CN103317734A - 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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- CN103317734A CN103317734A CN201210073837XA CN201210073837A CN103317734A CN 103317734 A CN103317734 A CN 103317734A CN 201210073837X A CN201210073837X A CN 201210073837XA CN 201210073837 A CN201210073837 A CN 201210073837A CN 103317734 A CN103317734 A CN 103317734A
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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, relate in particular 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
The radar-wave absorbing technology improves the effective means of overall fighting efficiency as increasing Modern weapon system existence and air defence ability, is subject to the great attention of each military power of the world.Radar absorbing mainly loses incident radar wave energy transform into heat energy by the mode of dielectric loss and magnetic loss.The weakness such as the radar-wave absorbing agent is golden powder and the fiber take ferrite as representative mainly, and the processing technology of this type of absorbing material is complicated, and density is larger, and environmental suitability is relatively 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.
CNT is since 1991 find, its unique mechanics, electricity, optics and magnetic performance have caused global scientist's extensive concern.Because the actings in conjunction such as small-size effect, quantum size effect and macro quanta tunnel effect of CNT are in the microwave energy scope level spacing after its electron energy level divides.CNT has great specific area and a large amount of surperficial dangling bonds simultaneously, causes interfacial polarization and multiple scattering to introduce new mechanism, has further strengthened its absorbing property, and the chiral structure of CNT also is conducive to improve its absorbing property.These peculiar performances have indicated that all it has potential using value in the preparation stealth material, and the absorbing material of CNT and the compound preparation of polymer has become one of important directions of modern radar absorbing material development.
But active force is large between carbon nanotube molecule, when dispersion amount is larger in polymeric matrix, more trend towards reuniting, the huge specific area of CNT also can cause the polymeric matrix viscosity to increase simultaneously, cause the composite material forming difficulty, thereby affect the whole mechanical property of composite, also can cause the raising of cost simultaneously.And the wave absorbtion of composite mainly is to be determined by the content of CNT and dispersing uniformity, in order to obtain effective carbon nanotube network, usually utilize the methods such as shearing stirring, the stirring of three rollers and ultrasonic dispersion, but the content of CNT is limited in the resin matrix, and the Wave suction composite material of preparation often can't satisfy the engineering application requirements.
Carbon nano-tube film (carbon nanometer paper) is that the intermolecular Van der Waals force of a kind of dependence CNT (single wall or many walls) 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, with its functional layer as the radar-wave absorbing composite, can not affect moulding and the performance of bulk composite material structure, than in resin, adding CNT, carbon nano-tube film is formed by connecting by CNT fully, has more excellent electrical conductance and radar wave absorbability.
Graphene be a class by the New Two Dimensional nano-carbon material that one deck carbon atom forms, be present the thinnest two-dimensional material in the world.The intensity of grapheme material is the highest in the known materials, and its conductive capability and current carrying density all are to surpass at present best SWCN, and its good quantum hall effect (Quantua Hall effect) also is proven.With the solution of graphene oxide with after CNT mixes, the sheet interlayer of the sidewall of CNT and graphene oxide can produce strong π-π and interact, because graphene sheet layer has a large amount of hydrophilic functional groups, can increase the dispersion effect of graphene oxide-carbon mano-tube composite in water, be beneficial to the moulding of carbon nanometer paper, also can increase intensity and electric conductivity and the electromagnetic performance of carbon nanometer paper simultaneously.
In addition, utilize the plating nickel on surface CNT to prepare carbon nano-tube film, change dielectric constant and the electromagnetic constant of carbon nano-tube film, thereby regulate wave absorbed crest value and the frequency separation of radar-wave absorbing composite.
