CN115117640A - Low-frequency radar absorbent with high weather resistance and preparation method thereof - Google Patents
Low-frequency radar absorbent with high weather resistance and preparation method thereof Download PDFInfo
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Abstract
The low-frequency radar absorbent with high weather resistance comprises a main component of nickel-zinc ferrite, a small amount of doped ferrum-silicon-aluminum and graphene, wherein the content of the nickel-zinc ferrite is more than or equal to 90wt%, the content of the ferrum-silicon-aluminum is 6-8 wt%, the content of the graphene is 1-2 wt%, and the ferrum-silicon-aluminum is sheet ferrum-silicon-aluminum processed by a special process, namely the sheet ferrum-silicon-aluminum with the particle size of 20 +/-10 mu m is obtained by ball-milling the ferrum-silicon-aluminum by using alcohol. The invention also discloses a preparation method of the low-frequency radar absorbent. The low-frequency radar absorbent has the advantages of strong weather resistance, good wave-absorbing performance, thin thickness and simple preparation method.
Description
Technical Field
The invention relates to a low-frequency radar absorbent and a preparation method thereof, in particular to a low-frequency radar absorbent with strong weather resistance and a preparation method thereof.
Background
In the field of radar detection, the lower the frequency of an electromagnetic wave, the longer the wavelength of the electromagnetic wave, the smaller the atmospheric attenuation, and the longer the detection distance. The radar wave-absorbing material can consume the energy of incident electromagnetic waves through the unique structure and physical characteristics of the radar wave-absorbing material, so that the electromagnetic waves are invisible. In recent years, research work on radar wave-absorbing materials mainly focuses on the aspects of thinning and weight reduction of a fire control radar frequency range (namely X, Ku wave band), and research on low-frequency electromagnetic waves is less.
At present, the traditional low-frequency wave-absorbing material, such as ferrite, has good wave-absorbing performance in a frequency band below 5GHz only when the thickness of the ferrite is very thick, and is generally used as a darkroom wave-absorbing brick, so the problems of wavelength and thickness need to be considered; for example, the alloy powder has better performance below 2GHz, but the weather resistance of the alloy powder is relatively poor, and the alloy powder is easy to rust in the actual use process, so the problems of performance and weather resistance need to be considered.
CN 114101685A discloses a low-frequency radar wave absorbent and a preparation method thereof, wherein the preparation method comprises the following steps: (1) adding the spherical iron-cobalt alloy micro powder, a grinding aid and a coating liquid into a ball milling tank, carrying out ball milling treatment, and drying to obtain silicon dioxide coated flaky iron-cobalt alloy micro powder; wherein the atomic ratio of iron to cobalt in the spherical iron-cobalt alloy micro powder is 65: 35; the grinding aid is calcium stearate; the coating liquid is tetraethoxysilane; (2) mixing the flaky iron-cobalt alloy micro powder and ferrocene to obtain mixed powder; (3) and placing the mixed powder in an inert atmosphere to carry out chemical reaction and heat treatment in sequence to obtain the low-frequency radar wave absorbent. However, the method is complex to prepare, strict requirements are imposed on the content of the spherical iron-cobalt alloy micro powder and the coating liquid in the coating liquid, the production cost is high, and although relevant test data of weather resistance is not recorded, generally speaking, the weather resistance of the alloy powder is poor.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defects in the prior art and provide a low-frequency radar absorbent with strong weather resistance, good wave-absorbing performance and thin thickness.
The invention further aims to solve the technical problem of providing a preparation method of the low-frequency radar absorbent with strong weather resistance.
The invention solves the technical problem by adopting the technical scheme that the low-frequency radar absorbent with strong weather resistance comprises a main component of nickel-zinc ferrite, a small amount of doped ferrum-silicon-aluminum (ferrum-silicon-aluminum alloy powder) and graphene, wherein the content of the nickel-zinc ferrite is more than or equal to 90wt%, the content of the ferrum-silicon-aluminum is 6-8 wt%, and the content of the graphene is 1-2 wt%.
