EP0018942B1 - Duktile magnetische Legierungen, Verfahren zu ihrer Herstellung und Magnet - Google Patents

Duktile magnetische Legierungen, Verfahren zu ihrer Herstellung und Magnet Download PDF

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Publication number
EP0018942B1
EP0018942B1 EP19800810124 EP80810124A EP0018942B1 EP 0018942 B1 EP0018942 B1 EP 0018942B1 EP 19800810124 EP19800810124 EP 19800810124 EP 80810124 A EP80810124 A EP 80810124A EP 0018942 B1 EP0018942 B1 EP 0018942B1
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EP
European Patent Office
Prior art keywords
alloy
magnetic
ductile
chromium
phase
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EP19800810124
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English (en)
French (fr)
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EP0018942A1 (de
Inventor
Wilfried Kurz
Remi Glardon
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Comadur SA
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Les Fabriques dAssortiments Reunies SA FAR
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Priority claimed from US06/029,477 external-priority patent/US4279668A/en
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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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C19/00—Alloys based on nickel or cobalt
    • C22C19/07—Alloys based on nickel or cobalt based on cobalt

Definitions

  • the present invention relates to magnetic alloys and to a method of making same.
  • the invention relates to ternary magnetic alloys of the type consisting of rare-earth or rare-earth-like elements, cobalt and at least one metal selected from the group which consists of iron, nickel, aluminium, chromium, copper, molybdenum or manganese, which are adapted for realizing permanent magnets of improved mechanical properties, such as ductility and toughness in use or fabrication.
  • Ferromagnetic alloys of the cobalt/rare-earth type have a high energy product and for this reason have been widely used. At present they are generally fabricated by powder metallurgy, i.e. by sintering, high-pressure pressing or the like techniques.
  • the alloys generally have the formula TRCoy, where TR is a rare-earth element such as samarium (Sm), gadolinium (Gd), praseodymium (Pr), cerium (Ce), neodymium (Nd), holmium (Ho) or an element similar to a rare-earth such as lanthanum (La) or yttrium (Y) or a mixture of such elements, y varies between 5 and 8.5.
  • TR is a rare-earth element such as samarium (Sm), gadolinium (Gd), praseodymium (Pr), cerium (Ce), neodymium (Nd), holmium (Ho) or an element similar to a rare-earth such as lanthanum (La) or yttrium (Y) or a mixture of such elements, y varies between 5 and 8.5.
  • Alloys containing copper as well as TRcy which are prepared by casting have also been proposed heretofore. These alloys are subjected to a magnetic hardening treatment but are also found to be very brittle and difficult to work, particularly by turning and similar machining operations.
  • Swiss Patent Nr. 601 481 discloses magnetic alloys having the formula TR (CO,X)y wherein X is at least one metal selected from the groups comprising iron, nickel, copper, aluminium, molybdenum and manganese.
  • TR is present in an amount of 5 to 22,5% (atomic) of the alloy, X varies between 5 and 65% (atomic) of the alloy and y lies between 3,5 and 10.
  • ductile fibres were obtained by an appropriate choice of composition together with the fabrication method using directed or directional solidification.
  • Another object of the invention is to provide magnets which are readily machined and yet retain the high magnetic-energy product B x H characteristic of rare-earth/cobalt magnets.
  • a metallic alloy for making ductile permanent magnet by directional solidification has a ductile phase composed essentially of Co in combination with chromium or iron plus chromium, which is dispersed in a magnetic matrix whose composition lies between TR (Co,X) 5 and TR z (Co,X) 17 , the alloy consisting essentially of TR, cobalt and X, where TR is at least one element selected from the group which consists of samarium, gadolinium praseodymium, cerium, neodymium, holmium, lanthanum and yttrium, X is at least,, one metal selected from the group comprising copper, iron, nickel, chromium, aluminium, molybdenum and manganese, TR is present in an amount of 10 to 15 at.% of the alloy, X is present in an amount of 10 to 40 at.% of the ally and cobalt is present in an amount of 50 to 80 at.% of the alloy.
  • TR is at least one element selected
  • X includes iron and/or chromium in an amount of 0.1 to 10% (atomic) of the alloy with 0,1 to 5% (atomic) chromium in any event and most advantageously, chromium in an amount of 0,5 to 5% (atomic) of the alloy (inclusive).
  • the ternary composition is a composition represented by the shaded region A, B, C, D of Fig. 5.
  • the magnetic properties cited hereunder are the saturation magnetization (M s ) and the coercive force (He),
  • Iron which also is included in component X also has a similar effect, but not so pronounced as Cr.