Summary of the invention
A kind of radar-wave absorbing composite material and preparation method thereof based on carbon nanocapsule thin film, realize by following steps:
(1) get CNT and anionic surface dispersant in 1: 1-1: 20 ratios are mixed, and wherein select commercially available many walls/single wall nickel-plating carbon nanotube, and its diameter is 6-30nm, and length is 10-50 μ m, and nickel content is 20-70%.The anionic surface dispersant can be selected Bio-Rad-Laboratories, dodecyl sodium sulfate, one or both mixing in the 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 CNT concentration is 0.01-1.0wt%, and surface dispersant concentration is 0.01-2wt%;
(3) mixed liquor in (2) step is poured in the magnetic stirring apparatus, the control temperature is disperseed 15-60min below 60 ℃; Froth breaking 10-100min;
(4) get CNT: the mass ratio of graphene oxide is 10: 1-10: 3 graphene oxide joins in the plasma water, is mixed with the solution of concentration 0.1-1mg/ml, ultrasonic dispersion 30-60min;
(5) CNT/graphene oxide solution is mixed, then utilize ultrasonic cell disruption instrument under the 100-800w condition, ultrasonic dispersion 10-100min, dispersion temperature are controlled in the 10-60 ℃ of scope;
(6) CNT/graphene oxide dispersion liquid is distributed in vitro, puts into centrifuge, and under the 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, permeable membrane is selected the permeable membrane of millipore company, wherein this permeable membrane can be selected nylon membrane, CN-CA, film, 0.22um or 0.45 μ m are selected in the aperture, the supernatant of CNT/graphene oxide dispersion liquid is carried out vacuum filtration, vacuum pump pressure is controlled in the 40-500Kpa scope, namely adopt the standby carbon nanocapsule thin film of vacuum filtration legal system;
(8) after suction filtration is finished, with the plasma water cleaning carbon nanocapsule thin film of 1-5 times of volume, until there is not foam to produce;
(9) carbon nanocapsule thin film with filter membrane and preparation together takes off, and is placed between two corrosion resistant plates, and baking oven is put in compacting, solidifies 2-10 hour under 60-150 ℃ of condition, peels off after curing is finished and obtains the carbon nanocapsule thin film structure;
(10) the carbon nanocapsule thin film structure is put into vacuum drying oven 300-350 ℃ of heat treatment 30-60min, and the electrical conductivity of carbon nanocapsule thin film reaches 100-2000S/m;
(11) press die size cutting carbon nanometer paper, put into the acetone diluted liquid of resin, infiltrate in advance 24-48 hour, put into baking oven 40 degree lower dry 2-4 hour, wherein resin can be selected epoxy resin or BMI;
(12) the 1-4 layer is infiltrated the carbon nanocapsule thin film lay in advance in the aluminum alloy mould innermost layer, middle lay 8-24 layer carbon fiber/resin prepreg material, close die, utilize compression molding, autoclave molding to prepare the radar-wave absorbing composite of carbon nanocapsule thin film, wherein carbon fiber/resin prepreg material can be selected epoxy resin/carbon fiber, bimaleimide resin/carbon fiber prepreg.
The reflection of radar wave rate of radar-wave absorbing composite in the 8-18GHz frequency range of the carbon nanocapsule thin film that makes by the present invention is less than-10dB--20dB.
Description of drawings
The structural representation of Fig. 1 radar-wave absorbing composite
The specific embodiment
As described in Figure 1: carbon nanocapsule thin film is inhaled wave energy layer 1 and is covered as on the composite structural laminate 2.
Embodiment 1
(1) get CNT and mix in 1: 10 ratio with Bio-Rad-Laboratories, wherein select commercially available many walls of nickel plating nickel-plating carbon nanotube, its diameter is 8-15nm, and length is 50 μ m, and nickel content is 60%;
(2) CNT and anionic surface mixture of dispersing agents are put into mortar and are ground 40min, pour beaker into, and adding plasma water to CNT concentration is 0.03wt%, and surface dispersant concentration is 0.3wt%;
(3) mixed liquor is poured in the magnetic stirring apparatus, and the control temperature is disperseed 60min, froth breaking 40min below 60 ℃;
(4) get graphene oxide (CNT: the mass ratio of graphene oxide is 10: 1) and join in the plasma water, be mixed with the solution of concentration 1mg/ml, ultrasonic dispersion 60min;
(5) CNT/graphene oxide dispersion liquid is distributed in vitro, then utilizes ultrasonic cell disruption instrument under the 540w condition, and ultrasonic dispersion 45min, dispersion temperature are controlled in the 20-30 ℃ of scope;
(6) CNT/graphene oxide dispersion liquid is distributed in vitro, puts into centrifuge, and under the rotating speed 4000rpm condition, centrifugal treating 40min chooses in vitro CNT/graphene oxide solution supernatant liquor;
(7) select vacuum suction filter to prepare carbon nanocapsule thin film, permeable membrane is selected the CN-CA of millipore company, membrane pore size is selected 0.22 μ m, the supernatant of CNT/graphene oxide dispersion liquid is carried out vacuum filtration, vacuum pump pressure is controlled in the 300Kpa scope, namely adopts the standby carbon nanocapsule thin film of vacuum filtration legal system;
(8) after suction filtration is finished, with the plasma water cleaning carbon nanometer paper of 3 times of volumes, until there is not foam to produce;
(9) carbon nanocapsule thin film with filter membrane and preparation together takes off, and is placed between two corrosion resistant plates, and baking oven is put in compacting, solidifies 4 hours under 120 ℃ of conditions, peels off after curing is finished and obtains the carbon nanocapsule thin film structure;
(10) the carbon nanocapsule thin film structure is put into 300 ℃ of heat treatment 60min of vacuum drying oven, and the electrical conductivity of carbon nanocapsule thin film reaches 500S/m;
(11) press die size cutting carbon nanometer paper, put into the acetone diluted liquid of resin, infiltrate in advance 24 hours, put into baking oven 40 degree lower dry 2 hours, wherein resin can be selected epoxy resin, BMI;
(12) infiltrate in advance the carbon nanocapsule thin film laies in the aluminum alloy mould innermost layer with 2 layers, 16 layers of carbon fiber/epoxy prepreg of middle lay, close die utilizes autoclave molding to prepare the radar-wave absorbing composite of carbon nanocapsule thin film; The reflection of radar wave rate of the radar-wave absorbing composite of carbon nanocapsule thin film in the 8-18GHz frequency range is less than-8dB.