Furthermore, the nickel-zinc ferrite is prepared by mixing and sintering raw materials of nickel oxide, zinc oxide and ferrous oxide as main bodies and copper oxide as a sintering aid.
Further, the iron-silicon-aluminum is sheet iron-silicon-aluminum processed by a special process, namely, the iron-silicon-aluminum is ball-milled to the sheet iron-silicon-aluminum with the particle size of 20um +/-10 um by using alcohol. The size of the flaky Fe-Si-Al particles is accurately controlled to be 20um +/-10 um by controlling the ball milling time.
Further, the mass ratio of the mixture of iron, silicon and aluminum in the Fe-Si-Al is 80-90: 5-10, and preferably 85:9: 6.
Further, the raw material contains 10-20 wt% of nickel oxide, 10-20 wt% of zinc oxide, 60-70 wt% of ferrous oxide and 1-2 wt% of auxiliary agent copper oxide.
The invention further solves the technical problem by adopting the technical scheme that the preparation method of the low-frequency radar absorbent with strong weather resistance comprises the following steps:
(1) mixing raw materials of nickel oxide, zinc oxide and ferrous oxide, and adding an auxiliary agent of copper oxide to obtain a mixture; performing wet ball milling on the mixture to obtain ball milling slurry;
(2) spray drying the ball-milling slurry obtained in the step (1) to obtain a dry mixture;
(3) sintering the dry mixture obtained in the step (2), and cooling to obtain a sintered wave absorbing agent material;
(4) finely grinding the sintered wave absorbing agent material obtained in the step (3), performing vibration grinding and crushing, and sieving to obtain a ferrite wave absorbing material;
(5) and (4) mixing the ferrite wave-absorbing material obtained in the step (4) with the specially-treated Fe-Si-Al and graphene, and uniformly stirring to obtain the low-frequency radar absorbent with strong weather resistance.
Further, in the step (1), the wet ball milling time is 1-3 hours, and the mass ratio of the mixture to the steel balls to the water in the ball milling process is 1-2: 8-15: 1-2.
Further, in the step (3), the sintering temperature is 1200-1300 ℃; and the heat preservation time of the sintering is 1-3 h.
Further, in the step (4), the mesh number of the sieved screen is 100-200 meshes.
Further, in the step (5), the specially processed sendust is sheet sendust with a particle size of 20um ± 10um obtained by alcohol ball milling.
Compared with the prior art, the invention has the following beneficial effects:
(1) according to the invention, the magnetic wave-absorbing material is subjected to composite design, nickel-zinc ferrite is taken as a main component, the lattice structure distortion is promoted by adjusting the contents of nickel and zinc, so that the material can obtain excellent magnetic performance under low frequency, a good low-frequency absorption effect is obtained, sendust and graphene are doped, the dielectric property of the material is adjusted, the dielectric loss is increased, the reflection loss peak is promoted to shift to low frequency, and the low-frequency absorption performance is optimized;
(2) the invention adopts a special process treatment method, firstly ball-milling the ferrum-silicon-aluminum by using alcohol, carrying out flakiness treatment, accurately controlling the size of flakinesed ferrum-silicon-aluminum particles to be 20um +/-10 um by controlling the ball-milling time, then uniformly mixing the ferrum-silicon-aluminum powder and graphene, and adopting alcohol ball milling to prevent the flakinesed ferrum-silicon-aluminum from being adhered and agglomerated in the drying process, wherein the most important of the process is to control the particle size of the ferrum-silicon-aluminum, the particle size is accurately controlled to be 20um +/-10 um, the particle size range is consistent with the particle size range of ferrite powder, the magnetic loss and the dielectric loss can be ensured to be uniformly dispersed in the whole material system, the longer the ball-milling time is, the smaller the ferrum-silicon-aluminum flakiness particles are, the maximum reflection loss peak value of the ferrum-silicon-aluminum can be increased, but the peak position can gradually move to a high-frequency part, so that the performance of the low-frequency part is reduced;
(3) the low-frequency radar absorbent composite material prepared by taking the ferrite as the main body has the characteristics of both ferrum-silicon-aluminum and graphene, can have extremely wide absorption bandwidth under thinner thickness, has wave-absorbing performance below-5 dB in the range of 0.5-5 GHz when the thickness is not more than 2mm, and has extremely good weather resistance;
(4) the processes involved in the invention are all conventional processes in the powder metallurgy industry, the process is simple, the cost is low, and the method is suitable for industrial mass production; meanwhile, the wave-absorbing coating can be further prepared by matching with resin, curing agent and the like, so that the wave-absorbing coating has a wider application range.
