CN103408899B - Tree-like structure micro-nano wave absorption agent/epoxy resin composite wave absorption material preparation method - Google Patents
Tree-like structure micro-nano wave absorption agent/epoxy resin composite wave absorption material preparation method Download PDFInfo
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Abstract
The present invention relates to a tree-like structure micro-nano wave absorption agent/epoxy resin composite wave absorption material preparation method, which specifically comprises: adopting polymer base hollow porous fibers as a raw material to obtain nano-scale stem hollow porous carbon fibers, adopting a vapor deposition method in a tubular furnace to grow nano-scale branch carbon nano-tubes on the surface of the stem structure and inside the stem structure to obtain a stem-branch composite carbon material, soaking the composite carbon material in a metal solution, drying, introducing hydrogen to reduce so as to load metal particle fruits on the stem-branch structure in an in situ manner to obtain a tree-like structure micro-nano wave absorption agent, and adding the wave absorption agent to an epoxy resin to cure to obtain the wave absorption stealth composite material. The tree-like structure micro-nano wave absorption agent/epoxy resin composite wave absorption material has the following characteristics that: characteristics of microporous structure, high specific surface area, high dielectric constant, and high magnetic permeability are provided, respective effects and synergistic coupling effects of hollow porous carbon fibers, carbon nano-tubes and metal particles can be provided, an excellent wave absorption performance is provided, and the composite wave absorption material has an excellent radar X-wave band wave absorption performance.
Description
Technical field
The invention belongs to the interleaving techniques field of porous carbon materials and nano material, being specifically related to a kind of is that matrix adopts vapour deposition process to prepare the preparation method of porous carbon fiber carbon nano-tube and " class tree construction " wave absorbing agent of loaded with nano metal particles and the composite wave-suction material with epoxy resin thereof with hollow carbon fibers.
Background technology
For taking hollow carbon fibers as the preparation method that matrix employing vapour deposition process prepares " class tree construction " wave absorbing agent of porous carbon fiber carbon nano-tube and loaded with nano metal particles thereof, yet there are no corresponding report at home and abroad, under regard to the research background that the present invention is correlated with and be introduced explanation.
Along with improving constantly of countries in the world military technique, wave-absorbing and camouflage technology as a kind ofly improving weapons system existence, break through and the effective means of deep strike ability, with laser, cruise missile be called the three great revolutionary movements of modern military technology.Wherein radar invisible is the emphasis of stealthy technique, accounts for more than 60% of stealthy technique.And to develop radar stealth technology main path be the efficient radar absorbings of research and development, the development of radar absorbing and use, to the development of future military, there is extremely important meaning.Traditional absorption agent ferrite, metal fine powder, silicon carbide and graphite isodensity are comparatively large, and mechanical property is bad; Its major absorbance peak of primary carbon nanotube is at C frequency range (4 ~ 8GHz), and the look-in frequency of short range tracking radar, maritime radar or missile-guidance radar is positioned at X frequency range (8 ~ 12GHz), therefore, grow primary carbon nanotube and loaded with nano metal particles with the hollow carbon fibers that density is little and at X-band, there is good assimilation effect as the epoxy resin composite material of absorbent preparation.
Hollow carbon fibers is a kind of porous carbon fiber with hollow structure, is a kind of new carbon developed in recent years.Hollow carbon fibers inside has hollow structure, and internal diameter is generally between 20-100 μm, and wall thickness is 1/4-1/10 of internal diameter.Its surfaces externally and internally respectively has the microporous layers that one deck is very thin, and the atomic hole rich content of below 1nm, adds in upper wall and also has abundant micropore, makes hertzian wave that reflection repeatedly, refraction and loss can occur between hole.Meanwhile, hollow carbon fibers is a kind of good dielectric materials, has fine electroconductibility, good absorption of electromagnetic wave ability.
Carbon nanotube is a kind of important new carbon, its large length-to-diameter ratio and stratiform hollow structure, and high specific inductivity gives its very large specific surface area and excellent wave-sucking performance.In addition, carbon nanotube also has strong mechanical performance, stablizes the feature such as physicochemical property and high reaction activity, in numerous wave absorbing agent, have obvious superiority, is used widely in invisbile plane and Stealth weapon.Nano-metal particle then has high magnetic permeability and very excellent magnetic loss characteristic, is a kind of good absorbing material.
