WO2003085147A1 - Alliage utilise dans un aimant lie, poudre d'aimant isotrope et anisotrope et son procede de production, et aimant lie - Google Patents

Alliage utilise dans un aimant lie, poudre d'aimant isotrope et anisotrope et son procede de production, et aimant lie Download PDF

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WO2003085147A1
WO2003085147A1 PCT/JP2002/006547 JP0206547W WO03085147A1 WO 2003085147 A1 WO2003085147 A1 WO 2003085147A1 JP 0206547 W JP0206547 W JP 0206547W WO 03085147 A1 WO03085147 A1 WO 03085147A1
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Prior art keywords
magnet
alloy
powder
magnet powder
hydrogen
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PCT/JP2002/006547
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English (en)
Japanese (ja)
Inventor
Yoshinobu Honkura
Norihiko Hamada
Chisato Mishima
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Aichi Steel Corporation
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Priority to AU2002346234A priority Critical patent/AU2002346234A1/en
Priority to US10/182,724 priority patent/US6955729B2/en
Priority to JP2003582322A priority patent/JP3565513B2/ja
Publication of WO2003085147A1 publication Critical patent/WO2003085147A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/023—Hydrogen absorption
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/0433—Nickel- or cobalt-based alloys
    • C22C1/0441—Alloys based on intermetallic compounds of the type rare earth - Co, Ni
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/001—Ferrous alloys, e.g. steel alloys containing N
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/10—Ferrous alloys, e.g. steel alloys containing cobalt
    • 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
    • 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
    • H01F1/0578—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 bonded together
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
    • H01F41/0273—Imparting anisotropy

Definitions

  • the present invention provides an alloy for a bond magnet that enables low-cost production of a bond magnet having excellent magnetic properties, an isotropic magnet powder and an anisotropic magnet powder obtained from the alloy, and a method for producing the same.
  • the present invention relates to a bonded magnet obtained from the above magnet powder.
  • Hard magnets are used in various devices such as motors.
  • motors there is a strong demand for small and high-power vehicles such as motor vehicles.
  • Such hard magnets are required not only to have high performance in terms of magnetic properties but also to be low-cost in order to strengthen global competitiveness.
  • RF eB-based magnets (rare-earth magnets) composed of rare-earth elements (R), boron (B), and iron (Fe) have been actively developed.
  • RF eB-based magnets include, for example, US Pat. No. 4,851,058 (hereinafter referred to as “Prior Art 1”) and US Pat. No. 5,541,608 (hereinafter referred to as “Prior Art 2”).
  • Primary Art 1 US Pat. No. 4,851,058
  • Primary Art 2 US Pat. No. 5,541,608
  • An anisotropic RFeB-based magnet alloy (composition) is disclosed.
  • prior art 1 includes about 10-40 &% (1, Pr or Nd and Pr, about 50-90a7 Fe, about 0.5 ⁇ ; L 0 at%
  • Prior art 2 discloses 12 to 40 at% of Nd, Pr or Nd and Pr, 10 at% or less of 'Co, and 3 to 8 & 7%. No. 8 and a balance of Fe are disclosed.
  • the prior art 2 is intended to improve the heat resistance by increasing the Curie temperature by adding Co.
  • a magnet powder having the above composition is obtained by a melt-span method which is a kind of rapid solidification method. This magnet powder (magnetic powder) is often used industrially as a raw material powder for bonded magnets (hard magnets).
  • the bonded magnet is obtained, for example, by first producing a pellet from the magnetic powder and a resin as a binder, feeding the pellet to a molding die, and performing pressure molding.
  • a pellet is fed into the mold, if the flow rate is low, the powder feeding time will be short, and the productivity of bonded magnets can be improved.
  • the pellet has a large bulk density, it is possible to uniformly supply the powder to the mold and reduce the defective rate of the bonded magnet. Therefore, the lower the fluidity and the higher the bulk density, the lower the cost of the bonded magnet, and the better the economic efficiency.
  • the fluidity and the bulk density depend on the particle shape of the magnetic powder.
