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Novel preparation method for ternary alloy type CdSeS quantum dots

A ternary alloy and quantum dot technology, applied in chemical instruments and methods, luminescent materials, etc., can solve problems such as low cost, poor reproducibility, and no strong reducibility, and achieve stable product properties, low cost, and stable optical properties. Effect

Inactive Publication Date: 2014-01-01
TIANJIN NAMEI NAMI TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Aiming at the problem that in the existing synthesis of CdSeS quantum dots, the reaction will produce a "popping" phenomenon and the reproducibility of the final quantum dots is poor due to the strong reducibility of trihydrocarbyl phosphine, we have designed a method that uses trialkylselenophosphine, trialkylthiophosphine and The stock solution B is obtained after the trialkylphosphine oxide is mixed, and the stock solution B is injected into the precursor solution A mixed with long-chain fatty acid cadmium and long-chain trialkylamine to react a new method for synthesizing CdSeS quantum dots, because the trialkyl The reaction of selenophosphine, trialkylthiophosphine and trialkylphosphine oxide with long-chain fatty acid cadmium does not generate water, thus avoiding the danger and inconvenience caused by the "burst" phenomenon at very high temperature (250-350°C), At the same time, trialkylselenophosphine, trialkylthiophosphine, and trialkylphosphine oxide have no strong reducing properties, have good stability in the air, ensure the repeatability of the experiment, and will not produce impurities due to reaction with air , it is also safer during storage and transportation, and the cost is lower

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  • Novel preparation method for ternary alloy type CdSeS quantum dots
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preparation example Construction

[0029] The invention provides a new preparation method of ternary alloy type CdSeS quantum dots, comprising the following steps:

[0030] a. Install mechanical stirring and inert gas protection device on the four-necked bottle, heat the long-chain fatty acid cadmium and long-chain trialkylamine to 250-350°C under the protection of inert gas to obtain precursor solution A;

[0031] The long-chain fatty acid cadmium is the cadmium source of the target CdSeS quantum dot, the type of the long-chain fatty acid cadmium is not limited, and the preferred divalent cadmium compound is cadmium myristate, cadmium palmitate, cadmium stearate or cadmium oleate , more preferably cadmium oleate and cadmium stearate.

[0032] Compared with the preparation method of the prior art, inorganic cadmium compounds are used, such as cadmium oxide, cadmium chloride, cadmium sulfate, cadmium carbonate, etc., all produce water or inorganic acid during high temperature reaction-these by-products are very ...

Embodiment 1

[0047] Install mechanical stirring and argon protection device on the 500ml four-necked bottle, add 12.157 grams (20.3 mmol) cadmium stearate (CdSt 2 ), 20ml oleic acid (OA) and 200ml trioctylamine (TOA), heated up under the protection of argon. Accurately weigh 0.746 g (1.66 mmol) of trioctylselenophosphine (TOPSe), 28.189 g (70 mmol) of trioctylsulfophosphine (TOPS) and 9.918 g of trioctylphosphine oxide (TOPO, stock solution) in a 50 ml beaker, Mix well and draw into a 50ml syringe. When the reaction temperature reaches 295°C and is stable, a light brown transparent liquid is obtained. Inject the stock solution within 5 seconds and maintain the temperature for 5 minutes. Transfer the reaction solution to a triangular flask filled with ethanol, let it stand for more than 8 hours, pour off the supernatant, centrifuge, and pour off the supernatant; add a small amount of chloroform to dissolve the remaining solid, and then add ethanol. Repeat operation. The remaining solid ...

Embodiment 2

[0050] Install mechanical stirring and argon protection device on the 100ml four-necked bottle, add 1197.76mg (2mmol) CdSt 2 , 2mlOA and 30mlTOA, heated up under the protection of argon. Accurately weigh 0.180gTOPSe, 1.208gTOPS and 2mlTOPO (stock solution) in a 10ml beaker, mix well, and draw into a 5ml syringe. When the reaction temperature reaches 310°C and is stable, a light brown transparent liquid is obtained. Inject the stock solution within 5 seconds and maintain the temperature for 5 minutes. Transfer the reaction solution to a triangular flask filled with ethanol, let it stand for more than 8 hours, pour off the supernatant, centrifuge, and pour off the supernatant; add a small amount of chloroform to dissolve the remaining solid, and then add ethanol. Repeat operation. The remaining solid was vacuum-dried for 2 hours to obtain 0.219 g of cadmium sulfur selenide quantum dot solid powder.

[0051] Measured on the A380 fluorescence spectrophotometer produced in Gang...

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Abstract

The invention provides a novel preparation method for ternary alloy type CdSeS quantum dots, which includes the following steps: mixing long-chain fatty acid cadmium with long-chain trialkylamine to obtain a precursor solution A; mixing trialkyl phosphine selenium, trialkyl phosphorus sulfide and trialkyl phosphine oxide to obtain a solution B, injecting the solution B in the precursor solution A for reaction, so as to obtain a CdSeS quantum dot solution C, removing non-reacted reactants, impurities and the long-chain trialkylamine as a solvent, and obtaining CdSeS quantum dot powder. The novel preparation method has the benefits that the preparation technology is simple, good safety, stability and repeatability are realized, the cost is low, high-quality quantum dots can be prepared in a large-scale manner; the optical property of the prepared quantum dots is stable, the spectroscopic property is excellent, the photoluminescence spectra are continuous and adjustable; the chemical reaction of the preparation method is limited in one container, the operation is simple, precise control of the reaction conditions is easier, and proprieties of products in batch production are more stable.

Description

technical field [0001] The invention belongs to the field of industrial manufacturing of quantum dot materials, and in particular relates to a new preparation method of ternary alloy type CdSeS quantum dots. Background technique [0002] Quantum dots (Qds), also known as quasi-zero-dimensional semiconductor nanocrystals (semi conductor nanocrystal), are nanocrystals composed of II-VI or III-V chemical elements. Due to the nanoscale effect, electrons and holes are quantum-confined. When the diameter is smaller than the Bohr diameter, quantum dot nanoparticles change from a continuous energy level to a discrete energy level structure with molecular characteristics. Therefore, after receiving energy (excitation), it can emit light of a specific wavelength. The reason why quantum dot research has been valued by the scientific and industrial circles, especially in the fields of biomedicine, anti-counterfeiting, LED, and solar cells, is that its unique photoluminescent properties...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/88
Inventor 曹世东
Owner TIANJIN NAMEI NAMI TECH CO LTD
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