  • Useful magnets can however be made especially well when the Cr additions are made to alloy compositions already containing a certain proportion of Fe.
  • the reasons for the effectiveness of Cr as a dendrite former in these materials can be partially explained by the results obtained by microprobe analysis for the compositions of the phases present: the Cr appears to be preferentially incorporated into the ductile dendrite phase, leaving relatively little in the matrix phases to interfere with their (magnetic) hardenability.
  • the Fe is similarly distributed preferentially into the ductile dendrites, though the effect is less pronounced as can be seen in Table 1.
  • the quantities of Cr required depend on the proportions of the components TR and X relative to the Co content as can be seen from the examples in Table 2 together with an indication of the magnetic hardening which can be achieved.
  • the incorporation of the Cr into the dendrite phase in the form of a solid solution does not markedly affect the ductility of the phase, although the magnetic saturation can be substantially modified; Fe additions increasing the value, and Cr additions strongly reducing it.
  • the dendrites do not seem to have a major effect on the magnetic properties of the bulk material. They do however have secondary effects by reducing squarences of the hysteresis loop. The reduction of M s of the dendrites due to the Cr is therefore an advantage as the loop squareness is less deformed.
  • Magnetic properties of the matrix phases are also affected by the addition of Cr but the effects are only small as relatively little Cr is incorporated into the matrix phases.
  • the value of M S is slightly reduced, but most importantly there is very little effect on the hardenability (H c ) as compared with that obtained in the Sm-Co-Cu materials without the dendrites. At the Cr concentration levels required to form the dendrites, the reactions responsible for the magnetic hardening appear undisturbed.
  • the alloy composition could be adjusted such that no TR(Co,X) 5 compound is formed, the magnet then consisting only of ductule Co dendrites and the TR 2 (Co,X) 17 phase.
  • TR(Co,X) 5 type phase is of considerable aid, and that the composition is advantageously adjusted such that approximately 5-30% of the magnet consists of this phase. (The proportion is for the finished material, after heat-treatment; before heat treatment the volume fraction of this phase is rather higher).
  • the ordinate in fig. 1 represents the temperature T while the abscissa shows the content in atomic percent of TR, the vertical lines 1, 2 and 3 indicating respectively the compositions within the ambit of the present invention.
  • X may be one or more metals selected from the group which consists of irori, nickel, aluminium, chromium, copper, molybdenum and manganese.
  • the alloy should contain 0.1 to 10% (atomic) iron and/or chromium with 0.1 to 5% (atomic) chromium present in any event.
  • the most preferred composition contains 0.5% to 5% and more advantageously 1 to 5% chromium (atomic).
  • An alloy is solidified along the line y (Fig. 1).
  • T represents the temperature and is plotted along the ordinate while the TR content, in atomic percent is plotted along the abscissa.
  • the lines 1, 2 and 3 represent the compound TR 2 (Co,X), 7' TR(Co,X) s and TR 2 (Co,X) 7 .
  • Ductile dendrites 32 (fig. 3) are obtained in the magnetic matrix 31 from the system of fig. 1.
  • the solidification front 33 separates the liquid phase 34 from the solid phase 35.
  • the interfaces are shown at 36 and the distance between the dendritic fibers 37 is larger than in the previous case, e.g. about 50 microns.
  • the fiber length may exceed 100 microns and the diameter of the fibers may be 25 to 30 microns on the average.
  • a molten alloy of the composition y (fig. 2) will cool along the arrow to give a eutectic mixture of the matrix of TR 2 (C O ,X), 7 and fibers or lamellae of another phase such as (Co,X).
  • X represents an element which can be substituted for cobalt such as iron, nickel, aluminium, copper, chromium, molybdenum and manganese for a mixture thereof such as iron and chromium with copper, or copper plus nickel, for example.
  • ductile fibers 11 (fig. 4) in a magnetic matrix 12 are obtained.
  • the solidification front 13 separates the liquid phase 14 from the solidifying phase 15.
  • At 16 are shown the various interfaces between the two phases.
  • 17 represents the distance between the ductile fibers which can vary between 1 and 10 microns according to the speed of solidification.
  • the fiber length is a multiple of a distance between the fibers and the fibers may extend continuously throughout the body or in length upward of 100 microns.
  • a brittle body can be made tougher according to the invention, by the introduction of a second ductile phase, with its associated interphase boundaries in the material.
  • a composite body formed of two brittle phases is tougher than either of the phases taken alone and the mechanical properties of the composite body containing the two phases are improved. Even better properties can be obtained when one of the phases is a ductile phase which is associated with the brittle phase.
