CN116156858A - Directional-arrangement zinc oxide coated sheet-shaped iron-silicon-chromium wave-absorbing material and preparation method thereof - Google Patents

Directional-arrangement zinc oxide coated sheet-shaped iron-silicon-chromium wave-absorbing material and preparation method thereof Download PDF

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CN116156858A
CN116156858A CN202211528723.XA CN202211528723A CN116156858A CN 116156858 A CN116156858 A CN 116156858A CN 202211528723 A CN202211528723 A CN 202211528723A CN 116156858 A CN116156858 A CN 116156858A
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王涛
吴彬
商荣翔
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Beijing Seven Star Flight Electronic Co ltd
Lanzhou University
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Lanzhou University
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Abstract

The invention relates to a directional arranged zinc oxide coated sheet iron silicon chromium wave-absorbing material and a preparation method thereof, belonging to the technical field of magnetic wave-absorbing materials. The preparation method comprises the steps of performing dispersion blending ball milling on the iron-silicon-chromium alloy soft magnetic powder and the zinc oxide nano particles, and coating the iron-silicon-chromium alloy soft magnetic powder and the zinc oxide nano particles by using organic resin to obtain zinc oxide coated flaky iron-silicon-chromium soft magnetic particles, so that the magnetic conductivity and impedance matching performance of the magnetic powder in the GHz frequency band are optimized; the flaky particles in the material are arranged in an oriented way through the magnetic field orientation, so that the efficient wave absorbing performance can be obtained at 1-4 GHz. The result shows that the oriented zinc oxide coated sheet iron silicon chromium wave-absorbing material can obtain excellent wave-absorbing performance under the microwave frequency band of 1-4GHz under the ultra-thin thickness of 1-3 mm, and is suitable for large-scale application as a low-frequency wave-absorbing material.

Description

Directional-arrangement zinc oxide coated sheet-shaped iron-silicon-chromium wave-absorbing material and preparation method thereof
Technical Field
The invention relates to a directional arranged zinc oxide coated sheet iron silicon chromium wave absorbing material and a preparation method thereof, belonging to the technical field of electromagnetic wave absorbing materials.
Background
The electromagnetic wave absorption technology has important application in the fields of electromagnetic interference resistance and national defense stealth of civil high-frequency devices. With the development of 5G communication technology and radar detection technology, the fields of microwave communication products, base stations, electronic countermeasure and the like put forward new requirements on the absorption frequency band of the wave-absorbing material, and the traditional microwave high frequency band (8-18 GHz) is expanded to the microwave low frequency band (1-4 GHz), so that the severe test on the low-frequency electromagnetic wave absorption performance of the wave-absorbing material is put forward. At present, the wave-absorbing material developed for the low frequency band has the defects of too large thickness, poor wave-absorbing performance and the like, and has a larger gap with the actual application requirement of the low frequency stealth material. Therefore, the development of the high-performance low-frequency wave-absorbing material is a key for breaking through the technical bottleneck of stealth materials.
The common wave-absorbing material is composed of magnetic metal micro powder, and the magnetic powder-binder compound is required to keep high complex permeability and excellent impedance matching performance at the working frequency of 1-4 GHz. In the previous research of the applicant (Chinese patent application No. 200910140535.8, named as a magnetic field oriented sheet-shaped soft magnetic composite material and a preparation method thereof), the preparation method of the magnetic field oriented sheet-shaped soft magnetic composite material effectively improves the magnetic permeability of the composite material, but the magnetic powder-binder composite has higher dielectric constant and poor matching performance due to the enhanced interfacial polarization of the sheet-shaped magnetic metal micropowder, which limits the wave absorbing performance at low frequency.
Disclosure of Invention
First, the technical problem to be solved
In order to solve the problems in the prior art, the invention provides the oriented zinc oxide coated sheet-shaped iron silicon chromium wave-absorbing material and the preparation method thereof, which have excellent wave-absorbing performance in a microwave frequency range of 1-4GHz, improve magnetic permeability, effectively optimize impedance matching performance and greatly improve low-frequency wave-absorbing performance of the material.
