CN101269992A - Surface ceramic bovine stephanoporate bamboo charcoal wave-suction material of load magnetic metal and method of producing the same - Google Patents
Surface ceramic bovine stephanoporate bamboo charcoal wave-suction material of load magnetic metal and method of producing the same Download PDFInfo
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Abstract
The present invention relates to a porous ceramic bamboo charcoal absorbing material that is used on the surface of load magnetic metal, and a preparation method thereof, belonging to the field of the absorbing material of electromagnetic wave. The generation of the ceramic surface of the bamboo charcoal, the inner load magnetic metal and the silicon-based ceramic crystal whisker in the pore channel can simultaneously has the functions of three loss mechanisms that comprise resistance, dielectric and magnetic media, so as to effectively absorb electromagnetic radiation.
Description
Technical field:
The present invention relates to a kind of carried magnetic metallic surface potteryization stephanoporate bamboo charcoal wave-suction material and preparation method thereof, belong to the electromagnetic wave absorbent material field.
Background technology:
In modern war, stealthy technique has become one of current most advanced and sophisticated military technique, and wherein the research of material obsorbing radar waves (abbreviation absorbing material) and application are the important component part (Kang Feiyu of stealthy technique development, Zheng Yongping, Peng Junfang, Chinese patent, 2003, CN1395466).Realize that stealthy technological approaches mainly contains two classes: the one, reduce the radar scattering cross section by configuration design as far as possible.But because of being subjected to the restriction of tactical and technical norms and envrionment conditions, carrying out the ideal design has sizable difficulty; The 2nd, use absorbing material.Then more or less freely because of developing absorbing material, and easy to implement, so absorbing material research becomes the research focus in the stealthy technique.In addition, along with developing rapidly of electronics and information industry, a large amount of outside launching electromagnetic waves of electronic product, thus cause the hertzian wave public hazards.Because the vital role of electromagnetic wave absorbent material in social life and national defense construction makes a big impact for space flight, national defense industry, communication and daily life, thereby the research and development electromagnetic wave absorbent material becomes the important topic of people's growing interest.
Summary of the invention:
The purpose of this invention is to provide a kind of carried magnetic metallic surface potteryization stephanoporate bamboo charcoal wave-suction material and preparation method thereof, generation by bamboo charcoal surface ceramic deposition and the inner silicon based ceramic whisker of internal load magneticmetal and duct, can bring into play the effect of resistor-type, dielectric type and three kinds of loss mechanisms of magneticmedium type simultaneously, realize absorption effectively electromagenetic wave radiation.
Carried magnetic metallic surface potteryization stephanoporate bamboo charcoal wave-suction material of the present invention, for natural bamboo after reaming, charing, the carried magnetic metal is again through the porous material of surface ceramic deposition; Also can be the commercially available direct carried magnetic metal of industrial bamboo charcoal powder, again through the porous material of silica sphere potteryization.It is characterized in that: be magnetic metal and growth of duct, the inside load of material has the silicon carbide ceramics whisker.
The preparation method of the above-mentioned carried magnetic metallic surface of the present invention potteryization stephanoporate bamboo charcoal wave-suction material may further comprise the steps successively:
(1) the reaming processing and the charing of natural bamboo: (a) soaked in expanding agent at least 10 hours after will being processed into the bamboo chip drying of desired shape and size, the bamboo chip after will soaking then is 120 ℃ of oven dry; 800～1000 ℃ temperature, charing is 1～3 hour under protection of inert gas atmosphere, makes the bamboo charcoal sheet again; Carbonization time is as the criterion with the complete charing of bamboo chip, and unsuitable too short or long, too short charing is incomplete, long energy dissipation, at least 1 hour usually of causing.
(2) carried magnetic metal: bamboo charcoal sheet in (1) or bamboo charcoal were flooded 12 hours in the salts solution of magneticmetal at least, filter out then 120 ℃ of oven dry;
(3) sol impregnation: the product in (2) was soaked in vacuum environment in the silicon dioxide gel 8 hours at least, filters out then, make the silicon dioxide gel gelation, again 120 ℃ of oven dry in 60 ℃ of maintenances at least 3 hours;
(4) surface ceramic deposition: 1450～1550 ℃ temperature charing 1～3 hour, make the surface generate the silicon carbide ceramics layer product in (3), inner duct forms the silicon carbide ceramics whisker.Carbonization time is unsuitable too short or long, the too short invention effect that do not reach, long energy dissipation, at least 1 hour usually of causing.
