CN102161500A - Preparation method of cobalt-doped zinc oxide nano-material - Google Patents
Preparation method of cobalt-doped zinc oxide nano-material Download PDFInfo
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- CN102161500A CN102161500A CN 201110045045 CN201110045045A CN102161500A CN 102161500 A CN102161500 A CN 102161500A CN 201110045045 CN201110045045 CN 201110045045 CN 201110045045 A CN201110045045 A CN 201110045045A CN 102161500 A CN102161500 A CN 102161500A
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- zinc oxide
- doped zinc
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Abstract
The invention discloses a preparation method of a cobalt-doped zinc oxide nano-material, which is used for solving the technical problem that the preparation temperature is high in the traditional method for preparing the cobalt-doped zinc oxide nano-material. The preparation method disclosed in the invention comprises the following steps of: mixing weighed Zn (CH3COO) 2. 2H2O and Co (CH3COO) 2. 4H2O together, adding ethanol according to the molar ratio of metal ions to the ethanol being 1:80-1:150, stirring with a glass rod and then vibrating with ultrasound; transferring the mixed solution into a high-pressure kettle, raising temperature to 150-200 DEG C at a temperature rise rate of 1-5 DEG C/min, holding for 3-10 hours and then cooling together with a furnace; and taking reactants out, vacuum-filtering and washing with deionized water and then drying to obtain the cobalt-doped zinc oxide nanomaterial. Since a liquid phase synthesis method is adopted, a cobalt-doped zinc oxide nanoparticle with the average size of 30nm is prepared, and the preparation temperature of the cobalt-doped zinc oxide nanoparticle is reduced. The preparation temperature is reduced from 200-700 DEG C to 150-190 DEG C as compared with the preparation temperature in the prior art.
Description
Technical field
The present invention relates to a kind of preparation method of nano zinc oxide material, particularly a kind of cobalt doped zinc oxide nano preparation methods.
Background technology
Document " Synthesis and characterization of Zn
1-xMn
xO nanowires; Appl.Phys.Lett.; 2008; 92:162102-162104 " preparation manganese doped zinc oxide nano-wire material method disclosed under a kind of argon shield; and having synthesized mean diameter by vapor phase process under 500 ℃ is 60nm; length is the zinc oxide nanowire of 100 μ m, has product diameter advantage of uniform.
But this method exist preparation temperature height (200～700 ℃), preparation time long (＞3h), high temperature service complexity, the high deficiency of power consumption, limited the widespread use of this method.
Summary of the invention
Prepare the high deficiency of manganese doped zinc oxide nano-wire material preparation temperature in order to overcome existing method, the invention provides a kind of cobalt doped zinc oxide nano preparation methods, adopt liquid phase synthetic method, can reduce the preparation temperature of cobalt doped zinc oxide nano material.
The technical solution adopted for the present invention to solve the technical problems is: a kind of cobalt doped zinc oxide nano preparation methods is characterized in may further comprise the steps:
(a) according to chemical constitution Zn
1-xCo
xO, wherein, x=0～0.1 takes by weighing Zn (CH
3COO)
22H
2O and Co (CH
3COO)
24H
2O;
(b) with load weighted Zn (CH
3COO)
22H
2O and Co (CH
3COO)
24H
2The O raw material directly mixes, and is 1: 80～1: 150 adding ethanol by metal ion and alcoholic acid mol ratio, after stirring with glass stick, shakes 10～30min in ultrasonic wave;
(c) mixing solutions with step (b) preparation changes in the autoclave, rises to 150～200 ℃, furnace cooling behind insulation 3～8h with the temperature rise rate of 1～3 ℃/min;
(d) take out the reactant that step (c) is prepared, with the deionized water filtering and washing repeatedly after, it is dry to put into vacuum drying oven, obtains cobalt doped zinc oxide nano material.
