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A method for one-step hydrothermal preparation of molybdenum disulfide quantum dots using sulfur as a sulfur source

A technology of molybdenum disulfide and quantum dots, which is applied in the field of nanomaterials, can solve the problems of difficult sulfur and limited application, and achieves the effects of low preparation cost, reduced synthesis difficulty and danger, and stable performance.

Active Publication Date: 2021-01-26
FUDAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The sulfur sources commonly used in the current hydrothermal method are mainly cysteine, thiourea, sodium sulfide, dibenzyl disulfide, etc., and the synthesis method using sulfur as the sulfur source has not been reported, mainly because sulfur is insoluble. water, which greatly limits its application in hydrothermal synthesis

Method used

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  • A method for one-step hydrothermal preparation of molybdenum disulfide quantum dots using sulfur as a sulfur source
  • A method for one-step hydrothermal preparation of molybdenum disulfide quantum dots using sulfur as a sulfur source
  • A method for one-step hydrothermal preparation of molybdenum disulfide quantum dots using sulfur as a sulfur source

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Experimental program
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Embodiment 1

[0022] Dissolve 96 mg of sulfur in 10 mL of 50% hydrazine hydrate and stir at room temperature in the dark until the sulfur powder is completely dissolved to obtain 0.3 M S-N 2 h 4 ·H 2 O (concentration is calculated based on the content of sulfur element). Then 22 mM sodium molybdate dihydrate (Na 2 MoO 4 ·H 2 O) Place in ultrapure water, add 44 mM S-N 2 h 4 ·H 2 O, followed by ultrasonication for 10 min, placed in a reactor at 200 °C for 8 h. like figure 1 and figure 2 As shown, the optimal excitation and emission wavelengths of the synthesized molybdenum disulfide quantum dots are 362 nm and 445 nm, respectively, and the average particle size of the molybdenum disulfide quantum dots synthesized by this method is below 5 nm.

Embodiment 2

[0024] Dissolve 96 mg of sulfur in 10 mL of 50% hydrazine hydrate, and stir at room temperature in the dark until the sulfur powder is completely dissolved to obtain 0.3 M S-N 2 h 4 ·H 2 O (concentration is calculated based on the content of sulfur element). Then 30 mM ammonium molybdate ((NH 4 ) 2 MoO 4 ) in ultrapure water, add 60 mM S-N 2 h 4 ·H 2 O, followed by ultrasonication for 5 min, placed in a reaction kettle at 200 °C for 4 h. like image 3 and Figure 4 As shown, the molybdenum disulfide quantum dots synthesized by this method have the property of tunable fluorescence emission, and can fluoresce under the excitation of 290 nm to 430 nm light, and the maximum excitation and emission wavelengths of the fluorescence are 350 nm and 454 nm, respectively.

Embodiment 3

[0026] Dissolve 96 mg of sulfur in 5.88 mL of 85% hydrazine hydrate, and stir at room temperature in the dark until the sulfur powder is completely dissolved to obtain 0.5 M S-N 2 h 4 ·H 2 O (concentration is calculated based on the content of sulfur element). Then 30 mM ammonium dimolybdate ((NH 4 ) 2 Mo 2 o 7 ) in ultrapure water, add 75 mM S-N 2 h 4 ·H 2 O, followed by ultrasonication for 10 min, placed in a reactor at 220 °C for 4 h. like Figure 5 and Figure 6 As shown, the fluorescence maximum excitation and emission wavelengths of molybdenum disulfide quantum dots synthesized by this method are 360 ​​nm and 460 nm, respectively, and it has a significant ultraviolet absorption peak at 228 nm, and an inconspicuous ultraviolet absorption peak at 292 nm. UV absorption peak.

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Abstract

The invention belongs to the technical field of nanometer materials, and specifically relates to a method for preparing molybdenum disulfide quantum dots in one step by hydrothermally using sulfur as a sulfur source. The method of the present invention comprises: preparation of sulfur source: dissolving sulfur in hydrazine hydrate, stirring at room temperature in the dark until the sulfur powder is completely dissolved, and obtaining sulfur-hydrazine hydrate complex; dissolving molybdenum source in pure water, stirring and mixing Evenly; Obtain molybdenum source solution; Add sulfur-hydrazine hydrate complex in the molybdenum source solution, control the final concentration of sulfur source to be 40-75mM, and the final concentration of molybdenum source is 20-35mM; Mix well, then mixed solution is transferred to In a hydrothermal reaction kettle, conduct a hydrothermal reaction at 180°C-220°C for 2-18 hours, wait for it to cool down to room temperature naturally, and collect the filtrate to obtain molybdenum disulfide quantum dots. The molybdenum disulfide quantum dots prepared by the present invention have the advantages of low preparation cost, stable performance, non-toxicity, etc., and the average particle size is below 5 nm, which can be applied to environmental analysis, biochemical analysis, food safety, optical imaging, biomarkers, chemical sensors and other fields.

Description

technical field [0001] The invention belongs to the technical field of nanometer materials, and in particular relates to a preparation method of molybdenum disulfide quantum dots. Background technique [0002] Molybdenum disulfide (MoS 2 ) has a layered structure of graphene-like materials, which are easily peeled off due to the relatively weak van der Waals force between layers. Its unique mechanical properties, electrical properties, chemical properties and optical properties make it widely used in supercapacitors, batteries, catalysts, etc. When MoS 2 When the size is less than 10nm, due to the quantum confinement effect, molybdenum disulfide quantum dots (MoS 2 QDs) exhibit unique optical properties such as photoluminescence, photochemical stability, single excitation / multiple emission, and size-dependent fluorescence emission, and are widely used in bioimaging and biomedicine. [0003] MoS 2 QDs include top-down (exfoliation by large-sized MoS2) and bottom-up (usin...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/67C01G39/06B82Y20/00B82Y40/00
CPCB82Y20/00B82Y40/00C01G39/06C01P2004/04C01P2004/64C09K11/671
Inventor 易涛钟亚平
Owner FUDAN UNIV
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