CN102849780A - Method for synthesizing ZnO nano-structure by using organic weak base - Google Patents
Method for synthesizing ZnO nano-structure by using organic weak base Download PDFInfo
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- CN102849780A CN102849780A CN2012103354263A CN201210335426A CN102849780A CN 102849780 A CN102849780 A CN 102849780A CN 2012103354263 A CN2012103354263 A CN 2012103354263A CN 201210335426 A CN201210335426 A CN 201210335426A CN 102849780 A CN102849780 A CN 102849780A
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Abstract
The invention relates to a method for synthesizing a ZnO nano-structure by using organic weak base. According to the invention, zinc acetate is added into a medium, and the mixture is stirred, such that a zinc acetate solution with a Zn<2+> concentration of 0.01-0.04M is obtained. The zinc acetate solution is subjected to a reaction for 1-3h in a constant-temperature water-bath tank with a temperature of 80-95 DEG C; and the materials are naturally cooled; an obtained product is separated, washed, and bake-dried, such that nano-structured ZnO is obtained. The medium is organic weak base or a mixed solution of water and organic weak base. The medium can serve as a solvent, and can serve as a reactant. According to the invention, through the change upon an organic-weak-base-to-water ratio, different zinc oxide nano-structures can be prepared. According to the invention, under the condition that no other surfactant or chelating agent is added, different ZnO nano-structures can be rapidly prepared. The method provided by the invention has the advantages of simple process, wide and easy-to-obtain raw materials, substantial controlling effect, low cost, suitability for industrialized large-scale productions, and the like.
Description
Technical field
The present invention relates to a kind of method of synthetic ZnO nano-structure, relate in particular to the method for the synthetic ZnO nano-structure of a kind of organic weak base.
Background technology
ZnO is the important low-cost semiconductor material of II-VI, is widely used in catalyzer, pressure-sensitive device, and photoelectron and photoelectrochemistry more receive people's concern in recent years.The preparation method of ZnO nanorod mainly comprises gas phase thermochemistry synthesis method, metal organic chemical vapor deposition, physical evaporation, molecular beam epitaxy, template and chemical hydrothermal method etc. at present.Comparatively speaking, it is simple that chemical hydrothermal method has equipment, and reaction conditions is gentle, need not catalyzer, the characteristics such as environmental friendliness.The technique of the standby ZnO nano-structure of general traditional hydrothermal solution legal system as reagent, also can be added some tensio-active agents or complexing agent with vulkacit H or sodium hydroxide usually.The people such as ZhouYing utilize hydrothermal method to adjust 95 ℃ of reactions of temperature of reaction 4h by adding polyethylene, have prepared zinc oxide nano rod (Ying Zhou et al.Materials Research Bulletin, 43,2113(2008)).The people such as EIJI HOSONO are take zinc acetate as raw material, by the ratio of control alcohol-water, do not add alkali, prepare spherical ZnO nano-structure (EIJI HOSONO et al.J SOL-GEL SCI TECHN., 29,71(2004)).The people such as Sriparna Chatterjee with zinc nitrate as the zinc source, add cetyl trimethylammonium bromide, at 90 ℃ of reaction kettle for reaction 12h, prepare template ZnO crystal (Sriparna Chatterjee et al.J NANOSCI NANOTECHNO., 11,10379 (2011)).This shows that by hydrothermal method, different solvent systems can be prepared the ZnO structure of different-shape.Present method utilizes organic weak base to substitute the ZnO nano-structure that traditional vulkacit H is prepared different shape first.Compare with traditional method, novel part of the present invention be organic weak base in experiment namely as raw material, can be used as again solvent, by changing the organic weak base content control nano particle form in the reaction medium.
Summary of the invention
The objective of the invention is to provide in order to improve the deficiencies in the prior art the method for the synthetic ZnO nano-structure of a kind of organic weak base.It is simple that the method has a synthesis technique, need not to add tensio-active agent or complexing agent, and cost is low, is fit to the advantage of scale operation.
Technical scheme of the present invention is: the method for the synthetic ZnO nano-structure of a kind of organic weak base, and its concrete steps are as follows:
Zinc acetate joined in the medium stir, join to get Zn
2+Concentration is the zinc acetate solution of 0.01～0.04M; Then zinc acetate solution is placed 80～95 ℃ of constant temperature water baths to react 1～3h, naturally cooling; With the product centrifugation, washing is dried, and obtains Nano ZnO again; Wherein said medium is the mixing solutions of organic weak base or water and organic weak base.
