CN113278897B - 一种铁基纳米晶软磁合金及其制备方法 - Google Patents
一种铁基纳米晶软磁合金及其制备方法 Download PDFInfo
- Publication number
- CN113278897B CN113278897B CN202110556414.2A CN202110556414A CN113278897B CN 113278897 B CN113278897 B CN 113278897B CN 202110556414 A CN202110556414 A CN 202110556414A CN 113278897 B CN113278897 B CN 113278897B
- Authority
- CN
- China
- Prior art keywords
- equal
- iron
- less
- magnetically soft
- 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.)
- Expired - Fee Related
Links
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 115
- 239000000956 alloy Substances 0.000 title claims abstract description 89
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 81
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title abstract description 12
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 12
- 239000000126 substance Substances 0.000 claims abstract description 11
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 9
- 229910052715 tantalum Inorganic materials 0.000 claims abstract description 6
- 238000003723 Smelting Methods 0.000 claims description 22
- 238000010438 heat treatment Methods 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 20
- 230000035699 permeability Effects 0.000 claims description 13
- 238000005266 casting Methods 0.000 claims description 8
- 230000001681 protective effect Effects 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 7
- 238000010791 quenching Methods 0.000 claims description 5
- 230000000171 quenching effect Effects 0.000 claims description 5
- 229910000859 α-Fe Inorganic materials 0.000 claims description 4
- 239000004615 ingredient Substances 0.000 claims description 2
- 238000002844 melting Methods 0.000 claims description 2
- 230000008018 melting Effects 0.000 claims description 2
- 238000011161 development Methods 0.000 abstract description 6
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000008204 material by function Substances 0.000 abstract description 2
- 230000001737 promoting effect Effects 0.000 abstract description 2
- 239000010949 copper Substances 0.000 description 24
- 229910052802 copper Inorganic materials 0.000 description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical group [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 9
- 230000006698 induction Effects 0.000 description 9
- 239000002994 raw material Substances 0.000 description 9
- 229910001004 magnetic alloy Inorganic materials 0.000 description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 7
- 238000001816 cooling Methods 0.000 description 7
- 238000011160 research Methods 0.000 description 7
