CN104907572A - Preparation method of NdFeB magnetic material - Google Patents
Preparation method of NdFeB magnetic material Download PDFInfo
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- CN104907572A CN104907572A CN201510420059.0A CN201510420059A CN104907572A CN 104907572 A CN104907572 A CN 104907572A CN 201510420059 A CN201510420059 A CN 201510420059A CN 104907572 A CN104907572 A CN 104907572A
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- earth metal
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- sintering
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- 229910001172 neodymium magnet Inorganic materials 0.000 title claims abstract description 47
- 239000000696 magnetic material Substances 0.000 title claims abstract description 13
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000005245 sintering Methods 0.000 claims abstract description 46
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 42
- 239000000956 alloy Substances 0.000 claims abstract description 42
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 36
- 150000002910 rare earth metals Chemical class 0.000 claims abstract description 33
- 239000000463 material Substances 0.000 claims abstract description 25
- 238000001704 evaporation Methods 0.000 claims abstract description 18
- 230000008020 evaporation Effects 0.000 claims abstract description 18
- 239000013078 crystal Substances 0.000 claims abstract description 15
- 239000002245 particle Substances 0.000 claims abstract description 15
- 229910052751 metal Inorganic materials 0.000 claims abstract description 12
- 239000002184 metal Substances 0.000 claims abstract description 12
- 239000007789 gas Substances 0.000 claims description 25
- 239000000843 powder Substances 0.000 claims description 25
- 239000000758 substrate Substances 0.000 claims description 24
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 23
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 claims description 23
- 238000000034 method Methods 0.000 claims description 22
- 229910052771 Terbium Inorganic materials 0.000 claims description 21
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 claims description 21
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 10
- 238000000227 grinding Methods 0.000 claims description 10
- 239000011261 inert gas Substances 0.000 claims description 10
- 229910001004 magnetic alloy Inorganic materials 0.000 claims description 10
- 238000002844 melting Methods 0.000 claims description 9
- 230000008018 melting Effects 0.000 claims description 9
- 239000003870 refractory metal Substances 0.000 claims description 8
- 230000015572 biosynthetic process Effects 0.000 claims description 7
- 229910052779 Neodymium Inorganic materials 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 239000011148 porous material Substances 0.000 claims description 6
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 238000000498 ball milling Methods 0.000 claims description 5
- 229910052796 boron Inorganic materials 0.000 claims description 5
- 230000000694 effects Effects 0.000 claims description 5
- 229910052742 iron Inorganic materials 0.000 claims description 5
- 230000002045 lasting effect Effects 0.000 claims description 5
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 claims description 5
- 238000003825 pressing Methods 0.000 claims description 5
- 238000012545 processing Methods 0.000 claims description 5
- BPJYAXCTOHRFDQ-UHFFFAOYSA-L tetracopper;2,4,6-trioxido-1,3,5,2,4,6-trioxatriarsinane;diacetate Chemical compound [Cu+2].[Cu+2].[Cu+2].[Cu+2].CC([O-])=O.CC([O-])=O.[O-][As]1O[As]([O-])O[As]([O-])O1.[O-][As]1O[As]([O-])O[As]([O-])O1 BPJYAXCTOHRFDQ-UHFFFAOYSA-L 0.000 claims description 5
- 238000007738 vacuum evaporation Methods 0.000 claims description 5
- 230000004927 fusion Effects 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 230000005389 magnetism Effects 0.000 abstract description 8
- 239000011162 core material Substances 0.000 abstract 1
- 230000009970 fire resistant effect Effects 0.000 abstract 1
- 238000003754 machining Methods 0.000 abstract 1
- 230000007547 defect Effects 0.000 description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 239000004411 aluminium Substances 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 229910052715 tantalum Inorganic materials 0.000 description 3
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 3
- 229910052721 tungsten Inorganic materials 0.000 description 3
- 239000010937 tungsten Substances 0.000 description 3
- 229910052720 vanadium Inorganic materials 0.000 description 3
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 2
- 229910000807 Ga alloy Inorganic materials 0.000 description 2
- 208000037656 Respiratory Sounds Diseases 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 150000004678 hydrides Chemical class 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000007596 consolidation process Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005496 eutectics Effects 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000007970 homogeneous dispersion Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
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- Hard Magnetic Materials (AREA)
- Powder Metallurgy (AREA)
- Manufacturing Cores, Coils, And Magnets (AREA)
Abstract
The invention provides a simple, convenient and cheap preparation method for a high-density NdFeB magnetic material which has enough residual magnetism and coercive force. For a sintered NdFeB magnetic material, the preparation method can be used to coat nanoscale rare earth metal or the alloy of the rare earth metal on micron-sized material particles through metallic vapor, by means of three stages of sintering treatment, air holes in a green body are eliminated, the density of the green body is improved, a crystal particle is prevented from excessive thickness to influence the coercive force, in the second stage of sintering, the mechanical strength of the magnetic material is improved obviously so that the magnetic material is more suitable for durable work in a high temperature environment, an evaporation plate used by an evaporation source solidifies the rare earth metal or the alloy of the rare earth metal on a plate-shaped or barrel-shaped grid-like core material made from fire-resistant metal, and the loss of the rare earth metal in the machining process is saved.