  • the workability of the body is improved by the double effect of the presence of a ductile phase and the existence of phase interfaces.
  • the mechanical and particularly the magnetic properties of the alloy according to the invention can be improved by controlling the solidification to give an oriental structure as described.
  • a directional-solidification furnace as described in U.S. patent 3,871,335 issued 13 March 1975 can be used to achieve this process.
  • Such a directional-solidification furnace may include a crucible which is moved at a predetermined speed relative to the heating elements just allowing the solidification conditions, the liquidus/solidus interface temperature gradient, solidification speed and the like to be established as is necessary to ensure the growth of the fiber phase.
  • the orientation is primarily important for obtaining the optimum magnetic properties.
  • Magnetic hardening in all cases is obtained by provoking precipitation as is conventional in the art.
  • the magnetic hardening can be carried out by subjecting the cast body to a solution treatment at a temperature above 900°C followed by precipitation by example at 400° to 700°C for one to two hours.
  • a similar improvement in the mechanical properties and magnetic properties of a body can be obtained by casting the alloy in a mold which is cooled at the base, thereby carrying out directed solidification.
  • a structure similar to that in fig. 4 is obtained although the fibers may be partly or completely in cellular or dendritic form.
  • the alloys shown in fig. 1, e.g. of composition y a structure similar to that shown in fig. 3, although the dendrites may have secondary branches, is formed.
  • composition range in which magnetic alloys may be prepared according to the invention are represented by the shaded region A, B, C, D of fig. 5, the presence of the ductile dendrites depending on the detailed choice of the mixture for TR and X.
  • the cobalt content is plotted along the lower axis in atomic percent
  • the TR content is plotted along the right hand axis in atomic percent
  • the replacement metal X is plotted along the left hand axis in atomic percent.
  • the shaded region ABCD of the diagram represents compositions of magnetic alloys with between 10 and 40 at.% of the element X, where X is one or more of the elements iron, nickel, aluminium, copper, chromium, molybdenum and manganese.
  • TR is present in an amount of 10 to 15 atomic percent of the alloy
  • X constitutes 10 to 40 atomic percent of the alloy and cobalt 50 to 80 atomic percent of the alloy.
  • composition ranges have TR con- situted by Sm or Sm mixed with up to 40% of Pr or Ce.
  • X is preferably a mixture of Cu, or Cu and Ni, together with Cr or Cr + Fe. Examples of such composi-tions are shown in tables 1 through 3.
  • the advantages of the magnets according to the present invention are numerous. They have high magnetic properties (BH max>10 MGOe, table 3) which are stable over long periods and under various environmental conditions. Their mechanical properties are superior to those of TR-cobalt magnets as are presently available, particularly with respect to their ability to be machined as proven by comparative tests. They can be machined by chip-removal methods, thereby allowing magnets of a wide range of shapes and sizes to be fabricated. They can be readily ground and hence given precision dimensions. Their toughness in use if superior to commercial TR-cobalt magnets. Finally, it is possible to cast large pieces by the methods described above, since the improvement of the mechanical properties of the pieces allows them to be better able to resist the thermal stresses occurring on cooling.
  • the ductile phase is composed essentially of cobalt and chromium or chromium + iron and the composition of the magnetic matrix is represented between TR(Co,X) s to TR 2 (Co,X) 17 .
  • Fig. 6 shows, in photomicrograph form the composite of the present invention in which the ductile cobalt dendrites can readily be distinguished from the brittle magnetic matrix.
  • Figs. 9 and 10 give the test results for these two alloys, showing the remarkable improvement resulting from the presence of the cobalt ductile dendrites. All of the compositions given have good magnetic properties as well.
  • the test method was a three-point bend test effected on a notched square-section bar, in which the fracture surface is triangular as defined by the notches.
  • Fig. 9 is a test diagram on an alloy with ductile dendrites showing the charge (c) applied to the bar versus the displacement (d).
  • Fig. 10 is a similar test diagram for an alloy without ductile dendrites.
  • the directionally solidified body has the same values for 4 7 r M s and Br of - 7.5 kGs.
  • the same body reduced to powder has the same value for Br but the values for 4 7 r M s in the first quadrant of the hysteresis loop are increased to - 9.0 kGs and in the second (technically important) quadrant, reduced by a similar amount due to the effect of the dendrites (see b. fig 11)

