CN1065152A - Terres rares-iron-cobalt-B anisotropic magnet - Google Patents

Terres rares-iron-cobalt-B anisotropic magnet Download PDF

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CN1065152A
CN1065152A CN 92101185 CN92101185A CN1065152A CN 1065152 A CN1065152 A CN 1065152A CN 92101185 CN92101185 CN 92101185 CN 92101185 A CN92101185 A CN 92101185A CN 1065152 A CN1065152 A CN 1065152A
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crystal grain
anisotropic magnet
magnet
particle diameter
hot
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武下拓夫
中山亮治
石井义成
小川保
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Mitsubishi Materials Corp
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    • 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
    • H01F1/0573—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 obtained by reduction or by hydrogen decrepitation or embrittlement

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  • Chemical & Material Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Hard Magnetic Materials (AREA)
  • Powder Metallurgy (AREA)

Abstract

The invention provides the little R-Fe-Co-B anisotropic magnet of a kind of coercitive temperature coefficient, it is made by obtain R-Fe-Co-B series permanent magnet powder through the hydrogen processing, its composition is: one or more elements among R:10-20%, Co:0.1-50%, B:3-20%, Ti, V, Nb, Ta, Al and the Si, and total content is: 0.001-5.0%, all the other are Fe and unavoidable impurities; It has the R with square crystal structure 2(Fe, Co) 14The Type B intermetallic compound is gathered the crystal grain collecting structure that forms for the crystal grain of principal phase mutually, and its average crystal grain particle diameter is 0.05-20 μ m; Its ratio that is shaped as maximum particle diameter and minimum grain size is less than 2 more than 50% of the whole crystal grain of grains constitute; This R-Fe-Co-B anisotropic magnet is hot-press forming body or hot hydrostatic pressing formed body.

