Doped magnetically soft alloy material with high-temperature oxidation resistance and wave absorbing performance as well as preparation method and application of doped magnetically soft alloy material

Abstract

The invention relates to a doped magnetically soft alloy material with high-temperature oxidation resistance and wave absorbing performance and a preparation method and application thereof, the chemical formula of the magnetically soft alloy material is Y < 2-x > Me < x > Fe < 17 > N < 3-delta >, Me is a titanium group element, x is more than or equal to 0.1 and less than or equal to 1, and delta is more than or equal to 0 and less than or equal to 1. Rare earth Y2Fe17 is selected as a basic alloy system, a titanium group element is doped to replace a Y atom, and the titanium group element with a specific content is doped, so that the high-temperature phase stability and the oxidation resistance of the alloy are remarkably improved, and meanwhile, the high-frequency electromagnetic wave absorption capacity of the alloy is maintained or improved; collaborative optimization of oxidation resistance, electromagnetic wave-absorbing performance and structural stability is realized, and extremely high practical value and application prospect are achieved.

Description

Technical Field

[0001] This invention relates to the field of functional metal materials technology, and in particular to a doped soft magnetic alloy material with high-temperature oxidation resistance and wave absorption properties, its preparation method and application. Background Technology

[0002] Currently, Y2Fe 17 Type 2:17 phase alloys have broad application potential in magnetic materials and microwave absorbing materials due to their excellent magnetic properties. However, their application in high-temperature environments is limited by problems such as a loose oxide layer and easy decomposition. Traditional methods such as surface coating and composite doping often lead to a decrease in magnetic or microwave absorption properties while improving oxidation resistance. Therefore, there is an urgent need for a method to achieve a synergistic improvement in oxidation resistance and microwave absorption properties at the intrinsic structural level of the material.

[0003] Existing technology CN120432294A discloses a magnetic powder core and its preparation method. The preparation method of the magnetic powder core includes four steps: preparing gas-atomized iron-silicon soft magnetic powder, insulating coating, pressing and molding, and annealing heat treatment. Among them, the iron-silicon soft magnetic powder is prepared by gas atomization process, which gives the iron-silicon soft magnetic powder excellent soft magnetic properties.

[0004] Existing technology CN120485661A discloses a corrosion-resistant magnetic temperature compensation alloy and its preparation method, belonging to the field of soft magnetic materials. Al, Ti, La, and B are added as pre-alloyed AlTiLaB alloy powder. This magnetic temperature compensation alloy is produced through melting, refining, adding AlTiLaB alloy powder, ultrasonic casting, and heat treatment. This alloy improves corrosion resistance, enhances magnetization, and reduces coercivity through multi-element synergy, making it suitable for high-power electromagnetic equipment in complex corrosive environments, exhibiting good performance stability and consistency.

[0005] Prior art CN120452982A discloses a low-loss, high-DC-bias soft magnetic composite material, its preparation method, and its applications. This low-loss, high-DC-bias soft magnetic composite material is composed of nano-titanium dioxide and iron-silicon-aluminum alloy powder. The nano-titanium dioxide and iron-silicon-aluminum alloy powder are combined in a core-shell structure, with the iron-silicon-aluminum alloy powder forming the core and the nano-titanium dioxide shell covering the outside. This low-loss, high-DC-bias soft magnetic composite material exhibits high DC-bias performance, high permeability, and low high-frequency loss. Furthermore, the preparation process of this soft magnetic composite material is simple, the prepared material has stable properties, and it possesses very high DC-bias performance, making it suitable for industrial mass production.

[0006] The prior art CN120505030A discloses a corrosion-resistant magnetic shielding coating material and its preparation method. It mainly modifies the coating of nickel ferrite and controls the key electromagnetic parameters and corrosion resistance of the material by controlling the coating of the corrosion-resistant medium, so as to obtain the relatively optimal comprehensive performance. On this basis, the modified nickel ferrite is compounded with polyurethane resin to construct a corrosion-resistant magnetic shielding coating to achieve the purpose of magnetic protection in harsh corrosive environments.

