CN104876616B - A kind of high temperature resistant absorbing material and preparation method thereof - Google Patents
A kind of high temperature resistant absorbing material and preparation method thereof Download PDFInfo
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- CN104876616B CN104876616B CN201510187494.3A CN201510187494A CN104876616B CN 104876616 B CN104876616 B CN 104876616B CN 201510187494 A CN201510187494 A CN 201510187494A CN 104876616 B CN104876616 B CN 104876616B
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Abstract
The invention discloses a kind of high temperature resistant absorbing material, be with quartz based on, quartz fibre acupuncture part as strengthen phase composite, contain chopped carbon fiber in the composite, the length of chopped carbon fiber is 5～6mm, and chopped carbon fiber volume content in the composite is 0.002～0.005g/cm3, the bulk density of the quartz fibre acupuncture part is 0.43～0.45g/cm3.The preparation method of the present invention is comprised the following steps：Choose raw material, prepare fiber preform, fiber preform repeatedly impregnated, gel and heat treatment be until complete densification.In the case where thickness is 3.5mm, reflectance can be less than 8dB in 8～18GHz band limits to the high temperature resistant absorbing material of the present invention, have preferable absorbing property in the case of thickness is less.The preparation method of the present invention, processing step are simple, produce without harmful, poisonous pollutant in technical process, and being compatible with the environment property is good.
Description
Technical field
The invention belongs to radar absorbing field, more particularly to a kind of high temperature resistant absorbing material and preparation method thereof.
Background technology
The radar-wave absorbing ceramic material developed at present mainly has two kinds.One kind is with ceramic particle as radar absorbent material, adopts
The granule that molding is prepared with heat pressing process strengthens ceramic material, and such as Si/C/N ceramic particles strengthen LAS glass, mullite, Si3N4
Deng ceramic material, but such material has the following disadvantages：1) dielectric properties are difficult to Gradient distribution, radar absorption frequency band compared with
It is narrow；2) granule enhancing ceramic material toughness is poor, and catastrophic failure easily occurs；3) heat pressing process is difficult to prepare large complicated structure
Part.Another kind is Continuous Fiber Reinforced Ceramic Matrix Composites, and this kind of material has high temperature resistant, high specific strength, high ratio due to which
Modulus, high tenacity, the advantages of be easy to molding complex large-scale component, become the primary study side of current radar microwave-absorbing ceramic material
To.
Such as China of the Chinese patent literature of Patent No. ZL 201110052115.1 and ZL 201110053460.7
Patent documentation discloses a kind of continuous carbofrax fibre strengthens radar-wave absorbing ceramics and its preparation side of composite material of silicon carbide
Method.Wherein, No. 201110052115.1 Chinese patent literatures of ZL disclose a kind of including matching layer, depletion layer and reflecting layer
Multi-functional superimposed type structure radar-wave absorbing ceramics, reflectance of the microwave-absorbing ceramic which is prepared in 8GHz～18GHz frequency ranges can be little
In -9dB；And No. 201110053460.7 Chinese patent literatures of ZL disclose it is a kind of include matching layer, depletion layer, dielectric layer and
The multi-functional superimposed type structure radar-wave absorbing ceramics in reflecting layer, its microwave-absorbing ceramic for preparing, under room temperature, 8GHz～18GHz frequency ranges
Interior reflectance is smaller than -8dB, and moreover, under 700 DEG C of high temperature examinations, its reflectance still has nearly less than the bandwidth of -8dB
10GHz or so.
Two kinds of radar-wave absorbing ceramics disclosed above all have excellent microwave absorbing property, but still have the following disadvantages：1) adopt
It is with silicon carbide fiber reinforced silicon carbide composite material, relatively costly；2) need silicon carbide fibre is carried out special handling to obtain
Desired electrical property, complex process；3) multiple structure is adopted, process parameter control is more difficult；4) using two-dimentional composite wood
Material version, without fiber reinforcement, interlaminar strength is undesirable for interlayer；5) using Two-dimensional Composites version prepare component compared with
For difficulty.
The Chinese patent literature of Patent No. ZL 201210139046.2 is proposed and adopts silicon carbide micro-powder for absorbent
The preparation method of three-dimensional quartz fiber reinforcement quartz absorbing material, solves the problems, such as above section, but the absorbing material for preparing is present
And inhale the narrower deficiency of wave frequency section.
The content of the invention
The technical problem to be solved in the present invention is to overcome the deficiencies in the prior art, there is provided a kind of low cost, simple structure, work
Skill is easy, technological parameter is easily-controllable and the high temperature resistant absorbing material with preferable broadband absorbing performance and preparation method thereof.
