CN106298141A - A kind of Fe-based nanocrystalline magnetically soft alloy material and preparation method thereof - Google Patents

A kind of Fe-based nanocrystalline magnetically soft alloy material and preparation method thereof Download PDF

Info

Publication number
CN106298141A
CN106298141A CN201610888758.2A CN201610888758A CN106298141A CN 106298141 A CN106298141 A CN 106298141A CN 201610888758 A CN201610888758 A CN 201610888758A CN 106298141 A CN106298141 A CN 106298141A
Authority
CN
China
Prior art keywords
alloy
magnetically soft
alloy material
nanocrystalline magnetically
based nanocrystalline
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201610888758.2A
Other languages
Chinese (zh)
Inventor
沈宝龙
汤永田
范星都
江沐风
江向荣
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
LONDERFUL NEW MATERIAL TECHNOLOGY CORP.
Southeast University
Original Assignee
Southeast University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Southeast University filed Critical Southeast University
Priority to CN201610888758.2A priority Critical patent/CN106298141A/en
Publication of CN106298141A publication Critical patent/CN106298141A/en
Pending legal-status Critical Current

Links

Classifications

    • 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
    • H01F1/15316Amorphous metallic alloys, e.g. glassy metals based on Co
    • 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
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/14Ferrous alloys, e.g. steel alloys containing titanium or zirconium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/16Ferrous alloys, e.g. steel alloys containing copper
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/18Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/32Ferrous alloys, e.g. steel alloys containing chromium with boron
    • 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
    • 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
    • H01F1/1535Preparation processes therefor by powder metallurgy, e.g. spark erosion

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Electromagnetism (AREA)
  • Dispersion Chemistry (AREA)
  • Power Engineering (AREA)
  • Soft Magnetic Materials (AREA)
  • Hard Magnetic Materials (AREA)

Abstract

The present invention relates to a kind of Fe-based nanocrystalline magnetically soft alloy material, it is characterised in that alloy composition meets molecular formula FeaCobNicZrdBeCuf, in formula, subscript a, b, c, d, e, f represent the atomic percent of corresponding alloying element respectively, and meet following condition: 44≤a≤88,0≤b≤44,0≤c≤44,5≤d≤10,1≤e≤5,0.5≤f≤1.5, a+b+c+d+e+f=100.Described alloy material is by body-centered cubic α (Fe, Co, Ni) the nanocrystal phase composition of noncrystal substrate and average grain size about 10nm.Compared with prior art, it is an advantage of the current invention that this nanometer crystal alloy has high saturated magnetic induction, high-curie temperature and low loss concurrently, and reduce the cost of raw material, have a good application prospect the most in high temperature environments.

