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CN112652436A - High-frequency soft magnetic material and preparation method thereof - Google Patents

High-frequency soft magnetic material and preparation method thereof Download PDF

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CN112652436A
CN112652436A CN202011485872.3A CN202011485872A CN112652436A CN 112652436 A CN112652436 A CN 112652436A CN 202011485872 A CN202011485872 A CN 202011485872A CN 112652436 A CN112652436 A CN 112652436A
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soft magnetic
magnetic material
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sputtering
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CN112652436B (en
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黎嘉威
刘西洋
贺爱娜
董亚强
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Ningbo Institute of Material Technology and Engineering of CAS
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
    • H01F1/147—Alloys characterised by their composition
    • H01F1/153—Amorphous metallic alloys, e.g. glassy metals
    • H01F1/15308—Amorphous metallic alloys, e.g. glassy metals based on Fe/Ni
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    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/0021—Reactive sputtering or evaporation
    • C23C14/0036—Reactive sputtering
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • C23C14/351—Sputtering by application of a magnetic field, e.g. magnetron sputtering using a magnetic field in close vicinity to the substrate
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    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
    • H01F1/147—Alloys characterised by their composition
    • H01F1/153—Amorphous metallic alloys, e.g. glassy metals
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Abstract

The invention discloses a high-frequency soft magnetic material with a chemical formula of Fe1‑x‑yAxByX is more than or equal to 15 and less than or equal to 45, y is more than or equal to 10 and less than or equal to 20, A is Co and/or Ni, B is nitride and has an oriented magnetic domain structure. The high-frequency soft magnetic material has a double-phase structure with magnetic nano-particles embedded in a nitride amorphous insulating matrix, and the grain size is less than 10 nm. The invention also provides a method for preparing the high-frequency soft magnetic material by combining reactive magnetron sputtering with an in-situ magnetic field. The high-frequency soft magnetic material provided by the invention has good high-frequency characteristics: the cut-off frequency is within the range of 1-10GHz, and the damping coefficient is less than or equal to 0.023; excellent soft magnetic properties: magnetic conductivity is more than or equal to 400(100MHz), saturation magnetization is more than or equal to 16kGs, and resistivity is more than or equal to 1000 mu omega cm, the coercive force is less than or equal to 100Oe, and the preparation method is simple and has lower cost.

Description

High-frequency soft magnetic material and preparation method thereof
Technical Field
The invention relates to the field of magnetic materials, in particular to a high-frequency soft magnetic material and a preparation method thereof.
Background
With the development of the electronic information industry, the development of high frequency, miniaturization, and integration of electronic components is becoming a inevitable direction. According to the international equipment route and the moore's law, the number of electronic components integrated on an integrated circuit doubles every two years, and meanwhile, the volume of electronic products tends to decline gradually, so that the miniaturization development of the electronic components is seriously restricted by the problems of electromagnetic interference and incapability of integrating the components. On the other hand, as the signal transmission rate is increased, the frequency of use of electronic components is further increased. Taking a mobile phone as an example, the working frequency bands of the traditional 2G mobile phones and the traditional 3G mobile phones respectively reach 900MHz and 2100MHz, the highest domestic frequency band of the fourth-generation mobile phones reaches 2635MHz, the maximum bandwidth reaches 20MHz, and the latest frequency range of FR1 of 5G is 450MHz-6000 MHz. Therefore, research on magnetic materials and devices suitable for the GHz band is a problem to be solved.
However, the conventional bulk material such as NiZn ferrite has a very low saturation magnetic induction, and cannot meet the development requirements of high frequency, miniaturization and integration. Therefore, a new generation of high frequency soft magnetic materials needs to be researched. According to the practical application requirements, the high-frequency soft magnetic material simultaneously has excellent soft magnetic properties of high saturation magnetization, high resistivity, high initial permeability and low coercive force, and excellent high-frequency characteristics of high cut-off frequency and low damping factor.
The Chinese patent with publication number CN105761878A discloses a reactive magnetron sputtering preparation method of a FeNCu soft magnetic material, wherein the coercive force is effectively reduced by adding nitrogen and copper elements, the coercive force is lower than 100Oe, but the saturated magnetization intensity is reduced by adding Cu elements, and is only 1200 emu/cc.
The Chinese patent with publication number CN111863372A discloses a method for preparing a bi-phase nanocrystalline structure ((Fe) by using a three-target co-sputtering methodzA1-Z)aCobQcBad)1-x-(RO2)xA soft magnetic material system. The biphase nanocrystalline soft magnetic material has high saturation magnetization and low coercive force, but is uniaxialThe anisotropy field is 6.5-8.5kA/m, the adjustable range of the magnetic anisotropy field is narrow, and the high-frequency characteristic is poor. In addition, when the film is prepared by co-sputtering, a certain amount of oxide solid small pieces are placed on the A target at the same time, so that the preparation process is complex, the restriction parameters are many, and the batch production is not facilitated.
