CN116174704A - Mixed high corrosion-resistant FeSiCr electromagnetic wave absorber and preparation method thereof - Google Patents
Mixed high corrosion-resistant FeSiCr electromagnetic wave absorber and preparation method thereof Download PDFInfo
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 20
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- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 8
- 239000010419 fine particle Substances 0.000 claims description 8
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/065—Spherical particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/068—Flake-like particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/142—Thermal or thermo-mechanical treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
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Abstract
The invention relates to a mixed type high corrosion resistant FeSiCr electromagnetic wave absorber, which is formed by uniformly distributing flaky FeSiCr powder and spherical FeSiCr powder; the mixed high corrosion resistance FeSiCr electromagnetic wave absorber comprises 5-15 wt% of flaky FeSiCr powder and the balance of spherical FeSiCr powder; the beneficial effects of the invention are as follows: the prepared mixed absorbent has the characteristics of high magnetic conductivity, controllable density and strong corrosion resistance in a microwave high-frequency band, and can be applied to a coating material with higher requirements on corrosion resistance and electromagnetic wave absorption performance in marine environment.
Description
Technical Field
The invention relates to the technical field of electromagnetic wave absorbers, in particular to a mixed high corrosion-resistant FeSiCr electromagnetic wave absorber and a preparation method thereof.
Background
The marine corrosive environment comprises a marine atmosphere area, a splash area, a tidal range area, a full immersion area and a sea mud area. The marine atmosphere has high humidity and contains salt, and the corrosion rate is often 4 to 5 times higher than that of inland atmosphere. The pipelines or facilities in the splash zone are often impacted by waves and floaters, the surfaces are dry and wet alternately, the water and oxygen supply are sufficient, and the pipelines or facilities in the splash zone are the most severely corroded areas in the marine environment. Marine corrosion is mainly localized corrosion, i.e., corrosion that occurs in a small area from the surface of the component, such as galvanic corrosion, pitting corrosion, crevice corrosion, and the like. The use of thick paste anticorrosive coatings is a major approach to preventing marine corrosion.
The FeSi metal powder is used as a traditional soft magnetic material, and has good conductivity, higher Curie temperature and larger saturation magnetization. However, in marine environments, feSi or FeSiAl alloys have poor corrosion resistance due to the influence of chloride ions, and the corrosion rate reaches about 0.2mm/year, with a corrosion resistance rating of 6. The metallic Cr can improve the oxidation resistance and corrosion resistance of the alloy and inhibit the growth of crystal grains. Smaller grain sizes facilitate the formation of continuous protective corrosion product films. And a certain amount of Cr is added into the FeSi alloy, so that the microstructure can be optimized, and the magnetic permeability, the ductility and the corrosion resistance of the material can be improved. Thus, feSiCr alloys are widely used as wave-absorbing materials in the microwave band. The particle size of the absorbent affects the peak value of the permeability and the iron content affects the frequency of the peak value, so that the prior art needs to fully consider that the iron content cannot be lower than 88wt% when designing the absorbent component, and the particle size of the absorbent is preferably about 10 μm.
In marine environment, the corrosion resistance and electromagnetic wave absorption characteristics of metal parts such as large ships, airplanes and the like are simultaneously considered, so that the development of the anticorrosive paint of the electromagnetic wave absorbent with high corrosion resistance is urgent for national defense and civil use.
In the prior art about FeSiCr, the surface coating aspect of powder is almost focused, for example, patent publication nos. CN111575603a and CN109054740a are all related to powder preparation and coating, and research on the corrosion resistance of FeSiCr powder is lacking.
Therefore, a mixed type high corrosion-resistant FeSiCr electromagnetic wave absorber and a preparation method thereof are provided, the mixed type high corrosion-resistant FeSiCr electromagnetic wave absorber prepared by the method has strong electromagnetic wave absorption performance in a microwave high-frequency band and strong corrosion resistance, and the method can simultaneously adjust the peak value and the density of the magnetic permeability of the electromagnetic wave absorber, so that the use requirement of a certain specific frequency band can be met.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a mixed type high corrosion-resistant FeSiCr electromagnetic wave absorber and a preparation method thereof.
