CN106653271B - A kind of preparation method of the rare-earth permanent magnet of high resistivity - Google Patents
A kind of preparation method of the rare-earth permanent magnet of high resistivity Download PDFInfo
- Publication number
- CN106653271B CN106653271B CN201710003772.4A CN201710003772A CN106653271B CN 106653271 B CN106653271 B CN 106653271B CN 201710003772 A CN201710003772 A CN 201710003772A CN 106653271 B CN106653271 B CN 106653271B
- Authority
- CN
- China
- Prior art keywords
- magnetic powder
- preparation
- magnet
- insulating trip
- rare
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 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
- 239000006247 magnetic powder Substances 0.000 claims abstract description 48
- 230000032683 aging Effects 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 29
- 238000011282 treatment Methods 0.000 claims abstract description 22
- 230000008569 process Effects 0.000 claims abstract description 20
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 18
- 229910052802 copper Inorganic materials 0.000 claims abstract description 18
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910001928 zirconium oxide Inorganic materials 0.000 claims abstract description 15
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 12
- 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
- 229910052710 silicon 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
- 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
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 3
- 238000005245 sintering Methods 0.000 claims description 30
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 27
- 229910052796 boron Inorganic materials 0.000 claims description 17
- 229910052742 iron Inorganic materials 0.000 claims description 17
- 239000012535 impurity Substances 0.000 claims description 10
- 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
- 239000011575 calcium Substances 0.000 claims description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims 1
- 229910052791 calcium Inorganic materials 0.000 claims 1
- 239000010703 silicon Substances 0.000 claims 1
- 238000013329 compounding Methods 0.000 abstract description 6
- 230000005672 electromagnetic field Effects 0.000 abstract description 3
- 235000012241 calcium silicate Nutrition 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 27
- 239000000956 alloy Substances 0.000 description 26
- 229910045601 alloy Inorganic materials 0.000 description 26
- 229910052779 Neodymium Inorganic materials 0.000 description 15
- 239000002245 particle Substances 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 14
- 238000003801 milling Methods 0.000 description 12
- 229910052692 Dysprosium Inorganic materials 0.000 description 11
- 235000012239 silicon dioxide Nutrition 0.000 description 9
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 8
- 239000001257 hydrogen Substances 0.000 description 8
- 229910052739 hydrogen Inorganic materials 0.000 description 8
- 239000000843 powder Substances 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
- 239000012300 argon atmosphere Substances 0.000 description 7
- 229910001172 neodymium magnet Inorganic materials 0.000 description 7
- 238000012545 processing Methods 0.000 description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- 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
- 150000002431 hydrogen Chemical class 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
- 230000008859 change Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000002955 isolation Methods 0.000 description 2
- 230000005389 magnetism Effects 0.000 description 2
- 238000002156 mixing Methods 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
- 238000002679 ablation Methods 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 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
- 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
- 238000013461 design Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 150000003949 imides Chemical class 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000005259 measurement 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
- 239000005022 packaging material Substances 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
- 230000009467 reduction Effects 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
- 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
Landscapes
- 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 present invention relates to a kind of preparation method of the rare-earth permanent magnet of high resistivity, include the following steps: 1) to R1Insulating trip is added in-M-B magnetic powder, wherein R1For one of rare earth element or a variety of compoundings, M is one of Ti, V, Cr, Mn, Co, Ga, Cu, Si, Al, Zr, Nb, W, Mo or a variety of compoundings, and the insulating trip is one of quartz, zirconium oxide, aluminium oxide, calcium silicates or a variety of compoundings；The mixture of the resulting magnetic powder of step 1) and insulating trip is filled into mold, orientation compacting is carried out；The resulting blank of step 2) is sintered, ageing treatment is carried out afterwards, obtains rare-earth permanent magnet.Permanent magnet obtained by present invention process overcomes the problem of other methods cannot greatly improve resistivity under the premise of guaranteeing magnet complete appearance；Magnet applications can be such that the eddy current loss in motor substantially reduces into the electromagnetic field environment and the motor that runs at high speed of high-frequency alternating.
Description
Technical field
The present invention relates to a kind of preparation method of magnet more particularly to a kind of preparation methods of rare-earth permanent magnet, belong to magnetic
The fabricating technology field of body.
