CN112250345B - FeSiAl sheet-shaped wave-absorbing material and preparation method thereof - Google Patents
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Abstract
The invention discloses a FeSiAl sheet-shaped wave-absorbing material and a preparation method thereof, relates to the technical field of electromagnetic shielding wave-absorbing materials, and solves the technical problems of low magnetic conductivity, weak electromagnetic shielding capability, high price and complex preparation process of the existing electromagnetic shielding wave-absorbing material, wherein the FeSiAl sheet-shaped wave-absorbing material is prepared from the following components in percentage by mass of 10: the FeSiAl wave-absorbing material is prepared from 0.45-0.85 mass percent of Fe9.4-10.0% of Fe, Si and Al, 5.5-6.1% of Si and the balance of Al, and has the advantages of high magnetic conductivity and strong electromagnetic shielding capability.
Description
Technical Field
The invention relates to the technical field of electromagnetic shielding wave-absorbing materials, in particular to a FeSiAl sheet-shaped wave-absorbing material and a preparation method thereof.
Background
The wave-absorbing material is capable of absorbing electromagnetic wave energy projected on the surface of the wave-absorbing material and converting the electromagnetic wave energy into heat energy or other forms of energy through the dielectric loss of the material, and is generally formed by compounding a base material or an adhesive with an absorbing medium, namely an absorbent. The ideal wave-absorbing material should have the characteristics of wide absorption frequency band, light weight, thin thickness, good physical and mechanical properties, simple and convenient use and the like, and the chemical components and the structure of the material should ensure that the wavelength of electromagnetic waves in the material is not changed due to the change of incident frequency.
At present, ferrite wave-absorbing materials, metal micro powder wave-absorbing materials, nano-grade wave-absorbing materials, polycrystalline iron fiber wave-absorbing materials and the like are widely researched and applied, and the wave-absorbing materials are not only widely applied to stealth of military equipment, but also applied to electromagnetic interference resistance.
The Fe-Si-Al alloy powder is a magnetic metal material, is used as a wave-absorbing material, has very wide application, has the characteristics of high magnetic conductivity, high dielectric constant and the like in a low-frequency band (4 GHz) compared with other wave-absorbing materials, has excellent soft magnetic performance, can break through the performance limit of ferrite materials, and is an ideal wave-absorbing agent in a low-frequency band.
At present, the most suitable process for the industrialization of the wave-absorbing powder is a high-energy ball milling method, ball-milled materials can be ground into a sheet structure with a very high radius-thickness ratio through the shearing and extrusion effects of a ball-milling medium, and the magnetic wave-absorbing material with the sheet structure can break through the Snake limitation, improve the magnetic conductivity of the material and improve the electromagnetic shielding effect.
At present, the wave absorbing film is complex in preparation process and high in material cost, so that attention is paid to how to further process the wave absorbing material with the sheet structure into the wave absorbing film.
Disclosure of Invention
The invention aims to: the invention provides a FeSiAl sheet-shaped wave-absorbing material and a preparation method thereof, aiming at solving the problems of low magnetic conductivity, weak electromagnetic shielding capability, high price and complex preparation process of the existing electromagnetic shielding wave-absorbing material.
The invention specifically adopts the following technical scheme for realizing the purpose:
the FeSiAl flaky wave-absorbing material is prepared from the following components in percentage by mass: 0.45-0.85 of FeSiAl wave-absorbing powder and colloid, wherein the mass fractions of Fe, Si and Al in the FeSiAl wave-absorbing powder are Fe9.4-10.0%, Si 5.5-6.1% and the balance of Al.
Further, the FeSiAl flaky wave-absorbing material is prepared from the following components in percentage by mass of 10: 0.65 of FeSiAl wave-absorbing powder and colloid.
Furthermore, the mass fractions of Fe, Si and Al in the FeSiAl wave-absorbing powder are Fe9.7%, Si5.8% and Al84.5%.
Further, the colloid is any one or combination of more of waterborne polyurethane, ethylene propylene diene monomer, polyvinyl alcohol, epoxy resin and PVB.
