EP0522177B2 - Aimant ayant des propriétés anisotropiques à base de terres rares - Google Patents

Aimant ayant des propriétés anisotropiques à base de terres rares Download PDF

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Publication number
EP0522177B2
EP0522177B2 EP92903728A EP92903728A EP0522177B2 EP 0522177 B2 EP0522177 B2 EP 0522177B2 EP 92903728 A EP92903728 A EP 92903728A EP 92903728 A EP92903728 A EP 92903728A EP 0522177 B2 EP0522177 B2 EP 0522177B2
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grains
crystallised
atmosphere
atomic
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German (de)
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EP0522177A4 (en
EP0522177A1 (fr
EP0522177B1 (fr
Inventor
Takuo Chuo-Kenkyusho Takeshita
Ryoji Chuo-Kenkyusho Nakayama
Yoshinari Chuo-Kenkyusho Ishii
Tamotsu Chuo-Kenkyusho Ogawa
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Diamet Corp
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Mitsubishi Materials Corp
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Priority claimed from JP3060828A external-priority patent/JP2773444B2/ja
Priority claimed from JP03060833A external-priority patent/JP3092672B2/ja
Priority claimed from JP03060837A external-priority patent/JP3092673B2/ja
Priority claimed from JP06086091A external-priority patent/JP3196224B2/ja
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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
    • H01F1/0575—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
    • H01F1/0573—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

