CN110211792A - A kind of rare earth permanent-magnetic material preparation method - Google Patents

A kind of rare earth permanent-magnetic material preparation method Download PDF

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Publication number
CN110211792A
CN110211792A CN201910350873.8A CN201910350873A CN110211792A CN 110211792 A CN110211792 A CN 110211792A CN 201910350873 A CN201910350873 A CN 201910350873A CN 110211792 A CN110211792 A CN 110211792A
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China
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rare earth
heat treatment
magnetic material
master alloy
earth permanent
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CN201910350873.8A
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刘廷坤
江平
宋渤海
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Shenzhen Jisheng Huali Technology Co Ltd
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Shenzhen Jisheng Huali Technology Co Ltd
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Priority to CN201910350873.8A priority Critical patent/CN110211792A/en
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0253Apparatus 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
    • H01F41/0293Apparatus 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)
  • Power Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Manufacturing Cores, Coils, And Magnets (AREA)
  • Hard Magnetic Materials (AREA)

Abstract

The present invention provides a kind of rare earth permanent-magnetic material preparation method, and the content of rare earth of NdFeB magnet is mainly reduced by crystal ingedient and structure regulating and improves coercivity, can effectively smooth and cleaning crystal boundary with heat treatment process by adjusting being sintered with optimization;Grain boundary structure can also be regulated and controled by adding microelement, these techniques can effectively improve material coercivity and comprehensive hard magnetic property while reducing NdFeB permanent magnetism content of rare earth.

