CN106298132A - A kind of SmCo of thermal deformation method preparation doping PrCu alloy5the method of permanent magnet - Google Patents
A kind of SmCo of thermal deformation method preparation doping PrCu alloy5the method of permanent magnet Download PDFInfo
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- CN106298132A CN106298132A CN201610885173.5A CN201610885173A CN106298132A CN 106298132 A CN106298132 A CN 106298132A CN 201610885173 A CN201610885173 A CN 201610885173A CN 106298132 A CN106298132 A CN 106298132A
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- 238000000034 method Methods 0.000 title claims abstract description 59
- 229910000938 samarium–cobalt magnet Inorganic materials 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 78
- 239000000956 alloy Substances 0.000 claims abstract description 50
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 34
- 230000005291 magnetic effect Effects 0.000 claims abstract description 24
- 238000005245 sintering Methods 0.000 claims description 23
- 238000000498 ball milling Methods 0.000 claims description 21
- 238000005266 casting Methods 0.000 claims description 18
- 238000000713 high-energy ball milling Methods 0.000 claims description 17
- 238000003723 Smelting Methods 0.000 claims description 14
- 239000000725 suspension Substances 0.000 claims description 14
- 238000010791 quenching Methods 0.000 claims description 13
- 230000000171 quenching effect Effects 0.000 claims description 13
- 238000007599 discharging Methods 0.000 claims description 12
- 238000002844 melting Methods 0.000 claims description 12
- 230000008018 melting Effects 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 12
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 12
- 238000011049 filling Methods 0.000 claims description 10
- 239000013078 crystal Substances 0.000 claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- 229910002804 graphite Inorganic materials 0.000 claims description 6
- 239000010439 graphite Substances 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000011812 mixed powder Substances 0.000 claims description 6
- 150000002910 rare earth metals Chemical class 0.000 claims description 6
- 230000005389 magnetism Effects 0.000 claims description 5
- 239000002131 composite material Substances 0.000 claims description 2
- 238000009792 diffusion process Methods 0.000 claims description 2
- 238000002955 isolation Methods 0.000 claims description 2
- 238000010168 coupling process Methods 0.000 abstract description 7
- 238000005859 coupling reaction Methods 0.000 abstract description 7
- 230000003993 interaction Effects 0.000 abstract description 5
- 239000000696 magnetic material Substances 0.000 abstract description 2
- 239000012071 phase Substances 0.000 description 21
- 230000000052 comparative effect Effects 0.000 description 9
- 238000007731 hot pressing Methods 0.000 description 8
- 238000009413 insulation Methods 0.000 description 5
- 229910001172 neodymium magnet Inorganic materials 0.000 description 5
- 229910000743 fusible alloy Inorganic materials 0.000 description 4
- 230000005415 magnetization Effects 0.000 description 4
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 3
- 239000010931 gold Substances 0.000 description 3
- RZJQYRCNDBMIAG-UHFFFAOYSA-N [Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Zn].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn] Chemical class [Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Zn].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn] RZJQYRCNDBMIAG-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 235000013339 cereals Nutrition 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000008878 coupling Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 229910004269 CaCu5 Inorganic materials 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000005294 ferromagnetic effect Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 239000006247 magnetic powder Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/0555—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 pressed, sintered or bonded together
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
-
- 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
- H01F41/0273—Imparting anisotropy
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Hard Magnetic Materials (AREA)
- Powder Metallurgy (AREA)
Abstract
A kind of SmCo of thermal deformation method preparation doping PrCu alloy5The method of permanent magnet, belongs to technical field of magnetic materials.It is 2～15wt.% that PrCu alloy powder for doping accounts for the weight ratio of total powder.SmCo5The deflection of magnet is 60%～90%.Using SPS technomania deformation method to prepare, during thermal deformation, PrCu phase is as interface phase, can completely cut off SmCo5And SmCo5Two Hard Magnetic phases, weaken SmCo5And SmCo5Exchange-coupling interaction between two Hard Magnetics phases, improves coercivity；During thermal deformation, PrCu phase is dispersed in grain boundaries after liquefying, and can promote SmCo5The thermal deformation of phase；The SmCo of doping PrCu alloy5The performance of heat distortion magnet significantly improves.The SmCo of the nanocrystalline doping PrCu alloy obtained5Magnet has good magnetic property, heat stability, decay resistance and mechanical property.
