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Hexagonal boron nitride nano-sheet with controllable layer number, and preparation method thereof

A technology of hexagonal boron nitride and nanosheets, which is applied in chemical instruments and methods, nitrogen compounds, nanotechnology, etc., can solve the problems of polluting the environment, difficult to control the reaction process, and expensive metal substrates, and achieve simple process and high production efficiency. High rate and good reproducibility

Active Publication Date: 2018-02-13
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method has the disadvantages that the reaction process is difficult to control, the price of metal substrates (such as Pt, Rh, Pd, Ru, etc.) is relatively expensive, the toxicity of transition metals and their salts is relatively large, or the environment is seriously polluted.

Method used

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  • Hexagonal boron nitride nano-sheet with controllable layer number, and preparation method thereof
  • Hexagonal boron nitride nano-sheet with controllable layer number, and preparation method thereof
  • Hexagonal boron nitride nano-sheet with controllable layer number, and preparation method thereof

Examples

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Embodiment 1

[0026] A hexagonal boron nitride nanosheet with a controllable layer number is prepared by the following method:

[0027] (1) Preparation of boron precursors containing calcium ions: add 0.1mol boric acid and 0.1mol concentrated ammonia water (about 7.5ml) to 10ml of deionized water in sequence, place them in a constant temperature water bath at 80°C for magnetic stirring, and then add 10 ml of calcium chloride solution with a concentration of 0.1 mol / L was added dropwise, stirred at a constant temperature for 0.5 h, and then placed in an oven at 110° C. for heat treatment for 12 h to obtain a boron precursor containing calcium ions.

[0028] (2) Preparation of hexagonal boron nitride nanosheets: Place the boron precursor containing calcium ions in step (1) in a vacuum tube furnace, and heat up at a rate of 5°C / min in an ammonia gas atmosphere with a flow rate of 60ml / min. The temperature was raised from room temperature to 1400°C, kept for 3 hours, and then naturally cooled t...

Embodiment 2

[0031] A hexagonal boron nitride nanosheet with a controllable layer number is prepared by the following method:

[0032] (1) Preparation of boron precursors containing calcium ions: add 0.1mol boric acid and 0.4mol concentrated ammonia water (about 30ml) to 10ml deionized water successively, place them in a constant temperature water bath at 60°C for magnetic stirring, and then gradually add 10 ml of calcium nitrate solution with a concentration of 0.05 mol / L was added dropwise, stirred at constant temperature for 2 hours, and then placed in an oven at 110° C. for heat treatment for 6 hours to obtain a boron precursor containing calcium ions.

[0033] (2) Preparation of hexagonal boron nitride nanosheets: Place the boron precursor containing calcium ions in step (1) in a vacuum tube furnace, and heat up at a rate of 20°C / min in an ammonia gas atmosphere with a flow rate of 200ml / min. The temperature was raised from room temperature to 1350°C, kept for 1 hour, and then natural...

Embodiment 3

[0036] A hexagonal boron nitride nanosheet with a controllable layer number is prepared by the following method:

[0037] (1) Preparation of boron precursors containing calcium ions: add 0.1mol ammonium pentaborate and 0.4mol concentrated ammonia water (about 30ml) to 10ml of deionized water in sequence, place them in a constant temperature water bath at 70°C for magnetic stirring, and then add 10 ml of calcium chloride solution with a concentration of 0.1 mol / L was added dropwise, stirred at constant temperature for 1.5 h, and then placed in a 120°C oven for heat treatment for 12 h to obtain a boron precursor containing calcium ions.

[0038] (2) Preparation of hexagonal boron nitride nanosheets: Place the boron precursor containing calcium ions in step (1) in a vacuum tube furnace, and heat up at a rate of 10°C / min in an ammonia gas atmosphere with a flow rate of 100ml / min. The temperature was raised from room temperature to 1450°C, kept for 3 hours, and then naturally coole...

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Abstract

The invention belongs to the field of inorganic nanometer materials, and particularly relates to a hexagonal boron nitride nano-sheet with controllable layer number, and a preparation method thereof.The method comprises the following steps: sequentially adding a boron source and ammonia water into deionized water, putting into a constant-temperature water bath pot, dropwise adding calcium salt under the magnetic stirring condition, stirring at constant temperature, and performing heat treatment to obtain a boron precursor containing calcium ions; putting the precursor into a vacuum tubular furnace, heating to a certain temperature under the atmosphere of ammonia gas, performing heat treatment reaction, and naturally cooling to room temperature to obtain the hexagonal boron nitride nano-sheet with controllable layer number. According to the method, the high-quality hexagonal boron nitride nano-sheet with controllable layer number can be catalytically synthesized by using calcium ions,the method has the advantages of simple process, high repeatability, high yield and the like, the requirement on different layer number of the boron nitride nano-sheets in different fields can be met,and application of the boron nitride nano-sheet in the field of a functional composite material can be promoted well.

Description

technical field [0001] The invention belongs to the field of inorganic nanometer materials, and in particular relates to a hexagonal boron nitride nanosheet with a controllable layer number and a preparation method thereof. Background technique [0002] Since K.S. Novoselov and A.K. Geim successfully prepared graphene by micromechanical exfoliation method in 2004, graphene and graphene-like two-dimensional materials have become one of the research hotspots. Several months after the preparation of graphene, the same K.S. Novoselov team used a similar method to successfully strip boron nitride nanosheets from boron nitride crystals (K.S. Novoselov, et al., Two-dimensional atomic crystals, PNAS, 2005, 102:10451-10453). Subsequently, the macroscale and controllable preparation of high-quality boron nitride nanosheets has been one of the research focuses of this material. [0003] Hexagonal boron nitride nanosheets (Boron nitride nanosheets, BNNSs), is a two-dimensional crystal...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/064B82Y40/00
CPCC01B21/064C01P2002/72C01P2004/03C01P2004/04C01P2004/62
Inventor 傅正义王恒解晶晶平航王为民王皓
Owner WUHAN UNIV OF TECH
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