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A method for preparing three-dimensional hollow molybdenum sulfide based on upconversion nanoparticles

A nanoparticle, hollow structure technology, applied in the field of materials chemistry, can solve problems such as harsh synthesis conditions

Active Publication Date: 2022-04-22
NANJING TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method overcomes the problem of harsh synthesis conditions of three-dimensional structure molybdenum sulfide, and the obtained three-dimensional structure molybdenum sulfide has different sizes and shapes according to the selection of templates. At the same time, the synthesis procedure is simple and the conditions are mild, which is suitable for large-scale production

Method used

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  • A method for preparing three-dimensional hollow molybdenum sulfide based on upconversion nanoparticles
  • A method for preparing three-dimensional hollow molybdenum sulfide based on upconversion nanoparticles
  • A method for preparing three-dimensional hollow molybdenum sulfide based on upconversion nanoparticles

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Pre-prepared 0.4mmol NaYF with a length of about 1.5μm 4 : Yb / Er microrods dispersed in 4mL ethanol, take 1mL of the above 0.1mol / L NaYF 4 : Put the ethanol solution of Yb / Er in a 2mL centrifuge tube, put it in a centrifuge and centrifuge at 12000rpm for 1min, disperse the lower sediment in 750μL ethanol for ultrasonication, after the dispersion is even, add 500μL 1mol / L dilute hydrochloric acid for 30s, put it in the centrifuge Centrifuge at 12000rpm for 15min in the machine, pour off the upper solution, disperse the lower precipitate in 750μL ethanol for ultrasonication, add 50μL 1mol / L dilute hydrochloric acid for 10s, and centrifuge at 12000rpm for 15min, and disperse the white precipitate obtained by centrifugation in 0.5mL H 2 Reserved in O. Add 1 mL of 0.2 mol / L NaYF to wash away the oleic acid ligand to 4 mL of 0.04 mmol of disodium edetate aqueous solution and 4 mL of 0.2 mmol of sodium fluoride aqueous solution 4 : The Yb / Er aqueous solution was stirred for ...

Embodiment 2

[0020] Pre-prepared 0.4mmol NaYF with a length of about 400nm 4 : Yb / Er / Gd microrods dispersed in 4mL ethanol, take 1mL above 0.1mol / L NaYF 4 : Put the ethanol solution of Yb / Er in a 2mL centrifuge tube, put it in a centrifuge and centrifuge at 12000rpm for 1min, disperse the lower sediment in 750μL ethanol for ultrasonication, after the dispersion is even, add 500μL 1mol / L dilute hydrochloric acid for 30s, put it in the centrifuge Centrifuge at 12000rpm for 15min in the machine, pour off the upper solution, disperse the lower precipitate in 750μL ethanol for ultrasonication, add 50μL 1mol / L dilute hydrochloric acid for 10s, and centrifuge at 12000rpm for 15min, and disperse the white precipitate obtained by centrifugation in 0.5mL H 2 Reserved in O. Add 1 mL of 0.2 mol / L NaYF to wash away the oleic acid ligand to 4 mL of 0.04 mmol of disodium edetate aqueous solution and 4 mL of 0.2 mmol of sodium fluoride aqueous solution 4 : The Yb / Er / Gd aqueous solution was stirred for 4...

Embodiment 3

[0022] Pre-prepared 0.4mmol NaYF with a length of about 500nm 4 : Yb / Er hexagonal prisms are dispersed in 4mL ethanol, take 1mL of the above 0.1mol / L NaYF 4 : Put the ethanol solution of Yb / Er in a 2mL centrifuge tube, put it in a centrifuge and centrifuge at 12000rpm for 1min, disperse the lower sediment in 750μL ethanol for ultrasonication, after the dispersion is even, add 500μL 1mol / L dilute hydrochloric acid for 30s, put it in the centrifuge Centrifuge at 12000rpm for 15min in the machine, pour off the upper solution, disperse the lower precipitate in 750μL ethanol for ultrasonication, add 50μL 1mol / L dilute hydrochloric acid for 10s, and centrifuge at 12000rpm for 15min, and disperse the white precipitate obtained by centrifugation in 0.5mL H 2 Reserved in O. Add 1 mL of 0.2 mol / L NaYF to wash away the oleic acid ligand to 4 mL of 0.04 mmol of disodium edetate aqueous solution and 4 mL of 0.2 mmol of sodium fluoride aqueous solution 4 : The Yb / Er aqueous solution was s...

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Abstract

The invention discloses a method for preparing molybdenum sulfide with a three-dimensional hollow structure based on upconversion nanoparticles. The specific method includes: first preparing up-conversion nanoparticles with regular shape and uniform size distribution; Sodium and ammonium tetrathiomolybdate, stir until uniform; transfer the mixture to a reaction kettle, react at 220°C for 12 hours, then cool to room temperature, and finally form upconversion particles @MoS 2 Composite material; at room temperature, the upconversion nanoparticles are etched with dilute hydrochloric acid to obtain a three-dimensional hollow structure MoS 2 . This method has the characteristics of mild reaction conditions, convenient operation, low equipment requirements, low raw material cost, controllable product shape, high yield and easy mass production. application prospects.

Description

technical field [0001] The invention belongs to the technical field of material chemistry, in particular to a method for preparing molybdenum sulfide with a three-dimensional hollow structure based on up-conversion nanoparticles Background technique [0002] In recent years, the research on two-dimensional transition metal sulfides has become one of the hot research fields, MoS 2 It is the most representative transition metal sulfide. MoS with three-dimensional structure 2 Compared with its two-dimensional layered structure, it can overcome various problems caused by stacking in practical applications, thereby effectively improving the application effect. [0003] Chemical vapor deposition is a traditional method for synthesizing MoS 2 method, when there is a suitable template in the system, MoS can be 2 Deposition on a template yields a three-dimensional structure, but chemical vapor deposition requires harsh synthesis conditions and specialized equipment, making it dif...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G39/06B82Y40/00
CPCC01G39/06B82Y40/00C01P2004/03C01P2004/04C01P2004/34C01P2004/64C01P2004/61C01P2004/62
Inventor 黄岭高潮韩迎东张坤宋浩
Owner NANJING TECH UNIV
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