EP0003466B1 - Process for the thermal treatment of Fe-Co-Cr alloys for permanent magnets - Google Patents

Process for the thermal treatment of Fe-Co-Cr alloys for permanent magnets Download PDF

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EP0003466B1
EP0003466B1 EP79420003A EP79420003A EP0003466B1 EP 0003466 B1 EP0003466 B1 EP 0003466B1 EP 79420003 A EP79420003 A EP 79420003A EP 79420003 A EP79420003 A EP 79420003A EP 0003466 B1 EP0003466 B1 EP 0003466B1
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minutes
stage
annealing
temperature
treatment
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EP0003466A1 (en
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Claude Bronner
Daniel Jullien
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Aimants Ugimac SA
Ugimag SA
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Aimants Ugimac SA
Ugimag SA
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    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D6/00—Heat treatment of ferrous alloys
    • C21D6/002—Heat treatment of ferrous alloys containing Cr

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  • the present invention relates to a process for heat treatment of Fe-Co-Cr alloys intended for the manufacture of permanent magnets as well as the magnets produced by this process.
  • These alloys have for composition (by weight): optionally one or more of the elements AI, Nb, Ta, W, Mo, V, Ti, Si, Cu in a total amount of less than 10%, the rest being iron.
  • French Patent No. 2,149,076 describes certain alloys of this type as well as their heat treatments.
  • a first form is molded and subjected to a high temperature homogenization treatment between 1200 and 1400 ° C for more than 10 minutes, followed by rapid quenching to room temperature.
  • the molded body can undergo, without particular difficulty, various shaping operations such as rolling, drilling, machining, etc. to bring it to a shape close to the final shape.
  • the body is subjected to an isothermal annealing treatment in a magnetic field, at a temperature between 580 and 650 ° C (preferably 600 to 640 ° C) for a period of 10 minutes to 2 hours, but preferably from 1 'order of 30 minutes.
  • the part is subjected to one or more tempers at temperatures between 530 and 650 ° C for 1 to 9 h, these tempers can be done at decreasing stepped temperatures.
  • these different incomes tend to decrease the rectangularity of the hysteresis cycle measured by the ratio q between the specific energy (BH) max and the product Br Hc of the residual induction by the coercive field.
  • the object of the present invention is to avoid these drawbacks and to allow the manufacture of anisotropic permanent magnets of the Fe-Cr-Co type having a coefficient il of rectangularity of the hysteresis curve constant during the incomes and whose specific energy can exceed 40 kJ / m 3 (5.10 8 Gaus-Oersteds) without additional wrought operation and, therefore, without risk of rupture.
  • the duration of the first stage is short enough to avoid precipitation of the fragile u phase in the alloy.
  • the holding temperature during this first step is preferably between 640 and 660 ° C.
  • the tempering treatment is preferably carried out in three stages of increasing duration at decreasing staged temperatures of approximately 30 ° C. These steps can be linked or separated by returns to room temperature.
  • a magnetic field is applied during the first annealing step, the curvature of the field lines of which is appropriate for the intended application of the magnet.
  • the second annealing step can be done with or without the action of a magnetic field.
  • the annealing treatment does not involve any action of a magnetic field.
  • the alloys used in the process according to the invention can be obtained in various ways, for example by melting the constituent elements in the pure state or in the pre-alloyed state, or by sintering pluvululent mixtures of the constituent elements or alloys of these elements.
  • the process can also be applied to alloys which have been given a privileged crystal structure by known means (thermal gradient, zone fusion, etc.).
  • the invention will be illustrated by the following exemplary embodiments and by the single figure which represents a diagram of the heat treatment of an alloy according to the invention, in order to obtain an anisotropic magnet, the hatched part of the curve representing the area of time and temperature where it is necessary to apply a magnetic field.
  • the treatment A according to the invention notably improves the magnetic properties of an isotropic magnet, in particular as regards the recatangularity of the hysteresis curve.
  • the weakly alloyed compositions (in Co and Cr) examples 3 and 4 have values of BHmax and of ⁇ which are much higher than those obtained with the loaded alloys (example 1) representative of the state of the art, and that the weakest alloy (example 4) itself offers magnetic characteristics greater than or equivalent to those of the alloy of intermediate composition (example 3).