The aim of the invention is realized by the following technical scheme:
the invention provides a mixed type high corrosion resistant FeSiCr electromagnetic wave absorber, which is formed by uniformly distributing flaky FeSiCr powder and spherical FeSiCr powder; the mixed high corrosion resistant FeSiCr electromagnetic wave absorber comprises 5-15 wt% of flaky FeSiCr powder and the balance of spherical FeSiCr powder by mass percent.
Further, the chemical components and the content of the flaky FeSiCr powder are as follows: 7-9 wt% of Si, 2-4 wt% of Cr and the balance of Fe;
the chemical components and the content of the spherical FeSiCr powder are as follows: 7-9 wt% of Si, 2-4 wt% of Cr and the balance of Fe.
Further, the particle size of the spherical FeSiCr powder is 2-5 μm.
Further, the particle size of the flaky FeSiCr powder is less than 10 mu m, and the long diameter is more than 20 mu m.
Further preferably, the chemical components and the content of the flaky FeSiCr powder and the spherical FeSiCr powder are as follows: 8wt% Si, 2.5wt% Cr, and the balance Fe.
The invention also provides a method for preparing the mixed high corrosion resistant FeSiCr electromagnetic wave absorbent, which comprises the following steps:
A. preparation of spherical FeSiCr powder:
a1, weighing iron rods, silicon particles and chromium ingots as raw materials according to the weight percentage of 7-9% of Si, 2-4% of Cr and the balance of Fe;
a2, smelting alloy in a vacuum induction smelting furnace from iron rods, silicon particles and chromium ingots, and carrying out water mist or aerosol method powder preparation after 2-3 minutes of molten solution is cleared;
a3, screening the powder obtained in the step a2 to obtain spherical FeSiCr powder with the particle size of 2-5 mu m and fine particles with the particle size of 5-10 mu m;
B. preparing flaky powder:
b1, adopting zirconia balls, adding 5-10 mu m fine particles into a ball mill according to the proportion of 1:20 of ball ratio, adding a special ball grinding agent, and carrying out wet grinding for 5 hours at the rotating speed of 400r/min to obtain flaky powder with the particle size of less than 10 mu m;
b2, drying the flaky powder obtained in the step b1 at 60 ℃ to obtain dried flaky powder;
C. powder stress relief annealing treatment:
putting the dried flaky powder into a vacuum tube furnace, introducing nitrogen for protection, and preserving the temperature for 3 hours at 700 ℃ to obtain flaky FeSiCr powder;
D. preparation of mixed powder:
the method comprises the steps of ball milling and mixing flaky FeSiCr powder and spherical FeSiCr powder according to the proportion that the flaky FeSiCr powder accounts for 5-15 wt% and the balance of spherical FeSiCr powder to obtain mixed FeSiCr powder, and obtaining the mixed high corrosion resistant FeSiCr electromagnetic wave absorber.
Further, in the step D, the rotation speed of ball milling and mixing is 200r/min, and the ball milling and mixing time is 10min. The spherical FeSiCr powder and the flaky FeSiCr powder can be uniformly distributed, and the particle size and shape of the spherical FeSiCr powder and the flaky FeSiCr powder cannot be changed.
Further, in the step A, the purities of the iron rod, the silicon particles and the chromium ingots are all more than 99.9 percent.
Further, in the step A, alloy is smelted in a vacuum induction smelting furnace, the vacuum before smelting is less than 0.1Pa, and the smelting process is controlled to be about 1 Pa.
Further, the zirconia balls are made of
And->
Is mixed with the three zirconia balls, and
and->
The mass ratio of the three zirconia balls is 8:3:1.
The description is as follows: the stress annealing has the effects of improving the permeability of the absorbent, improving the electrochemical uniformity of a material interface and improving the corrosion resistance.
The description is as follows: the morphology feature of the absorbent can greatly influence magnetic permeability, the flaky shape is beneficial to low frequency and the spherical shape is beneficial to high frequency, and the granularity of the absorbent can influence the peak value of the magnetic permeability, so that when the absorbent component is designed in the prior art, in order to ensure that the absorbent has good magnetic permeability, the granularity of the absorbent is controlled to be about 10 mu m, and the innovative discovery of the scheme is that FeSiCr powder is prepared into spherical FeSiCr powder with the particle size of 2-5 mu m and is ball-milled and mixed with flaky FeSiCr powder with the particle size of less than 10 mu m, and the obtained mixed absorbent can ensure that the absorbent has the characteristic of high magnetic permeability in a microwave high frequency band and has outstanding corrosion resistance.