Description
Technical field
The present invention is a kind of hot-pressing thermal deformation method preparation doping PrCu alloy using discharge plasma sintering technique
SmCo5The method of rare-earth permanent magnet, belongs to technical field of magnetic materials.
Background technology
Magnet to be realized practical, it is necessary to the high-performance anisotropy magnet that preparation is block, prepares massive anisotropic
The main method of magnet has traditional powder metallurgic method and hot-pressing thermal deformation method.SmCo5The preparation method of magnet is usually tradition
Powder metallurgic method.The crystal grain of anisotropy magnet prepared by traditional powder metallurgic method is all micron-sized.And hot-pressing thermal becomes
Shape method can prepare nanocrystalline anisotropy magnet.
Nanocrystalline magnet has single domain size, can improve the coercivity of material；Strong exchange coupling is there is between nanocrystalline
Close, improve the remanence ratio of material, the magnetic property of enhancing magnet.But the cluster effect between nano-particle is very strong, powder is orientated
Extremely difficult, it is impossible to use traditional method to prepare anisotropy magnet, so the method system that research worker uses hot-pressing thermal deformation
Take anisotropic nanocrystalline magnet, and obtain successfully.It is under certain temperature and pressure, first obtains nanocrystalline
Hot-pressed magnets, then makes nanocrystalline hot-pressed magnets carry out thermal deformation, reaches suitable deformation quantity, thus obtains deformation texture and formed
Nanocrystalline anisotropy magnet.The mechanical property of nanocrystalline magnet and decay resistance are all significantly better than the micron crystalline substance magnetic of sintering
Body.Therefore, thermal deformation method is used to prepare nanocrystalline SmCo5Magnet, is paid close attention to by researcher always.
SmCo5Compound has CaCu5The hexagonal structure of type, hexagonal crystallographic texture is owing to having less sliding in theory
System, so deformation difficulty, this also causes SmCo5There is high rigidity inductile feature at normal temperatures.But, work as SmCo5Crystal grain chi
Very little when reaching nanoscale, at high temperature carry out thermal deformation field, it is the highest, thus that the deflection of magnet can reach 90%
The anisotropy nanocrystalline magnet with good deformation texture can be obtained.2008, Univ Dayton's M.Q.Huang fast quenching and heat
Deformation method prepares SmCo system anisotropy nanocrystalline magnet, it is thus achieved that hard axis and remanence ratio M of easy axler-hard/Mr-easy=0.4,
Hci=9kOe, (BH)max=13.2MGOe.And this seminar proposes one and utilizes discharge plasma sintering system (being called for short SPS)
The new technique of preparation hot pressing heat distortion magnet, i.e. aximal deformation value, high temperature, the heavily stressed and SPS thermal deformation new technique of low strain dynamic rate.
The method goes out the magnet of nanocrystalline (20～50nm) initially with SPS hot pressed sintering, is then put into by magnet in mould and carries out SPS
Thermal deformation, obtains the c-axis direction (easy magnetizing axis) of the crystal grain lath-shaped nanoscale arranged in parallel with pressure direction and (～hundreds of receives
Rice) crystal grain, thus obtain preferable deformation texture and high magnetic property.To SmCo5For magnet, find only at aximal deformation value
Under (80～95%) be only possible to obtain obvious deformation texture.SmCo5Magnet, when deflection is 90%, defines strong
(00l) texture in direction, its (002) peak is far above other diffraction maximums, and the remanent magnetism of magnet is 8.4kGs, and remanence ratio is 90%, rectifys
Stupid power is 10kOe, and maximum magnetic energy product is 17.3MGOe, and the magnet after thermal deformation has strong anisotropy and high magnetic characteristics.