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Description

La présente invention concerne un procédé de traitement thermique des alliages Fe-Co-Cr destinés à la fabrication d'aimants permanents ainsi que les aimants réalisés par ce procédé. Ces alliages ont pour composition (en poids):

Figure imgb0001
éventuellement un ou plusiers des éléments AI, Nb, Ta, W, Mo, V, Ti, Si, Cu en quantité totale inférieure à 10 %, le reste étant du fer.The present invention relates to a process for heat treatment of Fe-Co-Cr alloys intended for the manufacture of permanent magnets as well as the magnets produced by this process. These alloys have for composition (by weight):
Figure imgb0001
 optionally one or more of the elements AI, Nb, Ta, W, Mo, V, Ti, Si, Cu in a total amount of less than 10%, the rest being iron.

Le brevet français n°2.149.076 décrit certains alliages de ce type ainsi que leurs traitements thermiques. On moule une première forme que l'on soumet à un traitement d'homogénéisation à haute température entre 1200 et 1400°C pendant plus de 10 minutes, suivi d'une trempe rapide jusqu'à la température ambiante. A ce stade, le corps moulé peut subir, sans difficulté particulière, diverses opérations de mise en forme telles que laminage, perçage, usinage, etc... pour l'amener à une forme proche de la forme définitive.French Patent No. 2,149,076 describes certain alloys of this type as well as their heat treatments. A first form is molded and subjected to a high temperature homogenization treatment between 1200 and 1400 ° C for more than 10 minutes, followed by rapid quenching to room temperature. At this stage, the molded body can undergo, without particular difficulty, various shaping operations such as rolling, drilling, machining, etc. to bring it to a shape close to the final shape.

Ensuite, le corps est soumis à un traitement isotherme de recuit dans un champ magnétique, à une température comprise entre 580 et 650°C (de préférence 600 à 640°C) pendant une période de 10 minutes à 2 heures, mais préférentiellement de l'ordre de 30 minutes. Après retour à la température ambiante, la pièce est soumise à un ou plusieurs revenus à des températures comprises entre 530 et 650°C pendant 1 à 9 h, ces revenus pouvant se faire à des températures étagées décroissantes. On constate alors que ces différents revenus ont tendance à diminuer la rectangularité du cycle d'hystérésis mesurée par le rapport q entre l'énergie spécifique (BH) max et le produit Br Hc de l'induction rémanente par le champ coercitif.Then, the body is subjected to an isothermal annealing treatment in a magnetic field, at a temperature between 580 and 650 ° C (preferably 600 to 640 ° C) for a period of 10 minutes to 2 hours, but preferably from 1 'order of 30 minutes. After returning to room temperature, the part is subjected to one or more tempers at temperatures between 530 and 650 ° C for 1 to 9 h, these tempers can be done at decreasing stepped temperatures. We then observe that these different incomes tend to decrease the rectangularity of the hysteresis cycle measured by the ratio q between the specific energy (BH) max and the product Br Hc of the residual induction by the coercive field.

D'autre part, si l'on veut obtenir une énergie spécifique (BH) max supérieure à 40 kJ/m3 (5.108 Gauss-Oersteds), il faut procéder, comme le montre l'exemple 12 du brevet francais précité, à une opération de corroyage supplémentaire (laminage ou forgeage) entraînant une réduction de la section transversale de la pièce. L'expérience montre que, dans de nombreux cas, cette opération conduit à une fissuration ou une rupture de la pièce due au fait qu'à ce stade, l'alliage est biphasé et fragile.On the other hand, if one wants to obtain a specific energy (BH) max greater than 40 kJ / m 3 (5.10 8 Gauss-Oersteds), it is necessary to proceed, as shown in example 12 of the aforementioned French patent, to an additional working operation (rolling or forging) resulting in a reduction in the cross section of the part. Experience shows that, in many cases, this operation leads to cracking or rupture of the part due to the fact that at this stage, the alloy is two-phase and fragile.

