CN103317734B - Method for preparing radar wave-absorbing composite material based on carbon nanometer film - Google Patents
Method for preparing radar wave-absorbing composite material based on carbon nanometer film Download PDFInfo
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- CN103317734B CN103317734B CN201210073837.XA CN201210073837A CN103317734B CN 103317734 B CN103317734 B CN 103317734B CN 201210073837 A CN201210073837 A CN 201210073837A CN 103317734 B CN103317734 B CN 103317734B
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Abstract
The invention provides a method for preparing a radar wave-absorbing composite material based on a carbon nanometer film, comprising the following steps of: mixing carbon nanotubes and an anion surface dispersant, grinding the mixture in a mortar, pouring the grinded mixture into a beaker, and adding plasma water; dispersing and defoaming an obtained mixed solution in a magnetic stirrer; adding graphene oxide into plasma water to preparing a solution, and ultrasonically dispersing; mixing a carbon nanotube solution and the graphene oxide solution, centrifuging the mixture after ultrasonically dispersing by an ultrasonic cell disruption instrument, and compacting and solidifying residue after vacuum pumping filtration of a supernatant of the carbon nanotube and graphene oxide solution; heat-treating; adding a carbon nanometer film into an acetone weak solution of a resin for pre-infiltrating, and then drying; and adding the carbon nanometer filmed with layer pre-infiltration into an innermost layer of an aluminium alloy mould, laying a layer of carbon fiber/resin pre-infiltrated material in the medium, locking the mould, and molding by mould compression. A radar wave reflection rate of the radar wave-absorbing composite material based on the carbon nanometer film in a frequency range from 8GHz to 18GHz is lower than -10- -20dB.
Description
Technical field
The present invention relates to a kind of Wave suction composite material preparation method, particularly relate to a kind of radar-wave absorbing composite material and preparation method thereof based on carbon nanocapsule thin film, belong to materials science field.
Background technology
Radar-wave absorbing technology, as the existence of increase Modern weapon system and air defence ability, improves the effective means of overall fighting efficiency, is subject to the great attention of each military power of the world.Radar absorbing converts incident radar wave to heat energy mainly through the mode of dielectric loss and magnetic loss and loses.Radar-wave absorbing agent is mainly golden powder and the fiber of representative with ferrite, and the processing technology of this type of absorbing material is complicated, and density is comparatively large, the weakness such as environmental suitability is poor.It is reported, F117 seldom launches an attack in the rainy day, exactly because the moist hydraulic performance decline that can make absorbing material.
Since CNT found from 1991, the mechanics of its uniqueness, electricity, optics and magnetic performance cause the extensive concern of global scientist.Due to actings in conjunction such as the small-size effect of CNT, quantum size effect and macro quanta tunnel effects, the level spacing after its electron energy level is divided is within the scope of microwave energy.CNT has great specific area and a large amount of surface dangling bonds simultaneously, and cause interfacial polarization and multiple scattering to introduce new mechanism, further enhance its absorbing property, the chiral structure of CNT is also conducive to improving its absorbing property.These peculiar performances all have potential using value predictive of it preparing in stealth material, and absorbing material prepared by CNT and polymer compound has become one of important directions that modern radar absorbing material develops.
But carbon nanotube molecule intermolecular forces is large, when in polymeric matrix, dispersion amount is larger, more trend towards reuniting, the specific area that CNT is huge simultaneously also can cause polymeric matrix viscosity to increase, cause composite material forming difficulty, thus affect the overall mechanical property of composite, also can cause the raising of cost simultaneously.And the wave absorbtion of composite is mainly determined by the content of CNT and dispersing uniformity, in order to obtain effective carbon nanotube network, usually the methods such as shearing stirring, three rollers stirrings and ultrasonic disperse are utilized, but the content of CNT is limited in resin matrix, the Wave suction composite material of preparation often cannot meet engineer applied requirement.
