Method for preparing CuInS2 nanocrystalline and CuInS2/ZnS core-shell structure nanocrystalline

A nanocrystal and material technology, which is applied in the preparation of CuInS2/ZnS core-shell nanocrystals (quantum dots) and the preparation of CuInS2 nanocrystals (quantum dots), can solve the problems of inseparability, low fluorescence quantum yield of nanocrystals, problems such as poor repeatability, to achieve the effect of wide spectrum coverage, easy availability of raw materials and stable, improved quantum yield

Inactive Publication Date: 2012-10-10
HUAZHONG AGRI UNIV
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Problems solved by technology

Peng et al. used indium stearate and copper acetate as metal precursors to synthesize high-quality, near-infrared CuInS by organic phase thermal injection. 2 Nanocrystals, but the synthesis method is complicated, the repeatability is poor, and the fluorescence quantum yield of the synthesized nanocrystals is low (less than 3%); Zhong et al synthesized CuInS with cuprous acetate and indium acetate 2 Nanocrystalline, but its maximum emission peak is at 740nm, which does not reach the near-infrared region; later, Li et al. synthesized near-infrared CuInS based on the same method as Zhong, using cuprous iodide and indium acetate as metal precursors. 2 nanocrystals, but because the reactivity of the two metal precursors is not well balanced, the nanocrystals are heterogeneous, and the system contains CuS and In 2 S 3 impurity, inseparable

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  • Method for preparing CuInS2 nanocrystalline and CuInS2/ZnS core-shell structure nanocrystalline
  • Method for preparing CuInS2 nanocrystalline and CuInS2/ZnS core-shell structure nanocrystalline
  • Method for preparing CuInS2 nanocrystalline and CuInS2/ZnS core-shell structure nanocrystalline

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Embodiment 1

[0030] 1) Weigh 2.92g of In(Ac) 3 and the 95% stearic acid of 36g are put into there-necked bottle, under nitrogen atmosphere, at 140 o C was reacted for 5 hours, cooled to room temperature, then washed three times with acetone, after filtering and vacuum drying, the crude product of indium stearate was obtained;

[0031] 2) Put it and 24g of 95% stearic acid into a three-necked bottle, and the other reaction conditions are the same as step 1). After the reaction product is washed with acetone, filtered, and vacuum-dried, it is ground into indium stearate powder;

[0032] 3) Dissolve 0.0191g of CuI and 0.1g of indium stearate powder in a mixed solvent containing 210 μl of oleic acid, 1 ml of dodecanethiol and 10 ml of octadecene, and raise the temperature to 70 o C, hold for 45 minutes, then increase to 225 o C, react for 55 minutes (and take samples after reacting to 5, 10, 20, 30, 40, 50 minutes respectively), cool to room temperature, disperse it in 5ml of chloroform an...

Embodiment 2

[0035] 1) Weigh 2.92gIn(Ac) 3 and the 95% stearic acid of 36g are put into there-necked bottle, under nitrogen atmosphere, at 140 o C was reacted for 5 hours, cooled to room temperature, then washed three times with acetone, filtered to obtain indium stearate, and after vacuum drying, the crude product of indium stearate was obtained;

[0036] 2) Put it and 24g of 95% stearic acid into a three-necked bottle, and the other reaction conditions are the same as step 1). After the reaction product is washed with acetone, filtered, and vacuum-dried, it is ground into indium stearate powder;

[0037] 3) 0.0191g of CuI and 0.1g of 95% indium stearate were dissolved in a mixed solvent containing 210 μl of oleic acid, 1ml of dodecyl mercaptan and 10ml of octadecene, and under a nitrogen atmosphere, the temperature was raised to 70 o C, hold for 45 minutes, then increase to 225 o C, react for 30 minutes;

[0038] 4) Dissolve 0.316g of zinc stearate in a mixed solvent of 2ml of octad...

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Abstract

The invention discloses a method for preparing CuInS2 nanocrystalline and CuInS2 / ZnS core-shell structure nanocrystalline, which is characterized in that stearic acid indium is reacted with cuprous iodide with the same mole in a mixed solution containing oleic acid, superfluous dodecanethiol and octadecene to obtain the CuInS2 nanocrystalline, a zinc stearate solution is added to obtain the CuInS2 / ZnS core-shell structure nanocrystalline. The CuInS2 nanocrystalline and the CuInS2 / ZnS core-shell structure nanocrystalline have the characteristics of homogeneous phase, low toxicity, good monodispersity, strong repeatability, wide spectrum coverage and high fluorescent quantum yield, wherein the fluorescent quantum yield of the CuInS2 nanocrystalline can reach as high as 8.7%; and the fluorescent quantum yield of the CuInS2 / ZnS nanocrystalline can reach as high as 60%. The method of the invention has the advantages of easy available and stable raw materials, safe and convenient operation and no requirement of rigorous condition; thereby the laboratory large-scale preparation and industrial production of the CuInS2 nanocrystalline and CuInS2 / ZnS core-shell structure nanocrystalline realize the possibility.

Description

technical field [0001] The invention belongs to the field of inorganic nanomaterials, in particular to CuInS 2 Preparation methods of nanocrystals (quantum dots). The present invention also relates to CuInS 2 / Preparation method of ZnS core-shell structure nanocrystals (quantum dots) Background technique [0002] Quantum dots (quantum dots, QDs) are three-dimensionally confined, approximately spherical inorganic semiconductor nanocrystals. Due to the excellent optical properties of inorganic semiconductor nanocrystals, many scientists are interested in fluorescent labeling. For example, bioluminescence imaging technology has become the most active subject direction at present. Unfortunately, the weak penetration ability of fluorescent nanocrystals emitting visible light limits their application in in vivo fluorescence imaging. In order to overcome the problem of weak penetration, a series of near-infrared quantum dots (750-900nm) have been developed, mainly including I...

Claims

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Application Information

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IPC IPC(8): C01G15/00B82Y30/00B82Y40/00B01J13/02
Inventor 韩鹤友谷小许黄亮
Owner HUAZHONG AGRI UNIV
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