CN101920942B - Method for controlling synthesis of zinc selenide multi-morphological nano material - Google Patents
Method for controlling synthesis of zinc selenide multi-morphological nano material Download PDFInfo
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- CN101920942B CN101920942B CN2010102871691A CN201010287169A CN101920942B CN 101920942 B CN101920942 B CN 101920942B CN 2010102871691 A CN2010102871691 A CN 2010102871691A CN 201010287169 A CN201010287169 A CN 201010287169A CN 101920942 B CN101920942 B CN 101920942B
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Abstract
The invention relates to a method for controlling the synthesis of a zinc selenide multi-morphological nano material, which comprises the following steps: taking out SeO2 powder or Se powder and NaOH, adding H2O to the SeO2 powder or the Se powder and the NaOH, carrying out magnetic stirring or ultrasonic oscillation to dissolve the SeO2 powder to generate a solution, adding one of hydrazine hydrate, glycol or ethylene diamine, stirring, transferring into a reaction kettle, adding zinc salt and surfactant polyvinyl pyrrolidone and continuously stirring for a period of time, then adding H2O until the reactant volume reaches 80% of the volume of the reaction kettle, reacting at a certain temperature for 12h, cooling to room temperature, washing with ethanol and distilled water, and drying in vacuum at 50 DEG C for 4h, wherein the self-assembly of the multi-morphological nano material into microspheres is controlled by whether the surfactant polyvinyl pyrrolidone is used or not. The method has the advantages of simple operation and controllability, and provides support for the preparation and the application research of the zinc selenide material. Besides, the obtained material has favorable application prospects in photocatalysis.
Description
Technical field
The invention belongs to the preparation field of zinc selenide nano material, particularly a kind of method of controlling synthesis of zinc selenide multi-morphological nano material.
Background technology
Zinc selenide is important II-VI family semiconductor material, and its energy gap is 2.68eV under the room temperature, is direct transition luminescence, and emission wavelength is positioned at blue light range, can be used for making blue light diode laser apparatus, light-detecting device, device for non-linear optical.The zinc selenide nano material of different-shape demonstrates some special physical propertiess.Therefore the zinc selenide nano material of controlled formation different-shape should be in different fields, and is significant.In addition, zinc selenide nano material may command gets microballoon, has opened up the Application Areas of zinc selenide material again.
The relevant report of zinc selenide microballoon (comprising hollow ball) has, and for example: Q.Peng utilizes hydrothermal method, obtains zinc selenide hollow ball (Angew.Chem.Int.Ed.2003,42,3027) through nanocrystalline gathering.H.Z.Zhong utilizes simple hot injection to prepare the zinc selenide microballoon, through nanoparticle in-situ polymerization (Langmuir.2007,23,9008).B.J.Xi utilizes the template self-assembly method to obtain nanometer rod self-assembly microspheres (Chem.Eur.J.2008,14,9786).These products that obtain possibly bring novel light, electricity, magnetic property, open up new Application Areas
Summary of the invention
Technical problem to be solved by this invention provides a kind of method of controlling synthesis of zinc selenide multi-morphological nano material; This method is simple to operate; Controlled, for the preparation and the applied research of zinc selenide material provides support, the material that obtains has a good application prospect aspect photochemical catalysis.
A kind of method of controlling synthesis of zinc selenide multi-morphological nano material of the present invention comprises:
Get the SeO of 2mmol
2Powder or Se powder and 0.1molNaOH add 15mLH
2O magnetic agitation or sonic oscillation, SeO
2After the dissolving of powder or Se powder generated solution, wherein a kind of of Hydrazine Hydrate 80, terepthaloyl moietie or the quadrol that adds 2mL stirred, and is transferred to reaction kettle, add 2mmol zinc salt and 0-0.2g tensio-active agent Vinylpyrrolidone polymer after, continue stirring 15min after, add H
2O makes the reactant volume reach 80% of reaction kettle volume, behind the 140-180 ℃ of following reaction 12h, is cooled to room temperature, and ethanol and distilled water wash obtain multi-morphological nano material in 50 ℃ of vacuum-drying 4h.
Said zinc salt is zinc nitrate, zinc chloride, zinc acetate or zinc sulfate.
Said Vinylpyrrolidone polymer is 0 o'clock, and the product that then obtains is the zinc selenide microballoon.
Said Vinylpyrrolidone polymer is not 0 o'clock, and the product that then obtains is a multi-morphological nano material.
The Vinylpyrrolidone polymer preferable range is 0～0.2g.
Said multiform looks are respectively to add the zinc selenide that Hydrazine Hydrate 80 obtains nanometer polyhedral, add the zinc selenide that terepthaloyl moietie obtains nano bar-shape, add the zinc selenide that quadrol obtains the nanometer thin sheet.
The present invention uses the hydrothermal method synthesis of zinc selenide multi-morphological nano material, whether reaches the difference of kind then through the adding of tensio-active agent, obtains the zinc selenide microballoon of self-assembly; Simultaneously, obtain different big or small zinc selenide nano-multicrystal bodies, the microballoon different through temperature controlling with surfaceness.
