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Method for preparing small-particle-size water-soluble cadium selenide quantum dot and its use

A cadmium selenide, quantum dot technology, applied in chemical instruments and methods, luminescent materials, etc., can solve the problems of high flammability of synthetic raw materials, restricted further use, harsh preparation conditions, etc., and achieves low price, good monodispersity, good water solubility

Inactive Publication Date: 2007-06-13
HUAZHONG AGRI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Lianhua et al. used weak acid salts of cadmium such as cadmium oxide and selenium powder as raw materials in the organic phase to synthesize oil-soluble II-VI quantum dots with excellent performance (Lianhua Qu et al., Alternative routes toward high quality CdSenanocrystals.Nano Letters, 2001, 1, 6: 333-337); Although II-VI type quantum dots such as cadmium selenide can be successfully synthesized with this method, the synthetic raw material is highly flammable, and the preparation conditions are harsh, and generally need to use a glove box, and To obtain water-soluble quantum dots, the quantum dots in the organic phase need to be transferred to the aqueous phase, and it is difficult to synthesize quantum dots smaller than 3nm, which limits the further use of this method
Liu Shuman et al. used cadmium carbonate and sodium selenosulfate as raw materials to synthesize cadmium selenide quantum dots in an aqueous solution in one step (Liu Shuman et al., Preparation and Characterization of CdSe Nanocrystals, Photoelectron Laser, 2003 (14), 1: 46-49), but the size distribution of the quantum dots is wide and the stability is not good, and further applications need to be precipitated step by step

Method used

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  • Method for preparing small-particle-size water-soluble cadium selenide quantum dot and its use
  • Method for preparing small-particle-size water-soluble cadium selenide quantum dot and its use
  • Method for preparing small-particle-size water-soluble cadium selenide quantum dot and its use

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 1. Weigh 684mg of cadmium chloride (analytical pure, produced by China Hengxin Chemical Reagent Factory, the same below), dissolve it in 50ml ultrapure water and prepare a solution with a concentration of 0.06mol / L, and add this solution to the solution shown in Figure 7. Into the 100mL three-neck round bottom flask shown in Fig. 1, pass high-purity nitrogen (99.99%, the same below) to remove oxygen for 30min, add thioglycolic acid (analytical grade, produced by Sinopharm Chemical Reagent Co., Ltd., the same below) 30μL, and use 1mol / L NaOH solution adjusts its pH value to 11;

[0025] 2. Weigh 158mg of selenium powder (purity: 99.99%, produced by Tianjin Guangfu Fine Chemical Research Institute), add it to a sodium sulfite solution with a concentration of 0.2mol / L, heat and reflux at 150°C for 60 minutes, and then cool to room temperature (25 DEG C, the same below), make sodium selenosulfate stock solution;

[0026] 3. In a water bath at about 90°C, under the control ...

Embodiment 2

[0029] l. Weigh 340 mg of cadmium chloride, dissolve it in 50 ml of ultrapure water to prepare a solution with a concentration of 0.03 mol / L, add this solution into a 100 mL three-necked round-bottomed flask as shown in Figure 7, and pass high-purity nitrogen to remove oxygen After 20 minutes, add 10 μL of thioglycolic acid and adjust its pH to 10 with 0.5 mol / L NaOH solution;

[0030] 2. Weigh 256 mg of selenium powder, add it to a sodium sulfite solution with a concentration of 0.1 mol / L, heat and reflux at 150°C for 30 minutes, and then lower it to room temperature (25°C) to prepare a sodium selenosulfate stock solution;

[0031] 3. In a water bath at about 90°C, under the control of an ultrasonic cleaner (the operating frequency of the ultrasonic cleaner is: 20KHz, and the power is 60Wcm -2, Ningbo Xinzhi Biotechnology Co., Ltd.), 20ml of newly prepared sodium selenosulfate solution was quickly added to the solution prepared in step 1, and the color of the solution changed...

Embodiment 3

[0033] 1. Weigh 910 mg of cadmium chloride, dissolve it in 50 ml of ultra-pure water to prepare a solution with a concentration of 0.08 mol / L, add this solution into a 100 mL three-necked round-bottomed flask as shown in Figure 7, and pass high-purity nitrogen gas to remove oxygen After 40 minutes, add 30 μL of thioglycolic acid, and adjust its pH value to 12 with 2mol / L NaOH solution;

[0034] 2. Weigh 395 mg of selenium powder, add it to a sodium sulfite solution with a concentration of 0.25 mol / L, heat and reflux at 150° C. for 90 minutes, and then lower it to room temperature (25° C.) to obtain a sodium selenosulfate stock solution;

[0035] 3. In a water bath at about 90°C, under the control of an ultrasonic cleaner (the operating frequency of the ultrasonic cleaner is: 20KHz, and the power is 60Wcm -2 , Ningbo Xinzhi Biotechnology Co., Ltd.), 20ml of newly prepared sodium selenosulfate solution was quickly added to the solution prepared in step 1, and the color of the so...

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Abstract

The invention discloses a method to prepare the small particle soluble CdSe quantum point. The CdCl and the Se powder are the material which is heated by the ultrasonic water bath. The invention needn't use the glove box and the low cost. The process can be finished in water and not use the regent exchange to transform the quantum point in organic phase to the water phase. The CdSe quantum point has the small particle and good stability, so it can be used in the biological probe and the electrochemical lighting material.

Description

technical field [0001] The invention relates to a new method for preparing cadmium selenide (CdSe) quantum dots (semiconductor nano crystals). In particular, it relates to a preparation method and application of small particle size water-soluble cadmium selenide quantum dots. Background technique [0002] Quantum dots (QDs for short) are three-dimensionally confined, approximately spherical inorganic semiconductor nanocrystals, usually between 2-8nm in size and composed of 200-10,000 atoms. Quantum dots have unique quantum size effects and surface effects, which make them have broad application prospects in luminescent materials and photosensitive sensors. Compared with ordinary organic fluorescent dyes, II-VI quantum dots such as cadmium selenide and cadmium sulfide have a series of excellent optical properties and photochemical stability: (1) the emission spectrum is narrow and symmetrical; (2) the emission wavelength can pass through the quantum The size and composition...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/54
Inventor 韩鹤友盛宗海梁建功
Owner HUAZHONG AGRI UNIV
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