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A doped core-shell nanomaterial and preparation method thereof

A core-shell nanomaterial and nanomaterial technology, which is applied in the field of nanomaterials and their preparation, can solve the problems of harsh reaction conditions, complicated reaction steps, and high cost, and achieves the advantages of good size controllability, good water solubility and low equipment requirements. Effect

Inactive Publication Date: 2017-01-25
SOUTHWEAT UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] At present, there are many methods for preparing high-quality nanocrystals, such as metal-organic methods, hydrothermal methods, and single-molecule precursor methods. For example, the patent document CN101891162A discloses "a low-cost synthetic Zn x Cd 1-x Se(0≤x≤1) and its related core-shell structure semiconductor nanocrystal method", patent document CN101948686B discloses "a method for synthesizing manganese-doped zinc selenide color-tunable fluorescent quantum dots in aqueous phase", patent document CN102517025B discloses "a method for preparing ZnSe / ZnS core-shell quantum dots", and patent document CN104974742A discloses "a method for preparing CdTeSeS / ZnTe core-shell quantum dots by aqueous phase microwave", but most of these preparation methods have harsh reaction conditions, If the reaction temperature is high, equipment such as an autoclave is required, the reaction steps are relatively complicated, and the reaction reagent still uses a large amount of organic matter, which is highly toxic and harmful to the health of researchers and developers, and is expensive and expensive.
Most importantly, most of the nanocrystals synthesized by these methods are oil-soluble nanocrystals, which have poor water solubility and low biocompatibility, which seriously limit their application in the field of biomedicine.

Method used

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  • A doped core-shell nanomaterial and preparation method thereof
  • A doped core-shell nanomaterial and preparation method thereof
  • A doped core-shell nanomaterial and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Cd 0.99 Cu 0.01 Preparation of Se / ZnS nanomaterials:

[0040] Step 1, take 0.0201g Cu(CH 3 COO) 2 ·H 2 O and 2.6787g Cd(CH 3 COO) 2 2H 2 O, dissolved in 30mL high-purity water at the same time, under the protection of nitrogen, add 1328uL mercaptoacetic acid, adjust the pH value to 10; obtain a cationic aqueous solution;

[0041] Step 2: Add 30 mL of high-purity water into the three-necked bottle, fill it with nitrogen for protection, add 0.78 g of sodium borohydride, stir thoroughly to dissolve it, add 0.7904 g of selenium powder, and react at room temperature for 20 minutes to obtain an anion precursor;

[0042] Step 3. Under the protection of nitrogen, raise the temperature of the anion precursor solution and keep it at 100°C, add the cation aqueous solution in step 1 to the anion precursor solution, fully stir, and react for 60 minutes to obtain the nuclear layer nanomaterial precursor solution; the stirring reaction The speed is 300r / min;

[0043] Step fou...

Embodiment 2

[0055] Cd 0.99 co 0.01 Preparation of Se / ZnS nanomaterials:

[0056] Step 1, take 0.0125g Co(CH 3 COO) 2 4H 2 O and 1.1584g Cd(CH 3 COO) 2 2H 2 O, dissolved in 20mL high-purity water at the same time, under nitrogen protection, add 1mL 3-mercaptopropionic acid, adjust the pH to 9, and obtain a cationic aqueous solution;

[0057] Step 2: Add 20 mL of high-purity water into the three-necked bottle, fill it with nitrogen for protection, add 0.386 g of sodium borohydride, stir well to dissolve it, add 0.3952 g of selenium powder, and react at room temperature for 15 minutes to obtain an anion precursor;

[0058] Step 3. Under nitrogen protection, raise the temperature of the anion precursor solution and keep it constant at 90°C, add the cation aqueous solution in step 1 to the anion precursor solution, fully stir, and react for 50 minutes to obtain the nuclear layer nanomaterial precursor solution; the stirring reaction The speed is 300r / min;

[0059] Step four, take 0.92...

Embodiment 3

[0061] Cd 0.95 Zn 0.05 Preparation of Se / ZnS nanomaterials:

[0062] Step 1, take 0.1112g Zn(CH 3 COO) 2 2H 2 O and 2.6677g Cd(CH 3 COO) 2 2H 2 O, dissolved in 20mL high-purity water at the same time, under the protection of nitrogen, add 4350uL glutathione, adjust the pH value to 9, and obtain a cationic aqueous solution;

[0063] Step 2. Add 50mL of high-purity water into the three-necked bottle, fill it with nitrogen for protection, add 0.9264g of sodium borohydride, stir well to dissolve it, add 0.9485g of selenium powder, and react at room temperature for 30 minutes; obtain anion precursor solution;

[0064] Step 3. Under nitrogen protection, raise the temperature of the anion precursor solution and keep it constant at 120°C, add the cation aqueous solution in step 1 to the anion precursor solution, stir fully, and react for 60 minutes to obtain the nuclear layer nanomaterial precursor solution; the stirring reaction The speed is 300r / min;

[0065] Step 4, get 2....

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Abstract

The invention discloses a doped core-shell nanometer material and a preparation method thereof. The chemical general formula of the material is Cd1-xMxSe / ZnS, and M is one of Cr, Mn, Fe, Co, Ni, Cu, Zn, Bi, Ce, Pr, Nd, Eu and Er. The preparation method comprises the steps that 1, a positive ion aqueous solution is prepared, a surface finishing agent is added, the pH value is adjusted, and positive ion precursor liquid is obtained; 2, Se powder is added to a NaBH4 aqueous solution, a reaction is carried out under protection of nitrogen, and negative ion precursor liquid is obtained; 3, at constant temperature, the negative ion precursor liquid and the positive ion precursor liquid are mixed for reacting, and core layer Cd1-xMxSe nanocrystalline precursor liquid is obtained; 4, a Zn<2+> and S<2-> ion aqueous solution is added through titrimetry, the reaction continues to be carried out, cooling is carried out under protection of nitrogen, detergent is added for centrifugation and washing, and the doped core-shell nanometer material is obtained. The material is free of toxins or low in toxin, and the preparation method is simple in step; the size is easy to control, and large-scale production can be achieved. A novel method is provided for preparing efficient and cheap biomedical materials.

Description

technical field [0001] The invention belongs to the field of nanometer materials and their preparation, in particular to a doped core-shell nanometer material and its preparation method. Background technique [0002] II-VI semiconductor nanomaterials have excellent optical properties such as wide excitation spectrum, narrow emission spectrum, and high photochemical stability, and have extremely broad application prospects in light-emitting diodes, photodetectors, solar cells, and field-effect transistors. Especially as a biomarker, its performance surpasses the widely used organic dye markers in many aspects, and it has become a new research hotspot in the field of biomedicine. [0003] Among them, CdTe, CdSe and other cadmium-based nanomaterials are the most widely studied due to their excellent optical properties, but Cd elements belong to the A-type toxic elements, which may bring toxicity to organisms, which greatly limits their applications in cell imaging, immune analy...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G9/08B82Y30/00B82Y40/00
Inventor 谢瑞士李园利
Owner SOUTHWEAT UNIV OF SCI & TECH
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