It is that matrix adopts vapour deposition process to prepare the preparation method of porous carbon fiber carbon nano-tube and " class tree construction " wave absorbing agent of loaded with nano metal particles and the composite wave-suction material with epoxy resin thereof with hollow carbon fibers that the present invention proposes a kind of.Three kinds of wave absorbing agents of different nature are proposed----hollow carbon fibers, carbon nanotube and nano-metal particle carry out the new system organically combined, and realize composite wave-suction material have good assimilation effect at X-band by dielectric loss and magnetic loss effect.This is the preparation method of novel wave-absorbing material of a kind of low cost, easy to operate, high yield, and design and the preparation science of absorbing material have been enriched in research, have important directive significance to novel wave-absorbing material research and development.
Summary of the invention
The object of the present invention is to provide a kind of is that matrix adopts vapour deposition process to prepare the preparation method of porous carbon fiber carbon nano-tube and " class tree construction " wave absorbing agent of loaded with nano metal particles and the composite wave-suction material with epoxy resin thereof with hollow carbon fibers.By carbon nano-tube on hollow carbon fibers and loaded with nano metal particles, make " class tree construction " wave absorbing agent/epoxy resin composite wave-absorbing material in X-band, have good assimilation effect.
The preparation method of class tree construction micro-nano wave absorbing agent/epoxy resin composite wave-absorbing material that the present invention proposes, described absorbing material is class tree construction, comprise the micron order hollow carbon fibers being positioned at " doing " portion, be positioned at the nano-scale carbon nanotube in " branch " portion, be positioned at the nanoscale metal particles in " really " portion; Concrete steps are as follows:
(1) " do "---the preparation of-micron order hollow carbon fibers: using the polymer-based carbon hollow porous fiber of purifying as raw material, after being cut into the staple fibre of 3 ~ 5cm, preoxidation 1 ~ 3h at 200 ~ 300 DEG C; The sample of gained is at 600 ~ 950 DEG C, and carbonization in rare gas element, carbonization time is 30 ~ 120min, then utilizes CO
2gas activates, and activation temperature is 600 ~ 950 DEG C, and soak time is 20 ~ 120 min, obtains hollow carbon fibers;
(2) " dry-branch " structure---preparation of-hollow carbon fibers/carbon nanotube: the hollow carbon fibers that step (1) obtains is immersed in and has in the metallic solution of katalysis, magnetic agitation 5 ~ 48h, carry out suction filtration, dry, apply vapour deposition process again, rare gas element is passed through successively in tube furnace, hydrogen and carbon-source gas, thus obtain all growing at the surfaces externally and internally of hollow carbon fibers " dry-branch " structure having carbon nanotube, wherein, logical hydrogen reducing metallic solution 30 ~ 120min at 400 ~ 700 DEG C of temperature, logical carbon-source gas carbon nano-tube 30 ~ 120min at 500 ~ 900 DEG C of temperature,
(3) preparation of " class tree construction " micro-nano wave absorbing agent: the hollow carbon fibers/carbon nanotube-sample obtained in step (2) is immersed in 5 ~ 48h in metallic solution, after carrying out suction filtration and drying, in tube furnace, applied chemistry vapour deposition process first logical rare gas element raised temperature to 400 DEG C gradually, then be 400 ~ 700 DEG C of logical hydrogen 30 ~ 120min reducing metal solution in temperature, what obtain in quartz boat is " class tree construction " micro-nano wave absorbing agent;
(4) preparation of wave-absorbing and camouflage composite material: " class tree construction " the micro-nano wave absorbing agent in step (3) is mixed in proportion with epoxy resin and solidifying agent, curing reaction aftershaping, its working method is: take 50 ~ 100g epoxy resin, be positioned over 1-2h in 80 DEG C of baking ovens, during this period, taking mass ratio is that 1-5% " class tree construction " micro-nano wave absorbing agent is placed in acetone soln, constant temperature water bath 80-100 DEG C, add the epoxy resin of preheating under high velocity agitation, treat that acetone volatilizees completely, add solidifying agent (mass ratio of solidifying agent and epoxy resin is 1:10), pour into after high-speed stirring 5-10min in mould, de-bubble, solidification, finally have to " class tree construction " micro-nano wave absorbing agent/epoxy resin composite wave-absorbing material.
