CN109295401A - A kind of new iron-based amorphous and nanocrystalline soft magnetic alloy and preparation method thereof - Google Patents

A kind of new iron-based amorphous and nanocrystalline soft magnetic alloy and preparation method thereof Download PDF

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CN109295401A
CN109295401A CN201811512188.2A CN201811512188A CN109295401A CN 109295401 A CN109295401 A CN 109295401A CN 201811512188 A CN201811512188 A CN 201811512188A CN 109295401 A CN109295401 A CN 109295401A
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alloy
based amorphous
soft magnetic
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nanocrystalline soft
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张超汉
陶平均
杨元政
李东洋
黄文豪
朱坤森
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Guangdong University of Technology
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Guangdong University of Technology
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    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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    • B22D11/06Continuous casting of metals, i.e. casting in indefinite lengths into moulds with travelling walls, e.g. with rolls, plates, belts, caterpillars
    • B22D11/0611Continuous casting of metals, i.e. casting in indefinite lengths into moulds with travelling walls, e.g. with rolls, plates, belts, caterpillars formed by a single casting wheel, e.g. for casting amorphous metal strips or wires
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    • 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
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    • C21D6/001Heat treatment of ferrous alloys containing Ni
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    • 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
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    • C21D9/00Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/52Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for wires; for strips ; for rods of unlimited length
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    • 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
    • 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
    • H01F1/15341Preparation processes therefor
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    • H01F41/00Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
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    • 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
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Abstract

The invention belongs to magnetically soft alloy technical fields more particularly to a kind of new iron-based amorphous and nanocrystalline soft magnetic alloy and preparation method thereof.The present invention provides a kind of new iron-based amorphous and nanocrystalline soft magnetic alloy, chemical formula Fe73.5‑xSi13.5B9Cu1Nb3Nix.The present invention also provides the preparation methods of above-mentioned alloy, comprising the following steps: step 1: by iron, silicon, boron source, copper, niobium and Ni-B alloy at alloy pig;Step 2: the alloy pig being crushed and obtains broken alloy pig, cleaning;Step 3: the broken alloy pig is obtained into alloy thin band by getting rid of band legal system;Step 4: the alloy thin band being heat-treated to obtain new iron-based amorphous and nanocrystalline soft magnetic alloy.The present invention provides a kind of new iron-based amorphous and nanocrystalline soft magnetic alloy and preparation method thereof, the technical issues of large-scale application for solving Fe-based amorphous nanocrystalline alloy in the prior art is severely limited.

Description

A kind of new iron-based amorphous and nanocrystalline soft magnetic alloy and preparation method thereof
Technical field
The invention belongs to magnetically soft alloy technical field more particularly to a kind of new iron-based amorphous and nanocrystalline soft magnetic alloy and its Preparation method.
Background technique
With being constantly progressive for society, due to computer network, high density recording technology, electric system and the micro- chinaware of high frequency The development in the fields such as part and needs increasingly require various components used to have high-performance, high-quality, small-sized, light weight, this Require that preparing the Metallic Functional Materials such as the magnetically soft alloy of these devices is continuously improved performance.Fe-based amorphous/nano-crystal soft-magnetic closes Fitting has the features such as excellent soft magnet performance, such as high saturated magnetic induction, low-coercivity, high magnetic permeability, low-loss, many decades Being the research hotspot in material and Condensed Matter Physics field always.In addition, the preparation work of Fe-based amorphous/nano-crystal soft magnetic alloy Skill is simple, low in cost, is widely used in fields such as transformer, inductor, sensors.Structure and performance according to material Feature is currently