CN109317689B - Permalloy magnetic nano wave-absorbing material with core-shell structure and preparation method thereof - Google Patents

Permalloy magnetic nano wave-absorbing material with core-shell structure and preparation method thereof Download PDF

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CN109317689B
CN109317689B CN201811293934.3A CN201811293934A CN109317689B CN 109317689 B CN109317689 B CN 109317689B CN 201811293934 A CN201811293934 A CN 201811293934A CN 109317689 B CN109317689 B CN 109317689B
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王磊
钟明龙
钟震晨
谭秋兰
熊厚冬
张莉丽
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Jiangxi University of Science and Technology
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Abstract

The invention discloses a permalloy magnetic nano wave-absorbing material with a core-shell structure and a preparation method thereof, wherein the stoichiometric ratio of the molecular formula of an inner core of the wave-absorbing material is mass percent, wherein the stoichiometric ratio is 79-82% of Ni, 11-16% of Fe and 2-10% of Mo. The preparation method comprises the following steps: s1, batching: taking Ni, Fe and Mo simple substances with the purity of more than or equal to 99.9 percent as raw materials, and mixing the raw materials according to mass percent; s2, smelting; s3, homogenizing; s4, preparing nanometer powder; s5, passivating; s6, oxidation heat treatment: and (4) putting the permalloy magnetic nano powder obtained in the step (S5) into an industrial atmosphere sintering furnace, introducing dry air, and preserving the heat for 0.5-3.5 hours at the temperature of 230-270 ℃. The permalloy magnetic nano wave-absorbing material with the core-shell structure prepared by the invention has the advantages of high magnetic conductivity of permalloy, size effect of nano materials and core-shell structure, and effectively improves the wave-absorbing performance of the material.