In the present invention, the polymer-based carbon hollow porous fiber described in step (1) is any one in polyacrylonitrile-radical hollow porous fiber, polypropylene-base hollow porous fiber, polyvinylidene fluoride hollow porous fiber, PVA-based hollow porous fiber or polytetrafluoroethylene (PTFE) base hollow porous fiber etc.
In the present invention, the metallic solution with katalysis described in step (2) be in nickelous nitrate, nickel oxide, nickelous chloride, single nickel salt, iron nitrate, ferrocene, ferric oxide, iron(ic) chloride, ferric sulfate, cobalt oxide, cobalt chloride, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES, rose vitriol or Vanadium Pentoxide in FLAKES etc. any one or organize combination more.Be wherein preferred with nickelous nitrate, iron nitrate or ferrocene metallic solution.
In the present invention, the carbon-source gas described in step (2) is any one in ethanol, methyl alcohol, ethane, methane, ethene, benzene, toluene or dimethylbenzene etc.Be wherein preferred with dehydrated alcohol carbon-source gas.
In the present invention, the metallic solution described in step (3) be in nickelous nitrate, nickel oxide, nickelous chloride, single nickel salt, iron nitrate, ferrocene, ferric oxide, iron(ic) chloride, ferric sulfate, cobalt oxide, cobalt chloride, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES, rose vitriol or Vanadium Pentoxide in FLAKES etc. any one or organize combination more.Be wherein preferred with iron nitrate or ferrocene metallic solution.
In the present invention, the epoxy resin described in step (4) is the one in bisphenol A-type E-51, E-44, E-42 or E-54 type epoxy resin.
In the present invention, the solidifying agent described in step (4) is the one in aromatic series agent solidifying agent phenylenediamine, two aminodiphenylmethane, two amido sulfobenzides, diethylenetriamine, tetraethylene pentamine or triethylene tetramine.
Superiority of the present invention:
(1) the present invention adopts a kind of superpolymer base hollow porous fiber to be that hollow carbon fibers prepared by raw material, and on hollow carbon fibers load carbon nanotube and nano-metal particle thus prepare the method for " class tree construction " wave absorbing agent, technique is simple, easy to operate, processing and manufacturing is with low cost, has great practical value.
(2) the present invention's nature and role of utilizing hollow carbon fibers pore structure special, can make incident electromagnetic wave multiple reflections, refraction etc. occur between hole and maximized loss hertzian wave, reach the object of electromagnetic wave absorption; And on the hollow carbon fibers carbon nano-tube that density is little and original position loaded with nano metal particles, make " class tree construction " wave absorbing agent have higher specific inductivity and magnetic permeability, reach, in X-band, there is good assimilation effect.
(3) the present invention adopts chemical Vapor deposition process to be prepared wave absorbing agent, and this method is very ripe, and parameter easily controls, and is easy to realize industrialization.
Accompanying drawing explanation
Fig. 1 is the suction ripple test curve of " class tree construction " wave absorbing agent prepared by embodiments of the invention 1.
Fig. 2 is the suction ripple test curve of " class tree construction " wave absorbing agent prepared by embodiments of the invention 2.
Fig. 3 is the suction ripple test curve of " class tree construction " wave absorbing agent prepared by embodiments of the invention 3.
Embodiment
The following examples further illustrate of the present invention, instead of limit the scope of the invention.
embodiment 1:(1) " do "---the preparation of-micron order hollow carbon fibers: polyacrylonitrile hollow porous fiber (PANHF) is cut into 3 ~ 5cm, to be immersed in dehydrated alcohol after 24h dry 8h at 80 DEG C, to make fiber purifying; After in the baking oven of 230 DEG C preoxidation 1h, temperature rise rate is 1.5 DEG C/min; The sample of gained is placed in quartz boat, and quartz boat is put into tube furnace.Under the condition of logical inert nitrogen gas, raise the temperature in tube furnace gradually, temperature rise rate is 1.5 DEG C/min, and when temperature reaches 700 DEG C carbonizedfibres 60min, make the carbonization of PAN preoxided thread, thus finally obtain hollow carbon fibers (HPCF).
