CN117051337A - Amorphous nanocrystalline alloy and preparation method and application thereof - Google Patents

Amorphous nanocrystalline alloy and preparation method and application thereof Download PDF

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Publication number
CN117051337A
CN117051337A CN202311050324.1A CN202311050324A CN117051337A CN 117051337 A CN117051337 A CN 117051337A CN 202311050324 A CN202311050324 A CN 202311050324A CN 117051337 A CN117051337 A CN 117051337A
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amorphous nanocrystalline
alloy
nanocrystalline alloy
vacuum
amorphous
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邓毕力
罗顶飞
潘振海
徐敏义
王玉川
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Anhui Zhimagnetic New Material Technology Co Ltd
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Anhui Zhimagnetic New Material Technology Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C45/00Amorphous alloys
    • C22C45/02Amorphous alloys with iron as the major constituent
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/26Methods of annealing
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/74Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
    • C21D1/773Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material under reduced pressure or vacuum
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C33/00Making ferrous alloys
    • C22C33/003Making ferrous alloys making amorphous alloys
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/002Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/02Ferrous alloys, e.g. steel alloys containing silicon
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/10Ferrous alloys, e.g. steel alloys containing cobalt
    • C22C38/105Ferrous alloys, e.g. steel alloys containing cobalt containing Co and Ni
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12Magnets 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
    • H01F1/14Magnets 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
    • H01F1/147Alloys characterised by their composition
    • H01F1/153Amorphous metallic alloys, e.g. glassy metals
    • H01F1/15333Amorphous metallic alloys, e.g. glassy metals containing nanocrystallites, e.g. obtained by annealing
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D2201/00Treatment for obtaining particular effects
    • C21D2201/03Amorphous or microcrystalline structure
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

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  • Engineering & Computer Science (AREA)
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  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
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  • Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Thermal Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Electromagnetism (AREA)
  • Dispersion Chemistry (AREA)
  • Power Engineering (AREA)
  • Soft Magnetic Materials (AREA)
  • Continuous Casting (AREA)

Abstract

The invention belongs to the technical field of amorphous nanocrystalline materials, and particularly relates to an amorphous nanocrystalline alloy, a preparation method and application thereof. The invention provides an amorphous nanocrystalline alloy, which comprises the following components in percentage by weight: fe (Fe) a Co b Ni c Si d B e M f ,1≤b≤10,3≤c≤5,11.5≤d≤13,5≤e≤7,0.1 f is more than or equal to 0.3; m is an unavoidable impurity. The amorphous nanocrystalline alloy provided by the invention has small impurity content, and the magnetic flux density of the amorphous nanocrystalline alloy material can be improved and the coercive force of the alloy can be reduced by adding the Ni element.