The Chinese patent with publication number CN111863378A discloses a compound of ((FezA)1-Z)aCrbMcNbd)1-x-(R2O3)xThe soft magnetic material system has one or several of Co, Ni and Ti as element A and one or several of Zr, Hf and Ta as element M, and has high saturation magnetization but low resistivity, such as ((Fe)0.5A0.5)30Cr50M30Nb1)0.9-(R2O3)0.1Is only 60 μ Ω cm.
Chinese patent publication No. CN104392823A discloses a novel compound (Fe)65Co35)1-xDyxSoft magnetic material system with a material thickness of 100nm, of which 5<x<15. The soft magnetic material is prepared by adopting a composite target magnetron sputtering mode and doping rare earth element Dy, so that the comprehensive soft magnetic performance and high-frequency characteristics of the soft magnetic film are optimized, the cut-off frequency reaches more than 2GHz, the in-plane uniaxial anisotropy is not obvious, and the magnetic anisotropy field needs to be improved. In addition, the sputtering target adopts a composite target, and other irrelevant impurities are inevitably introduced.
The above patent improves the performance of the soft magnetic material to a certain extent by optimizing the components and the process. However, the components and the preparation method of the above patent cannot simultaneously combine the comprehensive properties of a simple and efficient preparation method, low damping, high cut-off frequency, excellent soft magnetic properties (high magnetic permeability, high saturation magnetization, low coercive force), high resistivity and the like, at present, the damping factor of the high-frequency soft magnetic material reported in domestic and foreign documents is generally higher, the damping factor range is 0.03-0.07, and simultaneously, the soft magnetic properties and the high-frequency properties are weakened, so that the application requirements in the high-frequency field cannot be met. Therefore, there is an urgent need to develop a high-frequency soft magnetic material having low damping, high cut-off frequency, excellent soft magnetic properties (high magnetic permeability, high saturation magnetization, low coercive force), and high resistivity.
Disclosure of Invention
The invention provides an amorphous nanocrystalline high-frequency soft magnetic material with low damping, high cut-off frequency, excellent soft magnetic performance and high resistivity.
A high-frequency soft magnetic material with a chemical formula of Fe1-x-yAxByX is more than or equal to 15 and less than or equal to 45, y is more than or equal to 10 and less than or equal to 20, A is Co and/or Ni, B is nitride and has an oriented magnetic domain structure.
FeCoNi alloy with proper proportion is selected to ensure that the material has high saturation magnetization; by adding nitride with proper content to inhibit the growth of crystal grains and improve the resistivity of the material, the amorphous nanocrystalline high-frequency soft magnetic material with smaller crystal grain size and even distribution is obtained.
The high-frequency soft magnetic material is an alloy material with alpha-Fe nanocrystalline embedded in a nitride amorphous insulating matrix, is a magnetic and nonmagnetic, nanocrystalline and amorphous, conductive and insulating two-phase structure, and has higher resistivity and reduced eddy current loss compared with the traditional soft magnetic material.
Compared with the existing high-frequency soft magnetic material, the grain size is further refined, namely the material has higher magnetic anisotropy due to the dual-phase structure that the tiny nanocrystalline particles are embedded into the nitride amorphous insulating matrix, and the magnetic moments in the material are uniformly arranged due to the high magnetic anisotropy, so that a directional domain structure is formed.
The high-frequency soft magnetic material is an amorphous nanocrystalline dual-phase structure with conductive magnetic nanocrystalline grains embedded in an insulating nonmagnetic amorphous matrix, and the average grain size is less than 10 nm.
And B is a nitride consisting of one or more of Hf, Zr, Ti or rare earth elements and N element.
Large-size doping elements in the B elements are used as trace addition elements and can enter alpha-Fe nanocrystalline lattices to cause the alpha-Fe nanocrystalline lattices to expand and refine grains, and meanwhile, the large-size doping elements are easy to combine with N to form intergranular compounds, so that the resistivity is improved, and the performance of the high-frequency soft magnetic material is optimized; and large-size doping elements which are easier to combine with the N element are added, so that the reduction of the saturation magnetization of the material due to the reaction of Fe and the N element is avoided.
The width of the directional magnetic domain structure is less than 20 mu m, and the shape of the directional magnetic domain structure is approximate to a strip shape.
The directional magnetic domain structure with proper size has low self energy and lower damping factor, and compared with the material with disorderly orientation, the magnetic moment is easy to reverse under the action of an external magnetic field, thereby realizing the effective regulation and control of the magnetic anisotropic field of the material and improving the cut-off frequency of the material.