(2) " dry-branch " structure---preparation of-hollow carbon fibers/carbon nanotube: the nickel nitrate solution 50ml of configuration 0.1mol/L, the HPCF0.5g of preparation is flooded wherein and magnetic agitation 5h, rear taking-up suction filtration and at 80 DEG C dry 8h, obtain the hollow carbon fibers that the equal load of surfaces externally and internally has nickel salts.Then to put it in quartz boat and to be placed in tube furnace.Arranging temperature rise rate is 4.5 DEG C/min, under the protection of inert nitrogen gas, heats up gradually, and 400 DEG C time, passes into hydrogen, constant temperature 60min, then stops passing into of hydrogen.Under the protection of nitrogen, be warming up to 700 DEG C, pass into carbon source dehydrated alcohol gas; constant temperature 60min; finally stop passing into of dehydrated alcohol gas, at the protection borehole cooling of nitrogen, thus obtain there is the hollow carbon fibers (HPCF-CNTs) of carbon nanotube on surface and inner all length.
(3) preparation of " class tree construction " micro-nano wave absorbing agent: " dry-branch " structure of getting a certain amount of HPCF-CNTs, is immersed in 5h in the nickelous nitrate metallic solution of 0.3mol/L, rear suction filtration, drying.Then to put it in quartz boat and to be placed in tube furnace.Arranging temperature rise rate is 4.5 DEG C/min, under the protection of inert nitrogen gas, heats up gradually, and 400 DEG C time, passes into hydrogen, constant temperature 120min, then stops passing into of hydrogen, and reduction obtains metallic particles load in the surface of fiber and inside.Under the protection of nitrogen, lower the temperature gradually, final obtained " class tree construction " wave absorbing agent (ACHF-CNTs-Ni).
(4) preparation of wave-absorbing and camouflage composite material: claim epoxy resin (E-44) 240.00g, be positioned in hollow baking oven, be warming up to 120 DEG C, constant temperature 1h, to remove the bubble in epoxy resin.Under maintenance vacuum tightness-0.1MPa, take out epoxy resin after slow cooling to 120 DEG C, pour there-necked flask into, oil bath constant temperature 90 DEG C." class tree construction " wave absorbing agent of certain mass ratio is added in epoxy resin under high velocity agitation, ultrasonic 0.5h.Add 60.00g phenylenediamine solidifying agent, pour in 180mm*180mm mould after high-speed stirring 5min, 2h at 80 DEG C, 4h at 160 DEG C, final obtained " class tree construction " micro-nano wave absorbing agent/epoxy resin composite wave-absorbing material.
Fig. 1 is the suction ripple test curve that embodiment 1 prepares " class tree construction " wave absorbing agent.There is an absorption peak at X-band (8-12GHz) in this wave absorbing agent as can be seen from Figure 1, there is good wave-absorbing effect, maximum absorption band appears at the 9.25GHz place in X-band, and the frequency range of maximum absorption band is 7.2GHz (R <-5dB).
embodiment 2:(1) " do "---the preparation of-micron order hollow carbon fibers: staple fibre polypropylene-base hollow porous fiber (PPHF) being cut into 3 ~ 5cm, after to be immersed in dehydrated alcohol after 24h dry 8h at 80 DEG C, make fiber purifying.The PPHF of purifying is immersed in 24h in the resol (PF) being dissolved in ethanolic soln, then each 2h at 50 DEG C, 80 DEG C, 120 DEG C and 170 DEG C, the PF resin being adsorbed on fiber surface is slowly solidified, finally obtain load and have PF resin as the sample P PHF-PF of presoma, then the sample P PHF-PF of gained is placed in quartz boat, and quartz boat is put into tube furnace.Under the condition of logical inert nitrogen gas, raise the temperature in tube furnace gradually, temperature rise rate is 2.5 DEG C/min, and when temperature reaches 650 DEG C carbonizedfibres 60min, the PPHF fiber as template is burnt, phenolic resin carbonized, then CO2 is utilized to activate, activation temperature is 800 DEG C, and soak time is 50 min, finally obtains hollow porous active carbon fiber (ACHF).