Background technique
NdFeB material since the advent of the world, due to the features such as its high energy product, high-coercive force be widely used in computer,
The numerous areas such as communication, aerospace, motor become the ideal of manufacture high, small in size, light weight the magnetic functional material of efficiency
Material generates revolutionary impact to many application fields.But due to the self-characteristic of NdFeB material, resistivity is lower,
In the electromagnetic field environment and the motor that runs at high speed of high-frequency alternating, apparent eddy-current loss can be generated inside Nd-Fe-B magnet steel,
So as to cause magnet temperature raising, cause that energy loss, magnet performance decline, to lead to magnet steel ablation etc. various bad.Therefore it drops
Application of the low eddy-current loss for magnet in fields such as high frequency, exchange, high-speed motors is very crucial.
There are two the approach of reduction permanent magnet motor eddy-current loss is main: first is that passing through design rotor.Such as divide magnetic
Body unit reduces eddy-current loss, but manufacturing cost will be greatly improved by cutting magnet；Second is that the resistivity for improving permanent magnet is reduced
Eddy-current loss.This is because the eddy-current loss of PM rotor and resistivity are inversely.Therefore, the resistance of permanent magnet is improved
Rate becomes the emphasis of research to reduce eddy-current loss.
Chinese patent CN1185009 describes the preparation that the method that binder and insulating compound are added in rare-earth permanent magnet is come
The method of bonded permanent magnet improves the electrical insulating property of magnet by the effect of binder, insulating compound.
Japanese Patent Laid-Open 8-279407 describes a kind of preparation method of more magnetic pole electrical isolation R-Fe-B permanent magnets.It should
Magnet is sintered magnet, and the method that vacuum evaporation is used after sinter molding plates one layer of 2-10 μm of polyamides in magnet surface
Imide resin film improves magnet insulation performance.
Chinese patent CN104425092A, which is described, contacts Nd-Fe-B magnet steel ontology with non-metal sources such as C/N/B/Si/S,
Then it handles at high temperature.So that non-metal source is released active non-metallic atom and diffuse into Nd-Fe-B magnet steel ontology,
Improve magnet microscopic structure, improves magnet resistive rate.
Chinese patent CN104959618A describes the method nitrogenized NdFeB magnetic powder to improve resistivity.The patent is logical
Cross and magnetic powder is passed through ammonia under the conditions of 300-400 DEG C handles, magnetic powder surface is made to form nitration case, using nitration case every
Effect improves resistivity absolutely.
Chinese patent ZL201310314166 is described by using Ca (NO3)2Solution and KF solution are in NdFeB powder table
Face carries out Direct precipitation chemosynthesis reaction, then will have CaF2The powder of clad passes through orientation, hot pressing and hot change shape
The method of standby high resistivity magnet.
Above method is mostly the resistivity of magnet to be improved by improving the insulating properties of magnetic powder particle, but improve resistivity
Limitation and some processes operation difficulty is larger, is not easy to realize steady production.
Summary of the invention
The present invention provides a kind of high resistance for deficiency existing for the process aspect for improving permanent magnetism bulk resistor in the prior art
The preparation method of the rare-earth permanent magnet of rate.
The technical scheme to solve the above technical problems is that
A kind of preparation method of the rare-earth permanent magnet of high resistivity, which comprises the steps of:
1) to R1Insulating trip is added in-Fe-M-B magnetic powder, wherein R1For one of rare earth element or a variety of compoundings, M
For one of Ti, V, Cr, Mn, Co, Ga, Cu, Si, Al, Zr, Nb, W, Mo or a variety of compoundings, the insulating trip be quartz,
One of zirconium oxide, aluminium oxide, calcium silicates or a variety of compoundings；
2) it is filled into mold to the mixture of the resulting magnetic powder of step 1) and insulating trip, carries out orientation compacting；
3) the resulting blank of step 2) is sintered, carries out ageing treatment afterwards, obtains rare-earth permanent magnet.
Further, R described in step 1)1The weight fraction of each component is as follows in-Fe-M-B magnetic powder: R128.6~
0.92~1.2wt% of 33wt%, B, M≤2.3wt%, surplus is iron and impurity.
Further, R described in step 1)1- Fe-M-B magnetic powder is pairing bronze, and pairing bronze designated herein refers to two
Kind R1The physical mixture of-Fe-M-B magnetic powder.
Further, Hou Du≤0.1mm of insulating trip is added in step 1).