The high-frequency soft magnetic material has in-plane uniaxial anisotropy, and the magnetic anisotropy field is in the range of 30-80 Oe.
The saturation magnetization of the high-frequency soft magnetic material is more than or equal to 16kGs, the coercive force is less than or equal to 100Oe, and the magnetic conductivity under 100MHz is more than or equal to 400.
The damping factor of the high-frequency soft magnetic material is less than or equal to 0.023, and the cut-off frequency is in the range of 1-10 GHz.
The invention also provides a method for preparing the high-frequency soft magnetic material by combining reactive magnetron sputtering with an in-situ magnetic field, which comprises the following steps:
(1) cleaning and drying substrate material, placing the substrate on a sample holder, placing permanent magnets at two ends of the substrate, placing the substrate in a chamber, and pumping the chamber to a vacuum degree of 5 × 10-5Pa below;
(2)N2uniformly mixing with Ar to form mixed gas, N2The flow ratio of Ar/4-25%, introducing the mixed gas into the chamber, adjusting the pressure in the chamber to 1.2-1.6Pa, and the starting power to 30-40W, and starting;
(3) after stable glow starting, adjusting the sputtering power to be 40-120W, the air pressure in the cavity to be 0.3-1.2Pa, pre-sputtering for 10-20min, and removing impurities on the surface of the target material;
(4) and setting sputtering time and then sputtering to prepare the high-frequency soft magnetic material.
In the step (3), the target is an alloy target, and the size of the target is as follows: the thickness is 2-4mm, and the diameter is 50-60 mm.
Compared with a composite target material, the cleanliness of a sputtering chamber is ensured, and a soft magnetic film with good film forming quality can be prepared; compared with a multi-target co-sputtering mode, the alloy target co-sputtering mode reduces the influence of sputtering process parameters, the preparation process is simple and efficient, and the cost and the time are saved.
In the step (4), before the sputtering time is set, the sample rotates clockwise at the speed of 5-20 rpm.
In the step (4), the sputtering time is 2-50min, and the thickness of the prepared high-frequency soft magnetic material is 5nm-2 μm.
The thickness of the high-frequency soft magnetic material is proper, the relative volume fraction of an interface is low, the obstruction of the substrate to the magnetization process of the material is relatively reduced, and the coercive force is relatively reduced. When the thickness is very thin, the material is greatly affected by substrate stress, defects, lattice mismatch and the like, and the magnetization process of the material is hindered, so that the coercive force is very high. When the thickness of the material is thicker, the defects in the thin film are continuously increased, and meanwhile, the surface roughness of the thin film is increased, so that the coercive force is deteriorated.
The thickness of the high-frequency soft magnetic material is proper, the grain size of the film is small, the grain size is smaller than the exchange coupling length, the exchange coupling effect of the grains enables the magnetic moments of adjacent grains to be arranged consistently, and the exchange coupling effect is large, so that the magnetic anisotropy field is high.
Compared with the prior art, the invention has the following advantages:
(1) the high-frequency soft magnetic material has smaller grain size and an oriented magnetic domain structure by adding large-size doping elements and N elements, and realizes the regulation and control of a magnetic anisotropy field, thereby having lower damping factor, improving the cut-off frequency of the material, widening the high-frequency application range of the high-frequency soft magnetic material and having good high-frequency characteristic;
(2) the high-frequency soft magnetic material is an alloy material with alpha-Fe nanocrystalline embedded in a nitride amorphous insulating matrix, and compared with the traditional soft magnetic material, the structure has higher resistivity, reduces eddy current loss and has excellent soft magnetic performance;
(3) compared with a composite target material, the target material adopts an alloy target material mode, so that the cleanliness of a sputtering chamber is ensured, and a soft magnetic film with good film forming quality can be prepared; compared with a multi-target co-sputtering mode, the alloy target co-sputtering mode reduces the influence of sputtering process parameters, the preparation process is simple and efficient, and the production cost and time are saved.
Drawings
FIG. 1 is a schematic view of a process for producing a high-frequency soft magnetic material according to the present invention;
FIG. 2 is a schematic diagram of an in-situ magnetization field of the high-frequency soft magnetic material of the present invention;
FIG. 3 is a surface topography of an Atomic Force Microscope (AFM) in example 1 of the present invention, wherein (a) is a two-dimensional image of the AFM in example 1 of the present invention; (b) is an AFM three-dimensional image in the embodiment 1 of the invention;
FIG. 4 is a structure diagram of the directional domain of the high frequency soft magnetic material of the present invention;
FIG. 5 is a microscopic structure view of the high-frequency soft magnetic material of the present invention;
FIG. 6 is a comparison graph of M-H curves of the high-frequency soft magnetic material of the present invention, wherein (a) is the M-H curve in example 1 of the present invention; (b) the M-H curve in comparative example 1 of the present invention;
FIG. 7 is a zero field magnetic spectrum of the high frequency soft magnetic material of the present invention;
FIG. 8 is a field-swept magnetic spectrum of the high-frequency soft magnetic thin film of the present invention, wherein (a) is a graph showing a change in the real part of the permeability of the present invention; (b) is a graph of the change of the imaginary part of the permeability of the invention.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be noted that the following examples are only for illustrating the present invention and are not intended to limit the scope of the present invention.
