CN106298133B - Permanent-magnet material and its preparation method and application based on the primary norium of total association - Google Patents
Permanent-magnet material and its preparation method and application based on the primary norium of total association Download PDFInfo
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Abstract
The present invention provides a kind of double main phase permanent-magnet materials and its preparation method and application based on the primary norium of total association, consisting of: (RMaFe100‑a‑b‑cMbBc)1‑x{[(Pr1‑yNdy)1‑zRz]dFe100‑d‑e‑fMeBf}x, the permanent-magnet material includes RMaFe100‑a‑b‑ cMbBc[(Pr1‑yNdy)1‑zRz]dFe100‑d‑e‑fMeBfTwo kinds of main phases, wherein RMFor the primary norium of total association, quality composition includes: 20%~32%La, 48%~58%Ce, 4%~6%Pr and 15%~17%Nd；M is one of Mn, Co, Ni, Zr, Ti, Cu, Zn, Al, Ga, In, Sn, Ge and Si or a variety of；R is one of Y, La, Ce, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu or a variety of.Since permanent magnet of the invention is cheap, and comprehensive permanent magnetism is had excellent performance, therefore has very extensive application value.
Description
Technical field
The present invention relates to a kind of permanent-magnet materials and its preparation method and application based on the primary norium of total association.
Background technique
Neodymium iron boron has high remanent magnetism B as third generation rare earth permanent-magnetic materialr, high-coercive force Hcj, high energy product (BH)mSpy
Point is applied to the high-tech sectors such as aerospace, information and the energy, is one of important foundation material of modern industry.
But being continuously increased with global neodymium iron boron demand, the use of rear earth element nd also greatly increases, so that neodymium metal be caused to account for
To 90% or more of the neodymium iron boron cost of raw material.Very big pressure is caused to magnetic materials production producer and user.And due to
Rare earth is intergrowth mineral, therefore on the one hand the demand to narrow resources such as Pr, Nd, Tb, Dy leads to the high abundances rare earth such as La, Ce, Y
It is a large amount of overstock, cause the waste of rare earth resources.On the other hand, it is single that separation is extracted from the primary norium of total association
High pure rare earth metals complex process, not only consume a large amount of energy and resource, but also serious increase carrying capacity of environment.
If it is high-purity that directly separated single Pr, Nd, Tb, Dy etc. can be substituted using the primary norium of association altogether
Rare earth metal prepares permanent magnet, then can not only reduce or remit disappearing for complicated rare earth purification process, the reduction energy and resource significantly
It consumes, reduce cost, and the balanced use problem of China's rare earth resources can be substantially solved, mitigate carrying capacity of environment, have very
Important application value and strategic importance.
Currently, attention much has been obtained to reduce cost, without heavy rare earth or less with the research of neodymium metal
(CN102436892A, CN102800454A, CN102969112A, CN103137314A, CN103035350A).It is dilute in conjunction with China
The characteristics of soil resource, substituting single Nd with the most abundant Ce and LaCe alloy of reserves or mischmetal (LaCePrNd) becomes current
The hot spot of research, but due to La2Fe14B and Ce2Fe14B, which has, is far below Nd2Fe14The anisotropy field of B, and be not easy into
Phase.Therefore, in actual production, Rare-Earth Ce or the substitution of La can all cause the decline of permanent magnet performance, especially as La or
The substitution amount of person Ce is more than 60%, and magnet cost performance is extremely low, without practical value (JOURNAL OF APPLIED PHYSICS
115,113912(2014)。
Although the slightly higher permanent-magnet material of performance (JOURNAL OF can be obtained using melt spinning technology (belt-rejecting technology)
APPLIED PHYSICS 111,07A718 (2012)), but on the one hand this magnetism of material can be still very low, another party
Face, this magnet are a kind of thin slices (shape is fixed), are unable to widespread adoption.Therefore, it is former how to prepare high performance association altogether
Raw norium base sintered permanent magnet is still problem in the urgent need to address at present.
2007 Nian Zhongke tricyclics (CN 101471165B) are prepared for using the mode of dual alloy with high-coercive force and remanent magnetism
The permanent magnet hardly declined allows it is seen that the advantage of dual alloy.Iron and Steel Research Geueral Institute in 2012 (CN 102800454A,
CN 103187133A, CN 103714939A) disclose double main phases or more main phase magnets and its manufacturing method respectively again, and foretell
The permanent magnet of excellent combination property can be prepared by method made above.
