CN106653271A - Preparation method of high-resistivity rare-earth permanent magnet - Google Patents
Preparation method of high-resistivity rare-earth permanent magnet Download PDFInfo
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- CN106653271A CN106653271A CN201710003772.4A CN201710003772A CN106653271A CN 106653271 A CN106653271 A CN 106653271A CN 201710003772 A CN201710003772 A CN 201710003772A CN 106653271 A CN106653271 A CN 106653271A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 14
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 11
- 230000032683 aging Effects 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 28
- 238000011282 treatment Methods 0.000 claims abstract description 22
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 18
- 229910052802 copper Inorganic materials 0.000 claims abstract description 18
- 239000000203 mixture Substances 0.000 claims abstract description 13
- 239000010453 quartz Substances 0.000 claims abstract description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 4
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 3
- 229910052733 gallium Inorganic materials 0.000 claims abstract description 3
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 3
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 3
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 3
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 3
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 3
- 230000005291 magnetic effect Effects 0.000 claims description 84
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 27
- 238000005245 sintering Methods 0.000 claims description 23
- 229910052796 boron Inorganic materials 0.000 claims description 16
- 229910052742 iron Inorganic materials 0.000 claims description 16
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 12
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 12
- 239000012535 impurity Substances 0.000 claims description 10
- 238000013329 compounding Methods 0.000 claims description 6
- 229910000906 Bronze Inorganic materials 0.000 claims description 3
- 239000010974 bronze Substances 0.000 claims description 3
- KUNSUQLRTQLHQQ-UHFFFAOYSA-N copper tin Chemical compound [Cu].[Sn] KUNSUQLRTQLHQQ-UHFFFAOYSA-N 0.000 claims description 3
- 235000012241 calcium silicate Nutrition 0.000 claims description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 abstract description 10
- 150000001875 compounds Chemical class 0.000 abstract description 4
- 238000009413 insulation Methods 0.000 abstract description 4
- 230000005672 electromagnetic field Effects 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 3
- 239000006247 magnetic powder Substances 0.000 abstract description 3
- 229910052918 calcium silicate Inorganic materials 0.000 abstract 1
- 239000000378 calcium silicate Substances 0.000 abstract 1
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 32
- 239000000956 alloy Substances 0.000 description 26
- 229910045601 alloy Inorganic materials 0.000 description 26
- 229910052779 Neodymium Inorganic materials 0.000 description 15
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 14
- 239000002245 particle Substances 0.000 description 14
- 238000003801 milling Methods 0.000 description 12
- 229910052692 Dysprosium Inorganic materials 0.000 description 11
- 239000007789 gas Substances 0.000 description 9
- 239000000843 powder Substances 0.000 description 9
- 235000012239 silicon dioxide Nutrition 0.000 description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 8
- 239000001257 hydrogen Substances 0.000 description 8
- 229910052739 hydrogen Inorganic materials 0.000 description 8
- JHXCINJSAAFBDH-UHFFFAOYSA-N [Ca].O[Si](O)(O)O Chemical compound [Ca].O[Si](O)(O)O JHXCINJSAAFBDH-UHFFFAOYSA-N 0.000 description 7
- 229910052786 argon Inorganic materials 0.000 description 7
- 229910001172 neodymium magnet Inorganic materials 0.000 description 7
- 238000012545 processing Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 229910000831 Steel Inorganic materials 0.000 description 4
- 238000007731 hot pressing Methods 0.000 description 4
- 239000011810 insulating material Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000010959 steel Substances 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 229910052777 Praseodymium Inorganic materials 0.000 description 2
- 229910052771 Terbium Inorganic materials 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 230000005389 magnetism Effects 0.000 description 2
- 238000006396 nitration reaction Methods 0.000 description 2
- 229910052755 nonmetal Inorganic materials 0.000 description 2
- 239000004952 Polyamide Substances 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 238000002679 ablation Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910001634 calcium fluoride Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000002508 compound effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 150000003949 imides Chemical class 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 230000003137 locomotive effect Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 150000002843 nonmetals Chemical class 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000006069 physical mixture Substances 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000007738 vacuum evaporation Methods 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