Carbon nano-tube film (carbon nanometer paper) is that a kind of CNT (single wall or many walls) intermolecular Van der Waals force that relies on is formed by connecting, by CNT and the film-form self-supporting 3-D solid structure that forms of space therebetween, it has high conductivity, electromagnetic property and mechanical property, it can be used as the functional layer of radar-wave absorbing composite, the shaping of bulk composite material structure and performance can not be affected, CNT is added compared in resin, carbon nano-tube film is formed by connecting by CNT completely, has more excellent electrical conductance and thunderstorm activity ability.
Graphene is the New Two Dimensional nano-carbon material that a class is made up of one deck carbon atom, is two-dimensional material the thinnest in the world at present.The intensity of grapheme material is the highest in known materials, and its conductive capability and current carrying density are all above SWCN best at present, and its excellent quantum hall effect (Quantua Hall effect) is also proven.After the solution of graphene oxide is mixed with CNT, the sidewall of CNT and the sheet interlayer of graphene oxide can produce strong π-π and interact, because graphene sheet layer has a large amount of hydrophilic functional groups, the dispersion effect of graphene oxide-carbon mano-tube composite in water can be increased, be beneficial to the shaping of carbon nanometer paper, also can increase the intensity of carbon nanometer paper and electric conductivity and electromagnetic performance simultaneously.
In addition, utilize plating nickel on surface CNT to prepare carbon nano-tube film, change dielectric constant and the electromagnetic constant of carbon nano-tube film, thus regulate wave absorbed crest value and the frequency separation of radar-wave absorbing composite.
Summary of the invention
Based on a radar-wave absorbing composite material and preparation method thereof for carbon nanocapsule thin film, realized by following steps:
(1) get CNT to mix in 1: 1-1: 20 ratios with anionic surface dispersant, wherein select commercially available many walls/single wall nickel-plating carbon nanotube, its diameter is 6-30nm, and length is 10-50 μm, and nickel content is 20-70%.Anionic surface dispersant can select Bio-Rad-Laboratories, dodecyl sodium sulfate, one or both mixing in neopelex;
(2) CNT and anionic surface mixture of dispersing agents are put into mortar and grind 1-60min, pour beaker into, adding plasma water to carbon nanotube concentration is 0.01-1.0wt%, and Dispersion on surface agent concentration is 0.01-2wt%;
(3) pour in magnetic stirring apparatus by the mixed liquor of (2) step, control temperature, below 60 DEG C, disperses 15-60min; Froth breaking 10-100min;
(4) get CNT: the mass ratio of graphene oxide be 10: 1-10: 3 graphene oxide join in plasma water, be mixed with the solution of concentration 0.1-1mg/ml, ultrasonic disperse 30-60min;
(5) by CNT/graphene oxide solution mixing, then utilize ultrasonic cell disruption instrument under 100-800w condition, ultrasonic disperse 10-100min, dispersion temperature controls within the scope of 10-60 DEG C;
(6) CNT/graphene oxide dispersion is distributed in vitro, puts into centrifuge, and under rotating speed 1000-10000rpm condition, centrifugal treating 10-80min, chooses in vitro CNT/graphene oxide solution supernatant liquor;
(7) vacuum suction filter is selected to prepare carbon nanocapsule thin film, permeable membrane selects the permeable membrane of millipore company, wherein this permeable membrane can select nylon membrane, CN-CA, film, 0.22um or 0.45 μm is selected in aperture, the supernatant of CNT/graphene oxide dispersion is carried out vacuum filtration, vacuum pump pressure is controlled within the scope of 40-500Kpa, namely adopt vacuum filtration legal system for carbon nanocapsule thin film;
(8) after suction filtration completes, with the plasma water cleaning carbon nanocapsule thin film of 1-5 times of volume, until do not have foam to produce;
(9) together taken off by the carbon nanocapsule thin film of filter membrane and preparation, be placed between two corrosion resistant plates, compacting, puts into baking oven, under 60-150 DEG C of condition, solidify 2-10 hour, has solidified rear stripping and has obtained carbon nanocapsule thin film structure;
(10) carbon nanocapsule thin film structure puts into vacuum drying oven 300-350 DEG C of heat treatment 30-60min, and the electrical conductivity of carbon nanocapsule thin film reaches 100-2000S/m;
(11) by die size cutting carbon nanometer paper, put into the acetone diluted liquid of resin, pre-invasion 24-48 hour, put into dry 2-4 hour under 40 degree, baking oven, wherein resin can select epoxy resin or BMI;
(12) by 1-4 layer pre-invasion carbon nanocapsule thin film lay in aluminum alloy mould innermost layer, middle lay 8-24 layer carbon fiber/resin prepreg material, close die, utilize compression molding, radar-wave absorbing composite that autoclave molding prepares carbon nanocapsule thin film, wherein carbon fiber/resin prepreg material can select epoxy resin/carbon fiber, bimaleimide resin/carbon fiber prepreg.
