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Synthesis method of ZnSe hollow microspheres by alcohol thermal reduction

A technology of micro-spheres and synthesis method, applied in the field of nanomaterials, can solve the problems of harsh equipment and process requirements, and achieve the effects of environmental friendliness, mild reduction performance and high yield.

Inactive Publication Date: 2013-06-19
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, under the system of strong alkalinity and hydrazine hydrate, there are great potential safety hazards in the process, and the requirements for equipment and processes are more stringent

Method used

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  • Synthesis method of ZnSe hollow microspheres by alcohol thermal reduction
  • Synthesis method of ZnSe hollow microspheres by alcohol thermal reduction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Prepare distilled water and ethylene glycol with a volume ratio of 1:3 to form a mixed solution, weigh 2.5mmol analytically pure sodium selenite, 2.5mmol zinc acetate, 5mmol EDTA and 2g sodium hydroxide respectively, and dissolve them in the above mixed solution (pH value 10); after stirring, the resulting clear solution was transferred to a polytetrafluoroethylene-lined stainless steel autoclave, and distilled water was added to reach 80% of the reactor volume. After fully stirring, tighten the autoclave and put it in a constant temperature oven at 180°C for 12 hours. After the reaction was over, the reactor was taken out and allowed to cool naturally. Subsequently, the precipitate in the kettle was filtered, washed three times with distilled water, and then washed twice with absolute ethanol. Finally, the sample was dried in a vacuum oven at 60° C. for 4 hours to obtain ZnSe hollow microspheres. figure 1 For the X-ray diffraction spectrum of ZnSe hollow microspheres...

Embodiment 2

[0023] Prepare a mixed solution of distilled water and ethylene glycol with a volume ratio of 1:4, add a stoichiometric ratio of zinc salt and sodium selenite, control the concentration of NaOH to 0.8 mol / L (pH value is 12), and the molar ratio of EDTA and Zn The ratio is 1:1. After forming a colorless and transparent solution, transfer it to a stainless steel reactor with a polytetrafluoroethylene liner, add distilled water to 70% of the volume of the reactor, seal it, tighten it, and put it in a constant temperature oven at 140°C for 24 hours. After the reaction was over, the reactor was taken out and allowed to cool naturally. Subsequently, the precipitate in the kettle was filtered, washed three times with distilled water, and then washed twice with absolute ethanol. Finally, the sample was dried in a vacuum oven at 50° C. for 6 hours to obtain ZnSe hollow microspheres.

Embodiment 3

[0025] Prepare a mixed solution of distilled water and ethylene glycol with a volume ratio of 1:3, add a stoichiometric ratio of zinc salt and sodium selenite, control the concentration of NaOH to 0.9 mol / L (pH value is 12.4), and the molar ratio of EDTA and Zn The ratio is 3:1. After forming a colorless and transparent solution, transfer it to a stainless steel reactor with a polytetrafluoroethylene liner, add distilled water to 80% of the volume of the reactor, seal it, tighten it, and put it in a constant temperature oven at 200°C for 14 hours. After the reaction was over, the reactor was taken out and allowed to cool naturally. Subsequently, the precipitate in the kettle was filtered, washed three times with distilled water, and then washed twice with absolute ethanol. Finally, the sample was dried in a vacuum oven at 60° C. for 4 hours to obtain ZnSe hollow microspheres.

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Abstract

The invention discloses a method for preparing hollow ZnSe microspheres by an alcohol thermal reduction route. By using sodium selenite as a selenium source, ethylene glycol (EG) as a reducer and ethylene diamine tetraacetic acid (EDTA) as a complexant, one-step alcohol thermal reduction reaction is carried out in an EG-water mixed solution to prepare the hollow ZnSe microspheres. In the reaction process, no surfactant or any other template is needed, and the 140-220 DEG C hydrothermal reaction is carried out for 6-24 hours to obtain the zinc selenide hollow microspheres of which the diameter is 1-3 mu m and the wall thickness is 100-200 nm. The coordination of the EDTA with metallic ions in an alkaline environment has an important action on the formation of the hollow microspheres. The method has the characteristics of simple technical route and the like, is convenient to operate and is environment-friendly.

Description

Technical field [0001] The present invention involves the preparation method of selenium -based zinc hormone micron balls, which belongs to the field of nanomaterials. Background technique [0002] The II-Vi tribe (MS, MSE, MTE, M represents metal) semiconductor nanomaterials because of special optical non-linear and fluorescent characteristics such as important physical and chemical properties, in many fields (solar batteries, solid light, laser, infrared detectors, CPD effects, etc.) have huge application prospects.As a wide-band II-Vi tribe direct transition semiconductor material, ZNSE has a face-hearted cubic structure, and its body phase material forbidden bandwidth is 2.67EV at room temperature.The preferred materials for diodes, blue laser and other photoelectric materials.Its chemical properties are stable and have strong moisture resistance.Because the Na / micron structure ZNse has fluorescent effects and photoelectric effects, it presents excellent performance in the fi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B19/04B82Y30/00
Inventor 王雄蓝燕朱娟娟林颖
Owner NANJING UNIV OF SCI & TECH
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