Method for large-scale preparation of graphene and two-dimensional boron nitride crystal materials

A technology of crystal materials and two-dimensional crystals, applied in the direction of graphene, chemical instruments and methods, nitrogen compounds, etc., can solve problems such as difficult preparation of two-dimensional boron nitride nanomaterials, and achieve high product purity, complete structure, and low price cheap effect

Active Publication Date: 2014-02-12
中科榆林能源技术运营有限责任公司
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  • Abstract
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  • Application Information

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Problems solved by technology

Although the interlayer force of hexagonal boron nitride is much weaker than that within the layer, it is stronger than that between graphite layers. It is difficult to prepare two-dimensional boron nitride nanomaterials with atomic thickness.
However, there is currently no general method that can provide a low-cost exfoliation of graphite and boron nitride to prepare high-quality graphene and two-dimensional boron nitride crystal materials.

Method used

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  • Method for large-scale preparation of graphene and two-dimensional boron nitride crystal materials
  • Method for large-scale preparation of graphene and two-dimensional boron nitride crystal materials
  • Method for large-scale preparation of graphene and two-dimensional boron nitride crystal materials

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Weigh 0.1 g of flake graphite and 0.05 g of ammonia borane (NH 3 BH 3 ) in a ball mill jar, and milled on a planetary ball mill at 50°C, the medium balls are steel balls, the mass ratio of balls to materials during the milling process is 50:1, the rotational speed is 200 rpm, and the milling time is 1 hour. The obtained product is fully washed with ethanol, the obtained suspension is filtered, and then dried at 50 degrees to obtain the graphene material. Ethanol was distilled off from the filtrate under reduced pressure to recover white ammonia borane solid.

Embodiment 2

[0034] Weigh 0.1 g of expandable graphite and 0.1 g of ammonia borane (NH 3 BH 3) in a ball mill jar, and milled on a planetary ball mill at room temperature, the medium balls are steel balls, the mass ratio of balls to materials during the milling process is 500:1, the rotational speed is 150 rpm, and the milling time is 4 hours. The obtained product is fully washed with methanol, and the obtained suspension is filtered and then dried at 60 degrees to obtain a graphene material, and its transmission electron microscope photo is as follows: figure 1 shown. The filtrate is distilled off under reduced pressure to remove methanol, and the white ammonia borane solid can be recovered.

Embodiment 3

[0036] Weigh 0.1 g of expanded graphite and 0.3 g of ammonia borane (NH 3 BH 3 ) in a ball mill jar, and milled on a planetary ball mill at room temperature, the medium balls are steel balls, the mass ratio of balls to materials during the milling process is 200:1, the rotational speed is 150 rpm, and the milling time is 4 hours. The obtained product is fully washed with deionized water, the obtained suspension is filtered, and then dried at 60 degrees to obtain a graphene material. The filtrate is distilled off under reduced pressure to remove deionized water, and the white ammonia borane solid can be recovered. Raman spectroscopy results show that the obtained graphene material has a wavenumber of 2696cm -1 The G' peak, the symmetrical peak shape shows that the obtained graphene is of good quality. High-resolution transmission electron microscopy test results show that the obtained graphene has single-layer graphene and multi-layer graphene. The number of multi-layer grap...

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Abstract

The invention relates to a method for large-scale preparation of graphene and two-dimensional boron nitride crystal materials. The method is characterized in that in the presence of NH3BH3 as a ball milling assistant, a solid mixture having a mass ratio of an inorganic layered material to NH3BH3 of 1: 0.5-5 is subjected to ball milling treatment by a mechanical ball milling technology so that high-efficiency peeling on the inorganic layered material such as graphite and hexagonal boron nitride is realized; and the products are washed and filtered for NH3BH3 removal and the filtration products are dried so that the single-layer or multiple-layer graphene and two-dimensional boron nitride crystal materials are obtained. The graphene and two-dimensional boron nitride crystal materials have high purity and complete structures. The method has the advantages of easy acquisition of raw materials, operation simpleness, safety and low cost and is suitable for large-scale preparation of the graphene and two-dimensional boron nitride crystal materials.

Description

technical field [0001] The invention relates to a preparation method of graphene and two-dimensional boron nitride crystal materials. Specifically, it relates to a method for macro-preparing graphene and two-dimensional boron nitride crystal materials by exfoliating inorganic layered materials by mechanical ball milling. Background technique [0002] Two-dimensional crystals have infinitely repeating periodic structures in the plane, but only have nanoscale in the direction perpendicular to the plane, and can be regarded as nanomaterials with macroscopic dimensions, which have many unique properties. Since Geim of the University of Manchester first prepared stable single-layer graphene from highly oriented pyrolysis graphite in 2004, the research on two-dimensional crystals has aroused great interest of scientists in different fields such as physics, chemistry, and materials. Graphene is made of sp 2 A two-dimensional crystal material with a monoatomic layer formed by hybr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04C01B21/064C01B32/19
Inventor 陈萍柳林熊智涛胡大强
Owner 中科榆林能源技术运营有限责任公司
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