Definitions

  • the present invention relates to a R (where R represents at least one type of rare earth element including Y)-Fe-Co-B system anisotropic magnet possessing superior magnetic anisotropy and a small coercive force temperature coefficient, and relates more particularly to an anisotropic magnet comprising a hot press molded body or a hot isostatic press molded body.
  • the above R-Fe-B system permanent magnetic powder utilizes R-Fe-B system mother alloy as a raw material for the main phase of a R 2 Fe 14 B type intermetallic compound phase (hereinbelow termed the "R 2 Fe 14 B type phase”) which is a ferromagnetic phase; after the heat treatment of this mother alloy raw material in a H 2 atmosphere within a specified temperature range and the fostering of a phase-changed state in each of the RH x , Fe 2 B, and the remaining Fe phases, the H 2 is removed from the raw material by means of an H 2 -desorption process, and the R 2 Fe 14 B type phase, which is the ferromagnetic phase, is recreated; the R 2 Fe 14 B system permanent magnetic powder obtained as a result has an aggregate structure such that the main phase thereof is an extremely fine R 2 Fe 14 B type phase having a recrystallized structure and an average grain diameter of 0.05 - 3 ⁇ m.
  • the above R-Fe-Co-B system permanent magnetic powder uses R-Fe-Co-B system mother alloy having as a main phase thereof R 2 (Fe, Co) 14 B type intermetallic compound (hereinbelow termed R 2 (Fe, Co) 14 B type phase), which is a ferromagnetic phase, as a raw material thereof, and this is processed in a manner identical to the case of the above R-Fe-B system; this has an aggregate structure having as a main phase thereof an extremely fine R 2 (Fe, Co) 14 B type phase with a recrystallized structure and an average grain diameter of 0.05 - 3 ⁇ m.
  • R 2 (Fe, Co) 14 B type phase R 2 (Fe, Co) 14 B type phase
  • EP-A-0 274 034 discloses magnetically anisotropic magnetic powders including R-Fe-B-Ga alloys which may optionally contain further elements such as V, Si and Al.
  • the process of manufacturing these powders comprises inter alia the steps of hot pressing and plastic working of the material.
  • EP-A-0 304 054 discloses a process for producing a rare earth-iron-boron alloy magnet powder comprising the steps of:
  • the above R-Fe-B system and R-Fe-Co-B system permanent magnetic powders are unable to achieve sufficient magnetic anisotropy simply as a result of being formed as hot press molded bodies, so that, as disclosed in Japanese Patent Application, First Publication, Laid-Open No. Hei 2-39503, by carrying out a hot rolling process such as hot rolling or the like on the above hot press molded bodies and thus creating a rolled structure, the C axes of the crystal grains of the R 2 Fe 14 B phase or the R 2 (Fe, Co) 14 B type phase are oriented, and the magnetic anisotropy thereof is increased.
  • R-Fe-B system and R-Fe-Co-B system rolled magnets obtained by the further hot rolling of a hot press molded body possess superior magnetic anisotropy; but in comparison with magnets which are produced by the hot pressing of the above R-Fe-B system and R-Fe-Co-B system permanent magnetic powders obtained by means of hydrogen treatment, the temperature coefficient of the coercive force increases in an undesirable manner, and in the case in which such a rolled magnet is incorporated in a motor or the like, the performance of such a motor or the like varies based on temperature, and there is a problem in that the stability thereof is lacking.
  • the first anisotropic magnet prepared in accordance with the present invention is prepared by a first method as defined by Claim 1.
  • This first anisotropic magnet has a temperature coefficient of the coercive force which is small, and in comparison with the conventional rolled magnets, has almost no localized variations in magnetic anisotropy and also possesses superior resistance to corrosion. Furthermore, as the magnet has crystallized grain aggregate structure, it has superior magnetic anisotropy and a high coercive force in the vicinity of a R 2 (Fe, Co) 14 B type compound composition, that is to say, in the vicinity of a R 11.8 (Fe, Co) bal B 5.9 (atomic %) composition.
  • this first R-Fe-Co-B system anisotropic magnet first, a R-Fe-Co-B system mother alloy having a fixed component composition possessing Ga, Zr, and Hf, or a R-Fe-Co-B system mother alloy having a fixed component composition in which Al, V, and Si are added to the above alloy, is manufactured.