Further, in step 1) insulating trip weight be magnetic powder total weight 0.01~5wt%.
Further, the process conditions that orientation is suppressed in step 2) are as follows: room temperature, magnetic field strength 2T.
Further, hot pressed sintering is sintered to described in step 3).
Further, the temperature of sintering described in step 3) be 910~1090 DEG C, sintering time be 1.5~
6h。
Further, the temperature of ageing treatment is 450~600 DEG C in step 3), and the time of ageing treatment is 2~5h.
The beneficial effects of the present invention are:
1) permanent magnet obtained by present invention process overcomes other methods under the premise of guaranteeing magnet complete appearance
The problem of resistivity cannot be greatly improved；
2) magnet applications can make the vortex in motor into the electromagnetic field environment and the motor that runs at high speed of high-frequency alternating
Loss substantially reduces, and improves electric efficiency；
3) integrated artistic is simple and easy, and raw material is cheap and easy to get, it can be achieved that batch steady production.
Specific embodiment
Principles and features of the present invention are described below in conjunction with example, the given examples are served only to explain the present invention, and
It is non-to be used to limit the scope of the invention.
Embodiment 1:
1) it is melted using at least Nd, Tb, Co, Al, Fe, Cu of 99% purity by weight and ferro-boron in argon atmosphere medium-high frequency,
And alloy will be made in melt cast to chilling roller, the mass percent of alloy is 30%Nd, 0.5%Tb, 0.8%Co, 0.2%
Al, 0.2%Cu, 1%B, iron and inevitable impurity be the rest is；By alloy progress hydrogen, quick-fried, airflow milling grinding is averaged
The magnetic powder that granularity is 3.4 μm；
2) it is mixed after adding the quartz plate of 1.5wt% into magnetic powder, wherein the average-size of quartz plate is 0.36-0.29-
0.08mm, with a thickness of 0.08mm；
3) mixture is filled into mold, carries out orientation pressure in the environment of room temperature and magnetic field strength are the orientation field of 2T
System；
4) then green compact is put into vacuum sintering furnace, is sintered 5h at 1090 DEG C of temperature.After sintering, then carry out
510 DEG C of ageing treatments, aging time 4h obtain the magnet having a size of 50-35-28mm.D10-10mm sample is processed from magnet
Column tests magnetic property, processes 2-2-28mm square column test resistance rate.Comparative example 1:
The magnetic powder of formula same as Example 1, same particle sizes is not added into quartz plate, is directly in room temperature and magnetic field strength
Orientation compacting is carried out in the orientation field of 2T, obtains identical size in 1090 DEG C of sintering 5h of temperature, 510 DEG C of ageing treatment 4h of temperature
The magnet of 50-35-28mm.Magnetic property is tested along magnetizing direction processing D10-10mm sample column from magnet, processes the side 2-2-28mm
Column test resistance rate.
Embodiment 2:
1) it is melted using at least Nd, Dy, Co, Al, Fe, Cu of 99% purity by weight and ferro-boron in argon atmosphere medium-high frequency,
And alloy will be made in melt cast to chilling roller, the mass percent of alloy is 31.5%Nd, 0.5%Dy, 1.0%Co,
0.5%Al, 0.2%Cu, 0.92%B, iron and inevitable impurity be the rest is, quick-fried, airflow milling obtains by alloy progress hydrogen
The magnetic powder that average particle size is 3.0 μm；
2) the zirconium oxide piece of 5wt% is added in airflow milling magnetic powder and is mixed, and wherein the average-size of zirconium oxide piece is
0.23-0.20-0.05mm, with a thickness of 0.05mm；
3) mixture of the two is filled into mold, is carried out in the environment of room temperature and magnetic field strength are the orientation field of 2T
Orientation compacting；
4) then green compact is put into vacuum sintering furnace, is sintered 4.5h at 1060 DEG C of temperature.After sintering, then carry out
490 DEG C of ageing treatments, aging time 2h obtain the magnet having a size of 14-55-50mm.It is processed from magnet along magnetizing direction
D10-10mm sample column tests magnetic property, processes 2-2-50mm square column test resistance rate.