(II) technical scheme
In order to achieve the above purpose, the main technical scheme adopted by the invention comprises the following steps:
a preparation method of a directional arranged zinc oxide coated sheet iron silicon chromium wave-absorbing material comprises the following steps:
s1: the mass percentage of Fe is as follows 90 Si 7 Cr 3 The metal soft magnetic powder of (2) is annealed in inert atmosphere;
s2: fe treated in step S1 90 Si 7 Cr 3 Ball milling the powder and ZnO powder, and taking absolute ethyl alcohol as a ball milling medium to obtain flaky Fe 90 Si 7 Cr 3 A @ ZnO powder;
s3: ball milling the obtained flaky Fe 90 Si 7 Cr 3 Uniformly dissolving the @ ZnO powder and polyurethane in an acetone solution, and performing magnetic field rotation orientation when the solvent volatilizes to be in a viscous mixture state; and then carrying out high-temperature hot pressing on the dried composite product to obtain the oriented zinc oxide coated sheet-shaped iron-silicon-chromium wave-absorbing material.
In the above-described production method, preferably, in step S1, the Fe 90 Si 7 Cr 3 Is prepared by an air atomization method and is sieved to obtain the particle size of 3-6 mu m.
In the above-described production method, it is preferable that the annealing treatment is performed at a temperature of 450 to 600℃for 1 to 2 hours in step S1.
Further, the annealing treatment is carried out for 1 hour at 500-550 ℃.
In the above-described production method, preferably, in step S2, the ZnO powder is a nano-sized powder, and the Fe 90 Si 7 Cr 3 The powder and ZnO powder are added according to the mass ratio of 85-95:5-15。
The preparation method as described above, preferably, in step S2, the ball-milled ball-to-material ratio of 20:1, ball milling ball diameter is 3mm, ball milling rotating speed is 300r/min, and ball milling time is 1-3 hours.
In the above-described production method, preferably, in step S3, the flake Fe 90 Si 7 Cr 3 The weight ratio of the @ ZnO powder to the polyurethane is 3.5-4.5:1.
According to the preparation method, preferably, the acetone addition amount is added according to the polyurethane use amount in a volume ratio of 6-8:1.
The dosage of the acetone solution can be quickly volatilized on the premise of fully dissolving polyurethane, so that the influence of residues in the product on quality is avoided, and the acetone is preferable: the volume ratio of the polyurethane is 6-8:1.
In the above-described production method, preferably, in step S3, the condition of the magnetic field rotational orientation is that the magnetic field strength is 1 to 1.2T, and the rotational speed is 1 to 20r/min for 10 to 15 minutes.
In the above method, preferably, in step S3, the high-temperature hot-pressing condition is that the hot-pressing temperature is 100-150 ℃, the heat-preserving time is 10-20 minutes, and the pressure is 3-8 Mpa.
The oriented zinc oxide coated sheet iron silicon chromium wave absorbing material obtained by the preparation method has effective wave absorbing width (reflection loss < -10 dB) of 1-4GHz under the ultra-thin thickness of 1-3 mm, and the peak intensity of the reflection loss is between-15 dB and-20 dB.
(III) beneficial effects
The beneficial effects of the invention are as follows:
1. the oriented zinc oxide coated sheet-shaped iron-silicon-chromium wave-absorbing material provided by the invention uses Fe with high magnetic conductivity 90 Si 7 Cr 3 The magnetic powder is used as a matrix, and ZnO coated flaky Fe is prepared by adopting a dispersion blending ball milling mode 90 Si 7 Cr 3 The @ ZnO powder effectively inhibits the conductive network among particles and reduces the dielectric constant; at the same time, by flaking Fe 90 Si 7 Cr 3 The @ ZnO powder is subjected to magnetic field rotation orientation, so that flaky particles in the material are arranged in an oriented manner, the magnetic permeability is greatly improved, the impedance matching is optimized, and the low-frequency wave absorbing performance of the material is improved.
