CN115872763B - Ceramic electromagnetic wave absorbent and preparation method thereof - Google Patents
Ceramic electromagnetic wave absorbent and preparation method thereof Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 30
- 230000002745 absorbent Effects 0.000 title claims abstract description 8
- 239000002250 absorbent Substances 0.000 title claims abstract description 8
- 238000002360 preparation method Methods 0.000 title abstract description 7
- 150000003839 salts Chemical class 0.000 claims abstract description 19
- 239000006096 absorbing agent Substances 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 11
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical group [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 9
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 7
- 239000002184 metal Substances 0.000 claims description 7
- 229910052751 metal Inorganic materials 0.000 claims description 7
- 239000011812 mixed powder Substances 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- 239000012300 argon atmosphere Substances 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 239000004570 mortar (masonry) Substances 0.000 claims description 5
- 239000011780 sodium chloride Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 4
- 238000009837 dry grinding Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 229910021591 Copper(I) chloride Inorganic materials 0.000 claims description 2
- 241001274216 Naso Species 0.000 claims description 2
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 abstract description 29
- 229910010271 silicon carbide Inorganic materials 0.000 abstract description 29
- 238000010521 absorption reaction Methods 0.000 abstract description 23
- 239000011358 absorbing material Substances 0.000 abstract description 12
- 238000000034 method Methods 0.000 abstract description 10
- 239000002131 composite material Substances 0.000 abstract description 8
- 230000015572 biosynthetic process Effects 0.000 abstract description 5
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- 238000003786 synthesis reaction Methods 0.000 abstract description 4
- 238000005253 cladding Methods 0.000 abstract description 3
- 238000011065 in-situ storage Methods 0.000 abstract description 3
- 239000002055 nanoplate Substances 0.000 abstract description 3
- 239000011651 chromium Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 5
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- 238000011049 filling Methods 0.000 description 4
- 239000010936 titanium Substances 0.000 description 4
- 230000001105 regulatory effect Effects 0.000 description 3
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229910003465 moissanite Inorganic materials 0.000 description 2
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- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000012188 paraffin wax Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
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- 229910021389 graphene Inorganic materials 0.000 description 1
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- 239000010955 niobium Substances 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000012429 reaction media Substances 0.000 description 1
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- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
Abstract
The invention relates to a ceramic electromagnetic wave absorbent and a preparation method thereof, which belong to the technical field of composite materials, and are designed to prepare M at a lower temperature by a molten salt method x Si y C z The SiCw ceramic electromagnetic wave absorber enhances the absorption of electromagnetic waves (EMW). In-situ synthesis of M on the surface of silicon carbide whisker (SiCw) at high temperature by molten salt method x Si y C z SiCw, randomly stacked nanoplates to form M with a thickness of about 1-4 μm x Si y C z The layer uniformly coats the SiCw surface. Cladding M x Si y C z After the layer, the complex dielectric constant and EMW absorption capacity of SiCw are obviously improved due to the enhancement of interface polarization and conductivity, the Reflection Loss (RL) is between-10 dB and 25dB, and when the thickness of the MxSiyCz/SiCw ceramic electromagnetic wave absorber is 2-3 mm, the effective absorption bandwidth can cover the whole X wave band. M is M x Si y C z The SiCw has the advantages of light weight, wide bandwidth, strong absorption, thin thickness, adjustable performance and the like, and is a promising high-performance EMW absorbing material.
Description
Technical Field
The invention belongs to the technical field of composite materials, and relates to a ceramic electromagnetic wave absorbent and a preparation method thereof.
Background
Electromagnetic wave absorbing materials have attracted increasing attention due to the increasing severity of electromagnetic radiation and interference with high frequency electronic devices. The electromagnetic wave absorbing material mainly comprises a wave-transparent matrix and an absorbent.
At present, with the continuous improvement of the development requirements of electromagnetic wave absorbing materials, the research of novel high-performance electromagnetic wave absorbing materials is highly focused. SiC is one of the most promising microwave absorbing ceramics because of its high strength, oxidation resistance, high stability and high reliability. Among them, siC whiskers are of great interest because of their low density, good mechanical properties, high temperature resistance and adjustability, and their light weight and high strength. SiC has a single loss mechanism due to factors such as poor impedance matching and low conductivity, and is difficult to achieve an ideal wave absorbing effect.
