CN101220509A - Low-temperature hydrothermal method for manufacturing zinc oxide nanocrystalline whisker - Google Patents
Low-temperature hydrothermal method for manufacturing zinc oxide nanocrystalline whisker Download PDFInfo
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- CN101220509A CN101220509A CNA2007100712947A CN200710071294A CN101220509A CN 101220509 A CN101220509 A CN 101220509A CN A2007100712947 A CNA2007100712947 A CN A2007100712947A CN 200710071294 A CN200710071294 A CN 200710071294A CN 101220509 A CN101220509 A CN 101220509A
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Abstract
The invention discloses a low temperature water heating preparing method of zinc oxide nanometer whisker, and the steps are as follows: 1) Zn salt and alkali are prepared into uniform Zn(OH)4<2-> water solution; 2) the Zn(OH)4<2-> water solution is added into the mixed solvent of glycerol and water, and then polyacrylamide is added into the solvent, and the solvent is heated and magnetically stirred at 80 to 100 DEG C until the matter is dissolved completely, then the mixture is put in a high-pressure reactor and sealed; the reaction is done at 170 to 190 DEG C, and after the reaction is finished, the obtained matter is cooled to the room temperature, and then the product is washed repeatedly by de-ionized water and is done with vacuum drying at 80 to 100 DEG C. The preparing method of the invention has the advantages of simple operation, low cost, removing the processes of high temperature sintering and ball milling, saving energy, being beneficial to environmental protection and avoiding powder hard agglomeration, impurity and structural defect.
Description
Technical field
The present invention relates to the preparation method of zinc oxide nanocrystalline whisker, belong to the ceramic material technical field.
Background technology
Zinc oxide is a kind of important broad stopband direct band gap (E
g=3.37eV) semiconductor material has the hexagonal wurtzite crystal structure.The quantum size effect of zinc oxide nanocrystalline whisker, small-size effect, surface effects and interfacial effect make it have excellent electricity, optics, mechanics, photochemical catalysis, sensing capabilities, are a kind of semiconductor materials with significant application value.Zinc oxide nanocrystalline whisker can be widely used in aspects such as rubber accelerator, gas sensor, UV-preventing material, transformer.Because zinc oxide nanocrystalline whisker at room temperature has the exciton binding energy up to 60meV, can be used for making the short-wavelength light electrical part, as photodiode, ultraviolet light detector, high frequency filter and ultraviolet laser etc., make luminescent device and can obtain the higher gain of light, make zinc oxide have huge potential using value aspect the optical storage density increasing substantially.Zinc oxide nanocrystalline whisker also has high-level efficiency, low voltage phosphorescent, therefore can be with a wide range of applications at industrial circles such as Field Emission Display peace panel displays as the luminescent material of low voltage flat-panel monitor.
At present the preparation method of relevant zinc oxide nanocrystalline whisker mainly contains: vacuum method, vacuum control oxygen t method, vacuum arc method, with the zinc oxide concentrate be raw material wet chemistry method, to contain the zinc waste with metallurgy be the vapor phase process of raw material, with the liquid crystalline cpd be the ultrasonic sol method of template, nearly room temperature condition down one go on foot solid state reaction etc.But these preparation methods' equipment, technology and complex process, cost is higher.
Summary of the invention
The low-temperature hydrothermal method for manufacturing that the purpose of this invention is to provide the zinc oxide nanocrystalline whisker that a kind of technology is simple, cost is low.
The low-temperature hydrothermal method for manufacturing of zinc oxide nanocrystalline whisker of the present invention may further comprise the steps:
1) with Zn salt and alkali [OH in molar ratio
-]: [Zn] was mixed with uniform Zn (OH) in 10: 1～12: 1
4 2-The aqueous solution;
2) with Zn (OH)
4 2-The volume ratio that the aqueous solution is added to glycerol and water is in 13: 4～13: 6 the double solvents, Zn (OH)
4 2-The volume ratio of the aqueous solution and double solvents is 1: 6～7, adds the polyacrylamide of 1g/L～3g/L then, 80～100 ℃ of heating magnetic agitation dissolvings extremely fully down, continues sonic oscillation 5～30min;
3) with step 2) solution that makes places autoclave, sealing, at 170～190 ℃ of reaction 5～20h, reaction finishes and is cooled to room temperature, and product deionized water repetitive scrubbing 80～100 ℃ of following vacuum-dryings, promptly gets product.