(2) " dry-branch " structure---preparation of-hollow carbon fibers/carbon nanotube: the nickel nitrate solution 50ml of configuration 0.1mol/L, the ACHF0.5g of preparation is flooded wherein 5h, rear taking-up suction filtration and at 80 DEG C dry 8h, obtain the hollow carbon fibers that the equal load of surfaces externally and internally has nickel salts.All the other steps, with embodiment 1, obtain there is the hollow carbon fibers (ACHF-CNTs) of carbon nanotube on surface and inner all length.
(3) preparation of " class tree construction " micro-nano wave absorbing agent: " dry-branch " structure of getting a certain amount of ACHF-CNTs, is immersed in 5h in the nickelous nitrate metallic solution of 0.1mol/L, rear suction filtration, drying.Then to put it in quartz boat and to be placed in tube furnace.Arranging temperature rise rate is 4.5 DEG C/min, under the protection of inert nitrogen gas, heats up gradually, and 400 DEG C time, passes into hydrogen, constant temperature 60min, then stops passing into of hydrogen, and reduction obtains metallic particles load in the surface of fiber and inside.Under the protection of nitrogen, lower the temperature gradually, final obtained " class tree construction " wave absorbing agent (ACHF-CNTs-Ni).
(4) preparation of wave-absorbing and camouflage composite material: claim epoxy resin (E-51) 200.00g, be positioned over 2h in 80 DEG C of baking ovens, make resin preheating, viscosity reduces, during this period, by solidifying agent 4, 4 diaminodiphenylmethane (DDM) at 90 DEG C down to melting completely, taking mass ratio is that 1-5% " class tree construction " micro-nano wave absorbing agent is placed in the ultrasonic 30min of a certain amount of acetone soln, after add in the epoxy resin of preheating, constant temperature water bath 80 DEG C, and high-speed stirring is volatilized completely to acetone, take out, add 50gDDM solidifying agent, pour into after high-speed stirring 5-10min on the mould of 180mm*180mm, 2h at 80 DEG C, 4h at 160 DEG C, final obtained " class tree construction " micro-nano wave absorbing agent/epoxy resin composite wave-absorbing material.
Fig. 2 is the suction ripple test curve that embodiment 2 prepares " class tree construction " wave absorbing agent.There is biabsorption peak at X-band (8-12GHz) in this wave absorbing agent as can be seen from Figure 2, there is good wave-absorbing effect, the 10.5GHz place that maximum absorption band appears in X-band is-31.036dB, and the frequency range of maximum absorption band is 7.1GHz (R <-5dB).
embodiment 3:(1) " do "---the preparation of-micron order hollow carbon fibers: polyacrylonitrile hollow porous fiber (PANHF) is cut into 3 ~ 5cm, to be immersed in dehydrated alcohol after 24h dry 8h at 80 DEG C, to make fiber purifying; After in the baking oven of 230 DEG C preoxidation 1h, temperature rise rate is 1.5 DEG C/min; The sample of gained is placed in quartz boat, and quartz boat is put into tube furnace.Under the condition of logical inert nitrogen gas, raise the temperature in tube furnace gradually, temperature rise rate is 2.5 DEG C/min, and when temperature reaches 700 DEG C carbonizedfibres 60min, make the carbonization of PAN preoxided thread, thus finally obtain hollow carbon fibers (HPCF).
(2) " dry-branch " structure---preparation of-hollow carbon fibers/carbon nanotube: the nickel nitrate solution 50ml of configuration 0.1mol/L, the HPCF0.5g of preparation is flooded wherein and magnetic agitation 5h, rear taking-up suction filtration and at 80 DEG C dry 8h, obtain the hollow carbon fibers that the equal load of surfaces externally and internally has nickel salts.Then to put it in quartz boat and to be placed in tube furnace.Arranging temperature rise rate is 4.5 DEG C/min, under the protection of inert nitrogen gas, heats up gradually, and 400 DEG C time, passes into hydrogen, constant temperature 60min, then stops passing into of hydrogen.Under the protection of nitrogen, be warming up to 700 DEG C, pass into carbon source dehydrated alcohol gas; constant temperature 60min; finally stop passing into of dehydrated alcohol gas, at the protection borehole cooling of nitrogen, thus obtain there is the hollow carbon fibers (HPCF-CNTs) of carbon nanotube on surface and inner all length.