Preferred described organic weak base is N,N-DIMETHYLACETAMIDE, dimethyl formamide, methane amide, HMPA or N, N-dimethyl propylene acid amides.The volume ratio of water and organic weak base is 1:4 ~ 4:1 in the mixing solutions of preferably water and organic weak base.
The churning time that preferably zinc acetate is joined in the medium is 10～30min; The rotating speed of preferred centrifugation is 2000～4000rpm, and the centrifugation time is 5～15min.Preferred above-mentioned bake out temperature is 180～220 ℃.Preferred washing process is used absolute ethanol washing 3～5 times again for using first the deionized water washed product 3～5 times.
Beneficial effect:
1) the hydrothermal method technique of traditional making ZnO nanostructure often with vulkacit H as reagent, exist to need add the shortcomings such as tensio-active agent or complexing agent.Maximum characteristics of the present invention are to use organic weak base to substitute vulkacit H, and it can be used as again reagent namely as solvent, under the condition that need not add any subsidiary, synthesizes ZnO nano-structure.
2) the used equipment of the inventive method is simple, does not use large-scale or specific equipment, and technical threshold is low, and is easy to operate, and cost is low, is suitable for scale operation.
Description of drawings
Fig. 1 is organic weak base and the ZnO nano-structure scanning electron microscope (SEM) photograph of water different volumes than lower preparation;
Fig. 2 is organic weak base and the ZnO nano-structure XRD figure of water different volumes than lower preparation.
Embodiment
To help to understand the present invention by following example, but not limit content of the present invention.
Embodiment 1
Take by weighing 0.2195gZn (CH
3COO)
22H
2O puts into beaker, then measures the 50ml N,N-DIMETHYLACETAMIDE and joins in the beaker, and mechanical stirring 10min under 400 rev/mins of speed obtains muddy solution.Again above-mentioned reaction soln is placed 80 ℃ constant water bath box, reaction 1h.Reaction finishes, and naturally cools to room temperature.Centrifugation 5min obtains product under 2000 rev/mins of speed.Product is washed respectively 5 times with deionized water wash 3 times and dehydrated alcohol, then at 180 ℃ of dry 3h, obtain the ZnO nano-structure powder.Fig. 1 a is the X-ray diffractogram of present embodiment synthetic powder, spectral line peak and JCPDS among the figure, and the NO.36-1451 card conforms to substantially, and three characteristic strong peaks appear at 2 θ=31.20 °, 34.20 °, 35.60 ° in the XRD diffracting spectrum; (100), (002), (101) face of these three the corresponding ZnO of strong peak difference, near and the diffraction peak that weak ZnO (102), (110), (103) face 47.50 °, 56.60 °, 62.90 °, have occurred, show that prepared sample is six side's phase ZnO crystals, its crystallinity is good.Fig. 2 a is for originally executing the scanning electron microscope (SEM) photograph of routine synthetic powder, and visible ZnO nano material is particulate state, and the product diameter is about 60nm.
Embodiment 2
Take by weighing 0.2195gZn (CH
3COO)
22H
2O puts into beaker, then measures water and the dimethyl formamide that the 100ml volume ratio is 1:4 and joins in the beaker, and mechanical stirring 13min under 500 rev/mins of speed obtains muddy solution.Again above-mentioned reaction soln is placed 80 ℃ constant water bath box, reaction 1.5h.Reaction finishes, and naturally cools to room temperature.Centrifugation 10min obtains product under 2500 rev/mins of speed.Product is washed respectively 3 times with deionized water wash 5 times and dehydrated alcohol, then at 190 ℃ of dry 4h, obtain the ZnO nano-structure powder.Fig. 1 b is the X-ray diffractogram of present embodiment synthetic powder, spectral line peak and JCPDS among the figure, and the NO.36-1451 card conforms to substantially, and three characteristic strong peaks appear at 2 θ=31.20 °, 34.20 °, 35.60 ° in the XRD diffracting spectrum; (100), (002), (101) face of these three the corresponding ZnO of strong peak difference, near and the diffraction peak that weak ZnO (102), (110), (103) face 47.50 °, 56.60 °, 62.90 °, have occurred, show that prepared sample is six side's phase ZnO crystals, its crystallinity is good.Fig. 2 b is for originally executing the scanning electron microscope (SEM) photograph of routine synthetic powder, and visible ZnO nano material is hamburger shape, and particle diameter is about 100nm.
