CN1514684A - Carbon nano-pipe/ceramic composite material possessing microwave absorption function and its preparation method - Google Patents
Carbon nano-pipe/ceramic composite material possessing microwave absorption function and its preparation method Download PDFInfo
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- CN1514684A CN1514684A CNA031295630A CN03129563A CN1514684A CN 1514684 A CN1514684 A CN 1514684A CN A031295630 A CNA031295630 A CN A031295630A CN 03129563 A CN03129563 A CN 03129563A CN 1514684 A CN1514684 A CN 1514684A
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Abstract
Characters of the method are that content of added carbon nano tube 'CNT' is 0.1-30vol %, and ceramic system is one among SiO2, Si3N4, Al2O3 or ZrO2; CNT is of multi walls or single wall, diameter 20-40 nm, length-diameter ratio at least 100:1; surfactant utilized in the preparing procedure is one among C16TMAB, PAA or C16EO; disperse medium is one among trichloromethane, deionized water, acetone, absolute ethyl alcohol or absolute ethyl alcohol + water; composite powder is prepared through direct mixing or fast sol gel method and hot pressing sinter process in final procedure. The invented composite material possesses features of integrated structural function. Comparing with pure SiO2, intensity and toughness of material 5vol%CNT/SiO2 , which possesses character of microwave absorption, increases 140% and 53%.
Description
Technical field
The utility model relates to novel carbon nano-tube/pottery (oxide, non-oxidized substance) composite system that a class has the microwave absorbing function.Belong to function composite diphase material field.
Background technology
Carbon nano-tube has caused the great interest of researcher since the Iijima by Japan in 1991 finds [S.iijima, Nature (London), 354 (1991) 56.].Because its special structure and dielectric property, carbon nano-tube (CNTs) shows stronger wide-band microwave absorbent properties, that it also has simultaneously is in light weight, but the conductivity modulation, high-temperature oxidation resistance is strong and characteristics such as good stability, be a kind of promising desirable microwave absorption, might be used for stealth material, electromagnetic shielding material or darkroom absorbing material.But the research of this respect is also fewer at present.
Have the microwave absorbing characteristic although say nanotube, make this characteristic of material obtain embodying or using, nanotube must be compound as absorbent and other material, is prepared into composite material.At present, the researcher has begun to have carried out a series of relevant research work.
C.A.Grimes etc. [C .A.Grimes et al., Chemical Physical Letters, 319 (2000) 460.] have studied the dielectric constant spectrum of single wall CNT/ polymer composites in the 0.5-5.5GHz frequency range.Find the adding of nanotube, increased the imaginary part of the dielectric constant of material greatly, show the adding of nanotube, material is increased electromagnetic loss, prove that CNT might be used as the microwave absorbing medium really.
The absorbing property of the orientable carbon nanotubes grown film of the Zhu Changchun of Xi'an Communications University, Deng Ning [Zhu Changchun, Deng Ning, XI AN JIAOTONG UNIVERSITY Subject Index, 34,12 (2000) 102] research.Discovery has extremely strong absorbability to ruddiness and infrared laser.To the microwave of 10GHz, the suprabasil carbon nano-tube film of Cu also shows the certain absorption ability.
According to English " New Scientist " on January 26th, 2002: stealth aircraft is very expensive, suffers that in order to prevent the stealth aircraft that is parked in the airport in thunderstorm weather thunder and lightning attacks, and the Vito Mu Nike that wears of the state university of Michigan, United States has found a kind of method.He declares, utilizes one deck carbon nano-tube film to cover the stealth aircraft surface and just can prevent thunderbolt.There is the carbon nano-tube of tiny sieve aperture to be fixed in the thin epoxy resin-base of one deck, just can makes the composite panel of high conductivity and absorbing radar wave, and make the covering of stealth aircraft with it.Like this, attack if run into lightning, electric current just can flow through the composite panel surface, guides to the ground wire below the aircraft then, and can not cause catastrophic destruction (as a big hole of puncture on wing or destroy critical flight electronic equipment).The anti-thunder and lightning covering that this carbon nano-tube is made is being tested by Boeing of B-2 stealth aircraft manufacturer now.