The invention also aims to provide a preparation method of the FeSiAl sheet-shaped wave-absorbing material, which comprises the following steps:
step one, preparing FeSiAl alloy powder: smelting, centrifugally casting and ball-milling the Fe, Si and Al simple substances with the mass fraction to obtain FeSiAl alloy powder with the particle size of 100-200 mu m;
step two, preparing FeSiAl flake powder: carrying out wet ball milling on the FeSiAl alloy powder obtained in the step one in a high-energy ball mill for 60-120 min to obtain scaly FeSiAl flaky powder with the thickness of 0.5-1.0 mu m;
step three, preparing FeSiAl wave-absorbing powder: drying the FeSiAl flake powder obtained in the step two for 2 to 3 hours at the temperature of 100 to 150 ℃, then heating to 700 to 900 ℃ under the protection of inert gas, preserving heat for 2 hours at the temperature of 700 to 900 ℃, and finally cooling to room temperature to obtain FeSiAl wave-absorbing powder;
step four, preparing the FeSiAl sheet wave-absorbing material: and adding the colloid into the FeSiAl wave-absorbing powder obtained in the third step, stirring and mixing at the rotating speed of 500-700 rpm for 15-20 min, and then carrying out casting film forming, drying and hot pressing to obtain the wave-absorbing film with the thickness of 100-200 mu m, namely the FeSiAl flaky wave-absorbing material.
Further, in the second step, the ball milling speed of the high-energy ball mill is 800-1200 r/min.
Furthermore, in the third step, the heating rate is 3.0 ℃/min to 6.0 ℃/min.
Furthermore, in the third step, the cooling rate is 1.0 ℃/min to 2.0 ℃/min.
Further, in the fourth step, the drying specifically comprises: drying for 110-130 min at 88-92 deg.c.
Further, in the fourth step, the hot pressing specifically comprises: keeping the pressure for 55-65 s at the temperature of 100-150 ℃.
The invention has the following beneficial effects:
the FeSiAl flaky wave-absorbing material sheet adopted by the invention has high dielectric constant and initial permeability, and has a good wave-absorbing effect in a low-frequency band, and the prepared FeSiAl flaky wave-absorbing material sheet is thin, high in permeability at high frequency, strong in electromagnetic shielding capacity, and capable of meeting the performance requirements of electronic products on electromagnetic shielding wave-absorbing materials.
Drawings
FIG. 1 is a schematic diagram of FeSiAl wave-absorbing powder of the present invention.
Detailed Description
To make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings of the embodiments of the present invention,
example 1
FeSiAl sheet-shaped wave-absorbing material
The FeSiAl flaky wave-absorbing material is prepared from the following components in percentage by mass: 0.45 of FeSiAl wave-absorbing powder and colloid, wherein the mass fractions of Fe, Si and Al in the FeSiAl wave-absorbing powder are Fe9.4%, Si6.1% and Al84.5%; wherein the colloid is water-based polyurethane.
The preparation steps are as follows:
step one, preparing FeSiAl alloy powder: smelting, centrifuging, throwing and ball-milling the Fe, Si and Al simple substances with the mass fractions to obtain FeSiAl alloy powder with the particle size of 100 mu m;
step two, preparing FeSiAl flaky powder: wet ball milling the FeSiAl alloy powder obtained in the step one in a high-energy ball mill at the speed of 800 r/min for 120min to obtain 0.5 mu m-thick scaly FeSiAl flaky powder;
step three, preparing FeSiAl wave-absorbing powder: drying the FeSiAl flake powder obtained in the step two at the temperature of 100 ℃ for 3 hours, then heating to 700 ℃ at the speed of 3.0 ℃/min under the protection of inert gas, preserving the heat at the temperature of 700 ℃ for 2 hours, and finally cooling to room temperature at the speed of 1.0 ℃/min to obtain FeSiAl wave-absorbing powder;
step four, preparing the FeSiAl sheet wave-absorbing material: and adding the colloid into the FeSiAl wave-absorbing powder obtained in the third step, stirring and mixing at a rotation speed of 500 revolutions per minute for 20min, casting to form a film, drying at 88 ℃ for 130min, and maintaining the pressure at 100 ℃ for 65s to obtain the wave-absorbing film with the thickness of 100 microns, namely the FeSiAl flaky wave-absorbing material.