The invention has the beneficial effects as follows: owing to adopt liquid phase synthetic method, having prepared mean sizes is the cobalt doped zinc oxide nano particle of 30nm.Reduced cobalt doped zinc oxide nano particulate preparation temperature.Compared with prior art, its preparation temperature is reduced to 150～190 ℃ by 200～700 ℃.
Below in conjunction with the drawings and specific embodiments the present invention is elaborated.
Description of drawings
Fig. 1 is the inventive method embodiment 1～4 prepared Zn
1-xCo
xThe XRD figure spectrum of O nano material.
Fig. 2 is the inventive method embodiment 4 prepared Zn
1-xCo
xThe SEM photo of O (0≤x≤0.084) nano material.
Embodiment
Embodiment 1, takes by weighing 1.097g Zn (CH
3COO)
22H
2Co (the CH of O and 0g
3COO)
24H
2O; Two kinds of raw materials are directly mixed, add the ethanol of 23mL then, stir the back with glass stick and in ultrasonic wave, shake 10min; Then mixing solutions is changed in the autoclave, rise to 150 ℃, furnace cooling behind the insulation 8h with the temperature rise rate of 1 ℃/min; Take out reactant, with the deionized water filtering and washing repeatedly after, it is dry to put into vacuum drying oven, obtains cobalt doped zinc oxide nano material.
As can be seen from Figure 1, each diffraction peak can be demarcated with the diffraction peak of single hexagonal wurtzite zinc oxide.Not relevant with other crystalline structure assorted peak occurs, and the prepared Zn of present embodiment is described
1-xCo
xThe O nano material has single hexagonal wurtzite structure.According to the strong and sharp-pointed degree in peak of diffraction peak, can judge the prepared Zn of present embodiment
1-xCo
xO nano material crystallinity is good.In addition, structure relevant with Co on the diffraction peak occurs, and expression Co enters in the middle of the ZnO lattice by replacement Zn.
Embodiment 2, take by weighing 1.097g Zn (CH
3COO)
22H
2Co (the CH of O and 0.013g
3COO)
24H
2O; Two kinds of raw materials are directly mixed, add the ethanol of 30mL then, stir the back with glass stick and in ultrasonic wave, shake 15min; Then mixing solutions is changed in the autoclave, rise to 180 ℃, furnace cooling behind the insulation 7h with the temperature rise rate of 2 ℃/min; Take out reactant, with the deionized water filtering and washing repeatedly after, it is dry to put into vacuum drying oven, obtains cobalt doped zinc oxide nano material.
Embodiment 3, take by weighing 1.097g Zn (CH
3COO)
22H
2Co (the CH of O and 0.039g
3COO)
24H
2O; Two kinds of raw materials are directly mixed, add the ethanol of 30mL then, stir the back with glass stick and in ultrasonic wave, shake 20min; Then mixing solutions is changed in the autoclave, rise to 190 ℃, furnace cooling behind the insulation 5h with the temperature rise rate of 3 ℃/min; Take out reactant, with the deionized water filtering and washing repeatedly after, it is dry to put into vacuum drying oven, obtains cobalt doped zinc oxide nano material.
Embodiment 4, take by weighing 1.097g Zn (CH
3COO)
22H
2Co (the CH of O and 0.122g
3COO)
24H
2O; Two kinds of raw materials are directly mixed, add the ethanol of 44mL then, stir the back with glass stick and in ultrasonic wave, shake 30min; Then mixing solutions is changed in the autoclave, rise to 200 ℃, furnace cooling behind the insulation 3h with the temperature rise rate of 3 ℃/min; Take out reactant, with the deionized water filtering and washing repeatedly after, it is dry to put into vacuum drying oven, obtains cobalt doped zinc oxide nano material.
As can be seen from Figure 2, Co mixes does not influence prepared Zn to the pattern generation of product is tangible
1-xCo
xThe pattern of O nano material all is particulate state.
The contriver is in the disclosed process parameters range of technical scheme, and different parameter collocation are all tested, and have all obtained good effect.