(3) preparation of " class tree construction " micro-nano wave absorbing agent: " dry-branch " structure of getting a certain amount of HPCF-CNTs, is immersed in 5h in the nickelous nitrate metallic solution of 0.2mol/L, rear suction filtration, drying.Then to put it in quartz boat and to be placed in tube furnace.Arranging temperature rise rate is 4.5 DEG C/min, under the protection of inert nitrogen gas, heats up gradually, and 400 DEG C time, passes into hydrogen, constant temperature 90min, then stops passing into of hydrogen, and reduction obtains metallic particles load in the surface of fiber and inside.Under the protection of nitrogen, lower the temperature gradually, final obtained " class tree construction " wave absorbing agent (HPCF-CNTs-Ni).
(4) preparation of wave-absorbing and camouflage composite material: claim epoxy resin (E-51) 85.00g, be positioned over 2h in 80 DEG C of baking ovens, make resin preheating, viscosity reduces, during this period, taking mass ratio is that 1-5% " class tree construction " micro-nano wave absorbing agent is placed in the ultrasonic 30min of a certain amount of acetone soln, after add in the epoxy resin of preheating, constant temperature water bath 80 DEG C, and high-speed stirring is volatilized completely to acetone, take out, add 8.5g triethylene tetramine solidifying agent, be brushed to after high-speed stirring 5-10min on the iron plate of 180mm*180mm, cured at room temperature, final obtained " class tree construction " micro-nano wave absorbing agent/epoxy resin composite wave-absorbing material.
Fig. 3 is the suction ripple test curve that embodiment 3 prepares " class tree construction " wave absorbing agent.There is an absorption peak at X and Ku wave band (8-18GHz) in this wave absorbing agent as can be seen from Figure 3, there is good wave-absorbing effect, the 12.55GHz place that maximum absorption band appears in Ku wave band is-50.305dB, and the frequency range of maximum absorption band is 9.0GHz (R <-5dB).
The absorbing property detected result of " class tree construction " wave absorbing agent that table 1 is prepared for embodiment 1-3.
" class tree construction " wave absorbing agent that as can be seen from Table 1 prepared by each embodiment has excellent suction wave system energy at X-band.
Table 1:
Claims (7)
1. the preparation method of a kind tree construction micro-nano wave absorbing agent/epoxy resin composite wave-absorbing material, it is characterized in that, described absorbing material is class tree construction, comprise the micron order hollow carbon fibers being positioned at " doing " portion, be positioned at the nano-scale carbon nanotube in " branch " portion, be positioned at the nanoscale metal particles in " really " portion; Concrete steps are as follows:
(1) " do "---the preparation of-micron order hollow carbon fibers: using the polymer-based carbon hollow porous fiber of purifying as raw material, after being cut into the staple fibre of 3 ~ 5cm, preoxidation 1 ~ 3h at 200 ~ 300 DEG C; The sample of gained is at 600 ~ 950 DEG C, and carbonization in rare gas element, carbonization time is 30 ~ 120min, then utilizes CO
2gas activates, and activation temperature is 600 ~ 950 DEG C, and soak time is 20 ~ 120 min, obtains hollow carbon fibers;
(2) " dry-branch " structure---preparation of-hollow carbon fibers/carbon nanotube: the hollow carbon fibers that step (1) obtains is immersed in and has in the metallic solution of katalysis, magnetic agitation 5 ~ 48h, carry out suction filtration, dry, apply vapour deposition process again, rare gas element is passed through successively in tube furnace, hydrogen and carbon-source gas, thus obtain all growing at the surfaces externally and internally of hollow carbon fibers " dry-branch " structure having carbon nanotube, wherein, logical hydrogen reducing metallic solution 30 ~ 120min at 400 ~ 700 DEG C of temperature, logical carbon-source gas carbon nano-tube 30 ~ 120min at 500 ~ 900 DEG C of temperature,
(3) preparation of " class tree construction " micro-nano wave absorbing agent: the hollow carbon fibers/carbon nanotube-sample obtained in step (2) is immersed in 5 ~ 48h in metallic solution, after carrying out suction filtration and drying, in tube furnace, applied chemistry vapour deposition process first logical rare gas element raised temperature to 400 DEG C gradually, then be 400 ~ 700 DEG C of logical hydrogen 30 ~ 120min reducing metal solution in temperature, what obtain in quartz boat is " class tree construction " micro-nano wave absorbing agent;