  • this R-Fe-Co-B system mother alloy is heated in an atmosphere of hydrogen gas, is subjected to heat treatment at a temperature of 500 - 1000°C in an atmosphere of hydrogen gas or a mixed atmosphere of hydrogen gas and an inert gas, and then hydrogen removal processing is carried out at a temperature of 500 - 1000°C so as to produce a vacuum atmosphere having a hydrogen gas pressure of less than 1 Torr or an inert gas atmosphere in which the partial pressure of hydrogen gas is less than 1 Torr, and by cooling this, a R-Fe-Co-B system permanent magnetic powder is obtained.
  • the structure of the R-Fe-Co-B system permanent magnetic powder produced in the above manner comprises a recrystallized aggregate structure in which R 2 (Fe, Co) 14 B type intermetallic compound phase recrystallized grains, which are free of impurities or strains within the grains or at the grain boundaries, are aggregated.
  • the average recrystallized grain diameter of the recrystallized grains comprising this recrystallized aggregate structure is sufficiently within a range of 0.05 - 20 ⁇ m; however, a range of 0.05 - 3 ⁇ m, which is dose to the dimensions of a single magnetic domain grain diameter (approximately 0.3 ⁇ m), is more preferable.
  • the individual recrystallized grains having the above dimensions have a form such that the value of the ratio b/a of the smallest grain diameter a and the largest grain diameter b be less than 2; it is necessary that recrystallized grains having this form be present in an amount of more than 50 volume % of the total recrystallized grains comprising the structure of the individual powders.
  • the coercive force of the R-Fe-Co-B system permanent magnetic powder is improved, and the coercive force temperature coefficient ⁇ iHc in the temperature range of 25°C - 100°C becomes smaller than 0.6%/°C.
  • the recrystallized structure of the R-Fe-Co-B system permanent magnetic powder produced in this manner has a recrystallised aggregate structure comprising materially only R 2 (Fe, Co) 14 B type intermetallic compound phase in which a grain boundary phase is almost nonexistent, it is possible to raise the magnetization values of only the portion having no grain boundary phase, corrosion proceeding along the grain boundary phase is halted, and furthermore, as stress deformation resulting from thermoplastic processes does not exists, the likelihood of stress corrosion is small, and the resistance to corrosion thus increases.
  • the R-Fe-Co-B system permanent magnetic powder above is pressed to a green compact in a magnetic field, and by subjecting this green compact to hot pressing or a HIP process at a temperature of 600°C - 900°C, it is possible to produce a R-Fe-Co-B system anisotropic magnet which preserves the superior characteristics of the R-Fe-Co-B system permanent magnetic powder above. Furthermore, by conducting heat processing at 300°C - 1000°C where necessary, it is possible to increase the coercive force.
  • the green compact above is sintered by a conventional method, as the sintering temperature is normally high, the fine recrystallized grains of the R-Fe-Co-B system permanent magnetic powder grow into large crystallized grains, and as the magnetic characteristics, and particularly the coercive force, worsen, this is not preferable. Furthermore, as the imparting of magnetic anisotropy is conducted in a magnetic field, it is not necessary to conduct a thermoplastic process after hot pressing or the HIP process.
  • the amount of Co contained by adding Co to the composition of the anisotropic magnet, the coercive force and magnetic temperature characteristics (for example, the Curie point) of the anisotropic magnet are improved, and moreover, the effect of an increase in the resistance to corrosion is obtained; however, when the amount contained thereof is less than 0.1 atomic %, these effects cannot be obtained, while on the other hand, when the amount exceeds 50 atomic %, the magnetic characteristics worsen, so that this is not preferable. Accordingly, the amount of Co contained is set to a range of 0.1 - 50 atomic %. When the amount of Co contained is in a range of 0.1 - 20 atomic %, the coercive force increases to the greatest extent, so that it is most preferable to set the amount of Co contained to 0.1 - 20 atomic %.
  • the second anisotropic magnet in accordance with the present invention is a R-Fe-Co-B system anisotropic magnet as defined by Claim 3.
