CN108822797A - A kind of titanium silicon-carbon composite wave-absorbing agent and the preparation method and application thereof - Google Patents
A kind of titanium silicon-carbon composite wave-absorbing agent and the preparation method and application thereof Download PDFInfo
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- CN108822797A CN108822797A CN201810748081.1A CN201810748081A CN108822797A CN 108822797 A CN108822797 A CN 108822797A CN 201810748081 A CN201810748081 A CN 201810748081A CN 108822797 A CN108822797 A CN 108822797A
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- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
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- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/32—Radiation-absorbing paints
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- H—ELECTRICITY
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- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
Abstract
The invention discloses a kind of titanium silicon-carbon composite wave-absorbing agent, by Ti3SiC2Base core and Ni0.5Zn0.5Fe2O4Ferrite magnetic nano clad composition, the Ni0.5Zn0.5Fe2O4Ferrite and Ti3SiC2Mass ratio be 1:(3~6).Ti of the present invention3SiC2Composite wave-absorbing agent, Ni0.5Zn0.5Fe2O4The adjustable Ti of ferrite clad3SiC2Electromagnetic property improves composite wave-absorbing agent impedance matching performance;Meanwhile when Electromagnetic Field is in Ni0.5Zn0.5Fe2O4When ferrite clad, dielectric loss and magnetic loss will be generated, further enhance composite absorber absorbing property;Ti of the present invention3SiC2The preparation method of composite wave-absorbing agent, process conditions are easily-controllable, easy to operate, and production cost is low;The present invention utilizes Ti3SiC2The Ti that composite wave-absorbing agent is prepared3SiC2Composite wave-suction material has wideband, low-density, the strong characteristic for inhaling wave, and the surface density of composite wave-suction material is in 1.5kg/m2Within, absorption band is wide, and reflectance test is the result shows that the bandwidth better than -10dB (90% absorbs) is greater than 9.0GHz.
Description
Technical field
The invention belongs to functional material preparation technical fields, and in particular to a kind of titanium silicon-carbon composite wave-absorbing agent and its preparation side
Method and application.
Background technique
A large amount of uses of high-frequency electromagnetic equipment bring the electromagnetic pollution problem got worse;Meanwhile the radar exploration technique
It rapidly develops, constitutes a serious threat to military target.Absorbing material, can be by incoming electromagnetic wave energy by filling powder wave absorbing agent
It is converted into the energy of thermal energy or other forms and makes electromagnetic wave loss decaying, reaching improves periphery electromagnetic environment and the army of being effectively reduced
The radar detection characteristic signal purpose of thing target has very important technology and economical and practical value.In recent years, it grinds both at home and abroad
The wave absorbing agent material studied carefully mainly includes magnetic metal and its alloy, conductive carbon material, conduction high polymer, ferrite etc..They are
It can be absorbed by dielectric loss, ohmic loss or magnetic loss and electromagnetic wave energy of decaying.Titanium silicon-carbon (Ti3SiC2) material has
Certain electric conductivity, high-specific surface area and high-temperature oxidation resistance, can occur dielectric loss and ohmic loss when electromagnetic wave passes through,
Absorbing material field has very big application potential, but single Ti3SiC2The electromagnetic impedance match of material is poor, causes to electromagnetism
The absorption band of wave is relatively narrow.
Summary of the invention
The Ti that the purpose of the present invention is to provide a kind of electromagnetic impedance match is good, absorption band is wide3SiC2Composite wave-absorbing agent
And the preparation method and application thereof.
This Ti provided by the invention3SiC2Composite wave-absorbing agent, by Ti3SiC2Base core and Ni0.5Zn0.5Fe2O4Ferrite magnetic
Property nanometer clad composition, the Ni0.5Zn0.5Fe2O4Ferrite and Ti3SiC2Mass ratio be 1:(3~6).
