CN110241611A - A kind of high-temperature resistance carbon fiber magnetism Wave suction composite material and preparation method thereof - Google Patents
A kind of high-temperature resistance carbon fiber magnetism Wave suction composite material and preparation method thereof Download PDFInfo
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- CN110241611A CN110241611A CN201910528516.6A CN201910528516A CN110241611A CN 110241611 A CN110241611 A CN 110241611A CN 201910528516 A CN201910528516 A CN 201910528516A CN 110241611 A CN110241611 A CN 110241611A
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- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 72
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 72
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 71
- 239000002131 composite material Substances 0.000 title claims abstract description 33
- 230000005389 magnetism Effects 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000000835 fiber Substances 0.000 claims abstract description 74
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 40
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 38
- 239000000463 material Substances 0.000 claims abstract description 37
- 238000000034 method Methods 0.000 claims abstract description 37
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 36
- 230000008569 process Effects 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000008367 deionised water Substances 0.000 claims abstract description 21
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 21
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052582 BN Inorganic materials 0.000 claims abstract description 13
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims abstract description 11
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 11
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000004327 boric acid Substances 0.000 claims abstract description 11
- 239000004202 carbamide Substances 0.000 claims abstract description 11
- 239000008103 glucose Substances 0.000 claims abstract description 11
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims abstract description 11
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims abstract description 11
- 238000009832 plasma treatment Methods 0.000 claims abstract description 11
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 claims abstract description 10
- 239000006249 magnetic particle Substances 0.000 claims abstract description 10
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims abstract description 10
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims abstract description 10
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims abstract description 8
- 238000007901 in situ hybridization Methods 0.000 claims abstract description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 22
- 238000001035 drying Methods 0.000 claims description 14
- 229920002239 polyacrylonitrile Polymers 0.000 claims description 13
- 229920000297 Rayon Polymers 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 11
- 238000002386 leaching Methods 0.000 claims description 9
- 230000003647 oxidation Effects 0.000 claims description 7
- 238000011282 treatment Methods 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 3
- 229910052796 boron Inorganic materials 0.000 claims description 2
- 230000008859 change Effects 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims 1
- CKUAXEQHGKSLHN-UHFFFAOYSA-N [C].[N] Chemical compound [C].[N] CKUAXEQHGKSLHN-UHFFFAOYSA-N 0.000 claims 1
- 239000000243 solution Substances 0.000 abstract description 20
- 239000011358 absorbing material Substances 0.000 abstract description 7
- 238000010521 absorption reaction Methods 0.000 abstract description 6
- 239000011259 mixed solution Substances 0.000 abstract description 5
- 238000007747 plating Methods 0.000 description 6
- 238000002411 thermogravimetry Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 4
- 238000002310 reflectometry Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000001360 synchronised effect Effects 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 239000004519 grease Substances 0.000 description 2
- 238000005979 thermal decomposition reaction Methods 0.000 description 2
- 230000008901 benefit Effects 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
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- C04B35/62844—Coating fibres
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Abstract
The invention belongs to absorbing material preparation technical fields more particularly to a kind of high-temperature resistance carbon fiber magnetism Wave suction composite material and preparation method thereof.High-temperature resistance carbon fiber magnetism Wave suction composite material provided by the invention includes: carbon fibre material；Boron nitride coated in the carbon fibre material surface；With the magnetic-particle by being generated with the carbon fibre material outermost layer in-situ hybridization.It cleans, dry in deionized water the preparation method comprises the following steps: carbon fiber material is prepared into after oxidization fiber, boric acid and urea mixed solution are immersed after plasma treatment, it pads, dry, then the carbon fiber that surface is covered with boron nitride is made in high-temperature process, the carbon fiber that surface is covered with boron nitride ferric sulfate, cobaltous sulfate, nickel sulfate, glucose is immersed again to be added in solution made of deionized water, it pads, dry, then high-temperature resistance carbon fiber magnetism Wave suction composite material is made in high-temperature process.High-temperature resistance carbon fiber magnetism Wave suction composite material high temperature resistance provided by the invention is good, and electromagnetic wave absorption performance is good.
