CN110136952A - A kind of method that heavy rare earth obtains high saturation and magnetic intensity manganese bismuth melt spun alloy with compound diffusion - Google Patents

A kind of method that heavy rare earth obtains high saturation and magnetic intensity manganese bismuth melt spun alloy with compound diffusion Download PDF

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Publication number
CN110136952A
CN110136952A CN201910492021.2A CN201910492021A CN110136952A CN 110136952 A CN110136952 A CN 110136952A CN 201910492021 A CN201910492021 A CN 201910492021A CN 110136952 A CN110136952 A CN 110136952A
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rare earth
alloy
heavy rare
melt spun
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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China Jiliang University
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    • 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
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C22/00—Alloys based on manganese
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
    • 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
    • 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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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Power Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Hard Magnetic Materials (AREA)

Abstract

The invention discloses a kind of methods that heavy rare earth obtains high saturation and magnetic intensity manganese bismuth melt spun alloy with compound diffusion, 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

A kind of heavy rare earth obtains high saturation and magnetic intensity manganese bismuth melt spun alloy with compound diffusion 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 is below greatly 100 DEG C, therefore greatly limits it in height The use of temperature.Mn-Bi permanent-magnet alloy Curie temperature has positive coercive force temperature coefficient characteristic up to 360 DEG C, in It reports coercivity and is still up to 25.8kOe at 280 DEG C, would be particularly applicable under hot environment use, therefore widely ground by people Study carefully and pays close attention to.But since when peritectic reaction occurs for 719K, Mn atom is easy to be difficult from MnBi Liquid Phase Segregation MnBi alloy Pure single-phase MnBi is obtained, 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 heavy rare earth is obtained with compound diffusion The method of high saturation and magnetic intensity manganese bismuth melt spun alloy, comprises the steps of:
1) ingredient: according to nominal composition MnxBi100-x(molar fraction x=45,50,55), use purity be 99.99% with On 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 Obtain MnxBi100-xAlloy cast ingot；
3) coarse crushing: by Mn made from step 2)xBi100-xAlloy cast ingot is crushed；
4) fast quenching: by Mn made from step 3)xBi100-xAlloy cast ingot fragment is put into injection bore as the injection of 0.5mm quartz Guan Zhong, instrument vacuum degree is better than 10-3Pa before fast melt-quenching, and the argon gas being then charged in 0.6Pa or so is made protection gas, melted Body fast quenching gets rid of band；
5) low temperature diffusion is annealed: by Mn made from step 4)xBi100-xRapid tempering belt coats fluorination terbium, fluorine under oxygen-free environment Change the heavy rare earth fluorides such as dysprosium and be diffused processing, diffusion temperature is 150 DEG C~250 DEG C, and diffusion time is 3~5 hours, finally Obtain high saturation and magnetic intensity 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 is adopted Reaction is participated in argon gas protection starvation, 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 chemical combination Object uniformly coats melt spun alloy surface, and covering completely, can be achieved rare earth element in diffusion process and uniformly diffuse to manganese bismuth molecule Lattice in, to stablize low-temperature phase, improve the saturation magnetization of manganese bismuth alloy, 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 and is produced into This.
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 weigh as raw material Ingredient；
2) melting: the raw material prepared is put into electric arc furnace under protection of argon gas using arc melting method, melting Obtain Mn45Bi55Alloy
3) coarse crushing: by Mn made from step 2)45Bi55Alloy cast ingot is crushed；
4) fast quenching: by Mn made from step 3)45Bi55It is 0.5mm quartz injection-tube that alloy cast ingot fragment, which is put into injection bore, 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 melt Fast quenching gets rid of band；
5) low temperature diffusion is annealed: by Mn made from step 4)45Bi55Melt spun alloy is in the coating fluorination terbium under oxygen-free environment It is diffused under disposition, 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 weigh as raw material Ingredient；
2) melting: the raw material prepared is put into electric arc furnace under protection of argon gas using arc melting method, melting Obtain Mn45Bi55Alloy cast ingot；
3) coarse crushing: by Mn made from step 2)45Bi55Alloy cast ingot is crushed；
4) fast quenching: by Mn made from step 3)45Bi55It is 0.5mm quartz injection-tube that alloy cast ingot fragment, which is put into injection bore, 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 melt Fast quenching gets 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, is expanded Dissipating the time is 3 hours, final to obtain manganese bismuth melt spun alloy；
Sample prepared by above two method is tested its magnetic property using vibrating specimen magnetometer.Comparison The results are shown in Table 1.
Table 1
Serial number Classification Mn45Bi55Alloy saturation magnetization Ms (emu/g)
1 Heavy rare earth diffusion 59.884
2 Non- heavy rare earth diffusion 19.567
Embodiment 2:
1) ingredient: according to nominal composition Mn50Bi50, Mn, the Bi for being 99.99% or more using purity weigh as raw material Ingredient；
2) melting: the raw material prepared is put into electric arc furnace under protection of argon gas using arc melting method, melting Obtain Mn50Bi50Alloy cast ingot；
3) coarse crushing: by Mn made from step 2)50Bi50Alloy cast ingot is crushed；
4) fast quenching: by Mn made from step 3)50Bi50It is 0.5mm quartz injection-tube that alloy cast ingot fragment, which is put into injection bore, 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 melt Fast quenching gets rid of band；
5) low temperature diffusion is annealed: by Mn made from step 4)50Bi50Melt spun alloy coated under oxygen-free environment dysprosium fluoride into Row DIFFUSION TREATMENT, diffusion temperature are 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 weigh as raw material Ingredient；
2) melting: the raw material prepared is put into electric arc furnace under protection of argon gas using arc melting method, melting Obtain Mn50Bi50Alloy cast ingot；
3) coarse crushing: by Mn made from step 2)50Bi50Alloy cast ingot is crushed；
4) fast quenching: by Mn made from step 3)50Bi50It is 0.5mm quartz injection-tube that alloy cast ingot fragment, which is put into injection bore, 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 melt Fast quenching gets 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.Comparison The results are shown in Table 2.
Table 2
Serial number Classification Saturation magnetization Ms (T)
1 Add heavy rare earth compound 52.415
2 Do not add heavy rare earth compound 20.619
Embodiment 3:
1) ingredient: according to nominal composition Mn55Bi45, Mn, the Bi for being 99.99% or more using purity weigh as raw material Ingredient；
2) melting: the raw material prepared is put into electric arc furnace under protection of argon gas using arc melting method, melting Obtain Mn55Bi45Alloy cast ingot；
3) coarse crushing: by Mn made from step 2)55Bi45Alloy cast ingot is crushed；
4) fast quenching: by Mn made from step 3)55Bi45It is 0.5mm quartz injection-tube that alloy cast ingot fragment, which is put into injection bore, 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 melt Fast quenching gets rid of band；
5) low temperature diffusion is annealed: by Mn made from step 4)55Bi45Melt spun alloy coated under oxygen-free environment fluorination terbium into Row DIFFUSION TREATMENT 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 weigh as raw material Ingredient；
2) melting: the raw material prepared is put into electric arc furnace under protection of argon gas using arc melting method, melting Obtain Mn55Bi45Alloy cast ingot；
3) coarse crushing: by Mn made from step 2)55Bi45Alloy cast ingot is crushed；
4) fast quenching: by Mn made from step 3)55Bi45It is 0.5mm quartz injection-tube that alloy cast ingot fragment, which is put into injection bore, 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 melt Fast quenching gets 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 is 5 hours, final to obtain manganese bismuth melt spun alloy；
Sample prepared by above two method is tested its magnetic property using vibrating specimen magnetometer.Comparison The results are shown in Table 3.
Table 3
Serial number Classification Saturation magnetization Ms (T)
1 Add heavy rare earth compound 46.910
2 Do not add heavy rare earth compound 35.750
In the various embodiments described above, manganese bismuth is made by the step of ingredient-melting-coarse crushing-fast quenching-low temperature diffusion annealing Melt spun alloy, only last annealing steps do not use low temperature diffusion to anneal in each reference examples (prior art), but use and commonly move back Manganese bismuth melt spun alloy is made in ignition method, by the saturation magnetization data for testing each manganese bismuth melt spun alloy, it was therefore concluded that: it uses The saturation magnetization for the manganese bismuth melt spun alloy that heavy rare earth of the invention is obtained with compound method of diffusion is with respect to common annealing side Method at least improves 31% (Mn55Bi45), up to 206% (Mn45Bi55)；Compared with traditional low-temperature phase acquisition modes, the present invention Technical process 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 (2)