Example 1
A high-frequency soft magnetic material with a chemical formula of Fe55Co27Hf5N13The preparation method is shown in figure 1, and comprises the following specific steps:
(1) preparing Fe with a purity of 99.95%55Co30Hf15Cutting an alloy target material and a Si (100) substrate as required, cleaning the silicon wafer substrate by adopting an RCA semiconductor silicon wafer cleaning process, and drying the silicon wafer substrate by using nitrogen for later use;
(2) as shown in fig. 2, which is a schematic diagram of in-situ magnetic field application of high-frequency soft magnetic material, first, a ndfeb permanent magnet with a specific size is processed by wire cutting, and thenThe device is fixed on a sample support, the distance between two permanent magnets is 10mm, a substrate is positioned in the center of the space of the permanent magnets, the direction of an induction field is parallel to the surface of the substrate, and the size of the induction field is 500 Oe. Then the substrate holder is placed on a sample table, a cavity door is closed and vacuum pumping is carried out, and the vacuum degree of the cavity is 5 multiplied by 10-5Below Pa, preparing for sputtering;
(3) adjusting the gas flow ratio N2/(N2+ Ar) ═ 12%, reacting Ar with N2Fully mixing in a gas mixing chamber, opening a valve of the gas mixing chamber, introducing the mixed gas into a chamber, adjusting the air pressure of the chamber to be 1.2Pa, turning on a direct-current power supply, adjusting the starting power to be 30W, starting luminance, after the luminance is stably started, adjusting the air pressure in a sputtering chamber to be 0.3Pa, adjusting the starting power to be 70W, pre-sputtering for 15min, and removing impurities on the surface of the target material; the flow rate of nitrogen is 6sccm, and the flow rate of argon is 44 sccm;
(4) after the pre-sputtering is finished, opening a baffle of a magnetron sputtering platform, wherein the sputtering rate is 2.22nm/min, the direct-current sputtering power and the sputtering air pressure are 70W and 0.3Pa, the rotating speed of the sample platform is 5rpm, the sputtering time is 27min, and Fe deposited under the process condition55Co27Hf5N13The thickness of the high-frequency soft magnetic material is 60 nm;
the amorphous nanocrystalline two-phase high-frequency soft magnetic material prepared under the conditions has good film forming quality, can be obtained from AFM two-dimensional and three-dimensional images, and has the surface roughness of about 1.5nm, as shown in figures 3(a) and 3 (b); the magnetic domain structure of the high-frequency soft magnetic material is an oriented magnetic domain structure with the width smaller than 20 mu m, as shown in figure 4, a small and uniformly oriented magnetic domain is favorable for improving the high-frequency soft magnetic property of the material; the high-frequency soft magnetic material has fine and uniform crystal grains, and the size of the crystal grains is less than 10nm, as shown in figure 5.
The M-H curve of the high-frequency soft magnetic material prepared under the above process conditions is shown in fig. 6(a), the hard-axis coercivity is 10Oe, the easy-axis coercivity is 12Oe, and the high-frequency soft magnetic material has significant uniaxial anisotropy. Compared with comparative example 1, the M-H curve of the high-frequency soft magnetic material is shown in fig. 6(b), the hard axis coercive force of the high-frequency soft magnetic material prepared under the process conditions is reduced by 70Oe, and the easy axis coercive force of the high-frequency soft magnetic material is reduced by 20 Oe.
The zero-field magnetic spectrum measurement is performed on the high-frequency soft magnetic material by using a vector network analyzer and a microstrip line method, as shown in fig. 7, the resonance frequency reaches 3.0GHz, and the resonance line width and the damping factor are 1.06GHz and 0.022 respectively.
The vector network analyzer is utilized to perform magnetic field scanning spectrum measurement on the high-frequency soft magnetic material by adopting a microstrip line method, the variation range of an external magnetic field is 0-180Oe, the variation of the external magnetic field is 20Oe, and the real part and the imaginary part of the obtained magnetic conductivity are respectively shown in fig. 8(a) and fig. 8 (b). As the applied magnetic field increases from 0Oe to 180Oe, the resonant frequency increases from 3.0GHz to 6.0GHz, and the material exhibits good high-frequency characteristics.