Description
Technical field
The invention belongs to absorbing material preparation technical fields more particularly to a kind of high-temperature resistance carbon fiber magnetism to inhale wave composite wood
Material and preparation method thereof.
Background technique
In recent years, the microwave absorbing material of radar invisible is widely applied to the stealthy of the military platforms such as ocean, land
In system of defense, target radar reflective surface area can be effectively reduced, increases the difficulty that target is found.It is excellent in order to obtain
Magnetic loss is the effective way for improving electromaganic wave absorbing property in conjunction with dielectric material by microwave absorbing material.At present in carbonaceous
Material, such as carbon fiber, graphene and carbon nano tube surface modify various magnetic-particles to improve the absorbing property of carbonaceous material,
It can effectively be merged when it was found that preferable Fe, Co, Ni metal base magnetic material of soft magnet performance is in conjunction with carbonaceous absorbing material each
From the advantage and disadvantage of dielectric loss and magnetic loss, the wide Wave suction composite material of lightweight, absorption band is prepared.However, at present in carbon
The methods of plating, chemical plating, reduction are generallyd use on fiber prepares magnetisable coating.The shortcomings that these methods, has: 1, carbon fiber surface
The grease stain in face is difficult to clean, and causes particulate load loosely；2, the modes such as plating, chemical plating have certain pollution to environment；3, electric
The mode of plating and chemical plating causes magnetic-particle to hardly diffuse to inside fibrofelt；4, prepared carbon fiber-based absorbing material makes
With temperature generally at 500 DEG C；5, the electric conductivity of carbon fiber causes electromagnetic wave to be easy to be reflected.
Summary of the invention
In view of this, the purpose of the present invention is to provide a kind of high-temperature resistance carbon fiber magnetism Wave suction composite material and its preparations
Material electromagnetic wave absorption performance not only can be improved in method, carbon fiber magnetism Wave suction composite material provided by the invention, can be with
Improve the high temperature resistance of material.
The present invention provides a kind of high-temperature resistance carbon fiber magnetism Wave suction composite materials, comprising:
Carbon fibre material, the carbon fibre material are polyacrylonitrile-based carbon fibre or viscose base carbon fibre；
It is coated on the boron nitride on the carbon fibre material surface；
With the magnetic-particle by being generated with the carbon fibre material outermost layer in-situ hybridization.
The present invention also provides the preparation methods of above-mentioned carbon fiber magnetism Wave suction composite material, comprising:
S1: it using polyacrylonitrile fibre or viscose rayon as carbon fiber material, is gradually warmed up with 3~5 DEG C/min of rate
To 200~400 DEG C, the pre-oxidation treatment of progress 50~150 minutes, formation oxidization fiber, oxidization fiber is peace and quiet in deionized water,
Plasma treatment is carried out after drying；
S2: boric acid and urea are added in deionized water, the first solution is equipped to；
S3: by after the oxidization fiber that step S1 is handled is put into first solution and is padded 60 DEG C~120
DEG C drying；
S4: the oxidization fiber handled by step S3 is subjected to high-temperature process under the protection of nitrogen and obtains surface covering
There is the carbon fiber of boron nitride；
S5: deionized water is added in ferric sulfate, cobaltous sulfate, nickel sulfate, glucose, is equipped to the second solution；
S6: the carbon fiber is put into the second solution, is dried after padding at 60 DEG C~120 DEG C；
S7: resistance to by being prepared after the carbon fiber that step S6 is handled carries out high-temperature process under the protection of nitrogen
High-temperature carbon fiber magnetism Wave suction composite material；
Wherein, the carbon fiber is polyacrylonitrile-based carbon fibre or viscose base carbon fibre.
Preferably, drying temperature is 60 DEG C~100 DEG C in the step S1, and plasma processing condition is normal temperature and pressure, etc.
The ion processing time is 10~100 seconds.
Preferably, the mass ratio of boric acid, urea and plasma water is (1~5): (1~5) in the step S2: (20~
100)。
Preferably, the mass ratio of ferric sulfate in the step S5, cobaltous sulfate, nickel sulfate, glucose and plasma water is (1
~5): (1~5): (1~5): (0.1~5): (20~100).