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
- H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
- H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
- H01F1/0576—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together pressed, e.g. hot working
-
- 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
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
- H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
- H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
- H01F1/0577—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together sintered
-
- 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
- H01F41/0266—Moulding; Pressing
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Hard Magnetic Materials (AREA)
Abstract
The invention relates to a preparation method of a high-resistivity rare-earth permanent magnet. The method comprises the following steps that 1, an insulation sheet is added into R1-M-B magnetic powder, wherein R1 is one of or a compound of multiple rare earth elements, M is one of or a compound of multiple of Ti, V, Cr, Mn, Co, Ga, Cu, Si, Al, Zr, Nb, W and Mo, and the insulation sheet is one of or a compound of multiple of quartz, zirconia, aluminum oxide and calcium silicate; 2, a mold is filled with a mixture, obtained in the first step, of the magnetic powder and the insulation sheet, and orientation pressing is conducted; 3, a blank obtained in the second step is sintered, aging treatment is conducted, and the rare-earth permanent magnet is obtained. According to the permanent magnet obtained through the technology, on the premise that the integrity of the appearance of the magnet is guaranteed, and the problem that the electrical resistivity cannot be increased greatly through other methods is solved; the magnet is applied to the high frequency alternating electromagnetic field environment and a motor operating at a high speed, and eddy current loss in the motor can be greatly reduced.
Description
Technical field
The present invention relates to a kind of preparation method of magnet, more particularly to a kind of preparation method of rare-earth permanent magnet, belong to magnetic
The fabricating technology field of body.
Background technology
NdFeB material since the advent of the world, be widely used in the features such as due to its high energy product, high-coercive force computer,
The numerous areas such as communication, Aero-Space, motor, become manufacture efficiency height, small volume, the ideal of the magnetic functional material of light weight
Many applications are produced revolutionary impact by material.But due to the self-characteristic of NdFeB material, its resistivity is relatively low,
In the electromagnetic field environment and the motor that runs up of high-frequency alternating, Nd-Fe-B magnet steel inside can produce obvious eddy-current loss,
So as to cause magnet temperature to raise, energy loss, magnet performance is caused to decline, cause magnet steel ablation etc. various bad.Therefore drop
Application of the low eddy-current loss for magnet in fields such as high frequency, exchange, high-speed electric expreess locomotives is very crucial.
Reducing the approach of permanent magnet motor eddy-current loss mainly has two：One is by designing rotor.Such as split magnetic
Body unit reduces eddy-current loss, but cutting magnet will greatly improve manufacturing cost；Two is that the resistivity for improving permanent magnet is reduced
Eddy-current loss.This is because the eddy-current loss of PM rotor is with resistivity inversely.Therefore, the resistance of permanent magnet is improved
Rate becomes the emphasis of research reducing eddy-current loss.
Chinese patent CN1185009 is described and is added the preparation that the method for binding agent and insulating compound is come in rare-earth permanent magnet
The method of bonded permanent magnet, by binding agent, insulating compound effect improving the electrical insulating property of magnet.
Japanese Patent Laid-Open 8-279407 describes a kind of preparation method of many magnetic pole electric insulation R-Fe-B permanent magnets.Should
Magnet is sintered magnet, and it, using the method for vacuum evaporation, in magnet surface 2-10 μm of polyamides of last layer is plated after sinter molding
Imide resin film is improving magnet insulating properties.
Chinese patent CN104425092A is described and is contacted the non-metal sources such as Nd-Fe-B magnet steel body and C/N/B/Si/S,
Then process at high temperature.Non-metal source is set to discharge the non-metallic atom of activity and diffuse in Nd-Fe-B magnet steel body,
Improve magnet microscopic structure, improve magnet resistive rate.