Described expanding agent is sulfuric acid, nitric acid or the aqueous sodium hydroxide solution of 1～3mol/L.
The salts solution of described magneticmetal is the salts solution of iron, cobalt, nickel metal or the mixing salt solution of above-mentioned two or three metal.The concentration of salts solution can not be too low, otherwise the amount of absorption can't meet the demands, and preferably is not less than 2mol/L.
Above-mentioned charing is handled to be preferably under the protection of inert gas and is carried out, as nitrogen or argon shield atmosphere.
Natural bamboo of the present invention is for the inner bamboo kind that flourishing vesicular structure is arranged, as Thorny bamboo, mao bamboon etc.
Advantage of the present invention is that technology is simple, and processing and manufacturing is with low cost, and the electromagnetic wave absorption material of resistor-type, dielectric type and three kinds of loss mechanisms of magneticmedium type is brought into play in preparation simultaneously.
Carried magnetic metallic surface potteryization stephanoporate bamboo charcoal wave-suction material of the present invention, remove and kept the pore passage structure of bamboo charcoal prosperity, there is the silicon carbide ceramics whisker in inner duct also be magnetic metal and growth of load, the mechanism that can bring into play three kinds of loss effects as absorbing material simultaneously is: at first, bamboo charcoal among the present invention is through the high temperature carbonization more than 1450 ℃, degree of graphitization improves, and electroconductibility strengthens, and can be used as the resistor-type wave absorbing agent.The resistivity of the β-SiC on bamboo charcoal surface belongs to the impurity type semi-conductor between metal and semi-conductor, also can be used as the resistor-type wave absorbing agent.Secondly, in the pottery reaction process, silicon based ceramic whiskers such as Si/C/N that generates in the bamboo charcoal duct and Si/C/N/O are the dielectric type wave absorbing agents, mainly absorb hertzian wave by the loss of dielectric polarization relaxation, in addition, the magneticmetal particle of load or magnetic alloy particle can be used as magneticmedium type wave absorbing agent in the bamboo charcoal.The performance that the duct of the inner prosperity of bamboo charcoal simultaneously and interface have also increased the structure-type wave-absorption aspect.
Description of drawings:
Fig. 1: be the stereoscan photograph of surface ceramic deposition stephanoporate bamboo charcoal wave-suction material that utilizes the carried magnetic metal Ni of present method embodiment 1 preparation.
Fig. 2: be to utilize the surface ceramic deposition stephanoporate bamboo charcoal wave-suction material of carried magnetic metal Ni of present method embodiment 1 preparation at the reflectance map of 2～18GHz.
Fig. 3: be the X-ray diffraction spectrum of surface ceramic deposition stephanoporate bamboo charcoal wave-suction material that utilizes the carried magnetic metal Fe of present method embodiment 2 preparation.
Embodiment:
Embodiment 1
Cut the bamboo chip of 20mm * 8mm * 3mm on the cluster needling bamboo,, remove moisture the bamboo chip oven dry.Bamboo chip is immersed in the sodium hydroxide solution that concentration is 3mol/L 10 hours, then suction filtration and be 7 with deionized water rinsing to the pH value of filtrate.With bamboo chip 120 ℃ of oven dry.Place charring furnace 800 ℃ of charings under nitrogen protection to handle bamboo chip, soaking time is 3 hours, the preparation bamboo charcoal.
Bamboo charcoal is immersed in the nickel sulfate solution of 3mol/L 12 hours, then suction filtration.With bamboo charcoal 120 ℃ of oven dry.
Place the silicon dioxide gel that configures to permeate in a vacuum 10 hours bamboo charcoal, take out then in baking oven, make silicon dioxide gel generation gelation reaction, continue temperature oven dry then with 120 ℃ with 60 ℃ temperature heating 4 hours.