[0007] Therefore, providing a doped alloy material with high-temperature oxidation resistance and microwave absorption properties, as well as its preparation method and application, has become an urgent problem to be solved. Summary of the Invention

[0008] To address the aforementioned technical problems, this invention provides a doped alloy material with high-temperature oxidation resistance and microwave absorption properties, its preparation method, and its applications. The doped alloy material of this invention, by doping with a specific amount of titanium group elements, significantly improves its high-temperature phase stability and oxidation resistance, while maintaining or enhancing its high-frequency electromagnetic wave absorption capability, thus solving the problem of Y2Fe in the prior art. 17 The alloy materials suffer from severe oxidation, structural instability, and degradation of microwave absorption performance under high-temperature environments.

[0009] To achieve this objective, the present invention adopts the following technical solution:

[0010] In a first aspect, the present invention provides a doped soft magnetic alloy material possessing high-temperature oxidation resistance and microwave absorption properties, wherein the chemical formula of the soft magnetic alloy material is: Y 2-x Me x Fe 17 N 3-δ ;

[0011] Me is a group element of titanium, with the following conditions: 0.1≤x≤1 and 0≤δ≤1.

[0012] In the chemical formula of the soft magnetic alloy material, 0.1≤x≤1, for example, can be 0.1, 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9 or 1, and 0≤δ≤1, for example, can be 0, 0.2, 0.4, 0.6, 0.8 or 1, but is not limited to the listed values. Other unlisted values ​​within the above range are also applicable.

[0013] The doped soft magnetic alloy material with high-temperature oxidation resistance and wave absorption properties provided by this invention uses Y2Fe 17Based on the alloy system, some Y atoms are replaced by titanium group elements. Titanium group elements have a strong affinity for oxygen and can preferentially react with oxygen at high temperatures after doping, forming a dense oxide layer on the alloy surface. These oxides have the characteristics of high melting point and low oxygen diffusion coefficient, which can effectively block the inward diffusion of oxygen and the outward migration of iron elements, significantly improving its high-temperature phase stability and oxidation resistance, while maintaining or improving its high-frequency electromagnetic wave absorption capability.

[0014] As a preferred technical solution of the present invention, the titanium group elements include any one or a combination of at least two of Ti, Zr or Hf, wherein typical but non-limiting combinations include: the combination of Ti and Zr, the combination of Ti and Hf, and the combination of Zr and Hf.

[0015] As a preferred technical solution of the present invention, in the chemical formula of the soft magnetic alloy material, 0.1≤x≤0.5, for example, can be 0.1, 0.2, 0.3, 0.4 or 0.5, and 0.2≤δ≤0.4, for example, can be 0.2, 0.25, 0.3, 0.35 or 0.4, but is not limited to the listed values. Other unlisted values ​​within the above range are also applicable.

[0016] In a second aspect, the present invention provides a method for preparing a soft magnetic alloy material, the method comprising:

[0017] (1) According to Y 2-x Me x Fe 17 N 3-δ The raw materials are prepared according to the stoichiometric ratio to obtain a mixture, wherein 0.1≤x≤1 and 0≤δ≤1;

[0018] (2) The mixture is subjected to electric arc melting and then ball milling to obtain soft magnetic alloy powder;

[0019] (3) The soft magnetic alloy powder obtained in step (2) is subjected to gas nitriding to obtain the soft magnetic alloy material.