Comparative example 2a:
By Zirconium oxide powder and the mixing same as Example 2 for being formulated, adding 5wt% in the magnetic powder of same particle sizes.Directly
Orientation compacting is carried out in the orientation field that room temperature and magnetic field strength are 2T, in 1060 DEG C of sintering 4.5h of temperature, 490 DEG C of timeliness of temperature
2h is handled, the magnet of identical size 14-55-50mm is obtained.Magnetic is tested along magnetizing direction processing D10-10mm sample column from magnet
Performance processes 2-2-50mm square column test resistance rate.
Comparative example 2b:
By it is same as Example 2 formula, same particle sizes magnetic powder in do not add zirconium oxide, directly in room temperature and magnetic field strength
To carry out orientation compacting in the orientation field of 2T, obtained identical in 1060 DEG C of sintering 4.5h of temperature, 490 DEG C of ageing treatment 5h of temperature
The magnet of size 14-55-50mm.D10-10mm sample column is processed from magnet tests magnetic property, processing 2-2-50mm square column test
Resistivity.
Embodiment 3:
1) it is melted using at least Nd, Dy, Co, Al, Fe, Cu of 99% purity by weight and ferro-boron in argon atmosphere medium-high frequency,
And alloy will be made in melt cast to chilling roller, the mass percent of alloy is 31.2%Nd, 1.8%Dy, 1.5%Co,
0.4%Al, 0.20%Cu, 1.2%B, iron and inevitable impurity be the rest is, quick-fried, airflow milling obtains by alloy progress hydrogen
The magnetic powder that average particle size is 3.1 μm；
2) the silicic acid calcium tablet of 3.5wt% is added in airflow milling magnetic powder, wherein silicic acid calcium tablet average-size is 0.28-
0.21-0.06mm, with a thickness of 0.06mm；
3) mixture of the two is filled into mold, is carried out in the environment of room temperature and magnetic field strength are the orientation field of 2T
Orientation compacting；
4) then green compact is put into vacuum sintering furnace, is sintered 5.0h at 1065 DEG C of temperature.After sintering, then carry out
450 DEG C of ageing treatments, aging time 4.5h obtain the magnet having a size of 16-44-35mm.Add from magnet along magnetizing direction
Work D10-10mm sample column tests magnetic property, processes 2-2-35mm square column test resistance rate.
Comparative example 3:
By it is same as Example 3 formula, same particle sizes magnetic powder in do not add silicic acid calcium tablet, it is directly strong in room temperature and magnetic field
Orientation compacting is carried out in the orientation field that degree is 2T, is obtained in 1065 DEG C of sintering 5.0h of temperature, 450 DEG C of ageing treatment 4.5h of temperature
The magnet of identical size 16-44-35mm.Magnetic property is tested along magnetizing direction processing D10-10mm sample column from magnet, processes 2-
2-35mm square column test resistance rate.
Embodiment 4:
1) it is melted using at least Nd, Co, Al, Fe, Cu of 99% purity by weight and ferro-boron in argon atmosphere medium-high frequency, and will
Alloy is made in melt cast to chilling roller, the mass percent of alloy is 31.5%Nd, 1.5%Co, 0.3%Al, 0.20%
Cu, 0.98%B, iron and inevitable impurity be the rest is；It is 2.7 μ that by alloy progress hydrogen, quick-fried, airflow milling, which obtains average particle size,
The magnetic powder of m；
2) quartz plate of 2.5wt% is added in airflow milling magnetic powder；Wherein the average-size of quartz plate is 0.25-0.13-
0.03mm, with a thickness of 0.03mm；
3) mixture of the two is filled into mold, is carried out in the environment of room temperature and magnetic field strength are the orientation field of 2T
Orientation compacting；
4) then green compact is put into vacuum sintering furnace, is sintered 6.0h at 1040 DEG C of temperature；After sintering, then carry out
590 DEG C of ageing treatments, aging time 4.0h obtain the magnet having a size of 40-22-30mm.Add from magnet along magnetizing direction
Work D10-10mm sample column tests magnetic property, processes 2-2-30mm square column test resistance rate.
Comparative example 4a:
The scale of formula same as Example 4 is ground into the magnetic powder that granularity is respectively 2.7 μm.It is not added in this magnetic powder
Quartz plate is directly to carry out orientation compacting in 2T orientation field in room temperature and magnetic field strength, is sintered 6.0h at 1040 DEG C of temperature, temperature
Degree is 590 DEG C of ageing treatment 4.0h, obtains the magnet of identical size 40-22-30mm.D10- is processed along magnetizing direction from magnet
10mm sample column tests magnetic property, processes 2-2-35mm square column test resistance rate.