At last, place charring furnace 1500 ℃ of charings under nitrogen protection to handle bamboo charcoal, soaking time is 3 hours, obtains the surface ceramic deposition stephanoporate bamboo charcoal wave-suction material of carried magnetic metallic nickel.
With XL-30 type field launch environment scanning electron microscope (manufacturing of U.S. FEI Co.), section is handled through metal spraying, observe the longitudinal section of the surface ceramic deposition stephanoporate bamboo charcoal of carried magnetic metal Ni, the result as shown in Figure 1, whisker shape material is being filled in part bamboo charcoal duct, energy spectrum analysis shows that these materials are SiC, the effect of performance resistor-type wave absorbing agent.
Above-mentioned absorbing material being clayed into power, be distributed in the epoxy resin-base, is the oven dry of filming of the surface of aluminum plate of 5mm at 180 * 180mm, thickness then, makes the absorption of electromagnetic wave coating.When the content of absorbing material is 10%, when coat-thickness was 2mm, sample was seen Fig. 2 at the reflectivity of 2～18GHz.
Taking by weighing the 5g granularity is 500 purpose bamboo charcoal powder, and moisture is removed in oven dry.Bamboo charcoal powder is immersed in the sulphuric acid soln that concentration is 1mol/L 18 hours, then suction filtration and be 7 with deionized water rinsing to the pH value of filtrate.
With bamboo charcoal powder 120 ℃ of oven dry in baking oven.Again bamboo charcoal powder is immersed in the ferric chloride Solution of 2mol/L 18 hours, then suction filtration.With bamboo charcoal powder 120 ℃ of oven dry.
Place the silicon dioxide gel that configures to permeate in a vacuum 8 hours bamboo charcoal powder, the temperature of taking out then in baking oven with 60 ℃ kept 3 hours, made silicon dioxide gel generation gelation reaction, continued the temperature oven dry with 120 ℃.
At last, place charring furnace 1450 ℃ of charings under nitrogen protection to handle bamboo charcoal powder, soaking time is 2 hours, just obtains the surface ceramic deposition stephanoporate bamboo charcoal wave-suction material of carried magnetic metallic iron.
With the phase composition of Japan Rigakv D/max-2400 of science type x-ray diffractometer specimen, the result shows that the composition de-carbon of sample also has silicon carbide and micro-iron in addition as shown in Figure 3.
Embodiment 3
Cut the bamboo chip of 15mm * 6mm * 3mm from mao bamboon,, remove moisture the bamboo chip oven dry.Bamboo chip is immersed in the salpeter solution that concentration is 2mol/L 20 hours, then suction filtration and be 7 up to the pH of filtrate value with deionized water rinsing.With bamboo chip 120 ℃ of oven dry.Place charring furnace 1000 ℃ of charings under nitrogen protection to handle bamboo chip, soaking time is 1 hour, the preparation bamboo charcoal.
Bamboo charcoal is immersed in the ferric chloride Solution of 2.5mol/L 12 hours, then suction filtration.Bamboo charcoal is immersed in the nickel sulfate solution of 2.5mol/L 12 hours, then suction filtration.With bamboo chip 120 ℃ of oven dry.
Place the silicon dioxide gel that configures to permeate in a vacuum 12 hours bamboo charcoal, take out then in baking oven, make silicon dioxide gel generation gelation reaction, continue temperature oven dry with 120 ℃ with 60 ℃ temperature heating 5 hours.
At last, place charring furnace 1550 ℃ of charings under the nitrogen protection of inert gas to handle bamboo charcoal, soaking time is 1 hour, just obtains the surface ceramic deposition stephanoporate bamboo charcoal wave-suction material of carried magnetic metallic iron nickelalloy.
Cut the bamboo chip of 18mm * 8mm * 4mm from the Thorny bamboo,, remove moisture the bamboo chip oven dry.Bamboo chip is immersed in the sulphuric acid soln that concentration is 2mol/L 12 hours, then suction filtration and be 7 up to the pH of filtrate value with deionized water rinsing.With bamboo chip 120 ℃ of oven dry.Place charring furnace 900 ℃ of charings under nitrogen protection to handle bamboo chip, soaking time is 2 hours, the preparation bamboo charcoal.