Description

Amorphous nanocrystalline alloy and preparation method and application thereof
Technical Field
The invention belongs to the technical field of amorphous nanocrystalline materials, and particularly relates to an amorphous nanocrystalline alloy, a preparation method and application thereof.
Background
The amorphous nanocrystalline magnetically soft alloy material has the excellent characteristics of high saturation magnetic induction intensity, high magnetic permeability, low coercivity, low loss, good stability, high strength and toughness, wear resistance and corrosion resistance and the like, is used as a nanocrystalline alloy material with better cost performance in a metal magnetically soft material, and can replace silicon steel and ferrite to be used as ideal materials for medium-high frequency transformers, inductance components and the like.
The amorphous nanocrystalline magnetically soft alloy material is generally composed of iron, silicon, boron, niobium, copper and other components, and also comprises Fe-based amorphous nanocrystalline alloy doped with a large amount of Co elements, wherein the Co-based amorphous alloy has the advantages of low coercivity, low loss, good DC resistance, good high-temperature magnetic performance, giant magneto-impedance effect and the like. For example, the prior art discloses a high permeability amorphous nanocrystalline alloy having a composition expressed as Fe a Co b Si c B d Cu e M f M’ g Wherein M is at least one of V, ta and Nb, M' is at least one of Ti, zr, hf, ni, ge, cr, mn, W, zn, sn, sb, mo, Y and Al, and the a, b, c, d, e, f and g distributions represent the atomic content of the corresponding element and satisfy: a is more than or equal to 74 and less than or equal to 82,0.01, b is more than or equal to 5, c is more than or equal to 5 and less than or equal to 15, d is more than or equal to 4 and less than or equal to 13,0.2 and less than or equal to 1.5, f is more than or equal to 1 and less than or equal to 4, g is more than or equal to 0 and less than or equal to 1, and a+b+c+d+e+f+g=100.
However, the amorphous nanocrystalline alloy in the prior art is doped with more impurities, so that the performances such as magnetic flux density and the like of the amorphous nanocrystalline alloy are further affected.
Disclosure of Invention
The invention provides an amorphous nanocrystalline alloy and a preparation method and application thereof, and aims to solve the problem that the performance of the amorphous nanocrystalline alloy such as magnetic flux density is further affected due to the fact that the amorphous nanocrystalline alloy is doped with more impurities in the prior art.
For this purpose, the invention provides the following technical proposal,
the invention provides an amorphous nanocrystalline alloy, which comprises the following components in percentage by weight: fe (Fe) a Co b Ni c Si d B e M f ,1≤b≤10,3≤c≤5,11.5≤d≤13,5≤e≤7,0.1≤f≤0.3;
M is an unavoidable impurity.
In the above amorphous nanocrystalline alloy, as a preferred embodiment, the alloy is an amorphous nanocrystalline dual-phase structure;
and/or the average grain size of the nanocrystals is less than or equal to 10nm.
In the above amorphous nanocrystalline alloy, as a preferred embodiment, the coercivity of the amorphous nanocrystalline alloy is < 5A/m.
And/or, the maximum magnetic flux density of the amorphous nanocrystalline alloy is 1-1.2T.
In the above amorphous nanocrystalline alloy, as a preferred embodiment, the residual magnetism of the amorphous nanocrystalline alloy is < 100mT.
And/or, the rectangle ratio of the amorphous nanocrystalline alloy is less than 8%.
In the present invention, the sign of coercive force is H c The sign of the maximum magnetic flux density is B m The sign of remanence is B r Rectangular ratio of B r /B m
The invention also provides a preparation method of the amorphous nanocrystalline alloy, which comprises the following steps:
s1: preparing materials according to alloy components, vacuum smelting to obtain molten steel after the materials are prepared, and preserving the heat of the molten steel to form an alloy cast ingot after the heat preservation is finished;
s2: and (3) annealing the alloy ingot, and cooling after annealing to obtain the amorphous nanocrystalline alloy.
In the above preparation method, as a preferred embodiment, in step S1, the temperature of the vacuum melting is 1200-1300 ℃;
and/or the vacuum degree of the vacuum smelting is 15-20Pa.
In the above preparation method, as a preferred embodiment, in step S1, the temperature of the insulation is 1000-1150 ℃;
and/or the time when the heat preservation is finished is the complete melting of the alloy raw material.
In the above preparation method, as a preferred embodiment, in step S2, the annealing treatment is performed at a temperature of 550 to 600 ℃;
and/or the annealing treatment time is 10-15min.
In the above preparation method, as a preferred embodiment, in step S2, the cooled environment is a vacuum environment;
and/or the vacuum degree of the vacuum environment is 15Pa to 20Pa;
and/or the temperature of the vacuum environment is 10-15 ℃.
The invention also provides application of the amorphous nanocrystalline alloy in a medium-high frequency transformer.
The technical scheme provided by the invention has the following beneficial effects:
1. the invention provides an amorphous nanocrystalline alloy, which comprises the following components in percentage by weight: fe (Fe) a Co b Ni c Si d B e M f B is more than or equal to 1 and less than or equal to 10, c is more than or equal to 3 and less than or equal to 5, d is more than or equal to 11.5 and less than or equal to 13, e is more than or equal to 5 and less than or equal to 7,0.1, and f is more than or equal to 0.3; m is an unavoidable impurity. The amorphous nanocrystalline alloy provided by the invention has small impurity content, and the magnetic flux density of the amorphous nanocrystalline alloy material can be improved and the coercive force of the alloy can be reduced by adding the Ni element.
2. The invention also provides a preparation method of the amorphous nanocrystalline alloy, which comprises the following steps: s1: preparing materials according to alloy components, vacuum smelting to obtain molten steel after the materials are prepared, and preserving the heat of the molten steel to form an alloy cast ingot after the heat preservation is finished; s2: and (3) annealing the alloy ingot, and cooling after annealing to obtain the amorphous nanocrystalline alloy. The preparation method provided by the invention can be used for smelting alloy raw materials in a vacuum environment, so that the reaction of impurities in air and the alloy raw materials in the smelting process can be avoided, and the pure progress of the alloy is improved. In the process of forming the nanocrystalline, the annealing temperature is increased, and the average grain size of the nanocrystalline can be reduced, so that the magnetic flux density of the amorphous nanocrystalline alloy material is further improved.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions in the embodiments of the present invention will be clearly and completely described in the following in conjunction with the embodiments of the present invention. It will be apparent to those skilled in the art that the examples are merely to aid in understanding the invention and are not to be construed as a specific limitation thereof. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The examples of the present invention are implemented on the premise of the technical scheme of the present invention, and detailed implementation modes and processes are given, but the protection scope of the present invention is not limited to the following examples, in which the process parameters of specific conditions are not noted, and generally according to conventional conditions.
The endpoints of the ranges and any values disclosed in the present invention are not limited to the precise range or value, and the range or value should be understood to include values close to the range or value. For numerical ranges, one or more new numerical ranges may be obtained in combination with each other between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point values, and are to be considered as specifically disclosed in the present invention.
In the present invention, all values relating to the amounts of the components are "parts by weight" throughout unless specified and/or indicated otherwise. The process parameters for the specific conditions not noted in the examples below are generally as usual.
The alloy element composition of the following example is Fe 68.9 Co 10 Ni 4 Si 12 B 5 M 0.1
Example 1
The embodiment provides a preparation method of an amorphous nanocrystalline alloy, which comprises the following steps:
step one: and (3) mixing according to the target alloy element composition, adding the mixed alloy raw materials into a vacuum smelting furnace for vacuum smelting (the vacuum smelting temperature is 1250 ℃ and the vacuum degree is 15 Pa), and obtaining molten steel.
Step two: and carrying out heat preservation treatment on the obtained molten steel in a vacuum smelting furnace, wherein the heat preservation temperature is 1100 ℃, and pouring out the molten steel after the alloy raw materials are completely melted to obtain an alloy cast ingot.
Step three: annealing the alloy ingot at 550 ℃ for 15min, cooling, and vacuum cooling in a vacuum environment with the vacuum degree of 20Pa and the vacuum temperature of 10 ℃. And after cooling, obtaining the amorphous nanocrystalline alloy.
Example 2
The embodiment provides a preparation method of an amorphous nanocrystalline alloy, which comprises the following steps:
step one: and (3) mixing according to the target alloy element composition, adding the mixed alloy raw materials into a vacuum smelting furnace for vacuum smelting (the vacuum smelting temperature is 1250 ℃ and the vacuum degree is 15 Pa), and obtaining molten steel.
Step two: and carrying out heat preservation treatment on the obtained molten steel in a vacuum smelting furnace, wherein the heat preservation temperature is 1100 ℃, and pouring out the molten steel after the alloy raw materials are completely melted to obtain an alloy cast ingot.
Step three: annealing the alloy ingot at 600 ℃ for 15min, cooling, and vacuum cooling in a vacuum environment with the vacuum degree of 20Pa and the vacuum temperature of 10 ℃. And after cooling, obtaining the amorphous nanocrystalline alloy.
Example 3
The embodiment provides a preparation method of an amorphous nanocrystalline alloy, which comprises the following steps:
step one: and (3) mixing according to the target alloy element composition, adding the mixed alloy raw materials into a vacuum smelting furnace for vacuum smelting (the vacuum smelting temperature is 1250 ℃ and the vacuum degree is 15 Pa), and obtaining molten steel.
Step two: and carrying out heat preservation treatment on the obtained molten steel in a vacuum smelting furnace, wherein the heat preservation temperature is 1100 ℃, and pouring out the molten steel after the alloy raw materials are completely melted to obtain an alloy cast ingot.
Step three: annealing the alloy ingot at 580 ℃ for 15min, cooling, and vacuum cooling in a vacuum environment with the vacuum degree of 20Pa and the vacuum temperature of 10 ℃. And after cooling, obtaining the amorphous nanocrystalline alloy.
Example 4
The embodiment provides a preparation method of an amorphous nanocrystalline alloy, which comprises the following steps:
step one: and (3) mixing according to the target alloy element composition, adding the mixed alloy raw materials into a vacuum smelting furnace for vacuum smelting (the vacuum smelting temperature is 1250 ℃ and the vacuum degree is 15 Pa), and obtaining molten steel.
Step two: and carrying out heat preservation treatment on the obtained molten steel in a vacuum smelting furnace, wherein the heat preservation temperature is 1100 ℃, and pouring out the molten steel after the alloy raw materials are completely melted to obtain an alloy cast ingot.
Step three: annealing the alloy ingot at 550 ℃ for 10min, cooling, and vacuum cooling in a vacuum environment with the vacuum degree of 20Pa and the vacuum temperature of 10 ℃. And after cooling, obtaining the amorphous nanocrystalline alloy.
Example 5
The embodiment provides a preparation method of an amorphous nanocrystalline alloy, which comprises the following steps:
step one: and (3) mixing according to the target alloy element composition, adding the mixed alloy raw materials into a vacuum smelting furnace for vacuum smelting (the vacuum smelting temperature is 1250 ℃ and the vacuum degree is 15 Pa), and obtaining molten steel.
Step two: and carrying out heat preservation treatment on the obtained molten steel in a vacuum smelting furnace, wherein the heat preservation temperature is 1100 ℃, and pouring out the molten steel after the alloy raw materials are completely melted to obtain an alloy cast ingot.
Step three: annealing the alloy ingot at 550 ℃ for 12min, cooling, and vacuum cooling in a vacuum environment with the vacuum degree of 20Pa and the vacuum temperature of 10 ℃. And after cooling, obtaining the amorphous nanocrystalline alloy.
Comparative example 1
The alloy element composition of this comparative example is Fe 72.5 Co 10 Si 12 B 5 M 0.5
The comparative example provides a method for preparing an amorphous nanocrystalline alloy, comprising the following steps:
step one: and (3) mixing according to the target alloy element composition, adding the mixed alloy raw materials into a vacuum smelting furnace for vacuum smelting (the vacuum smelting temperature is 1250 ℃ and the vacuum degree is 15 Pa), and obtaining molten steel.
Step two: and carrying out heat preservation treatment on the obtained molten steel in a vacuum smelting furnace, wherein the heat preservation temperature is 1100 ℃, and pouring out the molten steel after the alloy raw materials are completely melted to obtain an alloy cast ingot.
Step three: annealing the alloy ingot at 550 ℃ for 15min, cooling, and vacuum cooling in a vacuum environment with the vacuum degree of 20Pa and the vacuum temperature of 10 ℃. And after cooling, obtaining the amorphous nanocrystalline alloy.
Comparative example 2
The alloy element composition of this comparative example is Fe 68.9 Co 10 Ni 4 Si 12 B 5 M 0.1
The comparative example provides a method for preparing an amorphous nanocrystalline alloy, comprising the following steps:
step one: and (3) mixing according to the target alloy element composition, adding the mixed alloy raw materials into a vacuum smelting furnace for vacuum smelting (the vacuum smelting temperature is 1250 ℃ and the vacuum degree is 15 Pa), and obtaining molten steel.
Step two: and carrying out heat preservation treatment on the obtained molten steel in a vacuum smelting furnace, wherein the heat preservation temperature is 1100 ℃, and pouring out the molten steel after the alloy raw materials are completely melted to obtain an alloy cast ingot.
Step three: annealing the alloy ingot at 400 ℃ for 15min, cooling, and vacuum cooling in a vacuum environment with the vacuum degree of 20Pa and the vacuum temperature of 10 ℃. And after cooling, obtaining the amorphous nanocrystalline alloy.
Test case
The coercivity, maximum magnetic flux density, rectangular ratio were measured for examples 1-5 and comparative examples 1-2, and the measurement results are shown in the following table:
H c (A/m) B m (T) B r /B m (%)
example 1 1.432 1.014 5.32
Example 2 2.467 1.035 4.20
Example 3 2.578 1.163 3.17
Example 4 3.145 1.104 7.22
Example 5 4.096 1.002 6.08
Comparative example 1 8.712 0.821 10.19
Comparative example 2 6.340 0.903 10.03
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the particular embodiments disclosed, but on the contrary, the intention is to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention as defined by the appended claims.