Preferably, described pad is rolled for three leachings three, and dip time is 5min~30min, and pick-up is 50%~300%.
Preferably, the temperature of high-temperature process described in step S4 is 300 DEG C~1000 DEG C, and the time of the high-temperature process is
10min~100min.
Preferably, the temperature of high-temperature process described in step S4 is 600 DEG C~700 DEG C.
Preferably, the temperature of high-temperature process described in step S7 is 300 DEG C~1000 DEG C, and the time of the high-temperature process is
10min~100min.
Preferably, the temperature of high-temperature process described in step S7 is 600 DEG C~650 DEG C.
Compared with prior art, the present invention provides a kind of carbon fiber magnetism Wave suction composite materials and preparation method thereof.This
The carbon fiber magnetism Wave suction composite material that invention provides includes carbon fibre material；Overlay on the boron nitride on carbon fibre material surface；With
Pass through the magnetic-particle generated with carbon fibre material outermost layer in-situ hybridization.The present invention is using plasma processing techniques to fiber table
Face performs etching, and on the one hand can effectively remove the grease stain of fiber surface, interfibrous cohesive force on the other hand can be improved；
By the way that oxidization fiber to be immersed in the solution that boric acid and urea are prepared, then carries out high-temperature process and coated in carbon fiber surface
One layer of boron nitride (BN), on the one hand can be improved the high temperature resistance of carbon fiber, on the other hand can reduce filamentary conductive energy,
Reduce reflection of the carbon fiber to electromagnetic wave；Using dipping and high-temperature heat treatment process, generated in carbon fiber outermost layer in-situ hybridization
Magnetic loss and dielectric loss material are effectively combined by magnetic-particle, improve material electromagnetic wave absorption performance.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to do simply to introduce, it should be apparent that, the accompanying drawings in the following description is only this
The embodiment of invention for those of ordinary skill in the art without creative efforts, can also basis
The attached drawing of offer obtains other attached drawings.
Fig. 1 is the thermogravimetric analysis figure for the polyacrylonitrile-based carbon fibre magnetism Wave suction composite material that the embodiment of the present invention 1 provides；
Fig. 2 is the reflectance test for the polyacrylonitrile-based carbon fibre magnetism Wave suction composite material that the embodiment of the present invention 1 provides
Result figure.
Fig. 3 is the thermogravimetric analysis figure for the viscose base carbon fibre magnetism Wave suction composite material that the embodiment of the present invention 2 provides；
Fig. 4 is the reflectance test result for the viscose base carbon fibre magnetism Wave suction composite material that the embodiment of the present invention 2 provides
Figure.
Fig. 5 is the thermogravimetric analysis figure for the carbon fiber magnetism Wave suction composite material that comparative example 1 of the present invention provides；
Fig. 6 is the reflectance test result figure for the carbon fiber magnetism Wave suction composite material that comparative example 1 of the present invention provides.
Specific embodiment
The following is a clear and complete description of the technical scheme in the embodiments of the invention, it is clear that described embodiment
Only a part of the embodiment of the present invention, rather than whole embodiments.Based on the embodiments of the present invention, ordinary skill
Personnel's every other embodiment obtained without making creative work, belongs to the model that the present invention protects
It encloses.
The present invention provides a kind of high-temperature resistance carbon fiber magnetism Wave suction composite materials, comprising:
Carbon fibre material, the carbon fiber are polyacrylonitrile-based carbon fibre or viscose base carbon fibre；
It is coated on the boron nitride on the carbon fibre material surface；
With the magnetic-particle by being generated with the carbon fibre material outermost layer in-situ hybridization.
On the one hand the high temperature resistance of carbon fiber can be improved in the boron nitride for being coated on carbon fibre material surface, on the other hand
Filamentary conductive energy can be reduced, reflection of the carbon fiber to electromagnetic wave is reduced；It is generated with carbon fibre material outermost layer in-situ hybridization
Magnetic-particle magnetic loss and dielectric loss material are effectively combined, improve material electromagnetic wave absorption performance.