[0020] In this invention, titanium group elements are introduced into an iron-based soft magnetic alloy to maintain phase stability and oxidation resistance under high-temperature conditions. The titanium group elements are introduced through arc melting, completely melting the mixed elemental metal powders to achieve homogeneous alloying. After ball milling, soft magnetic alloy powder is obtained. Through nitriding, nitrogen atoms diffuse into the alloy surface and gradually migrate inwards, resulting in strong bonding between Ti and N, forming fine, dispersed TiN nanoparticles or Ti-rich nitride phases. The remaining N is dissolved in Y₂Fe. 17 In the crystal lattice, interstitial nitrogen atoms are formed between Fe atoms. These nitrides and interstitial nitrogen atoms significantly change the electromagnetic properties of the material, allowing more electromagnetic waves to enter the interior of the material instead of being reflected by the surface.

[0021] As a preferred technical solution of the present invention, the raw materials include titanium group metals, yttrium, and ferrous iron.

[0022] Preferably, the titanium group metal element includes any one or a combination of at least two of Ti, Zr, or Hf, wherein typical but non-limiting combinations include: Ti and Zr, Ti and Hf, and Zr and Hf.

[0023] As a preferred technical solution of the present invention, the current of the electric arc melting in step (2) is 50-150A, for example, it can be 50A, 60A, 70A, 80A, 90A, 100A, 110A, 120A, 130A, 140A or 150A, but it is not limited to the listed values. Other unlisted values ​​within the above range are also applicable.

[0024] When the current of the arc melting process is too low, the melting is insufficient and the composition is severely uneven. High-melting-point metals such as Zr fail to melt completely and exist in the matrix as lumps or segregates, resulting in uneven nitriding reaction in subsequent nitriding operations. When the current of the arc melting process is too high, it will cause element volatilization, such as severe volatilization of Y, making its actual content far lower than the designed ratio, resulting in the inability to fully form the 2:17 phase and reducing the strength of the main phase used for microwave absorption.

[0025] Preferably, the current change rate of the electric arc melting in step (2) is 40-60A / min, for example, it can be 40A / min, 42A / min, 44A / min, 45A / min, 46A / min, 48A / min, 50A / min, 52A / min, 54A / min, 56A / min, 58A / min or 60A / min, but it is not limited to the listed values. Other unlisted values ​​within the above range are also applicable.

[0026] Preferably, the number of times the electric arc melting is performed in step (2) is 4-5 times, for example, 4 or 5 times.

[0027] Preferably, the time for each arc melting step (2) is 2-3 minutes, for example, 2 minutes, 2.2 minutes, 2.4 minutes, 2.6 minutes, 2.8 minutes or 3 minutes, but not limited to the listed values. Other unlisted values ​​within the above range are also applicable.

[0028] Preferably, the arc melting in step (2) is carried out in an inert atmosphere.

[0029] Preferably, the inert atmosphere comprises argon.

[0030] As a preferred technical solution of the present invention, the particle size of the soft magnetic alloy material in step (2) is 5-20μm, for example, it can be 5μm, 7μm, 10μm, 12μm, 14μm, 16μm, 18μm or 20μm, but it is not limited to the listed values. Other unlisted values ​​within the above range are also applicable.

[0031] As a preferred technical solution of the present invention, the temperature of the gas nitriding operation in step (3) is 450-500℃, for example, it can be 450℃, 460℃, 470℃, 480℃, 490℃ or 500℃, but it is not limited to the listed values. Other unlisted values ​​within the above range are also applicable.

[0032] When the nitriding operation temperature is too low, the nitrogen diffusion rate is slow, the nitrided layer is shallow, the nitrogen element does not fully enter the interior of the alloy, and there may be almost no nitrogen penetration into the core. The distance between iron atoms is not sufficiently increased, the negative ferromagnetic exchange increases, and the high-temperature oxidation resistance and microwave absorption performance decrease. When the nitriding operation temperature is too high, the excessive temperature will cause the sample to decompose and precipitate too much α-Fe phase, which is not conducive to impedance matching and leads to a decrease in microwave absorption performance.