Description

A kind of Fe-based nanocrystalline magnetically soft alloy material and preparation method thereof
Technical field
The present invention relates to a kind of Fe-based nanocrystalline magnetically soft alloy material, the invention still further relates to this nanocrystalline magnetically soft alloy material Preparation method.
Background technology
Soft magnetic materials is a human development class magnetic functional material the earliest, possesses higher pcrmeability, saturated magnetization strong The characteristics such as degree and resistivity.Nano crystal soft magnetic material is a novel soft magnetic materials of class, and it is by noncrystal substrate and is distributed in matrix On have nano-grade size crystal grain composition, can be obtained by non-crystaline amorphous metal is partially-crystallized.Nano crystal soft magnetic material has low rectifying The multiple advantages such as stupid power, high magnetic permeability and low-loss, can meet each class of electronic devices and develop to aspect energy-efficient, integrated Demand, and prepare easily, with low cost, be referred to as " third generation soft magnetism " material.
Research to nano-crystal soft magnetic alloy starts from 1988, and through the research of more than 30 years, current nano-crystal soft-magnetic closed Gold mainly has three individual system: FeSiBMCu (M=Nb, Mo, W, Ta etc.) to be that FINEMET alloy, FeMB (M=Zr, Hf, Nb etc.) are NANOPERM alloy and (Fe, Co) MBCu (M=Zr, Hf, Nb etc.) are HITPERM alloy.
FINEMET alloy have low-loss, high magnetic permeability and saturation magnetostriction constant level off to zero feature, and perm Alloy, Co base noncrystal alloy material are equally matched.Extensively apply though FINEMET alloy has obtained, but its saturation magnetization phase To relatively low, limit its range of application to a certain extent.NANOPERM alloy saturation magnetization is higher, and combination property is too late FINEMET alloy.FINEMET and NANOPERM alloy is owing to being limited by its amorphous phase and nanometer crystalline phase Curie temperature, only Less than 200 DEG C can be used in, will lose magnetism under hot environment.HITPERM alloy, has higher saturation induction density And Curie temperature, its high frequency characteristics is also superior to NANOPERM alloy, but coercivity is up to 70A/m, is lost the highest, thus limits It is in the application of high-temperature field.
Chinese patent CN102254665A discloses a kind of ferrum cobalt-based nanometer crystal alloy and preparation method thereof.The chemistry of alloy Composition be FeCoMBCu, M be Nb, one or more in Zr, Hf, Mo, W, Ta, concrete atomic percentage conc is Fe=40 42.8%, Co=40 42.8%, M=5 8%, B=5 12%, Cu=0.1 1.5%.This alloy has high saturated magnetic strength concurrently Answer intensity and high Curie temperature.But, in this alloy, the element percentage content of Co is the highest, is 40%~42.8%, High Co content makes this cost of alloy costly.
Magnetic material is had higher requirement by Aeronautics and Astronautics and developing rapidly of science and techniques of defence.The most electronic space flight The rotor material of the integrated power device of aircraft requires high temperature soft magnet performance and the heat stability with excellence, and operating temperature exists Between 500~600 DEG C.Electromotor within nuclear power station reactor and the magnetic material in generating set require can be in hot conditions Lower long-time military service.Therefore research has high saturation and magnetic intensity, low-loss and high-curie temperature concurrently, can make in high temperature environments With, the nano crystal soft magnetic material that the cost of raw material is cheap simultaneously is most important.
Summary of the invention
Technical problem: the present invention is directed to the above-mentioned state of the art and provide a kind of Fe-based nanocrystalline magnetically soft alloy material, this material Material has the excellent soft magnet performance such as high saturated magnetic induction, high-curie temperature and low high-frequency loss, receives with existing simultaneously Rice peritectic alloy is compared, and reduces the cost of raw material.
Technical scheme: the alloy composition of a kind of Fe-based nanocrystalline magnetically soft alloy material of the present invention meets molecular formula: FeaCobNicZrdBeCuf, in formula, subscript a, b, c, d, e, f represent the atomic percent of corresponding alloying element respectively, and meet Following condition: 44≤a≤88,0≤b≤44,0≤c≤44,5≤d≤10,1≤e≤5,0.5≤f≤1.5, and a+b+c+d + e+f=100.
Wherein:
The atomic percent of Fe is preferably 52.8≤a≤79.2.
The atomic percent of Co is preferably 8.8≤b≤35.2.
The atomic percent of Ni is preferably 8.8≤c≤26.4.
Described is nanocrystalline, and its structure includes noncrystal substrate and nanometer crystalline phase, and wherein nanometer crystalline phase is body-centered cubic structure α (Fe, Co, Ni), its average grain size about 10nm.