The present invention provides the Ti3SiC2The preparation method of composite wave-absorbing agent, includes the following steps:
(1) it is prepared by predetermined ratio and contains Ni2+、Zn2+And Fe3+Mixed nitrate solution, be added complexing agent, adjust PH to 7
~9, it is uniformly mixing to obtain mixed solution;
(2) by Ti3SiC2Powder is scattered in mixed solution obtained by step (1) by design proportion, is carried out at a predetermined temperature
Stirring, obtains the composite precursor sol of stable and uniform;
(3) composite precursor sol obtained by step (2) is dried, pre-burning, grinding, then is sintered, obtained
Ti3SiC2Composite wave-absorbing agent.
Preferably, in the step (1), Ni in mixed nitrate solution2+、Zn2+、Fe3+Concentration is 0.1~0.3mol/L,
The Ni2+、Zn2+、Fe3+Molar concentration rate is 1:1:4.
Preferably, in the step (1), complexing agent is that ethylenediamine tetra-acetic acid, citric acid or molar ratio are 3:1~4:1
Ethylenediamine tetra-acetic acid and citric acid mixture;The mole of complexing agent is 1.2~1.5 of cationic integral molar quantity in mixed solution
Times.
Preferably, in the step (1), by be added ammonium hydroxide adjust PH, the ammonium hydroxide mass percent concentration be 20~
40%.
Preferably, in the step (2), the Ti3SiC2Powder is prepared by solid phase reaction, is crushed to 200 meshes
Net.
Preferably, in the step (2), whipping temp is 70~90 DEG C, and mixing time is 4~6h.
Preferably, in the step (3), drying temperature is 100~130 DEG C;Calcined temperature is 200~400 DEG C, when pre-burning
Between be 2~4h;Sintering temperature is 500~700 DEG C, and sintering time is 2~3h.
The present invention also provides the Ti3SiC2The application of composite wave-absorbing agent, by Ti3SiC2Composite wave-absorbing agent is used to prepare
Ti3SiC2Composite wave-suction material, the Ti3SiC2Composite wave-suction material includes by weight percentage:Ti3SiC2Composite wave-absorbing agent 50
~70%, epoxy resin 24~40%, epoxy hardener 6~10%.
Preferably, the Ti3SiC2The preparation process of composite wave-suction material is:Under mechanical agitation, by Ti3SiC2
Composite wave-absorbing agent than is uniformly mixed with epoxy resin by design weight;The epoxy hardener of predetermined ratio is added, continues to stir ripe
Change 0.5~1.0h, adds nonessential organic solvent and adjust viscosity and nonessential auxiliary agent adjusting dispersibility and levelability, by mixture
Coated on aluminium sheet, toast after cooling down to obtain the final product.
Preferably, the mechanical stirring disperses integration apparatus using vertical mixing, and revolving speed is 1000~1500r/min.
Preferably, the epoxy resin is bisphenol A epoxide resin, cycloaliphatic epoxy resin, one in bisphenol F epoxy resin
Kind is a variety of;The epoxy hardener is poly- phthalein amine curing agent, in low molecule amine curing agent, cashew nut oil modified curing agent
It is one or more.
Preferably, the nonessential organic solvent is one of benzene class, alcohols, ketone or a variety of;It is described nonessential to help
Agent is one of coalescing agent, levelling agent, defoaming agent, dispersing agent, promotor or a variety of.
Preferably, the surface of the aluminium sheet reaches Sa2.5 grades through sandblasting or mechanical grinding processing.
