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Preparation method of porous niobium nitride powder microwave absorption material

A technology of microwave absorbing materials and niobium nitride, which is applied in the field of material science, can solve problems such as light weight and high efficiency of microwave absorbing materials, insufficient pore structure, and high powder density, and achieve excellent microwave absorption characteristics and good crystallinity , the effect of uniform particle size distribution

Active Publication Date: 2020-06-02
唐山市科硕特种陶瓷制造有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

(Preparation of nanometer NbN powder by liquid phase reduction [C] / / Metallurgical Engineering Science Forum. 2006.) However, the niobium nitride powder prepared by the above method is mostly solid structure, the pore structure is not rich enough and the powder density is high, so it is difficult to Meet the needs of light-weight and high-efficiency absorbing materials
[0006] At present, the preparation of niobium nitride powder into a porous structure and its application in the field of microwave absorption has not been reported so far.

Method used

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  • Preparation method of porous niobium nitride powder microwave absorption material
  • Preparation method of porous niobium nitride powder microwave absorption material
  • Preparation method of porous niobium nitride powder microwave absorption material

Examples

Experimental program
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Embodiment 1

[0028] Weigh 1.35g of niobium pentachloride, add 1.5mL of absolute ethanol and 0.2g of P123, then add 30mL of dichloromethane to obtain a mixed solution, transfer the mixed solution into the reaction bomb, and keep it in an oven at 110°C for 38h. After taking out the sample, wash it with dichloromethane for 3 times, then let it stand for 30 minutes, pour off the supernatant, and dry it in a drying oven at 80°C for 24 hours to obtain the niobium oxide xerogel, and pre-calcine the niobium oxide xerogel at 400°C , the heating rate was 1° C. / min, and the temperature was kept for 30 minutes to obtain niobium oxide powder. Weigh 8g of niobium oxide powder and 1.7g of cyanamide in 10mL of absolute ethanol and stir evenly, then keep warm in a drying oven at 80°C for 24h, and reduce the dried mixed powder to nitrogen at 800°C in flowing ammonia After 2h, a porous niobium nitride powder was obtained. During the nitriding process, when the temperature rises to 300°C, feed 400ml / min of a...

Embodiment 2

[0030] Weigh 1.5g of niobium pentachloride, add 1.2mL of absolute ethanol and 0.3g of P123, then add 30mL of dichloromethane to obtain a mixed solution, transfer the mixed solution into the reaction bomb, and keep it in an oven at 100°C for 42h. After taking out the sample, wash it with dichloromethane for 3 times, then let it stand for 30 minutes, pour off the supernatant, and dry it in a drying oven at 80°C for 24 hours to obtain the niobium oxide xerogel, and pre-calcine the niobium oxide xerogel at 400°C , the heating rate was 1° C. / min, and the temperature was kept for 30 minutes to obtain niobium oxide powder. Weigh 8g of niobium oxide powder and 2g of cyanamide, put them in 10mL of absolute ethanol and stir evenly, then keep them in an oven at 80°C for 24 hours, and then reduce and nitride the dried mixed powder at 900°C in flowing ammonia 2h to obtain porous niobium nitride powder. During the nitriding process, when the temperature rises to 300°C, feed 400ml / min of am...

Embodiment 3

[0032] Weigh 1g of niobium pentachloride, add 1mL of absolute ethanol and 0.1P123, then add 30mL of dichloromethane to obtain a mixed solution, transfer the mixed solution into the reaction bomb, and keep it in an oven at 1120°C for 24h. After taking out the sample, wash it with dichloromethane for 3 times, then let it stand for 30 minutes, pour off the supernatant, and dry it in a drying oven at 80°C for 24 hours to obtain niobium oxide xerogel, and pre-calcine the niobium oxide xerogel at 500°C , the heating rate was 1° C. / min, and the temperature was kept for 30 minutes to obtain niobium oxide powder. Weigh 7g of niobium oxide powder and 1g of cyanamide in 10mL of absolute ethanol and stir evenly, then keep warm in an 80°C drying oven for 24 hours, and then dry the mixed powder in flowing ammonia, and reduce and nitride it at 700°C 4h to obtain porous niobium nitride powder. During the nitriding process, when the temperature rises to 300°C, feed 400ml / min of ammonia gas, a...

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Abstract

The invention discloses a preparation method of a porous niobium nitride powder microwave absorption material, and belongs to the technical field of material science. The method includes: taking niobium pentachloride as a niobium source, adopting anhydrous ethanol as an oxygen donor, using dichloromethane as a solvent, employing polyoxyethylene-polyoxypropylene-polyoxyethylene (P123) as a pore-forming agent, preparing a niobium oxide xerogel by a sol-gel method, performing presintering to obtain niobium oxide powder, then mixing the niobium oxide powder with a structure stabilizer cyanamide, and then carrying out reduction nitridation reaction in an ammonia atmosphere to obtain porous niobium nitride powder. The niobium nitride powder prepared by the method is good in crystallinity and high in purity, has Nb4N5 serving as the phase, is uniform in particle size distribution, and has an abundant porous structure, the pore size and quantity can be adjusted by simply changing the dosage ofthe pore-forming agent, and meanwhile, the niobium nitride powder has excellent microwave absorption characteristic.

Description

technical field [0001] The invention belongs to the technical field of material science, and in particular relates to a preparation method of a porous niobium nitride powder microwave absorbing material. Background technique [0002] With the development of various new radars, advanced detectors and precision-guided weapons, modern warfare has continuously improved the stealth technology requirements of weapon systems. Strict working conditions require electromagnetic wave-absorbing stealth materials to meet the requirements of "thin thickness, low density, wide frequency band, Strong absorption, multiple spectrum bands, high stability” and other performance indicators. At present, common absorbing materials include ferrite, silicon carbide, and carbon fiber, etc., but due to their shortcomings such as high density, poor stability, narrow absorption frequency band, and large matching thickness, it is difficult to meet the requirements of complex and changeable environments. ...

Claims

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Application Information

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IPC IPC(8): C01B21/06B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00C01B21/06C01P2002/72C01P2004/03C01P2004/61C01P2004/64C01P2006/12C01P2006/17
Inventor 崔燚吕东风魏颖娜陈越军魏恒勇姚少巍卜景龙吴振刚陈颖呼世磊崔帅朱彬王学沛许凯政温佳杰
Owner 唐山市科硕特种陶瓷制造有限公司
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