Example 2
A high-frequency soft magnetic material with a chemical formula of Fe53Co33H5N9The preparation method is shown in figure 1, and comprises the following specific steps:
(1) preparing Fe with a purity of 99.95%55Co30Hf15Cutting an alloy target material and a Si (100) substrate as required, cleaning the silicon wafer by adopting an RCA semiconductor silicon wafer cleaning process, and drying the silicon wafer by using nitrogen for later use;
(2) as shown in fig. 2, which is a schematic diagram of in-situ magnetic field addition of a high-frequency soft magnetic material, a neodymium iron boron permanent magnet with a specific size is firstly processed by wire cutting and fixed on a sample holder, the distance between the two permanent magnets is 25mm, a substrate is positioned at the center of the space of the permanent magnets, the direction of an induction field is parallel to the surface of the substrate, and the size of the induction field is 70 Oe. Then the sample holder is placed on a sample table, the cavity door is closed and vacuum pumping is carried out, and the vacuum degree of the cavity is 5 multiplied by 10-5Below Pa, preparing for sputtering;
(3) adjusting the gas flow ratio N2/(N2+ Ar) ═ 12%, reacting Ar with N2Fully mixing in the gas mixing chamber, opening a valve of the gas mixing chamber, and introducing the mixed gas into the cavity. And (3) adjusting the air pressure of the chamber to be 1.2Pa, turning on a direct-current power supply, adjusting the starting power to be 30W, and starting. After stable glow starting, adjusting the air pressure in the sputtering chamber to 0.3Pa, adjusting the glow starting power to 70W, pre-sputtering for 15min, and removing impurities on the surface of the target material; the flow rate of nitrogen is 6sccm, and the flow rate of argon is 44 sccm;
(4) after the pre-sputtering is finished, opening a baffle of the magnetron sputtering platform for sputteringThe speed is 4.17nm/min, the direct current sputtering power and the sputtering air pressure are 70W and 0.3Pa, the rotating speed of the sample stage is 5rpm, the sputtering time is 12min, and Fe deposited under the process condition53Co33H5N9The thickness of the high-frequency soft magnetic material is 50 nm.
Example 3
A high-frequency soft magnetic material with a chemical formula of Fe47Co33Hf9N11The preparation method is shown in figure 1, and comprises the following specific steps:
(1) preparing Fe with a purity of 99.95%55Co30Hf15Cutting an alloy target material and a Si (100) substrate as required, cleaning the silicon wafer by adopting an RCA semiconductor silicon wafer cleaning process, and drying the silicon wafer by using nitrogen for later use;
(2) as shown in fig. 2, which is a schematic diagram of in-situ magnetic field application of a high-frequency soft magnetic material, a neodymium-iron-boron permanent magnet with a specific size is processed by wire cutting and fixed on a sample holder, the distance between the two permanent magnets is 10mm, a substrate is positioned at the center of the space of the permanent magnets, the direction of an induction field is parallel to the surface of the substrate, and the size of the induction field is 500 Oe. Then the sample holder is placed on a sample table, the cavity door is closed and vacuum pumping is carried out, and the vacuum degree of the cavity is 5 multiplied by 10-5Below Pa, preparing for sputtering;
(3) the same as the step (3) in example 1;
(4) after the pre-sputtering is finished, opening a baffle of a magnetron sputtering platform, wherein the sputtering rate is 3.24nm/min, the direct-current sputtering power and the sputtering air pressure are 70W and 0.5Pa, the rotating speed of the sample platform is 5rpm, the sputtering time is 37min, and Fe deposited under the process condition47Co33Hf9N11The thickness of the high-frequency soft magnetic material is 120 nm.
Example 4
A high-frequency soft magnetic material with a chemical formula of Fe48Co33Hf7N12The preparation method is shown in figure 1, and comprises the following specific steps:
(1) preparing Fe with a purity of 99.95%55Co30Hf15Cutting an alloy target material and a Si (100) substrate as required, cleaning the silicon wafer by adopting an RCA semiconductor silicon wafer cleaning process, and drying the silicon wafer by using nitrogen for later use;
(2) as shown in fig. 2, which is a schematic diagram of in-situ magnetic field application of a high-frequency soft magnetic material, a neodymium-iron-boron permanent magnet with a specific size is processed by wire cutting and fixed on a sample holder, the distance between the two permanent magnets is 10mm, a substrate is positioned at the center of the space of the permanent magnets, the direction of an induction field is parallel to the surface of the substrate, and the size of the induction field is 500 Oe. Then the sample holder is placed on a sample table, the cavity door is closed and vacuum pumping is carried out, and the vacuum degree of the cavity is 5 multiplied by 10-5Below Pa, preparing for sputtering;
(3) the same as the step (3) in example 1;
(4) after the pre-sputtering is finished, opening a baffle of a magnetron sputtering platform, wherein the sputtering rate is 3.53nm/min, the direct current sputtering power and the sputtering air pressure are 70W and 0.8Pa, the rotating speed of the sample platform is 5rpm, the sputtering time is 17min, and Fe deposited under the process condition48Co33Hf7N12The thickness of the high-frequency soft magnetic material is 60 nm.