Typically, why bis- (more) main phase magnet comprehensive performances are higher than single main phase magnet, in addition to what it showed " mixes
Outside conjunction " effect, the coupling between magnet is an important reason, therefore is substituted using high abundance rare earth or mischmetal part
Single main phase magnet performance of the preparations such as Nd is not high, can not achieve the effect of 1+1 > 2.Although and using double main phase magnets that can obtain
To the raising (CN102800454A) of performance, but it is still unobvious to promote effect.It is dilute using high abundance rare earth or mixing at present
It is all to need first to prepare high abundance rare earth or mischmetal by adding other rare earth element in double main phase magnets of soil preparation
At single main phase magnet, main phase magnet in pairs is then prepared with another main phase again, without directly using La, Ce or mischmetal
(MM) main phase of the iron boron magnet as one of them.Although the realization that this method is conducive to magnet preparation process (can not have to
New preparation process directly continues to use the preparation method of single main phase), but this double main phase magnets are reduced to a certain extent
Coupling advantage, be unfavorable for the promotion of magnet comprehensive performance and the effective use of rare earth resources.
Summary of the invention
In order to overcome the shortage of prior art, the present invention provides a kind of double main phases of primary norium base of association altogether forever
Magnetic material and preparation method thereof, this permanent-magnet material prepare permanent magnet using the primary norium of total association as base, not only valence
Lattice are cheap, are conducive to the balanced use of environmental protection and rare earth resources, and to contain only total association primary mixed for one of them main phase
Rare earth metal is closed without adding other rare earth element, is conducive to the coupling advantage and magnet comprehensive magnetic energy that improve double main phase magnets
Raising.
For ease of description, following title or term are defined and are illustrated:
1, raw material are prepared: removing the oxide layer on raw material surface using the mode of ball blast, polishing, and weighs original in proportion
Material.
2, it prepares rapid-hardening flake: after the raw material weighed up in proportion are mixed, being put into ZGSN-0.003 type vacuum induction rapid hardening
Crucible in furnace is heated to all raw material thawing under protection of argon gas, and then cooling keeps it in 1200~1600 DEG C, most
It is afterwards to be prepared into the rapid-hardening flake with a thickness of 0.1~0.5mm in the water-cooled copper roller of 1~5 meter per second for solution-cast to linear velocity.
3, hydrogen breaking: rapid-hardening flake is put into hydrogen broken furnace, is first evacuated down to 5Pa hereinafter, being then charged with the H of about 0.2Mpa2,
H is supplemented at any time2, make H2Pressure substantially remains under the pressure of 0.2Mpa, inhales hydrogen 1~2 hour, is then evacuated down at room temperature
5Pa hereinafter, 200~600 DEG C dehydrogenation 1~2 hour, obtain hydrogen break powder.
4, airflow milling: being put into QLM-100T type airflow mill for raw material (generally hydrogen breaks powder) to be ground, small in oxygen content
Under the content of 0.1ppm, airflow milling is carried out, obtains the air-flow milling that average particle size is 1~5 μm by adjusting selection by winnowing wheel speed.
In order to realize goal of the invention, the present invention provides the following technical scheme that
A kind of double main phase permanent-magnet materials based on the primary norium of total association, elemental composition are in mass ratio
(RMaFe100-a-b-cMbBc)1-x{[(Pr1-yNdy)1-zRz]dFe100-d-e-fMeBf}x, the permanent-magnet material includes RMaFe100-a-b-cMbBc
[(Pr1-yNdy)1-zRz]dFe100-d-e-fMeBfTwo kinds of main phases, wherein RMFor the primary norium of total association, quality group
At including: 20~32%La, 48~58%Ce, 4~6%Pr and 15~17%Nd；M be Mn, Co, Ni, Zr, Ti, Cu, Zn, Al,
One of Ga, In, Sn, Ge and Si or a variety of；R is one of Y, La, Ce, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu
Or it is a variety of, and 27≤a≤33,0≤b≤5,0.9≤c≤1.3,0.1≤x≤0.9,0≤y≤1,0≤z≤0.1,28≤d≤
32,0≤e≤5,0.9≤f≤1.2.
