Method for preparing ZnS quantum dot modified by mercaptoacetic acid

A technology of thioglycolic acid and quantum dots, applied in chemical instruments and methods, luminescent materials, etc., can solve the problems of cumbersome operation process, long time consumption, etc., and achieve the effects of simple preparation process, good dispersibility and low cost

Active Publication Date: 2011-11-16
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, both zinc powder and sulfur powder are flammable and explosive, and there is a certain risk, and the two-step method of first synthesizing and then modifying takes a long time, and the operation process is relatively cumbersome

Method used

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  • Method for preparing ZnS quantum dot modified by mercaptoacetic acid
  • Method for preparing ZnS quantum dot modified by mercaptoacetic acid
  • Method for preparing ZnS quantum dot modified by mercaptoacetic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 2.20g Zn(Ac) 2 2H 2 O (10mmol) was added to 50mL of deionized water to make Zn(Ac) with a concentration of 0.20mol / L 2 2H 2 O aqueous solution, add 4.5 mL of thioglycolic acid with a mass concentration of 90% under magnetic stirring, thioglycolic acid and Zn(Ac) 2 2H 2 The molar ratio of O is 5:1, then add 2.4g Na 2 S·9H 2 O (10mmol), Na 2 S·9H 2 O and Zn(Ac) 2 2H 2 The molar ratio of O is 1:1, adjust the pH=10 with ammonia water with a mass concentration of 25%, put it into a polytetrafluoroethylene high-pressure reactor after stirring evenly, the volume of the mixed solution accounts for 60% of the reactor volume, 130°C Keep warm for 14 hours. After the reaction kettle is naturally cooled, centrifuge and discard the supernatant, wash the precipitate twice with 20mL of absolute ethanol, then wash the precipitate twice with 20mL deionized water, and disperse the precipitate in deionized water to obtain a stable hydrosol; or dissolve the precipitate Vacuum dry...

Embodiment 2

[0025] 1.32g Zn(Ac) 2 2H 2 O (6mmol) was added to 50mL of deionized water to make Zn(Ac) with a concentration of 0.12mol / L 2 2H 2 O aqueous solution, add 4.5 mL of thioglycolic acid solution with a mass concentration of 90% under magnetic stirring, thioglycolic acid and Zn(Ac) 2 2H 2 The molar ratio of O is 9:1, then add 2.16g Na 2 S·9H 2 O (9 mmol), Na 2 S·9H 2 O and Zn(Ac) 2 2H 2 The molar ratio of O is 1.5:1, adjust the pH=9 with ammonia water with a mass concentration of 25%, put it into a polytetrafluoroethylene high-pressure reactor after stirring evenly, the volume of the mixed solution accounts for 60% of the reactor volume, 150°C Keep warm for 10 hours. After the reaction kettle is naturally cooled, centrifuge and discard the supernatant, wash the precipitate twice with 20mL of absolute ethanol, and then wash the precipitate twice with 20mL of deionized water. The precipitate is directly dispersed in deionized water to obtain a stable hydrosol; or The preci...

Embodiment 3

[0027] 3.96g Zn(Ac) 2 2H 2 O (18mmol) was added to 50mL of deionized water to make Zn(Ac) with a concentration of 0.36mol / L 2 2H 2 O aqueous solution, add 4.5 mL of thioglycolic acid solution with a mass concentration of 90% under magnetic stirring, thioglycolic acid and Zn(Ac) 2 2H 2 The molar ratio of O is 3:1, then add 6.48g Na 2 S·9H 2 O (27mmol), Na 2 S·9H 2 O and Zn(Ac) 2 2H 2 The molar ratio of O is 1.5:1, adjust the pH=9 with ammonia water with a mass concentration of 25%, put it into a polytetrafluoroethylene high-pressure reactor after stirring evenly, the volume of the mixed solution accounts for 60% of the reactor volume, 180°C Keep warm for 6 hours. After the reaction kettle is naturally cooled, centrifuge and discard the supernatant, wash the precipitate twice with 20mL of absolute ethanol, then wash the precipitate twice with 20mL of deionized water, and disperse the precipitate in deionized water to obtain a stable hydrosol; or place the precipitate i...

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Abstract

The invention provides a method for preparing a ZnS quantum dot modified by mercaptoacetic acid, belonging to the technical field of ZnS nano material preparation. The ZnS quantum dot modified by mercaptoacetic acid is synthesized in one step by using a hydro-thermal reaction method in an aqueous solution based on mercaptoacetic acid as a modifier. The method has the advantages that the synthesized ZnS quantum dot modified by mercaptoacetic acid has uniform in size, strong fluorescent signals and good dispersibility in water, and can form stable hydrosol; a carboxyl group connected to the surface of the ZnS quantum dot can be connected with a large biological molecule, which is suitable for detection of biological substances; and in addition, compared with other methods for preparing the ZnS quantum dot modified by mercaptoacetic acid, in the method provided by the invention, reaction and modification links are completed in one step, so that preparation process is simple and cost is low.

Description

technical field [0001] The invention belongs to the technical field of preparation of ZnS nanometer materials, and in particular provides a method for preparing ZnS quantum dots modified by thioglycolic acid, that is, synthesizing ZnS quantum dots modified by thioglycolic acid in one step through a hydrothermal reaction method. Background technique [0002] Semiconductor nanoparticles, also known as quantum dots, are nanocrystalline particles with a diameter between 1 and 100 nm composed of II B-VIB or IIIB-VB group elements. The radius of quantum dots is smaller than or close to the exciton Bohr radius, and has the characteristics of surface effect and small size effect, so it has unique optical and electrical properties. ZnS quantum dots are typical IIB-VIB wide-bandgap semiconductor luminescent materials, which have ultra-fast optical nonlinear response and (room temperature) photoluminescence, and are widely used in photoluminescence, electroluminescence, and fluorescent...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/56
Inventor 刘长霞纪圆圆马丽苏海佳谭天伟
Owner BEIJING UNIV OF CHEM TECH
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