Above-mentioned Zn salt can be Zn (CH
3COO)
22H
2O, Zn (NO
3)
2Or ZnCl
2
Beneficial effect of the present invention is: the preparation method is simple to operate, and is with low cost, saved high temperature sintering and mechanical milling process, is a kind of saving energy, and environmental method can be avoided powder hard aggregation, impurity and textural defect; Be convenient to suitability for industrialized production.
Description of drawings
Fig. 1 is the field emission scan photo of zinc oxide nanocrystalline whisker.
Fig. 2 is the transmission electron microscope photo of zinc oxide nanocrystalline whisker.
Embodiment
Further specify the preparation method below in conjunction with embodiment.
Embodiment 1
1) takes by weighing an amount of Zn (CH
3COO)
22H
2O and NaOH, [OH in molar ratio
-]: [Zn] is mixed with uniform Zn (OH) at 11: 1
4 2-The aqueous solution;
2) with 10mlZn (OH)
4 2-The volume ratio that the aqueous solution is added to 65ml glycerol and water is in 13: 5 the double solvents, adds the polyacrylamide of 2g/L again, 90 ℃ down the heating magnetic agitation continue sonic oscillation 30min to dissolving fully;
3) with step 2) solution that makes places the teflon-lined autoclave, sealing, at 180 ℃ of reaction 20h, reaction finishes and is cooled to room temperature, and centrifugation deionized water repetitive scrubbing is at 90 ℃ of following vacuum-drying 5h.Obtain zinc oxide nanocrystalline whisker.The nano whisker structure is seen illustrated in figures 1 and 2.
Embodiment 2
1) takes by weighing an amount of Zn (NO
3)
2And NaOH, [OH in molar ratio
-]: [Zn] is mixed with uniform Zn (OH) at 10: 1
4 2-The aqueous solution;
2) with 10mlZn (OH)
4 2-The volume ratio that the aqueous solution is added to 70ml glycerol and water is in 13: 5 the double solvents, adds the polyacrylamide of 3g/L again, 90 ℃ down the heating magnetic agitation continue sonic oscillation 30min to dissolving fully;
3) with step 2) solution that makes places the teflon-lined autoclave, sealing, at 190 ℃ of reaction 18h, reaction finishes and is cooled to room temperature, and centrifugation deionized water repetitive scrubbing at 90 ℃ of following vacuum-drying 5h, obtains zinc oxide nanocrystalline whisker.
Claims (2)
1. the low-temperature hydrothermal method for manufacturing of a zinc oxide nanocrystalline whisker is characterized in that may further comprise the steps:
1) with Zn salt and alkali [OH in molar ratio
-]: [Zn] was mixed with uniform Zn (OH) in 10: 1～12: 1
4 2-The aqueous solution;
2) with Zn (OH)
4 2-The volume ratio that the aqueous solution is added to glycerol and water is in 13: 4～13: 6 the double solvents, Zn (OH)
4 2-The volume ratio of the aqueous solution and double solvents is 1: 6～7, adds the polyacrylamide of 1g/L～3g/L then, 80～100 ℃ of heating magnetic agitation dissolvings extremely fully down, continues sonic oscillation 5～30min;
3) with step 2) solution that makes places autoclave, sealing, at 170～190 ℃ of reaction 5～20h, reaction finishes and is cooled to room temperature, and product deionized water repetitive scrubbing 80～100 ℃ of following vacuum-dryings, promptly gets product.