Example 2
FeSiAl sheet-shaped wave-absorbing material
The FeSiAl flaky wave-absorbing material is prepared from the following components in percentage by mass: 0.85 percent of FeSiAl wave-absorbing powder and colloid, wherein the mass fractions of Fe, Si and Al in the FeSiAl wave-absorbing powder are Fe10.0 percent, Si5.5 percent and Al84.5 percent; wherein the colloid is ethylene propylene diene monomer.
The preparation steps are as follows:
step one, preparing FeSiAl alloy powder: smelting, centrifuging, throwing and ball-milling the Fe, Si and Al simple substances with the mass fractions to obtain FeSiAl alloy powder with the particle size of 200 mu m;
step two, preparing FeSiAl flaky powder: carrying out wet ball milling on the FeSiAl alloy powder obtained in the step one in a high-energy ball mill at the speed of 1200 r/min for 60min to obtain fish scale-shaped FeSiAl flake powder with the thickness of 1.0 mu m;
step three, preparing FeSiAl wave-absorbing powder: drying the FeSiAl flake powder obtained in the step two at the temperature of 150 ℃ for 2 hours, then heating to 900 ℃ at the speed of 6.0 ℃/min under the protection of inert gas, preserving the heat at 900 ℃ for 2 hours, and finally cooling to room temperature at the speed of 2.0 ℃/min to obtain FeSiAl wave-absorbing powder;
step four, preparing the FeSiAl sheet wave-absorbing material: and adding the colloid into the FeSiAl wave-absorbing powder obtained in the third step, stirring and mixing at a rotation speed of 700 revolutions per minute for 15min, casting to form a film, drying at the temperature of 92 ℃ for 110min, and maintaining the pressure at the temperature of 150 ℃ for 55s to obtain the wave-absorbing film with the thickness of 200 mu m, namely the FeSiAl flaky wave-absorbing material.
Example 3
FeSiAl sheet-shaped wave-absorbing material
The FeSiAl flaky wave-absorbing material is prepared from the following components in percentage by mass: 0.65 of FeSiAl wave-absorbing powder and colloid; the mass fractions of Fe, Si and Al in the FeSiAl wave-absorbing powder are Fe9.7%, Si5.8% and Al84.5%; wherein the colloid is polyvinyl alcohol.
The preparation steps are as follows:
step one, preparing FeSiAl alloy powder: smelting, centrifuging, throwing and ball-milling the Fe, Si and Al simple substances with the mass fractions to obtain FeSiAl alloy powder with the particle size of 150 mu m;
step two, preparing FeSiAl flaky powder: wet ball milling the FeSiAl alloy powder obtained in the step one in a high-energy ball mill at the speed of 1000 r/min for 90min to obtain 0.8 mu m-thick scaly FeSiAl flaky powder;
step three, preparing FeSiAl wave-absorbing powder: drying the FeSiAl flake powder obtained in the step two for 2.5 hours at the temperature of 125 ℃, then heating to 800 ℃ at the speed of 4.5 ℃/min under the protection of inert gas, preserving heat for 2 hours at the temperature of 800 ℃, and finally cooling to room temperature at the speed of 1.5 ℃/min to obtain FeSiAl wave-absorbing powder;
step four, preparing the FeSiAl sheet wave-absorbing material: and adding the colloid into the FeSiAl wave-absorbing powder obtained in the third step, stirring and mixing at a rotation speed of 600 revolutions per minute for 18 minutes, casting to form a film, drying at 90 ℃ for 120 minutes, and maintaining the pressure at 125 ℃ for 60 seconds to obtain the wave-absorbing film with the thickness of 150 microns, namely the FeSiAl flaky wave-absorbing material.