[0033] As a preferred technical solution of the present invention, the gas pressure of the gas nitriding operation in step (3) is 0.05-0.15 MPa, for example, it can be 0.05 MPa, 0.06 MPa, 0.07 MPa, 0.08 MPa, 0.09 MPa, 1.0 MPa, 1.1 MPa, 1.2 MPa, 1.3 MPa, 1.4 MPa or 1.5 MPa, but is not limited to the listed values. Other unlisted values ​​within the above range are also applicable.

[0034] Thirdly, the present invention provides an application of a soft magnetic alloy material, which is applied in the fields of high-frequency communication devices, high-frequency electromagnetic wave absorbing materials, or high-frequency antenna technology.

[0035] Compared with the prior art, the present invention has at least the following beneficial effects:

[0036] (1) The chemical formula provided by this invention is Y 2-x Me x Fe 17 N 3-δ The doped soft magnetic alloy material with high temperature oxidation resistance and wave absorption properties is obtained by introducing titanium group elements into iron-based soft magnetic alloys, so that the alloy can maintain phase stability and oxidation resistance under high temperature conditions.

[0037] (2) The soft magnetic alloy material provided by the present invention has a minimum reflection loss of -57.43dB; the effective absorption bandwidth (EAB) in the X-band at high temperature reaches 4.2GHz, covering the entire X-band; the oxidation index n value is reduced to 0.5513, exhibiting self-passivation behavior;

[0038] (3) Compared with the undoped system, its oxide layer thickness is significantly reduced and the structure is dense. The phase structure does not change significantly after heat treatment, and the electromagnetic absorption performance also shows better high-temperature stability, making it suitable for microwave absorption applications in high-temperature environments. Attached Figure Description

[0039] Figure 1 Sample Y of Embodiment 1 of the present invention 1.5 Zr 0.5 Fe 17 N 3-δ Compared with Comparative Example 2 sample Y2Fe 17 XRD patterns before and after annealing at different temperatures;

[0040] Figure 2 These are the XRD patterns of the soft magnetic alloy materials of Examples 1-3 and Comparative Example 1 after annealing at 800℃.

[0041] Figure 3 These are the XRD patterns of the soft magnetic alloy materials of Examples 1-3 and Comparative Example 1 of this invention;

[0042] Figure 4 Sample Y of Embodiment 1 of the present invention 1.5 Zr 0.5 Fe 17 N 3-δ Compared with Comparative Example 2 sample Y2Fe 17 Cross-sectional view of the oxide layer and EDS analysis diagram. Detailed Implementation

[0043] The technical solution of the present invention will be further described below with reference to the accompanying drawings and specific embodiments. However, the following examples are merely simplified examples of the present invention and do not represent or limit the scope of protection of the present invention. The scope of protection of the present invention is determined by the claims.

[0044] Example 1

[0045] This embodiment provides a doped soft magnetic alloy material with high-temperature oxidation resistance and wave absorption properties. The chemical formula of the soft magnetic alloy material is Y. 1.5 Zr 0.5 Fe 17 N 3-δ , 0≤δ≤1.

[0046] This embodiment also provides a method for preparing the above-mentioned soft magnetic alloy material, the method comprising the following steps:

[0047] (1) According to the above Y 1.5 Zr 0.5 Fe 17 N 3-δ Y, Zr and Fe were prepared in stoichiometric ratios to obtain a mixture;

[0048] (2) The mixture is subjected to electric arc melting. During the melting process, the current is gradually increased from 50A to 120A at a rate of 50A / min. The mixture is kept at 120A for 2min and the melting is repeated 4 times. Then, the mixture is ball-milled to obtain soft magnetic alloy powder with an average particle size of 5μm.

[0049] (3) The soft magnetic alloy powder obtained in step (2) is subjected to gas nitriding operation at a temperature of 480°C and a pressure of 0.1 MPa to obtain the soft magnetic alloy material.

[0050] Example 2

[0051] This embodiment provides a doped soft magnetic alloy material with high-temperature oxidation resistance and wave absorption properties. The chemical formula of the soft magnetic alloy material is Y. 1.5 Hf 0.5 Fe 17 N 3-δ , 0≤δ≤1.