Chinese patent CN104959618A describes the method by the nitridation of NdFeB magnetics to improve resistivity.The patent is led to
Cross and magnetic is passed through into ammonia under the conditions of 300-400 DEG C is processed, make magnetic surface form nitration case, using nitration case every
Effect absolutely improves resistivity.
Chinese patent ZL201310314166 is described by using Ca (NO3)2Solution and KF solution are in NdFeB powder tables
Face carries out Direct precipitation chemosynthesis reaction, then will be with CaF2The powder of clad is by orientation, hot pressing and thermal deformation system
The method of standby high resistivity magnet.
Above method is mostly the resistivity by improving the insulating properties of magnetic powder particle to improve magnet, but improves resistivity
Limitation and some processes operation difficulty is larger, is difficult to realize steady production.
The content of the invention
A kind of deficiency that the present invention exists for the process aspect of raising permanent magnetism bulk resistor in prior art, there is provided high resistance
The preparation method of the rare-earth permanent magnet of rate.
The technical scheme that the present invention solves above-mentioned technical problem is as follows：
A kind of preparation method of the rare-earth permanent magnet of high resistivity, it is characterised in that comprise the steps：
1) to R1Add insulating trip in-M-B magnetics, wherein, R1The compounding of one or more in for rare earth element, M is
The compounding of one or more in Ti, V, Cr, Mn, Co, Ga, Cu, Si, Al, Zr, Nb, W, Mo, the insulating trip is quartz, oxygen
Change the compounding of one or more in zirconium, aluminum oxide, calcium silicates；
2) to step 1) obtained by the mixture of magnetic and insulating trip be filled in mould, carry out orientation compacting；
3) by step 2) obtained by blank be sintered, after carry out Ageing Treatment, obtain rare-earth permanent magnet.
Further, step 1) described in R1The weight fraction of each component is as follows in-M-B magnetics：R128.6～33wt%,
0.92～1.2wt% of B, M≤2.3wt%, balance of iron and impurity.
Further, step 1) described in R1- M-B magnetics are pairing bronze, and pairing bronze designated herein refers to two kinds
R1The physical mixture of-M-B magnetics.
Further, step 1) in add insulating trip Hou Du≤0.1mm.
Further, step 1) in insulating trip weight for magnetic gross weight 0.01～5wt%.
Further, step 2) in orientation compacting process conditions be：Room temperature, magnetic field intensity 2T.
Further, step 3) described in be sintered to hot pressed sintering.
Further, step 3) described in sinter temperature be 910～1090 DEG C, sintering time be 1.5～6h.
Further, step 3) in the temperature of Ageing Treatment be 450～600 DEG C, time of Ageing Treatment is 2～5h.
The invention has the beneficial effects as follows：
1) permanent magnet obtained by present invention process overcomes additive method on the premise of magnet complete appearance is ensured
The problem of resistivity can not be greatly improved；
2) magnet applications can make the vortex in motor in the electromagnetic field environment and the motor that runs up of high-frequency alternating
Loss is substantially reduced, and improves electric efficiency；
3) integrated artistic is simple, and raw material is cheap and easy to get, is capable of achieving batch steady production.
Specific embodiment
The principle and feature of the present invention are described below in conjunction with example, example is served only for explaining the present invention, and
It is non-for limiting the scope of the present invention.