- 229910052796 boron Inorganic materials 0.000 description 6
- 239000010453 quartz Substances 0.000 description 6
- 229910052710 silicon Inorganic materials 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 229910052786 argon Inorganic materials 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 3
- 229910052737 gold Inorganic materials 0.000 description 3
- 239000010931 gold Substances 0.000 description 3
- 229910052735 hafnium Inorganic materials 0.000 description 3
- 239000000696 magnetic material Substances 0.000 description 3
- 238000005507 spraying Methods 0.000 description 3
- 229910052726 zirconium Inorganic materials 0.000 description 3
- 239000013078 crystal Substances 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 229910000881 Cu alloy Inorganic materials 0.000 description 1
- 229910000976 Electrical steel Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000008094 contradictory effect Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C45/00—Amorphous alloys
- C22C45/02—Amorphous alloys with iron as the major constituent
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
- B22D11/06—Continuous casting of metals, i.e. casting in indefinite lengths into moulds with travelling walls, e.g. with rolls, plates, belts, caterpillars
- B22D11/0611—Continuous 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
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING 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
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/04—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering with simultaneous application of supersonic waves, magnetic or electric fields
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING 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
- C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
- C21D9/52—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for wires; for strips ; for rods of unlimited length
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/003—Making ferrous alloys making amorphous alloys
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/04—Making ferrous alloys by melting
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/04—Making ferrous alloys by melting
- C22C33/06—Making ferrous alloys by melting using master alloys
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/12—Ferrous alloys, e.g. steel alloys containing tungsten, tantalum, molybdenum, vanadium, or niobium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/16—Ferrous alloys, e.g. steel alloys containing copper
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