The saturation induction density of this alloy material is 1.54 1.79T, and coercivity is 7 28A/m.
Wherein the loss under the conditions of 1.0T, 50Hz, 10kHz of this alloy material is respectively 0.68 1.78W/kg and 465 875W/kg。
Wherein the loss under the conditions of 0.2T, 20kHz, 100kHz of this alloy is respectively 70 152W/kg and 433 1204W/ kg。
The preparation method of the Fe-based nanocrystalline magnetically soft alloy material of the present invention comprises the following steps:
Step 1: by Fe, Co, Ni, Zr, B and the Cu in alloy compositions according to alloy ingredient FeaCobNicZrdBeCuf Carrying out dispensing, in formula, subscript a, b, c, d, e, f represent the atomic percent of corresponding alloying element respectively, and meet following bar Part: 44≤a≤88,0≤b≤44,0≤c≤44,5≤d≤10,1≤e≤5,0.5≤f≤1.5, a+b+c+d+e+f=100, The most each material purity is all higher than 99%;
Step 2: raw material step 1 prepared loads in smelting furnace, carries out melting under inert atmosphere protection, after cooling To the uniform mother alloy ingot of composition;
Step 3: above-mentioned mother alloy ingot is broken for fritter sample, leaves nozzle bottom the alloy pig loading after crushing Quartz ampoule in, prepare continuous print non-crystaline amorphous metal by single roller chilling method;Non-crystaline amorphous metal is ribbon, and width is 1 2mm, Thickness is 20 25 μm;
Step 4: described non-crystaline amorphous metal is loaded in heat-treatment furnace, is evacuated to less than 1 × 10‐2Pa, is carried out at crystallization heat Reason, is then quickly quenching into room temperature, obtains nanocrystalline magnetically soft alloy material;Annealing temperature is 530 570 DEG C, temperature retention time of annealing It it is 45 75 minutes.
Beneficial effect: compared with prior art, it is an advantage of the current invention that:
(1), in the Fe-based nanocrystalline magnetically soft alloy that the present invention provides, add part with a small amount of Co and Ni simultaneously and replace Fe, subtract Lack the content of precious metal element in HITPERM alloy, greatly reduce the cost of raw material;
(2) have the Fe-based nanocrystalline magnetically soft alloy of alloy of the present invention composition not only possess high saturation induction density, High Curie temperature, also has relatively low coercivity and high-frequency loss, and wherein saturation induction density is up to 1.79T, Ju Liwen Degree is more than 900 DEG C, and coercivity is less than 28A/m, preferably 7 20A/m.For HITPERM alloy, there is the present invention The Fe-based nanocrystalline magnetically soft alloy of alloy composition reduces more than 40% in the iron loss of 1.0T, 10kHz;
(3) method preparing this nanocrystalline magnetically soft alloy material that the present invention provides is simple to operation, the alloy material prepared Material structure includes noncrystal substrate and nanometer crystalline phase, and wherein nanometer crystalline phase is the α (Fe, Co, Ni) of body-centered cubic structure, nanometer Jingjing particle size meansigma methods is less than 20nm, preferably 10nm.
Accompanying drawing explanation
Fig. 1 is (Fe in the embodiment of the present invention 10.7Co0.2Ni0.1)88Zr7B4Cu1Non-crystaline amorphous metal and the X-ray of nanometer crystal alloy Diffracting spectrum;
Fig. 2 is (Fe in the embodiment of the present invention 10.7Co0.2Ni0.1)88Zr7B4Cu1The DSC curve of non-crystaline amorphous metal;
Fig. 3 is (Fe in the embodiment of the present invention 10.7Co0.2Ni0.1)88Zr7B4Cu1The hysteresis curve of nanometer crystal alloy;
Fig. 4 is (Fe in the embodiment of the present invention 10.7Co0.2Ni0.1)88Zr7B4Cu1Nanometer crystal alloy is lost with magnetic induction Change curve;
Fig. 5 is (Fe in the embodiment of the present invention 20.8Co0.1Ni0.1)88Zr7B4Cu1Nanometer crystal alloy is lost with magnetic induction Change curve.
Detailed description of the invention
The molecular formula of the Fe-based nanocrystalline magnetically soft alloy material that the present invention provides is: FeaCobNicZrdBeCuf, subscript in formula A, b, c, d, e, f represent the atomic percentage conc of each corresponding element, 44≤a≤88,0≤b≤44,0≤c≤44,5≤d respectively ≤ 10,1≤e≤5,0.5≤f≤1.5, and a+b+c+d+e+f=100.
As preferably, the atomic percent of described Fe is preferably 52.8≤a≤79.2.
As preferably, the atomic percent of described Co is preferably 8.8≤b≤35.2.
As preferably, the atomic percent of described Ni is preferably 8.8≤c≤26.4.
Present invention also offers a kind of method preparing above-mentioned Fe-based nanocrystalline magnetically soft alloy material, comprise the steps:
Step 1: by Fe, Co, Ni, Zr, B and the Cu in alloy compositions according to alloy ingredient FeaCobNicZrdBeCuf Carrying out dispensing, subscript a, b, c, d, e, f represent the atomic percent of corresponding alloying element respectively, meet following condition: 44≤a≤ 88,0≤b≤44,0≤c≤44,5≤d≤10,1≤e≤5,0.5≤f≤1.5, and a+b+c+d+e+f=100;