roughly divided into two major classes in the amorphous and nanocrystalline soft magnetic alloy studied or applied: i.e.: 1) having high saturation magnetic induction The amorphous or nanometer crystal alloy of intensity are answered, mainly includes iron SiB system's amorphous alloy and iron SiBPCu system nano-crystal alloy.Iron SiB It is amorphous alloy performance characteristics is that saturation induction density is higher, about 1.4-1.7T, other than Bs, performance is better than silicon steel.Closely The iron SiBPCu nanometer crystal alloy of exploitation in several years, maximum feature are high Bs, generally about 1.8-1.9T, are much larger than iron SiB Amorphous alloy.And high Bs can reduce the usage amount of material, reduce cost, reduce device volume.But high Fe content iron The amorphous formation ability of SiBPCu nanometer crystal alloy is lower, it is difficult to prepare large-sized amorphous band.2) there is high initial magnetic It is alloy, Nanoperm (iron MB, M=Zr, Hf, Nb that the nanometer crystal alloy of conductance, which mainly includes Finemet (iron SiBCuNb), Deng) it is alloy and HITPERM (iron CoMB, M=Zr, Hf, Nb etc.) is alloy.Wherein, though Finemet alloy have it is excellent soft Magnetic property, but because iron content is lower, typical composition iron73.5Si13.5B9Cu1Nb3Saturation induction density be only 1.25T limits the application in the power electronic devices to miniaturization to a certain extent.And Nanoperm system with Hitperm system alloy is although saturation induction density with higher and magnetostriction coefficient level off to zero, a large amount of easy oxygen Change noble metal Zr, the elements such as Hf exist, increase producting process difficulty, limit its application field to a certain extent.Therefore, existing In some Fe-based amorphous nanocrystalline alloy systems, lower amorphous formation ability and low saturation induction density make Fe-based amorphous The large-scale application of nanometer crystal alloy is seriously constrained to the technical problem urgently to be resolved for those skilled in the art.
Summary of the invention
In view of this, being solved the present invention provides a kind of new iron-based amorphous and nanocrystalline soft magnetic alloy and preparation method thereof The technical issues of large-scale application of Fe-based amorphous nanocrystalline alloy receives serious limitation in the prior art.
The present invention provides a kind of new iron-based amorphous and nanocrystalline soft magnetic alloy, chemical formula Fe73.5- xSi13.5B9Cu1Nb3Nix;Wherein, 0≤x≤3.
The present invention also provides a kind of preparation methods of new iron-based amorphous and nanocrystalline soft magnetic alloy, comprising the following steps:
Step 1: will be by iron, silicon, boron source, copper, niobium and Ni-B alloy at alloy pig;
Step 2: the alloy pig being crushed and obtains broken alloy pig, cleaning;
Step 3: the broken alloy pig is obtained into alloy thin band by getting rid of band legal system;
Step 4: the alloy thin band being annealed to obtain new iron-based amorphous and nanocrystalline soft magnetic alloy.
Preferably, the width of the alloy thin band is 1~2mm;The alloy thin band with a thickness of
20~40 μm.
Preferably, the number of melting described in step 1 is 4~6 times.
Preferably, the temperature of the melting is 1100~1350 DEG C.
Preferably, the boron source includes boron and/or ferro-boron.
Preferably, the temperature of the annealing is 540~560 DEG C.
Preferably, the heating rate of the annealing is 20 DEG C/min.
Preferably, the time of the annealing is 60min.
Preferably, the chilling roller linear velocity got rid of with method is 45~55m/s.
Demand for development of the present invention for existing Fe-based amorphous nanocrystalline alloy system lightweight, miniaturization, design one The novel iron-based amorphous and nanocrystalline soft magnetic alloy with low cost, high saturated magnetic induction and low-coercivity of kind, the present invention are real New iron-based amorphous/the Nanoalloy for applying example preparation has strong amorphous formation ability, high saturated magnetic induction and low coercive The excellent soft magnet performance such as power.By adding a small amount of Co, Ni, one of Al and Gd metallic element greatly optimize alloy Amorphous formation ability, the shortcomings that improving the toughness and low saturation induction density of alloy strip steel rolled stock.Preparation of the embodiment of the present invention New iron-based amorphous and nanocrystalline soft magnetic alloy is the structure of completely amorphous state by XRD analysis.Its saturation magnetization energy Reach 1.58T, coercivity can be reduced to 3.6A/m, effectively optimize the soft magnet performance of FeSiBCuNb system amorphous alloy.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this Some embodiments of invention without any creative labor, may be used also for those of ordinary skill in the art To obtain other attached drawings according to these attached drawings.
