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A kind of aginse2 nano crystal and preparation method thereof

A technology of nanocrystals and precursor solutions, applied in the direction of nanotechnology, nanotechnology, chemical instruments and methods, etc., can solve the problems of preparing complex single precursors, complex operation process, and non-environmental protection, and achieve simple and repeatable process Good, short synthetic cycle effect

Active Publication Date: 2016-06-22
INST OF CHEM MATERIAL CHINA ACADEMY OF ENG PHYSICS
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  • Summary
  • Abstract
  • Description
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  • Application Information

AI Technical Summary

Problems solved by technology

Since then, some other methods have been discovered for AgInSe 2 Synthesis of nanocrystals (e.g. (a) DingshengWang, WenZheng, ChenhuiHao, QingPeng, YadongLi, Chem. , ShouhuaFeng, Nanoscale, 2014, 6, 6782–6789; (c) reported by LiWang, PengzhanYing, YuanDeng, HongZhou, ZhengliangDu, JiaolinCui, RSCAdv., 2014, 4, 33897–33904), but the above synthetic methods still have many shortcomings First of all, these synthetic methods are relatively cumbersome and not environmentally friendly, and most of them use toxic solvents (such as oleylamine, tri-n-octylphosphine, etc.), and secondly, these synthetic methods need to prepare complex single precursors. In addition, the nanocrystals prepared by these synthetic methods are all oil-soluble nanocrystals, which can only be dispersed in non-polar organic solvents, such as n-hexane, toluene and other solvents. In the field of photocatalytic degradation of dyes or photocatalytic hydrogen production, nanocrystals that can be dispersed in the water phase are obviously a better choice, that is, it is hoped that the nanocrystals used are water-soluble

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  • A kind of aginse2 nano crystal and preparation method thereof
  • A kind of aginse2 nano crystal and preparation method thereof
  • A kind of aginse2 nano crystal and preparation method thereof

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preparation example Construction

[0030] 1) Preparation of precursor solution

[0031] mixing silver nitrate, indium chloride and / or indium chloride tetrahydrate, selenium dioxide, polyvinylpyrrolidone and dimethylformamide as raw materials and stirring evenly to obtain a precursor solution;

[0032] 3) Compounding of nanocrystals

[0033] Put the precursor solution obtained according to step 1) into an autoclave, react at a constant temperature of 160-220°C for 3-20 hours, centrifuge the reacted solution and collect the solid, wash and dry the obtained solid with a solvent, that is Get AgInSe 2 Nanocrystalline;

[0034] When selecting indium chloride tetrahydrate in step 1), the mass ratio between raw materials is silver nitrate: indium chloride tetrahydrate: selenium dioxide: polyvinylpyrrolidone=30~37:53~64:60~110:200~2000 , Of course, when choosing indium chloride, its dosage can be converted by the above mass ratio. Oleic acid can also be added to the raw materials in step 1) and mixed and stirred evenl...

Embodiment 1

[0039] First, 34mg of silver nitrate, 60mg of indium chloride tetrahydrate, 88.8mg of selenium dioxide and 1g of polyvinylpyrrolidone (PVP) were added to 25mL of oleic acid and 10mL of dimethylformamide to form a mixed solution, and the above mixed solution was stirred for 40 minutes , to form a precursor solution; then add the precursor solution into a 50mL high-pressure reactor lined with tetrafluoroethylene, seal the reactor and place it in a programmed temperature-controlled oven for reaction at a temperature of 200°C. The time is 12 hours. After the reaction is over, after the reaction kettle is naturally cooled to room temperature, open the reaction kettle, take out the tetrafluoroethylene liner, and then carry out centrifugation on the reaction solution to collect the reaction product, and then use deionized water, ethanol, etc. to clean and centrifuge several times, and finally dried in a vacuum oven at 60°C for 4 hours to obtain AgInSe 2 Nanocrystals, which are solub...

Embodiment 2

[0041] First, 34mg of silver nitrate, 60mg of indium chloride tetrahydrate, 88.8mg of selenium dioxide and 0.5g of PVP were added to 25mL of oleic acid and 10mL of dimethylformamide, and stirred for 40 minutes to form a precursor solution; then the precursor solution was added to 50mL tetrafluoroethylene-lined autoclave. After sealing the kettle body, place it in a programmed temperature-controlled oven for reaction, set the reaction temperature to 200° C., and the reaction time to 12 hours.

[0042] After the reaction is over, cool the reaction kettle to room temperature naturally, open the reaction kettle, take out the tetrafluoroethylene liner, then centrifuge the reaction solution to collect the reaction product, and wash the reaction product with deionized water, ethanol, etc. successively. Centrifuge several times, and finally dry in a vacuum oven at 60°C for 4 hours to obtain AgInSe 2 Nanocrystalline, which is soluble in water.

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Abstract

The invention discloses AgInSe2 nanocrystalline and a preparation method thereof. The preparation method comprises the following steps: mixing and uniformly stirring silver nitrate, indium chloride and / or indium chloride tetrahydrate, selenium dioxide, polyvinylpyrrolidone and dimethyl formamide to obtain a precursor liquid; allowing the precursor liquid to have a constant-temperature reaction in a high-pressure kettle at the temperature of 160-220 DEG C for 3-20 hours to obtain the AgInSe2 nanocrystalline, wherein the AgInSe2 nanocrystalline is a metastable orthorhombic crystal system of which the space group is Pna21 and is soluble in water. The preparation method disclosed by the invention adopts simple and cheap raw materials and is simple in process, short in synthesis period, good in repeatability and environment-friendly; and the prepared AgInSe2 nanocrystalline can be well dispersed in a water phase and has application advantages in the fields such as biomedicines and water-phase optical catalysis.

Description

technical field [0001] The present invention relates to a kind of preparation method of nanocrystal and nanocrystal, particularly a kind of AgInSe 2 Preparation method of nanocrystal and corresponding AgInSe 2 Nanocrystalline. Background technique [0002] I-III-VI 2 Semiconductor nanocrystals have many excellent properties, such as low toxicity, large light absorption coefficient, narrow band gap, and light emission wavelength in the near-infrared region. Show attractive application prospects, aroused strong attention. as I-III-VI 2 An important member of the family of semiconductor nanocrystals, AgInSe 2 Nanocrystals have a band gap of about 1.24eV, which is conducive to good applications in the fields of bioluminescent labeling, photocatalysis, and solar cells. However, due to the lack of effective general synthesis methods, they mainly focus on the research of bulk and thin film morphology. Until 2006, Vittal's research group (MengT.Ng, ChrisB.Boothroyd, JagadeseJ....

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B19/00B82Y30/00B82Y40/00
CPCC01B19/002C01P2002/72C01P2002/85C01P2004/03C01P2004/61C01P2004/62
Inventor 刘忠平邓建国纪兰香白小峰马春彦杨雪梅
Owner INST OF CHEM MATERIAL CHINA ACADEMY OF ENG PHYSICS
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