The Shen Cengmin of Beijing University of Chemical Technology, Zhao Donglin professor [Shen Cengmin, Zhao Donglin, novel charcoal material, 16,1 (2001) 1] has studied the microwave absorbing property of nickel-plating carbon nanotube/epoxy resin.They have plated the layer of even metallic nickel with electroless plating method in carbon nano tube surface.When the carbon nano-tube microwave absorbing coating is 0.97mm at thickness, at 8GHz～18GHz, maximum absorption band 11.4GHz (R=-22.89dB) R＜-frequency range of 10dB is 3.0GHz, R＜-frequency range of 5dB is 4.7GHz.The nickel-plating carbon nanotube microwave absorbing coating is under same thickness, and maximum absorption band is at 14GHz (R=-11.85dB), R＜-frequency range of 10dB is 2.23GHz, the frequency range of R＜-5 dB is 4.6GHz.
Glatkowski Paul[Glatkowski Paul, Mack Patrick, Conroy Jeffrey et al., USPatent 6,265,465 (July, 2001)] etc. prepared a kind of electromagnetic shielding (Electromagneticshielding) function CNT/ polymer (PET) composite material that has.The content of CNT is from 0.001wt% to 15wt%, and draw ratio＞100 align portion C NTs by applying shearing force.Its reflectivity and dielectric constant have been tested.
Electromagnetic performance research situation from present CNT composite material just is confined on the CNT/ organic polymer composite material; Aspect the microwave absorbing research of CNT/ ceramic matric composite report is not being arranged as yet.[USPatent6,420,293 such as S.Chang, B1 (Jul 16,2002)] reported that the carbon nano-tube/ceramic nanocomposites that has than high-mechanical property, used powder are nanocrystalline powder, particle size range but does not report that its material system has microwave absorbing property in 1-100nm.To being initial powder body material with amorphous powder with greater than 100nm crystalline state powder, and the structure-function integration CNT/ ceramic composite bodies system with microwave absorbing function and high mechanical property, yet there are no document announcement.
For the CNT/ organic polymer, its poor mechanical property, serviceability temperature is low, can not carry, and also easy deformation is aging down at a high speed.Such as, aboard, can only be lower than under the 3marh and could use.Do microwave absorbing material if use carbon nano-tube/ceramic composite, then can show distinctive high-strength, high hard, the high chemical stability of ceramic material, excellent performance such as high temperature resistant, can satisfy load, high temperature resistant, exacting terms such as use down at a high speed.The application of exploitation aspect radar absorbing (RAM) and darkroom absorbing material.
Summary of the invention
Present situation at CNT/ ceramic research in the present CNT microwave absorbing composite material research the invention provides a kind of CNT/ ceramic composite and preparation method with microwave absorbing function.An outstanding advantage of the present invention is exactly the CNT/ ceramic composite that has prepared structure-function integration.The preparation of material may further comprise the steps:
(1) dispersion of CNT and dispersant are selected:
The CNTs that the present invention selects for use is the carbon nano-tube that nanometer port, Shenzhen Co., Ltd produces, and the purity of carbon nano-tube is greater than 90%, and diameter is at 20～40nm, and draw ratio is greater than 100, and density is 2.0g/cm
3, can be many walls, also can be single wall.
The decentralized medium of described CNT is analytically pure chloroform, deionized water, absolute ethyl alcohol.
16 alkyl-3 methyl ammonium bromide (the C that described surfactant adopts Shanghai chemical reagents corporation to provide
16TMAB, molecular weight), the C that produces of polyacrylic acid (PAA, molecular weight 5000) and U.S. AldrichChemical Company
16EO.These three kinds of surfactants can play good peptizaiton to CNT, it keeps the mechanism of dispersion stabilization mainly to be: organic polymer is adsorbed in carbon nano tube surface, rely on the Coulomb repulsion effect after the carbon nano tube surface of being adsorbed in of intermolecular steric hindrance and/or charged polyelectrolyte to overcome Van der Waals force between the carbon nano-tube, thereby play the effect of dispersing Nano carbon tubes.
Described surfactant concentrations scope forms concentration (CMC) greater than its critical micell.