Conductive phases such as Carbon Nanotubes (CNTs) and graphene are typically added to SiC to increase the conductivity and polarity of SiC materials, and are widely used to improve the conductivity and polarization loss of the materials. Furthermore, coating the surface of SiC whiskers in order to improve electromagnetic wave absorption has proven to be an effective and viable solution for improving the EMW absorption of SiC whiskers.
Ternary layered carbide ceramics MAX phases, e.g. Ti 3 SiC 2 、Ti 4 SiC 3 ，Y 3 Si 2 C 2 、Cr 2 SiC (excellent electrical conductivity, thermal conductivity, machinability, thermal shock resistance, etc.) and ceramic materials (high modulus, high temperature resistance, oxidation resistance, corrosion resistance, etc.) have been widely used for surface modification of SiC and SiC-based composite materials. Related researches show that the MAX phase carbide ceramic can be stably combined with SiC material to be combined on SiC, and the ternary layered ceramic coating not only effectively improves the sintering property of the ceramic, but also improves the mechanical and thermal properties. Thus, the ternary layered carbide ceramic MAX phase can be considered a new and promising coating to improve the electromagnetic wave absorption properties of SiC materials at high temperatures.
Based on the development requirements of wider bandwidth and stronger absorption capacity of electromagnetic wave absorbing materials and adjustable performance, a novel surface coating is needed to be found to improve the electromagnetic wave absorption capacity of the SiC whisker.
The molten salt method is a preparation method which has simple process, low synthesis temperature and capability of synthesizing powder materials with uniform size in batch in a short time, and can accelerate the formation of a coating by using molten salt as a reaction medium, wherein the thickness of the coating is adjusted by adjusting the ratio of reactants, the heat treatment temperature and the heat treatment timeParameters such as the like. Therefore, we have devised a process for preparing M using molten salt method x Si y C z It is necessary to develop an electromagnetic wave absorber for SiCw ceramics to enhance the electromagnetic wave (EMW) absorbing ability of SiC ceramics to meet the requirements of light weight, wide bandwidth, strong absorption, thin thickness and adjustability.
Disclosure of Invention
Technical problem to be solved
In order to avoid the defects of the prior art, the invention provides a ceramic electromagnetic wave absorber and a preparation method thereof.
Technical proposal
A ceramic electromagnetic wave absorbent is characterized in that the molecular general formula is M x Si y C z And SiCw, wherein x, y and z are determined as natural numbers between 1 and 4 according to stoichiometric ratio.
The method of the ceramic electromagnetic wave absorber is characterized by comprising the following steps:
step 1: dispersing SiC whisker in ethanol according to the proportion of 1:50-100, then drying at 60-80 ℃ for 2-6 hours, drying metal powder at 60-80 ℃ for 4-8 hours, and drying mixed fused salt of A and B at 80 ℃ for 4-8 hours;
step 2: mixing the mixed molten salt and the metal powder in a mass ratio of 1-5:2 uniformly in agate mortar by dry grinding to obtain mixed powder;
step 3: uniformly mixing the mixed powder and the SiC whisker, placing the mixture into an alumina crucible, placing the alumina crucible into a tube furnace, introducing argon atmosphere, heating at a heating rate of 2-5 ℃/min, and heating at 1000-1500 ℃ for 1-4 h;
step 4: taking out the material after the furnace temperature is cooled to room temperature, and cleaning the prepared material for a plurality of times by using deionized water; drying at 60-100 deg.c for 12-24 hr to obtain M x Si y C z SiCw ceramic electromagnetic wave absorber.
The purity of the SiC whisker is 99.9%, the diameter D is 0.1-2.5 mu m, and the length is 10-50 mu m.
The metal powder M is one of titanium powder Ti, chromium powder Cr, aluminum powder Al, vanadium powder V, niobium powder Nb or tin powder Sn.
The grain diameter of the metal is 300-500 meshes
The mixed molten salt of A and B is NaCl, KCl, KBr, naF, KNO 3 、CaCl 2 、NaSO 4 、KSO 4 、ZnCl 2 、Cul、CuCl 2 Any two of these.
The ratio of the two mixed fused salts A and B is 1-5:2.
The multiple times of cleaning is 4-10 times.