But, this SmCo5Magnet coercivity after deformation declines more, therefore, how to improve heat distortion magnet
Coercivity become the emphasis of current research.And Fangming Wan of Peking University et al. have developed at single-phase NdFeB magnet
The PrCu liquid phase alloy of middle doping low melting point, it is thus achieved that the magnet of high-coercive force.Its coercitive increase and the change of grain boundary layer
Relevant.Current research shows, in traditional NdFeB magnet, its Grain-Boundary Phase is not non-magnetic phase, has ferromagnetic, its
There is exchange-coupling interaction in intercrystalline.Therefore, once magnetic reversal farmland is at defect or sharp-pointed edge's forming core, due to magnetic reversal
The extension on farmland, reverse magnetization process is easy to carry out.But, after the nonmagnetic PrCu alloy that adulterates, grain boundaries defines thickness
With nonmagnetic boundary region, between crystal grain, go magnetic coupling more preferable, so in the more difficult continuity of intercrystalline magnetization inversion.Separately
Outward, due to grain boundary become more smooth, also counteracts that the forming core on magnetic reversal farmland.Therefore, doping PrCu alloy is single-phase
NdFeB magnet obtains the highest coercivity.
It addition, file CN102248157A also discloses that a kind of PrCu alloy that spreads in NdFeB magnetic powder improves coercivity
Method.The method of above-mentioned doping PrCu alloy has been obtained for good result in single-phase NdFeB magnet, but at SmCo5Magnetic
Body does not the most carry out relevant report.Therefore, the application proposes a kind of to use thermal deformation method preparation doping PrCu alloy
SmCo5The new method of permanent magnet.
At SmCo5High-energy ball milling powder is mixed into the liquid phase alloy PrCu powder of low melting point, then uses SPS to carry out thermal deformation
Obtain nanocrystalline anisotropic magnet.This method mainly has a following benefit: 1. in thermal deformation process PrCu phase as interface
Phase, can completely cut off SmCo5Hard Magnetic phase, weakens the exchange-coupling interaction between two Hard Magnetics phases, improves coercivity；In 2.PrCu alloy
Pr can substitute Sm enter SmCo5In principal phase, form (SmPr) Co5Compound, and (SmPr) Co5Saturation magnetization high
In SmCo5, it is thus possible to improve saturation magnetization and the remanent magnetism of magnet, thus improve the magnetic property of magnet；3. in thermal deformation
During PrCu phase liquefy after be dispersed in grain boundaries, it is also possible to coordinate SmCo5Thermal deformation, finally promote SmCo5Obtain good change
Shape texture.And SPS technology has high pressure, low temperature, quickly sinters advantage, it is possible to inhibiting grain growth, and can high pressure,
Magnet densification is made under conditions of low temperature.Therefore, the SmCo of PrCu alloy it is doped with5Magnet, becomes after thermal deformation and has well
Deformation texture and the nanocrystalline SmCo of high-coercive force5Permanent magnet.
Summary of the invention
It is an object of the invention to provide a kind of SmCo using SPS thermal deformation method preparation doping PrCu alloy5Rare earth permanent magnet
The method of body.
A kind of SmCo of the PrCu alloy that adulterates5Rare-earth permanent magnet, it is characterised in that the PrCu alloy for doping accounts for gross weight
The ratio of amount is 2～15wt.%.The deflection of built-up magnet is 60%～90%.In PrCu alloy, the molar content of Pr is excellent
Elect 10～90% as.