Le but de la présente invention est d'éviter ces inconvénients et de permettre la fabrication d'aimants permanents anisotropes du type Fe-Cr-Co présentant un coefficient il de rectangularité de la courbe d'hystérésis constant au cours des revenus et dont l'énergie spécifique peut dépasser 40 kJ/m3 (5.108 Gaus-Oersteds) sans opération de corroyage supplémentaire et, donc, sans risque de rupture.The object of the present invention is to avoid these drawbacks and to allow the manufacture of anisotropic permanent magnets of the Fe-Cr-Co type having a coefficient il of rectangularity of the hysteresis curve constant during the incomes and whose specific energy can exceed 40 kJ / m 3 (5.10 8 Gaus-Oersteds) without additional wrought operation and, therefore, without risk of rupture.

Elle peut permettre également la fabrication d'aimants permanents isotropes dont la courbe d'hystérésis présente une rectangularité plus grande que celle obtenue aec les traitements connus.It can also allow the manufacture of isotropic permanent magnets whose hysteresis curve has a greater rectangularity than that obtained with known treatments.

L'invention consiste à réaliser le traitement de recuit qui suit la trempe après homogénéisation en deux étapes:

  • - une première étape à une température comprise entre 630 et 670°C, pendant une durée comprise entre 5 et 30 minutes;
  • -une seconde étape immédiatement après, sans retour à basse température , à une température inférieure de 40 à 70°C à la précédente pendant au moins 10 minutes.
The invention consists in carrying out the annealing treatment which follows the quenching after homogenization in two stages:
  • - A first step at a temperature between 630 and 670 ° C, for a period between 5 and 30 minutes;
  • -a second step immediately after, without return to low temperature, at a temperature 40 to 70 ° C lower than the previous one for at least 10 minutes.

La durée la première étape est suffisamment courte pour éviter la précipitation de la phase u fragile dans l'alliage. La température de maintien pendant cette première étape est comprise de préférence entre 640 et 660°C.The duration of the first stage is short enough to avoid precipitation of the fragile u phase in the alloy. The holding temperature during this first step is preferably between 640 and 660 ° C.

Le traitement de revenu se fait préférentiellement en trois étapes de durée croissante à des températures étagées décroissantes d'environ 30°C. Ces étapes peuvent être enchaînées ou séparées par des retours à la température ambiante.The tempering treatment is preferably carried out in three stages of increasing duration at decreasing staged temperatures of approximately 30 ° C. These steps can be linked or separated by returns to room temperature.

Pour réaliser des aimants permanents anisotropes, on applique, pendant la première étape du recuit, un champ magnétique dont la courbure des lignes de champ est appropriée à l'application envisagée de l'aimant. La seconde étape du recuit peut se faire avec ou sans action d'un champ magnétique.To make anisotropic permanent magnets, a magnetic field is applied during the first annealing step, the curvature of the field lines of which is appropriate for the intended application of the magnet. The second annealing step can be done with or without the action of a magnetic field.

Bien entendu, pour obtenir des aimants isotropes, le traitement de recuit ne comporte aucune action d'un champ magnétique.Of course, to obtain isotropic magnets, the annealing treatment does not involve any action of a magnetic field.

Les alliages mis en oeuvre dans le procédé selon l'invention peuvent être obtenus de manières diverses, par exemple par fusion des éléments constitutifs à l'état pur ou à l'état préallié, ou par frittage de mélanges pluvérulents des éléments constitutifs ou d'alliages de ces éléments. On peut également appliquer le procédé à des alliages auxquels on a conféré une structure cristalline priviligiée par des moyens connus (gradient thermique, fusion de zone, etc...).The alloys used in the process according to the invention can be obtained in various ways, for example by melting the constituent elements in the pure state or in the pre-alloyed state, or by sintering pluvululent mixtures of the constituent elements or alloys of these elements. The process can also be applied to alloys which have been given a privileged crystal structure by known means (thermal gradient, zone fusion, etc.).

