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Boron nitride nanosheet powder and macro-quantity preparation method thereof

A technology of nanosheets and boron nitride, applied in chemical instruments and methods, nitrogen compounds, nanotechnology, etc., can solve the problems of small size, high cost, and low efficiency of nanosheets, and achieve mass production and simple process Effect

Inactive Publication Date: 2017-06-13
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

The synthesis temperature of this method is low, and the size of the obtained nanosheets is small and the crystallinity is poor.
[0006] Looking at the production technology of boron nitride nanosheets, the higher cost and lower efficiency seriously restrict further scientific research and practical application

Method used

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  • Boron nitride nanosheet powder and macro-quantity preparation method thereof
  • Boron nitride nanosheet powder and macro-quantity preparation method thereof
  • Boron nitride nanosheet powder and macro-quantity preparation method thereof

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preparation example Construction

[0033] In a typical implementation of the present invention, a method for the macro-preparation of boron nitride nanosheet powder comprises the following steps:

[0034] (1) Thoroughly mix the boron source and the nitrogen source precursor, heat to 1100-1500°C (preferably 1100-1400°C, especially preferably 1200-1300°C) in an atmosphere containing ammonia gas and keep it warm for 0.5-4h, Cool down to room temperature under the protection of nitrogen or argon to obtain a white crude product.

[0035] (2) pickling, filtering and drying the crude product obtained in step (1) to obtain boron nitride nanosheet powder with a purity of more than 99%.

[0036] With the aforementioned method, according to the amount of the precursor and the volume of the equipment, the output of a single batch can reach more than gram level. Under optimal synthesis conditions, 30-35 g of boron nitride nanosheets can be obtained from 100 g of reactants, and the net yield is as high as 90%.

[0037] Whe...

Embodiment 1

[0048] Example 1 will B 2 o 3 and Mg 3 N 2 Mix well at a molar ratio of 2:1, take 1g and place it in an open alumina crucible, then put it into a tube furnace, and vacuum to 10 -3 Pa, 200 standard milliliters per minute (sccm) of NH 3 , heating up to 1300°C. Turn off NH after 180min constant temperature reaction at 1300°C 3 , into 500sccm N 2 , at N 2 The temperature was cooled to room temperature in the atmosphere, and the crude product was obtained. Then the obtained product is ultrasonically pickled with 3 mol / L nitric acid for 5 hours, filtered and dried to obtain boron nitride nanosheet powder with a purity of more than 99%. figure 1 The physical photo of the unacid-washed crude product of BN nanosheets prepared for this example. figure 2 It is the physical photo of the BN nanosheet (boron nitride nanosheet, BN nanosheet, BNNS for short) after purification in this embodiment. In this example, a yield of 90% can be obtained. image 3 This is the XRD pattern of ...

Embodiment 2

[0049] Example 2 will B 2 o 3 and Mg 3 N 2 Mix thoroughly at a molar ratio of 1:1, take some and place them in an open alumina crucible, and then put them into a tube furnace. The furnace tube was purged of air by blowing 1000 standard milliliters per minute (sccm) of Ar. Then 200sccm Ar and 200sccm NH 3 The temperature was raised to 1300°C. Turn off the NH after reacting at a constant temperature of 1300°C for 60 minutes 3 , 500 sccm of Ar was introduced to cool down to room temperature, and the crucible was taken out to obtain a crude product. Then the obtained product is ultrasonically pickled with 3 mol / L nitric acid for 10 h, filtered and dried to obtain boron nitride nanosheet powder with a purity of more than 99%. Figure 5 This is the SEM image of the BN nanosheets obtained in this example, and scaly BN nanosheets can be observed. Image 6 For the Raman spectrum of the BNNS that this embodiment obtains, by 1367.9cm - 1 The peak can be judged as hexagonal stru...

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Abstract

The invention discloses boron nitride nanosheet powder and a macro-quantity preparation method thereof. The preparation method comprises the following steps: sufficiently mixing a boron source precursor and a nitrogen source precursor, heating to 1100 to 1500 DEG C in a nitrogen-containing reaction atmosphere, keeping the temperature for more than 0.5 h, then cooling to room temperature in a protective atmosphere, obtaining a crude product, and then postprocessing the crude product to obtain the boron nitride nanosheet powder. The purity of the boron nitride nanosheet powder is more than 99%, boron nitride nanosheets therein are hexagonal boron nitride nanosheets, the thicknesses of the hexagonal boron nitride nanosheets are 1 to 20 atom layer, and the radial dimensions of the hexagonal boron nitride nanosheets are 1 to 20 microns. The raw materials such as boron oxide and metal nitride adopted in the invention are cheap and easily obtained, the reaction can be completed in one step, the technology is simple, the conversion rate of the raw materials is more than 90%, and the purity of the product after acid pickling is more than 99%. Particularly, the boron nitride nanosheet powder higher than gram grade can be further prepared through a single patch of reactions, so that volume production is realized.

Description

technical field [0001] The invention specifically relates to a boron nitride nanosheet powder and a macro-preparation method thereof, belonging to the technical field of inorganic nanomaterials. Background technique [0002] Boron nitride nanosheets (BNNS) have many excellent physical and chemical properties, such as excellent electrical insulation, high thermal conductivity, wide direct band gap, large specific surface area, good biocompatibility, and good chemical inertness , high temperature resistance, and oxidation resistance, and has broad application prospects in many fields such as graphene electronic devices, deep ultraviolet luminescence, composite materials, heat dissipation materials, friction materials, drug loading, and catalyst loading. [0003] At present, there are two main directions for the synthesis of BN. One is to grow atomically flat BN nanosheets or continuous films on the substrate. One is the macro preparation of powdered BN nanosheets. [0004] R...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/064B82Y30/00B82Y40/00
CPCC01B21/064C01B21/0648C01P2002/72C01P2002/82C01P2004/03C01P2004/04C01P2004/24C01P2004/61C01P2006/80
Inventor 姚亚刚李涛涛
Owner SUZHOU INST OF NANO TECH & NANO BIONICS CHINESE ACEDEMY OF SCI
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