  • the particle shape of the magnetic powder produced by the above-mentioned prior arts 1 and 2 is a flake shape having a thickness of 20 to 50 m, and therefore has a higher fluidity and a lower bulk density than a spherical case.
  • the flakes are pulverized into spheres to reduce the fluidity and increase the bulk density.
  • the number of man-hours increases, and even if it is made spherical, it is actually difficult to effectively reduce the fluidity and increase the bulk density. This is because powders less than 50 m are generally prone to sticking-agglomeration where the original particle size is at most 50 m.
  • an HDDR (hydrogenat ion on disopropontlonat-desorptio-recombombinat ion) treatment method or a d-HDDR treatment method is used.
  • the magnetic powder obtained by these methods is composed of substantially spherical particles, it has better fluidity and bulk density than the magnetic powder obtained by the above-mentioned conventional techniques 1 and 2.
  • the HDDR treatment method is used to produce RFeB-based isotropic magnet powder (isotropic magnetic powder) and RFeB-based anisotropic magnet powder (anisotropic magnetic powder), and mainly consists of two processes. That is, in a hydrogen gas atmosphere of about lO OkPa (l atm), the temperature is maintained at 773 to 1273 K, the first step (hydrogenation step) in which the three-phase decomposition disproportionation reaction occurs, and then the vacuum is applied. Dehydrogenation step (second step).
  • d-HDR treatment is a method mainly used for producing RF eB-based anisotropic magnetic powder.
  • the reaction rate of RFeB-based alloy and hydrogen is controlled from room temperature to high temperature. This is done by doing Specifically, a low-temperature hydrogenation step (first step) in which the RF eB alloy absorbs hydrogen sufficiently at room temperature, and a high-temperature hydrogenation step (three-phase decomposition disproportionation reaction under low hydrogen pressure)
  • the second process consists of four steps: an evacuation process that dissociates hydrogen at the highest possible hydrogen pressure (third process), and a dehydrogenation process that removes hydrogen from the material (fourth process). become.
  • the difference from the HDD R treatment is that by providing multiple processes with different temperatures and hydrogen pressures, the reaction rate between the RF eB alloy and hydrogen can be kept relatively slow, and homogeneous anisotropic magnetic powder can be obtained. It is a point that is devised as follows.
  • HDDR processing was used: A method for producing FeB, system isotropic magnetic powder is disclosed in Japanese Patent Publication No. 7-68561 (Patent No. 2041426: hereinafter referred to as “related art 3”).
  • Patent No. 2041426 hereinafter referred to as “related art 3”.
  • an alloy ingot containing R, Fe, and B as main components is subjected to a pulverizing step and a homogenizing heat treatment step, and then is subjected to the above-described HP DR treatment to produce magnetic powder.
  • the two steps (pulverizing step and homogenizing heat treatment step) before the HDDR treatment are indispensable for obtaining isotropic magnetic powder having large magnetic properties.
  • the two processes are both expensive and inefficient.
  • the homogenization heat treatment process which carries out the high-temperature treatment at 873 to 1473 K, requires about twice the cost of HDDR treatment, and is extremely inefficient.
  • an alloy ingot consisting of about 10 to 20 a% of 1 and about 5 to 20% of B, the balance of Fe and various additional elements is subjected to a homogenizing heat treatment step.
  • the milling process is followed by HDD R. treatment to produce magnetic powder.
  • the B content of the alloys disclosed in the examples is shown in detail below 10.4 at%, but alloys with a B content exceeding 10.4 at% are 10.4 at% and 20 at%. At% alloy only.
  • the (BH) max of the anisotropic bonded magnet made from magnetic powder with a B content of 10.4 at% is 83 or more: I 12 kJ m 3 , and ⁇ Hc is 0.74 to 0.97 ⁇ / a ⁇
  • (BH) max of the anisotropic bonded magnet fabricated B amount from 20 at% of the magnetic particles is 80 ⁇ 93 k J / m 3 , iHc ⁇ ⁇ 0. 46 ⁇ 0. 75MA / m . All of these magnetic properties are inadequate. In particular, as the B content increases to 20 at%, the decrease in iHc becomes difficult.
