CN110172599A - Heavy rare earth compound diffusion is for high saturation and magnetic intensity manganese bismuth melt spun alloy method - Google Patents

Heavy rare earth compound diffusion is for high saturation and magnetic intensity manganese bismuth melt spun alloy method Download PDF

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CN110172599A
CN110172599A CN201910410112.7A CN201910410112A CN110172599A CN 110172599 A CN110172599 A CN 110172599A CN 201910410112 A CN201910410112 A CN 201910410112A CN 110172599 A CN110172599 A CN 110172599A
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rare earth
alloy
melt spun
heavy rare
diffusion
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涂元浩
吴琼
李进婷
泮敏翔
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China Jiliang University
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    • 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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/02—Making non-ferrous alloys by melting
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C12/00—Alloys based on antimony or bismuth
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
    • C23C10/28—Solid state diffusion of only metal elements or silicon into metallic material surfaces using solids, e.g. powders, pastes
    • C23C10/30—Solid state diffusion of only metal elements or silicon into metallic material surfaces using solids, e.g. powders, pastes using a layer of powder or paste on the surface
    • 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
    • H01F1/032—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 hard-magnetic materials
    • H01F1/04—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 hard-magnetic materials metals or alloys
    • H01F1/047—Alloys characterised by their composition
    • H01F1/053—Alloys characterised by their composition containing rare earth metals
    • H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/059—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and Va elements, e.g. Sm2Fe17N2
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus 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
    • H01F41/02—Apparatus 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
    • H01F41/0253—Apparatus 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 for manufacturing permanent magnets
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus 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
    • H01F41/02—Apparatus 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
    • H01F41/0253—Apparatus 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 for manufacturing permanent magnets
    • H01F41/0293—Apparatus 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 for manufacturing permanent magnets diffusion of rare earth elements, e.g. Tb, Dy or Ho, into permanent magnets

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Power Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

The invention discloses a kind of heavy rare earth with compound diffusion for the method for high saturation and magnetic intensity manganese bismuth melt spun alloy, manganese bismuth melt spun alloy is made by the step of ingredient-melting-coarse crushing-fast quenching-low temperature diffusion annealing, the heavy rare earth fluorides such as fluorination terbium, dysprosium fluoride are coated in MnxBi100‑xMelt spun alloy surface, heavy rare earth compound uniformly coat melt spun alloy surface, and covering is complete, rare earth element can be achieved in diffusion process uniformly to diffuse in the lattice of manganese bismuth molecule, to stablize low-temperature phase, the saturation magnetization of manganese bismuth alloy is improved, increase rate is up to 200% or more；Compared with traditional low-temperature phase acquisition modes, present invention process process is simple, easy to operate, reduces production cost.