The reflection of radar wave rate of radar-wave absorbing composite in 8-18GHz frequency range of the carbon nanocapsule thin film obtained by the present invention is less than-10dB--20dB.
Accompanying drawing explanation
The structural representation of Fig. 1 radar-wave absorbing composite
Detailed description of the invention
As described in Figure 1: carbon nanocapsule thin film is inhaled wave energy layer 1 and covered as on composite structural laminate 2.
Embodiment 1
(1) get CNT to mix in 1: 10 ratio with Bio-Rad-Laboratories, wherein select commercially available nickel plating many walls nickel-plating carbon nanotube, its diameter is 8-15nm, and length is 50 μm, and nickel content is 60%;
(2) CNT and anionic surface mixture of dispersing agents put into mortar grinding 40min, and pour beaker into, adding plasma water to carbon nanotube concentration is 0.03wt%, and Dispersion on surface agent concentration is 0.3wt%;
(3) mixed liquor is poured in magnetic stirring apparatus, and control temperature, below 60 DEG C, disperses 60min, froth breaking 40min;
(4) getting graphene oxide (CNT: the mass ratio of graphene oxide is 10: 1) joins in plasma water, is mixed with the solution of concentration 1mg/ml, ultrasonic disperse 60min;
(5) CNT/graphene oxide dispersion is distributed in vitro, then utilizes ultrasonic cell disruption instrument under 540w condition, ultrasonic disperse 45min, and dispersion temperature controls within the scope of 20-30 DEG C;
(6) CNT/graphene oxide dispersion is distributed in vitro, puts into centrifuge, and under rotating speed 4000rpm condition, centrifugal treating 40min, chooses in vitro CNT/graphene oxide solution supernatant liquor;
(7) vacuum suction filter is selected to prepare carbon nanocapsule thin film, permeable membrane selects the CN-CA of millipore company, membrane pore size selects 0.22 μm, the supernatant of CNT/graphene oxide dispersion is carried out vacuum filtration, vacuum pump pressure is controlled within the scope of 300Kpa, namely adopt vacuum filtration legal system for carbon nanocapsule thin film;
(8) after suction filtration completes, with the plasma water cleaning carbon nanometer paper of 3 times of volumes, until do not have foam to produce;
(9) together taken off by the carbon nanocapsule thin film of filter membrane and preparation, be placed between two corrosion resistant plates, compacting, puts into baking oven, solidifies 4 hours, solidified rear stripping and obtained carbon nanocapsule thin film structure under 120 DEG C of conditions;
(10) carbon nanocapsule thin film structure puts into vacuum drying oven 300 DEG C of heat treatment 60min, and the electrical conductivity of carbon nanocapsule thin film reaches 500S/m;
(11) by die size cutting carbon nanometer paper, put into the acetone diluted liquid of resin, pre-invasion 24 hours, to put under 40 degree, baking oven dry 2 hours, wherein resin can select epoxy resin, BMI;
(12) by 2 layers of pre-invasion carbon nanocapsule thin film lay in aluminum alloy mould innermost layer, middle lay 16 layers of carbon fiber/epoxy prepreg, close die, utilizes autoclave molding to prepare the radar-wave absorbing composite of carbon nanocapsule thin film; The reflection of radar wave rate of radar-wave absorbing composite in 8-18GHz frequency range of carbon nanocapsule thin film is less than-8dB.
