CN102180513A - Method for preparing hexagonal pyramid-like zinc oxide by low temperature combustion synthesis method - Google Patents
Method for preparing hexagonal pyramid-like zinc oxide by low temperature combustion synthesis method Download PDFInfo
- Publication number
- CN102180513A CN102180513A CN 201110145483 CN201110145483A CN102180513A CN 102180513 A CN102180513 A CN 102180513A CN 201110145483 CN201110145483 CN 201110145483 CN 201110145483 A CN201110145483 A CN 201110145483A CN 102180513 A CN102180513 A CN 102180513A
- Authority
- CN
- China
- Prior art keywords
- zinc oxide
- zinc
- nitrate
- ammonium acetate
- powder
- 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.)
- Granted
Links
Images
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention relates to a method for preparing hexagonal pyramid-like zinc oxide by a low temperature combustion synthesis method and belongs to the field of synthesis of new materials. The method comprises the following steps: on the basis of low temperature combustion synthesis, taking zinc nitrate as a zinc source, and adding ammonium acetate and ammonium nitrate as ancillary reactive materials; mixing the zinc nitrate, the ammonium acetate and the ammonium nitrate according to the mol ratio (1:3 to 7:0.1-1.5); adding deionized water to be grinded into a colloidal substance; the mol ratio between the added deionized water and the ammonium acetate is 1:1; ultrasonically dispersing the colloidal substance for 5 minutes with an ultrasonic processor with power of 150 W and frequency of 20 kHz, and then putting the colloidal substance into a muffle furnace for combustion synthesis at the temperature of 550-650 DEG C; and grinding and annealing the obtained powder for 3 hours at the temperature of 400-700 DEG C, namely, obtaining the hexagonal pyramid-like zinc oxide. The method can achieve the purpose of controllably preparing the hexagonal pyramid-like zinc oxide, is simple, convenient and rapid in process and less in energy consumption and is suitable for large-scale industrial production, and the obtained zinc oxide powder is widely used for various fields such as microelectronic devices, solar batteries, optical devices, etc.
Description
Technical field
The present invention relates to a kind of low-temperature burning synthesis preparation method of hecaprismo structure zinc oxide, belong to the synthetic field of novel material.
Background technology
Zinc oxide is a kind of important semiconductor material with wide forbidden band, the room temperature Time Bandwidth can reach 3.37eV, very big exciton bind energy (60mev) is arranged, have excellent in chemical character, thermostability, good performances such as luminous and opto-electronic conversion, make it potential widely application be arranged in various fields, luminescent material, photoelectric conversion material, coating and daily-use chemical industry material be can be used for, honourable electrode, transformer and multiple Optical devices also can be used for making.Zinc oxide with specific dimensions, pattern, dimension and monodispersity can be realized the further assembling of material, constructing function structural system because of its particular performances.Although oneself obtains significant progress the preparation of zinc oxide material, the regulation and control of its size and pattern are also in the primary stage.Realizing the controlled preparation of zinc oxide structure, not only can provide the ideal object for the physical problem that we further investigate in Jie's sight, quantum, the polarization system, also is basis and essential condition that the Zinc oxide-base device moves towards practicability.Synthetic existing a lot of reports of relevant zinc oxide material, comprise methods such as the synthetic and template of physical sputtering sedimentation, chemical Vapor deposition process, electrochemical synthesis method, thermal evaporation, laser method, microemulsion method, solvent thermal is synthetic, synthesized the Zinc oxide powder of variform.By contrast, it is quick, easy, with low cost that low-temperature combustion synthesis has, and can overcome other processing condition harshnesses, yield poorly, be not easy to shortcomings such as industrialization, but this method often forms agglomeration traits easily, be difficult to the powder of preparation good dispersity, thereby be necessary further improvement.
Summary of the invention
For overcoming the deficiencies in the prior art, the present invention adds the reaction auxiliary material and takes corresponding preparation method for the zinc source with the zinc nitrate when low-temperature burning is synthetic, realization is to the pattern regulation and control of target product, solve the easy agglomeration traits of powder, make it to become a kind of hecaprismo structure zinc oxide of favorable dispersity.
Zinc source during A. described low-temperature burning is a zinc nitrate, and the reaction auxiliary material of adding is ammonium acetate and ammonium nitrate; Be that mix 1:3 ~ 7:0.1 ~ 1.5 in molar ratio;
B. described preparation method operates according to the following steps:
(1) is that mix 1:3 ~ 7:0.1 ~ 1.5 in molar ratio with zinc nitrate, ammonium acetate and ammonium nitrate, adds deionized water and stirring and grind to form colloidal state that the deionized water of adding and ammonium acetate mol ratio are 1:1;
(2) colloidal materials of gained in the step (1) is carried out ultra-sonic dispersion, jitter time 5min with power 150W, frequency 20kHz processor for ultrasonic wave;
(3) to put into retort furnace burning synthetic with dispersions obtained in the step (2), and the burning synthesis temperature is 550 ~ 650
0C, burning is synthetic to obtain the safran powder, and powder is ground to dispersion;
(4) with the powder of gained in the step (3) 400
0C ~ 700
0The C environment was annealed 3 hours down, obtained loose yellow powder, was hecaprismo structure zinc oxide of the present invention.