Description

Heavy rare earth compound diffusion is for high saturation and magnetic intensity manganese bismuth melt spun alloy method
Technical field
The invention belongs to material science and technology fields, and in particular to a kind of preparation method of high-performance MnBi permanent-magnet alloy, The especially heavy rare earth compound low temperature diffusion method for preparing high saturation and magnetic intensity MnBi permanent-magnet alloy.
Background technique
With the rapid development of science and technology, especially in the fields such as automobile, aerospace, various extreme environmental conditions Under, there is tightened up requirement for a variety of materials.Material of the permanent magnet as most important functions, in national economy and science and technology neck Domain application is more and more wider.The magnetic property of Nd-Fe-B magnet Yin Qigao and good mechanical performance at present, by the concern of people. But since the Curie temperature of NdFeB magnet is only 318 DEG C, operating temperature greatly be below 100 DEG C, therefore greatly limit its The use of high-temperature.Mn-Bi permanent-magnet alloy Curie temperature has positive coercive force temperature coefficient characteristic up to 360 DEG C, Intrinsic coercivity is still up to 25.8kOe at 280 DEG C, would be particularly applicable under hot environment use, therefore extensive by people Research and concern.But since when peritectic reaction occurs for 719K, Mn atom is easy to from MnBi Liquid Phase Segregation, very MnBi alloy Pure single-phase MnBi is seldom arrived, its saturation magnetization is directly affected.
Since two kinds of manganese, bismuth melting point metal temperature difference are larger, molten metal mobility is poor so that low-temperature phase content compared with It is few, it is next often through Low Temperature Heat Treatment annealing, discharge plasma sintering etc. (is greater than 24 hours) for a long time in actual production Low-temperature phase content is improved, while waste of manpower and material resources, still not can guarantee the content of low-temperature phase.
Summary of the invention
The purpose of the present invention is to provide a kind of heavy rare earth to obtain high saturation and magnetic intensity manganese bismuth fast quenching with compound diffusion The method of alloy, to solve the problems mentioned in the above background technology.
The method of the third element doping is to improve another method of MnBi low-temperature phase content.Wherein heavy rare earth element is mixed The miscellaneous stability that low-temperature phase can be improved.The present invention proposes that a kind of method using heavy rare earth compound diffusion prepares high-performance manganese Bismuth melt spun alloy.It will be fluorinated the heavy rare earth fluorides such as terbium, dysprosium fluoride under oxygen-free environment and be coated in manganese bismuth melt spun alloy surface, so It is handled afterwards by low temperature diffusion so that heavy rare earth element is diffused into an atomic fashion in the lattice of manganese bismuth molecule, makes terbium element Being uniformly distributed in the alloy, improves the stability of low-temperature phase, significantly improves the saturation magnetization of melt spun alloy.
To achieve the above object, the present invention provides following specific technical solution:
A kind of method that heavy rare earth obtains high saturation and magnetic intensity manganese bismuth melt spun alloy with compound diffusion, comprises the steps of:
1) ingredient: according to nominal composition MnxBi100-x, molar fraction x=45,50,55, use purity for 99.99% or more Mn, Bi alloy carry out weighing and burden；
2) melting: the raw material prepared is put into electric arc furnace under protection of argon gas using arc melting method, melting obtains MnxBi100-xAlloy cast ingot；
3) coarse crushing: by Mn made from step 2xBi100-xAlloy cast ingot is crushed；
4) fast quenching: by Mn made from step 3)xBi100-xAlloy cast ingot fragment be put into injection bore be 0.5mm quartz injection-tube in, Instrument vacuum degree is better than 10-3Pa before fast melt-quenching, and the argon gas being then charged in 0.6Pa or so makees protection gas, carries out fast melt-quenching Get rid of band；
5) low temperature diffusion is annealed: by Mn made from step 4)xBi100-xRapid tempering belt coats fluorination terbium, dysprosium fluoride under oxygen-free environment Equal heavy rare earth fluorides are diffused processing, and diffusion temperature is 150 DEG C ~ 250 DEG C, and diffusion time is 3 ~ 5 hours, and final acquisition is high Saturation magnetization manganese bismuth melt spun alloy；
Wherein, Mn, Bi alloy of 99.99% or more purity are used to ensure final manganese bismuth purity；Electric arc melting link uses argon Gas shielded starvation participates in reaction, to reduce alloy purity and destroy reaction product；
Preferably, the heavy rare earth fluoride in step 5) is fluorination terbium or dysprosium fluoride.
Compared with prior art, the present invention has the advantage that
(1) heavy rare earth fluorides such as terbium, dysprosium fluoride will be fluorinated and is coated in MnxBi100-xMelt spun alloy surface, heavy rare earth compound are equal Completely, the crystalline substance that rare earth element uniformly diffuses to manganese bismuth molecule can be achieved in even cladding melt spun alloy surface, covering in diffusion process In lattice, to stablize low-temperature phase, the saturation magnetization of manganese bismuth alloy is improved, increase rate is up to 200% or more；
(2) compared with traditional low-temperature phase acquisition modes, present invention process process is simple, easy to operate, reduces production cost.
Specific embodiment
Below with reference to embodiment, the present invention will be further described.
The following examples are intended to illustrate the invention, but cannot be used to limit the scope of the invention.Item in embodiment Part can be adjusted according to actual conditions are further, under concept thereof of the invention all to method simple modifications of the invention Belong to the scope of protection of present invention.
Embodiment 1:
1) ingredient: according to nominal composition Mn45Bi55, Mn, the Bi for being 99.99% or more using purity is raw materials, progress weighing and burden；
2) melting: the raw material prepared is put into electric arc furnace under protection of argon gas using arc melting method, melting obtains Mn45Bi55Alloy；
3) coarse crushing: by Mn made from step 245Bi55Alloy cast ingot is crushed；
4) fast quenching: by Mn made from step 3)45Bi55Alloy cast ingot fragment be put into injection bore be 0.5mm quartz injection-tube in, Instrument vacuum degree is better than 10-3Pa before fast melt-quenching, and the argon gas being then charged in 0.6Pa or so makees protection gas, carries out fast melt-quenching Get rid of band；
