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Selenium precursor for preparing metal selenide nanometer material

A technology for metal selenide and nanomaterials, which is applied in the field of preparation of nanomaterials, can solve the problems of poor quality of selenide nanomaterials, harsh experimental conditions and the like, and achieves the effects of low cost, easy storage and transfer, and mild reaction conditions.

Inactive Publication Date: 2015-06-10
SHENZHEN DANBANG INVESTMENT GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, compared with phosphorus-containing organic solvents, there are still various problems in the use of these alternative reagents, such as the poor quality of the prepared selenide nanomaterials and harsh experimental conditions.

Method used

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  • Selenium precursor for preparing metal selenide nanometer material
  • Selenium precursor for preparing metal selenide nanometer material
  • Selenium precursor for preparing metal selenide nanometer material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Step 1: Add 3mL of oleylamine, 3mmol of selenium powder and 1.5mmol of dimethylamine borane complex into a 25mL flask, heat to 130°C while stirring, after five minutes the selenium powder dissolves, and the solution The color changes from colorless to dark brown and then to a colorless and transparent selenium solution. The selenium solution was cooled to 70°C and set aside.

[0043] Step 2: While performing step 1, add 3mmol copper chloride, 1.5mmol zinc chloride, 1.5mmol tin chloride and 10mL oleylamine into a 50mL three-necked flask to form a mixed solution, and place the flask in a standard Under the anhydrous and oxygen-free system (Schlenk system), the mixed solution was dehydrated and deoxygenated at 130° C. for 1 h.

[0044] Step 3: The temperature of the mixed solution after removing water and oxygen is raised to 230° C., and at this temperature, the selenium solution obtained in Step 1 is rapidly injected into the rapidly stirred mixed solution using a syring...

Embodiment 2

[0047] Step 1: Add 1.5mL of oleylamine, 1.5mmol of selenium powder and 0.75mmol of dimethylamine borane complex into a 25mL flask, heat to 120°C while stirring, and the selenium powder will dissolve after five minutes. The color of the solution changed from colorless to dark brown, and then to a colorless and transparent selenium solution. The selenium solution was cooled to 70°C and set aside.

[0048] Step 2: While performing step 1, add 1.5mmol of zinc acetylacetonate, 10mL of octadecene and 3mmol of hard fatty acid into a 50mL three-necked flask to form a mixed solution, and place the flask in a standard anhydrous and oxygen-free system (Schlenk system), at 130° C., remove water and oxygen from the formed mixed solution for 1 h.

[0049] Step 3: The temperature of the mixed solution after removing water and oxygen is raised to 230° C., and at this temperature, the selenium solution obtained in Step 1 is rapidly injected into the rapidly stirred mixed solution using a syri...

Embodiment 3

[0052] Step 1: Add 3mL of oleylamine, 3mmol of selenium powder and 1.5mmol of dimethylamine borane complex into a 25mL flask, heat to 110°C while stirring, after five minutes the selenium powder dissolves, and the solution The color changes from colorless to dark brown and then to a colorless and transparent selenium solution. The selenium solution was cooled to 70°C and set aside.

[0053] Step 2: While performing step 1, add 1.5mmol copper acetylacetonate, 1.5mmol indium chloride and 10mL oleylamine to a 50mL three-necked flask to form a mixed solution, and place the flask in a standard anhydrous and oxygen-free system (Schlenk system), the mixed solution was dehydrated and deoxygenated at 130° C. for 1 h.

[0054] Step 3: The temperature of the mixed solution after removing water and oxygen is raised to 230° C., and at this temperature, the selenium solution obtained in Step 1 is rapidly injected into the rapidly stirred metal precursor using a syringe. Incubate at 210 °C...

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Abstract

The invention discloses a selenium precursor for preparing a metal selenide nanometer material. The selenium precursor is prepared by heating a selenium-containing substance, a phosphorus-free organic solvent and a borane organic solvent, wherein the mole ratio of the borane organic solvent and the selenium-containing substance is higher than 1:1, and the borane organic solvent has reducibility and can be dissolved in the phosphorus-free organic solvent. The selenium precursor disclosed by the invention ensures that the usage of a virulent phosphorus-containing organic solvent which is easy to oxidize is prevented, has the characteristics of high activity and easiness for storage and taking, and can be used for synthesizing any metal selenide nanometer material.

Description

technical field [0001] The invention relates to the preparation of nanometer materials, in particular to a selenium precursor used for preparing metal selenide nanomaterials. Background technique [0002] Since the quantum confinement effect was first mentioned in the 1980s, nanomaterials have become a research hotspot. Among them, chalcogenide semiconductor nanomaterials have excellent electrical and optical properties, and are widely used in photovoltaics, thermoelectrics, biolabels, bioimaging, light-emitting diodes, and solid-state light emitters. At the same time, great progress has been made in the preparation of chalcogenides, especially selenide and telluride semiconductor nanomaterials. The preparation method includes organometallic precursor method, non-organometallic precursor method, unimolecular precursor method, microwave radiation method and the like. Among them, the most successful and commonly used preparation method is the organometallic precursor method....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B19/04B82Y30/00
CPCC01B19/002C01B19/007C01P2002/72C01P2004/04C01P2004/64
Inventor 刘萍
Owner SHENZHEN DANBANG INVESTMENT GROUP