- H01F1/147—Alloys characterised by their composition
- H01F1/14766—Fe-Si based alloys
- H01F1/14791—Fe-Si-Al based alloys, e.g. Sendust
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
- H01F1/147—Alloys characterised by their composition
- H01F1/153—Amorphous metallic alloys, e.g. glassy metals
- H01F1/15308—Amorphous metallic alloys, e.g. glassy metals based on Fe/Ni
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
- H01F1/147—Alloys characterised by their composition
- H01F1/153—Amorphous metallic alloys, e.g. glassy metals
- H01F1/15333—Amorphous metallic alloys, e.g. glassy metals containing nanocrystallites, e.g. obtained by annealing
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
- H01F1/147—Alloys characterised by their composition
- H01F1/153—Amorphous metallic alloys, e.g. glassy metals
- H01F1/15341—Preparation processes therefor
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C2200/00—Crystalline structure
- C22C2200/02—Amorphous
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C2200/00—Crystalline structure
- C22C2200/04—Nanocrystalline
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Metallurgy (AREA)
- Physics & Mathematics (AREA)
- Power Engineering (AREA)
- Dispersion Chemistry (AREA)
- Electromagnetism (AREA)
- Crystallography & Structural Chemistry (AREA)
- Thermal Sciences (AREA)
- Inorganic Chemistry (AREA)
- Soft Magnetic Materials (AREA)
- Continuous Casting (AREA)
Abstract
本发明属于功能材料技术领域,具体涉及一种铁基纳米晶软磁合金及其制备方法。一种铁基纳米晶软磁合金,所述铁基纳米晶软磁合金的化学式为FeaSibBcAldMeCufPg,化学式中M选自Nb、Mo和Ta中的至少两种以上;其中,70≤a≤76,10≤b≤17,7≤c≤9,0.5≤d≤2.5,1.5≤e≤4.5,0.6≤f≤1.2,0.8≤g≤1.4,a+b+c+d+e+f+g=100。本发明通过元素成分的选用以及各元素含量的优化,实现了高磁导率铁基纳米晶软磁合金同时具有非晶形成能力强、综合软磁性能优异的优点,从而大大推进了工业化生产,对铁基纳米晶软磁合金的发展具有重要的意义。
Description
技术领域
本发明属于功能材料技术领域,具体涉及一种铁基纳米晶软磁合金及其制备方法。
背景技术
铁基纳米晶软磁合金材料自问世以来,因具有高磁导率、低损耗、低矫顽力等特点而得到极大的重视和深入的研究,并广泛应用于开关电源和互感器等领域。
自1988年日立金属Yoshizawa等人发现了Fe-Si-B-Nb-Cu系合金以来,对铁基纳米晶合金材料的深入探究将软磁材料的研发推向了一个新高潮。经多年发展,铁基纳米晶软磁合金主要包括三个合金体系,即Fe-Si-B-M-Cu(M=Nb、Mo、Ta、W)系FINEMET合金、Fe-M-B-Cu(M=Zr、Hf、Nb)系NANOPERM合金和(Fe,Co)-M-B-Cu(M=Zr、Hf、Nb)系HITPERM合金。其中,NANOPERM合金虽然具有高饱和磁感应强度,但其综合软磁性能不及FINEMET合金;此外,该合金还含有大量易氧化的贵金属,如Zr、Hf、Nb等,这使其制备工艺复杂且成本高昂,至今都未能实现真正的广泛应用。在NANOPERM基础上发明的HITPERM合金体系,尽管其居里温度和饱和磁感应强度均高于NANOPERM合金,但由于合金体系中添加了大量的贵金属Co致使成本增加,所以该合金体系也未能实现广泛应用。因此,FINEMET合金体系的综合软磁性能最好且成本适中,并得到一定范围的应用。目前,在电子器件小型化以及能源利用可持续化的发展趋势下,市场迫切需求一种具有高磁导率的软磁合金材料。就铁基纳米晶软磁合金材料而言,要提高磁导率,就要尽可能地均匀化纳米晶α-Fe相尺寸和分布。因此,高磁导率与微观结构和高的热稳定性能是相互矛盾的。如何找到三者的平衡点,即以尽可能实现优异、稳定的综合软磁性能为前提,获得简化制备工艺和热处理条件的纳米晶软磁材料,是当前铁基纳米晶软磁合金材料研究中亟待解决的问题。
目前,铁基纳米晶软磁材料通过调整合金成分和优化热处理工艺在不同程度上改善了纳米晶合金材料的软磁性能,但仍然存在以下两个显著缺点:(1)热处理工艺上,对工艺要求苛刻,晶化处理保温时间太短,这极大地限制了其在工业上的应用;(2)软磁性能上,很难达到优异、稳定的综合软磁性能,实现高的磁导率。