The simple solvent thermal process of the present invention is synthesizing Zn below 200 ℃
1-xCo
xO is nanocrystalline, and its preparation temperature is lower, helps being extensive use of.
Claims (1)
1. a cobalt doped zinc oxide nano preparation methods is characterized in that comprising the steps:
(a) according to chemical constitution Zn
1-xCo
xO, wherein, x=0～0.1 takes by weighing Zn (CH
3COO)
22H
2O and Co (CH
3COO)
24H
2O;
(b) with load weighted Zn (CH
3COO)
22H
2O and Co (CH
3COO)
24H
2The O raw material directly mixes, and is 1: 80～1: 150 adding ethanol by metal ion and alcoholic acid mol ratio, after stirring with glass stick, shakes 10～30min in ultrasonic wave;
(c) mixing solutions with step (b) preparation changes in the autoclave, rises to 150～200 ℃, furnace cooling behind insulation 3～8h with the temperature rise rate of 1～3 ℃/min;
(d) take out the reactant that step (c) is prepared, with the deionized water filtering and washing repeatedly after, it is dry to put into vacuum drying oven, obtains cobalt doped zinc oxide nano material.
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|---|---|---|---|
| CN 201110045045 CN102161500A (en) | 2011-02-24 | 2011-02-24 | Preparation method of cobalt-doped zinc oxide nano-material |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110045045 CN102161500A (en) | 2011-02-24 | 2011-02-24 | Preparation method of cobalt-doped zinc oxide nano-material |
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| Publication Number | Publication Date |
|---|---|
| CN102161500A true CN102161500A (en) | 2011-08-24 |
Family
ID=44463002
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103446965A (en) * | 2013-09-09 | 2013-12-18 | 青岛科技大学 | Preparation method of nickel-doped alpha-Fe2O3 multi-level structure spinous microspheres |
| CN103602334A (en) * | 2013-08-06 | 2014-02-26 | 常州大学 | Sulfide fluorescent material and preparation method thereof |
| CN108190970A (en) * | 2018-01-08 | 2018-06-22 | 上海理工大学 | A kind of preparation method and applications of Co-doped ZnO gas sensitive |
| CN114180634A (en) * | 2020-09-15 | 2022-03-15 | 海安南京大学高新技术研究院 | ZnMnO with cage structure4Preparation process of nano sensing material |
-
2011
- 2011-02-24 CN CN 201110045045 patent/CN102161500A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 《Appl Phys A：Materials Science & Processing》 20091125 Jin Li et al. Enhanced blue-green emission and ethanol sensing of Co-doped ZnO nanocrystals prepared by a solvothermal route 537-542 1 第98卷, * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103602334A (en) * | 2013-08-06 | 2014-02-26 | 常州大学 | Sulfide fluorescent material and preparation method thereof |
| CN103602334B (en) * | 2013-08-06 | 2015-10-28 | 常州大学 | A kind of all-sulphide phosphor and preparation method thereof |
| CN103446965A (en) * | 2013-09-09 | 2013-12-18 | 青岛科技大学 | Preparation method of nickel-doped alpha-Fe2O3 multi-level structure spinous microspheres |
| CN103446965B (en) * | 2013-09-09 | 2015-04-08 | 青岛科技大学 | Preparation method of nickel-doped alpha-Fe2O3 multi-level structure spinous microspheres |
| CN108190970A (en) * | 2018-01-08 | 2018-06-22 | 上海理工大学 | A kind of preparation method and applications of Co-doped ZnO gas sensitive |
| CN114180634A (en) * | 2020-09-15 | 2022-03-15 | 海安南京大学高新技术研究院 | ZnMnO with cage structure4Preparation process of nano sensing material |
| CN114180634B (en) * | 2020-09-15 | 2023-06-13 | 海安南京大学高新技术研究院 | ZnMnO with cage-shaped structure 4 Preparation process of nano sensing material |
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Application publication date: 20110824 |