CN102504760B - Preparation method of silicon carbide and carbon nano tube composite wave-absorbing material - Google Patents
Preparation method of silicon carbide and carbon nano tube composite wave-absorbing material Download PDFInfo
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- CN102504760B CN102504760B CN201110351442.7A CN201110351442A CN102504760B CN 102504760 B CN102504760 B CN 102504760B CN 201110351442 A CN201110351442 A CN 201110351442A CN 102504760 B CN102504760 B CN 102504760B
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Abstract
The invention provides a preparation method of a silicon carbide and carbon nano tube composite wave-absorbing material, comprising the following steps of: dispersing the silicon carbide into a nitrate solution and immersing to form a metal-silicon carbide composite with 5-15% of a metal component by weight; after the immersion, evaporating slurry to be dry and drying at a temperature in a range of 60-120 DEG C for 6-24 hours; calcining the dried product at a temperature in a range of 300-600 DEG C for 4-6 hours and adding a material which needs to be grinded after being cooled into a quartz tube; introducing methane into one end of the quartz tube and communicating the other end of the quartz tube with atmosphere; setting a temperature-rising speed to be 5-15 DEG C/min and setting a reaction air speed to be 300-3000 per hour; raising the temperature to 500-900 DEG C and reducing the temperature to a room temperature after keeping at constant temperature for 1-5 hours; and taking out the obtained material, namely the silicon carbide and carbon nano tube composite wave-absorbing material. The silicon carbide and carbon nano tube composite wave-absorbing material prepared by the preparation method has the advantages of high-temperature resistance, and capability of enhancing the wave-absorbing property and the stability of the material.
Description
Technical field
The invention belongs to a kind of preparation method of absorbing material, relate to specifically the preparation method of a kind of silicon carbide and carbon nano tube composite wave-absorbing material.
Background technology
Along with the development of modern science and technology, the application of absorbing material in aerospace, military affairs and environmental area is more and more extensive.Particularly high temperature resistant absorbing material, as the critical material of national defense and military and aerospace field, is subject to the very big attention of countries in the world.Therefore, the exploitation of high-performance wave-absorbing material and research, become the hot subject of material circle.Current absorbing material is of a great variety, and environment for use and performance are different.The most frequently used absorbing material is take ferrite as representative, and it is typical magnetic loss absorbing material, and density is large, perishable, and is subject to the impact of Curie temperature and skin depth, is difficult to bring into play it and inhales ripple effect under high frequency, high temperature; The superpolymer absorbing material of exploitation, comprises chirality absorbing material in recent years, is difficult to especially use under high temperature atmosphere environment; Resistive absorbing material, as carbon fiber, silicon carbide etc., though can be used for hot environment, its wave absorbing efficiency and suction ripple scope face severe challenge.So we need further to improve the absorbing property of absorbing material, acquisition has high temperature resistant, corrosion resistant new and effective absorbing material.
The absorbing property of material is relevant with the pattern of material and structure, and particularly multiple absorbing material is composite, can significantly improve the absorbing property of material.The absorbing material of silicon carbide, carbon nanotube and physical strength advantages of higher stable, high temperature resistant, corrosion-resistant, anti-oxidant as a kind of physicochemical property, receives correlative study person's concern.For example: Chinese patent (publication number: CN 1544723) discloses a kind of composite fiber microwave absorbing material of silicon carbide-containing, it passes through nanometer silicon carbide, polyacrylonitrile-based carbon and auxiliary agent blend, spinning, again through surface treatment, make silicon carbide polyacrylonitrile carbon fiber composite wave-suction material, this material can be made into clothes and other radiation-proof fabric.Chinese patent (publication number: the preparation method who 101045533) discloses a kind of carbon nano tube compound material of surface load magnetic alloy particle.Its by carbon nanotube at the contribution aspect dielectric loss and magnetic alloy particle at the hertzian wave of decaying of the contribution aspect electromagnetic consumable.Chinese patent (publication number: the preparation method who 101289569) discloses a kind of multi-walled carbon nano-tubes/epoxide resin wave-absorbing and camouflage composite material.The method is utilized the dielectric loss of carbon nanotube and the epoxy resin hertzian wave of decaying, and defect carbon nano tube surface being caused by NaOH improves the dielectric loss of material.But, by adopting silicon carbide, be matrix, growth in situ, the research that forms the composite wave-suction material of carbon nanotube and silicon carbide have not been reported.