[0052] This embodiment also provides a method for preparing the above-mentioned soft magnetic alloy material, the method comprising the following steps:

[0053] (1) According to the above Y 1.5 Hf 0.5 Fe 17 N 3-δ The stoichiometric ratios of elemental Y, elemental Hf, and elemental Fe were used to prepare a mixture.

[0054] (2) The mixture is subjected to electric arc melting. During the melting process, the current is gradually increased from 50A to 120A at a rate of 50A / min. The current is maintained at 120A for 2min and the melting is repeated 4 times. Then, the mixture is ball-milled to obtain soft magnetic alloy powder with an average particle size of 8μm.

[0055] (3) The soft magnetic alloy powder obtained in step (2) is subjected to gas nitriding operation at a temperature of 480°C and a pressure of 0.08 MPa to obtain the soft magnetic alloy material.

[0056] Example 3

[0057] This embodiment provides a doped soft magnetic alloy material with high-temperature oxidation resistance and wave absorption properties. The chemical formula of the soft magnetic alloy material is Y. 1.5 (HfZr) 0.5 Fe 17 N 3-δ , 0≤δ≤1.

[0058] This embodiment also provides a method for preparing the above-mentioned soft magnetic alloy material, the method comprising the following steps:

[0059] (1) According to the above Y 1.5 (HfZr) 0.5 Fe 17 N 3-δ The stoichiometric ratios of elemental Y, elemental Hf, elemental Zr, and elemental Fe were used to prepare a mixture.

[0060] (2) The mixture is subjected to electric arc melting. During the melting process, the current is gradually increased from 50A to 120A at a rate of 50A / min. The mixture is kept at 120A for 2min and the melting is repeated 4 times. Then, the mixture is ball-milled to obtain soft magnetic alloy powder with an average particle size of 10μm.

[0061] (3) The soft magnetic alloy powder obtained in step (2) is subjected to gas nitriding operation at a temperature of 480°C and a pressure of 0.14 MPa to obtain the soft magnetic alloy material.

[0062] Depend on Figure 1 It can be seen that the alloy in Comparative Example 2 showed significant changes in diffraction peaks after high-temperature treatment, indicating that its main phase underwent some decomposition; while the Zr-doped sample in Example 1 showed almost no change in the position and relative intensity of its diffraction peaks after heating, proving that its crystal structure was stable and no obvious decomposition phenomenon was observed; Figure 2 , 3 It can be seen that Examples 1-3 all have good phase stability, with Example 3 > Example 2 > Example 1 in terms of phase stability, indicating that the soft magnetic alloy has strong high-temperature stability.

[0063] Example 4

[0064] This embodiment provides a doped soft magnetic alloy material with high-temperature oxidation resistance and wave absorption properties. The chemical formula of the soft magnetic alloy material is Y. 1.9 Zr 0.1 Fe 17 N 3-δ , 0≤δ≤1.

[0065] This embodiment also provides a method for preparing the above-mentioned soft magnetic alloy material, the method comprising the following steps:

[0066] (1) According to the above Y 1.9 Zr 0.1 Fe 17 N 3-δ Y, Zr and Fe were prepared in stoichiometric ratios to obtain a mixture;

[0067] (2) The mixture is subjected to electric arc melting. During the melting process, the current is gradually increased from 50A to 80A at a rate of 40A / min. It is kept at 120A for 2min and the melting is repeated 4 times. Then, it is ball-milled to obtain soft magnetic alloy powder with an average particle size of 5μm.

[0068] (3) The soft magnetic alloy powder obtained in step (2) is subjected to gas nitriding operation at a temperature of 450°C and a pressure of 0.15 MPa to obtain the soft magnetic alloy material.

[0069] Example 5

[0070] This embodiment provides a doped soft magnetic alloy material with high-temperature oxidation resistance and wave absorption properties. The chemical formula of the soft magnetic alloy material is YZrFe. 17 N 3-δ , 0≤δ≤1.