Embodiment 1：
1) melted in argon gas atmosphere medium-high frequency using Nd, Tb, Co, Al, Fe, Cu and ferro-boron of at least 99% purity by weight,
And will make alloy in melt cast to chilling roller, the mass percent of alloy be 30%Nd, 0.5%Tb, 0.8%Co, 0.2%
Al, 0.2%Cu, 1%B, the rest is iron and inevitable impurity；The alloy carries out hydrogen is quick-fried, airflow milling grinding obtains average
Granularity is 3.4 μm of magnetic；
2) mix after the quartz plate for adding 1.5wt% in magnetic, wherein the average-size of quartz plate is 0.36-0.29-
0.08mm, thickness is 0.08mm；
3) mixture is filled in mould, in the environment of normal temperature and magnetic field intensity are for the orientation field of 2T orientation pressure is carried out
System；
4) and then by pressed compact it is put in vacuum sintering furnace, at 1090 DEG C of temperature 5h is sintered.After terminating, then carry out
510 DEG C of Ageing Treatments, aging time is 4h, obtains the magnet that size is 50-35-28mm.D10-10mm samples are processed from magnet
Post tests magnetic property, processes 2-2-28mm square column test resistance rates.
Comparative example 1：
By formula same as Example 1, same particle sizes magnetic without quartz plate, be in normal temperature and magnetic field intensity directly
Orientation compacting is carried out in the orientation field of 2T, in 1090 DEG C of sintering 5h of temperature, 510 DEG C of Ageing Treatments 4h of temperature obtain same size
The magnet of 50-35-28mm.From on magnet along magnetizing direction processing D10-10mm samples post test magnetic property, 2-2-28mm side is processed
Post test resistance rate.
Embodiment 2：
1) melted in argon gas atmosphere medium-high frequency using Nd, Dy, Co, Al, Fe, Cu and ferro-boron of at least 99% purity by weight,
And will make alloy in melt cast to chilling roller, the mass percent of alloy be 31.5%Nd, 0.5%Dy, 1.0%Co,
0.5%Al, 0.2%Cu, 0.92%B, iron and inevitable impurity are the rest is, the alloy carries out hydrogen is quick-fried, airflow milling is obtained
Particle mean size is 3.0 μm of magnetic；
2) add the zirconium oxide piece of 5wt% in airflow milling magnetic and mix, the average-size of wherein zirconium oxide piece is
0.23-0.20-0.05mm, thickness is 0.05mm；
3) mixture of the two is filled in mould, is carried out in the environment of normal temperature and magnetic field intensity are for the orientation field of 2T
Orientation compacting；
4) and then by pressed compact it is put in vacuum sintering furnace, at 1060 DEG C of temperature 4.5h is sintered.After terminating, then carry out
490 DEG C of Ageing Treatments, aging time is 2h, obtains the magnet that size is 14-55-50mm.Process along magnetizing direction from magnet
D10-10mm samples post tests magnetic property, processes 2-2-50mm square column test resistance rates.
Comparative example 2a：
The Zirconium oxide powder of 5wt% will be added in formula same as Example 2, the magnetic of same particle sizes and mixed.Directly
Orientation compacting is carried out in normal temperature and magnetic field intensity are for the orientation field of 2T, in 1060 DEG C of sintering 4.5h of temperature, 490 DEG C of timeliness of temperature
2h is processed, the magnet of same size 14-55-50mm is obtained.Along magnetizing direction processing D10-10mm samples post test magnetic from magnet
Performance, processes 2-2-50mm square column test resistance rates.
Comparative example 2b：
By in formula same as Example 2, the magnetic of same particle sizes without zirconium oxide, directly in normal temperature and magnetic field intensity
To carry out orientation compacting in the orientation field of 2T, in 1060 DEG C of sintering 4.5h of temperature, 490 DEG C of Ageing Treatments 5h of temperature obtain identical
The magnet of size 14-55-50mm.D10-10mm samples post test magnetic property, processing 2-2-50mm square column tests are processed from magnet
Resistivity.