Comparative example 4b:
The scale of formula same as Example 4 is ground into the magnetic powder that granularity is respectively 3.2 μm.It is not added in this magnetic powder
Quartz plate is directly to carry out orientation compacting in 2T orientation field in room temperature and magnetic field strength, is sintered 6h at 1040 DEG C of temperature respectively,
Temperature is 590 DEG C of ageing treatment 4.0h, obtains the magnet of identical size 40-22-30mm.It is processed from magnet along magnetizing direction
D10-10mm sample column tests magnetic property, processes 2-2-35mm square column test resistance rate.
Embodiment 5:
1) molten in argon atmosphere medium-high frequency using at least Nd, Pr, Dy, Co, Al, Cu, Fe of 99% purity by weight and ferro-boron
Change, and alloy will be made in melt cast to chilling roller, the mass percent of alloy is 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 quick-fried, gas by alloy progress hydrogen
Stream mill obtains the magnetic powder that average particle size is 3.0 μm；
2) zirconium oxide of 0.01wt% is added in airflow milling magnetic powder；Wherein the average-size of zirconium oxide is 0.10-0.07-
0.02mm, with a thickness of 0.02mm；
3) mixture of the two is filled into mold, is carried out in the environment of room temperature and magnetic field strength are the orientation field of 2T
Orientation compacting；
4) then green compact is put into vacuum hotpressing stove, is sintered 1.5h at 910 DEG C of temperature.After the completion of sintering, system is opened
Begin to apply pressure progress hot pressed sintering, hot pressing temperature is 920 DEG C, pressure 110MPa, time 15min.Hot pressed sintering is completed
Afterwards, then 530 DEG C of ageing treatments are carried out, aging time 4.0h obtains the magnet E1 having a size of 20-42-33mm.From magnet E1
Magnetic property is tested along magnetizing direction processing D10-10mm sample column, processes 2-2-33mm square column test resistance rate.
Comparative example 5:
By same recipe, same particle sizes magnetic powder in do not add zirconium oxide piece, be directly 2T's in room temperature and magnetic field strength
Orientation carries out orientation compacting in field.Then green compact is put into vacuum hotpressing stove, in 910 DEG C of sintering 1.5h of temperature.Then in temperature
Degree is 920 DEG C, and pressure is hot pressed sintering 15min under 110MPa.530 DEG C of ageing treatment 4h are carried out again after the completion of hot pressed sintering, are obtained
To the magnet of identical size 20-42-33mm.D10-10mm sample column is processed from magnet and tests magnetic property, processes the side 2-2-33mm
Column test resistance rate.
Embodiment 6:
1) it is melted using at least Nd, Dy, Co, Al, Fe, Cu of 99% purity by weight and ferro-boron in argon atmosphere medium-high frequency,
And alloy will be made in melt cast to chilling roller, the mass percent of alloy is 27.3%Nd, 1.3%Dy, 1.8%Co,
0.3%Al, 0.2%Cu, 1.00%B, iron and inevitable impurity be the rest is.By alloy progress hydrogen, quick-fried, airflow milling is obtained
The magnetic powder that average particle size is 3.0 μm；
2) zirconium oxide and alumina mixture of 1.0wt% are added in airflow milling magnetic powder, the ratio of the two is 4:1.Its
Middle zirconium oxide, alumina wafer average-size be 0.25-0.20-0.06, thickness direction 0.1mm；
3) mixture of three is filled into mold, is carried out in the environment of room temperature and magnetic field strength are the orientation field of 2T
Orientation compacting；
4) then green compact is put into vacuum sintering furnace, is sintered 4.5h at 1060 DEG C of temperature.After sintering, then carry out
600 DEG C of ageing treatments, aging time 5h obtain the magnet having a size of 14-55-50mm.It is processed from magnet along magnetizing direction
D10-10mm sample column tests magnetic property, processes 2-2-50mm square column test resistance rate.
Comparative example 6:
By with do not add zirconium oxide and alumina wafer in the magnetic powder of 6 same recipe of comparative example, same particle sizes, directly in room temperature
With magnetic field strength 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 identical size 14-55-50mm.D10-10mm sample column is processed from magnet and tests magnetic property, processes 2-2-
50mm square column test resistance rate.