2. The preparation method of the oriented zinc oxide coated sheet iron silicon chromium wave-absorbing material provided by the invention has the advantages of simple coating process, convenient operation and low economic cost, and is beneficial to industrial production and practical application, so that the oriented zinc oxide coated sheet iron silicon chromium wave-absorbing material has good development prospect.
3. According to the preparation method of the oriented zinc oxide coated sheet-shaped iron silicon chromium wave-absorbing material, the oriented zinc oxide coated sheet-shaped iron silicon chromium wave-absorbing material is prepared by a specific method, and the material realizes high-efficiency wave-absorbing performance under the microwave frequency band of 1-4GHz under the thickness of a very thin (1-3 mm) wave-absorbing body.
Drawings
FIG. 1 is a schematic diagram of a process flow of a directional arrangement zinc oxide coated sheet iron silicon chromium wave absorbing material prepared by the method of the invention;
FIG. 2 shows the flaky Fe obtained in step S4 of example 1 of the present invention 90 Si 7 Cr 3 Scanning electron microscope image of @ ZnO powder;
FIG. 3 is a cross-sectional scanning electron microscope image of the oriented zinc oxide coated sheet-like iron-silicon-chromium wave-absorbing material obtained in example 1 of the present invention;
FIG. 4 shows the plate-like Fe obtained in step S4 of example 1 by using a vibrating sample magnetometer 90 Si 7 Cr 3 Magnetic property test result of @ ZnO powder;
FIG. 5 is a Reflection Loss (RL) curve of the wave-absorbing material prepared in example 1;
FIG. 6 is a Reflection Loss (RL) curve of the wave-absorbing material prepared in example 2;
FIG. 7 is a Reflection Loss (RL) curve of the wave-absorbing material prepared in example 3;
FIG. 8 is a complex dielectric constant of the composite wave-absorbing material prepared in comparative example 1;
FIG. 9 is a complex permeability of the composite wave-absorbing material prepared in comparative example 1;
FIG. 10 is a Reflection Loss (RL) curve of the wave-absorbing material prepared in example 4;
fig. 11 is a Reflection Loss (RL) curve of the wave-absorbing material prepared in example 4.
Detailed Description
The preparation method comprises the following steps of performing dispersion blending ball milling on iron-silicon-chromium alloy soft magnetic powder and zinc oxide nano particles, and coating by organic resin to obtain zinc oxide coated flaky iron-silicon-chromium soft magnetic particles, so as to optimize magnetic conductivity and impedance matching performance of magnetic powder in GHz frequency band; the flaky soft magnetic particles with shape anisotropy are subjected to the rotating force applied by an external magnetic field through magnetic field orientation, so that the easily magnetized surfaces are arranged along the magnetic field direction, the purpose of oriented arrangement of the flaky particles is achieved, and the efficient wave absorbing performance can be obtained at 1-4 GHz.
The invention provides a directional arranged zinc oxide coated sheet iron silicon chromium wave-absorbing material and a preparation method thereof, as shown in figure 1, and specifically comprises the following operations:
s1: firstly, preparing materials, and preparing Fe by using a high-pressure gas atomization method 90 Si 7 Cr 3 Then the granularity of the powder is controlled to be 3-6 mu m by a sample separating sieve; sieving the Fe 90 Si 7 Cr 3 And carrying out homogenizing annealing treatment on the powder, wherein the protective atmosphere is argon.
S2: fe obtained in step S1 90 Si 7 Cr 3 Powder, and ZnO powder, fe in parts by mass 90 Si 7 Cr 3 85-95 parts of powder and 5-15 parts of ZnO powder are added into a 2.5L steel pot for ball milling, the ball milling process parameters are that the ball material ratio is 20:1, the ball milling diameter is 3mm, absolute ethyl alcohol is used as a ball milling medium, the ball milling rotating speed is 300r/min, and the ball milling time is 1-3 hours for dispersion blending ball milling, so that the flaky Fe is obtained 90 Si 7 Cr 3 @ ZnO powder.