Summary of the invention
The present invention proposes the preparation method of the composite wave-suction material of a kind of resistant to elevated temperatures silicon carbide and carbon nanotube.
The present invention is take silicon carbide as substrate, and by carrying transition metal particle in its surface, then take methane as reductibility with reactant gases, In-stiu catalysis methane under certain temperature and air speed, forms the composite wave-suction material of carbon nanotube and silicon carbide.
The present invention is achieved by means of the following methods:
(1) adopt pickling process, silicon carbide is scattered in nitrate solution, it is the metal-silicon carbide mixture of 5-15% weight part that dipping forms metal component;
(2) after having flooded, by slurry evaporate to dryness, dry 6-24h at 60-120 ℃;
(3) dried material is calcined to 4-6h at 300-600 ℃, grind after cooling;
(4) pack the material after grinding into silica tube, silica tube one end passes into methane, the other end communicates with atmosphere, it is 5-15 ℃/min that temperature rise rate is set, the air speed of reaction is 300-3000/h, is warming up to 500-900 ℃, after constant temperature 1-5h, is down to room temperature, take out resulting materials, be silicon carbide and carbon nano tube composite wave-absorbing material.
Nitrate as above is iron nitrate, nickelous nitrate or Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES.
The specific surface area of silicon carbide as above is 30-150m
2/ g.
Feature of the present invention is, having adopted silicon carbide is substrate, carrying metal particles, and take methane as reducing gas and required carbon source, original position Formed nanotube on silicon carbide, forms the absorbing material with the special construction of carbon nanotube carbon coated SiClx.The absorbing material forming, metal content is very low, and is carbonized in the middle of silicon and carbon nanotube be wrapped in, and can effectively prevent its corrosion and oxidation.Silicon carbide and carbon nanotube, each other in conjunction with evenly, are conducive to absorbing property and the stability of strongthener simultaneously.The external diameter of gained carbon nanotube between 10-100nm, internal diameter 5-30nm, length is 0.5-20um.
Accompanying drawing explanation
Fig. 1 is the suction wave reflection rate collection of illustrative plates of embodiment 1 matrix material different thickness
Fig. 2 is the suction wave reflection rate spectrogram of embodiment 2 matrix material different thickness
Fig. 3 is the suction wave reflection rate spectrogram of embodiment 3 matrix material different thickness.
Embodiment
Embodiment 1
1, take 0.25g Ni (NO
3)
26H
2o, is dissolved in 30ml distilled water.After stirring, add 1g silicon carbide powder, it is the metal-silicon carbide mixture of 5% weight part that dipping forms metal component.
2, will after appeal slurry evaporate to dryness, put into baking oven, dry 24h. at 60 ℃
3, by the 300 ℃ of calcining 6h. in retort furnace of the material after dried
4,, by the material grind into powder of having calcined, take 0.5g and put into the silica tube that caliber is 12mm.
5, silica tube is loaded into the tube furnace on fixed bed, silica tube one end passes into methane, and one end communicates with atmosphere, and it is 5 ℃/min that temperature rise rate is set, and the air speed of reaction is 300/h, is warming up to 500 ℃, constant temperature 5h.
6, treat that fixed bed finishes working time, be down to room temperature, take out resulting materials, be silicon carbide/carbon nanometer tube composite materials.Described silicon carbide specific surface area is 30m
2/ g, the external diameter of gained carbon nanotube between 10-50nm, internal diameter 5-20nm, length is 0.5-15um..
7, Fig. 1 is the suction wave reflection rate collection of illustrative plates of this matrix material different thickness, can find out, the absorption frequency range of-10dB following (more than 90% absorbing the absorption that-20dB is 99%) can reach 3.5GHZ, and absorption intensity can reach 39.5dB.
1, take 0.74g Ni (NO
3)
26H2O, is dissolved in 30ml distilled water.After stirring, add 1g silicon carbide powder, it is the metal-silicon carbide mixture of 15% weight part that dipping forms metal component.
2, will after appeal slurry evaporate to dryness, put into baking oven, dry 12h. at 100 ℃
3, by the 500 ℃ of calcining 5h. in retort furnace of the material after dried
4,, by the material grind into powder of having calcined, take 0.5g and put into the silica tube that caliber is 12mm.