Bamboo charcoal is immersed in the ferric chloride Solution of 2mol/L 12 hours, then suction filtration.Bamboo charcoal is immersed in the nickel sulfate solution of 2mol/L 12 hours, then suction filtration.Again bamboo charcoal is immersed in the cobalt sulfate solution of 2mol/L 12 hours, then suction filtration.With bamboo chip 120 ℃ of oven dry.
Place the silicon dioxide gel that configures to permeate in a vacuum 15 hours bamboo charcoal, take out then in baking oven, make silicon dioxide gel generation gelation reaction, continue temperature oven dry with 120 ℃ with 60 ℃ temperature heating 5 hours.
At last, place charring furnace 1520 ℃ of charings under the nitrogen protection of inert gas to handle bamboo charcoal, soaking time is 2 hours, just obtains the surface ceramic deposition stephanoporate bamboo charcoal wave-suction material of carried magnetic metallic iron cobalt-nickel alloy.
Embodiment 5
Taking by weighing the 8g granularity is 500 purpose bamboo charcoal powder, and moisture is removed in oven dry.Bamboo charcoal powder is immersed in the sodium hydroxide solution that concentration is 2mol/L 15 hours, then suction filtration and be 7 with deionized water rinsing to the pH value of filtrate.
With bamboo charcoal powder 120 ℃ of oven dry down in baking oven.Again bamboo charcoal powder is immersed in the cobalt chloride solution of 2mol/L 16 hours, then suction filtration.With bamboo charcoal powder 120 ℃ of oven dry.
Place the silicon dioxide gel that configures to permeate in a vacuum 10 hours bamboo charcoal powder, take out then in baking oven, make silicon dioxide gel generation gelation reaction, continue temperature oven dry with 120 ℃ with 60 ℃ temperature heating 4 hours.
At last, place charring furnace 1480 ℃ of charings under nitrogen protection to handle bamboo charcoal powder, soaking time is 2.5 hours, just obtains the surface ceramic deposition stephanoporate bamboo charcoal wave-suction material of carried magnetic cobalt metal.
Claims (6)
1. carried magnetic metallic surface potteryization stephanoporate bamboo charcoal wave-suction material, for natural bamboo after reaming, charing, the carried magnetic metal through the porous material of surface ceramic deposition, is characterized in that again: be magnetic metal and growth of duct, the inside load of material has the silicon carbide ceramics whisker.
2. according to the absorbing material of claim 1, it is characterized in that: absorbing material is the direct carried magnetic metal of bamboo charcoal, again through the porous material of surface ceramic deposition.
3. the preparation method of claim 1 or 2 described carried magnetic metallic surface potteryization stephanoporate bamboo charcoal wave-suction materials may further comprise the steps successively:
(1) the reaming processing and the charing of natural bamboo: soak in expanding agent at least 10 hours after will being processed into the bamboo chip drying of desired shape and size, the bamboo chip after will soaking then is 120 ℃ of oven dry; 800～1000 ℃ temperature, charing is 1～3 hour under protection of inert gas atmosphere, makes the bamboo charcoal sheet again;
(2) carried magnetic metal: bamboo charcoal sheet in (1) or bamboo charcoal were flooded 12 hours in the salts solution of magneticmetal at least, filter out then 120 ℃ of oven dry;
(3) sol impregnation: the product in (2) was soaked in vacuum environment in the silicon dioxide gel 8 hours at least, filters out then, make the silicon dioxide gel gelation, again 120 ℃ of oven dry in 60 ℃ of maintenances at least 3 hours;
(4) surface ceramic deposition: with the temperature of the product in (3) at 1450～1550 ℃, under protection of inert gas atmosphere, charing 1～3 hour makes the surface generate the silicon carbide ceramics layer, and inner duct forms the silicon carbide ceramics whisker.
4. according to the preparation method of claim 3, it is characterized in that: described expanding agent is sulfuric acid, nitric acid or the aqueous sodium hydroxide solution of 1～3mol/L.
5. according to the preparation method of claim 3, it is characterized in that: the salts solution of described magneticmetal is the salts solution of iron, cobalt, nickel metal or two or three mixing salt solution of above-mentioned metal.