This method is fast and convenient, with low cost, has overcome that additive method power consumption is high, starting material are expensive, has been not easy to shortcoming such as industrialization, can obtain favorable dispersity, the controlled hecaprismo structure Zinc oxide powder of pattern.
Figure of description
The scanning electronic microscope of accompanying drawing 1: embodiment 1 is amplified the Zinc oxide powder of 10,000 times hecaprismo structure.
The scanning electronic microscope of accompanying drawing 2: embodiment 2 is amplified the Zinc oxide powder of 10,000 times hecaprismo structure.
The scanning electronic microscope of accompanying drawing 3: embodiment 3 is amplified the Zinc oxide powder of 20,000 times hecaprismo structure.
Embodiment
Below in conjunction with embodiment the present invention is elaborated, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
With zinc nitrate 0.1mol(29.75g), ammonium acetate 0.3mol(23.12g) and ammonium nitrate 0.01mol(0.80g) mix, add the 0.3mol deionized water and grind to form colloid, carried out ultra-sonic dispersion 5 minutes with the processor for ultrasonic wave of power 150W, frequency 20kHz; It is synthetic that the gained colloid is put into the retort furnace burning, and the burning synthesis temperature is 550
0C, the synthetic product that will burn is ground to dispersion; Powder after the grinding is 400
0Annealing is 3 hours under the C condition, obtains the Zinc oxide powder that has the hecaprismo structure in the accompanying drawing 1.
Embodiment 2
With zinc nitrate 0.1mol(29.75g), ammonium acetate 0.5mol(38.54g) and ammonium nitrate 0.08mol(6.40g), add the 0.5mol deionized water and grind to form colloid, carried out ultra-sonic dispersion 5 minutes with the processor for ultrasonic wave of power 150W, frequency 20kHz; It is synthetic that the gained colloid is put into the retort furnace burning, and the burning synthesis temperature is 600
0C, the synthetic product that will burn is ground to dispersion; Powder after the grinding is 550
0Annealing is 3 hours under the C condition, obtains the Zinc oxide powder that has the hecaprismo structure in the accompanying drawing 2.
Embodiment 3
With zinc nitrate 0.1mol(29.75g), ammonium acetate 0.7mol(53.96g) and ammonium nitrate 0.15mol(12.01g), add the 0.7mol deionized water and grind to form colloid, carried out ultra-sonic dispersion 5 minutes with the processor for ultrasonic wave of power 150W, frequency 20kHz; It is synthetic that the gained colloid is put into the retort furnace burning, and the burning synthesis temperature is 650
0C, the synthetic product that will burn is ground to dispersion; Powder after the grinding is 700
0Annealing is 3 hours under the C condition, obtains the Zinc oxide powder that has the hecaprismo structure in the accompanying drawing 3.
Claims (1)
1. the low-temperature burning synthesis preparation method of a hecaprismo structure zinc oxide is the zinc source with the zinc nitrate, and its feature comprises: A. adds the reaction auxiliary material, the B. preparation method, wherein:
A. described zinc source is a zinc nitrate, and the reaction auxiliary material of adding is ammonium acetate and ammonium nitrate; Zinc nitrate, ammonium acetate and ammonium nitrate proportioning be 1:3 ~ 7:0.1 ~ 1.5 in molar ratio;
B. described preparation method operates according to the following steps:
1) zinc nitrate, ammonium acetate and ammonium nitrate are mixed mutually by the A mol ratio, add deionized water and stirring and grind to form colloidal state, the deionized water of adding and ammonium acetate mol ratio are 1:1;
2) colloidal materials of step 1) gained is carried out ultra-sonic dispersion 5min with the processor for ultrasonic wave of power 150W, frequency 20kHz;
3) with step 2) it is dispersions obtained that to put into retort furnace burning synthetic, and the burning synthesis temperature is 550 ~ 650
0C, burning is synthetic to obtain the safran powder, and powder is ground to dispersion;
4) step 3) gained powder is ground the back 400 ~ 700
0C annealing 3 hours obtains loose yellow powder, is hecaprismo structure zinc oxide of the present invention.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110145483 CN102180513B (en) | 2011-06-01 | 2011-06-01 | Method for preparing hexagonal pyramid-like zinc oxide by low temperature combustion synthesis method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110145483 CN102180513B (en) | 2011-06-01 | 2011-06-01 | Method for preparing hexagonal pyramid-like zinc oxide by low temperature combustion synthesis method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102180513A true CN102180513A (en) | 2011-09-14 |
| CN102180513B CN102180513B (en) | 2013-03-06 |
Family
ID=44566840