Description

Permalloy magnetic nano wave-absorbing material with core-shell structure and preparation method thereof
Technical Field
The invention belongs to the field of magnetic nano wave-absorbing materials, and particularly relates to a permalloy magnetic nano wave-absorbing material with a core-shell structure and a preparation method thereof.
Background
The wave-absorbing material has important application value in civil use and military use. In military applications, the wave-absorbing material is also called stealth material and can be widely applied to various military products, such as stealth airplanes, stealth naval vessels and the like; in the civil aspect, the rapidly developed electronic technology brings great electromagnetic pollution to human life, and the absorption characteristic of the wave-absorbing material to electromagnetic waves can effectively solve the problem of electromagnetic pollution.
From the loss mechanism, the wave-absorbing materials are mainly divided into magnetic wave-absorbing materials and dielectric wave-absorbing materials. At present, the magnetic wave-absorbing material mainly comprises ferrite magnetic wave-absorbing material, metal micro powder magnetic wave-absorbing material, polycrystalline metal fiber magnetic wave-absorbing material, nano magnetic wave-absorbing material and the like. The unique structure of the nano material enables the nano material to have quantum effect, small-size effect, interface effect and the like, so that the nano magnetic wave-absorbing material not only has better electromagnetic wave absorption characteristic, but also has the advantages of thin coating, wide effective absorption frequency band and the like.
Because of its high magnetic permeability, permalloy is widely used in the field of electronic components. Since high permeability is generally associated with high magnetic loss characteristics, there are increasing reports on the wave absorption properties of permalloy and applications thereof as shielding materials. However, the permalloy magnetic powder is prepared by adopting a mechanical alloy ball milling method, and the purpose of improving the wave absorption performance is achieved by changing the form of the powder. In the research aspect of permalloy composite materials, researchers try to adopt the process methods of graphene compounding, carbon nanotube compounding and the like; or permalloy is used as an inner core, and oxide is deposited outside the permalloy to be used as a shell to form a core-shell structure, so that the wave absorbing performance of the material is improved.
In summary, the permalloy magnetic nano powder with high magnetic permeability is used as an inner core, and a nano composite structure with the magnetic alloy inner core wrapped by oxides is formed by adopting an oxidation heat treatment method. The material has the advantages of high permeability of permalloy, the advantage of the size effect of a nano material and the characteristic of a core-shell structure, and comprehensively considers multiple factors to improve the wave absorbing performance of the material. And because an oxide layer is formed on the outer surface of the material after oxidation heat treatment, the stability and corrosion resistance of the material are improved, and the material is more beneficial to the actual application and the industrial production requirement, so that the permalloy magnetic nano wave-absorbing material with the core-shell structure has better development prospect and application value.
Disclosure of Invention
The invention provides a permalloy magnetic nano wave-absorbing material with a core-shell structure and a preparation method thereof. Firstly, permalloy magnetic nano particles are prepared by adopting a plasma nano powder preparation technology, and then the magnetic nano particles with the core-shell structure are prepared by adopting an oxidation heat treatment method. The wave-absorbing material prepared by the process method has the advantages of high magnetic conductivity of the permalloy, size effect of the nano material and core-shell structure, and greatly improves the wave-absorbing performance of the material.
In order to achieve the purpose, the technical scheme of the invention is as follows:
the permalloy magnetic nano wave-absorbing material with the core-shell structure is characterized in that the stoichiometric ratio of the core molecular formula of the permalloy magnetic nano wave-absorbing material with the core-shell structure is mass percent, wherein the mass percent of Ni is 79-82, the mass percent of Fe is 11-16, the mass percent of Mo is 2-10, and the sum of the mass percent of the Ni and the mass percent of Fe is 100.
Further, in the above technical scheme, the stoichiometric ratio of the core molecular formula of the permalloy magnetic nano wave-absorbing material with the core-shell structure is mass percent, wherein Ni is 82, Fe is 16, and Mo is 2.
Further, the invention provides a preparation method of the permalloy magnetic nano wave-absorbing material with the core-shell structure, which comprises the following steps:
s1, batching: taking Ni, Fe and Mo simple substances with the purity of more than or equal to 99.9% as raw materials, and mixing the raw materials according to the mass percentages of Ni 79-82, Fe 11-16 and Mo 2-10;
s2, smelting: smelting the material prepared in the step S1 in a high-vacuum medium-frequency induction furnace under the protection of argon;
s3, homogenization treatment: annealing the ingot obtained in the step S2 at 1000-1100 ℃ for 24-48 hours under a vacuum condition;
s4, preparing nano powder: preparing the nano powder from the ingot casting obtained in the step S3 in a direct current arc plasma nano powder preparation system, wherein the adopted atmosphere is argon and hydrogen, and the volume ratio of the hydrogen is 20-40%;
s5, passivation treatment: after the nanometer powder obtained in the step S4 is deposited, pumping the cavity of the direct current arc plasma nanometer powder preparation system to a vacuum state, filling argon until the air pressure reaches 50kPa, then filling dry air every 30 minutes, and increasing the air pressure by 5kPa each time until one atmospheric pressure is reached; after a period of passivation, collecting and obtaining permalloy magnetic nano powder;
s6, oxidation heat treatment: and (4) putting the permalloy magnetic nano powder obtained in the step (S5) into an industrial atmosphere sintering furnace, introducing dry air, and preserving the heat for 0.5-3.5 hours at the temperature of 230-270 ℃.
Further, in the above technical solution, the temperature of the homogenizing annealing in step S3 is 1050 ℃, and the heat preservation time is 36 hours.
Further, in the above technical solution, the atmosphere ratio used in the step S4 of preparing the nano-powder is 30% of hydrogen.
Further, in the above technical solution, the arc stabilizing current adopted in the step S4 when preparing the nano powder in the dc arc plasma nano powder preparation system is 60 to 100A.
Further, in the above technical solution, the time of the passivation treatment in the step S5 is 8-10 hours.
Furthermore, in the technical scheme, the temperature of the time for the oxidation heat treatment in the step S6 is 250 ℃, and the heat preservation time is 1.5 hours.
And (5) detecting the electromagnetic parameters of the permalloy magnetic nano wave-absorbing material with the core-shell structure obtained in the step S6 and calculating the reflectivity R.
Preferably, in the above technical solution, the detection method is: mixing permalloy magnetic nano powder with a core-shell structure and paraffin according to a mass ratio of 4: 1, and preparing coaxial samples with the outer diameter and the inner diameter of 7mm and 3mm respectively and the thickness of about 3 mm; the detection instrument is an AgilentPNA-L5230C vector network analyzer for measurement, the complex permeability and the complex dielectric constant of the sample on a 1-18GHz frequency band are respectively measured, and the reflectivity R of the single-layer wave-absorbing material is calculated and simulated by adopting the following formula.
Figure BDA0001850668820000041
In the formula (1), epsilonr、μrAnd d is the complex dielectric constant, complex permeability and thickness of the wave-absorbing material, f is the frequency of the electromagnetic wave, c is the propagation speed of the electromagnetic wave in vacuum, and j is an imaginary unit.