Claims (7)

1. Magnetische Legierung für einen duktilen Permanentmagneten, umfassend eine duktile Phase aus einer zellularen oder dendritischen Struktur, die im wesentlichen aus Kobalt in einer magnetischen Matrix besteht, deren Zusammensetzung zwischen TR(Co,X)5 und TR2(CO,X)17 liegt, wobei die Legierung im wesentlichen aus TR, Kobalt und X besteht, worin TR mindestens ein Element ist ausgewählt aus der Gruppe, die aus Samarium, Gadolinium, Praseodym, Cer, Neodym, Holmium, Lanthan und Yttrium besteht, X mindestens ein Metall ist, ausgewählt aus der Gruppe, die aus Kupfer, Eisen, Nickel und Aluminium, Molybdän und Mangan besteht, wobei TR in einer Menge von 10 bis 15 At.-Gew.-% der Legierung vorliegt, X in einer Menge von 10 bis 40 At.-Gew.-% und Kobalt in einer Menge von 50 bis 80 At.-Gew.-% der Legierung vorliegen, dadurch gekennzeichnet, daß X Eisen und/oder Chrom in einer Menge von 0,1 bis 10% (atomar) der Legierung umfaßt, mit in jedem Falle 0,1 bis 5% (atomar) Chrom.
2. Legierung nach Anspruch 1, dadurch gekennzeichnet, daß X 0,5 bis 5 At.-Gew.-% Chrom enthält.
3. Legierung nach Anspruch 1, dadurch gekennzeichnet, daß TR im wesentlichen Samarium gemischt mit bis zu 50 At.-Gew.-% des gesamten TR von anderen Elementen vom Typ seltener Erden ist.
4. Legierung nach Anspruch 1, dadurch gekennzeichnet, daß X im wesentlichen aus Kupfer ist mit bis zu 50At.-Gew.-% des gesamten X.
5. Verfahren zum Herstellen einer duktilen magnetischen Legierung nach einem der Ansprüche 1 bis 4, gekennzeichnet durch die Schritte:
-Aufschmelzen eines Gemisches im wesentlichen der Elemente Co, X, TR;
-Abkühlen der Schmelze durch Steuern des Temperaturgradienten in der Flüssigphase und der Aufwachsrate des Solidus derart, daß nach der Verfestigung die Orientierung der leichten Magnetisierung der meisten TR-Co-Körner im wesentlichen parallel ist;
- Steuerung des Temperaturgradienten in der Flüssigphase und der Aufwachsrate des Solidus während des Abkühlschrittes derart, daß die Bildung einer feinen und gleichförmigen Verteilung einer duktilen Phase zellularer oder dendritischer Struktur innerhalb einer magnetischen Matrix sichergestellt wird, deren Zusammensetzung zwischen TR(Co,X)5 und TR2(Co,X)17 liegt; und
- Erhitzen der verfestigten Legierung zwecks magnetischer Härtung der TR-Co-Körner.
6. Körper aus magnetischer Legierung, hergestellt durch das Verfahren nach Anspruch 5, bestehend aus einer duktilen Phase in einer magnetischen Matrix, wobei die duktile Phase Co umfaßt, die magnetische Matrix vom Typ seltene-Erde-Kobalt ist und der Körper ein Energieprodukt von mindestens 6 M G Oe und eine mechanische Reißenergie von zumindest 40 Joule/m2 aufweist.
7. Körper nach Anspruch 6, dadurch gekennzeichnet, daß er ein Energieprodukt von mindestens 10 M G Oe besitzt.
EP19800810124 1979-04-12 1980-04-11 Duktile magnetische Legierungen, Verfahren zu ihrer Herstellung und Magnet Expired EP0018942B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US06/029,477 US4279668A (en) 1975-05-05 1979-04-12 Directionally solidified ductile magnetic alloy
US29477 1979-04-12