In the invention, a certain amount of Cr is added into the FeSi alloy, so that the corrosion resistance of the absorber can be properly optimized, the spherical shape is higher than the sheet-shaped corrosion resistance, the spherical FeSiCr powder with the size slightly smaller than that of the sheet-shaped powder is uniformly distributed with the spherical FeSiCr powder, and then the space distribution filled with each other is formed in the three-dimensional space, and the space structure which is tighter than the sheet-shaped FeSiCr powder and more dispersed than the spherical FeSiCr powder is formed.
The beneficial effects of the invention are as follows: 1) The proposal prepares 2-5 mu m spherical FeSiCr powder and 5-10 mu m fine particles by an atomization method, and the fine particles are ball-milled to prepare sheet powder with the particle diameter smaller than 10 mu m; the sheet-shaped powder is subjected to stress relief annealing and then is ball-milled and mixed with 2-5 mu m spherical FeSiCr powder to prepare a mixed type high corrosion-resistant FeSiCr electromagnetic wave absorbent, wherein the weight of the sheet-shaped FeSiCr powder in the mixed type absorbent is 5-15 percent; the mixed absorbent prepared by the scheme has the characteristics of high magnetic conductivity and strong corrosion resistance in a microwave high-frequency band, the tap density can be adjusted by the proportion of the flaky powder to the spherical powder, and the mixed absorbent can be suitable for a coating material with higher requirements on corrosion resistance and electromagnetic wave absorption performance in marine environments;
2) The mixed high corrosion resistant FeSiCr electromagnetic wave absorber of the invention can be completed by a traditional atomization powder making device, a ball mill and a tubular annealing furnace without special preparation equipment; the device is simple, the operation is simple, the cost is low, and industrialization is easy to realize;
3) The invention adopts zirconia grinding balls, controls the ball milling time, and obtains ideal flaky FeSiCr powder; the ratio of the flaky FeSiCr powder to the spherical FeSiCr powder is controlled, and the peak value and the density of the magnetic permeability of the electromagnetic wave absorbent can be adjusted at the same time, so that the use requirement of a specific frequency band is met.
Drawings
FIG. 1 is an SEM image of a hybrid highly corrosion-resistant FeSiCr electromagnetic wave absorber prepared in example 1 of the present invention;
FIG. 2 is a graph of dielectric constant versus frequency for the present invention;
FIG. 3 is a graph of permeability versus frequency for the present invention;
fig. 4 is a Tafel plot.
Detailed Description
The technical solution of the present invention will be described in further detail with reference to the accompanying drawings, but the scope of the present invention is not limited to the following description.
Example 1
1) Preparing spherical powder:
firstly, preparing raw materials by adopting high-purity iron rods, silicon particles and chromium ingots with purity of more than 99.9 percent; silicon and chromium are respectively mixed according to the proportion of 8 weight percent of Si, 2.5 weight percent of Cr and the balance of Fe;
then smelting alloy in a vacuum induction smelting furnace with the vacuum less than 0.1Pa before smelting, controlling the smelting process to be about 1Pa, and ensuring that the vacuum requirement on the raw material in smelting is met; 2-3 minutes after the molten liquid is cleared, carrying out water mist method powder preparation;
sieving the powder to obtain spherical FeSiCr powder with granularity of 2-5 microns and fine particle with granularity of 5-10 microns;
2) Preparation of flake powder
By using
And->
Adding 5-10 mu m fine particles into a ball mill according to the proportion of 1:20 of ball ratio, adding a proper amount of special ball grinding agent, wet-milling at the rotating speed of 400r/min for 5h, and obtaining the granularity<10 mu m of flaky powder, and then drying at 60 ℃ to obtain dried flaky powder;
3) Powder stress relief annealing treatment: introducing nitrogen into the dried flaky powder to protect the flaky powder in a vacuum tube furnace, and preserving the temperature for 3 hours at 700 ℃ to obtain flaky FeSiCr powder with the particle size of less than 10 mu m and the length-diameter ratio of more than 20;