Description

Terres rares-iron-cobalt-B anisotropic magnet
The present invention relates to magnetic characteristic excellent and coercitive temperature coefficient is little, be the R-Fe-Co-B anisotropic magnet of principal component with at least a element, Fe, Co and B in the rare earth element that comprises Y.More particularly, the R-Fe-Co-B anisotropic magnet that relates to hot pressing or hot hydrostatic pressing (calling HIP in the following text) formed body.
Record R-Fe-Co-B series permanent magnet powder in the Te Kaiping 1-132106 Japanese patent gazette, this R-Fe-Co-B series permanent magnet powder is the R with the ferromagnetism phase 2(Fe, Co) 14The Type B intermetallic compound is a raw material for the R-Fe-Co-B series foundry alloy of principal phase mutually, with the H of this kind foundry alloy raw material in given temperature range 2Heat-treat in the atmosphere, impel RHx, (Fe, Co) 2After B and remaining Fe respectively undergo phase transition mutually, adopt again and take off H 2Operation is removed H from raw material 2, and generate the R that belongs to the ferromagnetism phase therefrom 2(Fe, Co) 14Type B phase, the structure of resulting like this R-Fe-Co-B series permanent magnet powder be average grain diameter be 0.05～3 μ m superfine, with R 2(Fe, Co) 14The recrystallization texture of Type B phase is the collecting structure of principal phase.
Above-mentioned R-Fe-Co-B series permanent magnet powder, can not obtain enough magnetic anisotropy owing to only use hot pressing to make hot-press forming body, thereby open flat 2-39503 Japanese patent gazette according to the spy and put down in writing, above-mentioned hot-press forming body is carried out again hot rolling system processing such as hot rolling, form along R 2(Fe, Co) 14The rolled structure of the C direction of principal axis orientation of B phase crystal grain improves magnetic anisotropy therefrom.
But, the rolling magnet of R-Fe-Co-B series that above-mentioned hot-press forming body is carried out hot rolling again and obtain, though have excellent magnetic anisotropy, but increased coercitive temperature coefficient, the rolling magnet of this R-Fe-Co-B series is assembled in the occasion such as motor, because variation of temperature, the performance of motor etc. can change thereupon, thereby causes problem such as poor stability.
Moreover, the rolling magnet of R-Fe-Co-B series, because the discreteness of the different working moduluses that cause in place is brought the discreteness of magnetic anisotropy, in order to prevent these, the process that thermoplasticity the is processed complexity that becomes of having to.
Therefore, it is this fact that takes place owing to the hot-press forming body hot rolling that the inventor etc. increase according to above-mentioned coercitive temperature coefficient, if based on the magnet that obtains the magnetic anisotropy excellence without above-mentioned hot rolling, study with regard to the understanding that above-mentioned coercitive temperature coefficient increase can not take place, the result obtains such knowledge, promptly contains:
R：10～20%
Co：0.1～50%
B：3～20%
A kind of among Ti, V, Nb, Ta, Al and the Si or element more than two kinds, its total content is 0.001～5.0%,
Remaining is made up of Fe and unavoidable impurities,
The ratio b/a value of the maximum particle diameter b that is shaped as each crystal grain of crystal grain and minimum grain size a is less than 2, and the average grain diameter of crystal grain is of a size of 0.05～20 μ m, and the crystal grain collecting structure is by the R that gets square crystal structure 2(Fe, Co) 14The Type B intermetallic compound is that the crystal grain of principal phase constitutes mutually.
The R-Fe-Co-B series magnets exhibit that is made of the hot-press forming body or the HIP formed body of above-mentioned substance goes out excellent magnetic anisotropy, and its coercitive temperature coefficient can not increase.
The present invention makes according to such knowledge, and this R-Fe-Co-B anisotropic magnet is characterised in that it is hot-press forming body or the HIP formed body with above-mentioned constituent and crystal grain collecting structure, and its coercitive temperature coefficient is little.
Compare with existing rolling magnet, the discreteness of the magnetic anisotropy that the little R-Fe-Co-B anisotropic magnet of coercive force temperature coefficient of the present invention does not almost cause because of the place, its corrosion resistance might as well.
Also have, because R-Fe-Co-B anisotropic magnet of the present invention has the crystal grain collecting structure, so even at R 2(Fe, Co) 14Near the Type B compound component, promptly at R 11.8Fe AequumB 5.9Excellent magnetic anisotropy and high coercive force are also arranged near the component.
Below, the manufacture method of R-Fe-Co-B anisotropic magnet of the present invention is described.
The manufacture method of R-Fe-Co-B series permanent magnet powder that is used to make R-Fe-Co-B anisotropic magnet of the present invention is as follows: with fusion casting by fixed constituent make and contain Ti, V, Nb, Ta, the R-Fe-Co-B series foundry alloy of one or more elements among Al and the Si, this R-Fe-Co-B series foundry alloy is heated in hydrogen atmosphere, in temperature is 500-1000 ℃, heat-treat in the mixed-gas atmosphere of hydrogen atmosphere or hydrogen and inert gas, subsequently, in temperature is 500-1000 ℃, Hydrogen Vapor Pressure is to carry out dehydrogenation in following vacuum atmosphere of 1 Torr or the inert gas atmosphere of hydrogen partial pressure power below 1 Torr to handle, and cools off thereafter and makes.