To solve above-mentioned technical problem, technical scheme proposed by the present invention is：
A kind of high temperature resistant absorbing material, be with quartz based on, quartz fibre acupuncture part as strengthen phase composite, institute
Contain chopped carbon fiber in stating composite, the length of the chopped carbon fiber is 5～6mm, and chopped carbon fiber is in absorbing material
In volume content be 0.002～0.005g/cm3, the bulk density of the quartz fibre acupuncture part is 0.43～0.45g/cm3。
Above-mentioned absorbing material, it is preferred that described absorbing material surface is provided with glass coating, the thickness of the glass coating
Spend for 0.1～0.2mm.
Used as a total inventive concept, the present invention also provides a kind of preparation method of above-mentioned absorbing material, including following
Step：
1) it is that the chopped carbon fiber of 5～6mm, quartz fibre net tire, quartz fabric and Ludox are raw material to choose length；
2) chopped carbon fiber is dispersed in the quartz fibre net tire, then by quartz fibre net tire and described
Quartz fabric is alternately laminated to make quartz fibre acupuncture part, and is prepared into fiber preform using needling process；
3) fiber preform impregnated in and carry out in the Ludox 4～8h of vacuum impregnation, vacuum is less than
100Pa；
4) by step 3) dipping after fiber preform carry out gel, in the gel process temperature control be 180～200
DEG C, heating rate during gel is 1～2 DEG C/min, and gel temperature retention time is 2～4h；
5) by step 4) fiber preform after gel carries out heat treatment, the temperature of the heat treatment process in an inert atmosphere
At 750～850 DEG C, heating rate during heat treatment is 5～10 DEG C/min, and heat treatment time is 30～60min for degree control；
6) by step 5) the quartz fibre prefabricated component after heat treatment is repeated several times above-mentioned step 3), step 4) and step 5)
Until completing densification, the high temperature resistant absorbing material is obtained.
Above-mentioned preparation method, it is preferred that the step 1) in, the particle diameter of Ludox is 20～40nm, and solid content is more than
30%, pH are 3～6.
Above-mentioned preparation method, it is preferred that the step 2) in, the interlayer of the quartz fabric of fiber preform and quartzy net tire
Density is 11～13 layers/cm, and the needling density of fiber preform is 20～25 pins/cm2。
Above-mentioned preparation method, it is preferred that the step 6) in, repeat step 3), step 4) and step 5) number of times be 8
～12 times.
Above-mentioned preparation method, it is preferred that in the step 6) after, by the external coating of obtained high temperature resistant absorbing material
One layer of glass paste, obtains high temperature resistant absorbing material of the surface with glass coating after dry, sintering.
Above-mentioned preparation method, it is preferred that the solid content of described glass paste is 65～70%；The glass paste is adopted
Prepared with ball-milling technology：It is put into after glass dust is mixed with organic carrier in ball grinder, with 1:2 ratio of grinding media to material ball mill mixing,
Rotating speed during ball milling is 400 revs/min, and Ball-milling Time is 1～2h；The organic carrier be 79wt% butyl carbitols,
10wt% tributyl citrate, 3wt% ethyl celluloses, 3wt% Spans -85 and 5wt%1,4- butyrolactone.
Above-mentioned preparation method, it is preferred that the main component of the glass dust contains 59.3wt%SiO2, 22.4wt%
The Al of CaO, 13.5wt%2O3With the MgO of 2.96wt%.
Above-mentioned preparation method, it is preferred that temperature when being dried is 300～350 DEG C, drying time is 2～3h；Institute
Temperature when stating sintering is 850～900 DEG C, and sintering time is 0.5～1h, and sintering atmosphere is nitrogen.
Compared with prior art, it is an advantage of the current invention that：
1), in the case where thickness is 3.5mm, reflectance is in 8～18GHz frequency range models for high temperature resistant absorbing material of the invention
Can there can be preferable absorbing property in the case of thickness is less less than -8dB in enclosing；
2) high temperature resistant absorbing material of the invention adopts three-dimensional quartz fibre prickling part for reinforcement, good integrity, interlayer
Intensity is high, and easily prepared complex component；
3) high temperature resistant absorbing material of the invention adopts single layer structure form, compares the multilamellar absorbent structure tool of existing patent
Have the advantages that simple structure, parameter controllability are good；
4) high temperature resistant absorbing material raw materials used (quartz fibre, Ludox, carbon fiber) of the invention is domesticized, former
Material wide material sources and relative low price；The product and method of the present invention enriches the existing system of high temperature resistant absorbing material；
5) high temperature resistant absorbing material surface of the invention scribbles one layer of glass coating, and antioxygenic property is strong.
