CN101920942A - 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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- CN101920942A CN101920942A CN 201010287169 CN201010287169A CN101920942A CN 101920942 A CN101920942 A CN 101920942A CN 201010287169 CN201010287169 CN 201010287169 CN 201010287169 A CN201010287169 A CN 201010287169A CN 101920942 A CN101920942 A CN 101920942A
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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 presents 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) by nanocrystalline gathering.H.Z.Zhong utilizes simple hot injection to prepare the zinc selenide microballoon, by 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 may 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, ethylene glycol or the quadrol that adds 2mL stirred, and is transferred to reactor, add 2mmol zinc salt and 0-0.2g tensio-active agent polyvinylpyrrolidone after, after continuing to stir 15min, add H
2O makes the reactant volume reach 80% of reactor 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.
Described zinc salt is zinc nitrate, zinc chloride, zinc acetate or zinc sulfate.
Described polyvinylpyrrolidone is 0 o'clock, and the product that then obtains is the zinc selenide microballoon.
Described polyvinylpyrrolidone is not 0 o'clock, and the product that then obtains is a multi-morphological nano material.
The polyvinylpyrrolidone preferable range is 0～0.2g.
Described multiform looks are respectively to add the zinc selenide that hydrazine hydrate obtains nanometer polyhedral, add the zinc selenide that ethylene glycol 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 by 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 by 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 and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications 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 of 2mL, stir, be transferred to reactor, add 2mmol Zn (NO
3)
2Behind 0.2g tensio-active agent polyvinylpyrrolidone, after continuing to stir 15min, add H
2O makes the reactant volume reach 80%, 180 ℃ of reactor 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 of 2mL, stir, be transferred to reactor, add 2mmol Zn (NO
3)
2After, after continuing to stir 15min, add H
2O makes the reactant volume reach 80%, 180 ℃ of reactor 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 of 2mL, stir, be transferred to reactor, add 2mmol Zn (NO
3)
2After, after continuing to stir 15min, add H
2O makes the reactant volume reach 80%, 140 ℃ of reactor 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 ethylene glycol of 2mL, stir, be transferred to reactor, add 2mmol Zn (NO
3)
2After, after continuing to stir 15min, add H
2O makes the reactant volume reach 80%, 180 ℃ of reactor 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 reactor, add 2mmol Zn (NO
3)
2After, after continuing to stir 15min, add H
2O makes the reactant volume reach 80%, 180 ℃ of reactor 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 (5)
1. method of controlling synthesis of zinc selenide multi-morphological nano material 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, ethylene glycol or the quadrol that adds 2mL stirred, and is transferred to reactor, add 2mmol zinc salt and 0-0.2g tensio-active agent polyvinylpyrrolidone after, after continuing to stir 15min, add H
2O makes the reactant volume reach 80% of reactor 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.
2. according to claim 1ly a kind ofly control synthesis of zinc selenide multi-morphological nano material and be self-assembled into method into microballoon, it is characterized in that: described zinc salt is zinc nitrate, zinc chloride, zinc acetate or zinc sulfate.
3. according to claim 1ly a kind ofly control synthesis of zinc selenide multi-morphological nano material and be self-assembled into method into microballoon, it is characterized in that: described polyvinylpyrrolidone is 0 o'clock, and the product that then obtains is the zinc selenide microballoon.
4. according to claim 1ly a kind ofly control synthesis of zinc selenide multi-morphological nano material and be self-assembled into method into microballoon, it is characterized in that: when described polyvinylpyrrolidone was 0.2g, the product that then obtains was a multi-morphological nano material.
5. according to claim 1ly a kind ofly control synthesis of zinc selenide multi-morphological nano material and be self-assembled into method into microballoon, it is characterized in that: described multiform looks are respectively to add the zinc selenide that hydrazine hydrate obtains nanometer polyhedral, adding ethylene glycol obtains the zinc selenide of nano bar-shape, adds the zinc selenide that quadrol obtains the nanometer thin sheet.
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102586950A (en) * | 2012-02-24 | 2012-07-18 | 长春理工大学 | Method for preparing zinc selenide (ZnSe) nanofiber |
| CN102586949A (en) * | 2012-02-24 | 2012-07-18 | 长春理工大学 | Method for preparing zinc selenide nanobelt |
| CN102602898A (en) * | 2012-02-24 | 2012-07-25 | 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 |
| CN105016314A (en) * | 2015-02-05 | 2015-11-04 | 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 |
| CN109052340A (en) * | 2018-10-10 | 2018-12-21 | 陕西科技大学 | A kind of preparation method of selenium/selenizing vanadium compound phase material |
| CN109179340A (en) * | 2018-09-18 | 2019-01-11 | 西安交通大学 | Lead base chalcogenide alloy particle with nanostructure and preparation method thereof |
| CN110255508A (en) * | 2019-06-26 | 2019-09-20 | 南京睿扬光电技术有限公司 | A kind of high performance zinc selenide mixing coating materials and its preparation process |
| CN110562935A (en) * | 2019-09-20 | 2019-12-13 | 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 |
| CN113130865A (en) * | 2021-03-31 | 2021-07-16 | 中南大学 | Bimetallic selenide carbon microsphere composite material and preparation method and application thereof |
| CN116023813A (en) * | 2022-12-14 | 2023-04-28 | 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 |
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| CN102586950A (en) * | 2012-02-24 | 2012-07-18 | 长春理工大学 | Method for preparing zinc selenide (ZnSe) nanofiber |
| CN102586949A (en) * | 2012-02-24 | 2012-07-18 | 长春理工大学 | Method for preparing zinc selenide nanobelt |
| CN102602898A (en) * | 2012-02-24 | 2012-07-25 | 长春理工大学 | Method for preparing monodisperse zinc selenide particles |
| CN102602898B (en) * | 2012-02-24 | 2013-10-23 | 长春理工大学 | Method for preparing monodisperse zinc selenide particles |
| 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 |
| 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 |
| CN105016314A (en) * | 2015-02-05 | 2015-11-04 | 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 |
| CN109179340A (en) * | 2018-09-18 | 2019-01-11 | 西安交通大学 | Lead base chalcogenide alloy particle with nanostructure and preparation method thereof |
| 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 |
| CN109052340A (en) * | 2018-10-10 | 2018-12-21 | 陕西科技大学 | A kind of preparation method of selenium/selenizing vanadium compound phase material |
| CN110255508A (en) * | 2019-06-26 | 2019-09-20 | 南京睿扬光电技术有限公司 | A kind of high performance zinc selenide mixing coating materials and its preparation process |
| 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 |
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| 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 |
| CN113130865A (en) * | 2021-03-31 | 2021-07-16 | 中南大学 | Bimetallic selenide carbon microsphere composite material and preparation method and application thereof |
| CN116023813A (en) * | 2022-12-14 | 2023-04-28 | 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 |
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