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Method for preparing doping type hexagonal system nano ZnS at low temperature

A technology of hexagonal crystal system and doping type, which is applied in the field of preparation of hexagonal crystal β-ZnS, can solve the problems of high temperature required for the reaction, incomplete hexagonal ZnS crystal form, etc., and achieve regular product shape and size Uniform, easy-to-handle results

Inactive Publication Date: 2011-06-01
UNIV OF SCI & TECH BEIJING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the crystal form of the hexagonal ZnS obtained by this method is not very complete, and the temperature required for the reaction is still relatively high. These defects are exactly what the present invention will solve

Method used

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  • Method for preparing doping type hexagonal system nano ZnS at low temperature
  • Method for preparing doping type hexagonal system nano ZnS at low temperature
  • Method for preparing doping type hexagonal system nano ZnS at low temperature

Examples

Experimental program
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Effect test

Embodiment 1

[0025] First, make 0.5g of zinc acetate into a 3mL aqueous solution and add it to a 50mL three-neck round-bottomed flask, stir continuously, then add the copper acetate used for doping into the prepared zinc acetate aqueous solution [n(Zn 2+ ): n (Cu 2+ ) = 50:1], followed by adding 21mL of DMF, and then adding 0.6mL of surfactant thioglycolic acid [n (Zn 2+ ): n (thioglycolic acid) = 1:3.8], then adjust the pH value of the mixed solution with ammonia water, adjust the pH to about 8.5, and finally add 3mL thiourea (0.1734g) DMF solution [n (thiourea): n (Zn 2+ ) = 1:1]. The above-mentioned process of adding the reaction raw materials has been kept in a stirring state at room temperature. However, the course of the reaction was refluxed at 90°C for 14 hours after all material had been added. After the reaction is completed, add acetone twice the volume of the solution to obtain a precipitate, centrifuge to separate the obtained precipitate, and wash the precipitate four tim...

Embodiment 2

[0027] First, make 3mL aqueous solution of 0.5g zinc acetate into a 50mL three-neck round-bottomed flask, stir constantly, then add manganese acetate used for doping into the prepared zinc acetate aqueous solution [n(Zn 2+ ):n(Mn 2+ ) = 100:1], followed by adding 21mL of DMF, and then adding 0.6mL of surfactant thioglycolic acid [n (Zn 2+ ): n (thioglycolic acid) = 1:3.8], then adjust the pH value of the mixed solution with ammonia water, adjust the pH to about 8.5, and finally add 3mL thiourea (0.1734g) DMF solution [n (thiourea): n (Zn 2+ ) = 1:1]. The above-mentioned process of adding the reaction raw materials has been kept in a stirring state at room temperature. However, the course of the reaction was refluxed at 100°C for 5 hours after all material had been added. After the reaction is completed, add acetone twice the volume of the solution to obtain a precipitate, centrifuge to separate the obtained precipitate, and wash the precipitate four times with absolute eth...

Embodiment 3

[0029] First, make 3mL aqueous solution of 0.5g zinc acetate into a 50mL three-necked round-bottomed flask, stir continuously, then add terbium chloride used for doping into the prepared aqueous zinc acetate solution [n(Zn 2+ ): n (Tb 3+) = 150:1], followed by adding 21mL of DMF, and then adding 0.6mL of surfactant thioglycolic acid [n (Zn 2+ ): n (thioglycolic acid) = 1:3.8], then adjust the pH value of the mixed solution with ammonia water, adjust the pH to about 8.5, and finally add 3mL thiourea (0.1734g) DMF solution [n (thiourea): n (Zn 2+ ) = 1:1]. The above-mentioned process of adding the reaction raw materials has been kept in a stirring state at room temperature. However, the course of the reaction was refluxed at 95°C for 14 hours after all material had been added. After the reaction is completed, add acetone twice the volume of the solution to obtain a precipitate, centrifuge to separate the obtained precipitate, and wash the precipitate four times with absolute...

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Abstract

The invention provides a method for preparing doping type hexagonal system nano ZnS at a low temperature, belonging to the field of semiconductor materials. The method is characterized in that transition metal and rare earth-doped hexagonal system nano ZnS is synthesized by a reversed micelle method at the temperature of less than 100 DEG C, wherein an oil phase is an organic solvent, a water phase is a zinc salt aqueous solution, N,N-dimethylformamide is used as the solvent, a zinc salt is used as an zinc ion source, thiourea serves as a sulphur ion source, and mercaptoacetic acid serves as a surface active agent; and the heating temperature is controlled by an oil bath, and the whole reaction is carried out in the air, and any air isolating measure is not needed. The method is simple tooperate, the required reactions are carried out in a liquid phase, subsequent high-temperature annealing treatment is not needed, and reaction conditions are mild; and the method is energy-saving andenvironment-friendly, and an economically feasible way is provided for producing the hexagonal system nano ZnS with high stability and good water solubility on large scale.

Description

technical field [0001] The invention belongs to the field of semiconductor materials, and relates to a preparation method for synthesizing hexagonal β-ZnS doped with transition metal and rare earth ions by a reverse micelle method at a temperature lower than 100°C. Background technique [0002] ZnS is a wide bandgap (3.7eV) II-VI electron-excess intrinsic semiconductor material, which has good fluorescence effect and electroluminescence function, which makes it a hot spot in research and development at home and abroad (J. Hwang et al., Cur. Appl. Phys., 2005, 5:31–34). [0003] Doping metal ions or rare earth ions into semiconductor nanoparticles can change the energy level structure of semiconductors to obtain optical properties different from those of non-doped nanoparticles. Andrea Klausch et al obtained ZnS:Cu nanoparticles with good blue-green fluorescence in the range of 400-500nm by colloidal precipitation method (A. Klausch et al., J. Lumin., 2010, 130: 692–697). N...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G9/08B82Y40/00
Inventor 王丽萍黄顺刚袁欣孟凡国孙玉洁罗皓
Owner UNIV OF SCI & TECH BEIJING
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