6) preparation method of high temperature resistant absorbing material of the invention, not only processing step is simple, and equipment needed thereby small investment is whole
Produce without harmful, poisonous pollutant in individual technical process, being compatible with the environment property is good.
Description of the drawings
Fig. 1 is quartz fibre prefabricated component photo figure prepared by the embodiment of the present invention 1.
Fig. 2 is the photo figure of high temperature resistant absorbing material of the surface with glass coating prepared by the embodiment of the present invention 1.
Fig. 3 is the reflectance curves of high temperature resistant absorbing material prepared by the embodiment of the present invention 1.
Fig. 4 is the reflectance curves of high temperature resistant absorbing material prepared by the embodiment of the present invention 2.
Specific embodiment
For the ease of understanding the present invention, more complete is made to the present invention below in conjunction with Figure of description and preferred embodiment
Face, meticulously describe, but protection scope of the present invention is not limited to embodiment in detail below.
Unless otherwise defined, the implication that all technical terms used hereinafter are generally understood that with those skilled in the art
It is identical.Technical term used herein is intended merely to the purpose for describing specific embodiment, is not intended to limit the present invention
Protection domain.
Except there is a special instruction, the various reagents used in the present invention, raw material be commodity that can be commercially or
Person can be by product obtained in known method.
Embodiment 1：
A kind of high temperature resistant absorbing material of the present invention, be with quartz based on, quartz fibre acupuncture part answered to strengthen phase
Condensation material, containing the chopped carbon fiber that length is 5mm in composite, volume content of the chopped carbon fiber in absorbing material is
0.005g/cm3, the bulk density of quartz fibre acupuncture part is 0.444g/cm3。
In order to improve the antioxygenic property of absorbing material, absorbing material surface is additionally provided with the glass coating that thickness is 0.1mm.
The preparation method of the high temperature resistant absorbing material of the present embodiment, comprises the following steps：
1) it is 100 ± 5g/m to choose length for the 1K chopped carbon fibers of 5mm, surface density2Quartz fibre net tire, surface density
For 285 ± 5g/m2Quartz fibre plain and Ludox (Ludox particle diameter be 20～40nm, solid content is 32%, and pH value is
4) as raw material.
2) length is dispersed on each layer quartz fibre net tire for the 1K chopped carbon fibers of 5mm, then by quartz fibre
Net tire and quartz fibre plain is alternately laminated makes quartz fibre acupuncture part, and it is pre- to be prepared into quartz fibre using needling process
(interlayer density is 13 layers/cm to product, and needling density is 25 pins/cm2)；Quartz fibre prefabricated component photo is as shown in Figure 1.
3) by step 2) the quartz fibre prefabricated component for preparing impregnated in, and vacuum is
60Pa。
4) by step 3) dipping after quartz fibre prefabricated component carry out gel, in gel process temperature control be 180 DEG C, coagulate
Heating rate during glue is 2 DEG C/min, and gel temperature retention time is 2h.
5) by step 4) the quartz fibre prefabricated component after gel carries out heat treatment, the temperature of heat treatment process in nitrogen atmosphere
At 800 DEG C, heating rate during heat treatment is 10 DEG C/min, and heat treatment time is 30min for degree control.
6) by step 5) the quartz fibre prefabricated component after heat treatment is repeated 10 times above-mentioned step 3), step 4) and step 5)
Until completing densification, the high temperature resistant absorbing material is obtained.
In order to improve the antioxygenic property of absorbing material, in the high temperature resistant absorbing material surface brushing one of above-mentioned preparation
(solid content of glass paste is 65% to layer glass paste；Glass paste is prepared using ball-milling technology：By glass dust with it is organic
It is put in agate jar after the mixing of thing carrier, with 1:2 ratio of grinding media to material ball mill mixing, rotating speed during ball milling are 400 revs/min,
Ball-milling Time is 1h；Wherein organic carrier is 79wt% butyl carbitols, 10wt% tributyl citrate, 3wt% ethyls fibre
Dimension element, 3wt% Spans -85 and 5wt%1,4- butyrolactone, the main component of glass dust contain 59.3wt%SiO2, 22.4wt%
CaO, 13.5wt% Al2O3With the MgO of 2.96wt%), then it is dried 2 hours at 300 DEG C, finally in nitrogen atmosphere
Sintering 0.5 hour, sintering temperature are 850 DEG C, obtain high temperature resistant absorbing material of the surface with glass coating.