The R-Fe-Co-B series foundry alloy that will contain one or more elements among quantitative to some extent above-mentioned Ti, V, Nb, Ta, Al and the Si carries out homogenizing under 600～1200 ℃ temperature handles, and after above-mentioned dehydrogenation is handled, under 300～1000 ℃ temperature, heat-treat, owing to added above-mentioned processing procedure, thereby can make magnetic anisotropy and the excellent more R-Fe-Co-B series permanent magnet powder of corrosion resistance.
The structure of the R-Fe-Co-B series permanent magnet powder of making like this is by R 2(Fe, Co) 14The crystallization collecting structure again of the recrystal grain set of Type B intermetallic compound phase constitutes, and does not have impurity and distortion on its intracrystalline and the crystal boundary.
Constitute the recrystal grain of this crystallization collecting structure again, if its on average again the crystallization particle diameter in 0.05～20 mu m range, then be enough, if near the size of microcrystal size (about 0.3 μ m) of single magnetic domain, in the scope of 0.05～3 μ m, then better.
Have above-mentioned size each recrystal grain to be shaped as maximum particle diameter b better with ratio b/a＜2 of minimum grain size a, have the recrystal grain of this shape to account for the 50%(volume of whole recrystal grains) more than be necessary.Because the ratio b/a with above-mentioned maximum particle diameter b and minimum grain size a is less than 2 recrystal grain shape, therefore, R-Fe-Co-B series permanent magnet powder when coercive force improves, in 25～100 ℃ coercitive temperature coefficient aiHc less than-0.6%/℃.
In addition, because there is the crystal boundary phase hardly in the recrystallization texture of the R-Fe-Co-B that makes like this series permanent magnet powder, in fact only have by R 2(Fe, Co) 14The crystallization collecting structure again that the Type B intermetallic compound constitutes mutually, and the situation itself that does not have the crystal boundary phase can improve magnetization value, simultaneously, suppressed the corrosion undertaken by the crystal boundary phase, also have, do not have the stress distortion that causes by thermoplasticity processing, so reduced the possibility of stress corrosion, therefore, improved corrosion resistance.
The R-Fe-Co-B series permanent magnet powder of making like this is shaped in magnetic field, make the press-powder base, then this press-powder base is carried out hot pressing or HIP under 600～900 ℃ temperature, can the be maintained structure and the characteristic of above-mentioned R-Fe-Co-B series permanent magnet powder, and the little R-Fe-Co-B anisotropic magnet of the present invention of coercitive temperature coefficient.
And, as required, under 300～1000 ℃ temperature, heat-treat and can improve coercive force.
If at common sintering temperature, then because this sintering temperature generally is a high temperature, thereby the trickle recrystal grain of R-Fe-Co-B series permanent magnet powder has been grown with above-mentioned press-powder base, become big crystal grain, make magnetic characteristic, particularly coercive force reduces, so be bad.
Therefore, in the method for making R-Fe-Co-B anisotropic magnet of the present invention, necessary employing can be in the pressure sintering or the HIP method of the sintering temperature lower than common sintering temperature, to suppress the growth of crystal grain.Also have,, in magnetic field, be shaped, after hot pressing, HIP, needn't carry out thermoplasticity processing for giving magnetic anisotropy.
Below, the reason about constituent, average crystal grain particle diameter and the crystal grain of the little R-Fe-Co-B anisotropic magnet of the coercive force temperature coefficient of the invention described above being done be defined as above is described.
（a）R
R is one or more elements among Nd, Pr, Tb, Dy, La, Ce, Ho, Er, Eu, Sm, Gd, Tm, Yb, Lu and the Y, generally with Nd as main body, add above other rare earth element, particularly Tb, Dy and Pr, the effect that increases coercive force iHc is arranged,, or be higher than 20% if the content of R is lower than 10%, then the coercive force of anisotropy magnet all can descend, and can not get good magnetic characteristic.So the content of R is decided to be 10～20%.
（b）B
If the content of B is lower than 3%, or is higher than 20%, then the coercive force of anisotropy magnet all can descend, and can not get good magnetic characteristic, so the content of B is decided to be 3～20%.In addition, replacing a part of B with C, N, O, F also is fine.
（c）Co
Owing to add Co, thereby have coercive force and the magnetic temperature characterisitic (for example Curie point) that improves anisotropy magnet and improve corrosion proof effect, if but it contains quantity not sufficient 0.1%, then can not get desired effect, on the other hand, if content surpasses 50%, then magnetic characteristic can descend, so also bad.Therefore, the content of Co is decided to be 0.1～50%.The content of Co coercive force between 0.1～20% is the highest, so that the content of Co is decided to be is 0.1～20% better.
(d) Ti, V, Nb, Ta, Al and Si
The composition that these compositions contain as the R-Fe-Co-B anisotropic magnet, have the coercive force of raising and give good magnetic anisotropy and stable corrosion proof effect, but they contain quantity not sufficient 0.001% time, can not get desired effect, on the other hand, content surpasses at 5.0% o'clock, and magnetic characteristic can descend.So the total content of one or more elements among Ti, V, Nb, Ta, Al and the Si is decided to be 0.001～5.0%.
In addition, also contain at least a element among Ni, Cu, Zn, Ga, Ge, Zr, Mo, Hf, the W, content is 0.001～5.0%, and it makes the R-Fe-Co-B anisotropic magnet have good magnetic anisotropy and corrosion resistance.
(e) average crystal grain particle diameter
Constitute the R of R-Fe-Co-B anisotropic magnet structure 2(Fe, Co) 14The average crystal grain particle diameter of Type B phase crystal grain then is difficult to magnetize during less than 0.05 μ m, so bad, on the other hand, during greater than 20 μ m, then coercive force and rectangularity descend, and can not get high magnetic characteristic, so also bad.
