Method for preparing quantum dot of transitional metal chalcogenide compound

A transition metal chalcogenide and compound technology, which is applied in the field of colloidal chemical preparation of nanomaterials, can solve the problems of high reaction yield, short reaction time, slow reaction speed, etc., and achieves high reaction yield and poor generality. , the effect of short response time

Active Publication Date: 2015-12-09
NANJING UNIV OF POSTS & TELECOMM
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0008] The invention provides a colloidal chemical method for preparing transition metal chalcogenide quantum dots. The method is versatile and can be used for compounds formed by various transition metals such as molybdenum and tungsten and various chalcogen elements such as sulfur, selenium and tellurium. The preparation of quantum dots has short reaction time and high reaction yield, which can effectively solve the problems of poor versatility, slow reaction speed, low reaction efficiency and complicated preparation process of existing preparation methods.

Method used

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  • Method for preparing quantum dot of transitional metal chalcogenide compound
  • Method for preparing quantum dot of transitional metal chalcogenide compound
  • Method for preparing quantum dot of transitional metal chalcogenide compound

Examples

Experimental program
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Effect test

Embodiment 1

[0029] (a) Preparation of metal source reaction system

[0030] Add 105.6 mg of molybdenum hexacarbonyl powder and 309.3 mg of trioctylphosphine oxide powder into a 50 ml three-necked round bottom flask, heat to 50 ° C to dissolve, then add 5 mL of octadecene solution, repeat vacuuming-argon three times, Under the protection of high-purity argon, heat to 300°C.

[0031] (b) Preparation of non-metal source solution

[0032] Add 63.2 mg of selenium powder into the reaction bottle, add 714 μL of trioctylphosphine, ultrasonically dissolve, then add 1 mL of octadecene solution, vacuumize, and fill with argon.

[0033] (c) hot injection

[0034]After part (a) is heated to 300°C, all the selenium source solution prepared in (b) is injected into the molybdenum source reaction system, and kept at 300°C for 2 hours.

[0035] (d) centrifugal purification

[0036] Measure a certain amount of methanol, make a suspension with the molybdenum selenide quantum dots obtained in (c), centrif...

Embodiment 2

[0039] (a) Preparation of metal source reaction system

[0040] Add 105.6 mg of molybdenum hexacarbonyl powder and 309.3 mg of trioctylphosphine oxide powder into a 50 ml three-necked round bottom flask, heat to 50 ° C to dissolve, then add 5 mL of octadecene solution, repeat vacuuming-argon three times, Under the protection of high-purity argon, it was heated to 320°C.

[0041] (b) Preparation of non-metal source solution

[0042] Add 102.1 mg of tellurium powder and 3.57 mL of trioctylphosphine into the reaction flask, dissolve it by ultrasonic, then add 1 mL of octadecene solution, vacuumize and fill with argon.

[0043] (c) hot injection

[0044] After (a) was heated to 320°C, all the tellurium source solution prepared in (b) was injected into the molybdenum source reaction system, and kept at 320°C for 3 hours to react.

[0045] (d) centrifugal purification

[0046] Measure a certain amount of methanol, make a suspension with the molybdenum telluride quantum dots obta...

Embodiment 3

[0048] (a) Preparation of metal source reaction system

[0049] Add 140.8mg of tungsten hexacarbonyl powder and 309.3mg of trioctylphosphine oxide powder into a 50ml three-neck round bottom flask, heat to 50°C to dissolve, then add 5mL of octadecene solution, repeat vacuuming-argon three times, Under the protection of high-purity argon, heat to 350°C.

[0050] (b) Preparation of non-metal source solution

[0051] Add 63.2 mg of selenium powder into the reaction bottle, add 714 μL of trioctylphosphine, ultrasonically dissolve, then add 1 mL of octadecene solution, vacuumize, and fill with argon.

[0052] (c) hot injection

[0053] After part (a) is heated to 350°C, all the selenium source solution prepared in (b) is injected into the tungsten source reaction system, and kept at 350°C for 1 hour to react.

[0054] (d) centrifugal purification

[0055] Measure a certain amount of methanol, make a suspension with the tungsten selenide quantum dots obtained in (c), centrifuge a...

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Abstract

The invention discloses a method for preparing a quantum dot of a transitional metal chalcogenide compound and belongs to the field of preparing functional nanomaterials by colloidal chemical methods. The method disclosed by the invention comprises the following steps: mixing a metal carbonyl compound and trioctylphosphine oxide, heating and dissolving the mixture as a metal source precusor, by taking octadecene as a reaction solvent, heating the mixture under inert gas protection to reaction temperature, and preparing a metal source reaction system; by taking organic phosphorus as a coorinating solvent, preparing non-metal source sulfur powder, selenium powder or tellurium powder into a precusor solution; injecting the non-metal source solution into the metal source reaction system under inert gas protection and maintaining the reaction temperature and carrying out a heating reaction; and carrying out high speed centrifugal separation, and adding a mixed solution of n-butylamine / n-hexane into the obtained solid product to obtain a quantum dot material of the transitional metal chalcogenide compound in a collide dispersing state. The preparation method for the quantum dot material of the transitional metal chalcogenide compound disclosed by the invention is good in universality, fast in reaction speed, high in reaction yield, simple to operate, mild in reaction condition and easy for large-scaled production.

Description

technical field [0001] The invention relates to a preparation method of quantum dots of transition metal chalcogenides, which belongs to the colloid chemical method preparation technology of nanometer materials. Background technique [0002] Two-dimensional transition metal dichalcogenides (TMDs) refer to compounds with X-M-X sandwich structures formed by transition metal elements (M) and chalcogen nonmetal elements (X), such as MoS 2 、MoSe 2 、MoTe 2 、WS 2 、WSe 2 , WTe 2 、TiS 2 、TaS 2 , VS 2 Wait. Similar to graphene, two-dimensional transition metal chalcogenides have a two-dimensional layered structure, the metal atoms in the layer are chemically bonded to the chalcogen nonmetal atoms, and there is a weak van der Waals force between the layers. The material contains no carbon atoms, hence the name "inorganic graphene". As a typical representative of transition metal chalcogenide nanomaterials, molybdenum disulfide is a layered compound with an S-Mo-S sandwich san...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B19/04B82Y30/00
Inventor 宇文力辉汪联辉周佳佳邓尚平冯伟杨向荣张玉倩张琦
Owner NANJING UNIV OF POSTS & TELECOMM
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