Method for preparing macro-quantity hexagonal boron nitride powder through chemical vapor deposition

A chemical vapor deposition, hexagonal boron nitride technology, applied in chemical instruments and methods, inorganic chemistry, nitrogen compounds and other directions, can solve problems such as restricting the development process of boron nitride industrialization, difficulty and other problems, and achieve the promotion of industrialization process, The effect of simple process flow

Active Publication Date: 2018-08-21
SUZHOU INST OF NANO TECH & NANO BIONICS CHINESE ACEDEMY OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Although the existing preparation methods are rich and diverse, due to the limitations of the experiment itself, it is difficult to achieve superiority in terms of large output, high crystallinity, low cost, and environmental friendliness, which are severely restricted by high cost and low efficiency. The industrialization development process of boron nitride

Method used

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  • Method for preparing macro-quantity hexagonal boron nitride powder through chemical vapor deposition
  • Method for preparing macro-quantity hexagonal boron nitride powder through chemical vapor deposition
  • Method for preparing macro-quantity hexagonal boron nitride powder through chemical vapor deposition

Examples

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Embodiment 1

[0059] Example 1: Put B 2 O 3 And MgCl 2 Take 2g B with a molar ratio of 2:3 2 O 3 And 4.1g MgCl 2 Put it in an alumina crucible, then put it in a quartz tube furnace, and pass 200sccm of NH 3 , The temperature is raised to about 1000 ℃, and the NH is closed after the constant temperature reaction at about 1000 ℃ for 180 minutes 3 , Changed to 200sccm of Ar, lowered to room temperature in Ar atmosphere, and taken out to obtain a white macroscopic fluffy crude product. Then, the obtained product is soaked in 2mol / L dilute hydrochloric acid overnight, filtered, and dried to obtain macroscopic fluffy white porous hexagonal boron nitride powder with a purity of more than 99%. figure 1 This is a photograph of the crude product of hexagonal boron nitride prepared in this example. figure 2 This example is a photograph of the post-treated hexagonal boron nitride powder in this example. In this example, a yield of 95% can be obtained. image 3 In the SEM image of the hexagonal boron nitri...

Embodiment 2

[0060] Example 2: Put B 2 O 3 And MgCl 2 Take 2g B with a molar ratio of 2:3 2 O 3 And 4.1g MgCl 2 Put it in an alumina crucible, then put it in an alumina tube furnace, and pass 200sccm of NH 3 , The temperature is raised to about 1450℃, and the NH is turned off after a constant temperature reaction at about 1450℃ for 180 minutes 3 , Changed to 300sccm of Ar, lowered to room temperature in Ar atmosphere, and taken out to obtain a white macroscopic fluffy crude product. Then, the obtained product is soaked in 2mol / L dilute nitric acid overnight, filtered, and dried to obtain macroscopic fluffy white hexagonal boron nitride nanoplate powder with a purity of more than 99%. Image 6 In the SEM image of the hexagonal boron nitride obtained in this example, the high-crystalline boron nitride nanosheets can be seen stacked together. Figure 7 This is the TEM image of the hexagonal boron nitride obtained in this example. Figure 8 The XRD pattern of the hexagonal boron nitride nanosheets...

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Abstract

The invention discloses a method for preparing macro-quantity hexagonal boron nitride powder through chemical vapor deposition. The method comprises the following steps: heating a precursor in a nitrogen-containing reaction atmosphere to 900 to 1450 DEG C, maintaining the precursor at the temperature, and then cooling the precursor to room temperature in a protective atmosphere so as to obtain a crude product is obtained, wherein the precursor comprises a uniform mixture of boron oxide and magnesium chloride; and carrying out post-treatment on the crude product to obtain the hexagonal boron nitride powder. The raw materials used in the method are cheap and easily available; process flow is simple; the crude product can be obtained in one step; the reaction efficiency of the precursor is upto 95%; a product with a purity of up to 99% can be prepared through simple post-treatment of the crude product; and the reaction temperature range of the method can be changed so as to prepare two hexagonal boron nitride powder products with completely different morphologies and functions. The gram-level preparation of hexagonal boron nitride can be easily achieved via the method provided by theinvention.

Description

Technical field [0001] The invention particularly relates to a method for preparing macroscopic hexagonal boron nitride powder by a chemical vapor deposition method, which belongs to the technical field of inorganic nano materials. Background technique [0002] Boron nitride has the following four different variant structures: hexagonal boron nitride (HBN), rhombohedral boron nitride (RBN), cubic boron nitride (CBN) and wurtzite boron nitride (WBN). Among them, hexagonal boron nitride, which is very important, is white and is a classic graphene-like layered structure. It has excellent high thermal conductivity (the thermal conductivity is ten times that of quartz), high temperature resistance (melting point 3000 ℃), and oxidation resistance (1200 It starts to oxidize in the air above ℃), electrical insulation, hydrophobicity, lubrication, and good chemical stability (acid and alkali resistance) and biological compatibility, etc., also known as "white graphite". In the small fami...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/064B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00C01B21/064C01B21/0643C01P2002/01C01P2002/72C01P2002/80C01P2004/03C01P2006/12C01P2006/16C01P2006/80
Inventor 姚亚刚许燕翠
Owner SUZHOU INST OF NANO TECH & NANO BIONICS CHINESE ACEDEMY OF SCI
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