Description
Technical field
The present invention relates to the technical field forming permanent magnet, particularly relate to a kind of preparation method of Nd-Fe-B permanent magnet.
Background technology
The Nd-Fe-B permanent magnet of sintering has good magnetic, and Chang Zuowei permanent magnet is used in various power equipment.But due to the Nd in this material
2fe
14the existence of B, remanent magnetism and intrinsic coercivity along with variations in temperature very large, and in the power equipment in modern times, ubiquity the demand of the efforts environment of high temperature.Usually by before fusing or forming alloy in prior art, add cobalt (Co), dysprosium (Dy) or terbium (Tb) in hybrid metal.
But dysprosium (Dy), terbium (Tb) they are all very rare and expensive raw materials, the dysprosium (Dy) only containing about 5% in usual rare earth element, and and all comprise dysprosium (Dy) in the rare earth element of not all.In recent years due to the exhaustive exploitation of rare earth element, its reserves obviously decline, and the price of dysprosium (Dy), terbium (Tb) sharply rises.Simultaneously because these rare metals are difficult to purify, even and pure being also easy to is oxidized.Therefore industry also attempts employing its hydride or fluoride as additive.But the rapid diffusion of hydride makes and sinters relevant temperature and can not make original consolidation, and impact has carried out the service behaviour of material.Although and the interpolation of fluoride makes material obtain higher coercivity, its remanent magnetism then declines a lot.
Chinese patent CN104392818A discloses a kind of method improving sintered Nd-Fe-B permanent magnetic material magnetic property, passes through Dy
2the solution of O3 or Tb2O3 is coated in sintered Nd-Fe-B permanent magnetic material, then vat blue RS.But the method only to the dysprosium (Dy) on sintered Nd-Fe-B permanent magnetic material surface, the attachment of terbium (Tb), there is no improvement for material itself.
Chinese patent CN104575905A discloses a kind of method of adding nanometer aluminium powder and preparing sintered NdFeB, the aluminium powder of particle mean size 10nm-100nm is proportionally added in the micro mist of neodymium iron boron, although the method increase the coercivity of material, but owing to introducing aluminium powder in material, reduce further the Curie temperature of ndfeb magnet, and it has been generally acknowledged that the Curie temperature of Nd-Fe-B permanent magnet is lower, then reduction is very disadvantageous further.
Chinese patent CN104593660A discloses a kind of method of Nd-Fe-Bo permanent magnet material alloying Ga element, Ga element is added using Fe-Ga alloy as the form of raw material, the metal Ga avoiding liquid state during batching adds and holds volatile defect, but in this kind of method, Fe-Ga alloy form exists to have impact in material and have impact on Nd
2fe
14b crystal property.
Research is thought, improves sintering temperature and extends sintering time and can improve the density of sintered magnet, but owing to improving sintering temperature, extend sintering time and can cause growing up of crystal grain, and the coercivity of thick crystal grain is lower than thin crystal grain.Therefore the remanent magnetism of Nd-Fe-B permanent magnet wants the imaginary magnet significantly equaling magnet alloy real density lower than its sintered density at present.In addition, density is low also makes that magnet mechanical strength is low, surface gets rusty easily.To this defect, usual industry is thought to be needed to carry out sintering work under hyperbaric environment, make magnet material fine and close, but operations involving high pressure needs extremely expensive operation and maintenance cost, also has larger potential safety hazard simultaneously.
For the foregoing reasons, the research preparing remanent magnetism and the enough coercitive high density Nd-Fe-B permanent magnet with expectation is needed further deeply.
Summary of the invention
The object of the present invention is to provide a kind of simple, convenient, cheap preparation method with enough remanent magnetism and coercitive high density Nd-Fe-B permanent magnet.
