CN1793039A - Microwave absorbing composite material with silicon carbide-carbon and preparation process thereof - Google Patents

Microwave absorbing composite material with silicon carbide-carbon and preparation process thereof Download PDF

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Publication number
CN1793039A
CN1793039A CN 200510110086 CN200510110086A CN1793039A CN 1793039 A CN1793039 A CN 1793039A CN 200510110086 CN200510110086 CN 200510110086 CN 200510110086 A CN200510110086 A CN 200510110086A CN 1793039 A CN1793039 A CN 1793039A
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microwave absorbing
composite material
absorbing composite
preparation
powder
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CN 200510110086
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谭寿洪
周泽华
江东亮
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Shanghai Institute of Ceramics of CAS
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Shanghai Institute of Ceramics of CAS
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Abstract

The invention relates to a microwave absorbing compounding material that uses silicon carbide as basal material, and the manufacture method. The technology is that: adopting silicon carbide powder that has the diameter of 0.1-10um, graphite C power that has the diameter of 0.1-10um. After molding, the compounding material is sintered at 1700-2250 degree centigrade. The feature is that the density range is 1.6-3.2cm<SUP>3</SUP>, resistivity range is 10<SUP>0</SUP>-10<SUP>4</SUP>.cm, the real part of dielectric constant is 1-200. The material is machined to sectional area of 22.86*10.16mm<SUP>2</SUP>, and the thickness at 4, 8, 12mm, the microwave maximum of attenuation value of the X wave section at 8-12.4GHz is -40db, and the attenuation values in the whole X section are all above -20db.

Description

Silicon carbide-carbon microwave absorbing composite material and preparation method thereof
Technical field:
The present invention relates to a kind of microwave absorbing composite material with silicon carbide-carbon and preparation method thereof, a kind of more precisely is body material with silicon carbide and carbon, by Composition Control and technique change, to obtain to have matrix material of good microwave absorbing property and preparation method thereof.Belong to the ceramic matric composite field.
Background technology:
Because good characteristic of semiconductor and other over-all properties, silicon carbide ceramics is counted as a kind of very promising absorbing material.It is the structural wave-absorbing material of absorption agent that the research of this aspect at present mainly concentrates on the silicon carbide fiber, but because the price of silicon carbide fiber costliness and complicated preparation technology cause the manufacturing cost of this class material higher, very difficult acquisition is used widely.And, take all factors into consideration from aspects such as cost, performance, technologies, do not find as yet that at present a kind of material can have good microwave absorbing effect under the frequency band range of broad and complicated abominable application conditions, have cheap relatively manufacturing cost and simple preparation technology simultaneously concurrently.
Current research to the traditional microwave absorbing material mainly concentrates on electrical loss type absorbing materials such as carbon fiber, silicon carbide and fiber and the ferrite equimagnetic loss-type absorbing material.The absorbing property of above-mentioned electrical loss section bar material self is relatively poor, all needs by composition and technology controlling and process to obtain microwave absorbing property preferably.With the carbofrax material is example, [sieve is sent out as bibliographical information, Zhou Wancheng, burnt permanent, Zhao Donglin. " high temperature absorbing material present Research. " aerospace material technology .2000. (1) .8-11] expert on Japan crosses the method for purifying of utilizing, and obtains based on very high purity, the sic raw material that contains any impurity hardly, this material has the suction ripple frequency band and the absorbing property of broad, but this method technology is extremely complicated, and manufacturing cost is higher.And for silicon carbide fiber, as bibliographical information [Song Yongcai, Lu Yi, Feng Chunxiang. " development. " functional materials .1997.28 (6) .619 with mix type silicon carbide fiber of microwave absorbing property] adopt the three-decker material of mix type silicon carbide fiber, can obtain in 8-12GHz scope microwave attenuation and be-wave-absorbing effect more than the 12dB, but disadvantage is the higher and complex process of cost equally.As for ferrite equimagnetic loss-type absorbing material [Amin M B, James J R. " Techniques for utilizationof hexagonal ferrites in radar absorbers. " The Radar and Electronic Engineer.1981.57 (5) .209-214], though hertzian wave is easy to enter the also quick decay of material internal and is applied to the microwave absorbing field, but because its density is big, temperature stability is relatively poor, has therefore limited its range of application.
Summary of the invention:
The objective of the invention is at the deficiency of above-mentioned materials microwave absorbing property and preparation method's complexity and cost higher, take all factors into consideration from performance, cost and technology are equal angular, select the silicon carbide and the carbon granule powder of relative low price for use, prepare the silicon carbide-carbon microwave composite material by the method for pressureless sintering.The present invention is by composition and process optimization, acquisition uses the field the most widely in the X-band (8-12GHz) at microwave, have the resistor-type composite wave-absorbing pottery of good absorbing property, and significantly reduce the manufacturing cost of silicon carbide class absorbing material, widen its range of application.
Specifically:
(1) a kind of microwave absorbing composite material, its feature is a body material by SiC and C or graphite, wherein C or graphite are the 1-20wt% of total content;
(2) described microwave absorbing composite material microwave attenuation value in the X-band of 8-12.4GHz is to the maximum-40db, and the microwave attenuation value is all above-20db in whole X-band;
(3) processing step of the method for described microwave absorbing composite material is:
(a) with the particle diameter be the silicon-carbide particle powder of 0.1-10 μ m, and particle diameter is that C or the graphite granule powder of 0.1-10 μ m is initial powder, and by adding sintering aid, and adding binding agent, it is standby to mix the acquisition composite powder by ball milling, and wherein C or content of graphite are the 1-20wt% of composite powder total content;
(b) composite powder that step (a) is prepared dry-pressing formed after, by non-pressure sintering technology under the protective atmosphere or hot pressing mode sintering;
(4) sintering aid among the preparation method of described microwave absorbing composite material is a SiC base pottery sintering aid commonly used, as Al 2O 3Or B 4C, add-on is the 0.5-2wt% of body material;
(5) binding agent among the preparation method of described microwave absorbing composite material is a resol, and add-on is 5-15wt%;
(6) the pressureless sintering temperature is 1800-2250 ℃ among the preparation method of described microwave absorbing composite material, and protective atmosphere is argon gas or vacuum;
(7) the hot pressed sintering temperature is 1700-2050 ℃ among the preparation method of described microwave absorbing composite material, and pressure is 20-40MPa; Protective atmosphere is argon gas or vacuum.
The present invention mainly contains the characteristics of following several respects:
(1) microwave attenuation value height: 22.86 * a 10.16 * 12mm 3Material, the maximum microwave attenuation value that employing waveguide method in X-band is measured reaches-40db (decibel).Be higher than the silicon carbide of bibliographical information and the microwave attenuation of carbon class material far away.
(2) attenuation bend is wide: the microwave attenuation value that above-mentioned materials adopts waveguide method to measure in whole X-band all surpasses-20db, belongs in X-band promptly that full range is high decays.
(3) technology is simple, and preparation cost is low: select for use common silicon carbide and carbon to get final product, and only need adopt means such as not having pressure or hot pressed sintering to machine.
(4) cost performance height: preparation technology and cost also have the material of high microwave absorbing property far below silicon carbide fiber class microwave absorbing material far below other; The microwave attenuation performance also is higher than or is similar to the above-mentioned materials of report simultaneously.
(5) applied widely: compare with ferrite equimagnetic loss-type absorbing material, its density is low, and high-temperature behavior is good, applicable to the incompetent microwave absorbing of ferrite class material field.
The drawing explanation
Fig. 1 is for implementing the Changing Pattern of 1 described material different thickness material microwave pad value under X-band.
X-coordinate is a microwave frequency among Fig. 1, and unit is GHz, and ordinate zou is the microwave attenuation value, and unit is-dB, and three curves are representing respectively that thickness is 4,8, the microwave attenuation performance of 12mm material.
Embodiment
Below with a certain specific examples, the invention will be further described:
Embodiment 1
Processing step is:
(1) matrix powder is chosen as D 50The β of=0.2-2 μ m-SiC particle powder, its purity should reach D greater than 95wt% 50The graphite C particles powder of=0.5-5 μ m, and the sintering aid of interpolation 0.5-2wt%.As BAC or Al 2O 3, add-on is the 0.5-2wt% of silicon carbide-carbon matrix, promptly adds capable λ and adds λ.Wherein C or content of graphite are the 1-20wt% of composite powder total content.
(2) powder for preparing is solvent with alcohol after mixing 24 hours on the ball mill, adds the 5-15vol% phenol resin solution as binding agent, and remix take out oven dry, grind, and it was standby to cross 60 mesh sieves after 5 hours.
(3) composite powder compression moulding on vulcanizing press, the about 20MPa of forming pressure, pressurize 20s, and following by high temperature sintering furnace Ar protection at 1800-2250 ℃ of following sintering.
(4) material behind the sintering is measured its density with drainage, and density range is 1.6-3.2g/cm 3
(5) material behind the sintering is measured its resistance with two electrode methods, and to calculate corresponding resistivity be 10 0-10 4About Ω cm.
(6) material behind the sintering is processed to 22.86 * 10.16 * 2mm 3Size, use waveguide method, and by the HP8722ES vector network analyzer it is measured at real part ε ' of the specific inductivity of X-band (8-12.4GHz) and dielectric loss angle tangent tg δ, measuring the real part of permittivity scope is 1-200, the tangent of the dielectric loss angle value is between the 1-50.
(7) material behind the sintering is processed to 22.86 * 10.16mm 2Sectional area, thickness is respectively 4,8 and 12mm, uses waveguide method, and by Wiltron 54169A scalar network analyzer its microwave attenuation value at X-band (8-12.4GHz) is measured, the result of mensuration is with the form performance of decibel (dB).As shown in Figure 1.The microwave attenuation value is to the maximum-40db, and the microwave attenuation value above-20db, is a comparatively ideal microwave absorbing material all in whole X-band.
Embodiment 2
Adopt hot pressing mode to carry out sintering, sintering temperature is 1700-2050 ℃, and pressure is 20-40MPa, and other are as embodiment 1, and its microwave property as shown in Figure 1.