Drawings
Fig. 1 is a state diagram of a low-frequency radar wave-absorbing material subjected to a neutral salt spray test for 1000 hours in embodiment 1 of the invention.
FIG. 2 is a state diagram of pure sendust powder after undergoing a neutral salt spray test for 300 h.
Detailed Description
The invention is further described with reference to the following figures and specific examples.
Example 1
The low-frequency radar absorbent with high weather resistance is composed of a main component of nickel-zinc ferrite, a small amount of doped iron-silicon-aluminum and graphene, wherein the content of the nickel-zinc ferrite is 91wt%, the content of the iron-silicon-aluminum is 8wt%, and the content of the graphene is 1 wt%. The chemical formula of the nickel-zinc ferrite of the embodiment is Ni 0.5 Zn 0.5 Fe 2 O 4 The average particle size of the sendust sheet powder is 20 um.
The preparation method of the low-frequency radar absorbent with strong weather resistance comprises the following steps:
(1) nickel oxide, zinc oxide, ferrous oxide and copper oxide are mixed according to the mass ratio of 15: 17: 67: 1, mixing, adding deionized water, and performing wet ball milling for 2 hours to obtain ball milling slurry;
(2) spray drying the ball-milling slurry obtained in the step (1) to obtain a dry mixture
(3) Heating the dried mixture obtained in the step (2) to 1250 ℃, sintering and preserving heat for 2h, and then cooling to room temperature to obtain a sintered material;
(4) vibrating, grinding and crushing the sintered material obtained in the step (3), and sieving the crushed material with a 160-mesh sieve to obtain ferrite powder;
(5) carrying out alcohol ball milling on the Fe-Si-Al powder for 2h on a planetary ball mill, drying to obtain Fe-Si-Al flaky powder, and testing the average particle size to be 20 um;
(6) and (3) mixing the Fe-Si-Al flaky powder obtained in the step (5) with graphene according to a mass ratio of 8: 1, mixing and uniformly stirring to obtain a mixture;
(7) mixing the ferrite powder obtained in the step (4) with the mixture obtained in the step (6) according to the ratio of 91: 9, mixing and uniformly stirring to obtain the low-frequency radar wave absorbent;
the low-frequency radar wave absorbent of the embodiment was subjected to performance test. The test method is to mix the radar wave absorbent of the embodiment with resin according to the following ratio of 80: 20, stirring for two hours, adding a curing agent accounting for 50 percent of the mass of the resin, manually stirring for one minute to prepare the wave-absorbing coating, spraying the coating on an aluminum plate by a spray gun with the thickness of 2mm to prepare a coating test board, and carrying out actual measurement on the wave-absorbing performance. The following examples and comparative examples were tested in the same manner as in the present example. The results are shown in Table 1 and FIGS. 1-2.
As can be seen from the comparison between fig. 1 and fig. 2, fig. 1 is a state diagram of the low-frequency radar wave-absorbing material of embodiment 1 of the present invention after undergoing a neutral salt spray test for 1000 hours, and the low-frequency radar wave-absorbing material of the present invention is not corroded and has strong weather resistance. As can be seen from FIG. 2, the pure iron silicon aluminum alloy powder only undergoes 300h of neutral salt spray, so that rust spots and bubbles appear, and the weather resistance is poor.
Example 2
The low-frequency radar absorbent with high weather resistance is composed of a main component of nickel-zinc ferrite, a small amount of doped iron-silicon-aluminum and graphene, wherein the content of the nickel-zinc ferrite is 91wt%, the content of the iron-silicon-aluminum is 8wt%, and the content of the graphene is 1 wt%. The chemical formula of the nickel-zinc ferrite of the embodiment is Ni 0.5 Zn 0.5 Fe 2 O 4 The average particle size of the iron silicon aluminum flake powder is 13 um.
The preparation method of the low-frequency radar absorbent with strong weather resistance comprises the following steps:
(1) nickel oxide, zinc oxide, ferrous oxide and copper oxide are mixed according to the mass ratio of 15: 17: 67: 1, mixing, adding deionized water, and performing wet ball milling for 2 hours to obtain ball milling slurry;
(2) spray drying the ball-milling slurry obtained in the step (1) to obtain a dry mixture;
(3) heating the dried mixture obtained in the step (2) to 1250 ℃, sintering and preserving heat for 2h, and then cooling to room temperature to obtain a sintered material;
(4) vibrating, grinding and crushing the sintered material obtained in the step (3), and sieving the crushed material with a 160-mesh sieve to obtain ferrite powder;
(5) ball-milling Fe-Si-Al on a planetary ball mill for 2.5h by using alcohol, drying to obtain Fe-Si-Al flaky powder, and testing that the average particle size is 13 um;
(6) and (3) mixing the Fe-Si-Al flaky powder obtained in the step (5) with graphene according to a mass ratio of 8: 1, mixing and uniformly stirring to obtain a mixture;
(7) mixing the ferrite powder obtained in the step (4) with the mixture obtained in the step (6) according to the ratio of 91: 9, and stirring uniformly to obtain the low-frequency radar absorbent with strong weather resistance.
Example 3
The low-frequency radar absorbent with high weather resistance is composed of a main component of nickel-zinc ferrite, a small amount of doped iron-silicon-aluminum and graphene, wherein the content of the nickel-zinc ferrite is 91wt%, the content of the iron-silicon-aluminum is 8wt%, and the content of the graphene is 1 wt%. Ni of the present example 0.4 Zn 0.6 Fe 2 O 4 The average particle size of the iron silicon aluminum flake powder is 20 um.
The preparation method of the low-frequency radar absorbent with strong weather resistance comprises the following steps:
(1) mixing nickel oxide, zinc oxide, ferrous oxide and copper oxide according to a mass ratio of 12: 20: 67: 1, mixing, adding deionized water, and performing wet ball milling for 2 hours to obtain ball milling slurry;
(2) spray drying the ball-milling slurry obtained in the step (1) to obtain a dry mixture;
(3) heating the dried mixture obtained in the step (2) to 1230 ℃, sintering and preserving heat for 2h, and then cooling to room temperature to obtain a sintered material;
(4) vibrating, grinding and crushing the sintered material obtained in the step (3), and sieving the crushed material with a 160-mesh sieve to obtain ferrite powder;
(5) carrying out alcohol ball milling on the Fe-Si-Al powder for 2h on a planetary ball mill, drying to obtain Fe-Si-Al flaky powder, and testing the average particle size to be 20 um;
(6) and (3) mixing the Fe-Si-Al flaky powder obtained in the step (5) with graphene according to a mass ratio of 8: 1, mixing and uniformly stirring to obtain a mixture;
(7) mixing the ferrite powder obtained in the step (4) with the mixture obtained in the step (6) according to the ratio of 91: 9, and stirring uniformly to obtain the low-frequency radar absorbent with strong weather resistance.
Comparative example 1
The difference compared to example 1 is that the doped flaked sendust particles of comparative example 1 are less than 10um and the resulting radar absorber has a relatively larger peak of maximum reflection loss but insufficient performance at low frequencies.