Preferably, in double main phase permanent-magnet materials, the value range of x are as follows: 0.4≤x≤0.9, more preferably 0.6≤
x≤0.9。
The double main phase permanent-magnet materials provided according to the present invention, wherein " the primary norium of association altogether " refers to
Extracted from the primary Rare Earth Mine of total association without Rare Earth Elements Determination separation, the mixing that rare earth partition and raw ore are consistent
Rare earth metal.It can be primary mixed for the total association from baiyuneboite for the primary norium of total association of the invention
Close rare earth metal.
Can also include following component altogether in the primary norium of association described: Sm < 0.5%, Fe < 0.04%,
Si < 0.02%, Mg < 0.06%, Zn < 0.01%, W < 0.01%, Mo < 0.01%, Cu < 0.01%, Ti < 0.01%, Ca <
0.01%, Pb < 0.01%, Cr < 0.01%, C < 0.01%.
Preferably, double main phase permanent-magnet materials can be one of following material:
(RM32Fe63Zr3Al0.9B1.1)30((Pr0.4Nd0.6)30Fe67Al2B1)70；
(RM32Fe66Al1B1)10((Nd0.97Dy0.03)30Fe69B1)90；
(RM31Fe63Zr2Al1Si2B1)40((Pr0.2Nd0.8)31Fe67Co1B1)60；
(RM33Fe62Zr1Al1.8Si1B1.2)60((Pr0.2Nd0.8)32Fe66Ga0.8Sn0.2B1)40。
The present invention also provides the preparation methods of above-mentioned permanent-magnet material, and described method includes following steps:
(1) R is prepared respectivelyMaFe100-a-b-cMbBcAnd ((Pr1-yNdy)1-zRz)dFe100-d-e-fMeBfTwo kinds of main-phase alloys, and
The rapid-hardening flake with a thickness of 0.1~0.5mm is made, breaking powder using the hydrogen that hydrogen breaking obtains 1~3mm, (width is 1~3mm, thickness
For the piece type powder of 0.1~0.5mm)；
(2) by RMaFe100-a-b-cMbBcHydrogen breaks powder and ((Pr1-yNdy)1-zRz)dFe100-d-e-fMeBfHydrogen breaks powder according to mass ratio
It is uniformly mixed for the ratio of 10:90~90:10, is put into air-flow and is milled into the air-flow milling that average particle size is 1~5 μm；
(3) by air-flow milling under the protection of inert gas, the oriented moulding in the magnetic field of 0.5~2T；
(4) magnet being orientated is put into hot isostatic press, under the isostatic pressure of 50~400MPa, 400 DEG C~
At a temperature of 1100 DEG C of equal static pressure, 0.01~4h is suppressed.
The preparation method provided according to the present invention, it is preferable that in step (1), RMaFe100-a-b-cMbBc: ((Pr1- yNdy)1-zRz)dFe100-d-e-fMeBfMass component than range be 10:90~60:40.
The preparation method provided according to the present invention, it is preferable that the hot isostatic pressing power in step (4) is 50~200Mpa；It is excellent
Selection of land, hip temperature are 650~1040 DEG C；Preferably, the hot isostatic pressing time is 0.5~2h.
The preparation method provided according to the present invention, wherein the preparation method can also include step (5): by step (4)
Magnet after compression moulding is put into the sintering furnace of high vacuum to be sintered 0.01~2 hour under 800~1060 DEG C of sintering temperature.
The preparation method provided according to the present invention, wherein the preparation method can also include step (6): by step (5)
Obtained sintered body 200~500 DEG C at a temperature of be tempered 0.01~2h.
The present invention also provides above-mentioned double main phase permanent-magnet materials or according to double main phase permanent magnetism materials made from the method for the present invention
Material is in instrument and meter, household electrical appliances, motor, wind-power electricity generation, aerospace, mobile phone, communication equipment, rotating machinery, magnetotherapy appliance
And the application in sports goods.
Compared to La, Ce or MM the base sintered rare-earth permanent magnetic material prepared at present, the present invention is used at without rare earth purification
The primary norium raw material of total association of reason prepares permanent magnet, thus raw material process it is simple, it is few to the energy and resource consumption,
It is cheap, and be conducive to the balanced use of environmental protection and rare earth resources.In addition, due to double main phase magnetic prepared by the present invention
Main phase contains only the primary norium of total association without adding other rare earth element one of in body, therefore improves
The coupling advantage of double main phase magnets, to increase the comprehensive magnetic energy of magnet.Again, since preparation method of the invention uses
The special hot isostatic pressing for being conducive to double main phase magnets, not only simplifies preparation process, and further improve magnetic
Performance.
