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Method for preparing oil-soluble selenium or telluride semiconductor quantum dot without phosphine through dissolving chalcogenide oxide by alkanethiol

A technology of alkyl thiols and oxides, applied in chemical instruments and methods, nanotechnology, nano optics, etc., can solve problems such as long reflow time, unfavorable industrial production of quantum dots, and reaction temperature limitations, etc., to achieve good performance, The effect of reducing the preparation cost and reducing the risk

Inactive Publication Date: 2017-05-10
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this improvement removes the organic phosphine reagent, due to the low boiling point of water, the reaction temperature is limited, and usually requires a long reflux time to complete the reaction
Not conducive to the industrial production of quantum dots
In addition, this method has great limitations and is only suitable for the preparation of selenium or telluride semiconductor quantum dots containing cadmium and mercury.

Method used

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  • Method for preparing oil-soluble selenium or telluride semiconductor quantum dot without phosphine through dissolving chalcogenide oxide by alkanethiol
  • Method for preparing oil-soluble selenium or telluride semiconductor quantum dot without phosphine through dissolving chalcogenide oxide by alkanethiol
  • Method for preparing oil-soluble selenium or telluride semiconductor quantum dot without phosphine through dissolving chalcogenide oxide by alkanethiol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] 0.11g (1mmol) SeO 2 The powder was added to 2 mL of dodecyl mercaptan, the system was vacuumed for 10 minutes, and then nitrogen gas was introduced, and the operation was repeated 3 times. Stir at room temperature under the protection of nitrogen until SeO 2 The powder is completely dissolved to obtain a light yellow solution, which is used as a selenium precursor to synthesize semiconductor quantum dots from selenide.

[0037] 0.27g (1mmol) Cd (AC) 2 2H 2 O was added to a mixed solution of 1 mL oleic acid and 9 mL octadecene. The reaction system was evacuated and nitrogen was blown 3 times, 10 minutes each time. Then heated to 100°C under vacuum for 30 minutes, until Cd(AC) 2 2H 2 O dissolved. then in N 2 Under the protection of air, the solution was heated to 150°C, the selenium precursor prepared earlier was added, and the reaction was continued at 150°C for 10 minutes, as figure 1 As shown, CdSe semiconductor quantum dots were obtained.

Embodiment 2

[0039] 0.06g (0.5mmol) SeO 2 The powder was added to 5 mL of dodecyl mercaptan, the system was vacuumed for 10 minutes, and then nitrogen gas was introduced, and the operation was repeated 3 times. Stir at room temperature under the protection of nitrogen until SeO 2 The powder is completely dissolved to obtain a light yellow solution, which is used as a selenium precursor to synthesize semiconductor quantum dots from selenide.

[0040] 0.14g (0.5mmol) Cd (AC) 2 2H 2 O was added to a mixed solution of 1 mL oleic acid and 9 mL octadecene. The reaction system was evacuated and nitrogen was blown 3 times, 10 minutes each time. Then heated to 100°C under vacuum for 30 minutes, until Cd(AC) 2 2H 2 O dissolved. then in N 2 Under gas protection, the temperature of the solution was raised to 200° C., the previously prepared selenium precursor was added, and the reaction was continued at 200° C. for 30 minutes to obtain CdSe semiconductor quantum dots.

Embodiment 3

[0042] 0.16g (1mmol) TeO 2 The powder was added to 2 mL of dodecyl mercaptan, the system was vacuumed for 10 minutes, and then nitrogen gas was introduced, and the operation was repeated three times. Stirring at 100°C under the protection of nitrogen, the TeO 2 The powder was completely dissolved to obtain an orange solution, which was cooled to room temperature. This solution is used as a tellurium precursor for the synthesis of semiconductor quantum dots.

[0043] 0.32g (1.4mmol) CdCl 2 2H 2 O was added to a mixed solution of 5 mL oleylamine and 5 mL octadecene. The reaction system was evacuated and nitrogen was blown 3 times, 10 minutes each time. Then heated to 100°C under vacuum for 30 minutes, the CdCl 2 2H 2 O dissolved to give a milky white solution. then in N 2 Inject the previously prepared tellurium precursor under gas protection, and stop heating after 10 minutes of reaction, such as figure 2 As shown, CdTe semiconductor quantum dots with green fluoresce...

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Abstract

The invention belongs to the technical field of fluorescent quantum dot preparation, concretely relates to a method for preparing oil-soluble selenium or telluride semiconductor quantum dot without phosphine, and especially relates to a method for preparing a selenium or tellurium precursor by reducing and dissolving selenium dioxide or tellurium dioxide as raw materials in alkanethiol and preparing a high-quality functional selenium or telluride semiconductor quantum dots by utilizing the precursor. The selenium or tellurium dioxide is dissolved by using alkanethiol, so as to obtain a selenium or tellurium solution. The alkanethiol and the selenium or tellurium dioxide used in the invention are all common stable compounds, are low in price, green and environment-friendly. The prepared precursor is high in activity, and can be used for preparing various functional selenium or telluride quantum dots under a relatively mild condition; the method can effectively reduce the preparation cost, meanwhile the environmental pollution is reduced, and the method is significant on the industrial production of the selenium or telluride quantum dots and the relevant LED industry.

Description

technical field [0001] The invention belongs to the technical field of fluorescent quantum dot preparation, and specifically relates to a method for preparing oil-soluble selenium or telluride semiconductor quantum dots without phosphine, in particular to a method of using selenium dioxide or tellurium dioxide as raw materials in alkyl mercaptan The reduction and dissolution method prepares a selenium or tellurium precursor, and uses the precursor to prepare high-quality functional selenium or telluride semiconductor quantum dots. Background technique [0002] Fluorescent selenium or telluride semiconductor quantum dots have narrow fluorescence emission spectra, wide color gamut and good physical and chemical stability. New LED light sources based on such quantum dots have become one of the most competitive technologies in the field of lighting displays. With the increasing demand for selenium or telluride semiconductor quantum dots, the green mass production of selenium or ...

Claims

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Application Information

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IPC IPC(8): C09K11/88B82Y20/00B82Y40/00
CPCB82Y20/00B82Y40/00C09K11/881C09K11/883
Inventor 张皓姚栋辛蔚刘轶杨柏
Owner JILIN UNIV
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