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Method for preparing two-dimensional nanosheets by microwave-assisted liquid phase stripping of layered material

A layered material, liquid phase exfoliation technology, applied in the direction of nanotechnology, nanotechnology, nanotechnology, etc. for materials and surface science, can solve the problems of nanosheet size reduction, high operation risk, and long time consumption, etc., to achieve The effect of small peeling size reduction, high chemical stability, and high peeling rate

Active Publication Date: 2019-01-15
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the ion pre-intercalation / exchange-assisted method, due to the introduction of the "pre-expansion" mechanism, makes the yield of nanosheets higher, but the ion intercalation / exchange is only suitable for some layered materials, and the intercalation media selected are mostly Active alkali metal elements such as lithium, sodium, and potassium are highly dangerous and time-consuming to operate (Nanoscale 2014, 6, 12458-12462)
Mechanical force assistance, such as ultrasonic-assisted liquid phase exfoliation, is currently the most widely used liquid phase exfoliation method, but due to continuous ultrasonic action, the size of the obtained nanosheets is severely reduced, and structural defects are easily introduced, and the proportion of single-layer nanosheets is low (Science 2011, 331, 568-571)

Method used

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  • Method for preparing two-dimensional nanosheets by microwave-assisted liquid phase stripping of layered material
  • Method for preparing two-dimensional nanosheets by microwave-assisted liquid phase stripping of layered material
  • Method for preparing two-dimensional nanosheets by microwave-assisted liquid phase stripping of layered material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0064] Preparation of h-BN nanosheets

[0065] Mix 10 mg of h-BN precursor powder with 0.3 mL of BMIMPF 6 Mix in an agate mortar, wet grind for 3min; then add 2.7mL of BMIMPF 6 Wash and transfer the wet grinding mixture to a soluble polytetrafluoroethylene (PFA) lined tube, and then place it in a microwave reaction tube. The final mixture volume is 3 mL; add matching A magnetic stirrer was placed into a microwave reaction device (Discover SP ring-focused single-mode microwave synthesis system produced by CEM, USA), the microwave parameters were set to 30W / 30min, high-speed stirring, and the upper temperature limit was set to 170°C. After microwave irradiation, dilute the mixture to 6mL with dimethyl sulfoxide (DMSO), filter with glass sand core filter, adopt polytetrafluoroethylene (PTFE) filter membrane, and use 50mL of absolute ethanol (this implementation Example and the ethanol in the following examples are absolute ethanol) to rinse the microwave reaction tube and the f...

Embodiment 2

[0067] Preparation of h-BN nanosheets

[0068] Mix 10 mg of h-BN precursor powder and 0.3 mL of DMF in an agate mortar, and wet-mill for 3 min; then wash the wet-milled mixture with 2.7 mL of DMF and transfer it to a microwave reaction tube, and the final volume of the mixture is 3 mL; Add a matching magnetic stirrer into the microwave reaction tube, and place it into a microwave reaction device (Discover SP ring-focused single-mode microwave synthesis system produced by CEM, USA). The microwave parameters are set to 120W / 45min, the Power Max function is turned on, and the high-speed Stir and set the upper temperature limit to 95 °C. After microwave irradiation, dilute the mixture to 6mL with dimethyl sulfoxide (DMSO), filter with a glass sand core filter, and use a polytetrafluoroethylene (PTFE) filter membrane, rinse the microwave reaction tube with 50mL of ethanol during the suction filtration , filter cup; soak the obtained filter membrane in a beaker filled with 10mL eth...

Embodiment 3

[0073] Prepare g-C 3 N 4 Nanosheets

[0074] 10mg of g-C 3 N 4 Precursor powder with 0.3 mL of HMIMBF 4 Mix in an agate mortar, wet grind for 3min; then add 2.7mL of HMIMBF 4 Wash and transfer the wet grinding mixture to a soluble polytetrafluoroethylene (PFA) lined tube, and then place it in a microwave reaction tube. The final volume of the mixture is 3 mL; add matching A magnetic stirrer was placed into a microwave reaction device (Discover SP ring-focused single-mode microwave synthesis system produced by CEM, USA), the microwave parameters were set to 30W / 30min, high-speed stirring, and the upper temperature limit was set to 170°C. After microwave irradiation, dilute the mixture to 6mL with dimethyl sulfoxide (DMSO), filter with a glass sand core filter, and use a polytetrafluoroethylene (PTFE) filter membrane, rinse the microwave reaction tube with 50mL of ethanol during the suction filtration , filter cup; soak the obtained filter membrane in a beaker filled with ...

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Abstract

The invention discloses a method for preparing two-dimensional nanosheets by microwave-assisted liquid phase stripping of a layered material. The method comprises the following specific steps: 1) carrying out wet grinding of precursor powder of the layered material with a liquid medium in a mortar; 2) washing the wet-ground mixture with a same liquid medium and transferring into a microwave reaction tube; 3) placing the microwave reaction tube into a microwave reaction device, and carrying out microwave irradiation; 4) after microwave irradiation, washing and filtering the microwave mixture, and collecting a filter membrane; 5) carrying out ultrasonic dispersion of the obtained filter membrane in an organic solvent, and carrying out centrifugal separation, wherein a supernatant is a nanosheet dispersion liquid, and a precipitate is a separated unpeeled phase; and 6) filtering the obtained nanosheet dispersion liquid, collecting a filter membrane, and carrying out vacuum drying to obtain the nanosheet powder. The method is universal, fast and efficient in peeling various layered materials, and the prepared nanosheets are ultra-thin, large in size, small in peeling size reduction andhigh in chemical stability, and have broad application prospects in basic scientific researches, electronics, catalysis, energy, sensing and other hot fields.

Description

technical field [0001] The invention belongs to the field of nanomaterial preparation, and in particular relates to a general microwave-assisted liquid-phase exfoliation layered material to realize rapid and efficient preparation of single-layer / few-layer, large-scale, and high-chemical-stability two-dimensional nanosheets. Background technique [0002] Two-dimensional nanosheets refer to sheet-like nanomaterials with a lateral dimension of hundreds of nanometers to several micrometers and a thickness of only a few or even a single atomic layer. Since Novoselov and Geim et al. glued graphene from graphite with transparent glue in 2004, two-dimensional materials have large specific surface area and many nano-effects due to their atomic-level thickness and large horizontal / longitudinal size ratio. Excellent electrical, optical, magnetic, and mechanical properties have broad application prospects in the fields of catalysis, energy, sensing, and electronics, and provide rich res...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/06C01B21/082C01B19/04C01B21/064C01B35/14C01G23/00C01G25/00C01G31/02C01G35/00C01G39/02C01G39/06C01G41/00C01G41/02C01G45/02B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00C01B19/007C01B21/0605C01B21/064C01B35/14C01G23/007C01G25/00C01G31/02C01G35/00C01G39/02C01G39/06C01G41/00C01G41/02C01G45/02C01P2002/82C01P2004/04C01P2004/20C01P2004/62C01P2004/64Y02P20/54
Inventor 周涵吴伟许军谢培文陆云博范同祥
Owner SHANGHAI JIAO TONG UNIV
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