(2) CNT/ ceramic composite powder preparation:
Direct mixing method: take by weighing a certain amount of CNT and stir in decentralized medium, ultrasonic dispersion certain hour stirs ultrasonic dispersion with ceramic powder simultaneously in identical decentralized medium, then two kinds of suspension is mixed ultrasonic again dispersion certain hour.In adding the process of thermal agitation, make the organic dispersion medium volatilization, obtain composite granule.Ceramic powder employing relatively cheap (comparing with the price of nano-powder) unformed powder of price or particle diameter are greater than the crystalline state powder of 0.1 μ m.
Fast sol gel method: the CNT adding is contained in ceramic powder predecessor (metal alkoxide) aqueous solution of surfactant, stir, ultrasonic dispersion certain hour adds acid and/or base catalyst, make the hydrolysis of ceramic powder predecessor form colloidal sol, form gel at last.Washing, drying obtains composite granule.
Homogeneous precipitation method: the CNT adding is contained in ceramic powder predecessor (salt) aqueous solution of surfactant, stir, ultrasonic dispersion certain hour adds the precipitation from homogeneous solution agent, stirs, and obtains precipitation.To precipitate calcining, obtain the composite granule of amorphous ceramic powder predecessor and CNT.
Ceramic base of the present invention comprises SiO
2, ZrO
2, Al
2O
3Or Si
3N
4In a kind of, the CNT content range of being introduced: 0.1vol%～30vol%.
(3) finally burning till of composite material:
Composite material burn till the employing hot-pressing sintering technique.When sintering, the composite granule of various different CNT content forms Gradient distribution as requested, thereby realizes the different microwave absorbing property that require.
Material system provided by the present invention has the microwave absorbing function, also has the high mechanical property of pottery, has the characteristics of structure-function integration.Can be used on the electronic equipment and other stealthy device to microwave susceptible.It is desirable radar wave absorbing material (RAM).For example: the 5vol%CNT/SiO of fast sol-gel method preparation
2The intensity and the toughness of material are the highest, with pure SiO
2Compare, improved 140% and 53% respectively; And have the microwave absorbing characteristic again.Embody structure-function integration feature.
Description of drawings
Table 1 is CNT/SiO
2The microwave absorbing data of part sample
Fig. 1 is the TEM pattern of CNT that the present invention adopts
Fig. 2 is 10vol%CNT/SiO
2The X-ray diffractogram of block behind the composite material sintering
Fig. 3 is the composite granule transmission electron microscope pattern of sol-gel process preparation
Fig. 4 is CNT/SiO
2The high-resolution photo of composite material interface
Fig. 5 is 3vol%CNT/Si among the present invention
3N
4The microwave absorbing property of material (reflectivity-frequency relation curve)
Fig. 6 is the TEM pattern that homogeneous precipitation method prepares the 5vol%CNT/ composite granule
Embodiment
Embodiment 1: direct mixing method prepares 10vol%CNT/SiO
2Composite material
SiO
2Powder meta particle diameter is 3.1 microns, by Shanghai silicate is made by oneself.
Get 2g CNT and 19.44gSiO
2Powder stirs in the 400ml chloroform respectively, and ultrasonic dispersion 10 minutes mixes two kinds of suspension then and stirs, ultrasonic again dispersion 5 minutes, and powerful stirring under heating condition at last, the chloroform volatilization obtains composite granule.Composite granule is crossed 200 mesh sieves, then at 30MPa, N
2Under the atmosphere, 1300 ℃ of hot pressed sinterings obtain block materials.Fig. 2 is CNT and material 10vol%CNT/SiO
2X-ray diffractogram behind the sintering, as we can see from the figure: carbon nano-tube still keeps its architectural feature behind sintering.Block becomes corresponding size, test performance through cut.