Step 2: raw material step 1 prepared loads in smelting furnace, carries out melting under inert atmosphere protection, after cooling To the uniform mother alloy ingot of composition;
Step 3: mother alloy ingot is broken for fritter sample, leaves the stone of nozzle bottom the alloy pig loading after crushing Ying Guanzhong, prepares continuous print non-crystaline amorphous metal by single roller chilling method;
Step 4: described non-crystaline amorphous metal is loaded in heat-treatment furnace, is evacuated to less than 1 × 10‐2Pa, is carried out at crystallization heat Reason, is then quickly quenching into room temperature, obtains nanocrystalline magnetically soft alloy material.
As preferably, in described step 1, element of Fe, the purity of Co, Ni, Zr, B and Cu are all not less than 99wt.%.
As preferably, in described step 2, smelting temperature is 1,300 1800 DEG C.
As preferably, in described step 2, smelting time is 20 40 minutes.
As preferably, in described step 3, described non-crystaline amorphous metal is ribbon, and strip width is 1 2mm, thickness It is 25 30 μm.
As preferably, in described step 4, crystallization and thermal treatment process is: carried out in vacuum atmosphere by non-crystaline amorphous metal Temperature crystallization and thermal treatment, is then quickly quenching into room temperature.
As preferably, in described step 4, annealing temperature is 510 570 DEG C.
As preferably, in described step 4, annealing time is 30 90 minutes, more preferably 45 75 minutes.
With embodiment, the present invention is described in further detail below in conjunction with the accompanying drawings, it should be pointed out that the following stated is real Execute example and be intended to be easy to the understanding of the present invention, and it is not played any restriction effect.
Embodiment 1:
In the present embodiment, the molecular formula of the iron-base nanometer crystal alloy of high saturated magnetic induction high-curie temperature is expressed as (Fe0.7Co0.2Ni0.1)88Zr7B4Cu1, preparation process is as follows:
(1) by purity more than 99% raw material Fe, Co, Ni, Zr, B, Cu press the present embodiment chemical molecular formula prepare 15g;
(2) use arc-melting furnace by step (1) institute preparation raw material melt back five times under argon shield, make in alloy Each composition mix homogeneously;
(3) mother alloy ingot is broken for fritter sample, bottom the alloy pig loading after crushing, leaves the quartz of nozzle Guan Zhong, uses single roller chilling to get rid of band technology, gets rid of band with the speed of 40m/s in an ar atmosphere, prepare AMORPHOUS ALLOY RIBBONS;
(4) described non-crystaline amorphous metal is loaded in heat-treatment furnace, be evacuated to less than 5 × 10‐3Pa, is incubated 1 hour at 540 DEG C Rear quartz ampoule is put into quenching-in water is cooled to room temperature rapidly, obtains nanocrystalline magnetically soft alloy material.
Use the state alloy strip and through step quenched that D8Advance type polycrystal X ray diffractometer testing procedure (3) prepares (4) the XRD figure spectrum of the alloy strip after heat treatment, result is as shown in Figure 1, it is seen that, state of quenching band is non crystalline structure, after heat treatment Alloy bar with obvious crystallization peak, the internal crystallization of alloy is described.Through analyze this Crystallization Phases be body-centred cubic α (Fe, Co, Ni) phase, estimates its crystallite dimension about 11nm by Scherrer formula.
Use the DSC of state alloy strip of quenching prepared for NETZSCH DSC 404F3 differential scanning calorimeter measuring process (3) Curve, heating rate arranges 40 DEG C/min, and result is as in figure 2 it is shown, record the initial crystallization temperature T of AMORPHOUS ALLOY RIBBONSx1For 491 DEG C, secondary crystallization temperature Tx2Being 691 DEG C, the transition temperature of bcc fcc phase in opposite directions, i.e. Curie temperature reaches 858 DEG C.
Vibrating specimen magnetometer (VSM, Lakeshore 7407) is used to measure nanocrystalline after step (4) heat treatment The hysteresis curve of alloy strip uses DC magnetizing characteristic analyser (B H Curve Tracer, EXPH 100) to measure through step Suddenly the coercivity of the nanometer crystal alloy band after (4) heat treatment.Test result is as it is shown on figure 3, record the saturated magnetization of this alloy Intensity is 1.66T, and coercivity is 17A/m.