Therefore, the average crystal grain particle diameter is decided to be 0.05～20 μ m.This occasion is if the average crystal grain particle diameter is then better in 0.05～3 mu m range near the size of microcrystal size (0.3 μ m) of single magnetic domain.
(f) shape of crystal grain
Crystal grain with above-mentioned size, its shape with maximum particle diameter b and minimum grain size a than b/a less than 2 for good, have the crystal grain of this shape must account for the 50%(volume of whole crystal grain) more than.Owing to satisfy the condition of above-mentioned b/a＜2, thereby improved the coercive force of R-Fe-Co-B anisotropic magnet, improved corrosion resistance, coercitive temperature coefficient is diminished.
Below, with embodiment and comparative example the present invention is described particularly.
Prepare and variously to obtain with the plasma founding, contain Co and Ti, V, Nb, Ta, the R-Fe-Co-B series alloy ingot casting of one or more elements among Al and the Si and do not contain Ti fully, V, Nb, Ta, the R-Fe-Co-B series alloy ingot casting of any element among Al and the Si, these alloy cast ingots are carried out homogenizing respectively to be handled, just at hydrogen atmosphere, temperature is to keep 20 hours under 1130 ℃ the condition, thereafter, this ingot casting of handling through homogenizing is cut apart square into about 15mm as raw alloy, this raw alloy is placed in the nitrogen atmosphere of an air pressure and is heated to 830 ℃ from room temperature, the heat treatment that maintenance was carried out in the hydrogen atmosphere in 1 hour under 830 ℃ is then at 830 ℃, vacuum degree reaches 1 * 10 -1Carry out dehydrogenation under the condition below the Torr and handle, feed argon gas thereafter immediately and carry out chilling.After such hydrogen disposes, under vacuum, 630 ℃ condition, carry out two hours heat treatment.
Resulting raw alloy is ground gently with mortar, and obtaining particle mean size is the R-Fe-Co-B series permanent magnet powder of 40 μ m.
These R-Fe-Co-B series permanent magnet powders being pressed into certain shape in the magnetic field of 25KOe, making the press-powder base, is that 720 ℃, pressure are 1.5Ton/cm with these press-powder bases in temperature 2Condition under carry out hot pressing or be that 710 ℃, pressure are 1.5Ton/cm in temperature 2Condition under carry out hot hydrostatic pressing (HIP), heat-treat separately again, just under 620 ℃, vacuum condition, kept two hours, make the sintered magnet 1-45 of the present invention and the sintered magnet 1-14 of usefulness relatively therefrom.In addition, the press-powder base that is shaped in magnetic field carries out hot pressing by the consistent setting of pressing direction of orientation direction during with hot pressing.The sintered magnet 1-25 of the invention described above and relatively the sintered magnet 1-7 of usefulness make by above-mentioned pressure sintering, described sintered magnet 26-45 of the present invention and relatively the sintered magnet 8-14 of usefulness make by above-mentioned HIP method.Also have, all abundant densification of density turns to 7.5～7.6g/cm 3
In order to compare, the R-Fe-Co-B series permanent magnet powder that the alloy cast ingot that does not contain any element among Ti, V, Nb, Ta, Al and the Si is made is filled in the copper jar under vacuum, is heated to 720 ℃, carries out rolling several times, make the calendering rate reach 80%, make existing anisotropy magnet.
The anisotropy magnet 1-45 of the present invention that makes like this, relatively the anisotropy magnet 1-14 of usefulness and the constituent of existing anisotropy magnet are shown among the table 1-6, in addition, the ratio of maximum particle diameter/minimum grain size of also having measured average crystal grain particle diameter, each crystal grain of these anisotropy magnets carries out the magnetic characteristic of hot pressing or the R-Fe-Co-B anisotropic magnet that HIP obtained less than content (volume %), the coercitive temperature coefficient aiHc of the crystal grain of 2 shape and the press-powder base that obtains be pressed into shape in magnetic field, and these measured values are shown among the table 7-11.
Above-mentioned coercitive temperature coefficient aiHc is the coercive force iHc when measuring 25 ℃ 25Coercive force iHc when reaching 100 ℃ 100, get the ratio (iHc of its difference 100-iHc 25)/iHc 25, again divided by 75 ℃ of resulting values of temperature difference.
Figure 921011857_IMG4
Figure 921011857_IMG5
Figure 921011857_IMG6
Figure 921011857_IMG8
Figure 921011857_IMG9
Figure 921011857_IMG11
From table 1-11 as can be seen, the anisotropy magnet 1-45 of the present invention that contains one or more elements among Ti, V, Nb, Ta, Al and the Si, with do not contain existing anisotropy magnet these elements, that belong to rolling magnet fully and compare, magnetic characteristic is identical substantially, but coercitive temperature coefficient is especially little, also have, the amount of Ti, V, Nb, Ta, Al, Si depart from condition of the present invention, the anisotropy magnet 1-14 of usefulness relatively, its magnetic anisotropy is low, and the size and dimension of crystal grain is very big to the influence of magnetic characteristic.
One or more elements that the present invention owing to adopted also contains except that Co among Ti, V, Nb, Ta, Al and the Si are through the powder of hydrogen processing, thereby need be through thermoplasticity processing, just can obtain anisotropy R-Fe-Co-B series significant, that coercitive temperature coefficient is little simultaneously magnet, performance and the stability that improves electrically powered machines such as motor brought excellent effect.