[0071] This embodiment also provides a method for preparing the above-mentioned soft magnetic alloy material, the method comprising the following steps:

[0072] (1) According to the above YZrFe 17 N 3-δ Y, Zr and Fe were prepared in stoichiometric ratios to obtain a mixture;

[0073] (2) The mixture is subjected to electric arc melting. During the melting process, the current is gradually increased from 50A to 150A at a rate of 60A / min. It is kept at 120A for 2min and the melting is repeated 4 times. Then, it is ball-milled to obtain soft magnetic alloy powder with an average particle size of 20μm.

[0074] (3) The soft magnetic alloy powder obtained in step (2) is subjected to gas nitriding operation at a temperature of 500°C and a pressure of 0.05 MPa to obtain the soft magnetic alloy material.

[0075] Example 6

[0076] The difference between this embodiment and embodiment 1 is that the current for arc melting in step (2) is 30A.

[0077] The remaining preparation methods and parameters are consistent with those in Example 1.

[0078] Example 7

[0079] The difference between this embodiment and embodiment 1 is that the current for arc melting in step (2) is 170A.

[0080] The remaining preparation methods and parameters are consistent with those in Example 1.

[0081] Example 8

[0082] The difference between this embodiment and embodiment 1 is that the temperature of the gas nitriding operation in step (3) is 400°C.

[0083] The remaining preparation methods and parameters are consistent with those in Example 1.

[0084] Example 9

[0085] The difference between this embodiment and embodiment 1 is that the temperature of the gas nitriding operation in step (3) is 550°C.

[0086] The remaining preparation methods and parameters are consistent with those in Example 1.

[0087] Comparative Example 1

[0088] This comparative example provides an undoped soft magnetic alloy material with the chemical formula Y₂Fe. 17 N 3-δ x is 0, 0≤δ≤1, that is, no Zr element is added in step (1).

[0089] The remaining preparation methods and parameters are consistent with those in Example 1.

[0090] Comparative Example 2

[0091] This comparative example provides an undoped, non-nitrided alloy material, the chemical formula of which is Y₂Fe. 17 x is 0, meaning that no Zr element is added in step (1).

[0092] In its preparation method, except that step (1) only adds elemental Y and elemental Fe in proportion and step (3) does not perform gas nitriding operation, the rest are the same as in Example 1.

[0093] Comparative Example 3

[0094] This comparative example provides a doped alloy material Y 1.5 Zr 0.5 Fe 17 The only difference from Example 1 is that, except that step (3) of the preparation method does not involve gas nitriding, the rest is the same as Example 1.

[0095] Comparative Example 4

[0096] This comparative example provides a doped alloy material Y 1.5 Zr 0.5 Fe 17 N 3-δ The only difference from Example 1 is that -1≤δ<0, and the amount of nitriding is greater.

[0097] Comparative Example 5

[0098] This comparative example provides a doped alloy material Y 0.5 Zr 1.5 Fe 17 N 3-δ The only difference from Example 1 is that x is 1.5.

[0099] The remaining preparation methods and parameters are consistent with those in Example 1.

[0100] Comparative Example 6

[0101] This comparative example provides a doped alloy material Y 1.5 Ta 0.5 Fe 17 N 3-δ The only difference from Example 1 is that Zr is replaced with Ta.

[0102] The remaining preparation methods and parameters are consistent with those in Example 1.

[0103] Performance testing:

[0104] (1) Phase stability test: The soft magnetic alloy materials obtained in Examples 1-9 and Comparative Examples 1-6 were annealed at 400-800℃ and tested using an X-ray diffractometer (XRD);

[0105] (2) Antioxidant performance test: The mass change of the sample soft magnetic alloy material was tested using a simultaneous thermal analyzer (TG) in an air atmosphere at 500℃;

[0106] The cross-sectional structure after 50 hours of high-temperature oxidation was observed using scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS) to obtain the thickness and density of the oxide layer of the soft magnetic alloy material sample.