  • this second anisotropic magnet has a small coercive force temperature coefficient, has almost no localized variations in magnetic anisotropy in comparison with conventional rolled magnets, has superior corrosion resistance, and as this magnet possesses a crystallized grain aggregate structure, it has superior magnetic anisotropy and a high coercive force even in the vicinity of a R 2 (Fe, Co) 14 B type compound composition, that is to say, in the vicinity of a R 11.8 (Fe, Co) bal B 5.9 (atomic %) composition.
  • this second anisotropic magnet In order to produce this second anisotropic magnet, first, a R-Fe-Co-B system mother alloy having a fixed component composition containing one or a plurality of Ti, V, Nb, Ta, Al, and Si is subjected to melt casting, and using this as a raw material, it is acceptable to conduct processing which is identical to that in the case of the first anisotropic magnet above.
  • the effects of an increase in the coercive force and the stable imparting of superior magnetic anisotropy and resistance to corrosion can be obtained; however, when the total amount of these elements which is contained is less than 0.001 atomic %, the desired effects cannot be obtained, while on the other hand, when this amount exceeds 5.0 atomic %, the magnetic characteristics worsen. Accordingly, the total amount of one or a plurality of Ti, V, Nb, Ta, Al, and Si which is contained is set to a value in the range of 0.001 - 5.0 atomic %.
  • this second anisotropic magnet contains at least one of Ni, Cu, Zn, Ga, Ge, Zr, Mo, Hf, and W in an amount of 0.001 - 5.0 atomic %, it possesses superior magnetic anisotropy and resistance to corrosion.
  • first and second anisotropic magnets in accordance with the present invention were produced in the following manner, and the characteristics thereof were determined.
  • a first anisotropic magnet in accordance with the present invention was produced in the manner described hereinafter, and the characteristics thereof were determined.
  • the temperature of this raw material alloy was raised from room temperature to a temperature of 830°C in a hydrogen atmosphere at a pressure of 101 kPa (1 atmosphere), heat treatment was conducted in this hydrogen atmosphere at a temperature of 830°C for a period of 4 hours, and then, hydrogen was desorped at a temperature of 830°C so as to produce a vacuum degree of less than 13 Pa (1 X 10 -1 Torr), and directly thereafter, argon gas was introduced and rapid cooling conducted.
  • R-Fe-Co-B system permanent magnetic powders were press formed in a magnetic field so as to form green compacts, and these green compacts were subjected to hot pressing under conditions such that the temperature was 700°C and the pressure was 1.5 Ton/cm 2 . At this time, arrangement and hot pressing were conducted in such a manner that the orientation direction was identical with the press direction at the time of hot pressing.
  • the anisotropic magnets 79 - 109 of the present invention and the comparative anisotropic magnets 30 - 39 shown in Tables 20 - 23 were produced.
  • the densities of these anisotropic magnets were sufficiently accurate, being in a range of 7.5 to 7.6 g/cm 3 .
  • a R-Fe-Co-B system permanent magnetic powder produced from an ingot of an alloy containing no Ga, Zr, or Hf was placed in a copper can in a vacuum, this was heated to a temperature of 700°C and rolling was conducted a number of times so that the rolling ratio reached 80%, and the conventional anisotropic magnet 3 shown in Table 23 was obtained.
  • the various structures of the anisotropic magnets 79 - 109 of the present invention, the comparative anisotropic magnets 30 - 39, and the conventional anisotropic magnet 3 having the component compositions shown in Tables 20 - 22 were observed by means of a scanning electron microscope, and the average crystallized grain diameter, the amount of crystallized grains present having a form in which the ratio of the largest grain diameter / smallest grain diameter had a value of less than 2, the coercive force temperature coefficient ⁇ iHc and the magnetic characteristics were determined. The values obtained thereby are shown in Tables 24 - 27.
  • the method of calculation of the coercive force temperature coefficient ⁇ iHc is as given above.