Beneficial effect
This method is simple to operate, and is controlled, and for the preparation and the applied research of zinc selenide material provides support, the material that obtains has a good application prospect aspect photochemical catalysis.
Description of drawings
Fig. 1 is the nanocrystalline sign picture of zinc selenide of embodiment 1 preparation, (a) the nanocrystalline scanning electron microscope diagram sheet of zinc selenide; (b) the nanocrystalline transmission electron micrograph of zinc selenide; (c) show one nanocrystalline high power transmission electron micrograph; The x-ray diffraction pattern of the zinc selenide nano material that (d) obtains.
Fig. 2 is the sign picture of the zinc selenide microballoon of embodiment 2 preparations, (a) the low power scanning electron microscope diagram sheet of zinc selenide microballoon; (b) single zinc selenide microsphere surface high power scanning electron microscope diagram sheet.
Fig. 3 is the sign picture of the zinc selenide microballoon of embodiment 3 preparations, (a) the low power scanning electron microscope diagram sheet of zinc selenide microballoon; (b) single zinc selenide microsphere surface high power scanning electron microscope diagram sheet.
Fig. 4 is the sign picture of the zinc selenide microballoon of embodiment 4,5 preparations, (a) the scanning electron microscope diagram sheet of the nanometer stub self-assembly zinc selenide microballoon of embodiment 4 preparations; (b) the scanning electron microscope diagram sheet of the nanometer sheet self-assembly zinc selenide microballoon of embodiment 5 preparations.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in the restriction scope of the present invention.Should be understood that in addition those skilled in the art can do various changes or modification to the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
Get the SeO of 2mmol
2Powder and 0.1molNaOH add 15mLH
2O magnetic agitation (or sonic oscillation), SeO
2After the powder dissolving generates solution, add the Hydrazine Hydrate 80 of 2mL, stir, be transferred to reaction kettle, add 2mmol Zn (NO
3)
2Behind 0.2g tensio-active agent Vinylpyrrolidone polymer, after continuing to stir 15min, add H
2O makes the reactant volume reach 80%, 180 ℃ of reaction kettle volume, behind the 12h, is cooled to room temperature, behind ethanol and the distilled water wash 5 times, and 50 ℃ of vacuum-dryings, 4h can obtain the zinc selenide nanometer polyhedral.
Embodiment 2
Get the SeO of 2mmol
2Powder and 0.1molNaOH add 15mLH
2O magnetic agitation (or sonic oscillation), SeO
2After the powder dissolving generates solution, add the Hydrazine Hydrate 80 of 2mL, stir, be transferred to reaction kettle, add 2mmol Zn (NO
3)
2After, after continuing to stir 15min, add H
2O makes the reactant volume reach 80%, 180 ℃ of reaction kettle volume, behind the 12h, is cooled to room temperature, behind ethanol and the distilled water wash 5 times, and 50 ℃ of vacuum-dryings, 4h can obtain nanometer polyhedral self-assembly zinc selenide microballoon.Find out that by Fig. 2 microspherulite diameter is even.
Embodiment 3
Get the SeO of 2mmol
2Powder and 0.1molNaOH add 15mLH
2O magnetic agitation (or sonic oscillation), SeO
2After the powder dissolving generates solution, add the Hydrazine Hydrate 80 of 2mL, stir, be transferred to reaction kettle, add 2mmol Zn (NO
3)
2After, after continuing to stir 15min, add H
2O makes the reactant volume reach 80%, 140 ℃ of reaction kettle volume, behind the 12h, is cooled to room temperature, behind ethanol and the distilled water wash 5 times, and 50 ℃ of vacuum-dryings, 4h can obtain nanometer polyhedral self-assembly zinc selenide microballoon.Find out that by Fig. 3 microspherulite diameter is even, to compare surfaceness low, smooth with the microballoon that embodiment 2 makes, and the nanocrystalline size on surface is smaller.
Embodiment 4
Get the SeO of 2mmol
2Powder and 0.1molNaOH add 15mLH
2O magnetic agitation (or sonic oscillation), SeO
2After the powder dissolving generates solution, add the terepthaloyl moietie of 2mL, stir, be transferred to reaction kettle, add 2mmol Zn (NO
3)
2After, after continuing to stir 15min, add H
2O makes the reactant volume reach 80%, 180 ℃ of reaction kettle volume, behind the 12h, is cooled to room temperature, behind ethanol and the distilled water wash 5 times, and 50 ℃ of vacuum-dryings, 4h can obtain nanometer stub self-assembly zinc selenide microballoon.
Embodiment 5
Get the SeO of 2mmol
2Powder and 0.1molNaOH add 15mLH
2O magnetic agitation (or sonic oscillation), SeO
2After the powder dissolving generates solution, add the quadrol of 2mL, stir, be transferred to reaction kettle, add 2mmol Zn (NO
3)
2After, after continuing to stir 15min, add H
2O makes the reactant volume reach 80%, 180 ℃ of reaction kettle volume, behind the 12h, is cooled to room temperature, behind ethanol and the distilled water wash 5 times, and 50 ℃ of vacuum-dryings, 4h can obtain nanometer sheet self-assembly zinc selenide microballoon.