Fig. 1 is the process flow diagram of the new iron-based amorphous and nanocrystalline soft magnetic alloy of preparation of the embodiment of the present invention;
Fig. 2 is the X-ray diffractogram of amorphous thin ribbon prepared by the embodiment of the present invention 1~3;
Fig. 3 is the magnetization curve figure of new iron-based amorphous and nanocrystalline soft magnetic alloy prepared by the embodiment of the present invention 1~3;
Fig. 4 is that the coercivity of new iron-based amorphous and nanocrystalline soft magnetic alloy prepared by the embodiment of the present invention 1~3 changes song Line.
Specific embodiment
The following is a clear and complete description of the technical scheme in the embodiments of the invention, it is clear that described embodiment Only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, the common skill in this field Art personnel every other embodiment obtained without making creative work belongs to the model that the present invention protects It encloses.
The present invention provides a kind of new iron-based amorphous and nanocrystalline soft magnetic alloys and preparation method thereof, solve the prior art The technical issues of large-scale application of middle Fe-based amorphous nanocrystalline alloy receives serious limitation.Fig. 1 prepares iron-based non-for the present invention The process flow diagram of brilliant nano-crystal soft magnetic alloy.
Embodiment 1
New iron-based amorphous and nanocrystalline soft magnetic alloy manufactured in the present embodiment is Fe72.5Si13.5B9Cu1Nb3Ni1
(1) prepared by master alloy raw material: pressing Fe72.5Si13.5B9Cu1Nb3Ni1Atomic percent is converted to quality hundred by chemical formula Divide ratio, weighs Fe (99.9%), FeB (17.51%) alloy, Si (99%) block, Cu (99.9%) block, Nb respectively in proportion (99.9%) block and Ni (99.9%).
(2) foundry alloy melting: the raw material prepared is put into vacuum arc melting furnace, is evacuated to 5 × 10 to furnace body-3Afterwards It is filled with argon gas/nitrogen atmosphere protection and closes charging valve when air pressure in furnace is higher than atmospheric pressure 0.01Mpa.It is former to heat melting Material continues melting 3 minutes, is subsequently cooled to solidify, repeat melting 4 times, obtain after quickly being overturn after raw material is completely melt To the uniform alloy pig of ingredient.
(3) alloy pig cleans: alloy pig being broken for fritter alloy, and is put into the beaker equipped with ethyl alcohol or acetone and carries out Cleaning.
(4) prepared by amorphous thin ribbon: will be fitted into the quartz ampoule of lower ending opening after the cleaning of fritter alloy, is subsequently placed in and gets rid of band and set In standby induction coil, it is evacuated to 5 × 10-3Being filled with purity afterwards is 99.99% high-purity argon gas as protective gas, adjusts electricity Stream makes alloy melting, during which controls temperature at 1250 DEG C, controls the time 2 minutes, when alloy melting and when there is white light, utilizes gas Alloy under molten condition is ejected into the copper roller surface that revolving speed is 50m/s by pressure difference, and obtained width is about 1mm, and thickness is about 20 μ The amorphous ribbon strip of m.
(5) structure detection is carried out to alloy strip steel rolled stock with X-ray diffractometer, so that it is determined that the glass of alloy to form energy Power.Referring to fig. 2, Fig. 2 is the X-ray diffractogram of the amorphous thin ribbon of preparation of the embodiment of the present invention.As shown in Figure 2, complete amorphous State band about has the diffraction maximums of widthization disperse at 45 °, and in other ranges without obvious sharp crystallization peak.
(6) Crystallizing treatment: amorphous thin ribbon being put into heat-treatment furnace and is made annealing treatment, and is warming up to 440 DEG C with furnace, heat preservation Strip is taken out after then cooling to room temperature with the furnace, is obtained Fe-based amorphous wherein being 20 DEG C/min with furnace heating rate by 10min Nanometer crystal alloy.
The Fe-based amorphous nanocrystalline alloy prepared to the embodiment of the present invention 1 detects.
