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CuInS2 quantum dots with water-soluble zinc blende structure, CuInS2/ZnS core shell quantum dots with water-soluble zinc blende structure and preparation method thereof

A core-shell structure and quantum dot technology, applied in the field of compound semiconductor nanomaterial preparation, can solve the problems of limited biological application, inability to effectively realize biocompatibility modification, low fluorescence efficiency of quantum dots, etc. Chemical production, good repeatability

Active Publication Date: 2014-06-11
NANGTONG HAODI ANTICORROSION EQUIP
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  • Abstract
  • Description
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Problems solved by technology

CuInS obtained by most of the current synthesis methods 2 The fluorescence efficiency of quantum dots is generally low, generally less than 5%.
Due to the good coordination between thiol (-SH) and Cu and In atoms, the usual method of ligand exchange between thiol carboxylic acid ligands and quantum dot surface ligands cannot effectively realize CuInS 2 and CuInS 2 Biocompatibility modification of ZnS quantum dots, thereby limiting their biological applications

Method used

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  • CuInS2 quantum dots with water-soluble zinc blende structure, CuInS2/ZnS core shell quantum dots with water-soluble zinc blende structure and preparation method thereof
  • CuInS2 quantum dots with water-soluble zinc blende structure, CuInS2/ZnS core shell quantum dots with water-soluble zinc blende structure and preparation method thereof
  • CuInS2 quantum dots with water-soluble zinc blende structure, CuInS2/ZnS core shell quantum dots with water-soluble zinc blende structure and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] In the first step, weigh 22.2mg (0.1mmol) InCl 3 , 10.0mg (0.1mmol) CuCl and 218.5mg (1mmol) mercaptoundecanoic acid were placed in a three-necked flask, and 5ml of PEG-400 was added, under the conditions of magnetic stirring and argon protection, the mixture was heated to make InCl 3 and CuCl were completely dissolved and clarified, and vacuumized for 30 minutes to obtain a mixed precursor solution of In and Cu.

[0032] The second step is to backfill the system with argon, and heat the mixed precursor solution of In and Cu from room temperature to 230 °C at a heating rate of 1 °C / s for 30 minutes, then remove the heat source and cool to room temperature, and then centrifuge and purify to obtain CuInS 2 quantum dots.

[0033] Such as figure 1 As shown, the obtained CuInS 2 The XRD pattern of quantum dots proves that the obtained nanocrystals are sphalerite structure. The atomic ratio of Cu:In:S was calculated to be 1.17:1:2.62 by electron spectrum analysis of the o...

Embodiment 2

[0035] In the first step, weigh 22.2mg (0.1mmol) InCl 3 , 10.0mg (0.1mmol) CuCl and 218.5mg (1mmol) mercaptoundecanoic acid were placed in a three-necked flask, and 5ml of PEG-400 was added, under the conditions of magnetic stirring and argon protection, the mixture was heated to make InCl 3 and CuCl were completely dissolved and clarified, and vacuumized for 30 minutes to obtain a mixed precursor solution of In and Cu.

[0036] In the second step, argon is backfilled into the system, and the mixed precursor solution of In and Cu is heated from room temperature to 200° C. for 15 minutes at a heating rate of 1° C. / s, and then the third step is performed.

[0037] In the third step, the reaction temperature was adjusted to 220°C, and then Zn(SA) with a concentration of 0.1M was added dropwise 2 -PEG400 solution, after heating and reacting for 30min, remove the heat source and naturally cool to room temperature and centrifuge to obtain water-soluble sphalerite structure CuInS 2...

Embodiment 3

[0040] In the first step, weigh 22.2mg (0.1mmol) InCl 3 , 10.0mg (0.1mmol) CuCl and 437.5mg (2mmol) mercaptoundecanoic acid were placed in a three-necked flask, and 5ml of PEG-800 was added, under the conditions of magnetic stirring and argon protection, the mixture was heated to make InCl 3 and CuCl were completely dissolved and clarified, and vacuumized for 30 minutes to obtain a mixed precursor solution of In and Cu.

[0041] In the second step, argon is backfilled into the system, and the mixed precursor solution of In and Cu is heated from room temperature to 230° C. for 40 minutes at a heating rate of 1° C. / s, and then the third step is performed.

[0042] In the third step, the reaction temperature was adjusted to 220°C, and then Zn(SA) with a concentration of 0.1M was added dropwise 2 -PEG400 solution, after heating and reacting for 30min, remove the heat source and naturally cool to room temperature and centrifuge to obtain water-soluble sphalerite structure CuInS 2...

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Abstract

The invention relates to CuInS2 quantum dots with a water-soluble zinc blende structure, CuInS2 / ZnS core shell quantum dots with a water-soluble zinc blende structure and a preparation method thereof. In the CuInS2 quantum dots with the water-soluble zinc blende structure, the atomic ratio of Cu to In to S is 1.17 to 1 to 2.62, the XRD pattern of the CuInS2 quantum dots has three main structural characteristic peaks comprising 28.61 DEG, 47.51 DEG and 55.81 DEG which are corresponding to (111), (220) and (222) in the zinc blende crystal structure. The range of fluorescence-emission peak position of the CuInS2 / ZnS core shell quantum dots with the water-soluble zinc blende structure is 554-710 nm, and the fluorescence quantum yield is 15-30 %, so that the biomedical diagnostic requirements are satisfied. The method combines the popular and mature colloid chemistry synthesis method for preparing oil soluble quantum dots at present, the CuInS2 quantum dots with the water-soluble zinc blende structure and CuInS2 / ZnS core shell quantum dots with the water-soluble zinc blende structure are prepared by using PEG as solvent, sulfhydryl undecanoic acid as ligand and sulfur source, so that the step of biocompatibility modification is saved for later biomedical diagnosis. The quantum dots and the preparation method disclosed in invention have the advantages of short synthesis cycle, simple technology and good repeatability, and are beneficial to the mass production.

Description

technical field [0001] The invention relates to the technical field of preparation of compound semiconductor nanomaterials, in particular to CuInS with a water-soluble sphalerite structure 2 and CuInS 2 / ZnS core-shell quantum dot and its preparation method. Background technique [0002] Quantum dot (quantum dot, QD) is an aggregate composed of a small number of atoms or molecules, its size is generally less than 10nm, usually spherical or spherical, and its radius is smaller than or close to the exciton Bohr radius (electron and the distance between holes), which are semiconductor nanoparticles that can accept excitation light and generate fluorescence. Based on quantum effects, when the particle size enters the nanoscale, it will show some special properties that are obviously different from bulk materials, such as quantum size effect, dielectric confinement effect, surface effect, small size effect and macroscopic quantum tunneling effect. etc., and exhibit some unique...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/62G01N21/64G01N33/52
Inventor 常津郭伟圣
Owner NANGTONG HAODI ANTICORROSION EQUIP
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