Claims (3)

1, a kind of is the R-Fe-Co-B anisotropic magnet of principal component with at least a element in the rare earth element that comprises Y (following represent with R), Fe, Co and B, it is characterized in that the composition of this anisotropy magnet is (in an atomic percent):
R：10～20%、
Co：0.1～50%、
B：3～20%、
One or more elements among Ti, V, Nb, Ta, Al and the Si, its total content is: 0.001～5.0%,
Remaining is Fe and unavoidable impurities;
This R-Fe-Co-B anisotropic magnet has the R with square crystal structure 2(Fe, Co) 14The Type B intermetallic compound is gathered the crystal grain collecting structure that forms for the crystal grain of principal phase mutually;
In described crystal grain collecting structure, more than 50% (volume) of the ratio b/a that is shaped as the maximum particle diameter b of single crystal grain and minimum grain size a less than 2 whole crystal grain of grains constitute, and the average crystal grain grain size that constitutes the crystal grain of above-mentioned crystal grain collecting structure is 0.05～20 μ m, and this R-Fe-Co-B anisotropic magnet is hot-press forming body or hot hydrostatic pressing formed body.
2, R-Fe-Co-B anisotropic magnet according to claim 1 is characterized in that, the described crystal grain collecting structure of crystal grain of having gathered is in fact only by R 2(Fe, Co) 14The Type B intermetallic compound constitutes mutually.
3, R-Fe-Co-B anisotropic magnet according to claim 1 and 2 is characterized in that, described average crystal grain particle diameter is 0.05～3 μ m.
CN 92101185 1991-02-01 1992-02-01 Terres rares-iron-cobalt-B anisotropic magnet Pending CN1065152A (en)

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JP06086091A JP3196224B2 (en) 1991-02-01 1991-02-01 Rare earth-Fe-Co-B anisotropic magnet
JP60860/91 1991-02-01

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1061162C (en) * 1992-11-20 2001-01-24 通用汽车公司 Hot-pressed magnets formed from anisotropic powders

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US5474623A (en) * 1993-05-28 1995-12-12 Rhone-Poulenc Inc. Magnetically anisotropic spherical powder and method of making same
EP2043114B1 (en) 2006-11-30 2019-01-02 Hitachi Metals, Ltd. R-fe-b microcrystalline high-density magnet and process for production thereof
JP6198103B2 (en) * 2013-02-22 2017-09-20 日立金属株式会社 Manufacturing method of RTB-based permanent magnet
CN111681868B (en) * 2020-07-09 2022-08-16 福建省长汀金龙稀土有限公司 Method for treating neodymium iron boron alloy sheet after smelting

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JPS61139638A (en) * 1984-12-10 1986-06-26 Sumitomo Special Metals Co Ltd Manufacture of sintered permanent magnet material
JPS63282239A (en) * 1987-05-13 1988-11-18 Hitachi Metals Ltd Permanent magnet alloy
JPH02263404A (en) * 1989-04-04 1990-10-26 Hitachi Metals Ltd Rare earth group iron base permanent magnet

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1061162C (en) * 1992-11-20 2001-01-24 通用汽车公司 Hot-pressed magnets formed from anisotropic powders

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