With magnetic detection equipment (vibrating specimen magnetometer VSM and soft magnetism DC test instrument) to the strip after annealing respectively into Row saturation induction density (Ms) and coercivity (Hc) performance test.Gained performance parameter is as shown in the picture, wherein Bs=4 π × (ρ×Ms)×10-4(T)。
Referring to Fig. 3, Fig. 3 is the magnetization curve of the new iron-based amorphous and nanocrystalline soft magnetic alloy of preparation of the embodiment of the present invention Figure.Referring to fig. 4, Fig. 4 is that the coercitive variation of the new iron-based amorphous and nanocrystalline soft magnetic alloy of preparation of the embodiment of the present invention is bent Line.The result shows that iron-based amorphous and nanocrystalline soft magnetic alloy Fe prepared by the embodiment of the present invention 172.5Si13.5B9Cu1Nb3Ni1, Saturation magnetization is 1.58T, coercivity 6.8A/m.
Embodiment 2
New iron-based amorphous and nanocrystalline soft magnetic alloy manufactured in the present embodiment is Fe71.5Si13.5B9Cu1Nb3Ni2,It is prepared Step includes:
(1) prepared by master alloy raw material: pressing Fe71.5Si13.5B9Cu1Nb3Ni2Atomic percent is converted to quality hundred by chemical formula Divide ratio, weighs Fe (99.9%), FeB (17.51%) alloy, Si (99%) block, Cu (99.9%) block, Nb respectively in proportion (99.9%) block and Ni (99.9%).
(2) foundry alloy melting: the raw material prepared is put into vacuum arc melting furnace, is evacuated to 5 × 10 to furnace body-3Afterwards It is filled with argon gas/nitrogen atmosphere protection and closes charging valve when air pressure in furnace is higher than atmospheric pressure 0.01Mpa.It is former to heat melting Material continues melting 3 minutes, is subsequently cooled to solidify, repeat melting 4 times, obtain after quickly being overturn after raw material is completely melt To the uniform alloy pig of ingredient.
(3) alloy pig cleans: alloy pig being broken for fritter alloy, and is put into the beaker equipped with ethyl alcohol or acetone and carries out Cleaning.
(4) prepared by amorphous thin ribbon: will be fitted into the quartz ampoule of lower ending opening after the cleaning of fritter alloy, is subsequently placed in and gets rid of band and set In standby induction coil, it is evacuated to 5 × 10-3Being filled with purity afterwards is 99.99% high-purity argon gas as protective gas, adjusts electricity Stream makes alloy melting, during which controls temperature at 1250 DEG C, controls the time 2 minutes, when alloy melting and when there is white light, utilizes gas Alloy under molten condition is ejected into the copper roller surface that revolving speed is 50m/s by pressure difference, and obtained width is about 1mm, and thickness is about 20 μ The amorphous ribbon strip of m.
(5) structure detection is carried out to alloy strip steel rolled stock with X-ray diffractometer, so that it is determined that the glass of alloy to form energy Power.Referring to fig. 2, Fig. 2 is the X-ray diffractogram of the amorphous thin ribbon of preparation of the embodiment of the present invention.As shown in Figure 2, complete amorphous State band about has the diffraction maximums of widthization disperse at 45 °, and in other ranges without obvious sharp crystallization peak.
(6) Crystallizing treatment: amorphous thin ribbon being put into heat-treatment furnace and is made annealing treatment, and is warming up to 440 DEG C with furnace, heat preservation Strip is taken out after then cooling to room temperature with the furnace, is obtained Fe-based amorphous wherein being 20 DEG C/min with furnace heating rate by 10min Nanometer crystal alloy.
The Fe-based amorphous nanocrystalline alloy prepared to the embodiment of the present invention 2 detects.
With magnetic detection equipment (vibrating specimen magnetometer VSM and soft magnetism DC test instrument) to the strip after annealing respectively into Row saturation induction density (Ms) and coercivity (Hc) performance test.Gained performance parameter is as shown in the picture, wherein Bs=4 π × (ρ×Ms)×10-4(T)。
Referring to the magnetization curve figure for the Fe-based amorphous nanocrystalline alloy that Fig. 3, Fig. 3 are preparation of the embodiment of the present invention.Referring to figure The coercitive change curve of 4, Fig. 4 Fe-based amorphous nanocrystalline alloys prepared for the embodiment of the present invention.The result shows that the present invention Iron-based amorphous and nanocrystalline soft magnetic alloy Fe prepared by embodiment 271.5Si13.5B9Cu1Nb3Ni2, saturation magnetization is 1.35T, coercivity 4.5A/m.