Specific embodiment
The present invention is further described in detail With reference to embodiment, and the embodiment provided is only for explaining
The bright present invention, the range being not intended to be limiting of the invention.
Mischmetal R used in the following embodimentMPurchase presses matter from Suzhou Kang Ming Chemical Co., Ltd., chemical component
Measure ratio about are as follows: 27.8%La, 51.9%Ce, 5.1%Pr and 15.1%Nd, remaining is the impurity such as Sm, Fe, Si, Al, C.
Embodiment 1
(1) two kinds of master alloying R are preparedM32Fe63Zr3Al0.9B1.1(Pr0.4Nd0.6)30Fe67Al2B1, two kinds of total matter of master alloying
Amount is 2.5Kg, is prepared into the rapid-hardening flake with a thickness of 0.3mm respectively.
(2) above two master alloying is passed through into hydrogen breaking respectively, granularity is obtained and is evenly distributed the about particle of 1~3mm, so
Airflow milling powder is distinguished afterwards, obtains the particle that average particle size is about 2 μm.
(3) R in mass ratioM32Fe63Zr3Al0.9B1.1: (Pr0.4Nd0.6)30Fe67Al2B1More than the ratio mixing of 30:70
Air-flow milling, and wherein 10g is weighed, it is put into after sealing in the magnetic field orientating mold of argon gas protection, is orientated under the magnetic field of 1.5T
It forms (pressure is about 20MPa).
(4) magnet after molding is put into hot isostatic press under the isostatic pressure of 150MPa, 700 DEG C at a temperature of,
Compacting 0.5 hour, is then quickly cooled down by built-in cooler.
(5) magnet after hip moulding is put into the sintering furnace of high vacuum and is sintered, 1000 DEG C of sintering temperature, sintering
It is 0.5 hour, air-cooled to room temperature.
(6) by sintered magnet 490 DEG C tempering after 2 hours to get arrive the present embodiment double main phase permanent-magnet materials.
The material being prepared is processed into the small column of Φ 10mm × 10mm, and in the permanent magnetism B-H of NIM-2000HF type
Hysteresiscope measures the permanent magnetism performance of magnet (measurement temperature is room temperature, and about 20~22 DEG C, following embodiment is identical).Test knot
Fruit is listed in table 1.
As seen from Table 1, double main phase magnet performances made from the present embodiment are excellent, primary dilute in total association
In the case where native content 30%, magnet coercivity is more than 10kOe, and magnetic energy product is more than 40MGOe, it is already possible to realize practical application.
Comparative example 1
Double main phase magnets are prepared according to step same as Example 1, the difference is that, without described in embodiment 1
The step of (4), and step (4) is changed to: implementing isostatic cool pressing processing under the pressure of 150Mpa.Material made from this comparative example
Test result be also found in table 1.
By being compared with embodiment 1 as can be seen that the hot isostatic pressing step in embodiment 1 is replaced with this comparative example
Isostatic cool pressing step after, the magnetic property of material declines to a great extent.
Comparative example 2
Double main phase magnets are prepared according to step same as Example 1, the difference is that, step (4) are as follows: in 150Mpa
Pressure under implement isostatic cool pressing processing；And step (5) are as follows: by the sintering of step (4) treated magnet is put into high vacuum
It is sintered, 1000 DEG C of sintering temperature, is sintered 8 hours in furnace, it is air-cooled to room temperature.The test result of material made from this comparative example also arranges
In table 1.
By being compared with embodiment 1 as can be seen that the hot isostatic pressing step in embodiment 1 is replaced with this comparative example
Isostatic cool pressing step after, even if increasing sintering time, the magnetic property of material still can decline to a great extent.
Comparative example 3
Double main phase magnets are prepared according to step same as Example 1, the difference is that, step (4) are as follows: in 150Mpa
Pressure under implement isostatic cool pressing processing；And step (5) are as follows: by the sintering of step (4) treated magnet is put into high vacuum
It is sintered, 1040 DEG C of sintering temperature, is sintered 2 hours in furnace, it is air-cooled to room temperature.The test result of material made from this comparative example also arranges
In table 1.