Embodiment 3：
1) melted in argon gas atmosphere medium-high frequency using Nd, Dy, Co, Al, Fe, Cu and ferro-boron of at least 99% purity by weight,
And will make alloy in melt cast to chilling roller, the mass percent of alloy be 31.2%Nd, 1.8%Dy, 1.5%Co,
0.4%Al, 0.20%Cu, 1.2%B, iron and inevitable impurity are the rest is, the alloy carries out hydrogen is quick-fried, airflow milling is obtained
Particle mean size is 3.1 μm of magnetic；
2) the silicic acid calcium tablet of 3.5wt% is added in airflow milling magnetic, wherein silicic acid calcium tablet average-size is 0.28-
0.21-0.06mm, thickness is 0.06mm；
3) mixture of the two is filled in mould, is carried out in the environment of normal temperature and magnetic field intensity are for the orientation field of 2T
Orientation compacting；
4) and then by pressed compact it is put in vacuum sintering furnace, at 1065 DEG C of temperature 5.0h is sintered.After terminating, then carry out
450 DEG C of Ageing Treatments, aging time is 4.5h, obtains the magnet that size is 16-44-35mm.Add along magnetizing direction from magnet
Work D10-10mm sample post tests magnetic property, processes 2-2-35mm square column test resistance rates.
Comparative example 3:
By in formula same as Example 3, the magnetic of same particle sizes without silicic acid calcium tablet, it is directly strong in normal temperature and magnetic field
Spending in the orientation field for 2T carries out orientation compacting, and in 1065 DEG C of sintering 5.0h of temperature, 450 DEG C of Ageing Treatments 4.5h of temperature are obtained
The magnet of same size 16-44-35mm.From on magnet along magnetizing direction processing D10-10mm samples post test magnetic property, 2- is processed
2-35mm square column test resistance rates.
Embodiment 4：
1) melted in argon gas atmosphere medium-high frequency using Nd, Co, Al, Fe, Cu and ferro-boron of at least 99% purity by weight, and will
Melt cast makes alloy on chilling roller, the mass percent of alloy be 31.5%Nd, 1.5%Co, 0.3%Al, 0.20%
Cu, 0.98%B, the rest is iron and inevitable impurity；The alloy is carried out into that hydrogen is quick-fried, to obtain particle mean size be 2.7 μ to airflow milling
The magnetic of m；
2) quartz plate of 2.5wt% is added in airflow milling magnetic；Wherein the average-size of quartz plate is 0.25-0.13-
0.03mm, thickness is 0.03mm；
3) mixture of the two is filled in mould, is carried out in the environment of normal temperature and magnetic field intensity are for the orientation field of 2T
Orientation compacting；
4) and then by pressed compact it is put in vacuum sintering furnace, at 1040 DEG C of temperature 6.0h is sintered；After terminating, then carry out
590 DEG C of Ageing Treatments, aging time is 4.0h, obtains the magnet that size is 40-22-30mm.Add along magnetizing direction from magnet
Work D10-10mm sample post tests magnetic property, processes 2-2-30mm square column test resistance rates.
Comparative example 4a：
The scale of formula same as Example 4 is ground to form into the magnetic that granularity is respectively 2.7 μm.In this magnetic without
Quartz plate, directly carries out orientation compacting in normal temperature and magnetic field intensity are 2T orientations field, sinters 6.0h at 1040 DEG C of temperature, temperature
Spend for 590 DEG C of Ageing Treatments 4.0h, obtain the magnet of same size 40-22-30mm.D10- is processed from magnet along magnetizing direction
10mm samples post tests magnetic property, processes 2-2-35mm square column test resistance rates.
Comparative example 4b:
The scale of formula same as Example 4 is ground to form into the magnetic that granularity is respectively 3.2 μm.In this magnetic without
Quartz plate, directly carries out orientation compacting in normal temperature and magnetic field intensity are 2T orientations field, sinters 6h at 1040 DEG C of temperature respectively,
Temperature is 590 DEG C of Ageing Treatments 4.0h, obtains the magnet of same size 40-22-30mm.Process along magnetizing direction from magnet
D10-10mm samples post tests magnetic property, processes 2-2-35mm square column test resistance rates.