2. the low-temperature hydrothermal method for manufacturing of zinc oxide nanocrystalline whisker according to claim 1 is characterized in that said Zn salt is Zn (CH
3COO)
22H
2O, Zn (NO
3)
2Or ZnCl
2
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200710071294A CN100591810C (en) | 2007-09-13 | 2007-09-13 | Low-temperature hydrothermal method for manufacturing zinc oxide nanocrystalline whisker |
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|---|---|---|---|
| CN200710071294A CN100591810C (en) | 2007-09-13 | 2007-09-13 | Low-temperature hydrothermal method for manufacturing zinc oxide nanocrystalline whisker |
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| Publication Number | Publication Date |
|---|---|
| CN101220509A true CN101220509A (en) | 2008-07-16 |
| CN100591810C CN100591810C (en) | 2010-02-24 |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102337581A (en) * | 2011-09-20 | 2012-02-01 | 清华大学 | Method for preparing zinc oxide crystal whisker by using recyclable solvent in low-temperature hydrothermal way |
| CN102817078A (en) * | 2011-06-07 | 2012-12-12 | 新疆大学 | Synthesizing method of flower-cluster-shaped structure composed of CuO/ZnO composite oxide porous nano-grade blades |
| CN103726102A (en) * | 2014-01-20 | 2014-04-16 | 中国科学院理化技术研究所 | Method for preparing super-long one-dimensional mono-crystalline silicon nano/micron structure |
| CN103721698A (en) * | 2014-01-10 | 2014-04-16 | 中国天辰工程有限公司 | Zinc oxide catalyst of ordered layered structure and preparation method thereof |
| CN104828855A (en) * | 2015-05-05 | 2015-08-12 | 上海交通大学 | Ultra-long ZnO whisker with hierarchical structure and preparation method thereof based on hydrothermal ion induction technology |
| CN107673398A (en) * | 2017-10-11 | 2018-02-09 | 北京振兴华龙制冷设备有限责任公司 | A kind of preparation method of Nanometer-sized Rods ZnO and its application for preparing ventilating duct for air-conditioner |
| CN111547760A (en) * | 2020-05-11 | 2020-08-18 | 东北师范大学 | Preparation method and application of oxide substrate in-situ growth silver nanorod |
-
2007
- 2007-09-13 CN CN200710071294A patent/CN100591810C/en not_active Expired - Fee Related
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102817078A (en) * | 2011-06-07 | 2012-12-12 | 新疆大学 | Synthesizing method of flower-cluster-shaped structure composed of CuO/ZnO composite oxide porous nano-grade blades |
| CN102817078B (en) * | 2011-06-07 | 2015-07-15 | 新疆大学 | Synthesizing method of flower-cluster-shaped structure composed of CuO/ZnO composite oxide porous nano-grade blades |
| CN102337581A (en) * | 2011-09-20 | 2012-02-01 | 清华大学 | Method for preparing zinc oxide crystal whisker by using recyclable solvent in low-temperature hydrothermal way |
| CN102337581B (en) * | 2011-09-20 | 2014-05-07 | 清华大学 | Method for preparing zinc oxide crystal whisker by using recyclable solvent in low-temperature hydrothermal way |
| CN103721698A (en) * | 2014-01-10 | 2014-04-16 | 中国天辰工程有限公司 | Zinc oxide catalyst of ordered layered structure and preparation method thereof |
| CN103726102A (en) * | 2014-01-20 | 2014-04-16 | 中国科学院理化技术研究所 | Method for preparing super-long one-dimensional mono-crystalline silicon nano/micron structure |
| CN103726102B (en) * | 2014-01-20 | 2016-09-07 | 中国科学院理化技术研究所 | A kind of method preparing super-long one-dimensional mono-crystalline silicon nano/micron structure |
| CN104828855A (en) * | 2015-05-05 | 2015-08-12 | 上海交通大学 | Ultra-long ZnO whisker with hierarchical structure and preparation method thereof based on hydrothermal ion induction technology |
| CN107673398A (en) * | 2017-10-11 | 2018-02-09 | 北京振兴华龙制冷设备有限责任公司 | A kind of preparation method of Nanometer-sized Rods ZnO and its application for preparing ventilating duct for air-conditioner |
| CN107673398B (en) * | 2017-10-11 | 2019-05-14 | 北京振兴华龙制冷设备有限责任公司 | A kind of preparation method of Nanometer-sized Rods ZnO and its application for being used to prepare ventilating duct for air-conditioner |
| CN111547760A (en) * | 2020-05-11 | 2020-08-18 | 东北师范大学 | Preparation method and application of oxide substrate in-situ growth silver nanorod |
| CN111547760B (en) * | 2020-05-11 | 2022-08-09 | 东北师范大学 | Preparation method and application of oxide substrate in-situ growth silver nanorod |
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| Publication number | Publication date |
|---|---|
| CN100591810C (en) | 2010-02-24 |
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