5) low temperature diffusion is annealed: by Mn made from step 4)45Bi55Melt spun alloy is in the coating fluorination terbium progress under oxygen-free environment In the case of DIFFUSION TREATMENT, annealing temperature is 250 DEG C, and diffusion time is 3 hours, final to obtain manganese bismuth melt spun alloy；
Reference examples 1:
1) ingredient: according to nominal composition Mn45Bi55, Mn, the Bi for being 99.99% or more using purity is raw materials, progress weighing and burden；
2) melting: the raw material prepared is put into electric arc furnace under protection of argon gas using arc melting method, melting obtains Mn45Bi55Alloy cast ingot；
3) coarse crushing: by Mn made from step 245Bi55Alloy cast ingot is crushed；
4) fast quenching: by Mn made from step 3)45Bi55Alloy cast ingot fragment be put into injection bore be 0.5mm quartz injection-tube in, Instrument vacuum degree is better than 10-3Pa before fast melt-quenching, and the argon gas being then charged in 0.6Pa or so makees protection gas, carries out fast melt-quenching Get rid of band；
5) low-temperature annealing: by Mn made from step 4)45Bi55Rapid tempering belt is made annealing treatment, and annealing temperature is 250 DEG C, when diffusion Between be 3 hours, it is final to obtain manganese bismuth melt spun alloy；
Sample prepared by above two method is tested its magnetic property using vibrating specimen magnetometer.Comparing result As shown in table 1.
Table 1
Embodiment 2:
1) ingredient: according to nominal composition Mn50Bi50, Mn, the Bi for being 99.99% or more using purity is raw materials, progress weighing and burden；
2) melting: the raw material prepared is put into electric arc furnace under protection of argon gas using arc melting method, melting obtains Mn50Bi50Alloy cast ingot；
3) coarse crushing: by Mn made from step 250Bi50Alloy cast ingot is crushed；
4) fast quenching: by Mn made from step 3)50Bi50Alloy cast ingot fragment be put into injection bore be 0.5mm quartz injection-tube in, Instrument vacuum degree is better than 10-3Pa before fast melt-quenching, and the argon gas being then charged in 0.6Pa or so makees protection gas, carries out fast melt-quenching Get rid of band；
5) low temperature diffusion is annealed: by Mn made from step 4)50Bi50Melt spun alloy coats dysprosium fluoride under oxygen-free environment and is expanded Processing is dissipated, diffusion temperature is 200 DEG C, and diffusion time is 4 hours, final to obtain manganese bismuth melt spun alloy；
Comparative example 2:
1) ingredient: according to nominal composition Mn50Bi50.Mn, the Bi for being 99.99% or more using purity carry out weighing and burden as raw material；
2) melting: the raw material prepared is put into electric arc furnace under protection of argon gas using arc melting method, melting obtains Mn50Bi50Alloy cast ingot；
3) coarse crushing: by Mn made from step 250Bi50Alloy cast ingot is crushed；
4) fast quenching: by Mn made from step 3)50Bi50Alloy cast ingot fragment be put into injection bore be 0.5mm quartz injection-tube in, Instrument vacuum degree is better than 10-3Pa before fast melt-quenching, and the argon gas being then charged in 0.6Pa or so makees protection gas, carries out fast melt-quenching Get rid of band；
5) low-temperature annealing: by Mn made from step 4)50Bi50Melt spun alloy is made annealing treatment, and annealing temperature is 200 DEG C, annealing Time is 4 hours, final to obtain manganese bismuth melt spun alloy；
Sample prepared by above two method is tested its magnetic property using vibrating specimen magnetometer.Comparing result As shown in table 2.
Table 2
Embodiment 3:
1) ingredient: according to nominal composition Mn55Bi45, Mn, the Bi for being 99.99% or more using purity is raw materials, progress weighing and burden；
2) melting: the raw material prepared is put into electric arc furnace under protection of argon gas using arc melting method, melting obtains Mn55Bi45Alloy cast ingot；
3) coarse crushing: by Mn made from step 255Bi45Alloy cast ingot is crushed；
4) fast quenching: by Mn made from step 3)55Bi45Alloy cast ingot fragment be put into injection bore be 0.5mm quartz injection-tube in, Instrument vacuum degree is better than 10-3Pa before fast melt-quenching, and the argon gas being then charged in 0.6Pa or so makees protection gas, carries out fast melt-quenching Get rid of band；
5) low temperature diffusion is annealed: by Mn made from step 4)55Bi45Melt spun alloy coats fluorination terbium under oxygen-free environment and is expanded Dissipating processing diffusion temperature is 150 DEG C, and diffusion time is 5 hours, final to obtain manganese bismuth melt spun alloy.
Reference examples 3:
1) ingredient: according to nominal composition Mn55Bi45, Mn, the Bi for being 99.99% or more using purity is raw materials, progress weighing and burden；
2) melting: the raw material prepared is put into electric arc furnace under protection of argon gas using arc melting method, melting obtains Mn55Bi45Alloy cast ingot；
3) coarse crushing: by Mn made from step 255Bi45Alloy cast ingot is crushed；
4) fast quenching: by Mn made from step 3)55Bi45Alloy cast ingot fragment be put into injection bore be 0.5mm quartz injection-tube in, Instrument vacuum degree is better than 10-3Pa before fast melt-quenching, and the argon gas being then charged in 0.6Pa or so makees protection gas, carries out fast melt-quenching Get rid of band；
5) it anneals: by Mn made from step 4)55Bi45Melt spun alloy is made annealing treatment, and annealing temperature is 150 DEG C, diffusion time It is 5 hours, it is final to obtain manganese bismuth melt spun alloy；
Sample prepared by above two method is tested its magnetic property using vibrating specimen magnetometer.Comparing result As shown in table 3.
Table 3
In the various embodiments described above, manganese bismuth fast quenching is made by the step of ingredient-melting-coarse crushing-fast quenching-low temperature diffusion annealing Alloy, only last annealing steps do not use low temperature diffusion to anneal in each reference examples (prior art), but use common annealing side Legal system obtains manganese bismuth melt spun alloy, by the saturation magnetization data for testing each manganese bismuth melt spun alloy, it was therefore concluded that: use this hair The saturation magnetization for the manganese bismuth melt spun alloy that bright heavy rare earth is obtained with compound method of diffusion is extremely with respect to common annealing method 31%(Mn is improved less55Bi45), up to 206%(Mn45Bi55)；Compared with traditional low-temperature phase acquisition modes, present invention process mistake Journey is simple, easy to operate, reduces production cost.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding And modification, the scope of the present invention is defined by the appended.