Embodiment 5：
1) Nd, Pr, Dy, Co, Al, Cu, the Fe and ferro-boron using at least 99% purity by weight is molten in argon gas atmosphere medium-high frequency
Change, and alloy will be made in melt cast to chilling roller, the mass percent of alloy be 24.0%Nd, 6.0%Pr, 0.8%Dy,
1.5%Co, 0.6%Al, 0.20%Cu, 1.00%B the rest is iron and inevitable impurity.The alloy carries out hydrogen is quick-fried, gas
Stream mill obtains the magnetic that particle mean size is 3.0 μm；
2) zirconium oxide of 0.01wt% is added in airflow milling magnetic；Wherein zirconic average-size is 0.10-0.07-
0.02mm, thickness is 0.02mm；
3) mixture of the two is filled in mould, is carried out in the environment of normal temperature and magnetic field intensity are for the orientation field of 2T
Orientation compacting；
4) and then by pressed compact it is put in vacuum hotpressing stove, at 910 DEG C of temperature 1.5h is sintered.After the completion of sintering, system is opened
Beginning applies pressure carries out hot pressed sintering, and hot pressing temperature is 920 DEG C, and pressure is 110MPa, and the time is 15min.Hot pressed sintering is completed
Afterwards, then 530 DEG C of Ageing Treatments are carried out, aging time is 4.0h, obtains the magnet E1 that size is 20-42-33mm.From magnet E1
Along magnetizing direction processing D10-10mm samples post test magnetic property, 2-2-33mm square column test resistance rates are processed.
Comparative example 5：
By in same recipe, the magnetic of same particle sizes without zirconium oxide piece, directly in normal temperature and magnetic field intensity for 2T's
Orientation carries out orientation compacting in field.Then pressed compact is put in vacuum hotpressing stove, in 910 DEG C of sintering 1.5h of temperature.Then in temperature
Spend for 920 DEG C, pressure is hot pressed sintering 15min under 110MPa.Carry out 530 DEG C of Ageing Treatments 4h after the completion of hot pressed sintering again, obtain
To the magnet of same size 20-42-33mm.D10-10mm samples post test magnetic property is processed from magnet, 2-2-33mm side is processed
Post test resistance rate.
Embodiment 6：
1) melted in argon gas atmosphere medium-high frequency using Nd, Dy, Co, Al, Fe, Cu and ferro-boron of at least 99% purity by weight,
And will make alloy in melt cast to chilling roller, the mass percent of alloy be 27.3%Nd, 1.3%Dy, 1.8%Co,
0.3%Al, 0.2%Cu, 1.00%B, the rest is iron and inevitable impurity.The alloy carries out hydrogen is quick-fried, airflow milling is obtained
Particle mean size is 3.0 μm of magnetic；
2) zirconium oxide and alumina mixture of 1.0wt% are added in airflow milling magnetic, the ratio of the two is 4:1.Its
Middle zirconium oxide, the average-size of alumina wafer are 0.25-0.20-0.06, and thickness direction is 0.1mm；
3) mixture of three is filled in mould, is carried out in the environment of normal temperature and magnetic field intensity are for the orientation field of 2T
Orientation compacting；
4) and then by pressed compact it is put in vacuum sintering furnace, at 1060 DEG C of temperature 4.5h is sintered.After terminating, then carry out
600 DEG C of Ageing Treatments, aging time is 5h, obtains the magnet that size is 14-55-50mm.Process along magnetizing direction from magnet
D10-10mm samples post tests magnetic property, processes 2-2-50mm square column test resistance rates.
Comparative example 6：
By with the same recipe of comparative example 6, the magnetic of same particle sizes in without zirconium oxide and alumina wafer, directly in normal temperature
With magnetic field intensity to carry out orientation compacting in the orientation field of 2T, in 1060 DEG C of sintering 4.5h of temperature, 600 DEG C of Ageing Treatments of temperature
5h, obtains the magnet of same size 14-55-50mm.D10-10mm samples post test magnetic property is processed from magnet, 2-2- is processed
50mm square column test resistance rates.