Fig. 4 show alloy after step (4) heat treatment and is lost with magnetic induction change curve.Loss uses exchange Magnetization characteristic analyser (B H Curve Tracer, AC BH 100k) is measured, for beta alloy at different magnetic induction And the loss under different frequency, it can be seen that alloy loss under magnetic strength 1.0T, frequency 50Hz is 0.93W/kg.Utilize this friendship Stream magnetization characteristic analyser measurement alloy is at magnetic strength 1.0T, and the loss under the conditions of frequency 10kHz is 532W/kg, at magnetic strength 0.2T, Loss under the conditions of frequency 20kHz, 100kHz is respectively 88W/kg, 600W/kg.
Embodiment 2:
In the present embodiment, the molecular formula of the iron-base nanometer crystal alloy of high saturated magnetic induction high-curie temperature is expressed as (Fe0.8Co0.1Ni0.1)88Zr7B4Cu1, preparation process is as follows:
(1) by purity more than 99% raw material Fe, Co, Ni, Zr, B, Cu press the present embodiment chemical molecular formula prepare 15g;
(2) use arc-melting furnace by step (1) institute preparation raw material melt back five times under argon shield, make in alloy Each composition mix homogeneously;
(3) mother alloy ingot is broken for fritter sample, bottom the alloy pig loading after crushing, leaves the quartz of nozzle Guan Zhong, uses single roller chilling to get rid of band technology, gets rid of band with the speed of 40m/s in an ar atmosphere, prepare AMORPHOUS ALLOY RIBBONS;
(4) described non-crystaline amorphous metal is loaded in heat-treatment furnace, be evacuated to less than 5 × 10‐3Pa, is incubated 1 hour at 500 DEG C Rear quartz ampoule is put into quenching-in water is cooled to room temperature rapidly, obtains nanocrystalline magnetically soft alloy material.
Vibrating specimen magnetometer (VSM, Lakeshore 7407) is used to measure nanocrystalline after step (4) heat treatment The hysteresis curve of alloy strip uses DC magnetizing characteristic analyser (B H Curve Tracer, EXPH 100) to measure through step Suddenly the coercivity of the nanometer crystal alloy band after (4) heat treatment, the saturation magnetization recording this alloy is 1.60T, coercivity For 9A/m.
Fig. 5 show alloy after step (4) heat treatment and is lost with magnetic induction change curve.Loss uses exchange Magnetization characteristic analyser (B H Curve Tracer, AC BH 100k) is measured, for beta alloy at different magnetic induction And the loss under different frequency, it can be seen that alloy loss under magnetic strength 1.0T, frequency 50Hz is 0.82W/kg.Utilize this friendship Stream magnetization characteristic analyser measurement alloy is at magnetic strength 1.0T, and the loss under the conditions of frequency 10kHz is 519W/kg, at magnetic strength 0.2T, Loss under the conditions of frequency 20kHz, 100kHz is respectively 70W/kg, 433W/kg.
Embodiment 3:
In the present embodiment, the molecular formula of the iron-base nanometer crystal alloy of high saturated magnetic induction high-curie temperature is expressed as (Fe0.6Co0.3Ni0.1)88Zr7B4Cu1, preparation process is as follows:
(1) by purity more than 99% raw material Fe, Co, Ni, Zr, B, Cu press the present embodiment chemical molecular formula prepare 15g;
(2) use arc-melting furnace by step (1) institute preparation raw material melt back five times under argon shield, make in alloy Each composition mix homogeneously;
(3) mother alloy ingot is broken for fritter sample, bottom the alloy pig loading after crushing, leaves the quartz of nozzle Guan Zhong, uses single roller chilling to get rid of band technology, gets rid of band with the speed of 40m/s in an ar atmosphere, prepare AMORPHOUS ALLOY RIBBONS;
(4) described non-crystaline amorphous metal is loaded in heat-treatment furnace, be evacuated to less than 5 × 10‐3Pa, is incubated 1 hour at 520 DEG C Rear quartz ampoule is put into quenching-in water is cooled to room temperature rapidly, obtains nanocrystalline magnetically soft alloy material.
Vibrating specimen magnetometer (VSM, Lakeshore 7407) is used to measure nanocrystalline after step (4) heat treatment The hysteresis curve of alloy strip uses DC magnetizing characteristic analyser (B H Curve Tracer, EXPH 100) to measure through step Suddenly the coercivity of the nanometer crystal alloy band after (4) heat treatment.The saturation magnetization recording this alloy is 1.62T, coercivity For 25A/m.
Loss uses ac magnetization specificity analysis instrument (B H Curve Tracer, AC BH 100k) to measure through step (4) after heat treatment, alloy is lost with magnetic induction change curve.Record this alloy at magnetic strength 1.0T, frequency 50Hz, 10kHz bar Loss under part is respectively 1.68W/kg, 785W/kg, and the loss under the conditions of magnetic strength 0.2T, frequency 20kHz, 100kHz is respectively For 107W/kg, 886W/kg.
Above-described embodiment has carried out system detailed description to technical solution of the present invention, it should be understood that upper described example is only For the specific embodiment of the present invention, it is not limited to the present invention.All made in spirit of the present invention any amendment, benefit Fill or equivalent etc., should be included within the scope of the present invention.