For the Nd-Fe-B permanent magnet of sintering, desirable microstructure is Nd
2fe
14b crystal grain, one aspect of the present invention provides a kind of method preparing Nd-Fe-B permanent magnet, it is characterized in that:
There is provided a kind of Nd-Fe-B permanent magnet, the proportioning of Nd-Fe-B permanent magnet is: the neodymium of 10-15wt%, the boron of 6-8wt%, and all the other are iron, and melting under ar gas environment, makes alloy pig, then under ar gas environment, pass through ball mill grinding; The preferred diameter being used as the ball milling of abrasive media is 3-5 millimeter; Then the powder of ball mill grinding is ground into the powder of particle mean size 3 μm by airslide disintegrating mill;
Be filled with argon gas in vacuum evaporation room, by the heat effect of evaporation source, dysprosium (Dy), terbium (Tb) formed metallic vapour; Preferred partial pressure of ar gas is not less than 3 × 10
-1pa;
Above-mentioned metallic vapour output gas flow is adhered to the Nd-Fe-B permanent magnet alloy powder that airslide disintegrating mill grinds out; Preferably metallic vapour input is placed with in the rotary hydrogen broken furnace of Nd-Fe-B permanent magnet alloy powder, limit heating mutarotation turns, and during heating, body of heater rotates with the rotary speed of 5rpm, then body of heater rotating shaft one end input metallic vapour, the other end suitably applies negative pressure, duration 0.1-1 hour.
Wherein, the evaporation sheet material formation process that evaporation source uses is:
Solidifying body formation process: after the alloy melting of rare earth metal or rare earth metal, under remaining on the state lower than aforementioned fusion temperature, on the tabular made at refractory metal by the alloy graining of rare earth metal or rare earth metal or the latticed core of tubular;
The silk that core uses the refractory metals such as tungsten, vanadium, titanium, tantalum or its oxide to make is woven into latticed, and the mesh of grid, at 50-100 order, uses at least 3 layers of mesh overlay to make the grid core of tabular or tubular;
The metal of terres rares uses dysprosium (Dy), terbium (Tb); The alloy of rare earth metal uses in dysprosium (Dy), terbium (Tb) with the addition of and improves coercitive metal.
Like this as evaporation source use evaporation sheet material without the need to independent casting, after the rare earth metal that core adheres to or the alloy of rare earth metal run out of, only need core again to immerse the alloy of rare earth metal under molten state or rare earth metal, the alloy of rare earth metal or rare earth metal is solidified again.
By under the magnetic field of Nd-Fe-B permanent magnet alloy powder under the pressure of 3-5 ton/square centimeter and at least 2.5T, be molded into base substrate, wherein magnetic alloy particle be oriented to easy magnetizing axis along the magnetic direction applied during mold pressing;
Magnetic material alloys powder green bodies sinters, and sintering was divided into for three stages carried out, not life period interval and cooling processing between three stages;
First stage sinters: carry out in vacuum environment, eliminate the pore in base substrate, sintering temperature is 1200-1300 DEG C, sintering time continues 2-3 hour, the density obtaining base substrate reaches the 95-98.5% of magnetic alloy density, extend sintering time although lasting and improve the density in addition further leeway of improving of sintering temperature for base substrate, likely cause the less desirable thick of crystal grain;
Second stage sinters: in inert gas environment, controls under 30-50 atmospheric environment, with 1000-1100 DEG C, and sintering 1-2 hour;
Phase III sinters: in inert gas environment, under normal pressure, under the environment of 800 DEG C, cool gradually with the speed of 200 DEG C/h;
By triphasic sintering processes, in first stage sintering, eliminate the pore in base substrate, improve the density of base substrate, turn avoid that crystal grain is too thick affects coercivity; And in second stage sintering, sintering temperature and duration all lower than the first sintering stage, and have suitable pressure sintering, avoid the defect that undesirable crystal grain is thick, improve again the density of base substrate simultaneously further; In phase III sintering, the speed that control temperature declines, the defects such as the crackle avoiding magnet material to cause because temperature reduces suddenly and chipping, significantly improve the mechanical strength of magnet material, work durable under being more suitable for hot environment.
By method of the present invention, make on the one hand Nd-Fe-B permanent magnet have at least one in the dysprosium (Dy) of non-equilibrium diffusion or terbium (Tb), the prompting of non-homogeneous dispersion makes Nd in material
2fe
14b crystal grain borders goes out preferential build, more easily forms eutectic phase, makes material have good coercivity and remanent magnetism.