Advantageous effects
The invention provides a ceramic electromagnetic wave absorbent and a preparation method thereof, belongs to the technical field of composite materials, and designs a method for preparing M at a lower temperature by using a molten salt method x Si y C z The SiCw ceramic electromagnetic wave absorber enhances the absorption of electromagnetic waves (EMW). In-situ synthesis of M on the surface of silicon carbide whisker (SiCw) at high temperature by molten salt method x Si y C z SiCw, randomly stacked nanoplates to form M with a thickness of about 1-4 μm x Si y C z The layer uniformly coats the SiCw surface. Cladding M x Si y C z After the layer, the complex dielectric constant and EMW absorption capacity of SiCw are obviously improved due to the enhancement of interface polarization and conductivity, the Reflection Loss (RL) is between-10 dB and 25dB, and when the thickness of the MxSiyCz/SiCw ceramic electromagnetic wave absorber is 2-3 mm, the effective absorption bandwidth can cover the whole X wave band. M is M x Si y C z The SiCw has the advantages of light weight, wide bandwidth, strong absorption, thin thickness, adjustable performance and the like, and is a promising high-performance EMW absorbing material.
The superiority compared with the prior art can be seen through experimental effect:
in-situ synthesis of M on the surface of silicon carbide whisker (SiCw) at high temperature by molten salt method x Si y C z SiCw, randomly stacked nanoplates to form M with a thickness of about 1-4 μm x Si y C z The layer uniformly coats the SiCw surface. Cladding M x Si y C z After the layer, the complex dielectric constant and the EMW absorption capacity of SiCw are obviously improved due to the enhancement of interface polarization and conductivity. M is M x Si y C z SiCw composite materialWhen M is Y, RLmin with the thickness of only 2.2mm is-22 dB, the effective absorption bandwidth is 2.87GHz, 69% of the X-band (8.2-12.4 GHz) is covered, and by adjusting the thickness of the wave-absorbing material, the effective reflection loss can cover the whole X-band when the thickness is changed from 2.0mm to 3 mm. M is M x Si y C z The SiCw has the advantages of light weight, wide bandwidth, strong absorption, thin thickness, adjustable performance and the like, and is a promising high-performance EMW absorbing material.
Drawings
Fig. 1: when the paraffin filling content is 50%, the wave absorbing performance corresponding to different thicknesses is achieved;
fig. 2: an effect of increasing the real part of the dielectric constant;
fig. 3: the imaginary part of the dielectric constant increases the effect.
Detailed Description
The invention will now be further described with reference to examples, figures:
example 1:
2g of SiCw was stirred in 200ml for 30 minutes to disperse, and then 2g of NaCl, 2g of KCl salt and 1g of yttrium powder (Y) were dry-milled and mixed uniformly in agate mortar. Subsequently, the mixed powder and 2g of SiC whiskers were uniformly mixed and placed in an alumina crucible, and heated in a tube furnace at a heating rate of 5 ℃/min under an argon atmosphere at 1100℃for 2 hours. After the oven temperature was cooled to room temperature, the prepared samples were rinsed with deionized water multiple times to remove residual salts. Drying at 100deg.C for 24 hr to obtain Y 3 Si 2 C 2 Compared with pure SiCw, the novel SiCw ceramic electromagnetic wave absorber has effectively improved real part and imaginary part of dielectric constant. When the paraffin-like filling content is 50%, the wave absorbing performance corresponding to different thicknesses is shown as figure 1, siCw/Y 3 Si 2 C 2 The RLmin of the composite material is-22 dB when the thickness is only 2.1mm, the effective absorption bandwidth is 2.87GHz when the thickness is 2.2mm, 68% of the effective absorption bandwidth is covered in an X wave band (8.2-12.4 GHz), and the effective reflection loss can cover the whole X wave band when the thickness is adjusted from 2.0mm to 2.7mm by regulating the thickness of the wave absorbing material. The dielectric constant real and imaginary part lifting effect is shown in fig. 2, fig. 3.
Example 2:
4g of SiCw was stirred in 400ml for 60 minutes to disperse, and then 4g of NaCl, 4g of KCl salt and 2g of chromium powder (Cr) were mixed uniformly in agate mortar by dry grinding. Subsequently, the mixed powder and 4g of SiC whiskers were uniformly mixed and placed in an alumina crucible, and heated in a tube furnace at a heating rate of 5 ℃/min under an argon atmosphere at 1200 ℃ for 2 hours. After the oven temperature was cooled to room temperature, the prepared samples were rinsed with deionized water multiple times to remove residual salts. Drying at 80deg.C for 18 hr to obtain Cr 2 Compared with pure SiCw, the novel ceramic electromagnetic wave absorber of SiC/SiCw has effectively improved real part and imaginary part of dielectric constant. When the paraffin-like filling content is 50%, siCw/Cr 2 The RLmin of the SiC composite material is-16.9 dB when the thickness is only 2.0mm, the effective absorption bandwidth is 2.27GHz when the thickness is 2.2mm, 50% of the effective absorption bandwidth is covered in an X-band (8.2-12.4 GHz), and the effective reflection loss can cover the whole X-band when the thickness is adjusted from 2.0mm to 2.7mm by regulating the thickness of the wave-absorbing material.