[0107] (3) Electromagnetic performance test: After the soft magnetic alloy material sample was plasma ball milled for 8 hours, it was prepared into a sample sheet with high temperature glue; the complex permittivity, complex permeability and reflection loss were tested at a frequency of 6 GHz; its high temperature in-situ absorption performance was tested in the range of 25-400℃ to obtain the effective absorption bandwidth (EAB) of the X band.

[0108] The results of the antioxidant performance test are shown in Table 1.

[0109] Table 1

[0110]

[0111] The electromagnetic performance test results are shown in Tables 2 and 3.

[0112] Table 2

[0113]

[0114] Table 3

[0115]

[0116] The test results show that:

[0117] (1) As can be seen from Examples 1 to 5, the reflection loss of the sample after doping can be as low as -57.43dB; the effective absorption bandwidth (EAB) in the X-band at high temperature reaches 4.2GHz, covering the entire X-band; the reflection loss at 400℃ can reach 31.45; the oxidation index n value is reduced to 0.5513, showing self-passivation behavior and effectively forming a dense oxide layer.

[0118] (2) As can be seen from the combined examples 1 and 6 and 7, when the current of the arc melting of the present invention is too low, the melting is insufficient and the composition is seriously uneven. High melting point metals such as Zr cannot be completely melted and exist in the matrix in the form of lumps or segregates, which leads to uneven nitriding reaction in the subsequent nitriding operation. When the current of the arc melting is too high, it will cause element volatilization, such as serious volatilization of Y, which makes its actual content far lower than the design ratio, resulting in the inability to fully form the 2:17 phase and reducing the strength of the main phase used for wave absorption capability.

[0119] (3) As can be seen from the combined examples 1 and 8 and 9, when the nitriding operation temperature of the present invention is too low, the nitrogen diffusion rate is slow, the nitrided layer is shallow, the nitrogen element does not fully enter the interior of the alloy, the core may have almost no nitrogen penetration, the distance between iron atoms is not sufficiently increased, the negative ferromagnetic exchange increases, and the high-temperature oxidation resistance and microwave absorption performance decrease. When the nitriding operation temperature is too high, the excessive temperature will cause the sample to decompose and precipitate too much α-Fe phase, which is not conducive to impedance matching and leads to a decrease in microwave absorption performance.

[0120] (4) As can be seen from Example 1 and Comparative Example 1, the high-temperature oxidation resistance of the present invention is significantly reduced when it is not doped with titanium group elements.

[0121] (5) As can be seen from Example 1 and Comparative Example 2, Y2Fe 17 It suffers from severe oxidation, structural instability, and degradation of microwave absorption performance under high-temperature conditions. Figure 1 It can be seen that Y2Fe 17 The alloy exhibited significant changes in diffraction peaks after high-temperature treatment, indicating that its main phase underwent a certain degree of decomposition; from Figure 4 The microstructure shows that the oxide layer formed after oxidation of the undoped sample is about 5 μm thick, while the oxide layer of the Zr-doped alloy prepared in Example 1 is significantly thinner, with a thickness of about 3 μm, and exhibits a more compact structure, showing stronger oxidation resistance.

[0122] (6) As can be seen from Example 1 and Comparative Example 3, when nitriding is not performed, the interstitial N atoms are not introduced, resulting in a smaller interatomic spacing of Fe atoms and an increase in negative ferromagnetic exchange between Fe atoms, which leads to a decrease in the soft magnetic properties of the sample and a reduction in magnetic loss. At the same time, since some metal nitrides are not introduced, dipole polarization between different phases cannot be generated, reducing properties such as dielectric loss.