By being compared with embodiment 1 as can be seen that the hot isostatic pressing step in embodiment 1 is replaced with this comparative example
Isostatic cool pressing step after, by adjusting sintering temperature, sintering time can also reach preferable magnetic property, but compared to implementation
Example 1 is as a result, its magnetic property is still lower.
Comparative example 4
Magnet is prepared according to step same as Example 1, the difference is that, step (1) is to prepare single main phase to close
Gold (RM32Fe63Zr3Al0.9B1.1)30[(Pr0.4Nd0.6)30Fe67Al2B1]70, rather than the alloy of separately formulated two kinds of main phases；And
And step (2) is that this single main-phase alloy hydrogen is broken and airflow milling powder obtains the particle that average particle size is 2 μm.This comparative example system
The test result of the material obtained is also found in table 1.
Double main phase magnets are not used by comparing can be seen that with embodiment 1, but by way of element substitution
It is prepared into single main phase, even if increasing its magnetic property (can be referring to comparative example 5), magnetic property is also than double using hot isostatic pressing technique
Main phase magnet performance is much lower.
Comparative example 5
Magnet is prepared according to step same as Example 1, the difference is that, step (1) is to prepare single main phase to close
Gold (RM32Fe63Zr3Al0.9B1.1)30[(Pr0.4Nd0.6)30Fe67Al2B1]70, rather than the alloy of separately formulated two kinds of main phases；Step
Suddenly (2) are this single main-phase alloy hydrogen is broken and airflow milling powder obtains the particle that average particle size is 2 μm；Step (4) are as follows:
Implement isostatic cool pressing processing under the pressure of 150Mpa；And step (5) are as follows: treated, and magnet is put into high vacuum by step (4)
Sintering furnace in be sintered, 1040 DEG C of sintering temperature, be sintered 2 hours, it is air-cooled to room temperature.The test knot of material made from this comparative example
Fruit is also found in table 1.
By being compared with embodiment 1 and comparative example 4 as can be seen that even for single main phase magnet, by hot isostatic pressing
Processing replaces with isostatic cool pressing processing, and magnetic property also can decrease, this also illustrates that hot isostatic pressing technique is also applied for single master
Phase magnet.However compared to double main phase magnets, influence of this replacement to magnetic property is smaller.
Comparative example 6
(1) two kinds of master alloying R are prepared in mass ratio respectivelyM16Pr16Fe63Zr3Al0.9B1.1And (RM0.22Pr0.18Nd0.6)30Fe67Al2B1, the gross mass of two kinds of master alloyings is 2.5Kg, is then prepared into the rapid-hardening flake with a thickness of 0.3mm respectively；
(2) rapid-hardening flake of step (1) is passed through into hydrogen breaking respectively, obtains the particle that average particle size is about 1~3mm, then
Airflow milling powder respectively, obtains the particle that average particle size is about 2 μm.
(3) R in mass ratioM16Pr16Fe63Zr3Al0.9B1.1: (RM0.22Pr0.18Nd0.6)30Fe67Al2B1For the ratio of 30:70
The above air-flow milling is mixed, and weighs wherein 10g, is put into after sealing in the magnetic field orientating mold of argon gas protection, in the magnetic of 1.5T
Oriented moulding off field (pressure is about 20MPa).
(4) magnet after molding is put into hot isostatic press under the isostatic pressure of 150MPa, 700 DEG C at a temperature of,
Compacting 0.5 hour, is then quickly cooled down by built-in cooler.
(5) magnet after hip moulding is put into the sintering furnace of high vacuum and is sintered, 1000 DEG C of sintering temperature, sintering
It is 0.5 hour, air-cooled to room temperature.
(6) sintered magnet is just obtained to the magnet of this comparative example for 2 hours after 490 DEG C of tempering.
The above-mentioned sintered magnet being prepared is processed into Φ 10mm × 10mm small column in the permanent magnetism of NIM-2000HF type
B-H hysteresiscope measures the permanent magnetism performance (measurement temperature be room temperature, about 20~22 DEG C) of magnet.Test result is also found in table 1.