The present invention is a kind of SmCo using SPS technomania deformation method preparation doping PrCu alloy5The side of rare-earth permanent magnet
Method, the method mainly comprises the following steps:
(1) melting, SmCo5It is respectively adopted suspension smelting furnace with PrCu alloy cast ingot to prepare；
(2) SmCo is prepared5Powder, uses high-energy ball milling method by SmCo5Ingot casting ball milling becomes SmCo5Amorphous powder；
(3) preparing PrCu powder, PrCu alloy is carried out fast quenching and obtains fast quenching thin strap, then employing high-energy ball milling method will
PrCu strip ball milling becomes PrCu amorphous powder；
(4) mixed powder, uses the method for ball milling by SmCo5It is uniform that powder and PrCu powder mix powder in proportion；
(5) powder is die-filling, is loaded in WC sintered-carbide die by the composite powder of mix homogeneously；
(6) hot-pressed magnets, uses discharging plasma sintering equipment, vacuum, pressure 450～500MPa, 680～720 DEG C
With insulation 30 seconds under conditions of hot pressed sintering, it is thus achieved that the SmCo of isotropic nanocrystalline doping PrCu alloy5Magnet；
(7) heat distortion magnet, loads hot-pressed magnets in graphite jig, use discharging plasma sintering equipment, vacuum,
Pressure 30～60MPa, heat distortion temperature is 800～900 DEG C, and deflection is 60～90%, it is thus achieved that anisotropic nanocrystalline
The SmCo of doping PrCu alloy5Permanent magnet；
(8) heat treatment, puts into heat distortion magnet in tube furnace, is incubated 1 hour under 650～680 DEG C of ar gas environments, promotees
Entering the diffusion of PrCu alloy, strengthen the isolation of the magnetic between crystal grain and improve the coercivity of magnet, Pr replaces part Sm and carries simultaneously
The high remanent magnetism of magnet.
Beneficial effects of the present invention
(1) relative to the SmCo of undoped p PrCu alloy5The mode of thermal deformation rare-earth permanent magnet, doping PrCu alloy
SmCo5Thermal deformation permanent magnet, during thermal deformation, PrCu phase is as interface phase, can weaken SmCo5And SmCo5Two Hard Magnetics
Exchange-coupling interaction between Xiang, improves coercivity；
(2) during thermal deformation, PrCu phase is dispersed in grain boundaries after liquefying, and can promote SmCo5The thermal deformation of phase and
Obtain good deformation texture；
(3) SmCo of the nanocrystalline doping PrCu alloy obtained5Permanent magnet, have good magnetic property, heat stability,
Decay resistance and mechanical property.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the invention will be further described, but protection scope of the present invention is not limited only to down
State embodiment.
Embodiment 1
(1) melting.SmCo5Ingot casting uses suspension smelting furnace to prepare；Pr10Cu90Low-melting alloy uses suspension smelting furnace system
Standby；
(2) SmCo is prepared5Powder.Use high-energy ball milling method by SmCo5Ingot casting ball milling becomes SmCo5Amorphous powder；
(3) PrCu powder is prepared.PrCu alloy being carried out fast quenching and obtains fast quenching thin strap, then employing high-energy ball milling method will
PrCu strip ball milling becomes PrCu amorphous powder；
(4) mixed powder.Use ball-milling method by SmCo5Powder and PrCu powder mix homogeneously, PrCu powder accounts for the 2wt.% of gross weight；
(5) powder is die-filling.The powder of mix homogeneously is loaded in WC sintered-carbide die；
(6) hot-pressed magnets.Use discharging plasma sintering equipment, vacuum, pressure 500MPa, 680 DEG C and insulation 30 seconds
Under conditions of hot pressed sintering, it is thus achieved that the SmCo of isotropic nanocrystalline doping PrCu alloy5Permanent magnet；
(7) heat distortion magnet.Hot-pressed magnets is loaded in graphite jig, use discharging plasma sintering equipment, vacuum,
Pressure 30MPa, heat distortion temperature is 800 DEG C, and deflection is 60%, it is thus achieved that the doping PrCu alloy that anisotropy is nanocrystalline
SmCo5Permanent magnet.
(8) heat treatment.Heat distortion magnet is put in tube furnace, under 650 DEG C of ar gas environments, be incubated 1 hour.
Comparative example 1
(1) melting.SmCo5Ingot casting uses suspension smelting furnace to prepare；
(2) SmCo is prepared5Powder.Use high-energy ball milling method by SmCo5Ingot casting ball milling becomes SmCo5Amorphous powder；
(3) powder is die-filling.By SmCo5Amorphous powder loads in WC sintered-carbide die；
(4) remaining step is with reference to embodiment 1.
