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Preparation method of water-soluble composite InP/ZnS luminescent quantum dots for fingerprint appearance

A water-soluble composite and quantum dot technology, applied in chemical instruments and methods, diagnostic records/measurements, applications, etc., to achieve the effects of mild conditions, low synthesis temperature, and simple operation

Inactive Publication Date: 2011-04-27
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no report on the fingerprint display of III-V composite InP / ZnS quantum dots with good fluorescence stability and stronger intensity.

Method used

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  • Preparation method of water-soluble composite InP/ZnS luminescent quantum dots for fingerprint appearance
  • Preparation method of water-soluble composite InP/ZnS luminescent quantum dots for fingerprint appearance
  • Preparation method of water-soluble composite InP/ZnS luminescent quantum dots for fingerprint appearance

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] (1). Synthesis of water-soluble InP / ZnS: the synthesis temperature of InP is 150°C, TGA / Zn 2+ =2.4, the phase inversion temperature is 40°C.

[0020] Synthesis of InP in the organic phase: In an inert gas glove box, 0.4gInCl 3 , 0.45gP(N(CH 3 ) 2 ) 3 , 5g of surfactant dodecylamine (DDA) etc. are dissolved in a 50ml reaction kettle with 5ml of toluene, after sealing, take it out from the glove box, place it in a 70°C oven and heat it for 1h to dissolve the raw materials, and then heat to The reaction was carried out at 150°C and kept for 24 hours. After the reaction was completed, it was cooled to room temperature, and the upper layer solution was removed and washed with methanol several times. The product was dried in a vacuum oven at 60°C for 12 hours to obtain InP solid powder.

[0021] (2).InP quantum dots are transferred to the water phase: take 0.58g Zn(Ac) 2 2H 2 O and 0.59 g of thioglycolic acid (TGA) were added to 20 ml of deionized water, that is, Zn 2+...

Embodiment 2

[0025] Change synthesis temperature, change TGA / Zn 2+ Proportioning, the specific steps are as follows:

[0026] (1). Synthesis of water-soluble InP / ZnS: the synthesis temperature of InP is 165°C, TGA / Zn 2+ =1.9, the phase inversion temperature is 40°C.

[0027] Synthesis of InP in the organic phase: In an inert gas glove box, 0.4gInCl 3 , 0.45gP(N(CH 3 ) 2 ) 3 , 5g of surfactant dodecylamine (DDA) etc. are dissolved in a 50ml reaction kettle with 5ml of toluene, after sealing, take it out from the glove box, place it in a 70°C oven and heat it for 1h to dissolve the raw materials, and then heat to The reaction was carried out at 165°C and kept for 24 hours. After the reaction was completed, it was cooled to room temperature, the upper layer solution was opened and washed with methanol several times, and the product was dried in a vacuum oven at 60°C for 12 hours to obtain InP solid powder.

[0028] (2). Take 0.58g Zn(Ac) 2 2H 2 O and 0.47gTGA were added to 20ml deioni...

Embodiment 3

[0032] Change synthesis temperature, change phase inversion temperature, concrete steps are as follows:

[0033] (1). Synthesis of water-soluble InP / ZnS: the synthesis temperature of InP is 180°C, TGA / Zn 2+ =2.4, the phase inversion temperature is 50°C.

[0034] Change the reaction synthesis temperature to 180° C., and the operation of synthesizing InP in other specific organic phases is the same as that in Example 1 (1), to obtain InP solid powder.

[0035] (2). Take 0.58g Zn(Ac) 2 2H 2 O and 0.59g TGA were added to 20ml deionized water, that is, Zn 2+ The molar concentration is 0.13mol / L, and the molar ratio is TGA / Zn 2+ =2.4 solution. Take 0.006g of the InP powder prepared by (1) in 10ml of the mixed solution of hexane and butanol (the volume ratio of hexane and butanol is 2:1) and ultrasonically disperse for 2min, add 10ml of the ZT solution prepared above, at 50℃ Stirring was continued at temperature for 1 h. Concrete operation is with embodiment 1 (2).

[0036] (...

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Abstract

The invention discloses a preparation method of water-soluble luminescent quantum dots for fingerprint appearance, belonging to the field of biomarkers. The chemical composition of the water-soluble luminescent quantum dots is InP / ZnS. The preparation method comprises the following steps: under the inert atmosphere, weighing and adding an indium source, a phosphorus source, a surface active agent and a methylbenzene solvent of proper amount at certain stoichiometric ratio into a reactor, wherein the heating temperature is 150-200 DEG C, reacting for 18-36 hours to obtain gray black solution; using methyl alcohol to clean for a plurality of times; putting products in a vacuum drying box at certain temperature, drying for 8-12 hours to obtain solid powder of InP; dissloving a certain amount of solid powder into an organic solvent, adding alkaline solution (pH is 7.5-10.5) containing mercaptoacetic acid and zinc ions, stirring for a period of time at the temperature of 40-60 DEG C; removing an upper organic layer and obtaining lower-layer water-phase solution; and taking a certain amount of solution, adding the alkaline solution containing the mercaptoacetic acid and the zinc ions, stirring for 0.5-1.5 hours under the irradiation of ultraviolet light and obtaining water-soluble InP / ZnS end products.

Description

technical field [0001] The invention relates to a preparation method of water-soluble fluorescent quantum dots and its application in fingerprint display, and belongs to the fields of nanometer material preparation technology and biological analysis and detection technology. technical background [0002] As a fast-growing cross-cutting frontier science, nanomaterials science has attracted extensive attention from researchers in various disciplines in recent years. Among them, semiconductor quantum dots, as a typical and very important nanomaterial, have received more and more attention in the application of solar cells, optoelectronic devices, light-emitting diodes, and biological cell imaging. At present, more II-VI semiconductor quantum dots, such as CdSe, CdS, CdTe, etc., contain heavy metal ions Cd 2+ , limiting its application in biomarkers. Compared with this, the toxicity of InP quantum dots of the III-V group is relatively much less, and it has better biocompatibil...

Claims

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Application Information

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IPC IPC(8): C09K11/70A61B5/117A61B5/1172
Inventor 刘建军熊海左胜利于迎春
Owner BEIJING UNIV OF CHEM TECH
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