  • the anisotropic magnets 79 - 109 In accordance with the present invention which contain one or a plurality of Ga, Zr, and Hf have superior magnetic characteristics, and in particular, have superior maximum energy product (BH) max and residual magnetic flux density Br, and furthermore, have superior anisotropy. Furthermore, in comparison with the conventional anisotropic magnet 3 obtained by means of rolling, the anisotropic magnet 79 - 109 of the present invention possess essentially identical magnetic characteristics; however, the coercive force temperature coefficient ⁇ iHc thereof is markedly smaller, having a value of approximately -0.5%/°C. In addition, in the case of the comparative anisotropic magnets 30 - 39, the compositions of which lie outside the ranges of the present invention, the magnetic characteristics and magnetic anisotropy worsen.
  • ingots of various alloys having component compositions containing one or a plurality of Al, V, and Si in addition to a R-Fe-Co-B system alloy containing one or a plurality of Ga, Zr, and Hf obtained by means of high frequency induction melting and casting were prepared; these ingots were processed by a method identical to that of the anisotropic magnets 79 - 109 and the comparative anisotropic magnets 30 - 39 above, and R-Fe-Co-B system permanent magnetic powders having a mean particle size of 40 ⁇ m were produced.
  • the average crystallized grain diameter, the amount (volume %) of crystallized grains present for which the value of the ratio of the largest grain diameter / smallest grain diameter was less than 2, the coercive force temperature coefficient ⁇ iHc and the magnetic characteristics of these anisotropic magnets were determined in a manner identical to that above. The results thereof are shown in Table 29.
  • the temperature of these raw material alloys was raised from room temperature to 830°C in an atmosphere of hydrogen gas at a pressure of 101 kPa (1 atmosphere), heat treatment was carried out in an atmosphere of hydrogen gas at a temperature of 830°C for a period of 1 hour, hydrogen was desorped at a temperature of 830°C in order to produce a vacuum degree of less than 13 Pa (1 X 10 -1 Torr), and immediately thereafter, argon gas was introduced and rapid cooling conducted. After the conclusion of this hydrogen treatment, heat processing was conducted in a vacuum at a temperature of 630°C for a period of 2 hours.
  • the raw material alloys thus obtained were slightly crushed in mortars, and magnetic powders having a mean particle size of 40 ⁇ m were obtained.
  • anisotropic magnets 120 - 164 of the present Invention and the comparative anisotropic magnets 43 - 56 which were produced in the above manner, anisotropic magnets 120 - 144 of the present invention and comparative anisotropic magnets 43 - 49 were produced by means of hot pressing, while anisotropic magnets 145 - 164 of the present invention and comparative anisotropic magnets 50 - 56 were produced by means of an HIP method. The density thereof was in all cases sufficiently accurate, being within a range of 7.5 - 7.6 g/cm 3 .
  • a R-Fe-Co-B system permanent magnetic powder produced from an ingot of an alloy containing no Ti, V, Nb, Ta, Al, or Si was placed in a copper can in a vacuum, this was heated to a temperature of 720°C, and rolling was conducted a number of times so that the rolling ratio reached a value of 80%, and thus a conventional anisotropic magnet 4 was obtained.
  • the component compositions of the anisotropic magnets 120 - 164 of the present invention, the comparative anisotropic magnets 43 - 56, and the conventional anisotropic magnet 4 obtained in the above manner are shown in Tables 30 - 35.
  • the average crystallized grain diameter, the amount (volume %) of crystallized grains present having a form in which the value of the ratio of the largest grain diameter / smallest grain diameter is less than 2 the magnetic characteristics, and the coercive force temperature coefficient ⁇ iHc of these anisotropic magnets were determined by a method identical to that given above, and the resulting values are shown in Tables 36 - 40.
  • the invention by means of using a hydrogen treated powder of a R-Fe-Co-B system containing one or a plurality of Ga, Zr, and Hf, or containing one or a plurality of Ti, V, Nb, Ta, Al, and Si, it is possible to obtain an anisotropic magnet for which the magnetic anisotropy is large, and moreover, the coercive force temperature coefficient is small, so that there is no need to conduct a magnetic anisotropizing process such as a thermoplastic process or the like, as in the conventional method, and production costs can be thereby reduced considerably. Accordingly, the invention contributes greatly to the ability to produce electronic machines such as motors and the like and to improvements in stability.