S3: ball milling to obtain flake Fe 90 Si 7 Cr 3 Uniformly dissolving @ ZnO powder and polyurethane in an acetone solution to coat with organic resin, and carrying out magnetic treatment when the solvent volatilizes to be in a viscous stateA field rotational orientation; and then carrying out high-temperature hot pressing on the dried composite product to obtain the oriented zinc oxide coated sheet-shaped iron-silicon-chromium wave-absorbing material.
The specific preparation method of the high-pressure gas atomization method comprises the following steps: adding 99% pure Fe, si and Cr simple substances into a smelting crucible to smelt according to the mass percentage of Fe being 90%, si being 7% and Cr being 3%, pouring the molten raw materials into a heat-preserving crucible (the heat-preserving temperature being 1000 ℃), flowing out through a small hole with the diameter of 5mm at the bottom of the heat-preserving crucible, atomizing under the impact of high-pressure argon, condensing and screening to obtain Fe with the particle size of 3-6 mu m 90 Si 7 Cr 3 And (3) powder.
Further, preferably, in step S1, the annealing temperature is 450 to 600℃and the incubation time is 1 to 2 hours. When the temperature reaches the recrystallization temperature, the grains can grow again to form uniform equiaxed grains, so that lattice distortion can be effectively eliminated, and dielectric relaxation phenomenon (1-4 GHz) under an application frequency band is reduced. And along with the rise of the annealing temperature, the domain wall formants and natural formants of the material move to lower frequency, so that the magnetic permeability of the material is increased at an application frequency band (1-4 GHz), and the wave absorbing performance of the material is effectively improved. When the annealing temperature exceeds 450-600 ℃, the alloy element generates diffusion phenomenon, the original crystal structure is destroyed, the magnetic conductivity is reduced, and the wave absorbing performance is weakened. More preferably, the annealing temperature is 500 to 550℃and the incubation time is 1 hour.
Preferably, in step S2, the particle size of the ZnO powder is preferably in the range of 20 to 100nm, and the nano-sized ZnO powder having a high resistivity can be uniformly coated on the flake Fe during the ball milling 90 Si 7 Cr 3 The surface of the material prevents the formation of a conductive network among particles, greatly reduces the dielectric constant and optimizes the impedance matching performance.
Further, preferably, in step S3, the flake Fe 90 Si 7 Cr 3 The weight ratio of the @ ZnO powder to the polyurethane is 3.5-4.5:1. It was found that at a thickness of 1-3 mm, when the mass ratio of the raw materials is higher than 4.5:1, the impedance matching performance of the material deteriorates, and the wave absorbing performance declines. With increasing polyurethane usage, the reflection loss peak moves to high frequencyWhen the mass ratio of the raw materials is lower than 3.5:1, the reflection loss peak moves to be out of the working frequency range, so that the flaky Fe is 90 Si 7 Cr 3 The @ ZnO powder and polyurethane are preferably added according to a mass ratio of 3.5-4.5:1.
In the method described above, preferably, in step S3, the mixture is placed in a mold by magnetic field rotation orientation, the magnetic field being set to a magnitude of 1 to 1.2T (tesla), the rotation speed being 1 to 20r/min, for 10 to 15 minutes.
Further, the magnetic field rotation orientation process condition is that the magnetic field strength is 1T and the orientation time is 15 minutes.
In the above method, preferably, in step S3, the condition of high-temperature hot pressing is that the hot pressing temperature is 100-150 ℃, the heat preservation time is 10-20 minutes, and the pressure is 3-8 Mpa, so as to obtain the dense wave-absorbing material. When the pressure is less than 3Mpa or the temperature is less than 100 ℃, residual air holes in the material can weaken the wave absorbing performance.
Most preferably, the condition of high-temperature hot pressing is that the hot pressing temperature is 120 ℃, the heat preservation time is 15 minutes, and the pressure is 4Mpa.
The invention will be better explained by the following detailed description of the embodiments with reference to the drawings.
Example 1
(1) The formula comprises the following components: the mass percentage is as follows: (Fe) 90 Si 7 Cr 3 ) 95 (ZnO) 5
(2) The preparation process comprises the following steps:
s1: fe prepared by gas atomization method 90 Si 7 Cr 3 After sieving the powder (3-6 μm), it was annealed at 500℃for 1 hour under an argon atmosphere.
S2: annealing Fe 90 Si 7 Cr 3 r powder and ZnO powder, and Fe is taken according to mass parts 90 Si 7 Cr 3 95 parts of powder and 5 parts of ZnO powder are subjected to dispersion ball milling, and the ball milling process parameters are as follows: ball-material ratio is 20:1, ball-milling medium is absolute ethyl alcohol, the adding amount of the absolute ethyl alcohol reaches 4/5 of the volume of a ball-milling tank, so that collision probability between particles and ball-milling beads is guaranteed, and flaking is improvedThe ball milling speed is 300r/min, the ball milling efficiency is 3mm, and the ball milling time is 2 hours.
S3: ball milling to obtain flake Fe 90 Si 7 Cr 3 Uniformly dissolving @ ZnO powder and polyurethane in acetone solution (Fe 90 Si 7 Cr 3 The mass ratio of the @ ZnO powder to the polyurethane is 4:1, the acetone is added according to the polyurethane dosage and the volume ratio of acetone to polyurethane=7:1, when the mixture is in a viscous state, the magnetic field rotation orientation is carried out, the magnetic field strength is 1T, and the orientation time is 15 minutes. And after the orientation is finished, transferring the material to a 60 ℃ oven for drying for 24 hours, and then carrying out high-temperature hot pressing on the dried product at the temperature of 120 ℃ and the pressure of 4Mpa for 15 minutes to obtain the composite wave-absorbing material.
Performance test:
determination of Fe obtained in step S2 Using a Cold field scanning Electron microscope (SEM, hitachi S-4800) 90 Si 7 Cr 3 And (3) the surface morphology and microstructure of the composite wave-absorbing material obtained in the step S3. Fe (Fe) 90 Si 7 Cr 3 The scanning electron microscope image of the @ ZnO powder is shown in FIG. 2, and the result shows that Fe is obtained 90 Si 7 Cr 3 The @ ZnO powder is flaky particles, no agglomeration phenomenon exists among the particles, and a layer of continuous zinc oxide particles are bonded on the surface of the magnetic powder. The scanning electron microscope image of the composite wave-absorbing material is shown in figure 3, and the result shows that the flaky magnetic particles in the composite wave-absorbing material are orderly and parallelly arranged along the magnetic field plane direction.
The magnetic properties of the composite wave absorbing material were measured using a vibrating sample magnetometer (VSM, lake Shore 7304). As a result, as shown in FIG. 4, after the non-magnetic zinc oxide is added, the sample still has higher saturation magnetization Ms (188.7 emu/g) and has excellent soft magnetic performance.
And testing the complex permeability and complex dielectric constant of the composite wave-absorbing material by adopting an Agilent-E8363B vector network analyzer. The testing principle is that a microwave signal source sends a single-frequency signal to pass through a coaxial sample, the phase and the amplitude of the single-frequency signal are obtained according to feedback data, then the single-frequency signal enters the next frequency point to scan, and after the measurement is completed, a computer processes and outputs the data. Before measurement, the measurement system must be calibrated, after the calibration is completed, the sample is placed into the test fixture, the coaxial cable is connected, and the operation computer outputs the electromagnetic parameters of the measured sample. And calculates the Reflection Loss (RL) of the electromagnetic wave in the material by transmission line theory, the reflection value of which is calculated by the following equation:
Figure BDA0003973763310000071
Figure BDA0003973763310000072
wherein ε r Is complex dielectric constant, mu of material r Is the complex permeability of the material, t is the thickness of the material, f is the frequency, c is the speed of light in free space 3 x 10 8 m/s, j is an imaginary unit, Z in Is the impedance of the wave absorber, Z 0 Is the impedance of free space.
The reflection loss of the wave-absorbing material prepared in example 1 was calculated, the curve of the reflection loss with frequency is shown in fig. 5, and samples with different thicknesses, such as Reflection Loss (RL) of 1.0mm, 1.5mm, 2.0mm, 2.5mm and 3mm, have good microwave absorption performance in the microwave frequency range of 1-4GHz, and the peak-to-peak intensity of the reflection loss is-19 dB when the thickness is 3 mm.
Example 2
(1) The formula comprises the following components: the mass percentage is as follows: (Fe) 90 Si 7 Cr 3 ) 95 (ZnO) 5
(2) The preparation process comprises the following steps:
s1: fe prepared by gas atomization method 90 Si 7 Cr 3 After sieving the powder (3-6 μm), it was annealed at 500℃for 1 hour under an argon atmosphere.
S2: annealing Fe 90 Si 7 Cr 3 Powder, and ZnO powder, fe in parts by mass 90 Si 7 Cr 3 95 parts of powder and 5 parts of ZnO are subjected to dispersion ball milling, and the ball milling process parameters are as follows: ball-to-material ratioThe ball milling medium is absolute ethyl alcohol in a ratio of 20:1, the adding amount reaches 4/5 of the volume of a ball milling tank, so as to ensure the collision probability and the flaking efficiency between particles and ball milling beads, the ball milling beads are 3mm in size, the ball milling rotating speed is 300r/min, and the ball milling time is 1 hour.
S3: ball milling to obtain flake Fe 90 Si 7 Cr 3 Uniformly dissolving @ ZnO powder and polyurethane in acetone solution (Fe 90 Si 7 Cr 3 The mass ratio of the @ ZnO powder to the polyurethane is 4:1, the acetone is added according to the polyurethane dosage according to the volume ratio of acetone to polyurethane=7:1, and when the mixture is in a viscous state, the mixture is subjected to magnetic field rotation orientation, the magnetic field strength is 1T, and the orientation time is 15 minutes. And after the orientation is finished, transferring the material to a 60 ℃ oven for drying for 24 hours, and then carrying out high-temperature hot pressing on the dried product at the temperature of 120 ℃ and the pressure of 4Mpa for 15 minutes to obtain the composite wave-absorbing material.
The reflection loss of the wave-absorbing material prepared in example 2 is calculated, the curve of the reflection loss with frequency is shown in fig. 7, and the Reflection Loss (RL) of samples with different thicknesses, specifically 1.2mm, 1.5mm, 2.0mm, 2.5mm and 3mm, in the microwave frequency range of 1-4GHz is shown in fig. 6, so that the wave-absorbing material has good microwave absorption performance, and compared with example 1, the reflection loss peak shifts to low frequency. When the thickness is 3mm, the peak intensity of the reflection loss is-18 dB.
Example 3
(1) The formula comprises the following components: the mass percentage is as follows: (Fe) 90 Si 7 Cr 3 ) 90 (ZnO) 10
(2) The preparation process comprises the following steps:
s1: fe prepared by gas atomization method 90 Si 7 Cr 3 After sieving the powder (3-6 μm), it was annealed at 550℃for 1 hour under an argon atmosphere.
S2: annealing Fe 90 Si 7 Cr 3 Taking Fe as powder and ZnO powder according to mass parts 90 Si 7 Cr 3 Mixing 90 parts of powder and 10 parts of ZnO powder, and performing dispersion ball milling, wherein the ball milling process parameters are as follows: ball-material ratio is 20:1, ball-milling medium is absolute ethyl alcohol, ball-milling ball size is 3mm, ball-milling rotating speed is 300r/min,ball milling time was 3 hours.
S3: ball milling to obtain flake Fe 90 Si 7 Cr 3 Uniformly dissolving @ ZnO powder and polyurethane in acetone solution (Fe 90 Si 7 Cr 3 The mass ratio of the @ ZnO powder to the polyurethane is 4:1, the acetone is added according to the polyurethane dosage according to the volume ratio of acetone to polyurethane=7:1, and when the mixture is in a viscous state, the mixture is subjected to magnetic field rotation orientation, the magnetic field strength is 1T, and the orientation time is 15 minutes. And after the orientation is finished, transferring the material to a 60 ℃ oven for drying for 24 hours, and then carrying out high-temperature hot pressing on the dried product at the temperature of 120 ℃ and the pressure of 4Mpa for 15 minutes to obtain the composite wave-absorbing material.
The reflection loss of the wave absorbing material prepared in example 3 is calculated, the curve of the obtained reflection loss with frequency is shown in fig. 7, and from the aspect of wave absorbing effect, samples with different thicknesses, specifically, reflection Loss (RL) of 1.0mm, 1.5mm, 2.0mm, 2.5mm and 3mm have good microwave absorption performance in the microwave frequency range of 1-4 GHz. When the thickness is 3mm, the peak intensity of the reflection loss is-18 dB.
Comparative example 1
Based on example 1, epoxy resin was used to replace polyurethane to Fe 90 Si 7 Cr 3 The @ ZnO powder is subjected to surface modification, only epoxy resin is used for replacing polyurethane, and other operations are unchanged. The results are shown in fig. 8 and 9, wherein epsilon 'is the real part of the permittivity, epsilon "is the imaginary part of the permittivity, mu' is the real part of the permeability, and mu" is the imaginary part of the permeability.
Experimental results show that compared with epoxy resin, the sample using polyurethane has lower dielectric constant due to the difference of the viscosity and the adhesive force of the resin base material, is favorable for optimizing impedance matching and improving microwave absorption performance.
Example 4
Based on example 1, fe in step S3 90 Si 7 Cr 3 The mass ratio of @ ZnO powder to polyurethane (noted as Fe 90 Si 7 Cr 3 @ ZnO: pu) was adjusted to 3:1, 4:1, 5:1. 6:1, otherwise the procedure is the same as in example 1.
The reflection loss result of the material with the thickness of 1mm is shown in FIG. 10, the reflection loss result of the material with the thickness of 3mm is shown in FIG. 11, and the experimental result shows that with Fe 90 Si 7 Cr 3 The mass ratio of the @ ZnO powder to the polyurethane raw material is increased, the absorption peak of the material moves towards low frequency, and the wave absorbing performance is weakened. At a material thickness of 1-3 mm, an optimal absorption effect is achieved when the raw material mass ratio is 4:1, if the raw material ratio is continuously reduced, a thicker material thickness is required to achieve the same absorption effect, otherwise, the reflection loss peak will move outside the working frequency band.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any person skilled in the art may make modifications or alterations to the above disclosed technical content to equivalent embodiments. However, any simple modification, equivalent variation and variation of the above embodiments according to the technical substance of the present invention still fall within the protection scope of the technical solution of the present invention.

Claims (10)

1. The preparation method of the oriented zinc oxide coated sheet iron silicon chromium wave-absorbing material is characterized by comprising the following steps of:
s1: the mass percentage of Fe is as follows 90 Si 7 Cr 3 The metal soft magnetic powder of (2) is annealed in inert atmosphere;
s2: fe treated in step S1 90 Si 7 Cr 3 Ball milling the powder and ZnO powder, and taking absolute ethyl alcohol as a ball milling medium to obtain flaky Fe 90 Si 7 Cr 3 A @ ZnO powder;
s3: ball milling the obtained flaky Fe 90 Si 7 Cr 3 Uniformly dissolving the @ ZnO powder and polyurethane in an acetone solution, and performing magnetic field rotation orientation when the solvent volatilizes to be in a viscous mixture state; then hot pressing the dried composite product at high temperature to obtain oriented zinc oxide coated sheetIron-silicon-chromium wave-absorbing material.