Embodiment 2: sol-gel process prepares 5vol%CNT/SiO
2
Surfactant CTMAB90mg is dissolved in the 200ml deionized water, mixes with the 78ml tetraethoxysilane; Take by weighing CNT1.0g, add in this mixed solution, stir ultrasonic dispersion 10 minutes.Then under magnetic stirrer, hydrochloric acid (HCl) solution that dropwise adds 1.16M is regulated pH value to 0.5～1, after continuing to stir hydrolysis 1～5h, dropwise add about the ammonia spirit regulator solution pH value to 10 of 1.2M, colloidal sol forms gel fast about 5 minutes.Gel is left standstill 0.5-2h, and suction filtration is used deionized water wash then, removes NH wherein
4Cl uses absolute ethanol washing again.Filter cake after the washing 100 ℃ of oven dry, is ground, cross 200 mesh sieves.Then in chamber type electric resistance furnace 500 ℃ the calcining 1～2 h, the CNT/SiO that is uniformly mixed
2Composite granule, the transmission electron microscope pattern photo of powder as shown in Figure 3.Press example 1 described method sintering processing sample then, test performance.Fig. 4 is a material sintering rear interface high-resolution photo, shows CNT and SiO
2Matrix has good physical chemistry compatibility.Table 1 is with real
Execute the reflectivity data that example 2 methods prepare the composite material millimere-wave band.
Embodiment 3 direct mixing methods prepare 3vol%CNT/Si
3N
4Composite material
Prepare the method for composite granule according to embodiment 1, preparation 1wt%CNT/Si
3N
4Composite granule, then at 1600 ℃, 30MPa, N
2Hot pressed sintering under the atmosphere.Be processed into corresponding size, test its reflectivity.Fig. 5 is its reflectivity collection of illustrative plates in millimere-wave band.
Embodiment 4 homogeneous precipitation methods prepare 5vol%CNT/Al
2O
3Composite material
Take by weighing 0.5gCNT, join the NH that 1.85L concentration is 2M
4HCO
3In the aqueous solution, stir, ultrasonic dispersion certain hour is the Al (NO of 0.2M then with 1.85L concentration
3)
2Solution splashes in the powerful mixed solution that stirs, and obtains precipitation.After sedimentation and filtration, drying, calcine 1h for 500 ℃, obtain the composite granule of unbodied forerunner and CNT.With 1400 ℃ of powders, 30MPa hot pressed sintering, be incubated half an hour, obtain CNT/Al
2O
3Composite material.
Table 1
| ??CNT ??(vol％) | Size (mm) | Frequency band (GHz) | Reflectivity (dB) |
| ??1 | ?6.92×3.42× ????30 | ?26.5-40 | ??≥10.47 |
| ??5 | ?6.92×3.42× ????30 | ?26.5-40 | ??≥54.94 |
| ??10 | ?6.90×3.40× ????6.27 | ?26.5-40 | ??≥40.21 |
Claims (5)
1. carbon nano-tube/the ceramic composite with microwave absorbing function is characterized in that the content of carbon nanotubes of being introduced is 0.1～30vol%; Described ceramic systems is SiO
2, ZrO
2, Al
2O
3Or Si
3N
4In a kind of.
2. by the described carbon nano-tube/ceramic composite of claim 1, it is characterized in that described CNT or be Single Walled Carbon Nanotube, or be multi-walled carbon nano-tubes with microwave absorbing function; Draw ratio was at least 100: 1, and diameter is 20～40nm.
3. by claim 1 or 2 described carbon nano-tube/ceramic composites, it is characterized in that specifically consisting of 10vol%CNT/SiO with microwave absorbing function
2Or be 5vol%CNT/SiO
2, or 1vol%CNT/SiO
2Or 3vol%CNT/Si
3N
4Or be 5vol%CNT/Al
2O
3
4. by the described preparation method of claim 1 with carbon nano-tube/ceramic composite of microwave absorbing function, comprise that decentralized medium, surfactant select for use, preparation of CNT/ ceramic composite powder and sintering process process is characterized in that:
(1) surfactant is C
16TMAB, PAA or C
16A kind of among the EO;
(2) decentralized medium is a kind of in chloroform, deionized water, acetone, absolute ethyl alcohol or the absolute ethyl alcohol+water;
(3) the CNT/ ceramic composite powder prepares or is direct mixing method, or fast sol-gel method or homogeneous precipitation method;
(4) sintering is to adopt hot-pressing sintering method, 1200～1650 ℃ of hot pressing temperatures, and pressure 20～40MPa, the time is 20～60min
5. described by claim 4, have the carbon nano-tube/ceramic composite and the preparation method of microwave absorbing function, it is characterized in that the used ceramic powder of direct mixing method or be amorphous powder or particle diameter crystalline state powder greater than 0.1 μ m.
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