Claims (9)

1. a Fe-based nanocrystalline magnetically soft alloy material, it is characterised in that the alloy composition of this nanocrystalline magnetically soft alloy material meets Molecular formula: FeaCobNicZrdBeCuf, in formula, subscript a, b, c, d, e, f represent the atomic percent of corresponding alloying element respectively, and And meet following condition: 44≤a≤88,0≤b≤44,0≤c≤44,5≤d≤10,1≤e≤5,0.5≤f≤1.5, and a + b+c+d+e+f=100.
2. Fe-based nanocrystalline magnetically soft alloy material as claimed in claim 1, it is characterised in that the atomic percent of Fe is preferably 52.8≤a≤79.2。
3. Fe-based nanocrystalline magnetically soft alloy material as claimed in claim 1, it is characterised in that the atomic percent of Co is preferably 8.8≤b≤35.2。
4. Fe-based nanocrystalline magnetically soft alloy material as claimed in claim 1, it is characterised in that the atomic percent of Ni is preferably 8.8≤c≤26.4。
5. Fe-based nanocrystalline magnetically soft alloy material as claimed in claim 1, it is characterised in that described is nanocrystalline, its structure bag Including noncrystal substrate and nanometer crystalline phase, wherein nanometer crystalline phase is the α (Fe, Co, Ni) of body-centered cubic structure, its average grain size About 10nm.
6. the Fe-based nanocrystalline magnetically soft alloy material as described in any claim in Claims 1-4, it is characterised in that this conjunction The saturation induction density of gold copper-base alloy is 1.54 1.79T, and coercivity is 7 28A/m.
7. the Fe-based nanocrystalline magnetically soft alloy material as described in any claim in Claims 1-4, it is characterised in that this conjunction Gold copper-base alloy loss under the conditions of 1.0T, 50Hz, 10kHz is respectively 0.68 1.78W/kg and 465 875W/kg.
8. the Fe-based nanocrystalline magnetically soft alloy material as described in any claim in Claims 1-4, it is characterised in that this conjunction Gold loss under the conditions of 0.2T, 20kHz, 100kHz is respectively 70 152W/kg and 433 1204W/kg.
9. a preparation method for the Fe-based nanocrystalline magnetically soft alloy material as described in any claim in Claims 1-4, It is characterized in that the method comprises the following steps:
Step 1: by Fe, Co, Ni, Zr, B and the Cu in alloy compositions according to alloy ingredient FeaCobNicZrdBeCufCarry out Dispensing, in formula, subscript a, b, c, d, e, f represent the atomic percent of corresponding alloying element respectively, and meet following condition: 44 ≤ a≤88,0≤b≤44,0≤c≤44,5≤d≤10,1≤e≤5,0.5≤f≤1.5, a+b+c+d+e+f=100, wherein Each material purity is all higher than 99%;
Step 2: raw material step 1 prepared loads in smelting furnace, carries out melting, become after cooling under inert atmosphere protection Divide uniform mother alloy ingot;
Step 3: above-mentioned mother alloy ingot is broken for fritter sample, leaves the stone of nozzle bottom the alloy pig loading after crushing Ying Guanzhong, prepares continuous print non-crystaline amorphous metal by single roller chilling method;Non-crystaline amorphous metal is ribbon, and width is 1 2mm, thickness It is 20 25 μm;
Step 4: described non-crystaline amorphous metal is loaded in heat-treatment furnace, is evacuated to less than 1 × 10‐2Pa, carries out crystallization and thermal treatment, and After be quickly quenching into room temperature, obtain nanocrystalline magnetically soft alloy material;Annealing temperature is 530 570 DEG C, and annealing temperature retention time is 45 75 minutes.
CN201610888758.2A 2016-10-11 2016-10-11 A kind of Fe-based nanocrystalline magnetically soft alloy material and preparation method thereof Pending CN106298141A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610888758.2A CN106298141A (en) 2016-10-11 2016-10-11 A kind of Fe-based nanocrystalline magnetically soft alloy material and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610888758.2A CN106298141A (en) 2016-10-11 2016-10-11 A kind of Fe-based nanocrystalline magnetically soft alloy material and preparation method thereof