Preferably, the baking temperature be 40~50 DEG C, baking time be 1.0~2.0h, cooling time be 0.5~
1.0h。
Ti3SiC2Powder is a kind of typical MAX phase ceramic-metal composite, the double grading with metal and ceramics,
Ti3SiC2Conductivity up to 4.5 × 106S/m has the excellent characteristics such as high temperature oxidation resistance, low-density and high mechanical strength, assigns
Give Ti3SiC2Material becomes the huge advantage of electromagnet wave absorbent.By in Ti3SiC2Material surface cladding
Ni0.5Zn0.5Fe2O4Ferrite magnetic nano layer, adjustable Ti3SiC2Electromagnetic property, improve composite wave-absorbing agent impedance
With performance;Meanwhile when Electromagnetic Field is in Ni0.5Zn0.5Fe2O4When ferrite magnetic nano clad, stronger magnetic loss will be also generated
Consumption and dielectric loss further enhance Ti by introducing magnetic loss3SiC2The absorbing property of composite absorber.
Compared with prior art, advantageous effects of the invention:
(1) Ti of the present invention3SiC2Composite wave-absorbing agent, with the Ti with certain conductivity3SiC2It, will for basic raw material
Ni0.5Zn0.5Fe2O4Ferrimagnetism layer is coated on Ti3SiC2Surface forms unique core-shell structure, hinders with excellent electromagnetism
Anti- matching properties possess magnetic loss caused by significant dielectric polarization and magnetization effect, Ti3SiC2Composite wave-absorbing agent, which has, to be absorbed
The advantages of bandwidth, density is low and resistance to high temperature oxidation.
(2) Ti of the present invention3SiC2Composite wave-absorbing agent preparation method, process conditions are easily-controllable, easy to operate, technique at
This is low, is conducive to industrialized production.
(3) Ti of the present invention3SiC2The application of composite wave-absorbing agent, the Ti being prepared3SiC2Composite wave-suction material has
Wideband, areal density and the strong characteristic for inhaling wave, the surface density of composite wave-suction material is in 1.5kg/m2Within, absorption band is wide,
The reflectivity of test is greater than 9.0GHz better than the bandwidth of -10dB (90% absorbs).
Detailed description of the invention
Fig. 1 uses Ti by the embodiment of the present invention 13SiC2The scanning electron microscope (SEM) photograph of powder.
Fig. 2 is 1 gained Ti of the embodiment of the present invention3SiC2The scanning electron microscope (SEM) photograph of composite wave-absorbing agent.
Fig. 3 is 4~6 gained Ti of the embodiment of the present invention3SiC2Absorbing property of the composite wave-suction material in 8~18GHz frequency range
Figure.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, rather than whole embodiments, based on the embodiments of the present invention, the common skill in this field
Art personnel every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses, present invention will be further explained below with reference to the attached drawings and specific examples.
Embodiment 1
The present invention provides a kind of Ti3SiC2The preparation method of composite wave-absorbing agent, includes the following steps:
(1) 7.3g Ni (NO is weighed respectively3)2·6H2O、7.5g Zn(NO3)2·6H2O and 40.4gFe (NO3)·9H2O,
And it is dissolved in the beaker equipped with 500mL deionized water and mixed nitrate solution is made;37.8g complexing agent lemon is then added
Acid is slow added into the ammonia spirit that concentration is 40%, adjusts PH to 7, and uniform stirring forms mixed solution;
(2) by 35.7g Ti3SiC2Powder is scattered in mixed solution, is placed under 80 DEG C of water bath devices and is carried out heating stirring
5h obtains the composite precursor sol of stable and uniform;
(3) composite precursor sol obtained is placed on to drying in 120 DEG C of drying box, is formed after moisture evaporation
Gel is coated on Ti3SiC2After powder surface, pre-burning 3h, is ground later at 400 DEG C, is placed in chamber type electric resistance furnace 600 DEG C
Lower sintering 2h, obtains Ti3SiC2Composite wave-absorbing agent.
Ti used in the present embodiment3SiC2The scanning electron microscope pattern photo of powder granule is as shown in Figure 1, it is seen that Ti3SiC2
Particle base karyomorphism looks are sheet;Ti3SiC2The scanning electron microscope pattern photo of composite wave-absorbing agent is as shown in Figure 2, it is seen that
Ni0.5Zn0.5Fe2O4Ferrite nano magnetosphere is evenly coated at Ti3SiC2Powder surface.