Claims (6)
1. radar-wave absorbing composite material and preparation method thereof based on carbon nanocapsule thin film, realize by following steps:
(1) get CNT and anionic surface dispersant by 1: 1-1: 20 mass ratioes mix;
(2) with CNT with cloudyly put into mortar from the surface dispersant mixture and grind 1-60min, pour beaker into, adding plasma water to CNT concentration is 0.01-1.0wt%, surface dispersant concentration is 0.01-2wt%;
(3) mixed liquor in (2) step is poured in the magnetic stirring apparatus, the control temperature is disperseed 15-60min at 20-60 ℃; Froth breaking 10-100min;
(4) get CNT: the mass ratio of graphene oxide is 10: 1-10: 3 graphene oxide joins in the plasma water, is mixed with the solution of concentration 0.1-1mg/ml, ultrasonic dispersion 30-60min;
(5) CNT/graphene oxide solution is mixed, then utilize ultrasonic cell disruption instrument under the 100-800w condition, ultrasonic dispersion 10-100min, dispersion temperature are controlled in the 10-60 ℃ of scope;
(6) CNT/graphene oxide dispersion liquid is distributed in vitro, puts into centrifuge, and under the 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 liquid is carried out vacuum filtration, vacuum pump pressure is controlled in the 40-500Kpa scope, namely adopt the standby carbon nanocapsule thin film of vacuum filtration legal system;
(8) after suction filtration is finished, with the plasma water cleaning carbon nanocapsule thin film of 1-5 times of volume, until there is not foam to produce;
(9) carbon nanocapsule thin film with filter membrane and preparation together takes off, and is placed between two corrosion resistant plates, and baking oven is put in compacting, solidifies 2-10 hour under 60-150 ℃ of condition, peels off after curing is finished and obtains the carbon nanocapsule thin film structure;
(10) the carbon nanocapsule thin film structure is put into vacuum drying oven 300-350 ℃ of heat treatment 30-60min, and the electrical conductivity of carbon nanocapsule thin film reaches 100-2000S/m;
(11) press die size cutting carbon nanocapsule thin film, put into the acetone diluted liquid of resin, infiltrate in advance 24-48 hour, put into baking oven 40 degree lower dry 2-4 hour;
(12) the 1-4 layer is infiltrated the carbon nanocapsule thin film lay in advance in the aluminum alloy mould innermost layer, middle lay 8-24 layer carbon fiber/resin prepreg material, close die utilizes compression molding, autoclave molding to prepare the radar-wave absorbing composite of 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 μ m, 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 is selected Bio-Rad-Laboratories, dodecyl sodium sulfate, one or both mixing in the 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 the step (7), when vacuum suction filter prepares carbon nanocapsule thin film, permeable membrane is selected the permeable membrane of millipore company, wherein this permeable membrane is selected nylon membrane, CN-CA, film, aperture are selected 0.22um or 0.45 μ m.
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: resin is selected epoxy resin or BMI in the step (10).
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: carbon fiber in the step (12)/resin prepreg material is selected epoxy resin/carbon fiber or bimaleimide resin/carbon fiber prepreg.
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