Embodiment 2
(1) melting.SmCo5Ingot casting uses suspension smelting furnace to prepare；Pr30Cu70Low-melting alloy uses suspension smelting furnace system
Standby；
(2) SmCo is prepared5Powder.Use high-energy ball milling method by SmCo5Ingot casting ball milling becomes SmCo5Amorphous powder；
(3) PrCu powder is prepared.PrCu alloy being carried out fast quenching and obtains fast quenching thin strap, then employing high-energy ball milling method will
PrCu strip ball milling becomes PrCu amorphous powder；
(4) mixed powder.Use ball-milling method by SmCo5Powder and PrCu powder mix homogeneously, PrCu powder accounts for the 6wt.% of gross weight；
(5) powder is die-filling.The powder of mix homogeneously is loaded in WC sintered-carbide die；
(6) hot-pressed magnets.Use discharging plasma sintering equipment, vacuum, pressure 480MPa, 700 DEG C and insulation 30 seconds
Under conditions of hot pressed sintering, it is thus achieved that the SmCo of isotropic nanocrystalline doping PrCu alloy5Permanent magnet；
(7) heat distortion magnet.Hot pressing built-up magnet is loaded in graphite jig, use discharging plasma sintering equipment,
Vacuum, pressure 40MPa, heat distortion temperature is 850 DEG C, and deflection is 70%, it is thus achieved that the doping PrCu conjunction that anisotropy is nanocrystalline
The SmCo of gold5Permanent magnet.
(8) heat treatment.Heat distortion magnet is put in tube furnace, under 660 DEG C of ar gas environments, be incubated 1 hour.
Comparative example 2
(1) melting.SmCo5Ingot casting uses suspension smelting furnace to prepare；
(2) SmCo is prepared5Powder.Use high-energy ball milling method by SmCo5Ingot casting ball milling becomes SmCo5Amorphous powder；
(3) powder is die-filling.By SmCo5Amorphous powder loads in WC sintered-carbide die；
(4) remaining step is with reference to embodiment 2.
Embodiment 3
(1) melting.SmCo5Ingot casting uses suspension smelting furnace to prepare；Pr60Cu40Low-melting alloy uses suspension smelting furnace system
Standby；
(2) SmCo is prepared5Powder.Use high-energy ball milling method by SmCo5Ingot casting ball milling becomes SmCo5Amorphous powder；
(3) PrCu powder is prepared.PrCu alloy being carried out fast quenching and obtains fast quenching thin strap, then employing high-energy ball milling method will
PrCu strip ball milling becomes PrCu amorphous powder；
(4) mixed powder.Use ball-milling method by SmCo5Powder and PrCu powder mix homogeneously, PrCu powder accounts for gross weight
10wt.%；
(5) powder is die-filling.The powder of mix homogeneously is loaded in WC sintered-carbide die；
(6) hot-pressed magnets.Use discharging plasma sintering equipment, vacuum, pressure 500MPa, 700 DEG C and insulation 30 seconds
Under conditions of hot pressed sintering, it is thus achieved that the SmCo of isotropic nanocrystalline doping PrCu alloy5Permanent magnet；
(7) heat distortion magnet.Hot pressing built-up magnet is loaded in graphite jig, use discharging plasma sintering equipment,
Vacuum, pressure 50MPa, heat distortion temperature is 880 DEG C, and deflection is 80%, it is thus achieved that the doping PrCu conjunction that anisotropy is nanocrystalline
The SmCo of gold5Permanent magnet.
(8) heat treatment.Heat distortion magnet is put in tube furnace, under 670 DEG C of ar gas environments, be incubated 1 hour.
Comparative example 3
(1) melting.SmCo5Ingot casting uses suspension smelting furnace to prepare；
(2) SmCo is prepared5Powder.Use high-energy ball milling method by SmCo5Ingot casting ball milling becomes SmCo5Amorphous powder；
(3) powder is die-filling.By SmCo5Amorphous powder loads in WC sintered-carbide die；
(4) remaining step is with reference to embodiment 3.