The present invention also provides the preparation methods of above-mentioned carbon fiber magnetism Wave suction composite material, comprising:
S1: it using polyacrylonitrile fibre or viscose rayon as carbon fiber material, is gradually warmed up with 3~5 DEG C/min of rate
To 200~400 DEG C, the pre-oxidation treatment of progress 50~150 minutes, formation oxidization fiber, oxidization fiber is peace and quiet in deionized water,
Plasma treatment is carried out after drying；
S2: boric acid and urea are added in deionized water, the first solution is equipped to；
S3: by after the oxidization fiber that step S1 is handled is put into first solution and is padded 60 DEG C~120
DEG C drying；
S4: the oxidization fiber handled by step S3 is subjected to high-temperature process under the protection of nitrogen and obtains surface covering
The carbon fiber of boron nitride；
S5: deionized water is added in ferric sulfate, cobaltous sulfate, nickel sulfate, glucose, is equipped to the second solution；
S6: the carbon fiber is put into the second solution, is dried after padding at 60 DEG C~120 DEG C；
S7: resistance to by being prepared after the carbon fiber that step S6 is handled carries out high-temperature process under the protection of nitrogen
High-temperature carbon fiber magnetism Wave suction composite material；
Wherein, the carbon fiber is polyacrylonitrile-based carbon fibre or viscose base carbon fibre.
In above-mentioned high-temperature resistance carbon fiber magnetism Wave suction composite material preparation method provided by the invention, first by carbon fiber
Raw material is prepared into oxidization fiber, then cleans, dries in deionized water to oxidization fiber, the temperature of drying is preferably 60 DEG C~100
DEG C, more preferably 100 DEG C.Then plasma treatment is carried out, the condition of plasma treatment is preferably normal temperature and pressure, plasma treatment
Time is preferably 10~100 seconds, and more preferably 20~30 seconds.Plasma treatment can more effectively remove the oil of fiber surface
Stain, and interfibrous cohesive force can be improved.Oxidization fiber is immersed in boric acid and urea mixed solution again after plasma treatment,
The mass ratio of boric acid, urea and plasma water is preferably (1~5): (1~5): (20~100) in mixed solution, 60 after padding
DEG C~120 DEG C of drying, then the carbon fiber that surface is coated with boron nitride is made in high-temperature process, pads preferably three leachings three and rolls, soaks
The stain time is preferably 5min~30min, more preferably 30min, and pick-up is preferably 50%~300%, and more preferably 300%.
The temperature of high-temperature process is preferably 300 DEG C~1000 DEG C, and more preferably 600 DEG C~700 DEG C, the time of high-temperature process is preferably
10min~100min, more preferably 60min.Then the carbon fiber that surface is coated with boron nitride is immersed into ferric sulfate, sulfuric acid again
Cobalt, nickel sulfate, glucose are added made of deionized water in solution, ferric sulfate in solution, cobaltous sulfate, nickel sulfate, glucose and
The mass ratio of plasma water is preferably (1~5): (1~5): (1~5): (1~5): (20~100), 60 DEG C~120 after padding
DEG C drying, then high-temperature resistance carbon fiber magnetism Wave suction composite material is made in high-temperature process, pads preferably three leachings and three rolls, when dipping
Between preferably 5min~30min, more preferably 30min, pick-up is preferably 50%~300%, more preferably 300%.High temperature
The temperature of processing is preferably 300 DEG C~1000 DEG C, and more preferably 600 DEG C~650 DEG C, which can be by the carbon of carbon fiber
Rate controls in a certain range, to play more effective dielectric loss performance.The time of high-temperature process be preferably 10min~
100min, more preferably 60min.
For the sake of becoming apparent from, it is described in detail below by embodiment.