综上所述,目前市场上缺乏热处理工艺简单,同时具备优异、稳定的软磁性能的高磁导率纳米晶软磁合金材料及其制品。因此,开发一种能通过简单热处理工艺方法获得优异、稳定软磁性能的纳米晶软磁合金对于当前铁基纳米晶软磁合金材料的研究和应用具有极其重要意义。
发明内容
鉴于以上现有技术中材料的软磁性能较差的问题,本发明的目的在于提供一种铁基纳米晶软磁合金及其制备方法,用于解决现有技术中的问题。
为实现上述目的及其他相关目的,本发明是通过以下技术方案获得的。
本发明的目的之一在于提供一种铁基纳米晶软磁合金,所述铁基纳米晶软磁合金的化学式为FeaSibBcAldMeCufPg,化学式中M选自Nb、Mo和Ta中的至少两种以上;其中,70≤a≤76,10≤b≤17,7≤c≤9,0.5≤d≤2.5,1.5≤e≤4.5,0.6≤f≤1.2,0.8≤g≤1.4,a+b+c+d+e+f+g=100。
本发明在研究中意外发现,通过掺杂Nb、Mo和/或Ta可以有效抑制晶粒的长大。
优选地,71.5≤a≤74.5。
优选地,11≤b≤16。
优选地,7.5≤c≤8.5。
优选地,0.8≤d≤1.6。
优选地,2≤e≤4。
优选地,0.7≤f≤1。
优选地,1≤g≤1.2。
优选地,所述铁基纳米晶软磁合金由非晶相和纳米晶相组成,所述纳米晶相为体心立方结构的α-Fe纳米晶相,所述纳米晶相的晶粒尺寸为11~12nm。
优选地,所述铁基纳米晶软磁合金的矫顽力小于0.4A/m,相对磁导率为100000~180000。
本发明的目的之二在于提供上述所述的铁基纳米晶软磁合金的制备方法,包括如下步骤:所述铁基纳米晶软磁合金由非晶带材在磁场中进行热处理制备获得。
优选地,所述非晶带材的宽度为2~6mm,厚度为15~30μm。
优选地,所述热处理的温度为400~580℃。本发明中温度能直接影响晶粒的尺寸,经多次试验研究发现,只有当热处理的温度为400~580℃时,得到合金的尺寸最佳。
更优选地,所述热处理的温度为450~550℃。
优选地,所述磁场的强度为0.2~0.4T。本发明中施加磁场可以诱导磁晶各向异性,提升磁导率。
优选地,所述热处理的时间为60~120min。
更优选地,所述热处理的时间为60~90min。
优选地,所述非晶带材的制备方法为:
1)按照化学式FeaSibBcAldMeCufPg中各元素的摩尔比,进行配料;
2)将步骤1)配料在保护气氛下熔炼,然后铸造得到合金锭;
3)将所述合金锭进行破碎,然后通过单辊快淬法得到非晶带材。
更优选地,步骤1)中,所述各元素的纯度为99%以上。
更优选地,步骤1)中,配料方式:
方法一:以Fe、Si、B、Al、M、Cu、P和Fe3P为原料;
方法二:以Fe23Ta2、Fe、Si、B、Al、M、Cu、P和Fe3P为原料;
方法三:以Fe、Si、B、Al、M、Cu和P为原料。
更优选地,步骤2)中,所述熔炼前先抽真空至5×10-3Pa以下,然后在保护气氛下熔炼。
更优选地,步骤2)中,所述熔炼温度为1050℃~1100℃。
更优选地,步骤2)中,所述熔炼处理时间为40~80min。
更优选地,步骤2)中,所述保护气氛为氩气。
与现有技术相比,本发明具有以下有益效果:
本发明通过元素成分的选用以及各元素含量的优化,实现了高磁导率铁基纳米晶软磁合金同时具有非晶形成能力强、综合软磁性能优异、热稳定性高的优点,从而大大推进了工业化生产,对铁基纳米晶软磁合金的发展具有重要的意义。
附图说明
图1显示为实施例1、实施例2和实施例3的XRD图。
图2显示为实施例1、实施例2和实施例3以及对比例的相对磁导率图。
图3显示为实施例1、实施例2和实施例3以及对比例的矫顽力图。
具体实施方式
以下由特定的具体实施例说明本发明的实施方式,熟悉此技术的人士可由本说明书所揭露的内容轻易地了解本发明的其他优点及功效。
在进一步描述本发明具体实施方式之前,应理解,本发明的保护范围不局限于下述特定的具体实施方案;还应当理解,本发明实施例中使用的术语是为了描述特定的具体实施方案,而不是为了限制本发明的保护范围。下列实施例中未注明具体条件的试验方法,通常按照常规条件,或者按照各制造商所建议的条件。
当实施例给出数值范围时,应理解,除非本发明另有说明,每个数值范围的两个端点以及两个端点之间任何一个数值均可选用。除非另外定义,本发明中使用的所有技术和科学术语与本技术领域技术人员通常理解的意义相同。除实施例中使用的具体方法、设备、材料外,根据本技术领域的技术人员对现有技术的掌握及本发明的记载,还可以使用与本发明实施例中所述的方法、设备、材料相似或等同的现有技术的任何方法、设备和材料来实现本发明。
本申请实施例中,采用X射线衍射法测定铁基纳米晶软磁合金的物相组成。
本申请实施例中,采用湖南联众科技有限公司的型号为MATS-3000M的硅钢铁损测试装置来测定矫顽力和磁导率。
实施例1
本实施例中,制备化学式为Fe74.5Si12B8Al1.5Nb1.5Mo0.5Cu1P1的铁基纳米晶软磁合金,包括如下步骤:
1)将纯度为99.99%的Fe、Si、B、Cu、Nb、Mo、Al纯原料以及市售Fe3P中间合金锭(含量为99.9%),按照Fe74.5Si12B8Al1.5Nb1.5Mo0.5Cu1P1进行配料。
3)将配料好的混合物放置于高频感应熔炼炉中进行熔炼,抽真空至5×10-3Pa,然后充入保护气体氩气进行熔炼,于1080℃持续熔炼60min,随后倒入铸型铜模中,冷却得到合金锭。
4)将合金锭破碎后装入底部留有喷嘴的石英管中,随后置于铸造设备感应线圈中使合金金熔融后,采用单辊快淬法,将熔融合金喷到转速为40m/s的旋转铜辊上,制备出宽度为4mm、厚度为20μm的非晶带材。
5)将非晶条带材分割为多个相同的样品,分别置于真空管式炉中,在强度为0.20T的磁场中于450℃下热处理90min,热处理结束后随炉冷至室温,得到铁基纳米晶软磁合金。其中,磁场方向平行于真空管式炉的轴向设置。
实施例2