Embodiment 3
New iron-based amorphous and nanocrystalline soft magnetic alloy manufactured in the present embodiment is Fe70.5Si13.5B9Cu1Nb3Ni3, preparation Step includes
(1) prepared by master alloy raw material: pressing Fe70.5Si13.5B9Cu1Nb3Ni3Atomic percent is converted to quality hundred by chemical formula Divide ratio, weighs Fe (99.9%), FeB (17.51%) alloy, Si (99%) block, Cu (99.9%) block, Nb respectively in proportion (99.9%) block and Ni (99.9%).
(2) foundry alloy melting: the raw material prepared is put into vacuum arc melting furnace, is evacuated to 5 × 10 to furnace body-3Afterwards It is filled with argon gas/nitrogen atmosphere protection and closes charging valve when air pressure in furnace is higher than atmospheric pressure 0.01Mpa.It is former to heat melting Material continues melting 3 minutes, is subsequently cooled to solidify, repeat melting 4 times, obtain after quickly being overturn after raw material is completely melt To the uniform alloy pig of ingredient.
(3) alloy pig cleans: alloy pig being broken for fritter alloy, and is put into the beaker equipped with ethyl alcohol or acetone and carries out Cleaning.
(4) prepared by amorphous thin ribbon: will be fitted into the quartz ampoule of lower ending opening after the cleaning of fritter alloy, is subsequently placed in and gets rid of band and set In standby induction coil, it is evacuated to 5 × 10-3Being filled with purity afterwards is 99.99% high-purity argon gas as protective gas, adjusts electricity Stream makes alloy melting, during which controls temperature at 1250 DEG C, controls the time 2 minutes, when alloy melting and when there is white light, utilizes gas Alloy under molten condition is ejected into the copper roller surface that revolving speed is 50m/s by pressure difference, and obtained width is about 1mm, and thickness is about 20 μ The amorphous ribbon strip of m.
(5) structure detection is carried out to alloy strip steel rolled stock with X-ray diffractometer, so that it is determined that the glass of alloy to form energy Power.Referring to fig. 2, Fig. 2 is the X-ray diffractogram of the amorphous thin ribbon of preparation of the embodiment of the present invention.As shown in Figure 2, complete amorphous State band about has the diffraction maximums of widthization disperse at 45 °, and in other ranges without obvious sharp crystallization peak.
(6) Crystallizing treatment: amorphous thin ribbon being put into heat-treatment furnace and is made annealing treatment, and is warming up to 440 DEG C with furnace, heat preservation Strip is taken out after then cooling to room temperature with the furnace, is obtained Fe-based amorphous wherein being 20 DEG C/min with furnace heating rate by 10min Nanometer crystal alloy.
The Fe-based amorphous nanocrystalline alloy prepared to the embodiment of the present invention 3 detects.
With magnetic detection equipment (vibrating specimen magnetometer VSM and soft magnetism DC test instrument) to the strip after annealing respectively into Row saturation induction density (Ms) and coercivity (Hc) performance test.Gained performance parameter is as shown in the picture, wherein Bs=4 π × (ρ×Ms)×10-4(T)。
Referring to the magnetization curve figure for the Fe-based amorphous nanocrystalline alloy that Fig. 3, Fig. 3 are preparation of the embodiment of the present invention.Referring to figure The coercitive change curve of 4, Fig. 4 Fe-based amorphous nanocrystalline alloys prepared for the embodiment of the present invention.The result shows that the present invention Iron-based amorphous and nanocrystalline soft magnetic alloy Fe prepared by embodiment 370.5Si13.5B9Cu1Nb3Ni3, saturation magnetization is 1.32T, coercivity 3.6A/m.
The above is only a preferred embodiment of the present invention, it is noted that for making the professional technique of the art Personnel are that by various modifications to these embodiments without departing from the technical principles of the invention, and these Modification also should be regarded as the range that the present invention should protect.