Claims (4)

  1. Une méthode afin de préparer un aimant anisotrope du système Terre Rare-Fe-Co-B qui est un corps moulé sous compression à chaud ou un corps moulé sous compression isostatique à chaud comprenant :
    un élément de terre rare incluant Y,
    B,
    0,001-5% d'atomes au total d'un ou de plusieurs de Ga, Zr et Hf, et
    0,1-50% d'atomes de Co ;
    avec le reste étant du Fe et des impuretés inévitables ; ledit corps ayant une structure d'agrégat de grains cristallisés comprenant, matériellement, seulement une phase d'un composé intermétallique du type R2(TM)14B avec une structure tétragonale, où R est au moins un élément des terres rares incluant Y, et TM est Fe et Co, les grains cristallisés ayant une dimension de 0,05-20 µm ; et le rapport entre le diamètre b le plus grand des grains et le diamètre a le plus petit des grains est inférieur à deux pour des grains individuels cristallisés constituant plus de 50 % en volume des grains cristallisés totaux de la structure d'agrégat,
       la méthode comprenant les étapes de :
    (i) chauffer un alliage mère R-Fe-Co-B incluant un ou plusieurs de Ga, Zr et Hf dans une atmosphère d'hydrogène gazeux incluant optionnellement un gaz inerte, à 500-1000 °C,
    (ii) enlever l'hydrogène de l'atmosphère à une température de 500-1000°C de manière à produire une atmosphère de vide ayant une pression d'hydrogène gazeux plus petite que 0,13 kPa (moins que 1 Torr) ou une atmosphère de gaz inerte dans laquelle la pression partielle d'hydrogène gazeux est plus petite que 0,13 kPa (moins que 1 Torr),
    (iii) refroidir l'alliage afin d'obtenir une poudre magnétique permanente d'un système R-Fe-Co-B ayant une structure d'agrégat recristallisée comprenant matériellement qu'une phase de composé intermétallique du type R2(Fe,Co)14B.
    (iv) presser la poudre magnétique en un comprimé vert dans un champs magnétique, et
    (v) soumettre le comprimé vert à un moulage sous presse chaude ou à un moulage sous presse isostatique chaude à une température de 600-900°C.
  2. Une méthode selon la revendication 1, dans laquelle l'aimant comprend un total de 0,01-2,0% d'atomes d'un ou d'une multitude de Al, V et Si.
  3. Une méthode afin de préparer un aimant anisotrope du système Terre Rare-Fe-Co-B qui est un corps moulé sous compression à chaud ou un corps moulé sous compression isostatique à chaud comprenant :
    un élément de terre rare incluant Y,
    B,
    0,001-5% d'atomes au total d'un ou de plusieurs de Ti, V, Nb, Ta, Al et Si et
    0,1-50% d'atomes de Co ;
    avec le reste étant du Fe et des impuretés inévitables ; ledit corps ayant une structure d'agrégat de grains cristallisés comprenant, matériellement, seulement une phase d'un composé intermétallique du type R2(TM)14B avec une structure tétragonale, où R est au moins un élément des terres rares incluant Y, et TM est Fe et Co, les grains cristallisés ayant une dimension de 0.05-20 µm ; et le rapport entre le diamètre b le plus grand des grains et le diamètre a le plus petit des grains est inférieur à deux pour des grains individuels cristallisés constituant plus de 50 % en volume des grains cristallisés totaux de la structure d'agrégat,
       la méthode comprenant les étapes de :
    (i) chauffer un alliage mère R-Fe-Co-B incluant un ou plusieurs de Ti, V, Nb, Ta, Al et Si dans une atmosphère d'hydrogène gazeux incluant optionnellement un gaz inerte, à 500-1000 °C,
    (ii) enlever l'hydrogène de l'atmosphère à une température de 500-1000°C de manière à produire une atmosphère de vide ayant une pression d'hydrogène gazeux plus petite que 0.13 kPa (moins que 1 Torr) ou une atmosphère de gaz inerte dans laquelle la pression partielle d'hydrogène gazeux est plus petite que 0.13 kPa (moins que 1 Torr),
    (iii) refroidir l'alliage afin d'obtenir une poudre magnétique permanente d'un système R-Fe-Co-B ayant une structure agrégée recristallisée comprenant matériellement qu'une phase de composé intermétallique du type R2(Fe,Co)14B.
    (iv) presser la poudre magnétique en un comprimé vert dans un champs magnétique, et
    (v) soumettre le comprimé vert à un moulage sous presse chaude ou à un moulage sous presse isostatique chaude à une température de 600-900°C.
  4. Une méthode selon n'importe laquelle des revendications précédentes, dans laquelle le diamètre moyen des grains cristallisés est 0.05-3 µm.
EP92903728A 1991-01-28 1992-01-28 Aimant ayant des propriétés anisotropiques à base de terres rares Expired - Lifetime EP0522177B2 (fr)

