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Preparation method of Nb3O7F nanoarray/graphene heterojunction composite material

A composite material and nanoarray technology, applied in nanotechnology, nanotechnology, chemical instruments and methods, etc., can solve the problems of poor heterojunction uniformity, difficult heterojunction growth, and difficult covalent surface, etc. Conditions are easy to control, good photoelectric performance, good effect

Active Publication Date: 2017-12-01
CHINA UNIV OF MINING & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The object of the present invention is to provide a kind of Nb 3 o 7 F nanoarray / graphene heterojunction preparation method to solve the problems existing in the prior art, such as when directly using graphene as a substrate, it is difficult to stably disperse in aqueous solution, the surface is not easy to be covalent, and the growth of heterojunction is difficult However, when graphene oxide is directly used as the substrate, the degree of reduction is low, the performance cannot be improved, and the uniformity of the heterojunction is not good.

Method used

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  • Preparation method of Nb3O7F nanoarray/graphene heterojunction composite material
  • Preparation method of Nb3O7F nanoarray/graphene heterojunction composite material
  • Preparation method of Nb3O7F nanoarray/graphene heterojunction composite material

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Embodiment 1

[0060] (1) Weigh 16.9mg graphene and add it to a plastic beaker, add 40mL H 2 O, be mixed with graphene aqueous solution, carry out ultrasonic stripping after stirring, make graphene form uniform dispersion liquid;

[0061] (2) Then add 0.5mL HF to the above-mentioned dispersion liquid, stir and supplement with ultrasound for 6h, so that the surface of the exfoliated graphene is fully etched to form a carbon-fluorine bond;

[0062] (3) 1.623g NbCl 5 Add to the above solution, stir magnetically for 30min at room temperature, and add 0.65mL HF and 40mL H 2 O, stir for 30s;

[0063] (4) Transfer the above solution to a 100mL polytetrafluoroethylene liner, then put the polytetrafluoroethylene liner into a micro-reactor and seal it; put the reactor into an oven, and heat the reaction at 120°C for 24h , and then cooled with the furnace;

[0064] (5) Centrifuge the precipitate, wash it with normal temperature deionized water for 5 times, and wash it with absolute ethanol for 3 ti...

Embodiment 2

[0067] (1) Weigh 16.9mg of graphene into the beaker, add 40mL of H 2 O, prepared into a graphene aqueous solution, then added 2g of P123, stirred in a water bath at 70°C for 30min, to completely dissolve the P123; then carried out ultrasonic stripping to form a uniform dispersion of graphene;

[0068] (2) Then add 0.5mL HF to the above-mentioned dispersion liquid, stir and supplement with ultrasound for 6h, so that the surface of the exfoliated graphene is fully etched to form a carbon-fluorine bond;

[0069] (3) Weigh 1.623g NbCl 5 Added to the above solution, magnetically stirred at room temperature for 1 h; and added 0.65mL HF and 40mL H 2 O, stir for 30s;

[0070] (4) Transfer the stirred mixed solution to a 100mL polytetrafluoroethylene lining, then put the polytetrafluoroethylene lining into a micro-reactor and seal it well; Heating and reacting for 24h, then cooling with the furnace;

[0071] (5) Centrifuge the precipitate, wash it 5 times with deionized water, and ...

Embodiment 3

[0074] (1) Weigh 16.9mg of graphene into the beaker, add 40mL of H 2 0, be formulated with graphene aqueous solution, add 2g citric acid then, stir 30min in water bath at 70 ℃, make citric acid dissolve completely; Then carry out ultrasonic exfoliation, make graphene form uniform dispersion liquid;

[0075] (2) Then add 0.5mL HF to the above-mentioned dispersion liquid, stir and supplement with ultrasonic 5h, make the graphene surface of exfoliation be fully etched, form carbon-fluorine bond;

[0076] (3) Weigh 1.623g NbCl 5 Added to the above solution, magnetically stirred at room temperature for 1 h; and added 0.65mL HF and 40mL H 2 O, stir for 30s;

[0077] (4) Transfer the stirred mixed solution to a 100mL polytetrafluoroethylene lining, then put the polytetrafluoroethylene lining into a micro-reactor and seal it well; Heating and reacting for 24h, then cooling with the furnace;

[0078] (5) Centrifuge the precipitate, wash it 5 times with deionized water, and wash it ...

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Abstract

The invention discloses a preparation method of an Nb3O7F nanoarray / graphene heterojunction composite material. The preparation method comprises the following steps: preparing a graphene water solution, stirring, and carrying out ultrasonic stripping until graphene forms uniform dispersion liquid; adding hydrofluoric acid into the dispersion liquid, simultaneously carrying out stirring and ultrasonic treatment so as to adequately etch the surface of stripped graphene to form a carbon-fluorine bond; weighing NbCl5 powder, adding the NbCl5 powder into the solution, adequately stirring, adding hydrofluoric acid, and continuing to adequately stir; transferring the solution into a reaction kettle with a Teflon liner, and carrying out hydrothermal reaction; after the reaction is finished, carrying out centrifugal separation on a product, washing by virtue of deionized water and absolute ethyl alcohol, and drying in a drying oven; and carrying out thermal treatment on the dried product to remove organic matters, so as to finally obtain the Nb3O7F nanoarray / graphene heterojunction composite material. The preparation method has the beneficial effects that the process is simple, the operation conditions are easily controlled, and the low-temperature preparation of the graphene heterojunction material is realized.

Description

technical field [0001] The invention relates to a preparation method of a graphene-based heterojunction material, specifically a kind of Nb 3 o 7 Preparation method of F nanoarray / graphene heterojunction material. Background technique [0002] In recent years, the rapid development of new semiconductor photocatalytic materials has provided a new option for the degradation of organic pollutants; at the same time, some new semiconductor photocatalytic materials can break through the traditional TiO 2 The limitations of photocatalytic materials, especially the high carrier recombination rate and low spectral response, have attracted extensive attention from scholars. Recently, Nb 3 o 7 F due to TiO 2 The electronic structure and energy band structure are similar, good crystallinity, single phase, excellent chemical inertness, strong anti-oxidation ability, high photocatalytic activity, low carrier recombination rate, etc., are considered to be a promising optical catalyti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/06C01B32/194C01G33/00B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00C01G33/00B01J27/06C01P2004/64C01P2004/62C01P2004/80C01P2002/72C01P2004/04C01P2004/03B01J35/39
Inventor 黄飞李臻闫爱华柴夏辉张敏彭柏鑫冯昊赵辉
Owner CHINA UNIV OF MINING & TECH
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