Claims (3)

1. a kind of heavy rare earth is with compound diffusion for the method for high saturation and magnetic intensity manganese bismuth melt spun alloy, it is characterised in that packet Include following steps:
1) ingredient: according to nominal composition MnxBi100-x, x is molar fraction, use purity for 99.99% or more Mn, Bi alloy Carry out weighing and burden；
2) melting: the raw material prepared is put into electric arc furnace under protection of argon gas using arc melting method, melting obtains MnxBi100-xAlloy cast ingot；
3) coarse crushing: by Mn made from step 2xBi100-xAlloy cast ingot is crushed；
4) fast quenching: by Mn made from step 3)xBi100-xAlloy cast ingot fragment be put into injection bore be 0.5mm quartz injection-tube in, Instrument vacuum degree is better than 10-3Pa before fast melt-quenching, and the argon gas being then charged in 0.6Pa or so makees protection gas, carries out fast melt-quenching Get rid of band；
5) low temperature diffusion is annealed: MnxBi100-x rapid tempering belt made from step 4) is coated heavy rare earth fluoride under oxygen-free environment It is diffused processing, diffusion temperature is 150 DEG C ~ 250 DEG C, and diffusion time is 3 ~ 5 hours, final to obtain high saturation and magnetic intensity manganese Bismuth melt spun alloy.
2. a kind of heavy rare earth according to claim 1 is with compound diffusion for high saturation and magnetic intensity manganese bismuth melt spun alloy Method, which is characterized in that the molar fraction x=45,50,55.
3. a kind of heavy rare earth according to claim 1 is with compound diffusion for high saturation and magnetic intensity manganese bismuth melt spun alloy Method, which is characterized in that heavy rare earth fluoride in step 5) is fluorination terbium or dysprosium fluoride.
CN201910410112.7A 2019-05-16 2019-05-16 Heavy rare earth compound diffusion is for high saturation and magnetic intensity manganese bismuth melt spun alloy method Pending CN110172599A (en)

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Application publication date: 20190827