2. The method according to claim 1, wherein in step S1, the Fe 90 Si 7 Cr 3 Is prepared by an air atomization method and is sieved to obtain the particle size of 3-6 mu m.
3. The method according to claim 1, wherein in step S1, the annealing is performed at a temperature of 450 to 600℃for 1 to 2 hours.
4. The method of claim 1, wherein in step S2, the Fe 90 Si 7 Cr 3 The powder and ZnO powder are added according to the mass ratio of 85-95:5-15.
5. The preparation method according to claim 1, wherein in the step S2, the ball-milling ratio of ball-milling is 20:1, the ball-milling diameter is 3mm, the ball-milling rotating speed is 300r/min, and the ball-milling time is 1-3 hours.
6. The method according to claim 1, wherein in step S3, the Fe in a flake form 90 Si 7 Cr 3 The weight ratio of the @ ZnO powder to the polyurethane is 3.5-4.5:1.
7. The method according to claim 1, wherein in step S3, the condition of the magnetic field rotation orientation is that the magnetic field strength is 1 to 1.2T, the rotation speed is 1 to 20r/min, and the duration is 10 to 15 minutes.
8. The preparation method according to claim 1, wherein the high-temperature hot-pressing condition is a hot-pressing temperature of 100-150 ℃, a heat-preserving time of 10-20 minutes and a pressure of 3-8 Mpa.
9. An oriented zinc oxide coated sheet iron silicon chromium wave absorbing material prepared by the preparation method of any one of claims 1 to 8.
10. The oriented zinc oxide coated sheet iron silicon chromium wave absorbing material according to claim 9, wherein the wave absorbing material has an effective wave absorbing width of 1-4GHz at an ultra-thin thickness of 1-3 mm, and the reflection loss peak intensity is between-15 dB and-20 dB.
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106673640A (en) * 2016-12-15 2017-05-17 陕西科技大学 Barium ferrite / zinc oxide composite wave-absorbing material and preparation method thereof
CN108777931A (en) * 2018-05-23 2018-11-09 中国科学院宁波材料技术与工程研究所 A kind of high magnetic permeability electromagnetic wave absorbent material and preparation method thereof
CN112194903A (en) * 2020-09-21 2021-01-08 深圳市鸿富诚屏蔽材料有限公司 Heat-conducting wave-absorbing silica gel composite material and preparation method thereof
CN112846196A (en) * 2020-12-31 2021-05-28 莱芜职业技术学院 Preparation method for preparing flaky iron-silicon-chromium soft magnetic composite material
CN115190757A (en) * 2022-07-28 2022-10-14 中南大学湘雅三医院 Multi-dimensional FeCo2O4 modified flaky iron-silicon-chromium composite wave absorber material

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106673640A (en) * 2016-12-15 2017-05-17 陕西科技大学 Barium ferrite / zinc oxide composite wave-absorbing material and preparation method thereof
CN108777931A (en) * 2018-05-23 2018-11-09 中国科学院宁波材料技术与工程研究所 A kind of high magnetic permeability electromagnetic wave absorbent material and preparation method thereof
CN112194903A (en) * 2020-09-21 2021-01-08 深圳市鸿富诚屏蔽材料有限公司 Heat-conducting wave-absorbing silica gel composite material and preparation method thereof
CN112846196A (en) * 2020-12-31 2021-05-28 莱芜职业技术学院 Preparation method for preparing flaky iron-silicon-chromium soft magnetic composite material
CN115190757A (en) * 2022-07-28 2022-10-14 中南大学湘雅三医院 Multi-dimensional FeCo2O4 modified flaky iron-silicon-chromium composite wave absorber material

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