本实施例中,制备化学式为Fe71.2Si15 B9Al1Nb0.4Mo1.6Cu0.8P1的铁基纳米晶软磁合金,包括如下步骤:
1)将纯度为99.99%的Fe、Si、B、Cu、Nb、Mo、Al纯原料以及市售Fe3P中间合金锭(含量为99.9%),按照Fe71.2Si15 B9Al1Nb0.4Mo1.6Cu0.8P1进行配料。
3)将配料好的混合物放置于高频感应熔炼炉中进行熔炼,抽真空至5×10-3Pa,然后充入保护气体氩气进行熔炼,于1080℃持续熔炼60min,随后倒入铸型铜模中,冷却得到合金锭。
4)将合金锭破碎后装入底部留有喷嘴的石英管中,随后置于铸造设备感应线圈中使合金金熔融后,采用单辊快淬法,将熔融合金喷到转速为35m/s的旋转铜辊上,制备出宽度为4mm、厚度为20μm的非晶带材。
5)将非晶条带材分割为多个相同的样品,分别置于真空管式炉中,在强度为0.30T的磁场中于500℃下热处理70min,热处理结束后随炉冷至室温,得到铁基纳米晶软磁合金。其中,磁场方向平行于真空管式炉的轴向设置。
实施例3
本实施例中,制备化学式为Fe74.5Si13.2B7Al0.8Ta1.5Nb1Cu0.8P1.2的铁基纳米晶软磁合金,包括如下步骤:
1)将高纯的Fe、Ta原料按照合金成分(原子百分比)为Fe23Ta2的比例进行配料,将配好的Fe23Ta2合金原料放入电弧熔炼炉的水冷铜坩埚内,首先抽真空至5×10-3Pa以下,然后充入适量保护气体氩气进行熔炼,熔炼均匀后随炉冷却,同样条件下重复电弧熔炼5次,得到成分均匀的Fe23Ta2中间合金锭。
2)将纯度为99.99%的Fe、Si、B、Cu、Nb、Mo、Al纯原料以及市售Fe3P中间合金锭(含量为99.9%)以及Fe23Ta2中间合金锭,按照Fe74.5Si13.2B7 Al0.8Ta1.5Nb1Cu0.8P1.2进行配料。
3)将配料好的混合物放置于高频感应熔炼炉中进行熔炼,抽真空至5×10-3Pa,然后充入保护气体氩气进行熔炼,于1080℃持续熔炼60min,随后倒入铸型铜模中,冷却得到合金锭。
4)将合金锭破碎后装入底部留有喷嘴的石英管中,随后置于铸造设备感应线圈中使合金金熔融后,采用单辊快淬法,将熔融合金喷到转速为40m/s的旋转铜辊上,制备出宽度为4mm、厚度为20μm的非晶带材。
5)将非晶条带材分割为多个相同的样品,分别置于真空管式炉中,在强度为0.40T的磁场中于540℃下热处理50min,热处理结束后随炉冷至室温,得到铁基纳米晶软磁合金。其中,磁场方向平行于真空管式炉的轴向设置。
对比例1
本对比例同实施例1,区别仅仅在于本对比例1在不施加磁场下进行热处理,其余均相同。
图1为实施例1-3所得的合金的XRD图;图2为实施例1-3以及对比例所得的合金的相对磁导率图,图3为实施例1-3以及对比例所得的合金的矫顽力图。
从图1的XRD图可知,经在磁场中热处理后的非晶带材为纳米晶结构。铁基纳米晶软磁合金由非晶基体相和纳米晶相组成,纳米晶相为体心立方结构的α-Fe纳米晶相,实施例1中的纳米晶相的晶粒尺寸为11.9nm,实施例2中的纳米晶相的晶粒尺寸为11.6nm,实施例3中的纳米晶相的晶粒尺寸为11.2nm。经研究发现,Nb、Mo、Ta的添加能够抑制铁晶粒的长大,从而细化晶粒。
从图2的磁导率图可知,与对比例相比,实施例1-3的合金均具有高相对磁导率,特别是实施例3中,在20Hz下相对磁导率高达169000。
从图3的磁导率图可知,与对比例相比,实施例1-3的合金均具有低的矫顽力,合金在磁感应强度为20Hz下,矫顽力低至0.15A/m。
上述实施例仅例示性说明本发明的原理及其功效,而非用于限制本发明。任何熟悉此技术的人士皆可在不违背本发明的精神及范畴下,对上述实施例进行修饰或改变。因此,举凡所属技术领域中具有通常知识者在未脱离本发明所揭示的精神与技术思想下所完成的一切等效修饰或改变,仍应由本发明的权利要求所涵盖。
Claims (8)
1.一种铁基纳米晶软磁合金,其特征在于,所述铁基纳米晶软磁合金的化学式为FeaSibBcAldMeCufPg,化学式中M选自Nb、Mo和Ta中的至少两种以上;其中,70≤a≤76,10≤b≤17,7≤c≤9,0.5≤d≤2.5,1.5≤e≤4.5,0.6≤f≤1.2,0.8≤g≤1.4,a+b+c+d+e+f+g=100;
所述铁基纳米晶软磁合金由非晶带材在磁场中进行热处理制备获得,
所述热处理的温度为400~580℃;
所述磁场的强度为0.2~0.4T;
所述热处理的时间为60~120min。
2.根据权利要求1所述的铁基纳米晶软磁合金,其特征在于,71.5≤a≤74.5;
和/或,11≤b≤16;
和/或,7.5≤c≤8.5;
和/或,0.8≤d≤1.6;
和/或,2≤e≤4;
和/或,0.7≤f≤1;
和/或,1≤g≤1.2。
3.根据权利要求1所述的铁基纳米晶软磁合金,其特征在于,所述铁基纳米晶软磁合金由非晶相和纳米晶相组成,所述纳米晶相为体心立方结构的α-Fe纳米晶相,所述纳米晶相的晶粒尺寸为11~12nm。
4.根据权利要求1所述的铁基纳米晶软磁合金,其特征在于,所述铁基纳米晶软磁合金的矫顽力小于0.4A/m,相对磁导率为100000~180000。
5.根据权利要求1所述的铁基纳米晶软磁合金,其特征在于,所述非晶带材的宽度为2~6mm,厚度为15~30μm。
6.根据权利要求1所述的铁基纳米晶软磁合金,其特征在于,所述非晶带材的制备方法为:
1)按照化学式FeaSibBcAldMeCufPg中各元素的摩尔比,进行配料;
2)将步骤1)配料在保护气氛下熔炼,然后铸造得到合金锭;
3)将所述合金锭进行破碎,然后通过单辊快淬法得到非晶带材。
7.根据权利要求5所述的铁基纳米晶软磁合金,其特征在于,步骤1)中,所述各元素的纯度为99%以上。
8.根据权利要求5所述的铁基纳米晶软磁合金,其特征在于,步骤2)中,所述熔炼温度为1050℃~1100℃;
和/或,所述熔炼处理时间为40~80min。
