Preparation of water-soluble CdS:Ag doped nano-crystalline through microwave method

A nanocrystal, water-soluble technology, which is applied in the field of water-phase preparation of doped CdS:Ag semiconductor nanocrystal materials, can solve the problems of complex process, fluorescence attenuation, narrow adjustable range, etc., and achieves low preparation cost and repeatability. Good and efficient effect

Inactive Publication Date: 2013-02-13
JILIN INST OF CHEM TECH +1
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Problems solved by technology

[0003]The fluorescent properties of CdS nanocrystals can be changed by doping technology, but this method is generally limited to the field of organic phase synthesis, mainly doping manganese and copper metal ions in the In CdS nanocrystals, although the emission peak position of CdS nanocrystals is changed to a certain extent, the adjustable range is very narrow, generally no more than 20 nm
Moreover, the method of organic phase doping has complex processes, harsh conditions, high toxicity, and great harm to the health of operators. It is difficult to synthesize in large quantities and cannot realize industrialization.
At present, the aqueous phase doping technology cannot change the fluorescence properties of CdS nanocrystals. The main reason is that surface metal ions, such as copper ions, undergo redox reactions with mercapto compounds, which seriously affects the stability of the solution, resulting in fluorescence attenuation. Appropriate ways to improve

Method used

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  • Preparation of water-soluble CdS:Ag doped nano-crystalline through microwave method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] 1) Preparation of cadmium source

[0018] Take 100 mL of water into a three-necked flask, and then dissolve 29 mg of CdCl 2 2.5H 2 O and 25 μL thioglycolic acid in water, adjust the pH to 9 with NaOH to form a stable cadmium metal complex, the molar ratio of cadmium salt and dispersant is 1:2.5.

[0019] 2) Preparation of doped cadmium source

[0020] Add 5 mL 0.01 molL to 100 mL water -1 Ag + , after completely dissolving, add 1.25 μL of mercaptopropionic acid, mix well, pour into the constant pressure funnel installed on the upper right side of the three-necked flask, and set aside;

[0021] 3) Preparation of sulfur source

[0022] Weigh 156 mg Na 2 S solid, dissolved in 10 mL of water, take 1 mL of Na 2 S solution was poured into the constant pressure funnel on the upper left side of the three-necked flask;

[0023] 4) Open the right side discharge valve on the constant pressure funnel, and slowly put the Ag + The solution is added dropwise to the cadmium so...

Embodiment 2

[0028] 1) Preparation of cadmium source

[0029] Take 100 mL of water into a three-necked flask, and then dissolve 290 mg of CdCl 2 2.5H 2 O and 250 μL thioglycolic acid in water, adjust the pH to 9 with NaOH to form a stable cadmium metal complex, the molar ratio of cadmium salt and dispersant is 1:2.5;

[0030] 2) Preparation of doped cadmium source

[0031] Add 5 mL of 0.1 molL to 100 mL of water -1 Ag + , after completely dissolved, add 12.5μm MPA, mix evenly, pour into the constant pressure funnel installed on the upper right side of the three-necked flask, and set aside;

[0032] 3) Preparation of sulfur source

[0033] Weigh 1.56 g Na 2 S solid, dissolved in 10 mL of water, take 1 mL of Na 2 S solution was poured into the constant pressure funnel on the upper left side of the three-necked flask;

[0034] 4) Open the right side discharge valve on the constant pressure funnel, and slowly put the Ag + The solution is added dropwise to the cadmium source solution, ...

Embodiment 3

[0039] 1) Preparation of cadmium source

[0040] Take 100 mL of water into a three-necked flask, and then dissolve 29 mg of CdCl 2 2.5H 2 O and 25 μL thioglycolic acid in water, adjust the pH to 9 with NaOH to form a stable cadmium metal complex, the molar ratio of cadmium salt and dispersant is 1:2.5, through the airway inserted directly above the constant pressure funnel into the high Pure argon, remove the oxygen contained in the solution;

[0041] 2) Preparation of doped cadmium source

[0042] Add 5 mL 0.01 molL to 100 mL water -1 Ag + , after it is completely dissolved, pour it into the constant pressure funnel installed on the upper right side of the three-necked flask, pass high-purity argon through the air tube inserted directly above the constant pressure funnel, remove the oxygen contained in the solution, and add 12.5 μL of mercaptopropane acid, mix well, set aside;

[0043] 3) Preparation of sulfur source:

[0044] Weigh 156 mg Na 2 S solid, dissolved in 1...

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Abstract

The invention discloses a method and device for synthesizing a CdS:Ag doped nano-crystalline material in the chemical industry fields and aims to provide a preparation method, which is environment-friendly, simple, easy, low in energy consumption and free from injury of operators. The method comprises the following steps of: preparing a cadmium source, a doped cadmium source and a sulphur source; mixing the doped cadmium source with the sulphur source; and promoting growth of doped CdS:Ag nano-crystalline through microwave. Doped CdS:Ag nano-crystalline nucleus in a precursor rapidly grows under the action of microwave; doped CdS:Ag nano-crystalline solutions of different fluorescent wavelengths are obtained within different action times; the solutions are clear and transparent; the fluorescence emission spectrum coverage range is wide; the quantum efficiency is high; the powdered CdS:Ag doped nano-crystalline material is obtained after freeze-drying; and the CdS:Ag doped nano-crystalline material has better chemical stability and light stability.

Description

technical field [0001] The invention belongs to an aqueous phase preparation method of a doped CdS:Ag semiconductor nano crystal material, in particular to a preparation method and a synthesis device of a CdS:Ag nano crystal whose fluorescence emission wavelength covers the entire visible light region. Background technique [0002] Cadmium sulfide (CdS) is an important semiconductor material with high luminescence quantum yield. In recent years, the synthesis of high-quality CdS nanocrystals in aqueous phase using mercapto compounds as stabilizers has begun to be studied. Recent studies have found that CdS is a very promising semiconductor material in photoelectric conversion. However, the fluorescence emission peaks of CdS nanocrystals stabilized with mercapto compounds are mainly concentrated at 420–510 nm, and it is difficult to extend to the entire visible region. Therefore, the development of CdS nanocrystals is limited. [0003] The fluorescent properties of CdS nano...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/56
Inventor 沈启慧刘岩
Owner JILIN INST OF CHEM TECH
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