  • the reaction rate between the RF eB-based alloy and hydrogen can be controlled gently in each step, so that the amount of heat generated during the disproportionation reaction between the RF eB-based alloy and hydrogen can be reduced. This is because the amount of heat absorbed during dehydrogenation can be suppressed.
  • the homogenizing heat treatment process is performed using an alloy ingot consisting of about 12 to 15 at% of 1 and about 6 to 9 at% of 8 and the balance; Fe.
  • anisotropic magnetic powder is manufactured by d-HDDR treatment. Therefore, similarly to the above-described manufacturing method, the same can be said in that the manufacturing cost is also high.
  • hard magnets excel in long-term characteristics such as corrosion resistance. It is also important.
  • hard magnets incorporated in household motors and motors for automobiles used in high-temperature environments are required to have excellent heat resistance from the viewpoint of ensuring the reliability of motors.
  • the above-mentioned rare earth magnets are liable to be deteriorated due to oxidative corrosion of Fe and R which are the main components thereof, and it is difficult to stably secure their high magnetic properties.
  • a rare earth magnet when used at room temperature or higher, its magnetic properties tend to decrease rapidly.
  • the temporal change of such a magnet is usually quantitatively indexed by the permanent demagnetization rate (%), but in most rare earth magnets, the permanent demagnetization rate exceeds 10%. .
  • the permanent demagnetization rate is a reduction rate of the magnetic flux that is not restored even after re-magnetization after a long time (1000 hours) at a predetermined high temperature. Disclosure of the invention
  • the present invention has been made in view of such circumstances.
  • RF e B-based magnet powders that are obtained without performing the homogenizing heat treatment process, which is a high cost factor, have low cost and have excellent magnetic properties, and are subjected to HDDR processing or d-HDDR processing, and a method of manufacturing the same.
  • the present invention provides a bond magnet that is not only low-cost and excellent in magnetic properties but also has little aging deterioration, and further provides an RF eB-based magnet alloy, an RFeB-based magnet powder, and a method for producing such a hard magnet capable of obtaining such a hard magnet The purpose is also.
  • the inventor of the present invention has intensively studied to solve this problem, and has conducted various systematic experiments. As a result, the present inventors have developed a novel magnet alloy having a different B content from that of the related art, and have completed the following invention.
  • the alloy for bonded magnets of the present invention is a rare earth element containing iron (Fe) as a main component and 12 to 16 atomic% (at%) of yttrium (Y) (hereinafter referred to as “: R”). ) And at least 10.8 to 15 at% of boron (B).
  • the present invention contains at least Fe, which is the main component, R containing 12 to 16 at% of Y, and 10.8 to 15 at% of 8, It may be a magnetic alloy characterized by being subjected to HDDR treatment or d-HDR treatment, which is one of the above.
  • the alloy for bonded magnets of the present invention (hereinafter, simply referred to as “magnet alloy” as appropriate) has a different B content from the RF e B-based magnet alloy that has been developed so far, and has a relatively large B content. .
  • the present inventors have found that in a magnetic alloy having a large amount of B, precipitation of the primary crystal, Hiichi Fe, is suppressed. And, as a result of suppressing the precipitation of Fe that causes a decrease in magnetic properties, it is possible to omit the homogenizing heat treatment step, which was conventionally considered to be indispensable for improving the magnetic properties, and reduce the cost of magnet powder and the like. Now you can get it.
  • B-rich phase an RtF e phase (hereinafter referred to as “B-rich phase”) is formed in the early stage of the structure. It is probable that the precipitation of primary Fe was suppressed because primary Fe, i.e., Fe, was taken into the B-rich phase.
  • a high iHc magnet powder was obtained. This can be considered as follows.
  • Hi Fe, Fe 2 B, R hydride.
  • the hydrogen absorption time is 360 minutes or more.
  • B is set to 10.8 at% or more.