5, silica tube is loaded into the tube furnace on fixed bed, silica tube one end passes into methane, and one end communicates with atmosphere, and it is 10 ℃/min that temperature rise rate is set, and the air speed of reaction is 1200/h, is warming up to 700 ℃, constant temperature 3h.
6, treat that fixed bed finishes working time, be down to room temperature, take out resulting materials, be silicon carbide/carbon nanometer tube composite materials.Described silicon carbide specific surface area is 60m
2/ g, the external diameter of gained carbon nanotube between 30-100nm, internal diameter 10-30nm, length 1-20um.
7, Fig. 2 is the suction wave reflection rate spectrogram of this matrix material different thickness, can find out, the absorption frequency range of-10dB following (more than 90% absorbing the absorption that-20dB is 99%) can reach 5.1GHZ, and absorption intensity can reach 37.6dB.
Embodiment 3
1, take 0.5g Co (NO
3)
2.6H
2o, is dissolved in 30ml distilled water.After stirring, add 1g silicon carbide powder, it is the metal-silicon carbide mixture of 10% weight part that dipping forms metal component.
2, will after appeal slurry evaporate to dryness, put into baking oven, dry 6h. at 120 ℃
3, by the 600 ℃ of calcining 4h. in retort furnace of the material after dried
4,, by the material grind into powder of having calcined, take 0.5g and put into the silica tube that caliber is 12mm.
5, silica tube is loaded into the tube furnace on fixed bed, silica tube one end passes into methane, and one end communicates with atmosphere, and it is 15 ℃/min that temperature rise rate is set, and the air speed of reaction is 3000/h, is warming up to 900 ℃, constant temperature 1h.
6, treat that fixed bed finishes working time, be down to room temperature, take out resulting materials, be silicon carbide/carbon nanometer tube composite materials.Described silicon carbide specific surface area is 150m
2/ g, the external diameter of gained carbon nanotube between 20-80nm, internal diameter 8-25nm, length 1-15um.
7, Fig. 3 is the suction wave reflection rate collection of illustrative plates of this matrix material different thickness, can find out ,-10dB following (more than 90% absorbing the absorption that-20dB is 99%) absorbs frequency range and can reach 3.6GHZ, and absorption intensity can reach 50.5dB.
Claims (1)
1. a preparation method for silicon carbide and carbon nano tube composite wave-absorbing material, is characterized in that comprising the steps:
(1) adopt pickling process, silicon carbide is scattered in nitrate solution, it is the metal-silicon carbide mixture of 5-15% weight part that dipping forms metal component;
(2) after having flooded, by slurry evaporate to dryness, dry 6-24 h at 60-120 ℃;
(3) dried material is calcined at 300-600 ℃ to 4-6 h, ground after cooling;
(4) pack the material after grinding into silica tube, silica tube one end passes into methane, the other end communicates with atmosphere, it is 5-15 ℃/min that temperature rise rate is set, the air speed of reaction is 300-3000/h, is warming up to 500-900 ℃, after constant temperature 1-5 h, is down to room temperature, take out resulting materials, be silicon carbide and carbon nano tube composite wave-absorbing material;
The specific surface area of described silicon carbide is 30-150 m
2/ g;
Described nitrate is iron nitrate, nickelous nitrate or Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES.
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| CN103422192B (en) * | 2013-08-05 | 2015-10-07 | 江苏科技大学 | Fe-Co alloy/C/C composite nano fiber microwave absorption, preparation method and application thereof |
| CN103754878B (en) * | 2014-01-06 | 2015-10-14 | 上海交通大学 | The method of the spontaneous carbon nanotube of a kind of silicon-carbide particle surface in situ |
| CN105670559B (en) * | 2015-12-29 | 2018-01-16 | 西北工业大学 | The preparation method of in-situ authigenic carbon nanocoils/porous ceramics absorbing material |
| CN110564366B (en) * | 2019-09-30 | 2022-08-19 | 哈尔滨工业大学 | Using NiCl 2 Preparation method for preparing high-temperature-resistant dielectric wave absorber C @ SiC whisker powder |
| CN113231638B (en) * | 2021-04-12 | 2023-06-09 | 贵州亿源电子有限公司 | Preparation method of nano wave-absorbing material |
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