Claims (10)

1. a kind of new iron-based amorphous and nanocrystalline soft magnetic alloy, which is characterized in that its chemical formula is Fe73.5- xSi13.5B9Cu1Nb3Nix;Wherein, 0≤x≤3.
2. a kind of preparation method of new iron-based amorphous and nanocrystalline soft magnetic alloy, which comprises the following steps:
Step 1: will be by iron, silicon, boron source, copper, niobium and Ni-B alloy at alloy pig;
Step 2: the alloy pig being crushed and obtains broken alloy pig, cleaning;
Step 3: the broken alloy pig is obtained into alloy thin band by getting rid of band legal system;
Step 4: the alloy thin band being annealed to obtain new iron-based amorphous and nanocrystalline soft magnetic alloy.
3. the preparation method of new iron-based amorphous and nanocrystalline soft magnetic alloy according to claim 2, which is characterized in that described The width of alloy thin band is 1~2mm;The alloy thin band with a thickness of 20~40 μm.
4. the preparation method of new iron-based amorphous and nanocrystalline soft magnetic alloy according to claim 2, which is characterized in that step The number of melting described in 1 is 4~6 times.
5. the preparation method of new iron-based amorphous and nanocrystalline soft magnetic alloy according to claim 2, which is characterized in that described The temperature of melting is 1100~1350 DEG C.
6. the preparation method of new iron-based amorphous and nanocrystalline soft magnetic alloy according to claim 2, which is characterized in that described Boron source includes boron and/or ferro-boron.
7. the preparation method of new iron-based amorphous and nanocrystalline soft magnetic alloy according to claim 2, which is characterized in that described The temperature of annealing is 540~560 DEG C.
8. the preparation method of new iron-based amorphous and nanocrystalline soft magnetic alloy according to claim 2, which is characterized in that described The heating rate of annealing is 20 DEG C/min.
9. the preparation method of new iron-based amorphous and nanocrystalline soft magnetic alloy according to claim 2, which is characterized in that described The time of annealing is 60min.
10. the preparation method of new iron-based amorphous and nanocrystalline soft magnetic alloy according to claim 2~9 any one, It is characterized in that, the chilling roller linear velocity got rid of with method is 45~55m/s.
CN201811512188.2A 2018-12-11 2018-12-11 A kind of new iron-based amorphous and nanocrystalline soft magnetic alloy and preparation method thereof Pending CN109295401A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112164541A (en) * 2020-10-15 2021-01-01 太原理工大学 Anti-direct-current iron-based nanocrystalline alloy and preparation method thereof
CN112877613A (en) * 2020-12-28 2021-06-01 江苏三环奥纳科技有限公司 Iron-based amorphous soft magnetic alloy and preparation method and application thereof
CN112877616A (en) * 2021-01-11 2021-06-01 秦皇岛市燕秦纳米科技有限公司 Preparation method of low-remanence amorphous nanocrystalline soft magnetic material
CN114694908A (en) * 2022-05-30 2022-07-01 天津三环奥纳科技有限公司 Low-temperature-resistant nanocrystalline magnetically soft alloy iron core, manufacturing method and application
WO2024130939A1 (en) * 2022-12-19 2024-06-27 青岛云路先进材料技术股份有限公司 Amorphous nanocrystalline soft magnetic alloy and preparation method therefor

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01247557A (en) * 1988-03-30 1989-10-03 Hitachi Metals Ltd Manufacture of hyperfine-crystal soft-magnetic alloy
CN103060722A (en) * 2011-10-21 2013-04-24 江苏奥玛德新材料科技有限公司 Iron-based amorphous or nanocrystalline soft magnetic alloy and preparation method thereof
CN104561841A (en) * 2013-10-25 2015-04-29 上海瀚涛纳米科技有限公司 High-saturation-magnetization iron-base amorphous nanocrystal soft magnetic alloy and preparation method thereof