L'invention sera Illustrée par les exemples de réalisation suivants et par la figure unique qui repre- sente un schéma du traitement thermique d'un alliage selon l'invention, pour obtenir un aimant anisotrope, la partie hachurée de la courbe représentant la zone de temps et de température où il est nécessaire d'appliquer un champ magnétique.The invention will be illustrated by the following exemplary embodiments and by the single figure which represents a diagram of the heat treatment of an alloy according to the invention, in order to obtain an anisotropic magnet, the hatched part of the curve representing the area of time and temperature where it is necessary to apply a magnetic field.

Exemple 1Example 1

On a coulé un alliage Fe-Co-Cr de composition suivante (en poids):

Figure imgb0002
et on lui a fit subir le traitement thermique suivant, schématisé sur la figure:

  • 1 ) homogénéisation à 1300°C suivie d'une trempe à l'eau jusqu'à température ambiante
  • 2) chauffage jusqu'à 655°C et maintien, pendant 15 minutes, en présence d'un champ magnétique de 159 kA/m (2000 Oersteds),
  • 3) refroidissement en 5 minutes, en présence du champ magnétique ci-dessus jusqu'à 600°C,
  • 4) maintien à 600°C, pendant 15 minutes, sans champ magnetique,
  • 5) trempe à l'eau ou refroidissement à l'air jusqu'à la température ambiante,
  • 6) revenus étages 1 h30 à 580°, puis 5 h à 550°C, puis 15 h à 520°C.
A Fe-Co-Cr alloy of the following composition (by weight) was poured:
Figure imgb0002
 and he was subjected to the following heat treatment, shown diagrammatically in the figure:
  • 1) homogenization at 1300 ° C followed by quenching with water to room temperature
  • 2) heating to 655 ° C and maintaining, for 15 minutes, in the presence of a magnetic field of 159 kA / m (2000 Oersteds),
  • 3) cooling in 5 minutes, in the presence of the above magnetic field to 600 ° C,
  • 4) maintenance at 600 ° C, for 15 minutes, without magnetic field,
  • 5) water quenching or air cooling to room temperature,
  • 6) floor returns 1 h 30 at 580 °, then 5 h at 550 ° C, then 3 h at 520 ° C.

A titre de comparaison, on a réalisé le traitement de l'art antérieur dans lequel, après les 15 minutes à 655°C, on est descendu en 15 minutes à 400°C. On a mesuré, dans chaque cas, les caractéristiques magnétiques de l'aimant obtenu, et établi le rapport:

Figure imgb0003
By way of comparison, the treatment of the prior art was carried out in which, after 15 minutes at 655 ° C., it was lowered in 15 minutes to 400 ° C. In each case, the magnetic characteristics of the magnet obtained were measured, and the relationship established:
Figure imgb0003

Les résultats ont été rassemblés dans le tableau I dans lequel on a désigné par:

  • -A et B deux résultats d'essais dans une même coulée pour laquelle le recuit a été fait, selon l'invention, en deux étapes,
  • -C et D deux résultats issus de la même coulée que ci-dessus ayant subi le traitement de comparaison,
  • -1, 2 et 3 les mesures faites respectivement après le recuit, après le deuxiéme revenu et après le troisième revenu.
The results have been collated in Table I in which we have designated by:
  • -A and B two test results in the same casting for which the annealing was done, according to the invention, in two stages,
  • -C and D two results from the same casting as above having undergone the comparison treatment,
  • -1, 2 and 3 the measurements made respectively after the annealing, after the second income and after the third income.

Ces résultats montrent clairement qu'avec le procédé selon l'invention, on obtient des aimants anisotropes ayant une énergie spécifique supérieure à 40 kJ/m3 et un coefficient η supérieur à 0,60, ce qui n'était pas possible avec le procédé de l'art antérieur sans opération supplémentaire de corroyage. De plus, le durées de traitement sont raisonables et n'élèvent pas le prix de revient.These results clearly show that with the method according to the invention, anisotropic magnets are obtained having a specific energy greater than 40 kJ / m 3 and a coefficient η greater than 0.60, which was not possible with the method of the prior art without additional wrought operation. In addition, the processing times are reasonable and do not increase the cost price.