4) Preparation of mixed powder: ball-milling and mixing flaky FeSiCr powder and spherical FeSiCr powder, wherein the flaky FeSiCr powder accounts for 5 weight percent, and the balance is spherical FeSiCr powder; the rotation speed of ball milling and mixing of the ball mill is 200r/m, and after ball milling is carried out for 10min, the mixed high corrosion resistant FeSiCr electromagnetic wave absorber is obtained;
5) And (3) testing a compression ring: mixing the mixed high corrosion resistant FeSiCr electromagnetic wave absorber with paraffin according to the ratio of 6:1, pressing into an annular sample with phi 7mm multiplied by phi 3mm multiplied by 3mm, and measuring electromagnetic parameters of the mixed high corrosion resistant FeSiCr electromagnetic wave absorber to obtain the maximum value of the magnetic conductivity imaginary part of 2.05 and the frequency of 2.6GHz;
6) Corrosion resistance test: mixing the mixed high corrosion-resistant FeSiCr electromagnetic wave absorber with carbon black and polyvinylidene fluoride according to the ratio of 8:1:1, adding a proper amount of N-methyl pyrrolidone, stirring for 20min, vacuumizing, drying at 50 ℃ to prepare a sheet, testing an open circuit and a Tafel graph by using an electrochemical workstation, and measuring that the corrosion rate is 0.00446mm/year and the corrosion resistance grade is grade 2.
In this embodiment, in step 2),
and->
The mass ratio of the three zirconia balls is 8:3:1.
Example 2
This embodiment differs from embodiment 1 only in that: in the step 2), the flaky FeSiCr powder accounts for 10 weight percent, and the rest is spherical FeSiCr powder; finally, the maximum value of the magnetic conductivity imaginary part is 2.06, and the frequency is 2.9GHz; the corrosion rate was 0.00462mm/year and the corrosion rating was grade 2.
Example 3
The procedure of this example corresponds to example 1, and the only difference between this example and example 1 is: cr was changed to 3wt% in step 1). Finally, testing to obtain the maximum value of the imaginary part of the magnetic conductivity of 2.14 and the frequency of 3.0GHz; the corrosion rate was 0.00437mm/year and the corrosion rating was grade 2.
As can be seen from the comparison of example 1 and example 3, the peak value of the imaginary part of the magnetic permeability, the frequency and the corrosion resistance are all increased as the Cr content is increased.
From the comparison of the embodiment 1 and the embodiment 2, the proportion of the flaky FeSiCr powder is increased, the imaginary part of the magnetic permeability is slightly increased, but the frequency of the peak value moves to high frequency, and the corrosion resistance is reduced; therefore, the scheme can simultaneously adjust the peak value and the density of the magnetic permeability of the electromagnetic wave absorber by controlling the proportion of the flaky FeSiCr powder to the spherical FeSiCr powder, and further can meet the use requirement of a specific frequency band.
The foregoing is merely a preferred embodiment of the invention, and it is to be understood that the invention is not limited to the form disclosed herein but is not to be construed as excluding other embodiments, but is capable of numerous other combinations, modifications and environments and is capable of modifications within the scope of the inventive concept, either as taught or as a matter of routine skill or knowledge in the relevant art. And that modifications and variations which do not depart from the spirit and scope of the invention are intended to be within the scope of the appended claims.
Claims (10)
1. The mixed high corrosion resistant FeSiCr electromagnetic wave absorber is characterized in that the mixed high corrosion resistant FeSiCr electromagnetic wave absorber is a mixed absorber in which both flake FeSiCr powder and spherical FeSiCr powder are uniformly distributed;
the mixed high corrosion resistant FeSiCr electromagnetic wave absorber comprises 5-15 wt% of flaky FeSiCr powder and the balance of spherical FeSiCr powder by mass percent.
2. The hybrid highly corrosion-resistant FeSiCr electromagnetic wave absorber according to claim 1, characterized in that:
the chemical components and the content of the flaky FeSiCr powder are as follows: 7-9 wt% of Si, 2-4 wt% of Cr and the balance of Fe;
the chemical components and the content of the spherical FeSiCr powder are as follows: 7-9 wt% of Si, 2-4 wt% of Cr and the balance of Fe.