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202110556414.2A CN113278897B (zh) | 2021-05-21 | 2021-05-21 | 一种铁基纳米晶软磁合金及其制备方法 |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202110556414.2A CN113278897B (zh) | 2021-05-21 | 2021-05-21 | 一种铁基纳米晶软磁合金及其制备方法 |
Publications (2)
Publication Number | Publication Date |
---|---|
CN113278897A CN113278897A (zh) | 2021-08-20 |
CN113278897B true CN113278897B (zh) | 2022-07-19 |
Family
ID=77280544
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202110556414.2A Expired - Fee Related CN113278897B (zh) | 2021-05-21 | 2021-05-21 | 一种铁基纳米晶软磁合金及其制备方法 |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN113278897B (zh) |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111020410A (zh) * | 2019-11-13 | 2020-04-17 | 中国科学院宁波材料技术与工程研究所 | 一种铁基纳米晶软磁合金及制备方法 |
-
2021
- 2021-05-21 CN CN202110556414.2A patent/CN113278897B/zh not_active Expired - Fee Related
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111020410A (zh) * | 2019-11-13 | 2020-04-17 | 中国科学院宁波材料技术与工程研究所 | 一种铁基纳米晶软磁合金及制备方法 |
Also Published As
Publication number | Publication date |
---|---|
CN113278897A (zh) | 2021-08-20 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN102543347B (zh) | 一种铁基纳米晶软磁合金及其制备方法 | |
CN104087833B (zh) | 高频性能优良的铁基纳米晶软磁合金及其制备方法 | |
CN102304669B (zh) | 高饱和磁感应强度低成本铁基纳米晶软磁合金 | |
CN110670000B (zh) | 一种纳米晶软磁合金、非晶软磁合金及其制备方法 | |
JP7387008B2 (ja) | サブナノスケールの秩序クラスターを含む鉄基アモルファス合金、その調製方法及びそれを用いたナノ結晶合金誘導体 | |
CN106756643B (zh) | 一种铁基非晶纳米晶软磁合金及其制备方法 | |
CN109930080B (zh) | 一种无铜纳米晶软磁合金及其制备方法 | |
CN111057970B (zh) | 一种高磁导率的非晶纳米晶合金的制备方法 | |
CN110387500B (zh) | 一种高磁感高频铁基纳米晶软磁合金及其制备方法 | |
CN107393673B (zh) | 一种铁基非晶纳米晶软磁合金及其制备方法 | |
CN106756644B (zh) | 一种基于硅元素的铁基非晶纳米晶软磁合金及其制备方法 | |
CN106917042A (zh) | 一种高频高磁感应强度铁基纳米晶软磁合金及其制备方法 | |
CN106373690A (zh) | 一种具有良好工艺性能、高饱和磁感应强度的纳米晶软磁合金及其制备方法 | |
CN103602931A (zh) | 一种铁基非晶纳米晶软磁合金及其制备方法 | |
CN102936685A (zh) | 具有高饱和磁通密度的Fe基软磁合金及其制备方法 | |
CN102304680A (zh) | 一种低成本且具有优异软磁性能的铁基非晶/纳米晶薄带及其制备方法 | |
CN115732160A (zh) | 一种全金属铁基纳米晶软磁合金及其制备方法和磁芯 | |
CN111748755A (zh) | 一种新型高饱和磁感铁基软磁非晶合金及制备方法 | |
CN110670001A (zh) | 富硅含p型铁基非晶纳米晶合金及铁基非晶合金纳米晶磁芯的制备方法 | |
Zhou et al. | Excellent soft magnetic properties and enhanced glass forming ability of Fe-Si-BC-Cu nanocrystalline alloys | |
CN110093565B (zh) | 晶化窗口宽、软磁性能可控的铁基纳米晶合金及其制备方法 | |
CN113278897B (zh) | 一种铁基纳米晶软磁合金及其制备方法 | |
CN112962024B (zh) | 一种类Finemet型Fe基纳米晶软磁合金及其制备方法 | |
CN113628823B (zh) | 高耐蚀性的铁基纳米晶软磁合金及制备方法 | |
CN111485182B (zh) | 一种利用元素间正混合热制备的铁基非晶纳米晶合金及其制备方法和应用 |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant | ||
CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20220719 |
|
CF01 | Termination of patent right due to non-payment of annual fee |