A kind of push boat type semi-continuous method boron nitride nanotube preparation furnace and using method thereof

A technology of boron nitride nanotubes and furnace tails, which is applied in chemical instruments and methods, nitrogen compounds, inorganic chemistry, etc., can solve the problem that the synthesis of BNNTs is not too large, the effective utilization rate of reducing gas is not high, and the waste gas cannot be effectively treated and other problems, to achieve the effect of continuous large-scale synthesis, rich and diverse product structure, avoiding repeated opening times and idle time

Active Publication Date: 2022-07-19
WUHAN INSTITUTE OF TECHNOLOGY
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Problems solved by technology

Chinese patent CN201359434Y discloses a push boat type two-tube reduction furnace, which is used for the reduction of metal powder, but on the one hand, the structure of the device is relatively complicated, with many temperature control areas and small temperature differences, which is not very suitable for the synthesis of BNNTs Significance; on the other hand, the device does not have a gas circulation system, and the effective utilization rate of the reducing gas is not high
However, this equipment not only cannot create the atmosphere required for the reaction, but also the waste gas generated by the reaction cannot be effectively treated, which has environmental protection problems; in addition, the equipment has different temperature reaction zones, resulting in more heating equipment, and materials need to be advanced in different reaction zones , inconvenient to operate

Method used

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  • A kind of push boat type semi-continuous method boron nitride nanotube preparation furnace and using method thereof
  • A kind of push boat type semi-continuous method boron nitride nanotube preparation furnace and using method thereof
  • A kind of push boat type semi-continuous method boron nitride nanotube preparation furnace and using method thereof

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Experimental program
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Effect test

Embodiment 1

[0030] Utilize the present invention to provide such as figure 1 The method for synthesizing smooth-walled boron nitride nanotubes with the equipment shown is as follows:

[0031] Check in advance to ensure that the equipment is in good working order overall. Start the electric control heating device A, set the temperature to heat the furnace 8, and the heating rate is 4-8°C / min. Close the furnace head door 3 and the furnace tail furnace door 4, open the furnace head exhaust pipe 1 and the furnace tail air intake pipe 2, vacuum and exhaust the furnace chamber 8, and then continue to transport into the furnace chamber 8 through the furnace tail intake pipe 2 Ammonia, the flow of ammonia is controlled at 0.4-1.0L / min, and the pipeline gas circulation machine is kept in the open working state. Immediately after, the ceramic boat covered with ultrafine boron carbide powder is put into the furnace chamber 8 of the furnace body B to carry out a heat preservation reaction, the reac...

Embodiment 2

[0033] Utilize the present invention to provide such as figure 1 The method for synthesizing bamboo-type boron nitride nanotubes by the equipment shown is basically similar to that in Example 1, except that the heating rate is 6-10°C / min, the flow rate of ammonia gas is 0.6-1.2L / min, and the holding temperature is 900°C. -1400℃, holding time 3-6h. XRD, Raman spectrum, TEM analysis were carried out to the bamboo-shaped BNNTs obtained in Example 2, and the results were as follows. Figure 3-5 shown.

[0034] from image 3 It can be seen in the characteristic XRD diffraction spectrum of the BNNTs sample that the characteristic diffraction peaks are very clear, indicating that the sample has a good degree of crystallinity. The d values ​​of the characteristic diffraction peaks are at 0.33492, 0.21843, 0.20786 and 0.16693 nm, corresponding to the (002), (100), (101) and (004) crystal planes of hexagonal boron nitride, respectively. From this, the unit cell constants of the prod...

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Abstract

The invention relates to a boat-type semi-continuous method for preparing boron nitride nanotubes and a method for using the same. The set of equipment includes an electric temperature control heating device A, a furnace body B, a furnace head C and a furnace tail D. The electric temperature control heating device A is used to adjust and control the temperature of the furnace body B. The furnace in the furnace body B passes through the furnace tube and the two The furnace head C on the side is communicated with the furnace tail D, and a circulating water holder for cooling is arranged on the outer surface of the furnace tube. The raw materials react with ammonia gas in the furnace chamber of the furnace body B, and then are transferred to the furnace tube between the furnace body B and the furnace tail D for cooling. At the same time, the next batch of raw materials are transported to the furnace chamber for reaction. The furnace tail D is taken out, thereby realizing continuous production. The device has the advantages of convenient operation, rich and diverse product structures, and is especially suitable for industrial production applications. It has high equipment safety and good stability, and can continuously synthesize BNNTs with different structures on a large scale.

Description

technical field [0001] The invention relates to the technical field of synthesis of mechanical and inorganic non-metallic materials, in particular to a boat-type semi-continuous boron nitride nanotube preparation furnace and a method for using the same. Background technique [0002] The synthesis method of boron nitride (BN) occupies an extremely important position in the research of boron nitride materials. A method for industrialized large-scale synthesis of high-purity boron nitride has been developed, which can provide a solid foundation and guarantee for the theoretical research and practical application of boron nitride. [0003] Boron nitride nanotubes (BNNTs) are one of the most important boron nitride materials with excellent mechanical, thermal, and electromagnetic properties. The existing preparation methods of BNNTs mainly include arc discharge method, laser ablation method, vapor deposition method (CVD), high temperature synthesis method, etc. Among them, the ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B21/064
Inventor 谷云乐范明聪王吉林吉钰纯
Owner WUHAN INSTITUTE OF TECHNOLOGY
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