Embodiment 2
The present invention provides a kind of Ti3SiC2The preparation method of composite wave-absorbing agent, includes the following steps:
(1) 10.9g Ni (NO is weighed respectively3)2·6H2O、11.2g Zn(NO3)2·6H2O and 60.6gFe (NO3)·
9H2O, and be dissolved in the beaker equipped with 500mL deionized water and mixed nitrate solution is made;98.5g complexing is then added
Agent ethylenediamine tetra-acetic acid is slow added into the ammonia spirit that concentration is 30%, adjusts PH to 8, and uniform stirring forms mixed solution;
(2) by 71.4g Ti3SiC2Powder is scattered in mixed solution, is placed under 90 DEG C of water bath devices and is carried out heating stirring
4h obtains the composite precursor sol of stable and uniform;
(3) composite precursor sol obtained is placed on to drying in 130 DEG C of drying box, is formed after moisture evaporation
Gel is coated on Ti3SiC2After powder surface, pre-burning 4h, is ground later at 300 DEG C, is placed in chamber type electric resistance furnace 700 DEG C
Lower sintering 2h, obtains Ti3SiC2Composite wave-absorbing agent.
Embodiment 3
The present invention provides a kind of Ti3SiC2The preparation method of composite wave-absorbing agent, includes the following steps:
(1) 7.3g Ni (NO is weighed respectively3)2·6H2O、7.5g Zn(NO3)2·6H2O and 40.4gFe (NO3)·9H2O,
And it is dissolved in the beaker equipped with 500mL deionized water and mixed nitrate solution is made;Then be added 15.9g citric acid and
43.8g ethylenediamine tetra-acetic acid mixing complexing agent is slow added into the ammonia spirit that concentration is 40%, adjusts PH to 7, uniform stirring
Form mixed solution;
(2) by 59.5g Ti3SiC2Powder is scattered in mixed solution, is placed under 80 DEG C of water bath devices and is carried out heating stirring
4h obtains the composite precursor sol of stable and uniform;
(3) composite precursor sol obtained is placed on to drying in 130 DEG C of drying box, is formed after moisture evaporation
Gel is coated on Ti3SiC2After powder surface, pre-burning 3h, is ground later at 400 DEG C, is placed in chamber type electric resistance furnace 500 DEG C
Lower sintering 2h, obtains Ti3SiC2Composite wave-absorbing agent.
Embodiment 4
By 1 gained Ti of embodiment3SiC2Composite wave-absorbing agent is used to prepare Ti3SiC2Composite wave-suction material, preparation process are:
Integration apparatus is dispersed using vertical mixing, by 50.0gTi3SiC2Composite wave-absorbing agent, 40.0g bisphenol A epoxide resin are in 1000r/
1.0h is dispersed with stirring under the conditions of min;10.0g low molecule amine curing agent is added, continues stirring curing 0.5h, adds 7.0g diformazan
Benzene solvent and 0.2g coalescing agent, and mixture is coated on 180mm ╳ 180mm aluminium sheet using spraying process, 50 DEG C of bakings
After 1.0h, cooling 0.5h to get.Ti obtained by the present embodiment3SiC2The performance parameter of composite wave-suction material is as shown in the table:
Embodiment 5
By 2 gained Ti of embodiment3SiC2Composite wave-absorbing agent is used to prepare Ti3SiC2Composite wave-suction material, preparation process are:
Integration apparatus is dispersed using vertical mixing, by 75.0gTi3SiC2Composite wave-absorbing agent, 40.0g cycloaliphatic epoxy resin exist
1.0h is dispersed with stirring under the conditions of 1500r/min;The poly- phthalein amine hardener of 10.0g is added, continues stirring curing 0.5h, addition 7.0g is just
Butanol solvent and 0.1g levelling agent, and mixture is coated on 180mm ╳ 180mm aluminium sheet using spraying process, 40 DEG C of bakings
After 1.5h, cooling 0.5h to get.Ti obtained by the present embodiment3SiC2The performance parameter of composite wave-suction material is as shown in the table:
Embodiment 6