Embodiment 1
S1: using polyacrylonitrile fibre as carbon fiber material, 300 DEG C is gradually heated to 5 DEG C/min of rate, is carried out
100 minutes pre-oxidation treatments form oxidization fiber, and oxidization fiber is peace and quiet in deionized water, in normal temperature and pressure after 100 DEG C of drying
Lower plasma treatment 30 seconds；
S2: 6g boric acid and 18g urea are added in 200mL deionized water, the first solution is equipped to；
S3: the oxidization fiber handled by step S1 being put into the first solution of step S2 outfit, and three leachings three are rolled,
Dip time is 30min, then pick-up 300% is dried at 100 DEG C；
S4: the oxidization fiber handled by step S3 is obtained under the protection of nitrogen in 650 DEG C of high-temperature process 60min
Carbon fiber；
S5: 4.1g ferric sulfate, 7.1g cobaltous sulfate, 3.3g nickel sulfate, 1g glucose are added in 100mL deionized water,
It is equipped to the second solution；
S6: the step S4 carbon fiber being prepared is put into the second solution, and three leachings three are rolled, and dip time 30min rolls
Then remaining rate 300% is dried at 100 DEG C；
S7: will be after the carbon fiber that step S6 is handled carries out 650 DEG C of high-temperature process 60min under the protection of nitrogen
High-temperature resistance carbon fiber magnetism Wave suction composite material is prepared.
Such as Fig. 1, synchronous solving (DSC/DTA-TG) STA449F5 thermogravimetric analysis is measured, and this product compares carbon fiber
At 650 DEG C, oxidation is complete substantially, and product prepared by the present invention aoxidizes at 900 DEG C and just reaches stable；
Such as Fig. 2, it is measured according to GJB2038A-2011 " radar absorbing reflectivity test method ", it is prepared
Material electromagnetic wave loss in 10.5-26GHz frequency range is less than -10dB.
Embodiment 2
S1: using viscose fiber as carbon fiber material, 300 DEG C is gradually heated to 5 DEG C/min of rate, carries out 100 points
The pre-oxidation treatment of clock forms oxidization fiber, and oxidization fiber is peace and quiet in deionized water, after 60 DEG C of drying it is equal at normal temperatures and pressures from
Subprocessing 20 seconds；
S2: 9 boric acid and 27g urea are added in 200mL deionized water, the first solution is equipped to；
S3: the oxidization fiber handled by step S1 being put into the first solution of step S2 outfit, and three leachings three are rolled,
Dip time is 30min, then pick-up 300% is dried at 100 DEG C；
S4: the oxidization fiber handled by step S3 is obtained under the protection of nitrogen in 700 DEG C of high-temperature process 60min
Carbon fiber；
S5: 5g ferric sulfate, 8g cobaltous sulfate, 4g nickel sulfate, 0.5g glucose are added in 100mL deionized water, are equipped with
At the second solution；
S6: the step S4 carbon fiber being prepared is put into the second solution, and three leachings three are rolled, then pick-up 300% exists
100 DEG C of drying；
S7: will be after the carbon fiber that step S6 is handled carries out 600 DEG C of high-temperature process 60min under the protection of nitrogen
High-temperature resistance carbon fiber magnetism Wave suction composite material is prepared.
Such as Fig. 1, synchronous solving (DSC/DTA-TG) STA449F5 thermogravimetric analysis is measured, and this product compares carbon fiber
Thermal decomposition temperature improves 150 DEG C；
Such as Fig. 2, it is measured according to GJB2038A-2011 " radar absorbing reflectivity test method ", it is prepared
Material electromagnetic wave loss in 11.07-26GHz frequency range is less than -10dB.
Comparative example 1
S1: using polyacrylonitrile fibre as carbon fiber material, 300 DEG C is gradually heated to 5 DEG C/min of rate, is carried out
100 minutes pre-oxidation treatments form oxidization fiber, and oxidization fiber is peace and quiet in deionized water, in normal temperature and pressure after 100 DEG C of drying
Lower plasma treatment 30 seconds；
S2: 4.1g ferric sulfate, 7.1g cobaltous sulfate, 3.3g nickel sulfate, 1g glucose are added in 100mL deionized water,
It is equipped to mixed solution；
S3: the oxidization fiber handled by step S1 being put into the mixed solution of step S2 outfit, and three leachings three are rolled,
Dip time is 30min, then pick-up 300% is dried at 100 DEG C；
S4: the oxidization fiber handled by step S3 is obtained under the protection of nitrogen in 650 DEG C of high-temperature process 60min
Carbon fiber；
Such as Fig. 5, synchronous solving (DSC/DTA-TG) STA449F5 thermogravimetric analysis is measured, and the product of embodiment 3 is compared
It is substantially unchanged compared with carbon fiber thermal decomposition temperature；
Such as Fig. 6, it is measured according to GJB2038A-2011 " radar absorbing reflectivity test method ", it is prepared
Material electromagnetic wave loss in 8.7-16GHz frequency range is less than -10dB, absorbs compared with the absorbing material that boron nitride is inner layer covering
Frequency band is narrow.