Embodiment 4
(1) melting.SmCo5Ingot casting uses suspension smelting furnace to prepare；Pr90Cu10Low-melting alloy uses suspension smelting furnace system
Standby；
(2) SmCo is prepared5Powder.Use high-energy ball milling method by SmCo5Ingot casting ball milling becomes SmCo5Amorphous powder；
(3) PrCu powder is prepared.PrCu alloy being carried out fast quenching and obtains fast quenching thin strap, then employing high-energy ball milling method will
PrCu strip ball milling becomes PrCu amorphous powder；
(4) mixed powder.Use ball-milling method by SmCo5Powder and PrCu powder mix homogeneously, PrCu powder accounts for gross weight
15wt.%；
(5) powder is die-filling.The powder of mix homogeneously is loaded in WC sintered-carbide die；
(6) hot-pressed magnets.Use discharging plasma sintering equipment, vacuum, pressure 450MPa, 720 DEG C and insulation 30 seconds
Under conditions of hot pressed sintering, it is thus achieved that the SmCo of isotropic nanocrystalline doping PrCu alloy5Permanent magnet；
(7) heat distortion magnet.Hot pressing built-up magnet is loaded in graphite jig, use discharging plasma sintering equipment,
Vacuum, pressure 60MPa, heat distortion temperature is 900 DEG C, and deflection is 90%, it is thus achieved that the doping PrCu conjunction that anisotropy is nanocrystalline
The SmCo of gold5Permanent magnet.
(8) heat treatment.Heat distortion magnet is put in tube furnace, under 680 DEG C of ar gas environments, be incubated 1 hour.
Comparative example 4
(1) melting.SmCo5Ingot casting uses suspension smelting furnace to prepare；
(2) SmCo is prepared5Powder.Use high-energy ball milling method by SmCo5Ingot casting ball milling becomes SmCo5Amorphous powder；
(3) powder is die-filling.By SmCo5Amorphous powder loads in WC sintered-carbide die；
(4) remaining step is with reference to embodiment 4.
Under table 1 room temperature (20 DEG C), embodiment and the magnetic property of comparative example and density contrast
| Performance | Coercivity (kOe) | Remanent magnetism (kGs) | Density (g/cm3) |
| Embodiment 1 | 20.44 | 7.11 | 8.28 |
| Comparative example 1 | 18.25 | 7.16 | 8.25 |
| Embodiment 2 | 24.21 | 7.50 | 8.31 |
| Comparative example 2 | 20.35 | 7.55 | 8.28 |
| Embodiment 3 | 19.11 | 8.13 | 8.33 |
| Comparative example 3 | 17.56 | 8.22 | 8.28 |
| Embodiment 4 | 15.16 | 7.81 | 8.35 |
| Comparative example 4 | 10.15 | 8.30 | 8.29 |
Sum up
The present invention utilizes discharge plasma sintering to be prepared for the SmCo of a kind of PrCu alloy that adulterates5Rare-earth permanent magnet.Relatively
SmCo in undoped p PrCu alloy5The mode of thermal deformation rare-earth permanent magnet, the SmCo of doping PrCu alloy5Thermal deformation rare earth is forever
Magnet, during thermal deformation, PrCu phase is as interface phase, can completely cut off SmCo5And SmCo5Two Hard Magnetic phases, reduce counterdiffusion,
Weaken SmCo5And SmCo5Exchange-coupling interaction between two Hard Magnetics phases, improves coercivity；PrCu phase during thermal deformation
It is dispersed in grain boundaries after liquefaction, SmCo can be promoted5The thermal deformation of phase；The SmCo of doping PrCu alloy5Heat distortion magnet ratio is not mixed
Miscellaneous SmCo5The performance of heat distortion magnet significantly improves.The SmCo of the nanocrystalline doping PrCu alloy obtained5Magnet has well
Magnetic property, heat stability, decay resistance and mechanical property.