Example 5
A high-frequency soft magnetic material with a chemical formula of Fe56Ni30Zr6N8The preparation method is shown in figure 1, and comprises the following specific steps:
(1) preparing Fe with a purity of 99.95%55Ni30Zr15Cutting an alloy target material and a Si (100) substrate as required, cleaning the silicon wafer by adopting an RCA semiconductor silicon wafer cleaning process, and drying the silicon wafer by using nitrogen for later use;
(2) as shown in fig. 2, which is a schematic diagram of in-situ magnetic field application of a high-frequency soft magnetic material, a neodymium-iron-boron permanent magnet with a specific size is processed by wire cutting and fixed on a sample holder, the distance between the two permanent magnets is 10mm, a substrate is positioned at the center of the space of the permanent magnets, the direction of an induction field is parallel to the surface of the substrate, and the size of the induction field is 500 Oe. Then the sample holder is placed on a sample table, the cavity door is closed and vacuum pumping is carried out, and the vacuum degree of the cavity is 5 multiplied by 10-5Below Pa, preparing for sputtering;
(3) the same as the step (3) in example 1;
(4) after the pre-sputtering is finished, opening a baffle of a magnetron sputtering platform, wherein the sputtering rate is 2.42nm/min, the direct-current sputtering power and the sputtering air pressure are 70W and 0.3Pa, and the rotating speed of the sample platform is 5rpm, sputtering time is 33min, Fe deposited under the process condition56Ni30Zr6N8The thickness of the high-frequency soft magnetic material is 80 nm.
Example 6
A high-frequency soft magnetic material with a chemical formula of Fe54Ni31Ti5N10The preparation method is shown in figure 1, and comprises the following specific steps:
(1) preparing Fe with a purity of 99.95%55Ni30Ti15Cutting an alloy target material and a Si (100) substrate as required, cleaning the silicon wafer by adopting an RCA semiconductor silicon wafer cleaning process, and drying the silicon wafer by using nitrogen for later use;
(2) as shown in fig. 2, which is a schematic diagram of in-situ magnetic field application of a high-frequency soft magnetic material, a neodymium-iron-boron permanent magnet with a specific size is processed by wire cutting and fixed on a sample holder, the distance between the two permanent magnets is 10mm, a substrate is positioned at the center of the space of the permanent magnets, the direction of an induction field is parallel to the surface of the substrate, and the size of the induction field is 500 Oe. Then the sample holder is placed on a sample table, the cavity door is closed and vacuum pumping is carried out, and the vacuum degree of the cavity is 5 multiplied by 10-5Below Pa, preparing for sputtering;
(3) the same as the step (3) in example 1;
(4) after the pre-sputtering is finished, opening a baffle of a magnetron sputtering platform, wherein the sputtering rate is 2.4nm/min, the direct-current sputtering power and the sputtering air pressure are 70W and 0.3Pa, the rotating speed of the sample platform is 5rpm, the sputtering time is 25min, and Fe deposited under the process condition54Ni31Pr5N01The thickness of the high-frequency soft magnetic material is 60 nm.
Example 7
A high-frequency soft magnetic material with a chemical formula of Fe49Ni36Pr5N10The preparation method is shown in figure 1, and comprises the following specific steps:
(1) preparing Fe with a purity of 99.95%55Ni30Pr15Cutting an alloy target material and a Si (100) substrate as required, cleaning the silicon wafer by adopting an RCA semiconductor silicon wafer cleaning process, and drying the silicon wafer by using nitrogen for later use;
(2) FIG. 2 is a schematic diagram of in-situ magnetization of high-frequency soft magnetic material, firstThe neodymium iron boron permanent magnet with a specific size is processed by utilizing linear cutting and is fixed on a sample support, the distance between the two permanent magnets is 10mm, the substrate is positioned in the center of the space of the permanent magnets, the direction of an induction field is parallel to the surface of the substrate, and the size of the induction field is 500 Oe. Then the sample holder is placed on a sample table, the cavity door is closed and vacuum pumping is carried out, and the vacuum degree of the cavity is 5 multiplied by 10-5Below Pa, preparing for sputtering;
(3) the same as the step (3) in example 1;
(4) after the pre-sputtering is finished, opening a baffle of a magnetron sputtering platform, wherein the sputtering rate is 2.5nm/min, the direct current sputtering power and the sputtering air pressure are 70W and 0.3Pa, the rotating speed of a sample platform is 5rpm, the sputtering time is 24min, and Fe deposited under the process condition49Ni36Pr5N10The thickness of the high-frequency soft magnetic material is 60 nm.