Claims (6)
1., based on a radar-wave absorbing composite material and preparation method thereof for carbon nanocapsule thin film, realized by following steps:
(1) get CNT to mix by 1:1-1:20 mass ratio with anionic surface dispersant;
(2) by CNT with cloudyly put into mortar from Dispersion on surface agent composition and grind 1-60min, pour beaker into, adding plasma water to carbon nanotube concentration is 0.01-1.0wt%, and Dispersion on surface agent concentration is 0.01-2wt%;
(3) pour in magnetic stirring apparatus by the mixed liquor of (2) step, control temperature, at 20-60 DEG C, disperses 15-60min; Froth breaking 10-100min;
(4) CNT is got: the mass ratio of graphene oxide is that the graphene oxide of 10:1-10:3 joins in plasma water, is mixed with the solution of concentration 0.1-1mg/ml, ultrasonic disperse 30-60min;
(5) by CNT/graphene oxide solution mixing, then utilize ultrasonic cell disruption instrument under 100-800w condition, ultrasonic disperse 10-100min, dispersion temperature controls within the scope of 10-60 DEG C;
(6) CNT/graphene oxide dispersion is distributed in vitro, puts into centrifuge, and under rotating speed 1000-10000rpm condition, centrifugal treating 10-80min, chooses in vitro CNT/graphene oxide solution supernatant liquor;
(7) select vacuum suction filter to prepare carbon nanocapsule thin film, the supernatant of CNT/graphene oxide dispersion is carried out vacuum filtration, vacuum pump pressure is controlled within the scope of 40-500Kpa, namely adopt vacuum filtration legal system for carbon nanocapsule thin film;
(8) after suction filtration completes, with the plasma water cleaning carbon nanocapsule thin film of 1-5 times of volume, until do not have foam to produce;
(9) together taken off by the carbon nanocapsule thin film of filter membrane and preparation, be placed between two corrosion resistant plates, compacting, puts into baking oven, under 60-150 DEG C of condition, solidify 2-10 hour, has solidified rear stripping and has obtained carbon nanocapsule thin film structure;
(10) carbon nanocapsule thin film structure puts into vacuum drying oven 300-350 DEG C of heat treatment 30-60min, and the electrical conductivity of carbon nanocapsule thin film reaches 100-2000S/m;
(11) by die size cutting carbon nanocapsule thin film, put into the acetone diluted liquid of resin, pre-invasion 24-48 hours, put into dry 2-4 hour under 40 degree, baking oven;
(12) by 1-4 layer pre-invasion carbon nanocapsule thin film lay in aluminum alloy mould innermost layer, middle lay 8-24 layer carbon fiber/resin prepreg material, close die, utilizes compression molding, radar-wave absorbing composite that autoclave molding prepares carbon nanocapsule thin film.
2. a kind of radar-wave absorbing composite material and preparation method thereof based on carbon nanocapsule thin film as claimed in claim 1, it is characterized in that: described CNT is commercially available many walls/single wall nickel-plating carbon nanotube, its diameter is 6-30nm, and length is 10-50 μm, and nickel content is 20-70%.
3. a kind of radar-wave absorbing composite material and preparation method thereof based on carbon nanocapsule thin film as claimed in claim 1, it is characterized in that: described anionic surface dispersant selects Bio-Rad-Laboratories, dodecyl sodium sulfate, one or both mixing in neopelex.
4. a kind of radar-wave absorbing composite material and preparation method thereof based on carbon nanocapsule thin film as claimed in claim 1, it is characterized in that: in step (7), when vacuum suction filter prepares carbon nanocapsule thin film, permeable membrane selects the permeable membrane of millipore company, wherein this permeable membrane selects nylon membrane, CN-CA, and 0.22um or 0.45 μm is selected in aperture.
5. a kind of radar-wave absorbing composite material and preparation method thereof based on carbon nanocapsule thin film as claimed in claim 1, is characterized in that: in step (11), resin selects epoxy resin or BMI.
6. a kind of radar-wave absorbing composite material and preparation method thereof based on carbon nanocapsule thin film as claimed in claim 1, is characterized in that: in step (12), carbon fiber/resin prepreg material selects epoxy resin/carbon fiber or bimaleimide resin/carbon fiber prepreg.
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