Embodiment 7:
1) it is melted using at least Nd, Dy, Co, Al, Fe, Cu of 99% purity by weight and ferro-boron in argon atmosphere medium-high frequency,
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 be the rest is, the quick-fried, gas by alloy progress hydrogen
Stream mill obtains the magnetic powder that average particle 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 be the rest is, quick-fried, airflow milling obtains by alloy progress hydrogen
The magnetic powder that average particle size is 3.0 μm.It with alloy B magnetic powder is proportionally that 4:1 is mixed by alloy A magnetic powder.
2) the silicic acid calcium tablet of 3.0wt% is added in airflow milling mixing magnetic powder, wherein silicic acid calcium tablet average-size is 0.21-
0.21-0.05mm, with a thickness of 0.03mm；
3) mixture of the two is filled into mold, is carried out in the environment of room temperature and magnetic field strength are the orientation field of 2T
Orientation compacting；
4) then green compact is put into vacuum sintering furnace, is sintered 5.0h at 1075 DEG C of temperature.After sintering, then carry out
520 DEG C of ageing treatments, aging time 4.5h obtain the magnet having a size of 14-42-31mm.Add from magnet along magnetizing direction
Work D10-10mm sample column tests magnetic property, processes 2-2-31mm square column test resistance rate.
Comparative example 7:
By it is same as Example 7 formula, same ratio mix magnetic powder in do not add silicic acid calcium tablet, directly in room temperature and magnetic
Orientation compacting is carried out in the orientation field that field intensity is 2T, in temperature 1075 DEG C of sintering 5.0h, 520 DEG C of ageing treatment 4.5h of temperature,
Obtain the magnet of identical size 14-42-31mm.Magnetic property is tested along magnetizing direction processing D10-10mm sample column from magnet, is added
Work 2-2-31mm square column test resistance rate.
Table 1: the magnetic property and resistivity measurement data of 1~7 gained magnet of Examples 1 to 7 and comparative example
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, and do not add
The magnet of insulating materials is compared, and remanent magnetism reduces, and coercivity is basically unchanged, and resistivity is largely increased, in addition, by embodiment
2 compared with the experimental data of comparative example 2a it is found that addition zirconium oxide piece magnet resistive rate will much higher than addition zirconia powder
Magnet resistive rate.Although the isolation effect of zirconia powder is limited, magnetic this is because zirconia powder can completely cut off magnetic powder
Contacting with each other for any point can all lead to the conduction of vortex between powder, to reduce the insulating effect of zirconia powder, similarly, Ren Heqi
He is added in magnet the insulating materials of form, does not all have the identical technical effect of same sheet insulating materials；From comparative example
4a is compared with the experimental data of comparative example 4b it is found that the two magnet Br is suitable, Hcj is improved, resistivity improves.This is because magnetic
Powder Particle Size is thinner, and Grain-Boundary Phase is more, and the obstruction of crystal boundary relative eddy is bigger.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of preparation method of the rare-earth permanent magnet of high resistivity, which comprises the steps of:
1) to R1Insulating trip is added in-Fe-M-B magnetic powder, wherein R1For one of rare earth element or a variety of, M Ti, V, Cr,
One of Mn, Co, Ga, Cu, Si, Al, Zr, Nb, W, Mo or a variety of, the insulating trip are quartz, zirconium oxide, aluminium oxide, silicon
One of sour calcium is a variety of, and the weight of insulating trip is 0.01~5wt% of magnetic powder total weight；
2) mixture of the resulting magnetic powder of step 1) and insulating trip is filled into mold, carries out orientation compacting；
3) the resulting blank of step 2) is sintered, carries out ageing treatment afterwards, obtains rare-earth permanent magnet.
2. preparation method according to claim 1, which is characterized in that R described in step 1)1Each group in-Fe-M-B magnetic powder
The weight fraction divided is as follows: R10.92~1.2wt% of 28.6~33wt%, B, M≤2.3wt%, surplus is iron and impurity.
3. preparation method according to claim 1 or 2, which is characterized in that R described in step 1)1- Fe-M-B magnetic powder is
Pairing bronze.
4. preparation method according to claim 1 or 2, which is characterized in that the middle Hou Du that insulating trip is added of step 1)≤
0.1mm。
5. preparation method according to claim 1 or 2, which is characterized in that the weight of insulating trip is that magnetic powder is total in step 1)
0.5~3wt% of weight.