Applications Claiming Priority (13)

Application Number Priority Date Filing Date Title
JP3060828A JP2773444B2 (ja) 1991-01-28 1991-01-28 希土類−Ｆｅ−Ｂ系異方性磁石
JP60828/91 1991-01-28
JP6082891 1991-01-28
JP60833/91 1991-01-30
JP6083391 1991-01-30
JP03060833A JP3092672B2 (ja) 1991-01-30 1991-01-30 希土類−Ｆｅ−Ｃｏ−Ｂ系異方性磁石
JP60837/91 1991-01-31
JP6083791 1991-01-31
JP03060837A JP3092673B2 (ja) 1991-01-31 1991-01-31 希土類−Ｆｅ−Ｂ系異方性磁石
JP6086091 1991-02-01
JP60860/91 1991-02-01
JP06086091A JP3196224B2 (ja) 1991-02-01 1991-02-01 希土類−Ｆｅ−Ｃｏ−Ｂ系異方性磁石
PCT/JP1992/000073 WO1992013353A1 (fr) 1991-01-28 1992-01-28 Aimant a base de terres rares, de fer et de bore et a base de terres rares de fer, de cobalt et de bore ayant des proprietes anisotropes

Publications (4)

Publication Number Publication Date
EP0522177A1 EP0522177A1 (fr) 1993-01-13
EP0522177A4 EP0522177A4 (en) 1993-09-15
EP0522177B1 EP0522177B1 (fr) 1995-07-12
EP0522177B2 true EP0522177B2 (fr) 2003-07-30

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CA (1) CA2079223A1 (fr)
DE (1) DE69203405T3 (fr)
WO (1) WO1992013353A1 (fr)

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US5352301A (en) * 1992-11-20 1994-10-04 General Motors Corporation Hot pressed magnets formed from anisotropic powders

Family Cites Families (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA1316375C (fr) * 1982-08-21 1993-04-20 Masato Sagawa Materiaux magnetiques et aimants permanents
JPS61295342A (ja) * 1985-06-24 1986-12-26 Hitachi Metals Ltd 永久磁石合金の製造方法
JPS6217149A (ja) * 1985-07-16 1987-01-26 Sumitomo Special Metals Co Ltd 高性能焼結永久磁石材料の製造方法
JPS62202506A (ja) * 1985-11-21 1987-09-07 Tdk Corp 永久磁石およびその製法
JPS63178505A (ja) * 1987-01-20 1988-07-22 Hitachi Metals Ltd 異方性Ｒ−Ｆｅ−Ｂ−Ｍ系永久磁石
JPS63211705A (ja) * 1987-02-27 1988-09-02 Hitachi Metals Ltd 異方性永久磁石及びその製造方法
JPS63211706A (ja) * 1987-02-27 1988-09-02 Hitachi Metals Ltd ボンド磁石用磁粉の製造方法
JPS63235406A (ja) * 1987-03-24 1988-09-30 Daido Steel Co Ltd ラジアル異方性永久磁石の製造方法
CN1012477B (zh) * 1987-08-19 1991-05-01 三菱金属株式会社 稀土-铁-硼磁体粉末及其制备方法
JPH01257308A (ja) * 1987-09-09 1989-10-13 Hitachi Metals Ltd ボイスコイルモーター用磁石
JPH07105301B2 (ja) * 1987-09-10 1995-11-13 日立金属株式会社 磁気異方性Ｎｄ―Ｆｅ―Ｂ磁石材の製法
JP2803727B2 (ja) * 1987-09-14 1998-09-24 大同特殊鋼株式会社 永久磁石の製造方法
JPH02138706A (ja) * 1988-11-18 1990-05-28 Daido Steel Co Ltd 異方性永久磁石
JPH02263404A (ja) * 1989-04-04 1990-10-26 Hitachi Metals Ltd 希土類鉄系永久磁石

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CA2079223A1 (fr) 1992-07-29
EP0522177A4 (en) 1993-09-15
DE69203405T2 (de) 1996-02-15
EP0522177A1 (fr) 1993-01-13
WO1992013353A1 (fr) 1992-08-06
DE69203405D1 (de) 1995-08-17
DE69203405T3 (de) 2004-05-06
EP0522177B1 (fr) 1995-07-12

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