Embodiment 7：
1) melted in argon gas atmosphere medium-high frequency using Nd, Dy, Co, Al, Fe, Cu and ferro-boron of at least 99% purity by weight,
And alloy A, alloy B will be made in melt cast to chilling roller.The mass percent of alloy A be 27.5%Nd, 2.9%Dy,
1.0%Co, 0.2%Al, 0.15%Cu, 0.98%B, iron and inevitable impurity are the rest is, the alloy carries out hydrogen is quick-fried, gas
Stream mill obtains the magnetic that particle mean size is 3.2 μm.The mass percent of alloy B be 18.5%Nd, 14.0%Dy, 3.0%Co,
0.3%Al, 0.25%Cu, 0.96%B, iron and inevitable impurity are the rest is, the alloy carries out hydrogen is quick-fried, airflow milling is obtained
Particle mean size is 3.0 μm of magnetic.It is proportionally 4 by alloy A magnetics and alloy B magnetics:1 mixing.
2) the silicic acid calcium tablet of 3.0wt% is added in airflow milling mixes magnetic, wherein silicic acid calcium tablet average-size is 0.21-
0.21-0.05mm, thickness is 0.03mm；
3) mixture of the two is filled in mould, is carried out in the environment of normal temperature and magnetic field intensity are for the orientation field of 2T
Orientation compacting；
4) and then by pressed compact it is put in vacuum sintering furnace, at 1075 DEG C of temperature 5.0h is sintered.After terminating, then carry out
520 DEG C of Ageing Treatments, aging time is 4.5h, obtains the magnet that size is 14-42-31mm.Add along magnetizing direction from magnet
Work D10-10mm sample post tests magnetic property, processes 2-2-31mm square column test resistance rates.
Comparative example 7:
Without silicic acid calcium tablet in the magnetic that formula same as Example 7, same ratio are mixed, directly in normal temperature and magnetic
Field intensity to carry out orientation compacting in the orientation field of 2T, in 1075 DEG C of temperature sintering 5.0h, 520 DEG C of Ageing Treatments 4.5h of temperature,
Obtain the magnet of same size 14-42-31mm.From on magnet along magnetizing direction processing D10-10mm samples post test magnetic property, plus
Work 2-2-31mm square column test resistance rate.
Table 1：The magnetic property and resistivity measurement data of embodiment 1～7 and the gained magnet of comparative example 1～7
From the above data, it can be seen that after addition zirconium oxide piece, quartz plate, the insulating materials such as silicic acid calcium tablet, with without
The magnet of insulating materials is compared, and its remanent magnetism is reduced, and coercivity is basically unchanged, and resistivity is largely increased, in addition, by embodiment
2 understand compared with the experimental data of comparative example 2a, and the magnet resistive rate for adding zirconium oxide piece will be far above addition zirconia powder
Magnet resistive rate.This is because, although zirconia powder can completely cut off magnetic, but the isolation effect of zirconia powder is limited, magnetic
The conduction that can all cause to be vortexed that contacts with each other of any point between powder, so as to reduce the insulating effect of zirconia powder, in the same manner, Ren Heqi
The insulating materials of his form is added in the middle of magnet, does not all have same sheet insulating materials identical technique effect；From comparative example
4a understands compared with the experimental data of comparative example 4b, the two magnet Br quite,
Hcj is improved, resistivity is improved.This is because granularity of magnet powder is thinner, Grain-Boundary Phase is more, the obstruction of crystal boundary relative eddy
It is bigger.
The foregoing is only presently preferred embodiments of the present invention, not to limit the present invention, all spirit in the present invention and
Within principle, any modification, equivalent substitution and improvements made etc. should be included within the scope of the present invention.