Exemple 2Example 2

De même, on a appliqué un traitement identique selon l'invention, mais, cette fois, en l'absence de champ magnétique pour réaliser des aimants isotropes et un traitement de comparaison selon fart antérieur identique au cas précédent, mais sans champ magnétique.Similarly, an identical treatment was applied according to the invention, but, this time, in the absence of a magnetic field to produce isotropic magnets and a comparison treatment according to the prior art identical to the previous case, but without magnetic field.

Les résultats sont indiqués au tableau Il dans lequel on a désigné par A' l'essai pour lequel le recuit a été fait selon l'invention, et par C' pour lequel le traitement de recuit de l'art antérieur a été appliqué, les indices 1, 2 et 3 ayant le même signification que précédemment.

Figure imgb0004
Figure imgb0005
Figure imgb0006
 The results are indicated in Table II in which the test for which the annealing was carried out according to the invention is designated by A 'and by C' for which the annealing treatment of the prior art has been applied, the indices 1, 2 and 3 having the same meaning as above.
Figure imgb0004
Figure imgb0005
Figure imgb0006

On constate que le traitement A selon l'invention améliore notablement les propiétés magnétiques d'un aimant isotrope, en particulier en ce qui concerne la recatangularité de la courbe d'hystérésis.It can be seen that the treatment A according to the invention notably improves the magnetic properties of an isotropic magnet, in particular as regards the recatangularity of the hysteresis curve.

Exemple 3Example 3

On a traité une composition constitutée (en poids) de 17 % Co, 26 Cr, 0,5 % W, le reste étant essentiellement du fer, de la façon suivante:

  • - homogénéisation à 1320°C pendant 1h et trempe à l'eau,
  • - chauffage jusqu'à 655°C maintenu 15 minutes en présence d'un champ magnétique de 159 kA/m (2000 Oersteds),
  • -refroidissement en 5 minutes à 590°C en présence du champ magnétique,
  • -maintien à 590°C (sans champ) pendant 30 minutes et trempe à l'eau,
  • -trois revenus étagés 1h30 à 580°C, puis 5 h à 550°C, puis 15 h à 520°C.
A compound composition (by weight) of 17% Co, 26 Cr, 0.5% W was treated, the remainder being essentially iron, as follows:
  • - homogenization at 1320 ° C for 1 hour and quenching with water,
  • - heating to 655 ° C maintained for 15 minutes in the presence of a magnetic field of 159 kA / m (2000 Oersteds),
  • cooling in 5 minutes at 590 ° C in the presence of the magnetic field,
  • -maintain at 590 ° C (without field) for 30 minutes and soak in water,
  • -three storey returns 1:30 at 580 ° C, then 5 h at 550 ° C, then 3 h at 520 ° C.

Les résultats de deux essais effectués sur cette composition après recuit (1) après le deuxième revenu (2) et après le troisième revenu (3), sont les suivants:

Figure imgb0007
The results of two tests carried out on this composition after annealing (1) after the second tempering (2) and after the third tempering (3), are the following:
Figure imgb0007

Exemple 4Example 4

On a traité une composition comprenant (en poids)15 % de Co, 24 % de Cr, 1 % W, le solde étant essentiellement du fer, de la manière suivante:

  • - homogénéisation à 1250°C pendant 1 h, suivie d'une trempe à l'eau,
  • - chauffage à 670°C et maintien pendant 15 minutes en présence d'un champ magnétique de 159 kA/m (2000 Oersteds),
  • -refroidissement en 5 minutes à 590°C (sous champ) et maintien pendant 30 minutes (hors champ) suivi d'une trempe à l'eau (ou d'un refroidissement à l'air) jusqu'à la température ambiante,
  • -triple revenu étagé de 1 h 30 à 580°C, puis 5 h à 550°C, puis 15 h à 520°C.
A composition comprising (by weight) 15% Co, 24% Cr, 1% W was treated, the balance being essentially iron, in the following manner:
  • - homogenization at 1250 ° C for 1 h, followed by quenching with water,
  • - heating to 670 ° C and holding for 15 minutes in the presence of a magnetic field of 159 kA / m (2000 Oersteds),
  • - cooling in 5 minutes to 590 ° C (under field) and holding for 30 minutes (out of field) followed by quenching with water (or air cooling) to room temperature,
  • - triple stage income from 1 h 30 at 580 ° C, then 5 h at 550 ° C, then 15 h at 520 ° C.

Les résultats obtenus sur deux échantillons sont reportés dans le tableau IV suivant (avec les mêmes notations).

Figure imgb0008
The results obtained on two samples are reported in the following Table IV (with the same notations).
Figure imgb0008

On peut constater que les compositions faiblement alliées (en Co et Cr) exemples 3 et 4, présentent des valeurs de BHmax et de η largement supérieures à celles obtenues avec les alliages chargés (exemple 1 ) représentatifs de l'état de la technique, et que le plus faiblement allié (exemple 4) offre lui- même des caractéristiques magnétiques supérieures ou équivalentes à celles de l'alliage de composition intermédiaire (exemple 3).It can be seen that the weakly alloyed compositions (in Co and Cr) examples 3 and 4 have values of BHmax and of η which are much higher than those obtained with the loaded alloys (example 1) representative of the state of the art, and that the weakest alloy (example 4) itself offers magnetic characteristics greater than or equivalent to those of the alloy of intermediate composition (example 3).

Claims (5)

1. A process for the thermal treatment of a Fe-Co-Cr alloy for a permanent magnet composed of 10 to 40% of Co, 10 to 40% of Cr; 0 to 10% of one or more of the following elements Al, Nb, Ta, W, Mo, T, Si and Cu; Fe, remainder, comprising an homogenisation at between 1200 and 1400°C for at least 10 minutes, followed by a rapid quenching, an annealing treatment and one or several tempering at temperatures comprised between 500 and 600°C, characterised in that the annealing is conducted in two stages, wherein the first stage is at a temperature of between 630 and 670°C for a period ofi between 5 and 30 minutes and the second stage which follows immediately after the first stage without a return to low temperature and at a temperature of from 40 to 70°C below the first stage and for at least 10 minutes.
2. A process as defined in claim 1, for the manufacture of anisotropic permanent magnet, characterised in that the magnetic field is applied to the alloy at least during the first annealing stage.
3. A process according to either claims 1 or 2 characterised in that the temperature of the first annealing stage is between 640 and 660°C.
4. A process according to either of Claims 1, 2 or 3, and further characterised in that the tempering treatment is conducted in three stages of increasing duration at decreasng temperatures of approximately 30°C each other.
5. An anisotropic permanent magnet produced by the process according one of the claims 2 to 4, said magnet having a maximum specific energy BH max above 40 kJ/m3(5.106 Gauss-Oersteds), characterised in that its coefficient 11 of rectangularity of the hysteresis cycle is greater than, or egal to 0.60.
EP79420003A 1978-01-19 1979-01-11 Process for the thermal treatment of Fe-Co-Cr alloys for permanent magnets Expired EP0003466B1 (en)

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FR7802104 1978-01-19
FR7802104A FR2415145A1 (en) 1978-01-19 1978-01-19 THERMAL TREATMENT PROCESS OF FE-CO-CR ALLOYS FOR PERMANENT MAGNETS

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DE19611461C2 (en) * 1996-03-22 1999-05-12 Dresden Ev Inst Festkoerper Use an iron-chromium-cobalt-based alloy

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IT1110740B (en) 1986-01-06
ATA35579A (en) 1983-06-15
CH635617A5 (en) 1983-04-15
FR2415145B1 (en) 1980-08-01
IT7919384A0 (en) 1979-01-17
DE2960005D1 (en) 1980-11-13
FR2415145A1 (en) 1979-08-17
ES476970A1 (en) 1979-06-16
JPS54109021A (en) 1979-08-27
BE873557A (en) 1979-07-18
IN151185B (en) 1983-03-05
EP0003466A1 (en) 1979-08-08
CA1132886A (en) 1982-10-05
BR7900316A (en) 1979-08-14
JPS5856731B2 (en) 1983-12-16
US4246049A (en) 1981-01-20
AT373629B (en) 1984-02-10

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