The preparation method of the radar absorbent of the comparative example comprises the following steps:
(1) nickel oxide, zinc oxide, ferrous oxide and copper oxide are mixed according to the mass ratio of 15: 17: 67: 1, mixing, adding deionized water, and performing wet ball milling for 5 hours to obtain ball milling slurry;
(2) spray drying the ball-milling slurry obtained in the step (1) to obtain a dry mixture;
(3) heating the dried mixture obtained in the step (2) to 1250 ℃, sintering and preserving heat for 2h, and then cooling to room temperature to obtain a sintered material;
(4) vibrating, grinding and crushing the sintered material obtained in the step (3), and sieving the crushed material with a 160-mesh sieve to obtain ferrite powder;
(5) carrying out alcohol ball milling on the Fe-Si-Al powder for 2h on a planetary ball mill, drying to obtain Fe-Si-Al flaky powder, and testing the average particle size to be 3 um;
(6) and (3) mixing the Fe-Si-Al flaky powder obtained in the step (5) with graphene according to a mass ratio of 8: 1, mixing and uniformly stirring to obtain a mixture;
(7) mixing the ferrite powder obtained in the step (4) with the mixture obtained in the step (6) according to the ratio of 91: 9, and uniformly stirring to obtain the radar absorbent.
Comparative example 2
The difference compared to example 2 is that comparative example 2 doped flaked sendust particles of greater than 20um resulted in poorer overall performance of the resulting radar absorber.
The preparation method of the radar wave absorbent of the comparative example comprises the following steps:
(1) nickel oxide, zinc oxide, ferrous oxide and copper oxide are mixed according to the mass ratio of 15: 17: 67: 1, mixing, adding deionized water, and performing wet ball milling for 5 hours to obtain ball milling slurry;
(2) spray drying the ball-milling slurry obtained in the step (1) to obtain a dry mixture;
(3) heating the dried mixture obtained in the step (2) to 1250 ℃, sintering and preserving heat for 2h, and then cooling to room temperature to obtain a sintered material;
(4) vibrating, grinding and crushing the sintered material obtained in the step (3), and sieving the crushed material with a 160-mesh sieve to obtain ferrite powder;
(5) carrying out alcohol ball milling on the Fe-Si-Al powder for 1h on a planetary ball mill, drying to obtain Fe-Si-Al flaky powder, and testing the average particle size to be 36 um;
(6) and (3) mixing the Fe-Si-Al flaky powder obtained in the step (5) with graphene according to a mass ratio of 8: 1, mixing and uniformly stirring to obtain a mixture;
(7) mixing the ferrite powder obtained in the step (4) with the mixture obtained in the step (6) according to the ratio of 91: 9, and uniformly stirring to obtain the radar absorbent.
Comparative example 3
Compared with example 3, except that the nickel zinc ferrite of comparative example 3 has a chemical formula of Ni 0.8 Zn 0.2 Fe 2 O 4 The overall performance of the resulting radar absorber is poor due to the relatively high nickel content and relatively low zinc content.
The preparation method of the radar wave absorbent of the comparative example comprises the following steps:
(1) nickel oxide, zinc oxide, ferrous oxide and copper oxide are mixed according to the mass ratio of 25: 7: 67: 1, mixing, adding deionized water, and performing wet ball milling for 5 hours to obtain ball milling slurry;
(2) spray drying the ball-milling slurry obtained in the step (1) to obtain a dry mixture;
(3) heating the dried mixture obtained in the step (2) to 1270 ℃, sintering and preserving heat for 2h, and then cooling to room temperature to obtain a sintered material;
(4) vibrating, grinding and crushing the sintered material obtained in the step (3), and sieving the crushed material with a 160-mesh sieve to obtain ferrite powder;
(5) carrying out alcohol ball milling on the Fe-Si-Al powder for 2h on a planetary ball mill, drying to obtain Fe-Si-Al flaky powder, and testing the average particle size to be 20 um;
(6) and (6) mixing the Fe-Si-Al flaky powder obtained in the step (5) with graphene according to a mass ratio of 8: 1, mixing and uniformly stirring to obtain a mixture;
(7) mixing the ferrite powder obtained in the step (4) with the mixture obtained in the step (6) according to the ratio of 91: 9, and uniformly stirring to obtain the radar absorbent.