Description

A kind of rare earth permanent-magnetic material preparation method
Technical field
The invention belongs to rare-earth permanent-magnet material technical fields, and in particular to a kind of rare earth permanent-magnetic material preparation method.
Background technique
The rare earth permanent-magnetic material that rare earth permanent-magnetic generator uses mainly includes neodymium iron boron, neodium magnet (Neodymium Magnet it) is also referred to as ndfeb magnet (NdFeB magnet), is the tetragonal crystal system crystalline substance formed by neodymium, iron, boron (Nd2Fe14B) Body.Neodymium iron boron is divided into sintered NdFeB and two kinds of Agglutinate neodymium-iron-boron, and Agglutinate neodymium-iron-boron all directions are all magnetic, corrosion-resistant;It burns Neodymium iron boron is tied because perishable, surface needs coating, generally there is zinc-plated, nickel, zinc electroplating bath, environmentally friendly nickel, ambrose alloy nickel, environmentally friendly ambrose alloy nickel etc.. Sintered NdFeB generally divides axial charging and radial magnetizing, is determined according to required working face.SinteringNd-Fe-B permanent magneticMaterial It is divided into low-coercivity (without letter) by magnetic polarization intensity coercivity size, medium coercivity M, high-coercive force H, extra-high coercive Power SH, ultra-high coercive force UH, high six class product of coercivity EH.Sintered Nd-Fe-B permanent magnetic material has excellent magnetic property, extensively General to be applied to the fields such as electronics, electric machinery, medical instrument, toy, packaging, hardware machinery, space flight and aviation, more typical has forever Magneto, loudspeaker, magnetic separator, computer disc driver, MR imaging apparatus instrument etc..It is prepared by NdFeB material Friendly particulate metal successful development powder metallurgic method (powder metallurgy process), General Motors Corporation's successful development Whirl spraying smelting process (melt-spinning process), can prepare ndfeb magnet.This magnet is that magnetism is only second to now The permanent magnet and most-often used rare-earth magnet of absolute zero holmium magnet.Ndfeb magnet is widely used in electronics Product, such as hard disk, mobile phone, earphone and battery-powered tool etc..But that there are coercivitys is bad for permanent-magnet material now, The method for solving the problems, such as this now is addition Dy, Tb heavy rare earth element, to directly effectively promote the coercivity and temperature of magnet Stability is spent, but since Dy, Tb atom are coupled with Fe atom anti-ferromagnetism, will cause the fast prompt drop of magnet remanence and magnetic energy product Low, furthermore Dy, Tb element abundance in rare earth resources are low and expensive, and DIRECT ALLOYING will lead to neodymium iron boron magnetic body cost It is significantly increased.
Application requirement magnet of the NdFeB permanent magnetism in fields such as motors not only has sufficiently high coercivity and magnetic energy product, also Demanding thermal stability.It is also very real that material cost is reduced while improving the comprehensive magnetic energy of NdFeB magnet Problem.Therefore, improving material cost performance by optimizing components, microstructure regulation and new process development is NdFeB permanent magnetism Main direction of studying.
The present invention is mainly reduced the content of rare earth of NdFeB magnet by crystal ingedient and structure regulating and improves coercive Power, can effectively smooth and cleaning crystal boundary with heat treatment process by adjusting being sintered with optimization;By adding microelement It is enough that Grain-boundary Junctions can be regulated and controled, these techniques can effectively improve material coercive while reducing NdFeB permanent magnetism content of rare earth Power and comprehensive hard magnetic property.
Summary of the invention
The main object of the present invention is to form the rare earth permanent magnet material that even compact, thickness are adjustable, at low cost, coercivity is high Material.
In order to solve the above problem, a kind of preparation method of rare earth permanent-magnetic material is provided:
Step 1: to prepare rare earth permanent-magnetic material by grain boundary decision technology, grain boundary decision technology is coating, vacuum steaming Plating, hot spray process.
Step 2: taking rare earths material Nd, Zr, Ta, Al, Zn, Sn, Ce, Fe, B, Nd, Pr, Ho, Dy, Tb and Hf, M1xM2y, In one kind or two or more combination, one kind or two or more combination in M Al, Zn, Sn, Mg, M2 is at least one in V, Si, Mn Kind element, wherein 60≤x≤80,30≤y≤40.
Step 3: M1 will be removedxM2yExcept raw material be put into electric arc furnaces and carry out 7-8 melting, obtain into split-phase after cooling To uniform master alloy slab, it is heat-treated for the first time;
Step 4: by M1xM2yPowder mixes with volatile organic solvent and is sprayed on the institute after being heat-treated for the first time State the surface of slab, dry and successively second heat treatment, hydrogenation treatment, Dehydroepiandrosterone derivative, powder processed and nitridation of progress.
Step 5: by the thickness control of the above alloy casting piece at 200 μm -800 μm, preferably 2000 μm, 250 μm;
Step 6: the grain diameter of the M1xM2y powder as diffusion source is less than 5 μ in second of heat treatment process m.Second of heat treatment is in 750-1000 DEG C and the lower progress 1-10h of argon gas protection;Preferably, the temperature of second of heat treatment It is 800-950 DEG C.
Step 7: master alloy slab obtained in step 3 is broken into the fritter of 8~9g, broken master alloy is small It is packaged enter mould tube in, mold lower ending opening, cut hole diameter is
0.7~1.0mm, nozzle are 2~4mm at a distance from roll surface;In vacuum quick quenching equipment, under an argon atmosphere, adopt It is heated with radio-frequency induction coil, after alloy melts completely, under argon pressure effect, master alloy is sprayed through the nozzle of mold bottom Out, being ejected into revolving speed is 20-
In the metallic roll of 30m/s, permanent-magnet alloy can be obtained.
Step 8: electric arc furnaces is the electric arc furnaces of argon gas protection.
Specific embodiment
Step 1: to prepare rare earth permanent-magnetic material by grain boundary decision technology, grain boundary decision technology is coating, vacuum steaming Plating, hot spray process.
Step 2: taking rare earths material Nd, Zr, Ta, Al, Zn, Sn, Ce, Fe, B, Nd, Pr, Ho, Dy, Tb and Hf, M1xM2y, In one kind or two or more combination, one kind or two or more combination in M Al, Zn, Sn, Mg, M2 is at least one in V, Si, Mn Kind element, wherein 60≤x≤80,30≤y≤40.
Step 3: M1 will be removedxM2yExcept raw material be put into electric arc furnaces and carry out 7-8 melting, obtain into split-phase after cooling To uniform master alloy slab, it is heat-treated for the first time;
Step 4: by M1xM2yPowder mixes with volatile organic solvent and is sprayed on the institute after being heat-treated for the first time State the surface of slab, dry and successively second heat treatment, hydrogenation treatment, Dehydroepiandrosterone derivative, powder processed and nitridation of progress.
Step 5: by the thickness control of the above alloy casting piece at 200 μm -800 μm, preferably 2000 μm, 250 μm;
Step 6: the grain diameter of the M1xM2y powder as diffusion source is less than 5 μ in second of heat treatment process m.Second of heat treatment is in 750-1000 DEG C and the lower progress 1-10h of argon gas protection;Preferably, the temperature of second of heat treatment It is 800-950 DEG C.
Step 7: master alloy slab obtained in step 3 is broken into the fritter of 8~9g, broken master alloy is small It is packaged enter mould tube in, mold lower ending opening, cut hole diameter is
0.7~1.0mm, nozzle are 2~4mm at a distance from roll surface;In vacuum quick quenching equipment, under an argon atmosphere, adopt It is heated with radio-frequency induction coil, after alloy melts completely, under argon pressure effect, master alloy is sprayed through the nozzle of mold bottom Out, it is ejected into the metallic roll that revolving speed is 20- 30m/s, permanent-magnet alloy can be obtained.
Step 8: electric arc furnaces is the electric arc furnaces of argon gas protection.