Claims (10)

1. An amorphous nanocrystalline alloy is characterized in that the expression of the alloy components is as follows: fe (Fe) a Co b Ni c Si d B e M f ,1≤b≤10,3≤c≤5,11.5≤d≤13,5≤e≤7,0.1≤f≤0.3;
M is an unavoidable impurity.
2. The amorphous nanocrystalline alloy according to claim 1, wherein the alloy is an amorphous nanocrystalline dual phase structure;
and/or the average grain size of the nanocrystals is less than or equal to 10nm.
3. The amorphous nanocrystalline alloy according to claim 1, characterized in that the coercivity of the amorphous nanocrystalline alloy is < 5A/m.
And/or, the maximum magnetic flux density of the amorphous nanocrystalline alloy is 1-1.2T.
4. The amorphous nanocrystalline alloy according to claim 1, wherein the amorphous nanocrystalline alloy has a remanence < 100mT.
And/or, the rectangle ratio of the amorphous nanocrystalline alloy is less than 8%.
5. A method for preparing the amorphous nanocrystalline alloy according to any one of claims 1 to 4, comprising the steps of:
s1: preparing materials according to alloy components, vacuum smelting to obtain molten steel after the materials are prepared, and preserving the heat of the molten steel to form an alloy cast ingot after the heat preservation is finished;
s2: and (3) annealing the alloy ingot, and cooling after annealing to obtain the amorphous nanocrystalline alloy.
6. The method of producing an amorphous nanocrystalline alloy according to claim 5, wherein in step S1, the temperature of the vacuum melting is 1200 to 1300 ℃;
and/or the vacuum degree of the vacuum smelting is 15-20Pa.
7. The method of producing an amorphous nanocrystalline alloy according to claim 5, wherein in step S1, the temperature of the heat preservation is 1000 to 1150 ℃;
and/or the time when the heat preservation is finished is the complete melting of the alloy raw material.
8. The method of producing an amorphous nanocrystalline alloy according to claim 5, wherein in step S2, the temperature of the annealing treatment is 550 to 600 ℃;
and/or the annealing treatment time is 10-15min.
9. The method of producing an amorphous nanocrystalline alloy according to claim 5, wherein in step S2, the cooled atmosphere is a vacuum atmosphere;
and/or the vacuum degree of the vacuum environment is 15Pa to 20Pa;
and/or the temperature of the vacuum environment is 10-15 ℃.
10. Use of the amorphous nanocrystalline alloy according to any one of claims 1 to 4 in medium-high frequency transformers.
CN202311050324.1A 2023-08-21 2023-08-21 Amorphous nanocrystalline alloy and preparation method and application thereof Pending CN117051337A (en)

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