Compared with the prior art, the invention has the advantages and positive effects that:
the permalloy magnetic nano wave-absorbing material with the core-shell structure prepared by the invention has the advantages of high magnetic conductivity of permalloy, size effect of nano materials and core-shell structure, and effectively improves the wave-absorbing performance of the material. Because an oxidation layer is formed on the outer surface of the material after the oxidation heat treatment, the formation of the oxidation layer can bring two beneficial effects: on one hand, the impedance matching of the material is optimized; on the other hand, the stability and the corrosion resistance of the material are improved, and the practical application and the industrial production requirements are better met, so that the permalloy magnetic nano wave-absorbing material with the core-shell structure has better development prospect and application value.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a process flow diagram of the preparation method of the present invention.
FIG. 2 is an X-ray diffraction pattern of the permalloy magnetic nano wave-absorbing material in the invention.
FIG. 3 is a transmission electron microscope image of permalloy magnetic nano wave-absorbing material with a core-shell structure in the invention.
FIG. 4 is a comparison graph of the wave-absorbing properties of the permalloy magnetic nano material before and after oxidation heat treatment.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived from the embodiments of the present invention by a person skilled in the art without any creative effort, should be included in the protection scope of the present invention.
All experimental procedures used in the following examples are conventional unless otherwise specified. Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
Example 1
(1) The formula is as follows:
Ni82Fe16Mo2(percent by mass)
(2) The preparation method comprises the following steps:
step 1: taking Ni, Fe and Mo simple substances with the purity of more than or equal to 99.9 percent as raw materials, and mixing the raw materials according to the mass percentages of Ni82, Fe16 and Mo 2;
step 2: smelting the prepared materials in a high-vacuum medium-frequency induction furnace under the protection of argon;
and step 3: carrying out homogenizing annealing on the ingot obtained in the step 2 at 1050 ℃ for 36 hours under the vacuum condition;
and 4, step 4: and (3) preparing the ingot subjected to the homogenization thermal annealing in the step (3) into carbon-coated core-shell structured nano powder in a direct-current arc plasma nano powder preparation system. The atmosphere proportion is 80 percent of argon and 20 percent of hydrogen. The arc was first struck with a small current of 38A, and after the time had stabilized the current was gradually increased to 80A and the molten state of the sample was observed.
And 5: after the nanometer powder obtained in the step 4 is deposited, pumping the cavity of the direct current arc plasma nanometer powder preparation system to 10 degrees-1And in a low vacuum state of about kPa, argon is filled until the air pressure of the cavity reaches 50kPa, then dry air is filled every 30 minutes, and the air pressure is increased by 5kPa every time until the air pressure in the cavity reaches one atmosphere. After passivating for 9 hours, collecting and collecting the permalloy magnetic nano powder.
Step 6: and (3) putting the permalloy magnetic nano powder obtained in the step (5) into an industrial atmosphere sintering furnace, introducing dry air, and preserving heat for 1.5 hours at the temperature of 250 ℃.
(3) Detection and characterization:
characterizing the phase composition of the nano powder obtained in the step 6 by adopting a PANalytical-Empyrean type X-ray diffractometer;
characterizing the morphological characteristics 6 of the nano powder obtained in the step 6 by adopting a TecnaiG2-20 type transmission electron microscope;
the electromagnetic parameters of the material were measured and the reflectance calculated using an AgilentPNA-L5230C vector network analyzer. And (3) passivating the nano powder and paraffin according to the mass ratio of 4: 1, and then the outer diameter and the inner diameter were 7mm and 3mm, respectively, and the thickness was about 2.5 mm. And measuring the complex permeability and the complex dielectric constant of the sample in a 1-18GHz frequency band, wherein the reflectivity R of the single-layer wave-absorbing material is calculated and simulated by adopting the following formula.
Figure BDA0001850668820000061
In the formula (1), epsilonr、μrAnd d is the complex dielectric constant, complex permeability and thickness of the wave-absorbing material, f is the frequency of the electromagnetic wave, c is the propagation speed of the electromagnetic wave in vacuum, and j is an imaginary unit.
Example 2
(1) The formula is as follows:
Ni79Fe16Mo5(percent by mass)
(2) The preparation method comprises the following steps:
example 2 is different from example 1 in that the atmosphere ratio in step 4 of example 1 was adjusted to 70% argon and 30% hydrogen, and the other steps were the same as example 1.
Example 3
(1) The formula is as follows:
Ni79Fe14Mo7(percent by mass)
(2) The preparation method comprises the following steps:
example 3 is different from example 1 in that the atmosphere ratio in step 4 of example 1 was adjusted to 60% argon and 40% hydrogen, and the other steps were the same as example 1.
Example 4
(1) The formula is as follows:
Ni82Fe16Mo2(percent by mass)
(2) The preparation method comprises the following steps:
example 4 is different from example 1 in that the oxidation heat treatment temperature in step 6 of example 1 was adjusted to 230 ℃ and the holding time was adjusted to 3.5 hours. The other protocol was the same as in example 1.
Example 5
(1) The formula is as follows:
Ni82Fe16Mo2(percent by mass)
(2) The preparation method comprises the following steps:
example 5 is different from example 1 in that the oxidation heat treatment temperature in step 6 of example 1 was adjusted to 270 ℃ and the holding time was adjusted to 0.5 hour. The other protocol was the same as in example 1.
The experimental results are as follows:
the permalloy magnetic nano wave-absorbing material with the core-shell structure is prepared by adopting a plasma nano powder preparation technology and an oxidation heat treatment method, has the advantages of high magnetic conductivity of permalloy, size effect of nano materials and core-shell structure, and effectively improves the wave-absorbing performance of the material.
X-ray diffraction data of the resulting compounds were collected by a PANalytical-Empyrean type X-ray diffractometer, Cu target, as shown in figure 2. The main phase composition is FeNi3The phase, after oxidation heat treatment, appeared a small amount of NiO phase.
The samples were characterized for morphology by a transmission electron microscope model TecnaiG2-20, as shown in FIG. 3. As can be seen from fig. 3, after the oxidative heat treatment, the permalloy magnetic nanoparticles exhibited a distinct core-shell structure morphology.
The complex permeability and the complex dielectric constant of the material are tested by an AgilentPNA-L5230C vector network analyzer, and the reflectivity R of the single-layer wave-absorbing material is calculated and simulated by adopting the following formula.
Figure BDA0001850668820000081
In the formula (1), epsilonr、μrAnd d is the complex dielectric constant, complex permeability and thickness of the wave-absorbing material, f is the frequency of the electromagnetic wave, c is the propagation speed of the electromagnetic wave in vacuum, and j is an imaginary unit. The calculated reflectance ratio of the permalloy magnetic nano material before and after the oxidation heat treatment is shown in fig. 4. It can be seen from the figure that when the thickness d of the wave-absorbing coating is 2.5mm, the reflectivity before oxidation heat treatment is more than-10 dB; after oxidation heat treatment, the minimum value of the reflectivity of the permalloy magnetic nano material with the core-shell structure reaches-60.2 dB, the absorption bandwidth with the reflectivity less than-20 dB reaches 2.7GHz, and the wave-absorbing performance is obviously improved.