Example 3:
6g of SiCw is taken and stirred in 600ml for 60 minutes for dispersion, and then 10g of NaCl, 10g of KCl salt and 3g of titanium powder (Ti) are evenly mixed in agate mortar by dry grinding. Subsequently, the mixed powder and 6g of SiC whiskers were uniformly mixed and placed in an alumina crucible, and heated in a tube furnace at a heating rate of 5 ℃/min under an argon atmosphere at 1300℃for 2.5 hours. After the oven temperature was cooled to room temperature, the prepared samples were rinsed with deionized water multiple times to remove residual salts. Drying at 100deg.C for 15 hr to obtain SiCw/Cr 2 SiC novel ceramic electromagnetic wave absorber, ti when paraffin wax like filling content is 50% 3 SiC 2 The RLmin of the SiCw composite material is-15.9 dB when the thickness is only 2.0mm, the effective absorption bandwidth is 2.39GHz, 51% of the effective absorption bandwidth is covered in an X wave band (8.2-12.4 GHz), and the effective reflection loss can cover the whole X wave band when the thickness is adjusted from 2.0mm to 2.8mm by regulating the thickness of the wave-absorbing material.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications, adaptations and alternatives may be made by one of ordinary skill in the art without departing from the principles of the present invention, and are intended to be considered as limiting the scope of the present invention.
Claims (5)
1. A ceramic electromagnetic wave absorbent is characterized in that the molecular general formula is M x Si y C z SiCw, wherein x, y and z are determined as natural numbers between 1 and 4 according to stoichiometric ratio;
wherein M is one of Ti, cr, al, V, nb, sn;
the ceramic electromagnetic wave absorber is prepared according to the following steps:
step 1: dispersing SiC whiskers in ethanol according to a ratio of 1:50-100, then drying at 60-80 ℃ for 2-6 hours, drying metal powder M at 60-80 ℃ for 4-8 hours, and drying mixed fused salt of A and B at 80 ℃ for 4-8 hours;
the mixed molten salt of A and B is NaCl, KCl, KBr, naF, KNO 3 、CaCl 2 、NaSO 4 、KSO 4 、ZnCl 2 、Cul、CuCl 2 Any two of these;
step 2: mixing the mixed molten salt and the metal powder M in a mass ratio of 1-5:2 uniformly in agate mortar by dry grinding to obtain mixed powder;
step 3: uniformly mixing the mixed powder and the SiC whisker, placing the mixture into an alumina crucible, placing the alumina crucible into a tube furnace, introducing argon atmosphere, heating at a heating rate of 2-5 ℃/min, and heating at 1000-1500 ℃ for 1-4 h;
step 4: taking out the material after the furnace temperature is cooled to room temperature, and cleaning the prepared material for a plurality of times by using deionized water; drying at 60-100 ℃ for 12-24 h to obtain M x Si y C z SiCw ceramic electromagnetic wave absorber.
2. The ceramic electromagnetic wave absorber according to claim 1, wherein: the purity of the SiC whisker is 99.9%, the diameter D is 0.1-2.5 mu m, and the length is 10-50 mu m.
3. The ceramic electromagnetic wave absorber according to claim 1, wherein: the particle size of the metal powder M is 300-500 meshes.
4. The ceramic electromagnetic wave absorber according to claim 1, wherein: the ratio of the two mixed fused salts A and B is 1-4:1.
5. The ceramic electromagnetic wave absorber according to claim 1, wherein: the multiple times of cleaning are 4-10 times.
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| EP2217865A4 (en) * | 2007-10-18 | 2014-03-05 | Alliance Sustainable Energy | High temperature solar selective coatings |
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| CN101232799A (en) * | 2008-03-05 | 2008-07-30 | 湖南大学 | Multiband electromagnetic wave absorb composite material and preparing method thereof |
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