Method for preparing oil soluble semiconductor nanocrystalline without phosphine

An oil-soluble, semiconductor technology, applied in nanotechnology, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of difficult control of selenium reactivity, unsuitable for industrial production of nanocrystals, high reaction temperature, and achieve good experimental repeatability, The effect of reducing the preparation cost and easy experimental operation

Inactive Publication Date: 2012-07-18
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although this improvement removes the organic phosphine reagent, the reactivity of selenium is difficult to control, and the reaction temperature is high, so it is not suitable for the industrial production of nanocrystals

Method used

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  • Method for preparing oil soluble semiconductor nanocrystalline without phosphine
  • Method for preparing oil soluble semiconductor nanocrystalline without phosphine
  • Method for preparing oil soluble semiconductor nanocrystalline without phosphine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Add 0.08g of Se powder into the mixed solution of 0.5ml of oleylamine and 0.5ml of dodecyl mercaptan, stir in the air, and wait until the Se powder is completely dissolved to obtain a wine red solution. This solution was used as a Se precursor for the synthesis of semiconductor nanocrystals.

[0024] 0.085g CuCl 2 2H 2 O, 0.056g SnCl 2 2H 2 O, 0.034g ZnCl 2 1. Add 1ml of dodecyl mercaptan to 10ml of oleylamine. The reaction system was evacuated and nitrogen was blown 3 times, 10 minutes each time. Then heated to 60 ° C under vacuum conditions for 0.5 hours, the CuCl 2 2H 2 O, SnCl 2 2H 2 O and ZnCl 2 Dissolved to obtain a milky white solution. then in N 2 The temperature of the solution was raised to 180°C under gas protection, and the previously prepared Se precursor was injected, and the reaction was continued at 180°C for 30 minutes, as shown in figure 1 As shown, get Cu 2 ZnSnSe 4 semiconductor nanocrystals.

Embodiment 2

[0026] Add 0.08g of Se powder into the mixed solution of 0.5ml of oleylamine and 0.5ml of dodecyl mercaptan, stir in the air, and wait until the Se powder is completely dissolved to obtain a wine red solution. This solution was used as a Se precursor for the synthesis of semiconductor nanocrystals.

[0027] 0.085g CuCl 2 2H 2 0.0.056g SnCl 2 2H 2 O, 0.068g ZnCl 2 1. Add 1ml of dodecyl mercaptan to 10ml of oleylamine. The reaction system was evacuated and nitrogen was blown 3 times, 10 minutes each time. Then heated to 60°C under vacuum for 0.5 hours to react the CuCl 2 2H 2 O, SnCl 2 2H 2 O and ZnCl 2 Dissolved to obtain a milky white solution. then in N 2Under the protection of gas, the solution was heated to 180°C, the Se precursor was injected, and the reaction was carried out for 30 minutes to obtain Cu 2 ZnSnSe 4 semiconductor nanocrystals.

Embodiment 3

[0029] Add 0.08g of Se powder into the mixed solution of 0.5ml of oleylamine and 0.5ml of dodecyl mercaptan, stir in the air, and wait until the Se powder is completely dissolved to obtain a wine red solution. This solution was used as a Se precursor for the synthesis of semiconductor nanocrystals.

[0030] 0.085g CuCl 2 2H 2 O, 0.056g SnCl 2 2H 2 O, 0.136g ZnCl 2 1. Add 1ml of dodecyl mercaptan to 10ml of oleylamine. The reaction system was evacuated and nitrogen was blown 3 times, 10 minutes each time. Then heated to 60°C under vacuum for 0.5 hours to react the CuCl 2 2H 2 O, SnCl 2 2H 2 O and ZnCl 2 Dissolved to obtain a milky white solution. then in N 2 Under the protection of gas, the solution was heated to 180°C, the Se precursor was injected, and the reaction was carried out for 30 minutes to obtain Cu 2 ZnSnSe 4 semiconductor nanocrystals.

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Abstract

The invention belongs to the technical field of semiconductor nanocrystallines and relates to a method for preparing an oil soluble semiconductor nanocrystalline with high quality. The method comprises the following steps of: preparing a selenium precursor by reducing and dissolving selenium powder in aliphatic amine by using alkyl sulfhydryl; and preparing the oil soluble semiconductor nanocrystalline with high quality by using the selenium precursor. During the preparation process, used raw materials comprise a metal source (a cadmium source, a copper source, a zinc source, a tin source, an indium source and a gallium source), the selenium powder, the aliphatic amine, the alkyl sulfhydryl and octadecene. The selenium precursor is prepared by reducing the selenium powder with the alkyl sulfhydryl, the alkyl sulfhydryl is low in price, and harmless and environment-friendly, and can stably exist in air, and the reaction of reducing the selenium powder with the alkyl sulfhydryl can be finished in the air, so the method reduces the cost for preparing the nanocrystalline effectively, is environment-friendly and is very suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of semiconductor nanocrystal preparation, and in particular relates to a phosphine-free method for preparing oil-soluble semiconductor nanocrystals, in particular to a method for preparing selenium precursors by reducing and dissolving selenium powder in aliphatic amines with alkylthiols body, and using this precursor to prepare high-quality oil-soluble semiconductor nanocrystals. Background technique [0002] Semiconductor nanocrystals are widely used in optoelectronic devices, photonic crystals, fluorescent coding, and biomarkers due to their quantum size effect. With the increasing demand for semiconductor nanocrystals, more and more synthesis methods have been developed, and the most effective method is the thermal injection method. This method mainly adopts the operation technology of instantaneously injecting the precursor solution into the system under high temperature conditions, effectively separat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B19/00C01B19/04B82Y40/00
Inventor 张皓刘轶姚栋杨柏
Owner JILIN UNIV
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