By the comparison with embodiment 1, the part Pr substitution R is used it can be seen from the data in table 1M, in identical rare earth
Coupling interaction can be weakened in the case where content, ultimately cause the decline of magnet performance.
Embodiment 2
Double main phase magnets are prepared according to step same as Example 1, the difference is that, step (4) are as follows: after molding
Magnet be put into hot isostatic press under the isostatic pressure of 120MPa, 900 DEG C at a temperature of, suppress 0.5 hour, then pass through
Built-in cooler is quickly cooled down；And without step (5) and (6).Test result is listed in table 1.
As long as the temperature that hot isostatic pressing is implemented it can be seen from the data in table 1, time are suitable, without the burning in later period
Knot, tempering, and magnet is directly made and not will lead to being remarkably decreased for magnetic property.This is highly beneficial for reducing preparation time
's.
Embodiment 3
(1) two kinds of master alloying R are preparedM32Fe66Al1B1(Nd0.97Dy0.03)30Fe69B1, two kinds of master alloying gross masses are
The rapid-hardening flake of 0.3mm is respectively prepared in 2.5Kg.
(2) above two master alloying is passed through into hydrogen breaking respectively, obtains the particle that average particle size distribution is about 1~3mm, so
Airflow milling powder is distinguished afterwards, obtains the air-flow abrasive particle that average particle size is respectively 1.5 μm and 3 μm.
(3) R in mass ratioM32Fe66Al1B1: (Nd0.97Dy0.03)30Fe69B1The above airflow milling is mixed for the ratio of 10:90
Powder, and wherein 10g is weighed, it is put into after sealing in the magnetic field orientating mold of argon gas protection, the oriented moulding (pressure under the magnetic field of 1.5T
Power is about 20MPa).
(4) magnet after molding is put into hot isostatic press under the isostatic pressure of 100MPa, 1040 DEG C at a temperature of,
Compacting 0.5 hour, is then quickly cooled down by built-in cooler.
The above-mentioned magnet being prepared is processed into Φ 10mm × 10mm small column in BH loop instrument to test, is surveyed
Test result is listed in table 1.
Embodiment 4
(1) two kinds of master alloying R are preparedM31Fe63Zr2Al1Si2B1(Pr0.2Nd0.8)31Fe67Co1B1, two kinds of total matter of master alloying
Amount is 2.5Kg, and the rapid-hardening flake of 0.3mm is respectively prepared.
(2) above two master alloying is passed through into hydrogen breaking respectively, obtains the particle that average particle size distribution is about 1~3mm, so
Airflow milling powder is distinguished afterwards, obtains the air-flow abrasive particle that average particle size is respectively 2 μm and 3 μm.
(3) R in mass ratioM31Fe63Zr2Al1Si2B1: (Pr0.2Nd0.8)31Fe67Co1B1More than the ratio mixing of 40:60
Air-flow milling, and wherein 10g is weighed, it is put into after sealing in the magnetic field orientating mold of argon gas protection, is orientated under the magnetic field of 1.5T
It forms (pressure is about 20MPa).
(4) magnet after molding is put into hot isostatic press under the isostatic pressure of 200MPa, 970 DEG C at a temperature of,
Compacting 0.8 hour, is then quickly cooled down by built-in cooler.
The above-mentioned magnet being prepared is processed into Φ 10mm × 10mm small column in BH loop instrument to test, is surveyed
Test result is listed in table 1.
Embodiment 5
(1) R is preparedM33Fe62Zr1Al1.8Si1B1.2(Pr0.2Nd0.8)32Fe65Ga0.8Sn0.2Co1B1Two kinds of master alloyings, always
Quality is 2.5Kg, and the rapid-hardening flake of 0.3mm is respectively prepared.
(2) above two master alloying is passed through into hydrogen breaking respectively, obtains the particle that average particle size distribution is about 1~3mm, so
Airflow milling powder is distinguished afterwards, obtains the air-flow abrasive particle that average particle size is respectively 2 μm and 3 μm.
(3) R in mass ratioM33Fe62Zr1Al1.8Si1B1.2: (Pr0.2Nd0.8)32Fe65Ga0.8Sn0.2Co1B1For the ratio of 60:40
Example mixes the above air-flow milling, and weighs wherein 10g, is put into the magnetic field orientating mold of argon gas protection after sealing, in the magnetic of 2T
Oriented moulding off field (pressure is about 20MPa).