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EP0018942A1 EP0018942A1 (de) 1980-11-12
EP0018942B1 true EP0018942B1 (de) 1984-07-04

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JPS60170127U (ja) * 1984-04-23 1985-11-11 服部　良助 ブラシ
JPS60170126U (ja) * 1984-04-23 1985-11-11 服部　良助 ブラシ
GB8605878D0 (en) * 1986-03-10 1986-04-16 Johnson Matthey Plc Casting transition metal alloy
JPS6410227U (de) * 1987-07-09 1989-01-19
KR101829292B1 (ko) * 2009-07-20 2018-03-29 보르그워너 인코퍼레이티드 터보차저 및 이를 위한 압축기 휠
US20140334968A1 (en) * 2011-11-18 2014-11-13 Tubitak Alloy for high temperature tooling applications

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* Cited by examiner, † Cited by third party
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FR1604641A (de) * 1967-11-15 1972-01-03
NL6816387A (de) * 1968-11-16 1970-05-20
CH519770A (de) * 1970-01-09 1972-02-29 Bbc Brown Boveri & Cie Verfahren zur Herstellung eines Dauermagneten
CH532126A (fr) * 1970-09-08 1972-12-31 Battelle Memorial Institute Procédé de fabrication d'un matériau pour aimants permanents et matériau obtenu par ce procédé
US3947295A (en) * 1973-02-09 1976-03-30 Matsushita Electric Industrial Co., Ltd. Hard magnetic material
CH607254A5 (de) * 1974-07-31 1978-11-30 Bbc Brown Boveri & Cie
CH601484A5 (de) * 1974-12-18 1978-07-14 Bbc Brown Boveri & Cie
CH601481A5 (de) * 1975-05-05 1978-07-14 Far Fab Assortiments Reunies
CH603802A5 (de) * 1975-12-02 1978-08-31 Bbc Brown Boveri & Cie
JPS52155124A (en) * 1976-06-18 1977-12-23 Hitachi Metals Ltd Permanent magnetic alloy

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EP0018942A1 (de) 1980-11-12
JPS5613454A (en) 1981-02-09
DE3068420D1 (en) 1984-08-09

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