03-13 | 2018-07-06 | 江苏巨珩新材料科技有限公司 | A kind of method for preparing three-dimensional zinc oxide nanoassemble structure |
| CN110813272A (en) * | 2019-11-08 | 2020-02-21 | 昆明理工大学 | Preparation method of flower-shaped nano ZnO catalyst |
| CN112915991A (en) * | 2021-01-19 | 2021-06-08 | 西南交通大学 | Preparation method of lamellar aggregated flower-shaped zinc oxide photocatalyst |
| CN113351216A (en) * | 2021-06-03 | 2021-09-07 | 厦门理工学院 | Low-dimensional self-assembled flower-shaped Cu2Preparation method and application of O-ZnO catalyst |
-
2014
- 2014-07-31 CN CN201410372178.9A patent/CN104118903A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| HUI ZHANG ET AL.: "Synthesis of flower-like ZnO nanostructures by an organic-free hydrothermal process", 《NANOTECHNOLOGY》 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104445367A (en) * | 2014-11-13 | 2015-03-25 | 华侨大学 | Preparation method of nanoflower-shaped zinc oxide |
| CN105215347A (en) * | 2015-09-07 | 2016-01-06 | 济南大学 | A kind of zinc oxide and gold nano grain composite and preparation method thereof |
| CN105215347B (en) * | 2015-09-07 | 2017-03-29 | 济南大学 | A kind of Zinc Oxide and gold nano grain composite and preparation method thereof |
| CN105540640A (en) * | 2016-01-26 | 2016-05-04 | 东北林业大学 | Preparation method of flower-shaped nanometer zinc oxide |
| CN105540640B (en) * | 2016-01-26 | 2017-04-26 | 东北林业大学 | Preparation method of flower-shaped nanometer zinc oxide |
| CN108249474A (en) * | 2018-03-13 | 2018-07-06 | 江苏巨珩新材料科技有限公司 | A kind of method for preparing three-dimensional zinc oxide nanoassemble structure |
| CN110813272A (en) * | 2019-11-08 | 2020-02-21 | 昆明理工大学 | Preparation method of flower-shaped nano ZnO catalyst |
| CN112915991A (en) * | 2021-01-19 | 2021-06-08 | 西南交通大学 | Preparation method of lamellar aggregated flower-shaped zinc oxide photocatalyst |
| CN113351216A (en) * | 2021-06-03 | 2021-09-07 | 厦门理工学院 | Low-dimensional self-assembled flower-shaped Cu2Preparation method and application of O-ZnO catalyst |
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Application publication date: 20141029 |