(4) magnet after molding is put into hot isostatic press under the isostatic pressure of 50MPa, 650 DEG C at a temperature of, pressure
System 2 hours, is then quickly cooled down by built-in cooler.
The above-mentioned magnet being prepared is processed into Φ 10mm × 10mm small column in BH loop instrument to test, is surveyed
Test result is listed in table 1.
Table 1
As long as keeping two kinds of main phases it can be seen from the result of embodiment 3-5, and rare earth element in one of them main phase
Contain RM, can be transferred through adjusting the sintered magnet that preparation process is had excellent performance, if can be in conjunction with hot isostatic pressing, magnetic
Performance can be further improved.
Technical solution of the present invention is described in detail in embodiment described above, it should be understood that the above is only
It for specific embodiments of the present invention, is not intended to restrict the invention, all technologies of the present invention for meeting condition of the present invention
Scheme can realize the present invention, embodiment numerous to list herein；All any modifications made in spirit of the present invention,
Supplement or similar substitution, should all be included in the protection scope of the present invention.
Claims (6)
1. a kind of preparation method of double main phase permanent-magnet materials based on the primary norium of total association, double main phases are forever
Magnetic material is one of following material:
(RM32Fe63Zr3Al0.9B1.1)30((Pr0.4Nd0.6)30Fe67Al2B1)70；
(RM32Fe66Al1B1)10((Nd0.97Dy0.03)30Fe69B1)90；
(RM31Fe63Zr2Al1Si2B1)40((Pr0.2Nd0.8)31Fe67Co1B1)60；With
(RM33Fe62Zr1Al1.8Si1B1.2)60((Pr0.2Nd0.8)32Fe66Ga0.8Sn0.2B1)40,
Wherein, RMFor the primary norium of total association, quality composition include: 20%~32%La, 48%~58%Ce,
4%~6%Pr and 15%~17%Nd,
The preparation method comprises the following steps:
(1) two kinds of main-phase alloys, and the rapid-hardening flake being made with a thickness of 0.1~0.5mm are prepared respectively, are put down using hydrogen breaking
The hydrogen that equal granularity is 1~3mm breaks powder；
(2) two kinds of main-phase alloy hydrogen are broken powder to be uniformly mixed according to the ratio that mass ratio is 10:90~90:10, is put into airflow milling
The air-flow that average particle size is 1~5 μm is made to be milled；
(3) by air-flow milling under the protection of inert gas, the oriented moulding in the magnetic field of 0.5~2T；
(4) magnet being orientated is put into hot isostatic press, under the isostatic pressure of 50~200Mpa, at 650~1040 DEG C
At a temperature of equal static pressure, 0.5~2h is suppressed.
2. preparation method according to claim 1, wherein airflow milling Powder Particle Size described in step (2) is 1~3 μm.
3. preparation method according to claim 1, wherein the preparation method further includes step
(5): the blank after step (4) compression moulding is put into the sintering furnace of high vacuum in 800~1060 DEG C of sintering temperature
0.01~2h of lower sintering.
4. preparation method according to claim 3, wherein the preparation method further includes step
(6): the sintered body that step (5) is obtained 200~500 DEG C at a temperature of be tempered 0.01~2h.
5. a kind of double main phase permanent-magnet materials based on the primary norium of total association, double main phase permanent-magnet materials are by weighing
Benefit requires any one of 1 to 4 the method to be made.
6. according to described in double main phase permanent-magnet materials made from any one of claims 1 to 4 the method or claim 5
Double main phase permanent-magnet materials are in instrument and meter, household electrical appliances, motor, wind-power electricity generation, aerospace, mobile phone, communication equipment, whirler
Application in tool, magnetotherapy appliance and sports goods.
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| CN108109801A (en) * | 2017-12-20 | 2018-06-01 | 宁波市鄞州智伴信息科技有限公司 | A kind of permanent magnet and its process for preparing rare earth |
| CN108133798A (en) * | 2017-12-20 | 2018-06-08 | 宁波市鄞州智伴信息科技有限公司 | A kind of rare-earth permanent magnet and preparation method thereof |
| CN111383808B (en) * | 2018-12-27 | 2021-07-13 | 京磁材料科技股份有限公司 | Preparation method of high-remanence high-coercivity neodymium iron boron magnet |
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