Comparative example 1
For comparison, in the sputtering process in step (1) of example 1, the high-frequency soft magnetic material is prepared by using a dc magnetron sputtering method, that is, the alloy target is placed on a dc magnetron sputtering target position with a sputtering power of 70W, a sample with a certain thickness is sputtered under a sputtering pressure of 0.3Pa, and the sample is taken out, wherein specific process parameters and material thickness are shown in table 1.
Comparative example 1 is a high-frequency soft magnetic material obtained under different preparation process parameters, and the preparation method and soft magnetic properties and high-frequency characteristic characterization method thereof are substantially the same as those of example 1. Except that the sputtering atmosphere used in the preparation of the high-frequency soft magnetic material in comparative example 1 was high-purity argon.
TABLE 1
Comparative example Sputtering gas pressure Sputtering power (W) Nitrogen flow ratio (%) Thickness of material (nm)
1 0.3 70 0 60
Comparative examples 2, 3 and 4
Comparative examples 2, 3 and 4 are high frequency soft magnetic materials obtained under different preparation process parameters, and the preparation method and soft magnetic properties and high frequency characteristic characterization method thereof are substantially the same as those of example 1. Except that the sputtering atmosphere used was high purity argon gas when preparing the high frequency soft magnetic materials of comparative examples 2, 3, and 4. Specific process parameters and material thicknesses are shown in table 2.
TABLE 2
Figure BDA0002839158260000101
Analysis of soft magnetic properties and high frequency characteristics of examples 1 to 7 and comparative examples 1 to 4:
1. static magnetic properties
The samples were subjected to M-H curve testing using a vibrating sample magnetometer, model 7410 manufactured by Lakeshore corporation, to obtain static magnetic parameters, the results of which are shown in FIG. 6 and Table 3.
TABLE 3
High frequency soft magnetic material 4πMs(kGs) Hce(Oe) Hch(Oe) Hk(Oe)
Example 1 16.1 12 10 54
Example 2 18.1 14 11.3 34
Example 3 16.9 15 9.5 62
Example 4 17 32 12 71
Example 5 16 19 15 56
Example 6 16.8 28 11 58
Example 7 17.2 13 11 67
Comparative example 1 20.2 82 30 120
Comparative example 2 18.7 90 22 132
Comparative example 3 18.2 77 19 220
Comparative example 4 17.6 52 31 84
Wherein, 4 pi MsIs the saturation magnetization, H, of the high frequency soft magnetic materialceAnd HceCoercive force H of easy axis and hard axis respectivelykIs the magnetic anisotropy field of the high frequency soft magnetic material.
Comparative examples 1 to 4 are FeCoHf high-frequency soft magnetic materials prepared on the basis of example 1, respectively, and the saturation magnetization intensity of the FeCoHf high-frequency soft magnetic materials is higher than that of examples 1 to 7 and is higher than 17.6kGs, but the coercive force is higher, which shows that the addition of nitrogen element is helpful for forming intergranular compounds, so that the grain growth is inhibited, the coercive force is reduced, and the theory is consistent with the random anisotropy model theory of Herzer. Meanwhile, nitrogen doping causes the content of nonmagnetic elements in the material to be reduced, and the saturation magnetization is relatively reduced. The addition of nitrogen element optimizes the magnetic anisotropy field of the material from a large range of 80-220Oe to a small range of 34-71Oe, effectively improves the magnetic permeability of the material and improves the comprehensive soft magnetic performance of the material.
2. High frequency characteristics
The high-frequency characteristic parameters were obtained by using a PNAE8386B vector network analyzer from Agilent corporation and testing the magnetic scanning spectrum and the magnetic zero-field spectrum of examples 1 to 7 and comparative examples 1 to 4, respectively, by the microstrip line method, and the results are shown in fig. 7, 8, and table 4.
TABLE 4
High frequency soft magnetic material Cut-off frequency (GHz) Resonance line width (GHz) Damping factor
Example 1 3.0 1.06 0.022
Example 2 4.3 1.08 0.023
Example 3 3.6 0.64 0.015
Example 4 3.2 0.67 0.017
Example 5 4.2 0.6 0.014
Example 6 4.6 0.56 0.011
Example 7 3.1 0.9 0.021
Comparative example 1 2.4 2.45 0.09
Comparative example 2 2.1 2.56 0.105
Comparative example 3 2.5 1.35 0.069
Comparative example 4 2.3 1.60 0.074
In the embodiments 1-7, the magnetic spectrums of the nitrogen-doped high-frequency soft magnetic materials are typical resonance type magnetic spectrums, the cut-off frequency of the materials can be adjusted within the range of 1-10GHz, and the damping factor is less than or equal to 0.023. From the field-swept magnetic spectra of examples 1-7, the resonance linewidth gradually increased with increasing applied magnetic field, and the material exhibited significant anisotropy and excellent high-frequency properties.