  • the homogenizing heat treatment step which significantly impairs economic efficiency, can be omitted, and iHe can be increased.
  • B exceeds 15 at%, the volume fraction of the B-rich phase in the magnet powder is high, and the maximum energy volume (BH) max is undesirably reduced.
  • the magnet powder in which the B amount and 20 at% is toying disclosure its iHc is 0. 46 ⁇ 0. 75 ⁇ 1 low. This is probably because the hydrogen absorption time was as short as 240 minutes, the reaction between the B-rich phase and hydrogen was insufficient, and the B-rich phase did not precipitate finely and densely during the subsequent dehydrogenation.
  • R is Y, lanthanum (La), cerium (Ce), praseodymium (Pr), neodymium (Nd), samarium (Sm), gadolinium (Gd), terbium (Tb), It is preferable that it is composed of at least one of dysprosium (Dy), holmium (Ho), erbium (Er), perium (Tm) and lutetium (Lu). Among them, particularly from the viewpoint of cost and magnetic properties, it is preferable to comprise at least one of Pr, Nd and Dy.
  • the magnet alloy of the present invention preferably further contains, in addition to the above elements, cobalt (Co) in an amount of 1 to 6 at%, more preferably 1 to 6 at%.
  • Co is an element that increases the temperature of the magnet and improves heat resistance. If 00 is less than 0. lat%, there is no substantial effect. ⁇ "Co is expensive, so industrial cost n — TM
  • the magnet alloy of the present invention includes gallium (Ga), zirconium (Zr), vanadium (V), aluminum (A1), titanium (Ti), hafnium (Hf) and copper (Cu) (hereinafter referred to as “first element group”). ) May be contained in a total of 0.1 to 2 at%. This is because these elements improve the coercive force iHc of the magnet. '
  • the magnet alloy of the present invention comprises at least one of niobium (Nb), tantalum (Ta) and nickel (Ni) (hereinafter referred to as “second element group”) in a total of 0.1 to 2 at%. May be included. This is because these elements increase the residual magnetic flux density (Br) of the magnet.
  • the maximum energy product (BH) max can be improved.
  • the total of them is less than 0.1 at%, there is no substantial effect, and if it exceeds 2 at%, on the other hand, iHc, Br or ( ⁇ ) max decreases, which is not preferable.
  • Ga is 0.1 to 1.0 at%, more preferably 0.2 to 0.4 at% (about 0.3 at%)
  • Nb is 0.1 to: L. 0 at. %, More preferably 0.1 to 0.4 at% (about 0.2 at%).
  • the alloy, the powder, and the like according to the present invention may appropriately contain unavoidable impurities.
  • Their composition is balanced by Fe, but to be honest, Fe is 59-77.2 at%.
  • the magnetic alloy of the present invention contains, apart from the R, 0.001 to 1.0 at% of La. As a result, aging of the magnet powder and the hard magnet made of the magnet alloy can be suppressed.
  • La is the element with the highest oxidation potential among the rare earth elements (RE).
  • RE rare earth elements
  • La acts as a so-called oxygen source, and La is selectively (preferably) oxidized over R (Nd, Dy, etc.), and consequently a magnet powder or a hard magnet containing La. Oxidation is suppressed.
  • Dy, Tb, Nd, .Pr, etc. instead of La, but these elements cannot sufficiently suppress the oxidation of magnet powder and hard magnets. In terms of cost, the use of La is preferred over those elements.
  • R in the magnet alloy at this time is a rare earth element other than La.
  • La has an effect of improving corrosion resistance and the like even when La is contained in a small amount exceeding the level of unavoidable impurities in the magnet alloy. Since the unavoidable impurity level of La is less than 0.001 at%, in the present invention, the La amount is 0.001 at% or more. On the other hand, if La exceeds 1.0 & 1%, iHc is undesirably reduced.