Publications (1)

Publication Number Publication Date
CN106298141A true CN106298141A (en) 2017-01-04

Family

ID=57718317

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610888758.2A Pending CN106298141A (en) 2016-10-11 2016-10-11 A kind of Fe-based nanocrystalline magnetically soft alloy material and preparation method thereof

Country Status (1)

Country Link
CN (1) CN106298141A (en)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108624852A (en) * 2017-03-15 2018-10-09 南京理工大学 A kind of ferrozirconium amorphous multilayer film of high-curie temperature and preparation method thereof
CN109778082A (en) * 2019-01-24 2019-05-21 南京航空航天大学 A kind of Fe-based amorphous alloy and its preparation method and application of high/low temperature annealing toughness
CN113363042A (en) * 2021-06-05 2021-09-07 合泰盟方电子(深圳)股份有限公司 Thin film inductance material, preparation method thereof and double-sided thin film inductor
CN115608996A (en) * 2021-07-28 2023-01-17 中国科学院宁波材料技术与工程研究所 Iron-based nanocrystalline magnetically soft alloy powder and preparation method thereof
CN117430373A (en) * 2023-12-21 2024-01-23 朗峰新材料启东有限公司 Anti-interference nanocrystalline composite magnetic core material and preparation method thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101080788A (en) * 2004-12-17 2007-11-28 日立金属株式会社 Magnetic core for current transformer, current transformer and watthour meter
CN101432827A (en) * 2006-04-28 2009-05-13 日立金属株式会社 Magnetic core for current transformer, current transformer, and watt-hour meter

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101080788A (en) * 2004-12-17 2007-11-28 日立金属株式会社 Magnetic core for current transformer, current transformer and watthour meter
CN101432827A (en) * 2006-04-28 2009-05-13 日立金属株式会社 Magnetic core for current transformer, current transformer, and watt-hour meter

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
K.E.KNIPLING,ET AL: "Nanocrystalline Fe8-22xCoxNixZr7B4Cu1 alloys: Soft magnets for vehicle electrification technologies (invited)", 《JOURNAL OF APPLIED PHYSICS》 *
K.SUZUKI,ET AL: "High saturation magnetization and soft magnetic properties of bcc Fe-Zr-B and Fe-Zr-B-M(M=Transition Metal) alloys with nanoscale grain size", 《MATERIALS TRANSACTIONS》 *

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108624852A (en) * 2017-03-15 2018-10-09 南京理工大学 A kind of ferrozirconium amorphous multilayer film of high-curie temperature and preparation method thereof
CN108624852B (en) * 2017-03-15 2020-04-10 南京理工大学 high-Curie-temperature Fe-Zr amorphous multilayer film and preparation method thereof
CN109778082A (en) * 2019-01-24 2019-05-21 南京航空航天大学 A kind of Fe-based amorphous alloy and its preparation method and application of high/low temperature annealing toughness
CN113363042A (en) * 2021-06-05 2021-09-07 合泰盟方电子(深圳)股份有限公司 Thin film inductance material, preparation method thereof and double-sided thin film inductor
CN113363042B (en) * 2021-06-05 2022-05-20 合泰盟方电子(深圳)股份有限公司 Thin film inductance material, preparation method thereof and double-sided thin film inductor
CN115608996A (en) * 2021-07-28 2023-01-17 中国科学院宁波材料技术与工程研究所 Iron-based nanocrystalline magnetically soft alloy powder and preparation method thereof
CN115608996B (en) * 2021-07-28 2024-05-03 中国科学院宁波材料技术与工程研究所 Iron-based nanocrystalline magnetically soft alloy powder and preparation method thereof
CN117430373A (en) * 2023-12-21 2024-01-23 朗峰新材料启东有限公司 Anti-interference nanocrystalline composite magnetic core material and preparation method thereof
CN117430373B (en) * 2023-12-21 2024-02-23 朗峰新材料启东有限公司 Anti-interference nanocrystalline composite magnetic core material and preparation method thereof