Take by weighing 0.7024gZn (CH
3COO)
22H
2O puts into beaker, then measures water and the methane amide that the 80ml volume ratio is 2:3 and joins in the beaker, and mechanical stirring 15min under 700 rev/mins of speed obtains muddy solution.Again above-mentioned reaction soln is placed 90 ℃ constant water bath box, reaction 1.5h.Reaction finishes, and naturally cools to room temperature.Centrifugation 12min obtains product under 3000 rev/mins of speed.Product is washed respectively 3 times with deionized water and dehydrated alcohol, then at 190 ℃ of dry 3h, obtain the ZnO nano-structure powder.Fig. 1 c is the X-ray diffractogram of present embodiment synthetic powder, spectral line peak and JCPDS among the figure, and the NO.36-1451 card conforms to substantially, and three characteristic strong peaks appear at 2 θ=31.20 °, 34.20 °, 35.60 ° in the XRD diffracting spectrum; (100), (002), (101) face of these three the corresponding ZnO of strong peak difference, near and the diffraction peak that weak ZnO (102), (110), (103) face 47.50 °, 56.60 °, 62.90 °, have occurred, show that prepared sample is six side's phase ZnO crystals, its crystallinity is good.Fig. 2 c is for originally executing the scanning electron microscope (SEM) photograph of routine synthetic powder, and visible ZnO nano material is twin nut shape, and diameter is about 200-300nm, and long is 3-5 μ m.
Embodiment 4
Take by weighing 0.3725gZn (CH
3COO)
22H
2O puts into beaker, then measures water and the HMPA that the 100ml volume ratio is 3:2 and joins in the beaker, and mechanical stirring 20min under 600 rev/mins of speed obtains muddy solution.Again above-mentioned reaction soln is placed 90 ℃ constant water bath box, reaction 3h.Reaction finishes, and naturally cools to room temperature.Centrifugation 8min obtains product under 2000 rev/mins of speed.Product is washed respectively 3 times with deionized water and dehydrated alcohol, then at 185 ℃ of dry 3h, obtain the ZnO nano-structure powder.Fig. 1 d is the X-ray diffractogram of present embodiment synthetic powder, spectral line peak and JCPDS among the figure, and the NO.36-1451 card conforms to substantially, and three characteristic strong peaks appear at 2 θ=31.20 °, 34.20 °, 35.60 ° in the XRD diffracting spectrum; (100), (002), (101) face of these three the corresponding ZnO of strong peak difference, near and the diffraction peak that weak ZnO (102), (110), (103) face 47.50 °, 56.60 °, 62.90 °, have occurred, show that prepared sample is six side's phase ZnO crystals, its crystallinity is good.Fig. 2 d is for originally executing the scanning electron microscope (SEM) photograph of routine synthetic powder, and visible ZnO nano material is nano bar-shape, and diameter is about 300-400nm, is about 5-6 μ m.
Embodiment 5
Take by weighing 0.3011gZn (CH
3COO)
22H
2O puts into beaker, then measures water and N that the 60ml volume ratio is 1:4, and N-dimethyl propylene acid amides joins in the beaker, and mechanical stirring 25min under 500 rev/mins of speed obtains muddy solution.Again above-mentioned reaction soln is placed 95 ℃ constant water bath box, reaction 2.5h.Reaction finishes, and naturally cools to room temperature.Centrifugation 14min obtains product under 3000 rev/mins of speed.Product is washed respectively 3 times with deionized water and dehydrated alcohol, then at 215 ℃ of dry 3h, obtain the ZnO nano-structure powder.Fig. 1 e is the X-ray diffractogram of present embodiment synthetic powder, spectral line peak and JCPDS among the figure, and the NO.36-1451 card conforms to substantially, and three characteristic strong peaks appear at 2 θ=31.20 °, 34.20 °, 35.60 ° in the XRD diffracting spectrum; (100), (002), (101) face of these three the corresponding ZnO of strong peak difference, near and the diffraction peak that weak ZnO (102), (110), (103) face 47.50 °, 56.60 °, 62.90 °, have occurred, show that prepared sample is six side's phase ZnO crystals, its crystallinity is good.Fig. 2 e is for originally executing the scanning electron microscope (SEM) photograph of routine synthetic powder, and visible ZnO nano material is long nano bar-shape, and diameter is about 400-500nm, long 8-10 μ m.
This ZnO nanorod has higher luminous efficiency and stable preferably, is expected to be applied in the fields such as illumination, demonstration and laser.
