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
- Publication number
- 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
- Authority
- CN
- China
- Prior art keywords
- zinc oxide
- preparation
- dimensional flower
- ultrapure water
- mixing solutions
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title abstract description 13
- 239000002086 nanomaterial Substances 0.000 title abstract 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 24
- 238000002360 preparation method Methods 0.000 claims abstract description 18
- 239000000463 material Substances 0.000 claims abstract description 14
- 229910021642 ultra pure water Inorganic materials 0.000 claims abstract description 11
- 239000012498 ultrapure water Substances 0.000 claims abstract description 11
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 239000004246 zinc acetate Substances 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims description 13
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 5
- 238000005119 centrifugation Methods 0.000 claims description 3
- -1 polytetrafluoroethylene Polymers 0.000 claims description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 2
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 5
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 3
- 231100000331 toxic Toxicity 0.000 abstract description 3
- 230000002588 toxic effect Effects 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 2
- 239000000243 solution Substances 0.000 abstract 2
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 239000011259 mixed solution Substances 0.000 abstract 1
- 230000001699 photocatalysis Effects 0.000 abstract 1
- 238000007146 photocatalysis Methods 0.000 abstract 1
- 239000004094 surface-active agent Substances 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000013543 active substance Substances 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000003643 water by type Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000004070 electrodeposition 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
- 239000012535 impurity Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000002207 thermal evaporation Methods 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
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 |
Applications Claiming Priority (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 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104118903A true CN104118903A (en) | 2014-10-29 |
Family
ID=51764576
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410372178.9A Pending CN104118903A (en) | 2014-07-31 | 2014-07-31 | Method for preparing three-dimensional flower-shaped zinc oxide nano material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104118903A (en) |
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 | Method for preparing three-dimensional zinc oxide nano self-assembly structure |
| CN110813272A (en) * | 2019-11-08 | 2020-02-21 | 昆明理工大学 | A kind of 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 | Method for preparing three-dimensional zinc oxide nano self-assembly structure |
| CN110813272A (en) * | 2019-11-08 | 2020-02-21 | 昆明理工大学 | A kind of 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 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104118903A (en) | Method for preparing three-dimensional flower-shaped zinc oxide nano material | |
| CN103990486B (en) | The preparation method of a kind of indium sulfide/carbonitride composite nano materials | |
| CN102773110B (en) | Preparation method of coin-shaped hollow structure SnS2/SnO2 composite photocatalyst material | |
| CN101920986B (en) | Preparation method of zinc oxide nanosphere | |
| CN109399584B (en) | A kind of hexagonal tubular carbon nitride and its preparation method and application | |
| CN106732668A (en) | A kind of hydrothermal preparing process of flower-shaped molybdenum bisuphide/cupric oxide composite nano materials | |
| CN106732589A (en) | A kind of preparation method of cupric oxide/cuprous oxide/graphene nanocomposite material | |
| CN102745752A (en) | Method of synthesizing mesoporous nickel cobalt oxide nanowire using hydrothermal method and application thereof | |
| CN107827145B (en) | A kind of nanometer zinc oxide material and preparation method thereof | |
| CN104030371B (en) | A method for synthesizing NiO microspheres with mesoporous sheet structure by soft template method | |
| CN105063740B (en) | A kind of truncated rectangular pyramids flake Bi2O3Nano crystal and preparation method thereof | |
| CN104291382A (en) | Preparation method of lanthanum ferrite porous micro-spheres | |
| CN105523578A (en) | Nanometer copper oxide with controllable morphology as well as preparation method and application of nanometer copper oxide | |
| CN106111161A (en) | A kind of ZnO/ZnS/CdS composite of porous nucleocapsid structure and preparation method thereof | |
| CN102285681A (en) | Low-temperature hydrothermal synthesis method of ZnO nano shuttle | |
| CN105712299B (en) | Water-insoluble metal hydroxide and preparation method thereof | |
| CN109174130B (en) | Two-dimensional surface SnS2-MoS2Method for preparing composite | |
| CN105084409B (en) | It is a kind of（200）Crystal face exposes the synthetic method of single dispersing CuO nanometer sheet | |
| CN105502480B (en) | Hydrangea-like strontium titanate nano powder preparation method | |
| CN101148266A (en) | Process for preparing In2O3 nano-wire | |
| CN108579773B (en) | A kind of perovskite-based composite nano materials and preparation method and purposes | |
| CN108033481B (en) | Preparation method of oriented porous copper sulfide nanomaterials | |
| CN102040246B (en) | Method for synthesizing manganous-manganic oxide nano material at room temperature by using mild path | |
| CN106517299B (en) | Flaky self-assembled basic copper carbonate flower ball and simple preparation method thereof | |
| CN108946773A (en) | A kind of carbonate form hydrotalcite-based compound raw powder's production technology |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20141029 |