By method of the present invention, on the other hand, dysprosium (Dy) or the terbium (Tb) of Nano grade are coated on the material granule of micron level, meticulous in particle size, make particle more responsive for the impact of magnetic, the magnetic energy impact applied extraly in mold process, thus the enough remanent magnetism of expectation can be obtained.
By method of the present invention, dysprosium (Dy) or terbium (Tb) in the material formed after sintering is made to be dispersed in the inside of material on the other hand, but the dysprosium (Dy) consumed or terbium (Tb) content significantly reduce 50% or more, be applicable in the Nd-Fe-B permanent magnet form of motor a kind of, overall dysprosium (Dy) or terbium (Tb) only account for the scope of about 0.3-5wt%, but make magnetic property similar to the process magnet with much bigger whole content.
By method of the present invention, on the other hand, multistage sintering method improves the density of base substrate, turn avoid that crystal grain is too thick affects coercivity, the speed that control temperature declines, the defects such as the crackle avoiding magnet material to cause because temperature reduces suddenly and chipping, significantly improve the mechanical strength of magnet material, work durable under being more suitable for hot environment.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is further described, but does not limit the invention to these detailed description of the invention.One skilled in the art would recognize that all alternatives, improvement project and the equivalents that present invention encompasses and may comprise in Claims scope.
Embodiment 1
There is provided a kind of Nd-Fe-B permanent magnet, the proportioning of Nd-Fe-B permanent magnet is: the neodymium of 10wt%, the boron of 8wt%, and all the other are iron, and melting under ar gas environment, makes alloy pig, then under ar gas environment, pass through ball mill grinding; The preferred diameter being used as the ball milling of abrasive media is 3 millimeters; Then the powder of ball mill grinding is ground into the powder of particle mean size 3 μm by airslide disintegrating mill;
Be filled with argon gas in vacuum evaporation room, by the heat effect of evaporation source, dysprosium (Dy), terbium (Tb) formed metallic vapour; Partial pressure of ar gas is 3 × 10
-1pa;
Above-mentioned metallic vapour output gas flow is adhered to the Nd-Fe-B permanent magnet alloy powder that airslide disintegrating mill grinds out, duration 0.1-1 hour;
By Nd-Fe-B permanent magnet alloy powder under the pressure of 3 tons/square centimeter and 2.5T magnetic field under, be molded into base substrate, wherein magnetic alloy particle be oriented to easy magnetizing axis along the magnetic direction applied during mold pressing;
Magnetic material alloys powder green bodies sinters, and sintering was divided into for three stages carried out, not life period interval and cooling processing between three stages;
First stage sinters: carry out in vacuum environment, eliminate the pore in base substrate, sintering temperature is 1200-1300 DEG C, sintering time continues 2 hours, the density obtaining base substrate reaches 95% of magnetic alloy density, extend sintering time although lasting and improve the density in addition further leeway of improving of sintering temperature for base substrate, likely cause the less desirable thick of crystal grain;
Second stage sinters: in inert gas environment, controls, under 30-50 atmospheric environment, with 1000-1100 DEG C, to sinter 1 hour;
Phase III sinters: in inert gas environment, under normal pressure, under the environment of 800 DEG C, cool gradually with the speed of 200 DEG C/h;
Wherein, the evaporation sheet material formation process that evaporation source uses is:
Solidifying body formation process: after the alloy melting of rare earth metal or rare earth metal, under remaining on the state lower than aforementioned fusion temperature, on the latticed core of the tabular made at refractory metal by the alloy graining of rare earth metal or rare earth metal;
The silk that core uses the refractory metals such as tungsten, vanadium, titanium, tantalum or its oxide to make is woven into latticed, and the mesh of grid, at 50 orders, uses at least 3 layers of mesh overlay to make the grid core of tabular;
The metal of terres rares uses dysprosium (Dy), terbium (Tb); The alloy of rare earth metal uses in dysprosium (Dy), terbium (Tb) with the addition of and improves coercitive metal, as Nd, Pr, Al, Cu, Ga.