As shown in Fig. 2 the photo figure of the high temperature resistant absorbing material of glass coating is carried for surface.It is illustrated in figure 3 this
The reflectance curves of bright high temperature resistant absorbing material, it can be seen that high temperature resistant reflection index of wave suction material is in 8～18GHz
Band limits is below -8dB, with preferable broadband absorbing performance.
Embodiment 2：
A kind of high temperature resistant absorbing material of the present invention, be with quartz based on, quartz fibre acupuncture part answered to strengthen phase
Condensation material, containing the chopped carbon fiber that length is 6mm in composite, volume content of the chopped carbon fiber in absorbing material is
0.004g/cm3, the bulk density of quartz fibre acupuncture part is 0.437g/cm3。
In order to improve the antioxygenic property of absorbing material, absorbing material surface is additionally provided with the glass that thickness is 0.12mm and applies
Layer.
The preparation method of the high temperature resistant absorbing material of the present embodiment, comprises the following steps：
1) it is 100 ± 5g/m to choose length for the 1K chopped carbon fibers of 6mm, surface density2Quartz fibre net tire, surface density
For 285 ± 5g/m2Quartz fibre plain and Ludox (Ludox particle diameter be 20～40nm, solid content is 30%, and pH value is
4) as raw material.
2) length is dispersed on each layer quartz fibre net tire for the 1K chopped carbon fibers of 6mm, then by quartz fibre
Net tire and quartz fibre plain is alternately laminated makes quartz fibre acupuncture part, and it is pre- to be prepared into quartz fibre using needling process
(interlayer density is 12 layers/cm to product, and needling density is 20 pins/cm2)。
3) by step 2) the quartz fibre prefabricated component for preparing impregnated in, and vacuum is
50Pa。
4) by step 3) dipping after quartz fibre prefabricated component carry out gel, in gel process temperature control be 200 DEG C, coagulate
Heating rate during glue is 1 DEG C/min, and gel temperature retention time is 4h.
5) by step 4) the quartz fibre prefabricated component after gel carries out heat treatment, the temperature of heat treatment process in nitrogen atmosphere
At 850 DEG C, heating rate during heat treatment is 5 DEG C/min, and heat treatment time is 60min for degree control.
6) by step 5) the quartz fibre prefabricated component after heat treatment is repeated 12 times above-mentioned step 3), step 4) and step 5)
Until completing densification, the high temperature resistant absorbing material is obtained.
In order to improve the antioxygenic property of absorbing material, in the high temperature resistant absorbing material surface brushing one of above-mentioned preparation
(solid content of glass paste is 70% to layer glass paste；Glass paste is prepared using ball-milling technology：By glass dust with it is organic
It is put in agate jar after the mixing of thing carrier, with 1:2 ratio of grinding media to material ball mill mixing, rotating speed during ball milling are 400 revs/min,
Ball-milling Time is 2h；Wherein organic carrier is 79wt% butyl carbitols, 10wt% tributyl citrate, 3wt% ethyls fibre
Dimension element, 3wt% Spans -85 and 5wt%1,4- butyrolactone, the main component of glass dust contain 59.3wt%SiO2, 22.4wt%
CaO, 13.5wt% Al2O3With the MgO of 2.96wt%), then it is dried 3 hours at 350 DEG C, finally in nitrogen atmosphere
Sintering 1 hour, sintering temperature are 900 DEG C, obtain high temperature resistant absorbing material of the surface with glass coating.
As shown in figure 4, for the present invention high temperature resistant reflection index of wave suction material curve chart, the high temperature resistant for preparing as seen from the figure
Reflection index of wave suction material is below -8dB in 9.5～18GHz band limits, with preferable broadband absorbing performance.
Claims (8)
1. a kind of preparation method of absorbing material, it is characterised in that comprise the following steps：
1) it is that the chopped carbon fiber of 5～6mm, quartz fibre net tire, quartz fabric and Ludox are raw material to choose length；
2) chopped carbon fiber is dispersed in the quartz fibre net tire, then by quartz fibre net tire and the quartz
Cloth is alternately laminated to make quartz fibre acupuncture part, and is prepared into fiber preform using needling process, wherein, chopped carbon fiber exists
Volume content in fiber preform is 0.002～0.005g/cm3, the bulk density of the quartz fibre acupuncture part is 0.43
～0.45g/cm3；
3) fiber preform impregnated in and carry out in the Ludox 4～8h of vacuum impregnation, vacuum is less than 100Pa；
4) by step 3) dipping after fiber preform carry out gel, in the gel process temperature control be 180～200 DEG C,
Heating rate during gel is 1～2 DEG C/min, and gel temperature retention time is 2～4h；
5) by step 4) fiber preform after gel carries out heat treatment, the temperature control of the heat treatment process in an inert atmosphere
At 750～850 DEG C, heating rate during heat treatment is 5～10 DEG C/min to system, and heat treatment time is 30～60min；
6) by step 5) the quartz fibre prefabricated component after heat treatment is repeated several times above-mentioned step 3), step 4) and step 5) until
Densification is completed, high temperature resistant absorbing material is obtained.