By 3 gained Ti of embodiment3SiC2Composite wave-absorbing agent is used to prepare Ti3SiC2Composite wave-suction material, preparation process are:
Integration apparatus is dispersed using vertical mixing, by 110.0gTi3SiC2Composite wave-absorbing agent, 40.0g bisphenol F epoxy resin exist
0.5h is stirred under the conditions of 2000r/min;10.0g low molecule amine hardener is added, continues stirring curing 0.5h, adds 8.0g diformazan
Benzene and n-butanol solvent, and mixture is coated on 180mm ╳ 180mm aluminium sheet using roll coating process, after 50 DEG C of baking 1.5h,
Cooling 1.0h to get.Ti obtained by the present embodiment3SiC2The performance parameter of composite wave-suction material is as shown in the table:
Comparative example 1
Integration apparatus is dispersed using vertical mixing, 50.0g flaky carbonyl iron powder, 40.0g bisphenol A epoxide resin are existed
1.0h is dispersed with stirring under the conditions of 1000r/min;10.0g low molecule amine curing agent is added, continues stirring curing 0.5h, addition
7.0g xylene solvent, and mixture is coated on 180mm ╳ 180mm aluminium sheet using spraying process, after 50 DEG C of baking 1.5h,
Cooling 0.5h to get.The performance parameter of composite wave-suction material obtained by this comparative example is as shown in the table:
Comparative example 2
Integration apparatus is dispersed using vertical mixing, 50.0g sheet iron aluminum silicon powder, 40.0g bisphenol A epoxide resin are existed
1.0h is dispersed with stirring under the conditions of 1000r/min;10g low molecule amine curing agent is added, continues stirring curing 0.5h, adds 7.0g
Xylene solvent, and mixture is coated on 180mm ╳ 180mm aluminium sheet using spraying process, it is cooling after 50 DEG C of baking 1.5h
0.5h to get.The performance parameter of composite wave-suction material obtained by this comparative example is as shown in the table:
Fig. 3 is 4~6 gained Ti of embodiment3SiC2Composite wave-suction material and 1~2 absorbing material of comparative example are in 8~18GHz frequency
The absorbing property figure of section, from figure 3, it can be seen that compared to absorbing material in comparative example 1~2, the resulting Ti of the present invention3SiC2It is multiple
Closing absorbing material has lower surface density (≤1.5kg/m2) and broader effective suction wavestrip it is wide (>=9.0GHz).
The above is only a preferred embodiment of the present invention, protection scope of the present invention is not limited merely to above-mentioned implementation
Example.To those of ordinary skill in the art, obtained improvement and change in the case where not departing from the technology of the present invention concept thereof
It changes and also should be regarded as protection scope of the present invention.
Claims (10)
1. a kind of titanium silicon-carbon composite wave-absorbing agent, which is characterized in that by Ti3SiC2Base core and Ni0.5Zn0.5Fe2O4Ferrimagnetism is received
Rice clad composition, the Ni0.5Zn0.5Fe2O4Ferrite and Ti3SiC2Mass ratio be 1:(3~6).
2. a kind of preparation method of titanium silicon-carbon composite wave-absorbing agent according to claim 1, which is characterized in that including following step
Suddenly:
(1) it is prepared by predetermined ratio and contains Ni2+、Zn2+And Fe3+Mixed nitrate solution, be added complexing agent, adjust PH to 7~9,
It is uniformly mixing to obtain mixed solution;
(2) by Ti3SiC2Powder is scattered in mixed solution obtained by step (1) by design proportion, is stirred at a predetermined temperature
It mixes, obtains the composite precursor sol of stable and uniform;
(3) composite precursor sol obtained by step (2) is dried, pre-burning, grinding, then is sintered, obtained
Ti3SiC2Composite wave-absorbing agent.