(4) preparation of wave-absorbing and camouflage composite material: " class tree construction " the micro-nano wave absorbing agent in step (3) is mixed in proportion with epoxy resin and solidifying agent, curing reaction aftershaping, its working method is: take 50 ~ 100g epoxy resin, be positioned over 1-2h in 80 DEG C of baking ovens, during this period, taking mass ratio is that 1-5% " class tree construction " micro-nano wave absorbing agent is placed in acetone soln, constant temperature water bath 80-100 DEG C, add the epoxy resin of preheating under high velocity agitation, treat that acetone volatilizees completely, add solidifying agent, the mass ratio 1:10 of solidifying agent and epoxy resin, pour into after high-speed stirring 5-10min in mould, de-bubble, solidification, finally obtain " class tree construction " micro-nano wave absorbing agent/epoxy resin composite wave-absorbing material.
2. the preparation method of class tree construction micro-nano wave absorbing agent/epoxy resin composite wave-absorbing material according to claim 1, is characterized in that polymer-based carbon hollow porous fiber described in step (1) is any one in polyacrylonitrile-radical hollow porous fiber, polyvinylidene fluoride hollow porous fiber, PVA-based hollow porous fiber or polytetrafluoroethylene (PTFE) base hollow porous fiber.
3. the preparation method of class tree construction micro-nano wave absorbing agent/epoxy resin composite wave-absorbing material according to claim 1, the metallic solution that it is characterized in that having described in step (2) katalysis is any one in nickelous nitrate, nickel oxide, nickelous chloride, single nickel salt, iron nitrate, ferrocene, ferric oxide, iron(ic) chloride, ferric sulfate, cobalt oxide, cobalt chloride, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES, rose vitriol or Vanadium Pentoxide in FLAKES.
4. the preparation method of class tree construction micro-nano wave absorbing agent/epoxy resin composite wave-absorbing material according to claim 1, is characterized in that carbon-source gas described in step (2) is any one in ethanol, methyl alcohol, ethane, methane, ethene, benzene, toluene or dimethylbenzene.
5. the preparation method of class tree construction micro-nano wave absorbing agent/epoxy resin composite wave-absorbing material according to claim 1, is characterized in that metallic solution described in step (3) is any one in nickelous nitrate, nickel oxide, nickelous chloride, single nickel salt, iron nitrate, ferrocene, ferric oxide, iron(ic) chloride, ferric sulfate, cobalt oxide, cobalt chloride, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES, rose vitriol or Vanadium Pentoxide in FLAKES.
6. the preparation method of class tree construction micro-nano wave absorbing agent/epoxy resin composite wave-absorbing material according to claim 1, is characterized in that epoxy resin described in step (4) is the one in bisphenol A-type E-51, E-44, E-42 or E-54 type epoxy resin.
7. the preparation method of class tree construction micro-nano wave absorbing agent/epoxy resin composite wave-absorbing material according to claim 1, is characterized in that described in step (4), solidifying agent is aromatic curing agent phenylenediamine.
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| CN113278255B (en) * | 2021-05-19 | 2022-03-25 | 湖南飞鸿达新材料有限公司 | High-frequency-band heat-conduction wave-absorbing insulating pad with heat conductivity and wave absorption |
| CN115450212B (en) * | 2022-09-16 | 2023-06-06 | 山东省公路桥梁建设集团有限公司 | High-steep slope pile foundation construction method based on concrete retaining wall |
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| CN101503579A (en) * | 2009-03-06 | 2009-08-12 | 清华大学 | Preparation of surface load magnetic alloy particle carbon nano-tube composite material |
| CN102461361A (en) * | 2009-04-24 | 2012-05-16 | 应用纳米结构方案公司 | Cnt-infused emi shielding composite and coating |
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