CN106007804B - A kind of high temperature resistant high impedance surface radar absorbing and preparation method thereof - Google Patents
A kind of high temperature resistant high impedance surface radar absorbing and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of high temperature resistant high impedance surface radar absorbings, are double-layer structure, include the medium substrate layer in bottom and the high impedance surface layer in surface layer, the medium substrate layer, which is oxide fibre, enhances oxide-base composite material；The high impedance surface layer in the high temperature resistant resistance coating of periodic patterns mainly by forming.The present invention preparation method include：It first chooses and preparation media substrate, then the coating of high temperature resistant resistance coating is printed on by medium substrate surface using silk-screen printing technique, to get to the high temperature resistant high impedance surface radar absorbing after drying and sintering.The high temperature resistant high impedance surface radar absorbing of the present invention can be resistant at least 1000 DEG C of high temperature, have preferable heat-resisting quantity and excellent inoxidizability.
Description
Technical field
The present invention relates to radar absorbing field more particularly to a kind of high temperature resistant high impedance surface radar absorbing and
Preparation method.
Background technology
Radar absorbing can be divided into room temperature (temperature in use is less than 200 DEG C) and high temperature two according to service temperature range
Major class.In comparison, the research comparative maturity of current ambient temperature radar absorbing, and also to the research of high temperature radar absorbing
In trying to explore.
It has disclosed at present and reports several high temperature microwave-absorbing ceramic structures and preparation method thereof.No. ZL201110052115.1
Chinese patent discloses a kind of composite material of silicon carbide microwave-absorbing ceramic of three-decker and preparation method thereof, the suction wave pottery of this report
Porcelain is made of matching layer, depletion layer and reflecting layer, need to have different dielectric properties according to each functional layer of design requirement, preparation
Reflectivity of the microwave-absorbing ceramic in 8GHz~18GHz frequency ranges is smaller than -9dB.ZL201110053460.7 Chinese patents disclose
A kind of composite material of silicon carbide microwave-absorbing ceramic of four-layer structure and preparation method thereof, the microwave-absorbing ceramic of this report by matching layer,
Depletion layer, dielectric layer and reflecting layer composition, need to have different dielectric properties, the suction wave of preparation according to each functional layer of design requirement
Reflectivity in ceramic room temperature 8GHz~18GHz frequency ranges is smaller than -8dB, and under 700 DEG C of high temperature examinations, reflectivity is less than -8dB
Bandwidth still have nearly 10GHz or so.But high temperature microwave-absorbing ceramic disclosed above is wanted according to the different electrical property of each functional layer
The silicon carbide fibre of different resistivity need to be prepared by asking, and realization acquires a certain degree of difficulty, and cost is higher；And suction wave reported above
Ceramics are multilayered structure, and the process is more complicated, and technological requirement is higher.For the above patent there are the problem of,
ZL201410128311.6 Chinese patents disclose microwave-absorbing ceramic and its preparation of a kind of single layer structure composite material of silicon carbide
Method, simple in structure, thinner thickness, but the Modulatory character of dielectric constant is not strong, is only capable of realizing the suction wave energy of specific band,
Can design space it is smaller.
Invention content
The technical problem to be solved by the present invention is to overcome the shortcomings of to mention in background above technology and defect, provide one
Kind high temperature resistant high impedance surface radar absorbing and preparation method thereof；Utilize high impedance surface and ceramic matric composite technology
It is combined the high temperature resistant high impedance surface absorbing material being prepared into, the electromagnetic property that can both utilized high impedance surface excellent makes suction
Wave material absorbing property has stronger designability and better absorbing property；Ceramic matric composite body can be utilized again
Being advantage makes absorbing material have preferable heat-resisting quantity and mechanical property.
In order to solve the above technical problems, technical solution proposed by the present invention is：
A kind of high temperature resistant high impedance surface radar absorbing is double-layer structure, includes the medium substrate layer in bottom
With the high impedance surface layer in surface layer, the medium substrate layer, which is oxide fibre, enhances oxide-base composite material；It is described
High impedance surface layer in the high temperature resistant resistance coating of periodic patterns mainly by forming.Depend on the high impedance table of medium substrate layer
The absorption to electromagnetic wave and decaying may be implemented in face.
Above-mentioned absorbing material, it is preferred that the oxide fibre enhancing oxide-base composite material includes quartz fibre
Enhancing silica matrix composites, aluminosilicate fibre enhancing aluminosilicate based composites, mullite fiber enhances mullite
Composite material or alumina fibre enhance alumina matrix composite.The these types of continuous oxidation fibres enhancing that the present invention chooses
Oxide composite can not only ensure the mechanical property and thermal shock resistance that absorbing material product has had, moreover it is possible to ensure to inhale
Wave material has high temperature resistant, antioxygenic property, after the high temperature resistant resistance coating covering on upper layer, still has required electrical
Energy.
Above-mentioned absorbing material, it is preferred that the material system of the high temperature resistant resistance coating is ruthenic oxide system glass base
Resistive coating.It is excellent that ruthenic oxide system glass base resistive coating can ensure that there is absorbing material high temperature resistant and resistance characteristic to stablize
Gesture.
Above-mentioned absorbing material, it is preferred that the periodic patterns of the high temperature resistant resistance coating refer to being distributed in matrix form
Square patch pattern, the length of side of matrix unit where aforementioned square patch is 12mm~21mm, the square patch
The length of side and matrix unit the length of side ratio be 0.5~0.8.
Above-mentioned absorbing material, it is preferred that the thickness of the high temperature resistant resistance coating is 0.01~0.04mm；The medium
The thickness of basal layer is 2~5mm.Select the thickness of the resistive coating that can ensure that resistance value is met the requirements；Choose the medium base
The thickness of bottom can not only ensure that absorbing material is light, thin, and also ensure the high impedance table for being attached to the medium substrate layer
Face layer can be best its high temperature resistant of performance and absorbing property.
The inventive concept total as one, the present invention also provides a kind of preparation method of above-mentioned absorbing material, including it is following
Step：
(1) it chooses and preparation media substrate：Choosing suitable continuous oxidation fibres according to design requirement enhances oxide
Based composites then prepare corresponding composite material as media substrate materials, finally, thick according to the design of medium substrate
Degree is machined composite material, obtains required medium substrate；
(2) high impedance surface layer is prepared：Using silk-screen printing technique, the painting of the high temperature resistant resistance coating will be used to prepare
The medium substrate surface that material is printed on step (1) preparation obtains the high temperature resistant high impedance surface radar after drying and sintering
Absorbing material.
Above-mentioned preparation method, it is preferred that in the step (2), the preparation method of high temperature resistant resistance coating is as follows：By glass
Through 1300 DEG C~1500 DEG C of temperature melting 1h~3h after glass material powder is uniformly mixed, then obtained glass melt is poured into
Quenching is carried out in deionized water, obtains glass, then glass marble is worn into elder generation and RuO after glass powder2Powder after mixing again with have
Airborne body is uniformly mixed and high temperature resistant resistance coating is made；
The mass percent of each chemical constituent is respectively in the wherein described glass raw material powder：
SiO230%~50%；
Al2O310%~25%；
PbO 12%~25%；
MgO 5%~15%；
CaO 5%~10%；
ZnO 3~10%；
BaO 2%~8% and B2O31%~5%.
The process that above-mentioned glass marble wears into glass powder carries out ball milling, ball milling in agate jar by ball-milling medium of acetone
Technical process in, ball material mass ratio be (2~3):1, rotational speed of ball-mill be 380r/min~450r/min, Ball-milling Time be 6h~
12h；Powder after ball milling crosses the mesh sieve of 200 mesh~400.
Above-mentioned glass powder and RuO2The mixed process of powder mixes in planetary gravity mixer, planetary gravity blender
Revolution speed 1280rpm~1500rpm, rotational velocity be revolution speed 30%~60%, 60~120min of mixing time.
Above-mentioned glass and RuO2Mixed powder and the mixed process of organic carrier carried out in three-roll grinder, three rollers are ground
The rotating speed of grinding machine is 250~450r/min, and grinding mixing time is 3~6h.
Above-mentioned preparation method, it is preferred that in the step (2), RuO2Powder accounts for glass powder and RuO2Powder gross mass
45%~85%, the mass fraction of organic carrier is 25%~20% in the high temperature resistant resistance coating；Organic carrier mainly by
Mass fraction is 80%~90% tributyl citrate, 2%~5% nitrocellulose, 10%~15% lecithin composition.
Above-mentioned preparation method, it is preferred that in the step (2), use during silk-screen printing technique meshcount for
180~300 mesh, printing pass are 1~3 time；Temperature in drying process is 150 DEG C~250 DEG C, and drying time is 2h~4h；
Peak firing temperature in sintering process is 1000 DEG C~1050 DEG C, and the heating rate in sintering process is 15 DEG C/min~20
DEG C/min, sintering time is 10min~120min.
Above-mentioned preparation method, it is preferred that in the step (2), high temperature resistant resistance dope viscosity is 170~300pa
s。
Compared with the prior art, the advantages of the present invention are as follows：
(1) high temperature resistant high impedance surface radar absorbing of the invention is multiple with continuous oxidation fibres enhancing oxide
Condensation material is medium substrate, and high impedance surface layer is very thin and sintering is on medium substrate surface, utilizes high impedance surface and ceramics
Based composites technology, which is combined, is prepared into high temperature resistant high impedance surface absorbing material, on the one hand, can utilize high impedance surface
Excellent electromagnetic property makes absorbing material absorbing property have stronger designability and better absorbing property；Another party
Face can utilize ceramic matric composite system advantage that absorbing material is made to have preferable temperature tolerance and mechanical property, thus have
There are preferable mechanical property and thermal shock resistance, so as to realize the integration for inhaling the multi-functionals such as wave, carrying and solar heat protection.
(2) high temperature resistant high impedance surface radar absorbing of the invention can be resistant at least 1000 DEG C of high temperature, have
Preferable heat-resisting quantity and excellent inoxidizability.
(3) high temperature resistant high impedance surface radar absorbing of the present invention has surmounted traditional material microstructure composition and has determined
The pattern of macro property can control the electromagnetic performance of material by adjusting the electromagnetic structure of sub-wavelength, can thickness compared with
Realize that required absorbing property meets the lightweight demand of component to alleviate the weight of product in the case of small.
(4) the high temperature resistant high impedance surface radar absorbing that the present invention obtains is simple in structure, entire step of preparation process
Simply, industrialized production can be efficiently applied to.
Description of the drawings
Fig. 1 is the structural schematic diagram of high temperature resistant high impedance surface radar absorbing of the present invention.
Fig. 2 is the high temperature resistant resistance coating photo prepared in the embodiment of the present invention 1.
Fig. 3 is the high temperature resistant high impedance surface radar absorbing tablet sample photo prepared in the embodiment of the present invention 1.
Fig. 4 be the embodiment of the present invention 1 in prepare high temperature resistant high impedance surface radar absorbing room temperature, 1000 DEG C with
And restore the reflectance curve of room temperature after 1000 DEG C of examinations.
Specific implementation mode
To facilitate the understanding of the present invention, it is done more entirely below in conjunction with Figure of description and preferred embodiment to inventing herein
Face meticulously describes, but protection scope of the present invention is not limited to specific embodiment.
Unless otherwise defined, all technical terms used hereinafter are generally understood meaning phase with those skilled in the art
Together.Technical term used herein is intended merely to the purpose of description specific embodiment, is not intended to the limitation present invention's
Protection domain.
Unless otherwise specified, various raw material, reagent, the instrument and equipment etc. used in the present invention can pass through city
Field is commercially available or can be prepared by existing method.
Embodiment 1：
A kind of high temperature resistant high impedance surface radar absorbing of the present invention, as shown in Figure 1, including the medium in bottom
Substrate and high impedance surface layer in surface layer, medium substrate are located at reflection by lining；Wherein, media substrate materials, which are chosen, does not come
Mineral wool enhances mullite composite material, thickness d=3.0mm of medium substrate；High impedance surface layer is by being in periodic patterns
High temperature resistant resistance coating (using ruthenic oxide as ruthenic oxide system glass base electricity that conductive phase, lead borosilicate glass are binder
Resistance coating) composition, thickness 0.02mm；The periodic patterns of high temperature resistant resistance coating are the square patch in matrix form distribution
Pattern, the length of side a=13.32mm of matrix unit, the length of side of square patch and the length of side of matrix unit where square patch
Ratio be x=0.63.
The preparation method of the high temperature resistant high impedance surface radar absorbing of the present embodiment, includes the following steps：
(1) preparation media substrate：Choosing mullite fiber according to design requirement enhances mullite composite material as medium
Base material, then, preparing mullite fiber using sol-gel technology enhances mullite composite material, and to composite material
It is machined, obtains the medium substrate that thickness is 3.0mm；
(2) high temperature resistant resistance coating is prepared：
(a) smelting glass：It is respectively SiO by each chemical constituent content245%, Al2O315%, PbO12%, MgO 8%,
CaO 5%, ZnO 7%, BaO 5%, B2O33% glass raw material powder is uniformly mixed, and is fitted into platinum crucible, then set together
In Muffle furnace, 1400 DEG C, melting 3h are raised to the heating rate of 20 DEG C/min, then, the glass melt after fusing is poured into
Quenching is carried out in deionized water, obtains glass dregs；
(b) glass is crushed：Obtained glass dregs are subjected to ball milling in agate jar, using acetone as ball-milling medium, ball
Expect that mass ratio is 2：100 DEG C of drying 1h after the completion of ball milling, 1, rotating speed 450r/min, Ball-milling Time 8h cross 250 mesh sieve, obtain
To glass powder；
(c) batch mixing：By obtained glass powder and RuO2Powder is 45 according to mass ratio：55 ratio is in planetary gravitational agitation
The revolution speed of batch mixing in machine, blender is 1460rpm, and rotational velocity is the 30% of revolution speed, mixing time 120min；
(d) coating is prepared：First by tributyl citrate, nitrocellulose and lecithin according to 80：5：15 mass ratio
It is configured to organic carrier, then, by glass obtained and RuO in above-mentioned steps (c)2Mixed powder presses 75 with organic carrier：25
Mass ratio mixing, then grind batch mixing in three-roll grinder, three-roll grinder rotating speed is 300r/min, and three-roll grinder is mixed
The material time is 3h, obtains high temperature resistant resistance coating (viscosity of coating is 250Pas), photo is as shown in Figure 2；
(3) high impedance surface layer is prepared：Using silk-screen printing technique (250 mesh of meshcount is printed 1 time), by step (2)
The medium substrate surface that the high temperature resistant resistance coating of preparation is printed on step (1) preparation then (is kept the temperature through drying at 250 DEG C
2h) and sintering process (1000 DEG C of peak firing temperature, heating rate be 20 DEG C/min, sintering time 10min), high impedance surface
Layer is just sintered that (high impedance surface layer thickness is 0.02mm, and it is in matrix form to have on high temperature resistant resistance coating on medium substrate surface
The square patch pattern of distribution, the length of side of matrix unit where square patch are 13.32mm, the length of side of square patch with
The ratio of the length of side of matrix unit be 0.63) to get to the present invention high temperature resistant high impedance surface radar absorbing, tablet
Photo is as shown in Figure 3.
The high temperature resistant high impedance surface radar absorbing of the present embodiment is tested within the scope of 4~8GHz, room temperature, 1000
DEG C, be returned to reflectivity under three state of temperatures of room temperature after 1000 DEG C of examinations, as shown in figure 4, test result is found, inhale wave material
For material under three state of temperatures, the reflectivity within the scope of 4~8GHz is respectively less than -5.5dB.
Embodiment 2：
A kind of high temperature resistant high impedance surface radar absorbing of the present invention, as shown in Figure 1, including the medium in bottom
Substrate and high impedance surface layer in surface layer, medium substrate are located at reflection by lining；Wherein, media substrate materials choose oxidation
Aluminum fiber enhances alumina matrix composite, thickness d=2.6mm of medium substrate；High impedance surface layer is by being in periodic patterns
High temperature resistant resistance coating (using ruthenic oxide as ruthenic oxide system glass base electricity that conductive phase, lead borosilicate glass are binder
Resistance coating) composition, the thickness of resistive coating is 0.03mm；The periodic patterns of high temperature resistant resistance coating are distributed in matrix form
Square patch pattern, the length of side a=18.87mm of matrix unit, the length of side and matrix of square patch where square patch
The ratio of the length of side of unit is x=0.74.
The preparation method of the high temperature resistant high impedance surface radar absorbing of the present embodiment, includes the following steps：
(1) preparation media substrate：Choosing alumina fibre according to design requirement enhances alumina composite material as medium
Base material, then, preparing alumina fibre using sol-gel technology enhances alumina composite material, and to composite material
It is machined, obtains the medium substrate that thickness is 2.6mm；
(2) high temperature resistant resistance coating is prepared：
(a) smelting glass：It is respectively SiO by each chemical constituent content238%, Al2O322%, PbO12%, MgO 8%,
CaO 7%, ZnO 5%, BaO 4%, B2O34% glass raw material powder is uniformly mixed according to a ratio, and is fitted into platinum crucible, then
It is placed in Muffle furnace together, is raised to 1450 DEG C, melting 2.5h with 20 DEG C/min, then, the glass melt after fusing is poured into
Quenching is carried out in ionized water, obtains glass dregs；
(b) glass is crushed：Glass dregs are subjected to ball milling, ball material mass ratio in agate jar by ball-milling medium of acetone
It is 2：1, rotating speed 450r/min, Ball-milling Time 12h, ball milling dry 1h in 100 DEG C, cross 300 mesh sieve after the completion, obtain glass
Powder；
(c) batch mixing：By glass powder and RuO2Powder is according to mass ratio 48：52 ratio is mixed in planetary gravity mixer
The revolution speed of material, planetary gravity blender is 1500rpm, and rotational velocity is the 40% of revolution speed, and mixing time is
120min；
(d) coating is prepared：First by tributyl citrate, nitrocellulose and lecithin according to 80：5：15 mass ratio
It is configured to organic carrier.Then, by glass obtained and RuO in above-mentioned steps (c)2Mixed powder presses 78 with organic carrier：22
Mass ratio mixing, then grind batch mixing in three-roll grinder, three-roll grinder rotating speed is 300r/min, grinds mixing time
For 3h, obtain high temperature resistant resistance coating (viscosity of coating is 300Pas)；
(3) high impedance surface layer is prepared：Using silk-screen printing technique (300 mesh of meshcount is printed 2 times), by step (2)
The medium substrate surface that the high temperature resistant resistance coating of middle preparation is printed on step (1) preparation then (is kept the temperature through drying at 250 DEG C
2h) and sintering process (1000 DEG C of peak firing temperature, heating rate be 20 DEG C/min, sintering time 30min), high impedance surface
Layer is just sintered that (thickness of high impedance surface layer is 0.03mm, on high impedance surface layer in medium substrate surface prepared by step (1)
With the square patch pattern being distributed in matrix form, the length of side 18.87mm of matrix unit where square patch, square patch
The ratio 0.74 of the length of side of piece and the length of side of matrix unit) to get to the present invention high temperature resistant high impedance surface radar-wave absorbing material
Material.
High temperature resistant high impedance surface radar absorbing made from the present embodiment is tested within the scope of 8~12GHz, room temperature,
1000 DEG C, be returned to reflectivity under three state of temperatures of room temperature after 1000 DEG C of examinations, test result is found, in three temperature
Under state, -10dB is respectively less than within the scope of 8~12GHz.
Claims (7)
1. a kind of high temperature resistant high impedance surface radar absorbing, which is characterized in that the absorbing material is double-layer structure, including
Medium substrate layer in bottom and the high impedance surface layer in surface layer, the medium substrate layer, which is oxide fibre, enhances oxygen
Compound based composites；The high impedance surface layer in the high temperature resistant resistance coating of periodic patterns mainly by forming；The oxygen
Compound fiber reinforcement oxide-base composite material includes quartz fibre enhancing silica matrix composites, aluminosilicate fibre enhancing aluminium
Silicate-based composite material, mullite fiber enhancing mullite composite material or alumina fibre enhance alumina base composite wood
Material；The material system of the high temperature resistant resistance coating is ruthenic oxide system glass base resistive coating；The high temperature resistant resistance coating
By being prepared for high temperature resistant resistance coating, the preparation method of high temperature resistant resistance coating is as follows：Glass raw material powder is mixed equal
Through 1300 DEG C~1500 DEG C of temperature melting 1h~3h after even, then obtained glass melt is poured into deionized water and is quenched
It is cold, obtain glass, then glass marble is worn into elder generation and RuO after glass powder2Powder is uniformly mixed system with organic carrier again after mixing
At high temperature resistant resistance coating；
The mass percent of each chemical constituent is respectively in the wherein described glass raw material powder：
SiO230%~50%；
Al2O310%~25%；
PbO 12%~25%；
MgO 5%~15%；
CaO 5%~10%；
ZnO 3~10%；
BaO 2%~8% and B2O31%~5%.
2. absorbing material as described in claim 1, which is characterized in that the periodic patterns of the high temperature resistant resistance coating refer to
In the square patch pattern that matrix form is distributed, the length of side of matrix unit is 12mm~21mm, institute where aforementioned square patch
The ratio for stating the length of side of square patch and the length of side of matrix unit is 0.5~0.8.
3. absorbing material as described in claim 1, which is characterized in that the thickness of the high temperature resistant resistance coating be 0.01~
0.04mm；The thickness of the medium substrate layer is 2~5mm.
4. a kind of preparation method of such as claims 1 to 3 any one of them absorbing material, which is characterized in that including following step
Suddenly：
(1) it chooses and preparation media substrate：
(2) high impedance surface layer is prepared：Using silk-screen printing technique, the coating for being used to prepare the high temperature resistant resistance coating is printed
Brush is inhaled after drying and sintering to get to the high temperature resistant high impedance surface radar in medium substrate surface prepared by step (1)
Wave material.
5. preparation method as claimed in claim 4, which is characterized in that in the step (2), RuO2Powder account for glass powder and
RuO2The 45%~85% of powder gross mass, the mass fraction of organic carrier is 20%~25% in the high temperature resistant resistance coating.
6. preparation method as claimed in claim 4, which is characterized in that in the step (2), using silk-screen printing technique process
Middle meshcount is 180~300 mesh, and printing pass is 1~3 time；Temperature in drying process is 150 DEG C~250 DEG C, when dry
Between be 2h~4h；Peak firing temperature in sintering process is 1000 DEG C~1050 DEG C, and the heating rate in sintering process is 15
DEG C/min~20 DEG C/min, sintering time is 10min~120min.
7. preparation method as claimed in claim 4, which is characterized in that in the step (2), high temperature resistant resistance dope viscosity is
170~300Pa s.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610330896.9A CN106007804B (en) | 2016-05-18 | 2016-05-18 | A kind of high temperature resistant high impedance surface radar absorbing and preparation method thereof |
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| CN201610330896.9A CN106007804B (en) | 2016-05-18 | 2016-05-18 | A kind of high temperature resistant high impedance surface radar absorbing and preparation method thereof |
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| CN106007804A CN106007804A (en) | 2016-10-12 |
| CN106007804B true CN106007804B (en) | 2018-10-02 |
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| CN109956667A (en) * | 2017-12-26 | 2019-07-02 | 北京有色金属研究总院 | A kind of alkali corrosion resistance glass coating resistant to high temperatures and preparation method thereof |
| CN109830809A (en) * | 2019-02-21 | 2019-05-31 | 南京邮电大学 | A kind of multi-layer annular Terahertz Meta Materials wave absorbing device |
| CN109720027B (en) * | 2019-03-05 | 2019-12-27 | 中南大学 | High-temperature-resistant structural wave-absorbing material based on metal coating and preparation method thereof |
| CN111170753B (en) * | 2020-01-21 | 2022-05-17 | 烟台大学 | Circuit-screen-containing ceramic wave-absorbing material with high-temperature resistance and preparation method thereof |
| CN111733595B (en) * | 2020-06-30 | 2023-01-03 | 中国人民解放军国防科技大学 | High-temperature oxidation-resistant flexible conductive oxide ceramic fiber fabric composite material and preparation method thereof |
| CN114621728A (en) * | 2020-12-10 | 2022-06-14 | 南京航空航天大学 | High-temperature-resistant broadband wave-absorbing structure composite material and preparation method thereof |
| CN114603937B (en) * | 2022-03-09 | 2023-03-31 | 电子科技大学 | High-temperature-resistant radar infrared compatible stealth material and preparation method thereof |
| CN115073005B (en) * | 2022-07-21 | 2022-11-08 | 西安宏星电子浆料科技股份有限公司 | Anti-precipitation LTCC insulating medium slurry |
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