From the measurement result of embodiment and comparative example as it can be seen that when Wave suction composite material is carbon fiber-boron nitride-magnetic-particle
When three-decker, the high temperature resistance of composite material is on the one hand improved, has on the other hand widened material electro-magnetic wave absorption frequency band,
Has the prospect in high temperature applicationss application.
Finally it is to be appreciated that foregoing description is merely a preferred embodiment of the present invention, those skilled in the art is in the present invention
Enlightenment under, without prejudice to the purpose of the present invention and the claims, multiple similar transformation, such change can be made
It changes and falls within the protection scope of the present invention.
Claims (10)
1. a kind of high-temperature resistance carbon fiber magnetism Wave suction composite material characterized by comprising
Carbon fibre material, the carbon fibre material are polyacrylonitrile-based carbon fibre or viscose base carbon fibre；
It is coated on the boron nitride on the carbon fibre material surface；
With the magnetic-particle by being generated with the carbon fibre material outermost layer in-situ hybridization.
2. the preparation method of high-temperature resistance carbon fiber magnetism Wave suction composite material described in a kind of claim 1, which is characterized in that packet
It includes:
S1: it using polyacrylonitrile fibre or viscose rayon as carbon fiber material, is gradually heated to 3~5 DEG C/min of rate
200~400 DEG C, 50~150 minutes pre-oxidation treatments are carried out, form oxidization fiber, the oxidization fiber is clear in deionized water
Only, plasma treatment is carried out after drying；
S2: boric acid and urea are added in deionized water, the first solution is equipped to；
S3: it will be dried after the oxidization fiber that step S1 is handled is put into first solution and is padded at 60 DEG C~120 DEG C
It is dry；
S4: the oxidization fiber handled by step S3 is subjected to high-temperature process under the protection of nitrogen surface must be arrived to be covered with nitrogen
Change the carbon fiber of boron；
S5: deionized water is added in ferric sulfate, cobaltous sulfate, nickel sulfate, glucose, is equipped to the second solution；
S6: the carbon fiber is put into the second solution, is dried after padding at 60 DEG C~120 DEG C；
S7: high temperature resistant will be prepared after the carbon fiber that step S6 is handled carries out high-temperature process under the protection of nitrogen
Carbon fiber magnetism Wave suction composite material；
Wherein, the carbon fiber is polyacrylonitrile-based carbon fibre or viscose base carbon fibre.
3. preparation method according to claim 2, which is characterized in that drying temperature is 60 DEG C~100 in the step S1
DEG C, plasma processing condition is normal temperature and pressure, and plasma processing time is 10~100 seconds.
4. preparation method according to claim 2, which is characterized in that boric acid, urea and plasma water in the step S2
Mass ratio be (1~5): (1~5): (20~100).
5. preparation method according to claim 2, which is characterized in that ferric sulfate, cobaltous sulfate, sulfuric acid in the step S5
The mass ratio of nickel, glucose and plasma water is (1~5): (1~5): (1~5): (0.1~5): (20~100).
6. preparation method according to claim 2, which is characterized in that described pad is rolled for three leachings three, and dip time is
5min~30min, pick-up are 50%~300%.
7. preparation method according to claim 2, which is characterized in that the temperature of high-temperature process described in step S4 is 300 DEG C
~1000 DEG C, the time of the high-temperature process is 10min~100min.
8. preparation method according to claim 2, which is characterized in that the temperature of high-temperature process described in step S4 is 600 DEG C
~700 DEG C.
9. preparation method according to claim 2, which is characterized in that the temperature of high-temperature process described in step S7 is 300 DEG C
~1000 DEG C, the time of the high-temperature process is 10min~100min.
10. preparation method according to claim 2, which is characterized in that the temperature of high-temperature process described in step S7 is 600 DEG C
~650 DEG C.
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