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201110145483 Expired - Fee Related CN102180513B (en) | 2011-06-01 | 2011-06-01 | Method for preparing hexagonal pyramid-like zinc oxide by low temperature combustion synthesis method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102180513B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102583505A (en) * | 2012-03-02 | 2012-07-18 | 浙江大学 | Preparation method for ZnO two-dimensional porous material |
| CN107032386A (en) * | 2017-04-12 | 2017-08-11 | 济南大学 | Tetrahedral Zinc oxide single crystal particle and preparation method thereof |
| CN107032387A (en) * | 2017-04-12 | 2017-08-11 | 济南大学 | A kind of six prism-frustum-shaped Zinc oxide particles and preparation method thereof |
| CN109553123A (en) * | 2018-12-05 | 2019-04-02 | 江苏大学 | A kind of iceberg shape ZnO micro materials and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101172641A (en) * | 2007-09-29 | 2008-05-07 | 苏州大学 | Method of producing fleshtone nano-zinc oxide |
-
2011
- 2011-06-01 CN CN 201110145483 patent/CN102180513B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101172641A (en) * | 2007-09-29 | 2008-05-07 | 苏州大学 | Method of producing fleshtone nano-zinc oxide |
Non-Patent Citations (1)
| Title |
|---|
| 《硅酸盐学报》 20100331 李像 等 用沉淀法和燃烧法合成纳米氧化锌 499-503 1 第38卷, 第3期 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102583505A (en) * | 2012-03-02 | 2012-07-18 | 浙江大学 | Preparation method for ZnO two-dimensional porous material |
| CN107032386A (en) * | 2017-04-12 | 2017-08-11 | 济南大学 | Tetrahedral Zinc oxide single crystal particle and preparation method thereof |
| CN107032387A (en) * | 2017-04-12 | 2017-08-11 | 济南大学 | A kind of six prism-frustum-shaped Zinc oxide particles and preparation method thereof |
| CN107032387B (en) * | 2017-04-12 | 2018-07-31 | 济南大学 | Six prism-frustum-shaped Zinc oxide particles of one kind and preparation method thereof |
| CN109553123A (en) * | 2018-12-05 | 2019-04-02 | 江苏大学 | A kind of iceberg shape ZnO micro materials and preparation method thereof |
| CN109553123B (en) * | 2018-12-05 | 2020-11-20 | 江苏大学 | Iceberg-shaped ZnO micron material and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102180513B (en) | 2013-03-06 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108946787B (en) | Preparation method of rare earth-based fluorite type high-entropy oxide powder material | |
| CN102580716B (en) | Method for synthesizing zinc oxide/graphene composite by solvothermal method | |
| CN104276850B (en) | Ultra-fine blue ceramic pigment of a kind of spinel type and preparation method thereof | |
| CN102180513B (en) | Method for preparing hexagonal pyramid-like zinc oxide by low temperature combustion synthesis method | |
| CN103951392B (en) | Method of synthesizing MgO/Y2O3 nano powder by microwave combustion | |
| CN101885071B (en) | Method for preparing copper-zinc-tin-selenium nano powder material | |
| CN102412390A (en) | Preparation method of Li4Ti5O12 wrapped natural graphite for lithium ion battery cathode | |
| CN105731527A (en) | Coprecipitation preparation method of nanoscale indium tin oxide powder | |
| CN109956493B (en) | Preparation method of cerium or/and zinc doped cuprous oxide nano material | |
| CN105932269A (en) | Method for preparing positive electrode material for lithium ion cell by spraying, combusting and pyrolyzing | |
| US20180237314A1 (en) | Synthesis of deep eutectic solvent chemical precursors and their use in the production of metal oxides | |
| CN104291386B (en) | A kind of preparation method of two-dimentional nickel hydroxide ultrathin nanometer film | |
| CN104973615A (en) | Microwave burning preparation method of nano gadolinium oxide powder | |
| CN102134470A (en) | Method for preparing porous carbon born nano ferrite wave-absorbing material | |
| CN103474616A (en) | Sol precipitation preparation method for carbon-coated lithium iron silicate cathode material | |
| CN106517360B (en) | A kind of particle self assembly cobaltosic oxide micron spherical powder and preparation method thereof | |
| CN103342396B (en) | Method for microwave liquid-phase synthesis of graphene-like two-dimensional nickel hydroxide nano material | |
| CN102897722B (en) | Alpha-In2Se3 nano-grade flower-ball solvothermal synthesizing method | |
| CN101214997A (en) | Method for fast preparing lamellate potassium titanate | |
| WO2013185453A1 (en) | Method for preparing monoclinic ga2s3 crystal and use in optics thereof | |
| CN100595160C (en) | Method for preparing tin oxide nanocrystalline coated by organic ligand | |
| CN101602596A (en) | A kind of lithium tantalate nano powder and preparation method thereof | |
| CN105600814B (en) | One kind prepares flower-like structure Cu2The method of O photoelectric materials | |
| CN102259909B (en) | Preparation method of lead carbonate combustion catalyst for solid propellant | |
| CN102161500A (en) | Preparation method of cobalt-doped zinc oxide nano-material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20130306 Termination date: 20140601 |