3. the preparation method of titanium silicon-carbon composite wave-absorbing agent according to claim 2, which is characterized in that in the step (1), mix
Close Ni in nitrate solution2+、Zn2+、Fe3+Concentration is 0.1~0.3mol/L, the Ni2+、Zn2+、Fe3+Molar concentration rate is 1:
1:4.
4. the preparation method of titanium silicon-carbon composite wave-absorbing agent according to claim 2, which is characterized in that in the step (1), network
Mixture is that ethylenediamine tetra-acetic acid, citric acid or molar ratio are 3:1~4:1 ethylenediamine tetra-acetic acid and citric acid mixture;Complexing
The mole of agent is 1.2~1.5 times of cationic integral molar quantity in mixed solution.
5. the preparation method of titanium silicon-carbon composite wave-absorbing agent according to claim 2, which is characterized in that in the step (2), stir
Mixing temperature is 70~90 DEG C, and mixing time is 4~6h.
6. the preparation method of titanium silicon-carbon composite wave-absorbing agent according to claim 2, which is characterized in that in the step (3), dry
Dry temperature is 100~130 DEG C;Calcined temperature is 200~400 DEG C, and burn-in time is 2~4h;Sintering temperature is 500~700 DEG C,
Sintering time is 2~3h.
7. a kind of application for requiring the 1 titanium silicon-carbon composite wave-absorbing agent according to power, which is characterized in that by Ti3SiC2Composite wave-absorbing agent
It is used to prepare Ti3SiC2Composite wave-suction material, the Ti3SiC2Composite wave-suction material includes by weight percentage:Ti3SiC2It is compound
Wave absorbing agent 50~70%, epoxy resin 24~40%, epoxy hardener 6~10%.
8. a kind of application for requiring the 7 titanium silicon-carbon composite wave-absorbing agent according to power, which is characterized in that the Ti3SiC2Composite wave-absorbing
The preparation process of material is:Under mechanical agitation, by Ti3SiC2Composite wave-absorbing agent and epoxy resin are equal by design weight ratio
Even mixing;The epoxy hardener of predetermined ratio is added, continues stirring 0.5~1.0h of curing, adds nonessential organic solvent and adjust
Viscosity and nonessential auxiliary agent adjust dispersibility and levelability, and mixture is coated on aluminium sheet, after baking is cooling to obtain the final product.
9. a kind of application for requiring the 8 titanium silicon-carbon composite wave-absorbing agent according to power, which is characterized in that the epoxy resin is bis-phenol
One of A epoxy resin, cycloaliphatic epoxy resin, bisphenol F epoxy resin are a variety of;The epoxy hardener is poly- phthalein amine
One of curing agent, low molecule amine curing agent, cashew nut oil modified curing agent are a variety of.
10. a kind of application for requiring the 8 titanium silicon-carbon composite wave-absorbing agent according to power, which is characterized in that described nonessential organic molten
Agent is one of benzene class, alcohols, ketone or a variety of;The nonessential auxiliary agent is coalescing agent, levelling agent, defoaming agent, dispersion
One of agent, promotor are a variety of.
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CN111153446A (en) * | 2020-02-14 | 2020-05-15 | 中南大学湘雅三医院 | Ferrite composite wave absorbing agent and preparation method and application thereof |
CN114656661A (en) * | 2022-02-22 | 2022-06-24 | 奇遇新材料科技(佛山)有限公司 | Iron-based wave absorbing film and preparation method thereof |
CN114656661B (en) * | 2022-02-22 | 2024-03-22 | 奇遇新材料科技(佛山)有限公司 | Iron-based wave absorbing film and preparation method thereof |
CN114656827A (en) * | 2022-03-22 | 2022-06-24 | 河北志盛威华特种涂料有限公司 | Wave-absorbing powder and preparation method thereof |
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