Claims (2)
1. method of controlling synthesis of zinc selenide multi-morphological nano material comprises:
Get the SeO of 2mmol
2Powder or Se powder and 0.1mol NaOH add 15mL H
2O magnetic agitation or sonic oscillation, SeO
2After the dissolving of powder or Se powder generated solution, wherein a kind of of Hydrazine Hydrate 80, terepthaloyl moietie or the quadrol that adds 2mL stirred, and is transferred to reaction kettle, add 2mmol zinc salt and 0.2g tensio-active agent Vinylpyrrolidone polymer after, continue stirring 15min after, add H
2O makes the reactant volume reach 80% of reaction kettle volume, behind the 140-180 ℃ of following reaction 12h, is cooled to room temperature, and ethanol and distilled water wash obtain multi-morphological nano material in 50 ℃ of vacuum-drying 4h; Wherein, the multiform looks are respectively to add the zinc selenide that Hydrazine Hydrate 80 obtains nanometer polyhedral, add the zinc selenide that terepthaloyl moietie obtains nano bar-shape, add the zinc selenide that quadrol obtains the nanometer thin sheet.
2. a kind of method of controlling synthesis of zinc selenide multi-morphological nano material according to claim 1 is characterized in that: said zinc salt is zinc nitrate, zinc chloride, zinc acetate or zinc sulfate.
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Families Citing this family (16)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102586950B (en) * | 2012-02-24 | 2013-10-23 | 长春理工大学 | Method for preparing zinc selenide (ZnSe) nanofiber |
| CN102586949B (en) * | 2012-02-24 | 2013-10-23 | 长春理工大学 | Method for preparing zinc selenide nanobelt |
| CN102602898B (en) * | 2012-02-24 | 2013-10-23 | 长春理工大学 | Method for preparing monodisperse zinc selenide particles |
| CN102659084A (en) * | 2012-05-14 | 2012-09-12 | 山东建筑大学 | Preparation method of zinc selenide nanometer powder |
| CN103159189A (en) * | 2013-04-03 | 2013-06-19 | 南京理工大学 | Synthesis method of ZnSe hollow microspheres by alcohol thermal reduction |
| CN105016314B (en) * | 2015-02-05 | 2017-02-22 | 天津大学 | Preparation method for zinc selenide nano hollow spheres |
| CN105923612A (en) * | 2016-04-20 | 2016-09-07 | 南方科技大学 | Metal-chalcogenide semiconductor material, preparation method and application thereof |
| CN106045517A (en) * | 2016-06-02 | 2016-10-26 | 夏晨曦 | Zinc selenide transparent nano-ceramic and preparation method thereof |
| CN108439354A (en) * | 2018-03-23 | 2018-08-24 | 桂林电子科技大学 | A kind of preparation method of metal selenide nano-powder |
| CN109179340B (en) * | 2018-09-18 | 2021-01-05 | 西安交通大学 | Lead-based chalcogenide alloy particles with nano structure and preparation method thereof |
| CN109052340B (en) * | 2018-10-10 | 2020-02-21 | 陕西科技大学 | Preparation method of selenium/vanadium selenide composite phase material |
| CN110255508B (en) * | 2019-06-26 | 2023-06-30 | 南京睿扬光电技术有限公司 | High-performance zinc selenide mixed film material and preparation process thereof |
| CN110562935B (en) * | 2019-09-20 | 2022-11-08 | 安徽大学 | Strip-shaped frame-shaped ZnSe nano material, preparation method thereof and application thereof in colorimetric detection of heavy metal ions |
| CN111604064A (en) * | 2020-05-12 | 2020-09-01 | 河南大学 | Pollution-free hydrothermal synthesis method of zinc selenide microspheres and synthesis method of composite material thereof |
| CN113130865B (en) * | 2021-03-31 | 2022-08-12 | 中南大学 | Bimetallic selenide carbon microsphere composite material and preparation method and application thereof |
| CN116023813B (en) * | 2022-12-14 | 2023-10-31 | 江苏视科新材料股份有限公司 | Preparation method of high-refractive-index blue-light-resistant modified epoxy acrylate material and optical filter |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101214932A (en) * | 2008-01-08 | 2008-07-09 | 上海大学 | Method for preparing nanometer tin selenide |
-
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101214932A (en) * | 2008-01-08 | 2008-07-09 | 上海大学 | Method for preparing nanometer tin selenide |
Non-Patent Citations (3)
| Title |
|---|
| 任晓光.水热/溶剂热法合成硒化锌纳米半导体材料及其性能研究.《中国优秀硕士学位论文全文数据库 工程科技I辑》.2008,(第7期),35-55. * |
| 赵秀琴等.硒化锌晶体的水热控制生长.《化学世界》.2008,(第10期),584-586. * |
| 陈渊等.烷烃溶剂热法合成单分散硒化锌准纳米球.《无机化学学报》.2008,第24卷(第7期),1177-1181. * |
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