Method of preparing superfine monolayer transition metal compound quantum dot solution

A quantum dot solution, transition metal technology, applied in tungsten compounds, niobium compounds, chemical instruments and methods, etc., can solve problems such as poor crystallinity, and achieve the effects of good repeatability, easy industrial production, and short reaction cycles

Inactive Publication Date: 2014-06-25
NANJING UNIV OF AERONAUTICS & ASTRONAUTICS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Currently, only a few methods have prepared smaller MoS 2 Quantum dots, such as Václav Stengl et al. using ultrasonic treatment, refluxing MoS at the boiling point of organic solvents 2 Obtained MoS 2 Quantum dots are around 40 nm, but the resulting MoS 2 The thickness and size distribution of is a broad Gaussian distribution; Hongtao Yu et al. used molybdenum hexacarbonyl and S powder to synthesize MoS with good dispersion less than 5nm in trioctylphosphine and octadecene solution. 2 Quantum dots, MoS 2 The size of quantum dots can be controlled by the reaction temperature, but the MoS prepared by this synthesis method 2 The crystallinity...

Method used

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  • Method of preparing superfine monolayer transition metal compound quantum dot solution
  • Method of preparing superfine monolayer transition metal compound quantum dot solution
  • Method of preparing superfine monolayer transition metal compound quantum dot solution

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Example 1 Ultra-small single-layer MoS 2 Preparation of quantum dot solution

[0025] (1) Mix 1.6M n-butyllithium solution and 2H-MoS 2 The solution was added to the reaction kettle liner in the argon-filled glove box and mixed, in which the n-butyllithium solution was mixed with 2H-MoS 2 The molar ratio is 3:1, placed in an incubator at 90 O After reacting at C for 12 hours, wash the incompletely reacted n-butyllithium in the glove box with n-hexane after the end of the reaction to obtain the intermediate product Li n MoS 2， (n is a single MoS 2 The number of Li atoms occupied after the reaction, the value of n will change with the reaction time, reaction temperature, and the mass ratio of the reactants, 0

[0026] (2) Place the intermediate product obtained in step 1 in a vacuum oven for 40 O C, vacuum-dried for 30 min to obtain a dry product weighing 1 g;

[0027] (3) According to the mass volume ratio (g / ml), add 300 ml of deionized water to the dried...

Embodiment 2

[0036] Example 2 Ultra-small single-layer WS 2 Quantum dot solution preparation

[0037] (1) Mix 2.2M n-butyllithium solution and WS 2 The solution was added to the reaction kettle liner in the glove box filled with argon and mixed, wherein the n-butyllithium solution was mixed with WS 2 The molar ratio is 4:1, placed in an incubator at 80 O After 24 hours of insulation reaction at C, wash the incompletely reacted n-butyllithium in the glove box with n-hexane solvent to obtain the intermediate product Li n WS 2 (n is a single layered WS 2 The number of Li atoms occupied after the molecular reaction is completed, the n value will change with the reaction time, reaction temperature, and the mass ratio of the reactant, 0

[0038] (2) Put the intermediate product obtained in step 1 into a vacuum drying oven, 40 O C, vacuum-dried for 30 min to obtain a dry product, weighing 1.1 g of the dry product;

[0039] (3) Add deionized water to the dried product obtained in st...

Embodiment 3

[0041] Example 3 Ultra-small monolayer MoSe 2 Quantum dot solution preparation

[0042] (1) Mix 2.4 M n-butyllithium solution and MoSe 2 The solution was added to the reaction kettle liner in a glove box filled with argon and mixed, in which the n-butyllithium solution was mixed with MoSe 2 The molar ratio is 6:1, placed in an incubator at 90 O After 36 hours of insulation at C, wash the incompletely reacted n-butyllithium in the glove box with n-hexane after the reaction to obtain the intermediate product Li n MoSe 2 (n is a single layered MoSe 2 The number of Li atoms occupied after the molecular reaction is completed, the n value will change with the reaction time, reaction temperature, and the mass ratio of the reactant, 0

[0043] (2) Put the intermediate product obtained in step 1 into a vacuum drying oven, 40 O C, vacuum-dried for 30 min to obtain a dried product, weighing 1.13 g of the dried product;

[0044] (3) Add deionized water to the dried product ...

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Abstract

The invention discloses a method of preparing a superfine monolayer transition metal compound quantum dot solution. The method comprises the following steps: (a) mixing a n-butyllithium solution with a transition metal compound solution to react to obtain an intermediate product, wherein the transition metal compound has the formula of MX2, M is a transition metal element and X is S or Se or Te; (b) drying the intermediate product to obtain a dried product; (c) adding deionized water into the dried product for ultrasonic reaction to obtain an ultrasonic product; (d) centrifuging the ultrasonic product obtained by the step c to obtain the supernate which is the superfine monolayer transition metal compound quantum dot solution. The solution prepared by the invention is uniform in distribution of particle size, has a monolayer structure, and is simple in process equipment, short in reaction period, good in repeatability and easy for industrial production.

Description

technical field [0001] The invention relates to the field of preparation of quantum dots, in particular to a method for preparing an ultra-small single-layer transition metal compound quantum dot solution. Background technique [0002] Transition metal compounds refer to compounds formed by transition group metals and oxygen group nonmetal elements, such as MoS 2 、MoSe 2 、MoTe 2 、WS 2 、WSe 2 , WTe 2 , NbS, etc., which have the same layered structure as graphene, and the layers are combined with weak van der Waals forces. When changing from a bulk to a single-layer 2D structure, there will be a change from indirect band gap to The sudden change of the direct bandgap, the single-layer transition metal compound has a high on-off ratio up to 1X10 8 , electron mobility 200 cm2*V -1 *s -1 , is a very good solid lubricant and catalyst, and the monolayer structure greatly improves its fluorescence effect. The thickness band gap of the transition metal compound compou...

Claims

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Application Information

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IPC IPC(8): C01G39/06C01G41/00C01G33/00C01B19/04C09K11/68C09K11/88
Inventor 曾海波蒋连福
Owner NANJING UNIV OF AERONAUTICS & ASTRONAUTICS
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