The magnetic spectra of comparative examples 1 to 4 are soft magnetic materials not doped with nitrogen, and the resonance frequencies are low, the resonance peak broadening is large, and the damping factors are larger than those of examples 1 to 7 doped with nitrogen. The invention provides the high-frequency soft magnetic material prepared by the nitrogen doping method, which effectively reduces the damping factor of the material, optimizes the high-frequency characteristic of the soft magnetic material and can regulate and control the use frequency of the material in a large range.
3. Electrical Properties
The resistivities of examples 1 to 7 and comparative examples 1 to 4 were measured using a step meter and a four-probe meter, respectively, and the results are shown in Table 5.
Table 5:
Figure BDA0002839158260000121
Figure BDA0002839158260000131
as shown in table 5, the resistivity of the nitrogen-doped soft magnetic material in the comparative example is significantly higher than that of the soft magnetic material not doped with nitrogen element in the comparative example, which shows that the addition of nitrogen element helps to form amorphous nitride, and form an amorphous nanocrystalline bidirectional soft magnetic material, and the magnetic and nonmagnetic, conductive and insulating, nanocrystalline and amorphous alternating granular film structure improves the resistivity by at least 50% compared with the material not doped with nitrogen element.
All documents referred to herein are incorporated by reference into this application as if each had been individually incorporated by reference. It is to be understood that any changes or modifications of the present invention may be made by those skilled in the art after reading the above teachings of the present invention, and such equivalents are also within the scope of the appended claims.

Claims (10)

1. A high-frequency soft magnetic material is characterized in that the chemical formula is Fe1-x-yAxByX is more than or equal to 15 and less than or equal to 45, y is more than or equal to 10 and less than or equal to 20, A is Co and/or Ni, B is nitride and has an oriented magnetic domain structure.
2. The high-frequency soft magnetic material according to claim 1, wherein the high-frequency soft magnetic material is an amorphous nanocrystalline dual-phase structure in which conductive magnetic nanocrystalline grains are embedded in an insulating nonmagnetic amorphous matrix, and the average grain size is less than 10 nm.
3. The high-frequency soft magnetic material according to claim 1, wherein B is a nitride consisting of one or more of Hf, Zr, Ti or a rare earth element and an N element.
4. The high frequency soft magnetic material according to claim 1, wherein the oriented magnetic domain structure has a width of less than 20 μm and a shape of a stripe.
5. The high-frequency soft magnetic material according to claim 1, wherein the high-frequency soft magnetic material has in-plane uniaxial anisotropy, and the magnetic anisotropy field is in the range of 30 to 80 Oe.
6. The high-frequency soft magnetic material according to claim 1, wherein the saturation magnetization of the high-frequency soft magnetic material is not less than 16kGs, the coercivity is not more than 100Oe, and the permeability at 100MHz is not less than 400.
7. The high-frequency soft magnetic material according to claim 1, wherein the damping factor of the high-frequency soft magnetic material is not more than 0.023 and the cutoff frequency is in the range of 1-10 GHz.
8. The method for producing a high-frequency soft magnetic material according to any one of claims 1 to 7, comprising:
(1) cleaning and drying substrate material, placing the substrate on a sample holder, placing permanent magnets at two ends of the substrate, placing the substrate in a chamber, and pumping the chamber to a vacuum degree of 5 × 10-5Pa below;
(2)N2uniformly mixing with Ar to form mixed gas, N2The flow ratio of Ar/4-25%, introducing the mixed gas into the chamber, adjusting the pressure in the chamber to 1.2-1.6Pa, and the starting power to 30-40W, and starting;
(3) after stable glow starting, adjusting the sputtering power to be 40-120W, the air pressure in the cavity to be 0.3-1.2Pa, pre-sputtering for 10-20min, and removing impurities on the surface of the target material;
(4) and setting sputtering time and then sputtering to prepare the high-frequency soft magnetic material.
9. The method for preparing a high-frequency soft magnetic material according to claim 8, wherein in the step (3), the target is an alloy target.
10. The method for preparing a high-frequency soft magnetic material according to claim 8, wherein in the step (4), the sputtering time is 2 to 50min, and the thickness of the prepared high-frequency soft magnetic material is 5nm to 2 μm.
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