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Method for preparing boron nitride nanotubes by annealing of inorganic boracic precursor

A boron nitride nanotube, boron precursor technology, applied in inorganic chemistry, chemical instruments and methods, nitrogen compounds and other directions, can solve the problems of difficulty in mass preparation, low yield, etc., and achieves low cost, simple preparation process, and reaction mild effects

Inactive Publication Date: 2009-11-18
WUHAN INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although some successes and progress have been made in the preparation of boron nitride nanotubes in recent years, the yields are usually very low and it is difficult to prepare them in large quantities.

Method used

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  • Method for preparing boron nitride nanotubes by annealing of inorganic boracic precursor
  • Method for preparing boron nitride nanotubes by annealing of inorganic boracic precursor
  • Method for preparing boron nitride nanotubes by annealing of inorganic boracic precursor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Example 1 Dry-blended self-propagating process

[0035] Taking calcium hexaboride (CaB 6 ) Is a boron source, cobalt oxide (Co 2 O 3 ) Introduce the preparation process of inorganic boron source precursor for catalyst The first step: ingredients. CaB 6 , Co 2 O 3 All are analytical reagents, weigh 50.03g CaB 6 , 50.25g Co 2 O 3 , Wherein the molar ratio B:Co is 1:0.21. The second step: mixing. Will weighed CaB 6 And Co 2 O 3 Add a high-speed mixer (18000 rpm) and mix for 5 minutes to make it fully uniform. The third step: molding. Pour the mixture into a steel mold, use a 500-ton press, hold the pressure for 15 minutes, shape, and take it out. The fourth step: reaction. Put the formed material into the reaction tank without sealing. Put the reaction tank in an argon-protected heating furnace, keep it at 750°C for 12 minutes, and cool it naturally. Open the tank and take out the product. The appearance is black honeycomb. The fifth step: crush. The reacted materials are adde...

Embodiment 2

[0037] Example 2 Dry powder ball milling process

[0038] Taking calcium hexaboride (CaB 6 ) Is a boron source, nickel chloride (NiCl 2 ) Introduce the preparation process of inorganic boron source precursor for the catalyst. The first step: ingredients. CaB 6 , NiCl 2 All are analytical reagents, weigh 50.04g CaB 6 , 40.09g NiCl 2 , Wherein the molar ratio B:Ni is 1:0.11. The second step: ball milling. Pour the prepared raw materials into a stainless steel ball mill tank, use stainless steel balls, adjust the parameters of the ball mill, autobiography 500 rpm, revolution 250 rpm, ball milling for 12 hours. The third step: molding. Pour the ball mill material into a steel mold, use a 500-ton press, hold the pressure for 13 minutes, shape, and take it out. The fourth step: reaction. Put the formed material into the reaction tank without sealing. Place the reaction tank in a heating furnace protected by argon, keep it at 850°C for 8 minutes, and cool it naturally. Open the tank and ...

Embodiment 3

[0040] Example 3 Liquid phase dispersion self-propagating process

[0041] With barium hexaboride (BaB 6 ) Is a source of boron, iron trioxide (Fe 2 O 3 ) Introduce the preparation process of inorganic boron source precursor for the catalyst. The first step: ingredients. BaB 6 , Fe 2 O 3 All are analytical reagents, weighing 60.03g BaB 6 , 35.09g Fe 2 O 3 , Where the molar ratio B:Fe is 1:0.24. Step 2: Disperse. Pour the weighed materials into a 1000ml beaker, add 500ml of distilled water, stir for 20 minutes, and ultrasonic for 10 minutes to make the materials evenly dispersed in the distilled water. The third step: suction filtration. The mixed liquid is filtered through a circulating water vacuum pump. The fourth step: drying. The obtained filter cake was dried in a vacuum drying oven at 80°C for 8 hours. The fifth step: crush. Add the dried filter cake to a high-speed mixer (18000 rpm) and mix for 5 minutes. The sixth step: molding. Pour the mixture into a steel mold, use a 50...

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Abstract

The invention relates to a novel method for preparing boron nitride nanotubes by annealing of an inorganic boracic precursor, comprising annealing the inorganic boracic precursor for 5-50h at the temperature of 800-1200 DEG C to obtain boron nitride nanotubes. The beneficial effects of the invention comprise that 1) annealing reaction of the boracic precursor is adopted to prepare boron nitride nanotubes, boron element is sintered with catalyst to form porous solid, the problem that the yield and the purity of boron nitride nanotubes are low is solved, the preparation yield limit of boron nitride nanotubes is surmounted, the preparation process is simple, the product yield of boron nitride nanotubes is above 80% and the purity is above 85%; 2) the chemical property of the prepared inorganic boracic precursor is stable which is applicable to batch manufacturing boron nitride nanotubes with low cost and high purity; the reaction condition of preparing precursor is mild, the process is simple, and the energy consumption and the cost are low, which is applicable to industrialized production and the precursor can be directly used to prepare boron nitride nanotubes.

Description

Technical field [0001] The invention relates to the field of preparation of ceramic materials and nano materials, in particular to a new method for preparing boron nitride nanotubes by annealing from an inorganic boron-containing precursor. Background technique [0002] In 1995, Chopra and others successfully prepared boron nitride nanotubes by plasma arc discharge method, which opened the prelude to the research of boron nitride nanotubes. Boron nitride nanotubes have high modulus, high strength and toughness comparable to carbon nanotubes, and excellent chemical and thermal stability. In addition, boron nitride nanotubes behave as wide band gap semiconductors, about 5.5 eV. These characteristics make boron nitride nanotubes attract research interests from many fields such as semiconductor devices, nanocomposite ceramics, and hydrogen storage materials. [0003] The preparation methods of boron nitride nanotubes mainly include arc melting method, high temperature chemical method...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/064B82B3/00
Inventor 谷云乐王吉林
Owner WUHAN INSTITUTE OF TECHNOLOGY
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