TABLE 1 detection results of wave absorbing properties of radar wave absorbers of examples 1 to 3 and comparative examples 1 to 3
Claims (10)
1. The low-frequency radar absorbent with high weather resistance is characterized by comprising a main component of nickel-zinc ferrite, a small amount of doped ferrum-silicon-aluminum and graphene, wherein the content of the nickel-zinc ferrite is more than or equal to 90wt%, the content of the ferrum-silicon-aluminum is 6-8 wt%, and the content of the graphene is 1-2 wt%.
2. The low-frequency radar absorbent with high weather resistance as claimed in claim 1, wherein the nickel-zinc ferrite is prepared by mixing and sintering raw materials of nickel oxide, zinc oxide and ferrous oxide as main bodies and copper oxide as a sintering aid.
3. The low-frequency radar absorbent with high weather resistance according to claim 1 or 2, wherein the sendust is a flaky sendust powder treated by a special process, i.e. the sendust powder is ball-milled by alcohol to a flaky sendust powder with a particle size of 20um ± 10 um.
4. The low-frequency radar absorbent with high weather resistance as claimed in any one of claims 1 to 3, wherein the weight ratio of iron, silicon and aluminum in the sendust is 80-90: 5-10.
5. The low-frequency radar absorbent with high weather resistance as claimed in claim 2, wherein the raw material comprises 10-20 wt% of nickel oxide, 10-20 wt% of zinc oxide, 60-70 wt% of ferrous oxide and 1-2 wt% of auxiliary agent copper oxide.
6. A method for preparing the weather-resistant low-frequency radar absorbent according to any one of claims 1 to 5, comprising the steps of:
(1) mixing raw materials of nickel oxide, zinc oxide and ferrous oxide, and adding an auxiliary agent of copper oxide to obtain a mixture; performing wet ball milling on the mixture to obtain ball milling slurry;
(2) spray drying the ball-milling slurry obtained in the step (1) to obtain a dry mixture;
(3) sintering the dry mixture obtained in the step (2), and cooling to obtain a sintered wave absorbing agent material;
(4) finely grinding the sintered wave absorbing agent material obtained in the step (3), performing vibration grinding and crushing, and sieving to obtain a ferrite wave absorbing material;
(5) and (4) mixing the ferrite wave-absorbing material obtained in the step (4) with the specially-treated Fe-Si-Al and graphene, and uniformly stirring to obtain the low-frequency radar absorbent with strong weather resistance.
7. The preparation method of the low-frequency radar absorbent with strong weather resistance according to claim 6, characterized in that in the step (1), the wet ball milling time is 1-3 h, and the mass ratio of a mixture in ball milling to steel balls to water is 1-2: 8-15: 1-2.
8. The preparation method of the low-frequency radar absorbent with strong weather resistance according to claim 6 or 7, wherein in the step (3), the sintering temperature is 1200-1300 ℃; and the sintering heat preservation time is 1-3 h.
9. The method for preparing a low-frequency radar absorbent with strong weather resistance according to any one of claims 6 to 8, wherein in the step (4), the mesh number of the sieved screen is 100 to 200 meshes.
10. The method for preparing the low-frequency radar absorbent with strong weather resistance according to any one of claims 6 to 9, wherein in the step (5), the specially treated sendust is a flake sendust with a particle size of 20um ± 10um obtained by alcohol ball milling.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115521710A (en) * | 2022-09-28 | 2022-12-27 | 湖南航天磁电有限责任公司 | Low-frequency wave-absorbing coating and preparation method thereof |
| CN115521139A (en) * | 2022-10-18 | 2022-12-27 | 北京无线电测量研究所 | Graphene-garnet type ferrite composite material, preparation and application |
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2022
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115521710A (en) * | 2022-09-28 | 2022-12-27 | 湖南航天磁电有限责任公司 | Low-frequency wave-absorbing coating and preparation method thereof |
| CN115521139A (en) * | 2022-10-18 | 2022-12-27 | 北京无线电测量研究所 | Graphene-garnet type ferrite composite material, preparation and application |
| CN115521139B (en) * | 2022-10-18 | 2023-10-20 | 北京无线电测量研究所 | Graphene-garnet type ferrite composite material, preparation and application |
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