6. according to the preparation method of claim 5, it is characterized in that: the concentration of salt solution of described magneticmetal is not less than 2mol/L.
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Cited By (7)
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| CN102503533A (en) * | 2011-10-25 | 2012-06-20 | 浙江大学 | Method for preparing silicon carbide honeycomb ceramics |
| CN103352322A (en) * | 2013-06-18 | 2013-10-16 | 浙江节节高炭业有限公司 | Method for preparing bamboo charcoal antibacterial fabric and bamboo charcoal antibacterial sanitary towel |
| CN104250442A (en) * | 2013-06-28 | 2014-12-31 | 深圳光启创新技术有限公司 | Microwave-absorbing composite material, preparation method of microwave-absorbing composite material, metamaterial and use of metamaterial |
| CN106495680A (en) * | 2016-11-08 | 2017-03-15 | 太原科技大学 | Carried magnetic metal simple-substance sheet calcium hexaluminate microwave absorbing ceramic compound material preparation method |
| CN106520071A (en) * | 2016-12-06 | 2017-03-22 | 吉林大学 | Rice husk based C/magnetic Co particle composite wave absorber and preparation method thereof |
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| CN113453524A (en) * | 2021-04-23 | 2021-09-28 | 中南林业科技大学 | Magnetic metal composite material based on bamboo-wood three-dimensional hole frame and preparation method and application thereof |
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2008
- 2008-04-25 CN CNB2008101049768A patent/CN100569701C/en not_active Expired - Fee Related
Cited By (13)
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| CN102503533A (en) * | 2011-10-25 | 2012-06-20 | 浙江大学 | Method for preparing silicon carbide honeycomb ceramics |
| CN102503533B (en) * | 2011-10-25 | 2013-06-05 | 浙江大学 | Method for preparing silicon carbide honeycomb ceramics |
| CN103352322A (en) * | 2013-06-18 | 2013-10-16 | 浙江节节高炭业有限公司 | Method for preparing bamboo charcoal antibacterial fabric and bamboo charcoal antibacterial sanitary towel |
| CN103352322B (en) * | 2013-06-18 | 2015-08-05 | 浙江节节高炭业有限公司 | A kind of preparation method of bamboo charcoal antibacterial cloth and bamboo charcoal antibacterial sanitary napkin |
| CN104250442A (en) * | 2013-06-28 | 2014-12-31 | 深圳光启创新技术有限公司 | Microwave-absorbing composite material, preparation method of microwave-absorbing composite material, metamaterial and use of metamaterial |
| CN104250442B (en) * | 2013-06-28 | 2016-12-28 | 深圳光启创新技术有限公司 | Wave suction composite material and preparation method thereof, Meta Materials and application thereof |
| CN106495680A (en) * | 2016-11-08 | 2017-03-15 | 太原科技大学 | Carried magnetic metal simple-substance sheet calcium hexaluminate microwave absorbing ceramic compound material preparation method |
| CN106495680B (en) * | 2016-11-08 | 2019-04-05 | 太原科技大学 | The sheet calcium hexaluminate microwave absorbing ceramic compound material preparation method of carried magnetic metal simple-substance |
| CN106520071A (en) * | 2016-12-06 | 2017-03-22 | 吉林大学 | Rice husk based C/magnetic Co particle composite wave absorber and preparation method thereof |
| CN106520071B (en) * | 2016-12-06 | 2018-05-25 | 吉林大学 | Rice husk base carbon/magnetism Co particle composite wave-absorbing agent and preparation method thereof |
| CN107394414A (en) * | 2017-07-18 | 2017-11-24 | 东南大学 | Wave absorbing device based on double-layer magnetic media implementation low-frequency range broadened bandwidth |
| CN107394414B (en) * | 2017-07-18 | 2020-07-31 | 东南大学 | Wave absorber for realizing low-frequency band bandwidth broadening based on double-layer magnetic medium |
| CN113453524A (en) * | 2021-04-23 | 2021-09-28 | 中南林业科技大学 | Magnetic metal composite material based on bamboo-wood three-dimensional hole frame and preparation method and application thereof |
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