Embodiment 2
There is provided a kind of Nd-Fe-B permanent magnet, the proportioning of Nd-Fe-B permanent magnet is: the neodymium of 15wt%, the boron of 6wt%, and all the other are iron, and melting under ar gas environment, makes alloy pig, then under ar gas environment, pass through ball mill grinding; The preferred diameter being used as the ball milling of abrasive media is 5 millimeters; Then the powder of ball mill grinding is ground into the powder of particle mean size 3 μm by airslide disintegrating mill;
Be filled with argon gas in vacuum evaporation room, by the heat effect of evaporation source, dysprosium (Dy), terbium (Tb) formed metallic vapour; Preferred partial pressure of ar gas 5 × 10
-1pa;
Above-mentioned metallic vapour output gas flow is adhered to the Nd-Fe-B permanent magnet alloy powder that airslide disintegrating mill grinds out, 1 hour duration;
By Nd-Fe-B permanent magnet alloy powder under the pressure of 5 tons/square centimeter and 3T magnetic field under, be molded into base substrate, wherein magnetic alloy particle be oriented to easy magnetizing axis along the magnetic direction applied during mold pressing;
Magnetic material alloys powder green bodies sinters, and sintering was divided into for three stages carried out, not life period interval and cooling processing between three stages;
First stage sinters: carry out in vacuum environment, eliminate the pore in base substrate, sintering temperature is 1200-1300 DEG C, sintering time continues 3 hours, the density obtaining base substrate reaches 98.5% of magnetic alloy density, extend sintering time although lasting and improve the density in addition further leeway of improving of sintering temperature for base substrate, likely cause the less desirable thick of crystal grain;
Second stage sinters: in inert gas environment, control under 50 atmospheric environment, with 1000-1100 DEG C, sinter 2 hours;
Phase III sinters: in inert gas environment, under normal pressure, under the environment of 800 DEG C, cool gradually with the speed of 200 DEG C/h
Wherein, the evaporation sheet material formation process that evaporation source uses is:
Solidifying body formation process: after the alloy melting of rare earth metal or rare earth metal, under remaining on the state lower than aforementioned fusion temperature, on the latticed core of the tubular made at refractory metal by the alloy graining of rare earth metal or rare earth metal;
The silk that core uses the refractory metals such as tungsten, vanadium, titanium, tantalum or its oxide to make is woven into latticed, and the mesh of grid, at 50-100 order, uses 4 layers of mesh overlay to make the grid core of tubular;
The metal of terres rares uses dysprosium (Dy), terbium (Tb); The alloy of rare earth metal uses in dysprosium (Dy), terbium (Tb) with the addition of and improves coercitive metal.
Embodiment 3
There is provided a kind of Nd-Fe-B permanent magnet, the proportioning of Nd-Fe-B permanent magnet is: the neodymium of 13wt%, the boron of 7wt%, and all the other are iron, and melting under ar gas environment, makes alloy pig, then under ar gas environment, pass through ball mill grinding; The preferred diameter being used as the ball milling of abrasive media is 4 millimeters; Then the powder of ball mill grinding is ground into the powder of particle mean size 3 μm by airslide disintegrating mill;
Be filled with argon gas in vacuum evaporation room, by the heat effect of evaporation source, dysprosium (Dy), terbium (Tb) formed metallic vapour; Partial pressure of ar gas is 3.5 × 10
-1pa;
Above-mentioned metallic vapour output gas flow is adhered to the Nd-Fe-B permanent magnet alloy powder that airslide disintegrating mill grinds out, 0.5 hour duration;
By Nd-Fe-B permanent magnet alloy powder under the pressure of 4 tons/square centimeter and 2.5T magnetic field under, be molded into base substrate, wherein magnetic alloy particle be oriented to easy magnetizing axis along the magnetic direction applied during mold pressing;
Magnetic material alloys powder green bodies sinters, and sintering was divided into for three stages carried out, not life period interval and cooling processing between three stages;
First stage sinters: carry out in vacuum environment, eliminate the pore in base substrate, sintering temperature is 1200-1300 DEG C, sintering time continues 2 hours, the density obtaining base substrate reaches 98% of magnetic alloy density, extend sintering time although lasting and improve the density in addition further leeway of improving of sintering temperature for base substrate, likely cause the less desirable thick of crystal grain;
Second stage sinters: in inert gas environment, controls, under 30-50 atmospheric environment, with 1000-1100 DEG C, to sinter 1.5 hours;
Phase III sinters: in inert gas environment, under normal pressure, under the environment of 800 DEG C, cool gradually with the speed of 200 DEG C/h.