Claims (7)

1, a kind of microwave absorbing composite material, its feature is a body material by SiC and C or graphite, wherein C or graphite are the 1-20wt% of total content.
2, by the described microwave absorbing composite material of claim 1, it is characterized in that described material microwave attenuation value in the X-band of 8-12.4GHz is to the maximum-40db, the microwave attenuation value is all above-20db in whole X-band.
3, the method for preparation microwave absorbing composite material as claimed in claim 1 is characterized in that processing step is:
(a) with the particle diameter be the silicon-carbide particle powder of 0.1-10 μ m, and particle diameter is that C or the graphite granule powder of 0.1-10 μ m is initial powder, and by adding sintering aid, and adding binding agent, it is standby to mix the acquisition composite powder by ball milling, and wherein C or content of graphite are the 1-20wt% of composite powder total content;
(b) composite powder that step (a) is prepared dry-pressing formed after, by non-pressure sintering technology under the protective atmosphere or hot pressing mode sintering.
4,, it is characterized in that described sintering aid is a SiC base pottery sintering aid commonly used, as Al by the preparation method of the described microwave absorbing composite material of claim 3 2O 3Or B 4C, add-on is the 0.5-2wt% of body material.
5, by the preparation method of the described microwave absorbing composite material of claim 3, it is characterized in that described binding agent is a resol, add-on is 5-15wt%.
6, by the preparation method of the described microwave absorbing composite material of claim 3, it is characterized in that the pressureless sintering temperature is 1800-2250 ℃, protective atmosphere is argon gas or vacuum.
7, by the preparation method of the described microwave absorbing composite material of claim 3, it is characterized in that the hot pressed sintering temperature is 1700-2050 ℃, pressure is 20-40MPa; Protective atmosphere is argon gas or vacuum.
CN 200510110086 2005-11-07 2005-11-07 Microwave absorbing composite material with silicon carbide-carbon and preparation process thereof Pending CN1793039A (en)

