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Size-controllable copper antimony sulfur nanocrystalline material and preparation method thereof

A nanocrystalline material, copper antimony sulfur technology, applied in the field of nanomaterials and nanometers, can solve the problems of single choice of organic coupling agent, limited reaction conditions, etc., and achieve the effect of meeting environmental requirements, low equipment requirements, and good reproducibility

Active Publication Date: 2018-03-16
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, currently reported copper antimony sulfur (Cu 12 Sb 4 S 13 ) The size of nanocrystals is relatively large, larger than its Bohr radius; the choice of organic coupling agent is relatively single, which limits the reaction conditions to a relatively small range

Method used

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  • Size-controllable copper antimony sulfur nanocrystalline material and preparation method thereof
  • Size-controllable copper antimony sulfur nanocrystalline material and preparation method thereof
  • Size-controllable copper antimony sulfur nanocrystalline material and preparation method thereof

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Embodiment 1

[0027] A method for preparing a size-controllable copper antimony sulfur nanocrystalline material, comprising the steps of:

[0028] (1) Add 1mmol of copper acetate and 1mmol of antimony acetate to 10mL of octadecene, then add 1ml of oleic acid, pass through argon protection gas, control the temperature at 60°C, and stir rapidly for 5 minutes to make the metal salt completely Dissolving to obtain a metal salt solution;

[0029] (2) Add 20ml of 1-dodecanethiol to the above metal salt solution, stir for 10 minutes to make it fully complex with the metal ion, then add 1mL of 1M elemental sulfur octadecene solution, heat to the set temperature of 100°C and react 30s;

[0030] (3) After the reaction is over, cool to room temperature, add a large amount of methanol to clean the copper antimony sulfur nanocrystals obtained by the reaction, and then dissolve the copper antimony sulfur nanocrystals into the n-hexane solution to obtain the n-hexane of the copper antimony sulfur nanocry...

Embodiment 2

[0033] A method for preparing a size-controllable copper antimony sulfur nanocrystalline material, comprising the steps of:

[0034] (1) Add 1mmol of copper acetate and 1mmol of antimony acetate to 10mL of octadecene, then add 1ml of oleic acid, pass through argon protection gas, control the temperature at 70°C, and stir rapidly for 10 minutes to make the metal salt completely Dissolving to obtain a metal salt solution;

[0035] (2) Add 12ml of 1-dodecanethiol to the above metal salt solution, stir for 10 minutes to make it completely complex with the metal ion, then add 1mL of 1M elemental sulfur octadecene solution, heat to the set temperature of 120°C and react 60s;

[0036] (3) After the reaction is over, cool to room temperature, add a large amount of methanol to clean the copper antimony sulfur nanocrystals obtained by the reaction, and then dissolve the copper antimony sulfur nanocrystals into the n-hexane solution to obtain the n-hexane of the copper antimony sulfur n...

Embodiment 3

[0039] A method for preparing a size-controllable copper antimony sulfur nanocrystalline material, comprising the steps of:

[0040] (1) Add 1mmol of copper acetate and 1mmol of antimony acetate to 10mL of octadecene, then add 1ml of oleic acid, pass through argon protection gas, control the temperature at 80°C, and stir for 15 minutes to make the metal salt completely Dissolving to obtain a metal salt solution;

[0041] (2) Add 6ml of 1-dodecanethiol to the above metal salt solution, stir for 10 minutes to make it fully complex with metal ions, then add 1mL of 1M octadecene solution of elemental sulfur, heat to the set temperature of 150°C and react 120s;

[0042] (3) After the reaction is over, cool to room temperature, add a large amount of methanol to clean the copper antimony sulfur nanocrystals obtained by the reaction, and then dissolve the copper antimony sulfur nanocrystals into the n-hexane solution to obtain the n-hexane of the copper antimony sulfur nanocrystals. ...

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Abstract

The present invention belongs to the nano material nanometer technical field, and particularly relates to a size-controlled copper antimony sulfur nano crystal material and a preparation method thereof, the preparation method includes the following steps: first, adding copper acetate and antimony acetate into octadecene, adding oleic acid, introducing argon shielding gas, controlling temperature and fast mixing to completely dissolve metal salts to obtain a metal salt solution; then adding the metal salt solution into 1-dodecanethiol, stirring for complete complexing with metal ions, then adding elemental sulfur octadecene solution, heating to set temperature for reaction; after the reaction, cooling to room temperature, adding a lot of methanol to wash copper antimony sulfur nano crystal obtained by the reaction, and taking the copper antimony sulfur nano crystal to dissolve into a n-hexane solution to obtain a copper antimony sulfur nano crystal n-hexane solution. Through control of the 1-dodecanethiol content, reaction temperature and reaction time, copper antimony sulfur (Cu12Sb4S13) nano crystal materials with different sizes can be prepared.

Description

technical field [0001] The invention belongs to the field of nanomaterials and nanotechnology, and in particular relates to a size-controllable copper-antimony-sulfur nanocrystal material and a preparation method thereof. Background technique [0002] Semiconductor nanocrystals are crystalline particles with a size between 1-10 nm. These particle sizes are usually smaller than the Bohr radius of charge carriers, so the electronic energy levels of these semiconductor nanocrystals are affected by size changes due to quantum confinement factors, and these semiconductor nanocrystals are called quantum dots. II-VI, III-V, IV-VI and IV semiconductors are usually prepared as semiconductor quantum dot materials, which exhibit unique properties different from intrinsic semiconductors. In the past few decades, semiconductor quantum dots have been intensively studied, and their unique properties have been used in many new nanodevices, such as light-emitting diodes, field-effect transi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C30B7/14C30B29/46B82Y30/00B82Y40/00
Inventor 刘曰利陈克强陈文周静周鹏王琳琳
Owner WUHAN UNIV OF TECH