  • the lower limit of the amount of La is 0.01 at%, 0.05 at%, and 0.1%, the effect of improving the corrosion resistance and the like is sufficiently exhibited, which is more preferable. From the viewpoint of improving the corrosion resistance and suppressing the decrease in iHc, it is more preferable that the 1 ⁇ > amount is 0.01 to 0.7 at%.
  • the La-containing alloy composition is not an alloy composition that allows the R 2 Fe phase to exist as a single phase or almost a single phase, but an alloy composition composed of a multi-phase structure such as RzFe Bi phase and B-rich phase. It is.
  • the magnetic alloy according to the present invention may be in an ingot or a powder regardless of its form.
  • the particle size and shape of the powder are not limited.
  • the magnet alloy of the present invention can be understood as isotropic magnet powder or anisotropic magnet powder.
  • the isotropic magnet powder of the present invention has an ingot of an alloy containing at least 1023 at% of R, which contains 12 to 16 at% of Y, and at least 10. It can be obtained through a manufacturing method of performing an HDDR treatment including a hydrogenation step of maintaining the hydrogen gas atmosphere at ⁇ 1 173 K and a dehydrogenation step of removing hydrogen after the hydrogenation step.
  • the anisotropic magnet powder of the present invention provides an ingot of an alloy containing at least 873, which contains Fe as the main component, R containing 12 to 16 at%, and 10.8 to 15 at%.
  • the method comprises a first exhaust step of maintaining the atmosphere in a hydrogen gas atmosphere of 0.12 to 1173 K at 0.1 to 20 kPa and a second exhaust step of removing hydrogen after the first exhaust step.
  • the bonded magnet of the present invention is a main component.
  • the method is characterized in that isotropic magnet powder obtained by HDDR treatment comprising a dehydrogenation step of removing hydrogen after the hydrogenation step is mixed with a binder and molded.
  • the bonded magnet of the present invention is characterized in that the main components are Fe and 12 or more: L containing 6 at% of R and 10. 8 to 15 & 7% of: 6
  • a low-temperature hydrogenation step in which an ingot of at least alloy containing at least 873 K or less is kept in a cryogen gas atmosphere, and after the low-temperature hydrogenation step is kept in a hydrogen gas atmosphere of 1023-1173 K at 20-100 kPa High temperature hydrogenation step, and after the high temperature hydrogenation step, 0.1 to 20?
  • D an anisotropic magnet obtained by a HDDR process, comprising: a first evacuation step of maintaining a hydrogen gas atmosphere of 1023 to 1173 K in an atmosphere; and a second evacuation step of removing hydrogen after the first evacuation step. It is characterized in that powder and a binder are mixed and molded under pressure.
  • Figure 1 is a bar graph comparing the fluidity of pellets for bonded magnets manufactured from magnet powder.
  • Figure 2 is a bar graph comparing the bulk density of pellets for bonded magnets manufactured from magnet powder.
  • Figure 3 is a bar graph comparing the cost performance of magnet powder produced by d-HDD treatment.
  • the magnet powder of the present invention can be obtained by subjecting the ingot of the magnet alloy (coarse powder) to the above-described HDR processing method or d-HDDR processing method.
  • the HDDR treatment according to the present invention is performed by subjecting an alloy (ingot) having a composition of 10.8 to 15 &%: 6 to a hydrogenation step and a dehydrogenation step.
  • the conditions for the hydrogenation step are as described above.
  • the dehydrogenation step is, for example, a step of setting the hydrogen pressure to an atmosphere of 10 Pa or less.
  • the temperature during the dehydrogenation step may be, for example, 1023 to 1173K.
  • the hydrogen pressure referred to in this specification means a partial pressure of hydrogen unless otherwise specified. Therefore, as long as the hydrogen partial pressure in each step is within a predetermined value, a vacuum atmosphere or a mixed atmosphere of an inert gas or the like may be used.
  • the processing time of each of the above steps depends on the processing amount per batch. For example, if the processing amount per batch is 10 kg, the hydrogenation step may be performed for 360 to 1800 minutes, and the dehydration step may be performed for about 30 to 180 minutes.
  • the HDDR process itself is disclosed in detail in the above-mentioned prior art 3 and the like, and may be appropriately referred to.