1. a kind of method that heavy rare earth obtains high saturation and magnetic intensity manganese bismuth melt spun alloy with compound diffusion, which is characterized in that It 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-x alloy cast ingot；
3) coarse crushing: MnxBi100-x alloy cast ingot made from step 2) is crushed；
4) fast quenching: it is 0.5mm quartz injection-tube that MnxBi100-x alloy cast ingot fragment made from step 3), which is put into injection bore, 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 melt Fast quenching gets 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, finally obtains high saturation and magnetic intensity Manganese bismuth melt spun alloy.
2. a kind of heavy rare earth according to claim 1 obtains high saturation and magnetic intensity manganese bismuth melt spun alloy with compound diffusion Method, which is characterized in that heavy rare earth fluoride in step 5) is fluorination terbium or dysprosium fluoride.
CN201910492021.2A 2019-06-06 2019-06-06 A kind of method that heavy rare earth obtains high saturation and magnetic intensity manganese bismuth melt spun alloy with compound diffusion Pending CN110136952A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106544630A (en) * 2016-10-25 2017-03-29 中国计量大学 A kind of preparation method of high saturation and magnetic intensity manganese bismuth permanent magnets films
CN110172599A (en) * 2019-05-16 2019-08-27 中国计量大学 Heavy rare earth compound diffusion is for high saturation and magnetic intensity manganese bismuth melt spun alloy method

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106544630A (en) * 2016-10-25 2017-03-29 中国计量大学 A kind of preparation method of high saturation and magnetic intensity manganese bismuth permanent magnets films
CN110172599A (en) * 2019-05-16 2019-08-27 中国计量大学 Heavy rare earth compound diffusion is for high saturation and magnetic intensity manganese bismuth melt spun alloy method

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
ZHENG,XIAOMEI;ZHANG,PENGYUE;TAO,SHAN;ET AL.: "Fabrication and magnetic properties of novel rare-earth-free Fe-Mn-Bi-P thin films by one-step electrodeposition", 《THIN SOLID FILMS》 *

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Application publication date: 20190816