Claims (4)
1. the SmCo of the PrCu alloy that adulterates5Rare-earth permanent magnet, it is characterised in that the PrCu alloy for doping accounts for gross weight
Ratio be 2～15wt.%.
2. according to the SmCo of a kind of PrCu alloy that adulterates described in claim 15Rare-earth permanent magnet, it is characterised in that built-up magnet
Deflection be 60%～90%.
3. according to the SmCo of a kind of PrCu alloy that adulterates described in claim 15Rare-earth permanent magnet, it is characterised in that PrCu alloy
The molar content of middle Pr is 10～90%.
4. the SmCo of the preparation a kind of PrCu alloy that adulterates described in claim 15The method of rare-earth permanent magnet, it is characterised in that adopt
Prepare with SPS technomania deformation method, mainly comprise the following steps:
(1) melting, SmCo5It is respectively adopted suspension smelting furnace with PrCu alloy cast ingot to prepare；
(2) SmCo is prepared5Powder, uses high-energy ball milling method by SmCo5Ingot casting ball milling becomes SmCo5Amorphous powder；
(3) prepare PrCu powder, PrCu alloy is carried out fast quenching and obtains fast quenching thin strap, then use high-energy ball milling method that PrCu is thin
PrCu amorphous powder is worn in dribbling；
(4) mixed powder, uses the method for ball milling by SmCo5It is uniform that powder and PrCu powder mix powder in proportion；
(5) powder is die-filling, is loaded in WC sintered-carbide die by the composite powder of mix homogeneously；
(6) hot-pressed magnets, uses discharging plasma sintering equipment, vacuum, pressure 450～500MPa, 680～720 DEG C and guarantor
Temperature is hot pressed sintering under conditions of 30 seconds, it is thus achieved that the SmCo of isotropic nanocrystalline doping PrCu alloy5Magnet；
(7) heat distortion magnet, loads hot-pressed magnets in graphite jig, uses discharging plasma sintering equipment, at vacuum, pressure
30～60MPa, heat distortion temperature is 800～900 DEG C, and deflection is 60～90%, it is thus achieved that anisotropic nanocrystalline doping
The SmCo of PrCu alloy5Permanent magnet；
(8) heat treatment, puts into heat distortion magnet in tube furnace, is incubated 1 hour under 650～680 DEG C of ar gas environments, promotes
The diffusion of PrCu alloy, strengthens the isolation of the magnetic between crystal grain and improves the coercivity of magnet, and Pr replaces part Sm and improves simultaneously
The remanent magnetism of magnet.
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| CN106935350A (en) * | 2017-03-13 | 2017-07-07 | 中南大学 | A kind of anisotropy SmCo5Type rare earth permanent-magnetic material and preparation method |
| CN108962523A (en) * | 2018-08-14 | 2018-12-07 | 徐靖才 | A kind of preparation method for the SmCo base nanocomposite permanent magnets adulterating SmCu alloy |
| CN110895984A (en) * | 2018-09-12 | 2020-03-20 | 河南科技大学 | Strong texture SmCo5Base nano composite permanent magnetic material and its preparation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106935350A (en) * | 2017-03-13 | 2017-07-07 | 中南大学 | A kind of anisotropy SmCo5Type rare earth permanent-magnetic material and preparation method |
| CN108962523A (en) * | 2018-08-14 | 2018-12-07 | 徐靖才 | A kind of preparation method for the SmCo base nanocomposite permanent magnets adulterating SmCu alloy |
| CN108962523B (en) * | 2018-08-14 | 2020-05-12 | 浙江中科磁业股份有限公司 | Preparation method of SmCu alloy-doped samarium-cobalt-based nano composite permanent magnet |
| CN110895984A (en) * | 2018-09-12 | 2020-03-20 | 河南科技大学 | Strong texture SmCo5Base nano composite permanent magnetic material and its preparation method |
| CN110895984B (en) * | 2018-09-12 | 2021-06-04 | 河南科技大学 | Strong texture SmCo5Base nano composite permanent magnetic material and its preparation method |
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