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Method for preparing three-dimensional hollow structure molybdenum sulfide on basis of upconversion nano-particles

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

Active Publication Date: 2019-09-20
NANJING UNIV OF TECH
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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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  • Method for preparing three-dimensional hollow structure molybdenum sulfide on basis of upconversion nano-particles
  • Method for preparing three-dimensional hollow structure molybdenum sulfide on basis of upconversion nano-particles
  • Method for preparing three-dimensional hollow structure molybdenum sulfide on basis of upconversion nano-particles

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Experimental program
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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 three-dimensional hollow structure molybdenum sulfide on the basis of upconversion nano-particles. The method specifically comprises the following steps: firstly, preparing upconversion nano-particles which are regular in morphology and uniform in size distribution; uniformly dispersing the upconversion nano-particles of which ligand is removed into a water solution; adding ethylene diamine tetraacetic acid, sodium fluoride and ammonium tetrathiomolybdate into the solution, and carrying out stirring till uniformity; transferring the mixed liquid into a reaction kettle, carrying out a reaction for 12 hours at 220 DEG C, and cooling the mixed liquid to the room temperature so as to finally obtain an upconversion granular @MoS2 composite material; and at the room temperature, etching the upconversion nano-particles by using diluted hydrochloric acid, so as to obtain MoS2 of a three-dimensional hollow structure. The method has the characteristics of being gentle in reaction condition, convenient to operate, low in equipment requirement, low in raw material price, controllable in product morphology, high in yield and easy in large-scale preparation, and has wide application prospects in the field of preparation of three-dimensional structure transition metal sulfide two-dimensional materials.

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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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 UNIV OF TECH
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