Example 4
FeSiAl sheet-shaped wave-absorbing material
The FeSiAl flaky wave-absorbing material is prepared from the following components in percentage by mass: 0.55 percent of FeSiAl wave-absorbing powder and colloid, wherein the mass fractions of Fe, Si and Al in the FeSiAl wave-absorbing powder are Fe9.5 percent, Si5.7 percent and Al84.8 percent; wherein the colloid is epoxy resin.
The preparation steps are as follows:
step one, preparing FeSiAl alloy powder: smelting, centrifuging, throwing and ball-milling the Fe, Si and Al simple substances with the mass fractions to obtain FeSiAl alloy powder with the particle size of 120 mu m;
step two, preparing FeSiAl flaky powder: carrying out wet ball milling on the FeSiAl alloy powder obtained in the step one in a high-energy ball mill at the speed of 900 revolutions per minute for 80 minutes to obtain fish scale-shaped FeSiAl flake powder with the thickness of 0.6 mu m;
step three, preparing FeSiAl wave-absorbing powder: drying the FeSiAl flake powder obtained in the step two at the temperature of 110 ℃ for 2 hours, heating the powder to the temperature of 750 ℃ at the speed of 4.0 ℃/min under the protection of inert gas, preserving the heat at the temperature of 750 ℃ for 2 hours, and cooling the powder to the room temperature at the speed of 1.2 ℃/min to obtain FeSiAl wave-absorbing powder;
step four, preparing the FeSiAl sheet wave-absorbing material: and adding the colloid into the FeSiAl wave-absorbing powder obtained in the third step, stirring and mixing at a rotation speed of 550 r/min for 16min, casting to form a film, drying at 89 ℃ for 115min, and maintaining the pressure for 58s at 110 ℃ to obtain the 120-micron-thickness wave-absorbing film, namely the FeSiAl flaky wave-absorbing material.
Example 5
FeSiAl sheet-shaped wave-absorbing material
The FeSiAl flaky wave-absorbing material is prepared from the following components in percentage by mass: 0.75 percent of FeSiAl wave-absorbing powder and colloid, wherein the mass fractions of Fe, Si and Al in the FeSiAl wave-absorbing powder are Fe9.8 percent, Si6.0 percent and Al84.2 percent; wherein the colloid is prepared from the following components in percentage by mass: 1 and PVB.
The preparation steps are as follows:
step one, preparing FeSiAl alloy powder: smelting, centrifuging, throwing and ball-milling the Fe, Si and Al simple substances with the mass fractions to obtain FeSiAl alloy powder with the particle size of 180 mu m;
step two, preparing FeSiAl flaky powder: wet ball milling the FeSiAl alloy powder obtained in the step one in a high-energy ball mill at the speed of 1100 r/min for 100min to obtain 0.9 mu m-thick scaly FeSiAl flaky powder;
step three, preparing FeSiAl wave-absorbing powder: drying the FeSiAl flake powder obtained in the step two at 140 ℃ for 3 hours, then heating to 850 ℃ at the rate of 5.0 ℃/min under the protection of inert gas, preserving the heat at 850 ℃ for 2 hours, and finally cooling to room temperature at the rate of 1.8 ℃/min to obtain FeSiAl wave-absorbing powder;
step four, preparing the FeSiAl sheet wave-absorbing material: and adding the colloid into the FeSiAl wave-absorbing powder obtained in the third step, stirring and mixing at a rotation speed of 650 rpm for 19min, casting to form a film, drying at 91 ℃ for 125min, and maintaining the pressure for 62s at 140 ℃ to obtain the wave-absorbing film with the thickness of 180 mu m, namely the FeSiAl flaky wave-absorbing material.
Examples of the experiments
In order to further illustrate the improvement of the FeSiAl sheet-shaped wave-absorbing material prepared in the embodiments 1-5 of the invention, the following tests are performed.