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101082090B (en) * 2007-07-01 2010-05-19 合肥工业大学 Preparation method of Mo/AIN multi-phase microwave absorbing material
CN102531605A (en) * 2010-12-20 2012-07-04 北京有色金属研究总院 High-heat-conductivity SiC-based microwave attenuating material and preparation method thereof
CN103833363A (en) * 2014-01-15 2014-06-04 北京科技大学 Silicon carbide graphite composite material and preparation method thereof
CN103936423A (en) * 2014-03-31 2014-07-23 西安科技大学 Silicon carbide-based microwave absorption composite material and preparation method thereof
CN104926330A (en) * 2015-06-17 2015-09-23 单计金 Furnace jacket wave-absorbing material and manufacturing method thereof
CN108865061A (en) * 2018-07-14 2018-11-23 合肥艾飞新材料有限公司 A kind of hollow plumbago alkene microballoon and preparation method thereof
CN108911756A (en) * 2018-08-27 2018-11-30 宁波伏尔肯科技股份有限公司 A kind of adjustable silicon carbide ceramics of resistance and preparation method thereof
CN109346848A (en) * 2018-10-31 2019-02-15 哈尔滨工业大学 A kind of SiC- ferrite/carbonaceous material high temperature Wave suction composite material and preparation method thereof
CN110078514A (en) * 2019-05-23 2019-08-02 中国科学院上海硅酸盐研究所 A kind of silicon carbide ceramics microwave reference source
CN111099917A (en) * 2018-10-29 2020-05-05 中国石油化工股份有限公司 Porous composite material for generating electric arc in microwave and preparation method thereof

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101082090B (en) * 2007-07-01 2010-05-19 合肥工业大学 Preparation method of Mo/AIN multi-phase microwave absorbing material
CN102531605A (en) * 2010-12-20 2012-07-04 北京有色金属研究总院 High-heat-conductivity SiC-based microwave attenuating material and preparation method thereof
CN103833363A (en) * 2014-01-15 2014-06-04 北京科技大学 Silicon carbide graphite composite material and preparation method thereof
CN103936423A (en) * 2014-03-31 2014-07-23 西安科技大学 Silicon carbide-based microwave absorption composite material and preparation method thereof
CN103936423B (en) * 2014-03-31 2016-04-06 西安科技大学 A kind of silicon carbide-based microwave absorbing composite material
CN104926330A (en) * 2015-06-17 2015-09-23 单计金 Furnace jacket wave-absorbing material and manufacturing method thereof
CN108865061A (en) * 2018-07-14 2018-11-23 合肥艾飞新材料有限公司 A kind of hollow plumbago alkene microballoon and preparation method thereof
CN108911756A (en) * 2018-08-27 2018-11-30 宁波伏尔肯科技股份有限公司 A kind of adjustable silicon carbide ceramics of resistance and preparation method thereof
CN111099917A (en) * 2018-10-29 2020-05-05 中国石油化工股份有限公司 Porous composite material for generating electric arc in microwave and preparation method thereof
CN111099917B (en) * 2018-10-29 2022-01-04 中国石油化工股份有限公司 Porous composite material for generating electric arc in microwave and preparation method thereof
CN109346848A (en) * 2018-10-31 2019-02-15 哈尔滨工业大学 A kind of SiC- ferrite/carbonaceous material high temperature Wave suction composite material and preparation method thereof
CN109346848B (en) * 2018-10-31 2021-03-12 哈尔滨工业大学 SiC-ferrite/carbonaceous material high-temperature wave-absorbing composite material and preparation method thereof
CN110078514A (en) * 2019-05-23 2019-08-02 中国科学院上海硅酸盐研究所 A kind of silicon carbide ceramics microwave reference source

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