2. preparation method as claimed in claim 1, it is characterised in that：The step 1) in, the particle diameter of Ludox is 20～
40nm, solid content are 3～6 more than 30%, pH.
3. preparation method as claimed in claim 1, it is characterised in that：The step 2) in, the quartz fabric of fiber preform with
The interlayer density of quartzy net tire is 11～13 layers/cm, and the needling density of fiber preform is 20～25 pins/cm2。
4. preparation method as claimed in claim 1, it is characterised in that：The step 6) in, repeat step 3), step 4) and step
Rapid number of times 5) is 8～12 times.
5. the preparation method as described in any one of Claims 1 to 4, it is characterised in that：In the step 6) after, will be obtained resistance to
One layer of glass paste of external coating of high temperature absorbing material, obtains high temperature resistant of the surface with glass coating and inhales after dry, sintering
Wave material.
6. preparation method as claimed in claim 5, it is characterised in that：The solid content of described glass paste is 65～70%；
The glass paste is prepared using ball-milling technology：It is put into after glass dust is mixed with organic carrier in ball grinder, with 1:2 ball
Than ball mill mixing, rotating speed during ball milling is 400 revs/min to material, and Ball-milling Time is 1～2h；The organic carrier is 79wt%
Butyl carbitol, 10wt% tributyl citrate, 3wt% ethyl celluloses, 3wt% Spans -85 and 5wt%1,4- butyrolactone.
7. preparation method as claimed in claim 6, it is characterised in that：The main component of the glass dust contains 59.3wt%
SiO2, 22.4wt% CaO, 13.5wt% Al2O3With the MgO of 2.96wt%.
8. preparation method as claimed in claim 5, it is characterised in that：Temperature when being dried is 300～350 DEG C, is dried
Time is 2～3h；The temperature during sintering is 850～900 DEG C, and sintering time is 0.5～1h, and sintering atmosphere is nitrogen.
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| CN106042515B (en) * | 2016-05-18 | 2017-11-21 | 中国人民解放军国防科学技术大学 | A kind of high temperature resistant radar absorbing of sandwich and preparation method thereof |
| CN106007804B (en) * | 2016-05-18 | 2018-10-02 | 中国人民解放军国防科学技术大学 | A kind of high temperature resistant high impedance surface radar absorbing and preparation method thereof |
| CN106220211B (en) * | 2016-07-26 | 2019-03-05 | 中国人民解放军国防科学技术大学 | A kind of composite material of silicon carbide microwave-absorbing ceramic and preparation method thereof based on Meta Materials |
| CN108129157B (en) * | 2018-01-02 | 2020-02-18 | 江西嘉捷信达新材料科技有限公司 | Quartz fiber reinforced quartz material and preparation method thereof |
| CN108437579A (en) * | 2018-05-16 | 2018-08-24 | 山东天磁新材料科技有限公司 | A kind of high temperature resistant Wave suction composite material and preparation method thereof |
| CN109503114B (en) * | 2018-10-30 | 2021-05-11 | 山东工业陶瓷研究设计院有限公司 | Preparation method of wave-transparent ablation heat-insulation integrated material |
| CN109524781B (en) * | 2018-11-21 | 2020-10-09 | 湖北三江航天江北机械工程有限公司 | Preparation method of Z-pin reinforced quartz composite ceramic wave-transparent radome |
| 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 |
| CN114605161B (en) * | 2020-12-03 | 2023-04-18 | 航天特种材料及工艺技术研究所 | Ceramic matrix composite with high fiber volume content and preparation method thereof |
| CN115196951B (en) * | 2022-07-19 | 2023-02-24 | 湖南工业大学 | Modified carbon fiber-mullite ceramic wave-absorbing material with multilayer structure and preparation method thereof |
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| JP2007036154A (en) * | 2005-07-29 | 2007-02-08 | Bussan Nanotech Research Institute Inc | Electromagnetic wave absorber |
| CN101224989A (en) * | 2008-01-29 | 2008-07-23 | 中国人民解放军国防科学技术大学 | Two-dimensional fiber cloth reinforced composite material and preparation method thereof |
| CN102249652B (en) * | 2011-04-29 | 2014-09-10 | 中国科学院上海硅酸盐研究所 | Fiber composite material with microwave absorbing function and preparation method thereof |
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