The magnetic conductivity of the FeSiAl sheet-shaped wave absorbing material prepared in the embodiments 1-5 of the invention is detected, referring to GB/T32596-2016 Universal Specification for electromagnetic shielding wave absorbing plate, and the specific measurement results are counted in the following table 1:
table 1 magnetic permeability of thin film sheet die-cut from FeSiAl sheet-like wave absorbing material prepared in embodiments 1 to 5 of the present invention
The results in table 1 show that the FeSiAl sheet-shaped wave-absorbing material prepared in embodiments 1 to 5 of the present invention has high magnetic permeability and strong electromagnetic shielding capability after being die-cut into thin film sheets, and can meet the performance requirements of electronic products on electromagnetic shielding materials.
Claims (9)
1. The FeSiAl flaky wave-absorbing material is characterized by comprising the following components in percentage by mass: 0.45-0.85 of FeSiAl wave-absorbing powder and colloid, wherein the mass fractions of Fe, Si and Al in the FeSiAl wave-absorbing powder are Fe9.4-10.0%, Si 5.5-6.1% and the balance of Al; the preparation method of the FeSiAl sheet-shaped wave-absorbing material comprises the following steps:
step one, preparing FeSiAl alloy powder, namely smelting, centrifugally casting and ball-milling the Fe, Si and Al simple substances with the mass fraction to obtain FeSiAl alloy powder with the particle size of 100-200 mu m;
step two, preparing FeSiAl flake powder, namely performing wet ball milling on the FeSiAl alloy powder obtained in the step one in a high-energy ball mill for 60-120 min to obtain fish scale-shaped FeSiAl flake powder with the thickness of 0.5-1.0 mu m;
step three, preparing FeSiAl wave-absorbing powder, namely drying the FeSiAl flaky powder obtained in the step two for 2 to 3 hours at the temperature of between 100 and 150 ℃, then heating the powder to the temperature of between 700 and 900 ℃ under the protection of inert gas, preserving the heat for 2 hours at the temperature of between 700 and 900 ℃, and finally cooling the powder to the room temperature to obtain the FeSiAl wave-absorbing powder;
and step four, preparing the FeSiAl sheet-shaped wave-absorbing material, namely adding the colloid into the FeSiAl wave-absorbing powder obtained in the step three, stirring and mixing for 15-20 min at the rotating speed of 500-700 r/min, and then carrying out casting film forming, drying and hot pressing to obtain the wave-absorbing film with the thickness of 100-200 mu m, namely the FeSiAl sheet-shaped wave-absorbing material.
2. The FeSiAl sheet-shaped wave-absorbing material as claimed in claim 1, wherein the FeSiAl sheet-shaped wave-absorbing material is prepared from the following components in a mass ratio of 10: 0.65 of FeSiAl wave-absorbing powder and colloid.
3. The FeSiAl sheet-shaped wave-absorbing material as claimed in claim 1, wherein the mass fractions of Fe, Si and Al in the FeSiAl wave-absorbing powder are Fe9.7%, Si 5.8% and Al84.5%.
4. The FeSiAl sheet-shaped wave-absorbing material as claimed in claim 1, wherein the colloid is any one or a combination of more of waterborne polyurethane, ethylene propylene diene monomer, polyvinyl alcohol, epoxy resin and PVB.
5. The FeSiAl sheet-shaped wave-absorbing material as claimed in claim 1, wherein in the second step, the ball-milling speed of the high-energy ball mill is 800-1200 r/min.
6. The FeSiAl sheet-shaped wave-absorbing material as claimed in claim 1, wherein in the third step, the temperature rise rate is 3.0 ℃/min to 6.0 ℃/min.
7. The FeSiAl sheet-shaped wave-absorbing material as claimed in claim 1, wherein in the third step, the cooling rate is 1.0 ℃/min to 2.0 ℃/min.
8. The FeSiAl sheet-shaped wave-absorbing material as claimed in claim 1, wherein in the fourth step, the drying is specifically drying for 110min to 130min at a temperature of 88 ℃ to 92 ℃.
9. The FeSiAl sheet-shaped wave-absorbing material of claim 1, wherein in the fourth step, the hot pressing is carried out for 55-65 s under the condition that the temperature is 100-150 ℃.
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