Claims (10)
1. a kind of preparation method of the rare-earth permanent magnet of high resistivity, it is characterised in that comprise the steps：
1) to R1Add insulating trip in-M-B magnetics, wherein, R1The compounding of one or more in for rare earth element, M be Ti, V,
The compounding of one or more in Cr, Mn, Co, Ga, Cu, Si, Al, Zr, Nb, W, Mo, the insulating trip be quartz, zirconium oxide,
The compounding of one or more in aluminum oxide, calcium silicates；
2) by step 1) obtained by the mixture of magnetic and insulating trip be filled in mould, carry out orientation compacting；
3) by step 2) obtained by blank be sintered, after carry out Ageing Treatment, obtain rare-earth permanent magnet.
2. preparation method according to claim 1, it is characterised in that step 1) described in R1Each component in-M-B magnetics
Weight fraction it is as follows：R10.92～1.2wt% of 28.6～33wt%, B, M≤2.3wt%, balance of iron and impurity.
3. preparation method according to claim 1 and 2, it is characterised in that step 1) described in R1- M-B magnetics are pairing
Bronze.
4. preparation method according to claim 1 and 2, it is characterised in that step 1) in add the Hou Du of insulating trip≤
0.1mm。
5. preparation method according to claim 1 and 2, it is characterised in that step 1) in the weight of insulating trip be that magnetic is total
0.01～5wt% of weight.
6. preparation method according to claim 1 and 2, it is characterised in that step 1) in the weight of insulating trip be that magnetic is total
0.5～3wt% of weight.
7. preparation method according to claim 1, it is characterised in that step 2) in the process conditions of orientation compacting be：Room
Temperature, magnetic field intensity 2T.
8. preparation method according to claim 1, it is characterised in that step 3) described in be sintered to hot pressed sintering.
9. the preparation method according to claim 1 or 8, it is characterised in that step 3) described in sintering temperature be 910～
1090 DEG C, sintering time is 1.5～6h.
10. preparation method according to claim 1, it is characterised in that step 3) in Ageing Treatment temperature be 450～
600 DEG C, the time of Ageing Treatment is 2～5h.
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| CN112768170A (en) * | 2020-12-30 | 2021-05-07 | 烟台正海磁性材料股份有限公司 | Rare earth permanent magnet and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5858124A (en) * | 1995-10-30 | 1999-01-12 | Hitachi Metals, Ltd. | Rare earth magnet of high electrical resistance and production method thereof |
| CN101872668A (en) * | 2009-04-23 | 2010-10-27 | 北京中科三环高技术股份有限公司 | Sintered NdFeB rear-earth permanent magnet with fine magnetization characteristic and manufacturing method thereof |
| CN104167271A (en) * | 2014-07-25 | 2014-11-26 | 安徽大地熊新材料股份有限公司 | High-resistivity rare earth iron series R-Fe-B magnet and manufacturing method thereof |
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2017
- 2017-01-04 CN CN201710003772.4A patent/CN106653271B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5858124A (en) * | 1995-10-30 | 1999-01-12 | Hitachi Metals, Ltd. | Rare earth magnet of high electrical resistance and production method thereof |
| CN101872668A (en) * | 2009-04-23 | 2010-10-27 | 北京中科三环高技术股份有限公司 | Sintered NdFeB rear-earth permanent magnet with fine magnetization characteristic and manufacturing method thereof |
| CN104167271A (en) * | 2014-07-25 | 2014-11-26 | 安徽大地熊新材料股份有限公司 | High-resistivity rare earth iron series R-Fe-B magnet and manufacturing method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112768170A (en) * | 2020-12-30 | 2021-05-07 | 烟台正海磁性材料股份有限公司 | Rare earth permanent magnet and preparation method thereof |
| CN112768170B (en) * | 2020-12-30 | 2022-11-01 | 烟台正海磁性材料股份有限公司 | Rare earth permanent magnet and preparation method thereof |
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