JP2015167183A (en) * 2014-03-04 2015-09-24 Necトーキン株式会社 Nanocrystal soft magnetic alloy powder and powder-compact magnetic core arranged by use thereof
CN105074843A (en) * 2013-02-15 2015-11-18 日立金属株式会社 Annular magnetic core using Fe iron-based nanocrystalline soft-magnetic alloy and magnetic component using said annular magnetic core
CN106636981A (en) * 2016-10-28 2017-05-10 上海理工大学 Soft magnet-based amorphous alloy product
CN107365950A (en) * 2017-07-24 2017-11-21 广东咏旺新材料科技有限公司 Fe Si B Nb Cu are Fe-based amorphous/nanocrystalline magnetically soft alloy material and preparation and Technology for Heating Processing
CN107393673A (en) * 2017-07-31 2017-11-24 东莞美壹磁电科技有限公司 A kind of iron-based amorphous and nanocrystalline soft magnetic alloy and preparation method thereof
CN109440021A (en) * 2018-11-13 2019-03-08 广东工业大学 A kind of iron-based amorphous and nanocrystalline soft magnetic alloy and its preparation method and application

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01247557A (en) * 1988-03-30 1989-10-03 Hitachi Metals Ltd Manufacture of hyperfine-crystal soft-magnetic alloy
CN103060722A (en) * 2011-10-21 2013-04-24 江苏奥玛德新材料科技有限公司 Iron-based amorphous or nanocrystalline soft magnetic alloy and preparation method thereof
CN105074843A (en) * 2013-02-15 2015-11-18 日立金属株式会社 Annular magnetic core using Fe iron-based nanocrystalline soft-magnetic alloy and magnetic component using said annular magnetic core
CN104561841A (en) * 2013-10-25 2015-04-29 上海瀚涛纳米科技有限公司 High-saturation-magnetization iron-base amorphous nanocrystal soft magnetic alloy and preparation method thereof
JP2015167183A (en) * 2014-03-04 2015-09-24 Necトーキン株式会社 Nanocrystal soft magnetic alloy powder and powder-compact magnetic core arranged by use thereof
CN106636981A (en) * 2016-10-28 2017-05-10 上海理工大学 Soft magnet-based amorphous alloy product
CN107365950A (en) * 2017-07-24 2017-11-21 广东咏旺新材料科技有限公司 Fe Si B Nb Cu are Fe-based amorphous/nanocrystalline magnetically soft alloy material and preparation and Technology for Heating Processing
CN107393673A (en) * 2017-07-31 2017-11-24 东莞美壹磁电科技有限公司 A kind of iron-based amorphous and nanocrystalline soft magnetic alloy and preparation method thereof
CN109440021A (en) * 2018-11-13 2019-03-08 广东工业大学 A kind of iron-based amorphous and nanocrystalline soft magnetic alloy and its preparation method and application

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
谢春晓等: "Co/Ni摩尔比对FeCoNiCrZr非晶合金晶化过程及磁性能的影响", 《中国有色金属学报》 *
陈先朝等: "Ni/Co比例及微量Dy对FeCoNiBSiNb块体非晶合金玻璃形成能力和磁性能的影响", 《热加工工艺》 *

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112164541A (en) * 2020-10-15 2021-01-01 太原理工大学 Anti-direct-current iron-based nanocrystalline alloy and preparation method thereof
CN112877613A (en) * 2020-12-28 2021-06-01 江苏三环奥纳科技有限公司 Iron-based amorphous soft magnetic alloy and preparation method and application thereof
CN112877616A (en) * 2021-01-11 2021-06-01 秦皇岛市燕秦纳米科技有限公司 Preparation method of low-remanence amorphous nanocrystalline soft magnetic material
CN112877616B (en) * 2021-01-11 2022-06-24 秦皇岛市燕秦纳米科技有限公司 Preparation method of low-remanence amorphous nanocrystalline soft magnetic material
CN114694908A (en) * 2022-05-30 2022-07-01 天津三环奥纳科技有限公司 Low-temperature-resistant nanocrystalline magnetically soft alloy iron core, manufacturing method and application
CN114694908B (en) * 2022-05-30 2023-11-24 天津三环奥纳科技有限公司 Low-temperature-resistant nanocrystalline magnetically soft alloy iron core, manufacturing method and application
WO2024130939A1 (en) * 2022-12-19 2024-06-27 青岛云路先进材料技术股份有限公司 Amorphous nanocrystalline soft magnetic alloy and preparation method therefor

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