Claims (7)

1. A preparation method of permalloy magnetic nano wave-absorbing material with a core-shell structure is characterized by comprising the following steps: the method comprises the following steps:
s1, batching: taking Ni, Fe and Mo simple substances with the purity of more than or equal to 99.9% as raw materials, and mixing the raw materials according to the mass percentages of Ni 79-82, Fe 11-16 and Mo 2-10;
s2, smelting: smelting the material prepared in the step S1 in a high-vacuum medium-frequency induction furnace under the protection of argon;
s3, homogenization treatment: annealing the ingot obtained in the step S2 at 1000-1100 ℃ for 24-48 hours under a vacuum condition;
s4, preparing nano powder: preparing the nano powder from the ingot casting obtained in the step S3 in a direct current arc plasma nano powder preparation system, wherein the adopted atmosphere is argon and hydrogen, and the volume ratio of the hydrogen is 20-40%;
s5, passivation treatment: after the nanometer powder obtained in the step S4 is deposited, pumping the cavity of the direct current arc plasma nanometer powder preparation system to a vacuum state, filling argon until the air pressure reaches 50kPa, then filling dry air every 30 minutes, and increasing the air pressure by 5kPa each time until one atmospheric pressure is reached; after a period of passivation, collecting and obtaining permalloy magnetic nano powder;
s6, oxidation heat treatment: and (4) putting the permalloy magnetic nano powder obtained in the step (S5) into an industrial atmosphere sintering furnace, introducing dry air, and preserving the heat for 0.5-3.5 hours at the temperature of 230-270 ℃.
2. The method of claim 1, wherein: the temperature of the homogenization annealing in step S3 was 1050 ℃, and the heat retention time was 36 hours.
3. The method of claim 1, wherein: the atmosphere proportion adopted when preparing the nano-powder in the step S4 is 30 percent of hydrogen.
4. The method of claim 1, wherein: step S4 arc stabilizing current adopted when preparing the nano powder in the direct current arc plasma nano powder preparation system is 60-100A.
5. The method of claim 1, wherein: in the above technical solution, the time of the passivation treatment in the step S5 is 8-10 hours.
6. The method of claim 1, wherein: the temperature of the time of the oxidation heat treatment of the step S6 was 250 ℃, and the heat-retention time was 1.5 hours.
7. The permalloy magnetic nano wave-absorbing material with the core-shell structure prepared by the preparation method according to any one of claims 1 to 6, which is characterized in that: the permalloy magnetic nano wave-absorbing material with the core-shell structure has the core molecular formula with the stoichiometric ratio of mass percent, wherein Ni is 82, Fe is 16 and Mo is 2.
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