Claims (7)
1. the method for the synthetic ZnO nano-structure of an organic weak base, its concrete steps are as follows:
Zinc acetate joined in the medium stir, join to get Zn
2+Concentration is the zinc acetate solution of 0.01～0.04M; Then zinc acetate solution is placed 80～95 ℃ of constant temperature water baths to react 1～3h, naturally cooling; With the product centrifugation, washing is dried, and obtains Nano ZnO again; Wherein said medium is the mixing solutions of organic weak base or water and organic weak base.
2. method according to claim 1 is characterized in that described organic weak base is N,N-DIMETHYLACETAMIDE, dimethyl formamide, methane amide, HMPA or N, N-dimethyl propylene acid amides.
3. method according to claim 1 is characterized in that the volume ratio of water and organic weak base is 1:4 ~ 4:1 in the mixing solutions of water and organic weak base.
4. method according to claim 1 is characterized in that the churning time that zinc acetate is joined in the medium is 10～30min.
5. method according to claim 1, the rotating speed that it is characterized in that centrifugation is 2000～4000rpm, the centrifugation time is 5～15min.
6. method according to claim 1 is characterized in that described bake out temperature is 180～220 ℃.
7. method according to claim 1 is characterized in that washing process for using first the deionized water washed product 3～5 times, uses absolute ethanol washing 3～5 times again.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106186047A (en) * | 2016-08-05 | 2016-12-07 | 武汉理工大学 | A kind of based on secondary nanosphere hierarchical Z nO nano material and preparation method thereof |
| CN108275713A (en) * | 2018-02-08 | 2018-07-13 | 东华大学 | The preparation method of the micro-nano ZnO of morphology controllable under the conditions of a kind of atmospheric low-temperature |
| CN110451555A (en) * | 2019-09-06 | 2019-11-15 | 辽宁星空钠电电池有限公司 | A kind of method that rapid precipitation prepares one-dimensional zinc hydroxide nanometer rods |
| CN111573712A (en) * | 2020-05-26 | 2020-08-25 | 安徽锦华氧化锌有限公司 | Preparation method for improving antibacterial property of nano zinc oxide |
| CN112110475A (en) * | 2020-09-24 | 2020-12-22 | 安徽省含山县锦华氧化锌厂 | Production process for preparing zinc oxide by using paste precursor |
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| JP2005298282A (en) * | 2004-04-13 | 2005-10-27 | Daicel Chem Ind Ltd | Suspension of zinc oxide particles |
| CN101214990A (en) * | 2007-12-28 | 2008-07-09 | 中国科学院上海硅酸盐研究所 | Normal temperature synthesis method for nanometer zinc oxide |
| CN101817548A (en) * | 2010-04-27 | 2010-09-01 | 中山大学 | Method for preparing zinc oxide hollow spheres |
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| JP2005298282A (en) * | 2004-04-13 | 2005-10-27 | Daicel Chem Ind Ltd | Suspension of zinc oxide particles |
| CN101214990A (en) * | 2007-12-28 | 2008-07-09 | 中国科学院上海硅酸盐研究所 | Normal temperature synthesis method for nanometer zinc oxide |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106186047A (en) * | 2016-08-05 | 2016-12-07 | 武汉理工大学 | A kind of based on secondary nanosphere hierarchical Z nO nano material and preparation method thereof |
| CN106186047B (en) * | 2016-08-05 | 2017-12-05 | 武汉理工大学 | One kind is based on secondary nanosphere hierarchical Z nO nano materials and preparation method thereof |
| CN108275713A (en) * | 2018-02-08 | 2018-07-13 | 东华大学 | The preparation method of the micro-nano ZnO of morphology controllable under the conditions of a kind of atmospheric low-temperature |
| CN110451555A (en) * | 2019-09-06 | 2019-11-15 | 辽宁星空钠电电池有限公司 | A kind of method that rapid precipitation prepares one-dimensional zinc hydroxide nanometer rods |
| CN111573712A (en) * | 2020-05-26 | 2020-08-25 | 安徽锦华氧化锌有限公司 | Preparation method for improving antibacterial property of nano zinc oxide |
| CN112110475A (en) * | 2020-09-24 | 2020-12-22 | 安徽省含山县锦华氧化锌厂 | Production process for preparing zinc oxide by using paste precursor |
| CN112110475B (en) * | 2020-09-24 | 2022-06-21 | 安徽省含山县锦华氧化锌厂 | Production process for preparing zinc oxide by using paste precursor |
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Application publication date: 20130102 |