It is as follows that the Nd-Fe-B permanent magnet adopting the present invention to prepare records parameter:
Claims (5)
1. a preparation method for Nd-Fe-B permanent magnet, is characterized in that:
(1) provide a kind of Nd-Fe-B permanent magnet, the proportioning of Nd-Fe-B permanent magnet is: the neodymium of 10-15wt%, the boron of 6-8wt%, and all the other are iron, and melting under ar gas environment, makes alloy pig, then under ar gas environment, pass through ball mill grinding; Then the powder of ball mill grinding is ground into the powder of particle mean size 3 μm by airslide disintegrating mill;
(2) be filled with argon gas in vacuum evaporation room, by the heat effect of evaporation source, the alloy of rare earth metal or rare earth metal is formed metallic vapour, and wherein partial pressure of ar gas is not less than 3 × 10
-1pa, adheres to above-mentioned metallic vapour output gas flow the Nd-Fe-B permanent magnet alloy powder that airslide disintegrating mill grinds out;
The evaporation sheet material formation process that above-mentioned evaporation source uses is:
After the alloy melting of rare earth metal or rare earth metal, under remaining on the state lower than aforementioned fusion temperature, on the tabular that the alloy graining of rare earth metal or rare earth metal is made at refractory metal or the latticed core of tubular;
By under the magnetic field of Nd-Fe-B permanent magnet alloy powder under the pressure of 3-5 ton/square centimeter and at least 2.5T, be molded into base substrate, wherein magnetic alloy particle be oriented to easy magnetizing axis along the magnetic direction applied during mold pressing;
(3) magnetic material alloys powder green bodies sintering, sintering was divided into for three stages carried out, not life period interval and cooling processing between three stages;
First stage sinters: carry out in vacuum environment, eliminate the pore in base substrate, sintering temperature is 1200-1300 DEG C, sintering time continues 2-3 hour, the density obtaining base substrate reaches the 95-98.5% of magnetic alloy density, extend sintering time although lasting and improve the density in addition further leeway of improving of sintering temperature for base substrate, likely cause the less desirable thick of crystal grain;
Second stage sinters: in inert gas environment, controls under 30-50 atmospheric environment, with 1000-1100 DEG C, and sintering 1-2 hour;
Phase III sinters: in inert gas environment, under normal pressure, under the environment of 800 DEG C, with the speed of 200 DEG C/h cooling forming gradually.
2. the preparation method of a kind of Nd-Fe-B permanent magnet as claimed in claim 1, it is characterized in that: metallic vapour attachment is by being placed with in the rotary hydrogen broken furnace of Nd-Fe-B permanent magnet alloy powder by metallic vapour input, limit heating mutarotation turns, during heating, body of heater rotates with the rotary speed of 5rpm, body of heater rotating shaft one end input metallic vapour again, the other end suitably applies negative pressure, duration 0.1-1 hour.
3. the preparation method of a kind of Nd-Fe-B permanent magnet as claimed in claim 1, it is characterized in that: the silk that the described latticed core making evaporation sheet material uses refractory metal or its oxide to make is woven into latticed, the mesh of grid, at 50-100 order, uses at least 3 layers of mesh overlay to make the grid core of tabular or tubular.
4. the preparation method of a kind of Nd-Fe-B permanent magnet as claimed in claim 1, is characterized in that: the metal of terres rares uses dysprosium (Dy), terbium (Tb); The alloy of rare earth metal uses in dysprosium (Dy), terbium (Tb) with the addition of and improves coercitive metal.
5. the preparation method of a kind of Nd-Fe-B permanent magnet as claimed in claim 1, is characterized in that: the diameter as the ball milling of abrasive media is 3-5 millimeter.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510420059.0A CN104907572B (en) | 2015-07-16 | 2015-07-16 | A kind of preparation method of Nd-Fe-B permanent magnet |
Applications Claiming Priority (1)
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| CN107564648A (en) * | 2017-09-19 | 2018-01-09 | 安徽大地熊新材料股份有限公司 | A kind of deposition process for preparing high-performance Ne-Fe-B magnetic |
| CN107564649A (en) * | 2017-09-19 | 2018-01-09 | 安徽大地熊新材料股份有限公司 | A kind of method of diffusion for preparing high-performance Ne-Fe-B magnetic |
| CN110129739A (en) * | 2019-06-19 | 2019-08-16 | 广东腾胜科技创新有限公司 | Equipment for evaporating terbium or dysprosium on the surface of magnetic materials |
| CN110808158A (en) * | 2019-09-12 | 2020-02-18 | 浙江东阳东磁稀土有限公司 | Method for improving coercive force of sintered neodymium-iron-boron magnet and sintered neodymium-iron-boron magnet |
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| CN110808158A (en) * | 2019-09-12 | 2020-02-18 | 浙江东阳东磁稀土有限公司 | Method for improving coercive force of sintered neodymium-iron-boron magnet and sintered neodymium-iron-boron magnet |
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