[0123] (7) As can be seen from Example 1 and Comparative Examples 4 and 5, when x is 1.5, the amount of 2:17 phase is insufficient due to the excessive amount of Zr element, resulting in a decrease in the content of the main absorbing phase and the segregation of excessive ZrFe2 phase, which ultimately leads to a decrease in absorbing performance and high-temperature performance. Compared with Comparative Example 4, it can be seen that when the amount of nitriding is greater, some titanium group elements will combine with nitrogen elements to form phases such as ZrN, which reduces the 2:17 phase, reduces the overall soft magnetic properties, and leads to a decrease in absorbing ability.

[0124] (8) As can be seen from Example 1 and Comparative Example 6, if Zr is replaced with Ta, the Ta element is difficult to enter Y2Fe. 17 In the crystal lattice, segregation is easily generated, resulting in the sample exhibiting a mixed phase overall. This also reduces the content of the 2:17 phase, decreases the overall soft magnetic properties, and leads to a decline in wave absorption capability.

[0125] In summary, this invention introduces titanium group elements into iron-based soft magnetic alloys, enabling the alloys to maintain phase stability and oxidation resistance under high-temperature conditions. Compared with the undoped system, its oxide layer thickness is significantly reduced and the structure is denser. The phase structure does not change significantly after heat treatment, and the electromagnetic absorption performance also exhibits superior high-temperature stability, making it suitable for microwave absorption applications in high-temperature environments.

[0126] The applicant declares that the above description is only a specific embodiment of the present invention, but the protection scope of the present invention is not limited thereto. Those skilled in the art should understand that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope disclosed in the present invention fall within the protection and disclosure scope of the present invention.

Claims

1. A doped soft magnetic alloy material with high-temperature oxidation resistance and wave absorption performance, characterized in that, The soft magnetic alloy material has a chemical formula Y 2-x Me x Fe 17 N 3-δ ; wherein Me is a titanium group element, 0.1≤x≤1, and 0≤δ≤1.

2. The soft magnetic alloy material according to claim 1, characterized by The titanium group element includes any one or a combination of at least two of Ti, Zr or Hf.

3. The soft magnetic alloy material according to claim 1 or 2, characterized in that, In the chemical formula of the soft magnetic alloy material, 0.1≤x≤0.5 and 0.2≤δ≤0.

4.

4. A method of producing a soft magnetic alloy material according to any one of claims 1 to 3, characterized by, The preparation method comprises: (1) according to Y 2-x Me x Fe 17 N 3-δ The stoichiometric ratio of the raw materials is configured to obtain a mixture, wherein 0.1≤x≤1, 0≤δ≤1. (2) arc melting the mixture, and then ball milling to obtain a soft magnetic alloy powder; (3) performing a gas nitriding operation on the soft magnetic alloy powder of step (2) to obtain the soft magnetic alloy material.

5. The preparation method according to claim 4, characterized in that, The raw material includes titanium group metal elements, Y elements and Fe elements. Preferably, the titanium group metal elements include any one or a combination of at least two of Ti elements, Zr elements or Hf elements.

6. The production method according to claim 4 or 5, characterized by, The current of the arc melting of step (2) is 50-150 A. Preferably, the current variation rate of the arc melting of step (2) is 40-60 A / min. Preferably, the number of times of the arc melting of step (2) is 4-5 times. Preferably, the time of each arc melting of step (2) is independently 2-3 min. Preferably, the arc melting of step (2) is performed in an inert atmosphere. Preferably, the inert atmosphere includes argon.

7. The method of any one of claims 4-6, wherein, The particle size of the soft magnetic alloy material of step (2) is 5-20 μm.

8. The method of any one of claims 4-7, wherein, The temperature of the gas nitriding operation of step (3) is 450-500 °C.

9. The method of any one of claims 4-8, wherein, The gas pressure of the gas nitriding operation of step (3) is 0.05-0.15 MPa.

10. Use of a soft magnetic alloy material according to any one of claims 1 to 3, characterized in that The soft magnetic alloy material is applied in the technical field of high-frequency communication devices, high-frequency electromagnetic wave absorbing materials or high-frequency antenna technology.

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