6. preparation method according to claim 1, which is characterized in that the process conditions of orientation compacting in step 2) are as follows: room
Temperature, magnetic field strength 2T.
7. preparation method according to claim 1, which is characterized in that be sintered to hot pressed sintering described in step 3).
8. preparation method according to claim 1 or claim 7, which is characterized in that sintering temperature described in step 3) be 910~
1090 DEG C, sintering time is 1.5~6h.
9. preparation method according to claim 1, which is characterized in that the temperature of ageing treatment is 450~600 in step 3)
DEG C, the time of ageing treatment is 2~5h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710003772.4A CN106653271B (en) | 2017-01-04 | 2017-01-04 | A kind of preparation method of the rare-earth permanent magnet of high resistivity |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710003772.4A CN106653271B (en) | 2017-01-04 | 2017-01-04 | A kind of preparation method of the rare-earth permanent magnet of high resistivity |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106653271A CN106653271A (en) | 2017-05-10 |
| CN106653271B true CN106653271B (en) | 2019-05-07 |
Family
ID=58842536
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710003772.4A Active CN106653271B (en) | 2017-01-04 | 2017-01-04 | A kind of preparation method of the rare-earth permanent magnet of high resistivity |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106653271B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Family Cites Families (2)
| 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 |
| CN104167271B (en) * | 2014-07-25 | 2017-07-21 | 安徽大地熊新材料股份有限公司 | A kind of high resistivity rare-earth iron series R Fe B magnets and preparation method thereof |
-
2017
- 2017-01-04 CN CN201710003772.4A patent/CN106653271B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106653271A (en) | 2017-05-10 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106409497B (en) | A kind of method of neodymium iron boron magnetic body grain boundary decision | |
| JP2022543491A (en) | RTB Permanent Magnet Material, Manufacturing Method, and Application | |
| CN103212714B (en) | Method for preparing neodymium iron boron material | |
| JP2022535480A (en) | Neodymium-iron-boron magnet material, raw material composition, manufacturing method, and application | |
| ES2912741T3 (en) | Preparation method for a rare earth permanent magnetic material | |
| CN109411173B (en) | Method for manufacturing NdFeB rare earth permanent magnet with adjustable intrinsic coercivity gradient | |
| EP2650886A1 (en) | High-corrosion resistant sintered ndfeb magnet and preparation method therefor | |
| WO2011134178A1 (en) | Method for manufacturing high performance neodymium-iron-boron permanent magnetic material | |
| TWI770730B (en) | NdFeB PERMANENT MAGNET MATERIAL, PREPARATION METHOD AND APPLICATION | |
| CN101499346A (en) | Sintered NdFeB permanent magnet with high working temperature and high corrosion resistance | |
| TWI569291B (en) | Neodymium rare earth permanent magnet and its manufacturing method | |
| WO2015140829A1 (en) | Permanent magnet, motor, and generator | |
| CN103474225A (en) | Preparation method of neodymium-iron-boron magnet doped with dysprosium and cerium | |
| JP2008130780A (en) | Rare-earth magnet | |
| CN103559972A (en) | Preparation method for sintered Nd-Fe-B permanent-magnet material | |
| CN102747318A (en) | Method for improving coercive force of sintered rare earth-iron-boron permanent magnetic material | |
| CN109509628B (en) | Preparation method of sintered neodymium iron boron composite powder | |
| CN106653271B (en) | A kind of preparation method of the rare-earth permanent magnet of high resistivity | |
| CN106158213A (en) | A kind of high-coercivity neodymium-iron-boronpermanent-magnet permanent-magnet material and preparation method thereof | |
| KR102454771B1 (en) | A Preparation Method of a Rare Earth Anisotropic Bonded Magnetic Powder | |
| CN103317146B (en) | Hydro-thermal method prepares the method for NdFeB magnetic powder | |
| CN109326404B (en) | Neodymium-iron-boron magnetic material and preparation method thereof | |
| CN107403675B (en) | A kind of preparation method of high thermal stability neodymium iron boron magnetic body | |
| CN104867645B (en) | A kind of nanocrystalline hot-pressed magnets of high-coercive force and preparation method thereof | |
| TWI807658B (en) | R-t-b series permanent magnet material and preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |