CN103985534B - R-T-B series magnet is carried out the method for Dy diffusion, magnet and diffusion source - Google Patents
R-T-B series magnet is carried out the method for Dy diffusion, magnet and diffusion source Download PDFInfo
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- CN103985534B CN103985534B CN201410238574.2A CN201410238574A CN103985534B CN 103985534 B CN103985534 B CN 103985534B CN 201410238574 A CN201410238574 A CN 201410238574A CN 103985534 B CN103985534 B CN 103985534B
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- 238000009792 diffusion process Methods 0.000 title claims abstract description 93
- 238000000034 method Methods 0.000 title claims abstract description 48
- 239000002245 particle Substances 0.000 claims abstract description 88
- 238000005275 alloying Methods 0.000 claims abstract description 40
- 239000008188 pellet Substances 0.000 claims abstract description 40
- 239000003870 refractory metal Substances 0.000 claims abstract description 23
- 230000008569 process Effects 0.000 claims abstract description 22
- 229910001279 Dy alloy Inorganic materials 0.000 claims abstract description 8
- 238000010276 construction Methods 0.000 claims abstract description 4
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 15
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 12
- 239000000758 substrate Substances 0.000 claims description 11
- 239000000843 powder Substances 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 239000012798 spherical particle Substances 0.000 claims description 5
- 239000008187 granular material Substances 0.000 claims description 3
- 150000003624 transition metals Chemical class 0.000 claims description 2
- 229910052727 yttrium Inorganic materials 0.000 claims description 2
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical group [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims 1
- 229910052796 boron Inorganic materials 0.000 claims 1
- 239000000155 melt Substances 0.000 claims 1
- 229910052723 transition metal Inorganic materials 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 24
- 238000012360 testing method Methods 0.000 description 29
- 230000000052 comparative effect Effects 0.000 description 23
- 238000011156 evaluation Methods 0.000 description 15
- 238000010438 heat treatment Methods 0.000 description 13
- 238000001704 evaporation Methods 0.000 description 11
- 230000008020 evaporation Effects 0.000 description 11
- 230000032683 aging Effects 0.000 description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 9
- 229910052771 Terbium Inorganic materials 0.000 description 9
- 239000013078 crystal Substances 0.000 description 9
- 238000001514 detection method Methods 0.000 description 9
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 6
- 239000010931 gold Substances 0.000 description 6
- 229910052737 gold Inorganic materials 0.000 description 6
- 230000005389 magnetism Effects 0.000 description 6
- 238000012545 processing Methods 0.000 description 6
- 150000002910 rare earth metals Chemical class 0.000 description 6
- 239000002699 waste material Substances 0.000 description 6
- 238000010586 diagram Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- 238000013021 overheating Methods 0.000 description 5
- 229910045601 alloy Inorganic materials 0.000 description 4
- 239000000956 alloy Substances 0.000 description 4
- 238000005520 cutting process Methods 0.000 description 4
- 229910052689 Holmium Inorganic materials 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000007711 solidification Methods 0.000 description 3
- 229910000807 Ga alloy Inorganic materials 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000011258 core-shell material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 238000010025 steaming Methods 0.000 description 2
- 229910000806 Latten Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
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- Powder Metallurgy (AREA)
- Hard Magnetic Materials (AREA)
Abstract
The invention discloses and R T B series magnet is carried out the method for Dy diffusion, magnet and diffusion source; for configuring the preparatory construction of R T B based sintered magnet, the preparatory construction in the Dy diffusion source in same process chamber in being included in process chamber and making Dy diffusion source be evaporated to the method that the Dy of sintered magnet spreads engineering; it is characterized in that: described Dy diffusion source is the Dy particle or Dy alloying pellet being arranged in refractory metal net, and the particle diameter of described Dy particle or Dy alloying pellet is 0.5～2mm.The present invention by will the particle diameter that be filled in refractory metal net 0.5～2mm Dy particle or Dy alloying pellet substitutes Dy plate or Dy alloy sheets uses, to save the usage amount of Dy material.
Description
Technical field
The present invention relates to a kind of method of Dy diffusion, magnet and Dy of carrying out magnet and spread source, it is a kind of right to be specifically related to
R-T-B series magnet carries out the method for Dy diffusion, magnet and Dy and spreads source.
Background technology
Grain boundary decision processes and is typically after manufacturing procedure (that is cutting action), carries out before surface treatment procedure.
So-called grain boundary decision method, it is simply that on the surface of R-T-B sintered magnet with heavy rare earth element (RH) blocks such as Dy, Tb or
Its alloy block or placing the heavy rare earth element such as sintered magnet and Dy, Tb in same process chamber in the way of being not directly contacted with
Block or its alloy block, and after suitable heat treatment, Dy, Tb of magnet surface can enter through the crystal boundary of sintered body magnet
Inside sintered body, make the heavy rare earth such as Dy, Tb from crystal boundary to principal phase R2T14The method being diffused inside B, it is on the one hand
So that the heavy rare earth element such as Dy, Tb in entrance crystal boundary quickly enters inside sintered body, from crystal boundary to principal phase R2T14B
Diffusion inside, is on the other hand to enter principal phase R2T14Dy within B instead of principal phase R2T14The R of B housing department, but
Not replacing the R of central part, thus form core shell structure, the composition difference of principal phase core shell structure both ensure that heavy rare earth element took
For the anisotropic raising of rear magnet, thus improve coercivity, also because this replacement is only a minimum part for principal phase, magnetic
The remanent magnetism of body is substantially constant or reduces the least.
Place in the way of being not directly contacted with in same process chamber the heavy rare earth element block such as sintered magnet and Dy, Tb or its close
Gold bullion, carry out RH (mainly including Dy, Tb or Ho) or its compound diffusion existing report in, as CN101506919A,
CN100470687C, CN102667978A etc., be to use dysprosium or the block of its compound or plate body heating evaporation
To magnet surface, then the technique toward magnet diffusion inside.But, when Dy spreads, it is impossible to directly use direct from market
The Dy material buied, this is because, the Dy material surface as diffusion source needs with the magnet surface as diffusion acceptor
Keep close contact, therefore, for improve heat-treatment furnace charging ratio, raising can industrialness, need obtain Dy thin plate or
Dy latten, and the large volume raw material that the Dy block bought on market can be used for cutting are few, and due to Dy material (gold
Belong to Dy or alloy Dy) it is difficult-to-machine material, poor ductility, it is particularly easy to crack, makes the conjunction of board-like material
Lattice rate is low, as easy as rolling off a log ruptures when processing, damages, causes cannot be used for volume production, thus, cause the work of grain boundary decision
Industryization is universal to be difficult to.
And, Dy plate need to be consistent with the shape of magnet, and therefore, the Dy material usage used during Dy diffusion is considerably beyond expansion
Dissipating required consumption, the produced waste material of Dy material cutting is too many in addition, there is the problem that utilization rate is too low.
Furthermore, the Dy material board-like material that obtained of cutting is also difficult to follow magnet shape and makes corresponding alteration of form, because of
This, the on-plane surface magnet such as arcuate magnet or annular magnet possibly even occurs that a part of Hcj of magnet is significantly improved, and
Another part then improves unconspicuous phenomenon.
Summary of the invention
It is an object of the invention to provide a kind of method that R-T-B series magnet is carried out Dy diffusion, to solve in prior art
The problems referred to above existed.The present invention by will the particle diameter that be filled in refractory metal net 0.5～2mm Dy particle or
Dy alloying pellet substitutes Dy plate or Dy alloy sheets uses, to save the usage amount of Dy material.
The technical scheme that the present invention provides is as follows:
The method that R-T-B series magnet is carried out Dy diffusion, configures the preparation of R-T-B based sintered magnet in being included in process chamber
Engineering, the preparatory construction in the Dy diffusion source in same process chamber, and make Dy diffusion source be evaporated to described sintered magnet
Dy spreads engineering, it is characterised in that: described Dy diffusion source is the Dy particle being arranged in refractory metal net or Dy conjunction
Gold grain, the particle diameter of described Dy particle or described Dy alloying pellet is 0.5～2mm.
Dy particle that the present invention is placed by dispersion or Dy alloying pellet, prepare the Dy diffusion source consistent with magnet shape,
To ensure diffuser efficiency and diffusing qualities, reduce the usage amount of Dy material, increase the evaporation supply-side of Dy diffusion simultaneously,
Here evaporation supply-side is the surface that Dy diffusion source comes close to or in contact with sintered magnet, uses as spread source at magnet and Dy
When the mode of stacked on top is placed, being the upper and lower surface in Dy diffusion source, meanwhile, the upper and lower surface of sintered magnet is formed and connects
Receipts face.
Dy particle or Dy alloying pellet are filled in refractory metal net and prepare Dy diffusion source by the present invention, and by Dy
Diffusion source, magnet intersect to stack places, and makes Dy diffusion source become controlled to the diffusion length of magnet, it is thus achieved that magnetic property is more
The magnet of equilibrium.
Further, the present invention is to use the Dy particle or Dy alloying pellet being filled in refractory metal net, therefore,
It is not only used on the magnet of regular shape, it is also possible to by changing the shape of refractory metal net, it is thus achieved that with arch magnetic
The arbitrary shape Dy diffusion source that the on-plane surface magnet shape such as iron or annular magnet is corresponding, so that Dy diffusion source is to on-plane surface
The diffusion length of magnet also becomes controlled, makes technique more stable, controlled, and obtains the magnet that Hcj equilibrium improves.
It should be noted that R-T-B based sintered magnet here is containing R2Fe14The magnet of B principal phase, described R is
At least one in the rare earth element comprising yttrium, described T is at least one the transition metal unit including Fe
Element.
Identical with Dy, Tb or Ho is also the element being commonly used in grain boundary decision, therefore, by disclosed
Content, when the grain boundary decision of Tb or Ho, also should fall in the protection domain of technical solution of the present invention.
It addition, for cost control and the consideration of industry operability, the present invention selects to use Dy particle or Dy to close
The particle diameter of gold grain is 0.5～2mm, but if other practitioners are for evading the consideration of patent content, selects to allow part
The particle diameter of Dy particle or Dy alloying pellet is slightly larger than above-mentioned size or is slightly less than Dy particle and the Dy alloy of above-mentioned size
Grain, it should also fall under the scope of the present invention.
The present invention is not intended in refractory metal net fill Dy particle or the mode of Dy alloying pellet, and it both can use
The refractory metal box of first prefabricated upper shed, puts into Dy particle or Dy alloying pellet the most wherein, then covers high-melting-point
Metal top cover, it would however also be possible to employ the first refractory metal bag of prefabricated side opening, puts into Dy particle the most wherein or Dy closes
Gold grain, the mode of re-closed opening.
In the embodiment recommended, described Dy alloying pellet is Dy metal and the alloy made by other low-melting-point metals
Particle, such as Dy-Fe-Ga alloy, Dy-Cu-Ga alloy etc..
In the embodiment recommended, for cost control and the consideration of industry operability, the thickness of described refractory metal net
Degree is 0.5mm～2mm.
In the embodiment recommended, described Dy diffusion source is the discrete Dy particle being arranged in described refractory metal net
Or Dy alloying pellet, described Dy particle or described Dy alloying pellet are spherical particle, and it is arranged in homogeneous evaporation source.
Preferably, described Dy particle or described Dy alloying pellet are shape, uniform spheric granules.It is highly preferred that institute
Stating Dy diffusion source is to lay the individual layer Dy particle or individual layer Dy alloying pellet being arranged in described refractory metal net.
In existing Dy diffusion process, it is desirable to provide the evaporation supply-side being evenly distributed, supply-side is evenly distributed, ability
Stably providing Dy atom to corresponding receiving plane, the present invention obtains the Dy diffusion being evenly distributed by the way of assembled arrangement
Source (as used the evenly distributed of Dy particle that shape, size, material are the most consistent or Dy alloying pellet, or use shape,
Several Dy particles or the regular intervals of several Dy alloying pellet that size, material are inconsistent arrange), provide distribution all with this
Even evaporation supply-side carries out Dy diffusion, it is thus achieved that high performance magnet.It addition, for ease of industrialized production, should use up and can drop
The thickness in low Dy diffusion source, therefore, Dy particle or the general single berth of Dy alloying pellet are located in refractory metal net, this
(when can avoid paved in multi-layers, the intersection of Dy particle or Dy alloying pellet is put the most beneficially to obtain the supply-side that is evenly distributed
Put).In view of above-mentioned reason, generally, the present invention selects to use Dy particle or the Dy alloy of regular shape
Particle, if but having including a small amount of inferior Dy particle or inferior Dy alloying pellet be mixed in the fabrication process, the most not
Affect the enforcement of the present invention, it should within listing protection scope of the present invention in.
In the present invention, the Dy particle of discrete arrangement or Dy alloying pellet can be by the refractory metals arranged that pressurizes up and down
Net is fixing, it is also possible to by the way of arranging partition, make Dy particle or the discrete arrangement of Dy alloying pellet.
In the embodiment recommended, described Dy particle or described Dy alloying pellet are prepared by such a way: 1) accurate
Standby surface is with the high temperature resistant substrate of several grooves；2) powder of Dy powder or formation Dy alloy is put in groove, molten
Melt；3) fused solution solidification obtains prefabricated spherical particle；4) surface processes, and obtains class spherical Dy particle or class is spherical
Dy alloying pellet.Obtain the skill that shape, uniform Dy spherical particle or Dy alloy type spheric granules are the present invention
One of art main points.
In the embodiment recommended, described high temperature resistant substrate is W substrate, Mo substrate, Nb substrate, Ta substrate, Ti
Substrate or Zr substrate.
In the embodiment recommended, described Dy particle or described Dy alloying pellet are prepared by such a way: 1) accurate
The standby Cu crucible with several grooves, as anode, and does negative electrode with tungsten bar；2) in Cu crucible, Dy powder it is filled with
Or form the powder of Dy alloy；3) arc discharge, melted, it is spherical prefabricated that fused solution obtains class at described recessed in-tank-solidification
Particle；4) surface processes, and obtains class spherical Dy particle or class spherical Dy alloying pellet.
In the embodiment recommended, in described process chamber, configure described sintered magnet, this sintered magnet is heated to
In the range of 750～1050 DEG C, the described Dy diffusion source being arranged in same process chamber is heated and is allowed to evaporate, this steaming
The Dy atom sent out provides described sintered magnet surface, and is allowed to adhere to.
In the embodiment recommended, the Dy of peripheral hardware refractory metal net is spread source and is directly placed at described sintered magnet table
Face.Owing to the existence of refractory metal net, Dy particle or Dy alloying pellet can be by suitably regulation refractory metal nets
Thickness, makes Dy particle or Dy alloying pellet and sintered magnet be spaced most suitable diffusion length and places, and without carving
Distance between meaning regulation sintered magnet and Dy particle or Dy alloying pellet.
Recommend embodiment in, described refractory metal net be Mo net, W net, Nb net, Ta net, Ti net or
Zr net.
Another object of the present invention is to provide a kind of Novel magnetic body.
Magnet, with the method manufacture that R-T-B based sintered magnet carries out Dy diffusion of above-mentioned record.
It is still another object of the present invention to provide a kind of Dy and spread source.
Diffusion source, including the Dy particle being filled in refractory metal net or Dy alloying pellet, described Dy particle or institute
State the particle diameter of Dy alloying pellet 0.5～2mm.
Seen from the above description, the present invention has a following feature:
1) present invention is placed by arrangement Dy particle or Dy alloying pellet, it is thus achieved that Dy spreads source, reduces Dy with this
The usage amount of material, it is ensured that diffuser efficiency and diffusing qualities, increases the evaporation supply-side in Dy diffusion source simultaneously；
2) can be by Dy particle or the distributed quantity of Dy alloying pellet in regulation Dy diffusion source, as used discrete mode
Place, to use minimum ball to reach same diffusion effect；
3) it can obtain preferable Dy diffusion effect in a low temperature of 750～850 DEG C；
4) Dy diffusion can be derived from by being fabricated to corresponding shape according to the shape of magnet by the present invention, and strong adaptability utilizes
Rate is high；
5) present invention is directly placed at sintered magnet surface by Dy spreads source, such that it is able to by adjusting high-melting-point gold
Belonging to the thickness of net, regulation Dy particle or Dy alloying pellet, to the diffusion length of sintered magnet, use more convenient；
6), in the present invention, the Dy obtaining being evenly distributed by the way of assembled arrangement spreads source, provides with this and is evenly distributed
Supply-side carry out Dy diffusion, it is thus achieved that high performance magnet.
Accompanying drawing explanation
Fig. 1 is the schematic diagram that embodiment prepares spherical Dy particle.
Fig. 2 is the signal face (vertical direction) that single berth is located at the Dy particle in Mo net；
Fig. 3 is the schematic diagram of the discrete Dy particle being laid in plane Mo net of individual layer.
Fig. 4 is the schematic diagram that single berth is located at the Dy particle in semicircle Mo net.
Fig. 5 is the schematic diagram of the discrete Dy particle being arranged in Mo net.
Fig. 6 is the use state diagram in arc Dy diffusion source.
Detailed description of the invention
Embodiment
As shown in fig. 1, preparation Dy diffusion source comprises the following steps that
1) surface is prepared with several shapes, the W substrate 1 of circular groove 10 that size is identical；
2) in groove 10, put into the Dy powder of equivalent weight, melted；
3) fused solution solidification obtains prefabricated spherical particle；
4) surface processes, and obtains spherical Dy particle 2；
Selecting the W substrate of band different size groove 10, making particle diameter respectively is 0.5mm, 1.0mm, 1.5mm, 2.0mm
Spherical Dy particle.
After obtaining spherical Dy particle 2, being paved with by Dy particle 2 individual layer of different-grain diameter at thickness is 0.5～2mm
Mo net 3 in, prepare Dy spread source, the most as shown in Figure 2, Mo net thickness embody the most in the drawings.
Can also be arranged in discrete for Dy particle 2 in plane Mo net 3 as shown in Figure 3, to use minimum
Grain reaches same diffusion effect, and the thickness of Mo net embodies the most in the drawings.
It is of course also possible to as shown in Fig. 4, Dy particle 2 is fills up in semicircle Mo net 3, different to be applicable to
Shape magnet, the thickness of Mo net embodies the most in the drawings.
Can also be arranged in discrete for Dy particle 2 in semicircle Mo net 3 as shown in Fig. 5, minimum to use
Particle reaches same diffusion effect, reduces Dy materials'use amount, and the thickness of Mo net embodies the most in the drawings.
Can also be arranged in discrete for Dy particle 2 in arc Mo net 3 as shown in Figure 6, the use in arc diffusion source
As shown in FIG., 5 is magnet to state, and the thickness of Mo net embodies the most in the drawings.
Test example 1
(one-tenth is grouped into Nd to the sintered magnet of Overheating Treatment of learning from else's experience28.9Dy2.6Cu0.1Al0.5Nb0.2B1.05Febal.) processing growth
15mm, wide 8mm, the product of thickness 5mm, 5mm direction is magnetic field orientating direction, and classify in three categories part, is respectively sky
White example, comparative example and test example.
Blank example: the magnet that sintered body is made directly carries out magnetic property detection as the magnet processed without grain boundary decision, evaluation
Its magnetic characteristic.
Comparative example: the magnet that sintered body is made is cleaned, after clean surface, in vacuum heat treatment furnace, with Dy metallic plate
The order stacking of (thickness is 1mm), Mo separation net (thickness is 2mm) and sintered magnet is placed, afterwards with 800 DEG C
Temperature DIFFUSION TREATMENT 6 hours in an ar atmosphere.
Test example: the magnet that sintered body is made is cleaned, after clean surface, in vacuum heat treatment furnace, by embodiment
(Dy particle is discrete to be arranged in plane Mo net, and Mo net thickness is 2mm, Dy particle in the Dy diffusion source prepared
Particle diameter be the stack thickness of 1mm, Dy particle be 1mm) and sintered magnet stacking place, exist with the temperature of 800 DEG C afterwards
DIFFUSION TREATMENT 6 hours in Ar atmosphere.
Ageing Treatment: above-mentioned magnet (comparative example and test example) after Dy grain boundary decision processes is all the temperature of 550 DEG C
Degree carries out Ageing Treatment, makes Dy element the most fully diffusion in magnet crystal boundary of evaporation.
Magnetic property evaluation procedure: sintered magnet use China metering institute NIM-10000H type BH block rare earth permanent magnetism without
Waste measurement system carries out magnetic property detection.
The magnet evaluation result of blank example, comparative example and test example is as shown in table 1:
The situation that the magnetic property of the blank example of table 1, comparative example and test example is evaluated
In Dy diffusion source, the usage amount of Dy material is the 1/3 of Dy plate body materials'use amount.
Test example 2
(one-tenth is grouped into Nd to the sintered magnet of Overheating Treatment of learning from else's experience23.4Pr5.5Dy2.6Cu0.1Al0.5Nb0.2B1.05Febal) processing
Growth 15mm, wide 8mm, the product of thickness 5mm, 5mm direction is magnetic field orientating direction, and classify in three categories part, respectively
For blank example, comparative example and test example.
Blank example: the magnet that sintered body is made directly carries out magnetic property detection as the magnet processed without grain boundary decision, evaluation
Its magnetic characteristic.
Comparative example: the magnet that sintered body is made is cleaned, after clean surface, in vacuum heat treatment furnace, with Dy metallic plate
The order stacking of (thickness is 1.5mm), Mo net (thickness is 0.5mm) and sintered magnet is placed, afterwards with 850 DEG C
Temperature DIFFUSION TREATMENT 6 hours in an ar atmosphere.
Test example: the magnet that sintered body is made is cleaned, after clean surface, in vacuum heat treatment furnace, by embodiment system
(Dy particle is discrete to be arranged in plane Mo net, and Mo net thickness is 0.5mm, Dy particle in the Dy diffusion source obtained
Particle diameter be the stack thickness of 1.5mm, Dy particle be 1.5mm) and sintered magnet stacking place, afterwards with the temperature of 850 DEG C
Spend DIFFUSION TREATMENT 6 hours in an ar atmosphere.
Ageing Treatment: above-mentioned magnet (comparative example and test example) after Dy grain boundary decision processes is all the temperature of 550 DEG C
Degree carries out Ageing Treatment, makes Dy element the most fully diffusion in magnet crystal boundary of evaporation.
Magnetic property evaluation procedure: sintered magnet use China metering institute NIM-10000H type BH block rare earth permanent magnetism without
Waste measurement system carries out magnetic property detection.
The evaluation result of the magnet of blank example, comparative example and test example is as shown in table 2:
The situation that the magnetic property of the blank example of table 2, comparative example and test example is evaluated
In Dy diffusion source, the usage amount of Dy material is the 1/3 of Dy plate body materials'use amount.
Test example 3
(one-tenth is grouped into Nd to the sintered magnet of Overheating Treatment of learning from else's experience31.5Al0.6Nb0.2B1.05Febal) processing growth 15mm,
Wide 8mm, the product of thickness 5mm, 5mm direction is magnetic field orientating direction, and classify in three categories part, the most blank example,
Comparative example and test example.
Blank example: the magnet that sintered body is made directly carries out magnetic property detection as the magnet processed without grain boundary decision, evaluation
Its magnetic characteristic.
Comparative example: the magnet that sintered body is made is cleaned, after clean surface, in vacuum heat treatment furnace, with Dy metallic plate
The order stacking of (thickness is 2.0mm), Mo net (thickness is 1.5mm) and sintered magnet is placed, afterwards with 900 DEG C
Temperature DIFFUSION TREATMENT 6 hours in an ar atmosphere.
Test example: the magnet that sintered body is made is cleaned, after clean surface, in vacuum heat treatment furnace, by embodiment system
(Dy particle is discrete to be arranged in plane Mo net, and Mo net thickness is 1.5mm, Dy particle in the Dy diffusion source obtained
Particle diameter be the stack thickness of 2.0mm, Dy particle be 2.0mm) and sintered magnet stacking place, afterwards with the temperature of 900 DEG C
Spend DIFFUSION TREATMENT 6 hours in an ar atmosphere.
Ageing Treatment: above-mentioned magnet (comparative example and test example) after Dy grain boundary decision processes is all the temperature of 550 DEG C
Degree carries out Ageing Treatment, makes Dy element the most fully diffusion in magnet crystal boundary of evaporation.
Magnetic property evaluation procedure: sintered magnet use China metering institute NIM-10000H type BH block rare earth permanent magnetism without
Waste measurement system carries out magnetic property detection.
The evaluation result of the magnet of blank example, comparative example and test example is as shown in table 3:
The situation that the magnetic property of the blank example of table 3, comparative example and test example is evaluated
In Dy diffusion source, the usage amount of Dy material is the 1/3 of Dy plate body materials'use amount.
Test example 4
(one-tenth is grouped into Nd to the sintered magnet of Overheating Treatment of learning from else's experience31.5Cu0.2Nb0.2B1.05Febal) processing growth 15mm,
Wide 8mm, the product of thickness 5mm, 5mm direction is magnetic field orientating direction, and classify in three categories part, the most blank example,
Comparative example and test example.
Blank example: the magnet that sintered body is made directly carries out magnetic property detection as the magnet processed without grain boundary decision, evaluation
Its magnetic characteristic.
Comparative example: the magnet that sintered body is made is cleaned, after clean surface, in vacuum heat treatment furnace, with Dy metallic plate
The order stacking of (thickness is 0.5mm), Mo net (thickness is 1mm) and sintered magnet is placed, afterwards with 950 DEG C
Temperature DIFFUSION TREATMENT 6 hours in an ar atmosphere.
Test example: the magnet that sintered body is made is cleaned, after clean surface, in vacuum heat treatment furnace, by embodiment system
(Dy particle is discrete to be arranged in plane Mo net, and Mo net thickness is the grain of 1mm, Dy particle in the Dy diffusion source obtained
Footpath be the stack thickness of 0.5mm, Dy particle be 0.5mm) and sintered magnet stacking place, afterwards with the temperature of 950 DEG C
DIFFUSION TREATMENT 6 hours in an ar atmosphere.
Ageing Treatment: above-mentioned magnet (comparative example and test example) after Dy grain boundary decision processes is all the temperature of 500 DEG C
Degree carries out Ageing Treatment, makes Dy element the most fully diffusion in magnet crystal boundary of evaporation.
Magnetic property evaluation procedure: sintered magnet use China metering institute NIM-10000H type BH block rare earth permanent magnetism without
Waste measurement system carries out magnetic property detection.
The evaluation result of the magnet of blank example, comparative example and test example is as shown in table 4:
The situation that the blank example of table 4, comparative example and the magnetic property evaluation of test example and crystallite dimension are evaluated
In Dy diffusion source, the usage amount of Dy material is the 1/3 of Dy plate body materials'use amount.
Test example 5
(one-tenth is grouped into Nd to the sintered magnet of Overheating Treatment of learning from else's experience28.9Dy2.6Cu0.2Nb0.2B1.05Febal) processing growth
15mm, wide 8mm, the product of thickness 5mm, 5mm direction is magnetic field orientating direction, is divided into 2 equal portions, the most right
Ratio and test example.
Comparative example: the magnet that sintered body is made is cleaned, and after clean surface, is divided into 9 groups, each group sintered magnet is put respectively
Insert in vacuum heat treatment furnace, with Dy metallic plate (thickness is as 1.5mm), Mo net (thickness is as 1.5mm) and sintering
The order stacking of magnet is placed, the most respectively with temperature DIFFUSION TREATMENT 6 hours in an ar atmosphere of 700～1100 DEG C.
Test example: the magnet that sintered body is made is cleaned, and after clean surface, is divided into 9 groups, each group sintered magnet is placed into
In vacuum heat treatment furnace, (Dy particle is discrete to be arranged in plane Mo net, Mo in Dy diffusion source embodiment prepared
Net thickness be the stack thickness that particle diameter is 1.5mm, Dy particle of 1.5mm, Dy particle be 1.5mm) and sintered magnet
Stacking is placed, the most respectively with temperature DIFFUSION TREATMENT 6 hours in an ar atmosphere of 700～1100 DEG C.
Ageing Treatment: above-mentioned magnet after Dy grain boundary decision processes carries out Ageing Treatment in the atmosphere of 500 DEG C, makes steaming
The Dy element sent out is the most fully diffusion in magnet crystal boundary.
Magnetic property evaluation procedure: sintered magnet use China metering institute NIM-10000H type BH block rare earth permanent magnetism without
Waste measurement system carries out magnetic property detection.