3. The hybrid highly corrosion-resistant FeSiCr electromagnetic wave absorber according to claim 2, characterized in that: the particle size of the spherical FeSiCr powder is 2-5 mu m.
4. A hybrid highly corrosion resistant FeSiCr electromagnetic wave absorber according to claim 3, characterized in that: the particle size of the flaky FeSiCr powder is less than 10 mu m, and the long diameter is more than 20 mu m.
5. The hybrid highly corrosion-resistant FeSiCr electromagnetic wave absorber according to claim 4, wherein: the chemical components and the contents of the flaky FeSiCr powder and the spherical FeSiCr powder are as follows: 8wt% Si, 2.5wt% Cr, and the balance Fe.
6. A process for preparing the hybrid highly corrosion resistant FeSiCr electromagnetic wave absorber of any one of claims 1 to 5, comprising the steps of:
A. preparation of spherical FeSiCr powder:
a1, weighing iron rods, silicon particles and chromium ingots as raw materials according to the weight percentage of 7-9% of Si, 2-4% of Cr and the balance of Fe;
a2, smelting alloy in a vacuum induction smelting furnace from iron rods, silicon particles and chromium ingots, and carrying out water mist or aerosol method powder preparation after 2-3 minutes of molten solution is cleared;
a3, screening the powder obtained in the step a2 to obtain spherical FeSiCr powder with the particle size of 2-5 mu m and fine particles with the particle size of 5-10 mu m;
B. preparing flaky powder:
b1, adopting zirconia balls, adding 5-10 mu m fine particles into a ball mill according to the proportion of 1:20 of ball ratio, adding a special ball grinding agent, and carrying out wet grinding for 5 hours at the rotating speed of 400r/min to obtain flaky powder with the particle size of less than 10 mu m;
b2, drying the flaky powder obtained in the step b1 at 60 ℃ to obtain dried flaky powder;
C. powder stress relief annealing treatment:
putting the dried flaky powder into a vacuum tube furnace, introducing nitrogen for protection, and preserving the temperature for 3 hours at 700 ℃ to obtain flaky FeSiCr powder;
D. preparation of mixed powder:
the method comprises the steps of ball milling and mixing flaky FeSiCr powder and spherical FeSiCr powder according to the proportion that the flaky FeSiCr powder accounts for 5-15 wt% and the balance of spherical FeSiCr powder to obtain mixed FeSiCr powder, and obtaining the mixed high corrosion resistant FeSiCr electromagnetic wave absorber.
7. The method for preparing the mixed highly corrosion-resistant FeSiCr electromagnetic wave absorber according to claim 6, wherein: in the step D, the rotation speed of ball milling and mixing is 200r/min, and the ball milling and mixing time is 10min.
8. The method for preparing the mixed highly corrosion-resistant FeSiCr electromagnetic wave absorber according to claim 7, wherein: in the step A, the purities of the iron rods, the silicon particles and the chromium ingots are all more than 99.9 percent.
9. The method for preparing the mixed highly corrosion-resistant FeSiCr electromagnetic wave absorber according to claim 8, wherein: and (C) smelting alloy in a vacuum induction smelting furnace, wherein the vacuum is less than 0.1Pa before smelting, and the smelting process is controlled to be about 1 Pa.
10. The method for preparing the mixed highly corrosion-resistant FeSiCr electromagnetic wave absorber according to claim 9, wherein: the zirconia balls are adopted
And->
Is mixed with the three zirconia balls and +.>
And->
The mass ratio of the three zirconia balls is 8:3:1./>
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202211414856.4A CN116174704A (en) | 2022-11-11 | 2022-11-11 | Mixed high corrosion-resistant FeSiCr electromagnetic wave absorber and preparation method thereof |
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| CN104036941A (en) * | 2014-06-10 | 2014-09-10 | 毛圣华 | Preparation method of amorphous metal powder non-magnetic sheet for wireless charger |
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| CN113773610A (en) * | 2021-10-09 | 2021-12-10 | 航天特种材料及工艺技术研究所 | Carbonyl iron powder wave-absorbing material and preparation method thereof |
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