Similar Documents

Publication Publication Date Title
Takenaka et al. Industrialization of nanocrystalline Fe–Si–B–P–Cu alloys for high magnetic flux density cores
CN102543347B (en) A kind of Fe-based nanocrystalline magnetically soft alloy and preparation method thereof
CN104087833B (en) Fe-based nanocrystalline magnetically soft alloy that high frequency performance is excellent and preparation method thereof
Wang et al. Composition design of high Bs Fe-based amorphous alloys with good amorphous-forming ability
CN101834046B (en) High saturation magnetization intensity Fe-based nanocrystalline magnetically soft alloy material and preparation method thereof
CN104934179B (en) Fe-based nanocrystalline magnetically soft alloy of strong amorphous formation ability and preparation method thereof
CN106298141A (en) A kind of Fe-based nanocrystalline magnetically soft alloy material and preparation method thereof
CN102304669B (en) Iron-based nanocrystalline soft magnetic alloy with high saturation magnetic induction and low cost
CN106756643B (en) A kind of iron-based amorphous and nanocrystalline soft magnetic alloy and preparation method thereof
CN106756644B (en) A kind of iron-based amorphous and nanocrystalline soft magnetic alloy and preparation method thereof based on element silicon
CN102719746A (en) Iron-based nanocrystalline magnetically soft alloy material and preparation method thereof
Kikuchi et al. Magnetic properties of ferromagnetic shape memory alloys Ni2Mn1− xFexGa
CN103489555A (en) Iron-based nano-crystalline soft magnetic alloy and method for manufacturing same
CN106119739A (en) Iron-based amorphous and nanocrystalline soft magnetic alloy and preparation method thereof
CN106917042A (en) A kind of high frequency high magnetic flux density Fe-based nanocrystalline magnetically soft alloy and preparation method thereof
CN109440021A (en) A kind of iron-based amorphous and nanocrystalline soft magnetic alloy and its preparation method and application
CN103602931A (en) Iron-based amorphous nanocrystalline soft magnetic alloy and preparation method thereof
CN105741998A (en) Toughness-enhanced iron-based bulk amorphous soft magnetic alloy and preparation method thereof
CN109930080A (en) A kind of no copper nanocrystallite magnetically soft alloy and preparation method thereof
CN109295401A (en) A kind of new iron-based amorphous and nanocrystalline soft magnetic alloy and preparation method thereof
CN102945719A (en) High-performance ferric-based nano-crystalline soft magnetic alloy and preparation method thereof
CN109112434A (en) A kind of new iron-based amorphous and nanocrystalline soft magnetic alloy and preparation method thereof
Lu et al. Microstructure and magnetic properties of Fe72. 5Cu1M2V2Si13. 5B9 (M= Nb, Mo,(NbMo),(MoW)) nanocrystalline alloys
CN105655079B (en) A kind of Fe-based nanocrystalline magnetically soft alloy material and preparation method thereof
Stoica et al. [(Fe 0.5 Co 0.5) 0.75 B 0.20 Si 0.05] 96 Nb 4 Metallic Glasses with Small Cu Additions

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
TA01 Transfer of patent application right

Effective date of registration: 20170411

Address after: 210088 Nanjing, Pukou, Taishan District, East Village Road, No. 6

Applicant after: Southeast University

Applicant after: LONDERFUL NEW MATERIAL TECHNOLOGY CORP.

Address before: 210088 Nanjing, Jiangsu, Pukou District, Taishan village, East Road, No. 6

Applicant before: Southeast University

TA01 Transfer of patent application right
RJ01 Rejection of invention patent application after publication

Application publication date: 20170104

RJ01 Rejection of invention patent application after publication