The evaluation result of the magnet of comparative example and test example is as shown in table 5:
The situation that the magnetic property of table 5 comparative example and test example is evaluated
As can be seen from the table, use the present invention Dy diffusion source after, 750 DEG C, 800 DEG C, 850 DEG C time
Obtaining good grain boundary decision effect, grain boundary decision can be carried out at low temperatures.
Above-described embodiment is only used for further illustrating the detailed description of the invention of the present invention, but the invention is not limited in embodiment,
Every any simple modification, equivalent variations and modification made above example according to the technical spirit of the present invention, each falls within
In the protection domain of technical solution of the present invention.
Claims (7)
1. pair method that R-T-B series magnet carries out Dy diffusion, prepares the beam worker of R-T-B based sintered magnet in being included in process chamber
Journey, the preparatory construction in the Dy diffusion source in same process chamber, and make Dy diffusion source be evaporated to the Dy diffusion of described sintered magnet
Engineering, it is characterised in that: described Dy diffusion source is Dy particle or the Dy alloying pellet being arranged in refractory metal net, described Dy
Grain or Dy alloying pellet are spherical particle or the spheric granules being arranged in homogeneous diffusion source, and its particle diameter is 0.5～2mm, described
Dy particle or Dy alloying pellet by Dy powder or formed the powder melts of Dy alloy be solidified on setting reeded substrate within and obtain
Arrive；Described R is at least one in the rare earth element comprising yttrium, and described T is at least one including Fe
Transition metal, described B is boron element.
The method that R-T-B series magnet is carried out Dy diffusion the most according to claim 1, it is characterised in that: described high-melting-point
The thickness of wire netting is 0.5～2mm, and described Dy diffusion source is the discrete Dy particle being arranged in described refractory metal net or Dy
Alloying pellet.
The method that R-T-B series magnet is carried out Dy diffusion the most according to claim 2, it is characterised in that: described Dy spreads
Source is to lay the individual layer Dy particle or individual layer Dy alloying pellet being arranged in described refractory metal net.
The method that R-T-B series magnet is carried out Dy diffusion the most according to claim 1, it is characterised in that: in described process
The indoor described sintered magnet of configuration, in the range of this sintered magnet is heated to 750～1050 DEG C, being arranged in same process chamber
Described Dy diffusion source heat and be allowed to evaporate, provide described sintered magnet surface the Dy atom evaporated, and be allowed to adhere to.
The method that R-T-B series magnet is carried out Dy diffusion the most according to claim 1, it is characterised in that: described Dy spreads
Source is directly placed at described sintered magnet surface.
The method that R-T-B series magnet is carried out Dy diffusion the most according to claim 1, it is characterised in that: described high-melting-point
Wire netting is Mo net, W net, Nb net, Ta net, Ti net or Zr net.
7. magnet, it is characterised in that: with the method manufacture recorded any one of claim 1～6.
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| CN101163814A (en) * | 2005-03-18 | 2008-04-16 | 株式会社爱发科 | Method of film formation, film formation apparatus, permanent magnet, and process for producing permanent magnet |
| CN101331566A (en) * | 2006-03-03 | 2008-12-24 | 日立金属株式会社 | R-Fe-B rare earth sintered magnet and method for producing same |
| CN101506919A (en) * | 2006-08-23 | 2009-08-12 | 株式会社爱发科 | Permanent magnet and process for producing the same |
| CN101517120A (en) * | 2006-09-14 | 2009-08-26 | 株式会社爱发科 | Vacuum evaporation processing equipment |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101163814A (en) * | 2005-03-18 | 2008-04-16 | 株式会社爱发科 | Method of film formation, film formation apparatus, permanent magnet, and process for producing permanent magnet |
| CN101331566A (en) * | 2006-03-03 | 2008-12-24 | 日立金属株式会社 | R-Fe-B rare earth sintered magnet and method for producing same |
| CN101506919A (en) * | 2006-08-23 | 2009-08-12 | 株式会社爱发科 | Permanent magnet and process for producing the same |
| CN101517120A (en) * | 2006-09-14 | 2009-08-26 | 株式会社爱发科 | Vacuum evaporation processing equipment |
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