Claims (2)

1. a kind of rare earth permanent-magnetic material preparation method, it is characterised in that preparation step is as follows:
Step 1: to prepare rare earth permanent-magnetic material by grain boundary decision technology, grain boundary decision technology is coating, vacuum evaporation, heat Spray coating method.
Step 2: taking rare earths material Nd, Zr, Ta, Al, Zn, Sn, Ce, Fe, B, Nd, Pr, Ho, Dy, Tb and Hf, M1xM2y, in a kind Or combination of more than two kinds, one kind or two or more combination in M Al, Zn, Sn, Mg, M2 is at least one of V, Si, Mn element, Wherein 60≤x≤80,30≤y≤40.
Step 3: M1 will be removedxM2yExcept raw material be put into electric arc furnaces and carry out 7-8 melting, it is relatively equal to obtain ingredient after cooling Even master alloy slab is heat-treated for the first time;
Step 4: by M1xM2yPowder mixes with volatile organic solvent and is sprayed on the casting after being heat-treated for the first time The surface of piece, dry and successively second heat treatment, hydrogenation treatment, Dehydroepiandrosterone derivative, powder processed and nitridation of progress.
Step 5: by the thickness control of the above alloy casting piece at 200 μm -800 μm, preferably 2000 μm, 250 μm;
Step 6: the grain diameter of the M1xM2y powder as diffusion source is less than 5 μm in second of heat treatment process.The Secondary heat treatment is in 750-1000 DEG C and the lower progress 1-10h of argon gas protection;Preferably, the temperature of second of heat treatment is 800-950℃。
Step 7: master alloy slab obtained in step 3 is broken into the fritter of 8~9g, broken master alloy is small packaged Enter in mould tube, mold lower ending opening, cut hole diameter is 0.7~1.0mm, and nozzle is 2~4mm at a distance from roll surface;In vacuum It in fast quenching equipment, under an argon atmosphere, is heated using radio-frequency induction coil, after alloy melts completely, is acted in argon pressure Under, master alloy is sprayed through the nozzle of mold bottom, is ejected into the metallic roll that revolving speed is 20-30m/s, and permanent magnetism conjunction can be obtained Gold.
2. preparation method as claimed in claim, it is characterised in that: electric arc furnaces is the electric arc furnaces of argon gas protection.
CN201910350873.8A 2019-04-28 2019-04-28 A kind of rare earth permanent-magnetic material preparation method Pending CN110211792A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105957673A (en) * 2016-03-14 2016-09-21 北京科技大学 Isotropic rare earth permanent magnetic powder and preparation method thereof
CN109065311A (en) * 2018-06-25 2018-12-21 江西理工大学 A kind of high-coercive force neodymium ferrocerium boron permanent-magnet alloy and preparation method
CN109473247A (en) * 2018-11-16 2019-03-15 宁波尼兰德磁业股份有限公司 A kind of preparation method of neodymium iron boron crystal boundary infiltration alloy casting piece
CN109585113A (en) * 2018-11-30 2019-04-05 宁波韵升股份有限公司 A kind of preparation method of Sintered NdFeB magnet

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105957673A (en) * 2016-03-14 2016-09-21 北京科技大学 Isotropic rare earth permanent magnetic powder and preparation method thereof
CN109065311A (en) * 2018-06-25 2018-12-21 江西理工大学 A kind of high-coercive force neodymium ferrocerium boron permanent-magnet alloy and preparation method
CN109473247A (en) * 2018-11-16 2019-03-15 宁波尼兰德磁业股份有限公司 A kind of preparation method of neodymium iron boron crystal boundary infiltration alloy casting piece
CN109585113A (en) * 2018-11-30 2019-04-05 宁波韵升股份有限公司 A kind of preparation method of Sintered NdFeB magnet

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Application publication date: 20190906