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Microwave preparation method of water soluble Pr doped Pr:CdTe quantum dots

A water-soluble, quantum dot technology, used in chemical instruments and methods, fluorescence/phosphorescence, luminescent materials, etc., can solve the problem of long time required for quantum dots emitting red fluorescence, poor particle size growth rate and crystallization performance, and sample heating. Non-uniformity and other problems, to achieve the effect of short heating induction period, prevention of crystal phase formation, and low cost

Inactive Publication Date: 2015-11-04
GUANGXI TEACHERS EDUCATION UNIV
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  • Abstract
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Problems solved by technology

[0003] At present, people mainly use the traditional hydrothermal method to synthesize quantum dots, but the quantum dots synthesized by the traditional hydrothermal method usually have a low quantum yield, and the synthesis of quantum dots that emit red fluorescence takes a long time and has a wide half-peak width.
One of the main reasons for the poor particle size growth rate and crystallization performance of quantum dots synthesized by the traditional hydrothermal method is that the traditional hydrothermal method is a slow heating process, which is realized by heat conduction and heat convection. The heating characteristics start from the surface of the sample. Thermal energy spreads from the outside to the inside, resulting in uneven heating of the sample

Method used

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  • Microwave preparation method of water soluble Pr doped Pr:CdTe quantum dots

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Embodiment 1

[0020] A water-soluble Pr-doped Pr: The microwave preparation method of CdTe quantum dots comprises the following steps:

[0021] Step 1, put sodium borohydride with a molar ratio of 5.1:1 and tellurium powder with a content of 99.9% in water, the amount of water is 10 parts by mass, and placed in a microwave synthesizer under nitrogen protection, heated to Stir and react at 75°C for 1 minute, then heat to 92°C and stir for 3 minutes to obtain a sodium telluride hydride solution; wherein, the specification of tellurium powder is 120 mesh sieve;

[0022] Step 2, adding cadmium chloride, praseodymium nitrate and modifier water-soluble N-acetyl-L-cysteine ​​solution in the container, wherein Cd 2+ The concentration is 0.12mol / L, Cd 2+ :Pr 3+ The molar ratio of the solution is 1:0.2, and the pH value of the solution is adjusted to 13.1. Under the protection of nitrogen, inject the sodium hydride telluride solution prepared in step 1, and then pass nitrogen gas from the top of th...

Embodiment 2

[0027] A water-soluble Pr-doped Pr: The microwave preparation method of CdTe quantum dots comprises the following steps:

[0028] Step 1. Put sodium borohydride with a molar ratio of 5.1:1 and tellurium powder with a content of 99.9% in water. The amount of water used is 20 parts by mass. Under the protection of nitrogen, place it in a microwave synthesizer and heat it to 70 ℃ for 2 minutes, then heated to 90 ℃ and stirred for 3 minutes to obtain tellurium sodium hydride solution; wherein, the specification of tellurium powder is 120 mesh sieve;

[0029] Step 2, adding cadmium chloride, praseodymium nitrate and modifier water-soluble N-acetyl-L-cysteine ​​solution in the container, wherein Cd 2+ The concentration is 0.12mol / L, Cd 2+ :Pr 3+ The molar ratio of the solution is 1:0.2, and the pH value of the solution is adjusted to 13.1. Under the protection of nitrogen, inject the sodium hydride telluride solution prepared in step 1, and then pass nitrogen gas from the top of t...

Embodiment 3

[0033] A water-soluble Pr-doped Pr: The microwave preparation method of CdTe quantum dots comprises the following steps:

[0034] Step 1, 0.2067g Te powder and 0.3125g NaBH 4 Put it into a container, add 5mL of distilled water, place it in a microwave synthesizer under the protection of nitrogen, heat at 70°C and stir for 2 minutes, then heat to 95°C and stir for 3 minutes to obtain sodium telluride hydride NaHTe solution; among them, The specification of tellurium powder is 150 mesh sieve;

[0035] Step two, 0.8221g CdCl 2 , 0.2441g Pr(N0 3 ) 3 and 2.1149g of N-acetyl-L-cysteine ​​were dissolved in 30mL of distilled water, where Cd 2+ The concentration is 0.12mol / L, Cd 2+ :Pr 3+ The molar ratio of the solution is 1:0.2, and the pH value of the solution is adjusted to 13.1. Under the protection of nitrogen, inject the sodium telluride hydride NaHTe solution prepared in step 1, and then pass nitrogen gas from the top to the bottom of the solution for 2 minutes to obtain P...

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Abstract

The invention discloses a microwave preparation method of water soluble Pr doped Pr:CdTe quantum dots. The method includes the steps: placing sodium borohydride and a tellurium powder in water with the mole ratio of 5.1:1, under nitrogen protection, placing in a microwave synthesizer, heating to 70-80 DEG C, carrying out a stirring reaction for 1-2 minutes, then heating to 90-95 DEG C, and carrying out a stirring reaction for 2-3 minutes, to obtain a sodium hydrogen telluride solution; then adding a water soluble N-acetyl-L-cysteine solution of a cadmium salt, a praseodymium salt and a modifier in a container, injecting the sodium hydrogen telluride solution, and then introducing nitrogen for 2-3 minutes from the upper side of the solution to the lower side of the solution, to obtain a Pr doped Pr:CdTe quantum dot precursor solution; and finally placing the precursor solution in a microwave reactor, and carrying out a heating reaction to obtain a water soluble Pr doped Pr:CdTe quantum dot solution. The method has the advantages of energy saving, high efficiency, rapid and uniform heating, no pollution, and convenient control.

Description

technical field [0001] The invention relates to the fields of luminescent nanometer materials and biochemical analysis, in particular to a microwave preparation method of water-soluble Pr-doped Pr:CdTe quantum dots. Background technique [0002] Quantum dots are inorganic semiconductor nanocrystals composed of II-VI or III-V elements with a diameter between 2 and 10 nm. Quantum dots have been widely used in biochemical analysis and biomedicine due to their excellent fluorescence properties. At the same time, the synthesis of high-quality, multifunctional fluorescent quantum dots has gradually attracted great attention. [0003] At present, people mainly use the traditional hydrothermal method to synthesize quantum dots, but the quantum dots synthesized by the traditional hydrothermal method usually have a low quantum yield, and the synthesis of quantum dots emitting red fluorescence takes a long time and has a wide half-peak width. One of the main reasons for the poor part...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/88G01N21/64
Inventor 肖琦黄珊谢江宁梁瑜黄初升盛家荣
Owner GUANGXI TEACHERS EDUCATION UNIV
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