  • the magnet powder obtained by this HDDR treatment method is industrially meaningful as an isotropic magnet powder.
  • the magnetic powder exhibits excellent magnetic properties, for example, iHc of 0.8 to 1.7 (MAX m) and (BH) max of 60 to: L 20 (k J / m 3 ).
  • the hydrogenation step which is the first step of the HDDR treatment
  • hydrogen and the RFeB-based alloy and hydrogen and the B-rich phase are sufficiently reacted.
  • the dehydrogenation step B-rich phase is finely and densely precipitated. And this finely precipitated; the B-rich phase pins the RF eB grain growth and makes the RF eB grains fine. As a result, a high coercive force (iHc) can be obtained.
  • the d-HDD R treatment according to the present invention is performed by subjecting an alloy (ingot) having a composition of 10.8 to 15 at% B to a low-temperature hydrogenation step, a high-temperature hydrogenation step, An exhaust process and a second exhaust process are performed.
  • the conditions for the high-temperature hydrogenation step and the first exhaust step are as described above.
  • the low-temperature hydrogenation step is, for example, a step of setting an atmosphere at a hydrogen pressure of 30 to 200 kPa.
  • the second evacuation step is, for example, a step of setting the hydrogen pressure to an atmosphere of 10 Pa or less, and the temperature at that time is, for example, about 102 to 117 K. Note that the first exhaust process and the second exhaust process together constitute a dehydrogenation process.
  • the processing time of each of the above steps depends on the amount of processing per batch. For example, if the processing volume per litter is 10 kg, the low-temperature hydrogenation step is 30 minutes or more, the high-temperature hydrogenation step is 360 to 180 minutes, and the first exhaustion step is 10 to 100 minutes. It suffices to perform 240 minutes and the second exhaustion process for about 10 to 120 minutes d.—
  • the HDDR treatment method itself is disclosed in detail in the above-mentioned prior art 9 and the like, so that it is appropriately referred to. Just do it.
  • the magnet powder obtained by the d-HDDR treatment is an anisotropic magnet powder exhibiting excellent magnetic properties.
  • the magnetic properties are, for example, ⁇ 110 is 0.8 to 1.7 (MA /), and (BH) max is 190 to 290 (kJ / m 3 ).
  • the first evacuation step which is the third step, while preserving the crystal orientation of the Fe 2 B phase
  • the following steps are performed: (1) Precipitation of the FeB crystal and precipitation of the B-rich phase finely and densely. You. The fine and dense precipitates: The RFeB phase stops the RF eB grain growth and makes the RF eB grains fine.
  • the second evacuation step hydrogen remaining inside the alloy is removed.
  • the ingot can be used as a raw material alloy. However, if a coarse powder that has been pulverized is used, each process can proceed efficiently.
  • the pulverization of the ingot and the pulverization performed after the above treatment can be performed using dry or wet mechanical pulverization (such as a jaw crusher, a disc mill, a ball mill, a vibration mill, and a jet mill).
  • the magnet powder obtained by subjecting the magnet alloy of the present invention to the above-mentioned HDDR treatment or d-HDDR treatment has a substantially spherical particle diameter.
  • the pellets manufactured using the magnet powder of the present invention have a low fluidity and a large bulk density.
  • the magnetic powder of the present invention has a moderate average particle size of about 50 to 200 ⁇ m. Therefore, not only the flowability and bulk density are improved, but also It is excellent in handling because it can suppress As a result, the productivity, quality, yield, and the like of bonded magnets are improved, and the cost of various magnets can be reduced.
  • the fluidity of a pellet obtained by mixing the above magnet powder and an organic resin as a binder in a range of 10 to 45 mass% is 0 ⁇ 55 to 0.64 (s / g).
  • the bulk density is 3.25 to 3.5 (g / cm 3 ).
  • the amount of the organic resin mixed with the magnet powder is 10 to 25mass% for the pellet for compression molding, 30 to 45mass% for the pellet for injection molding, and the pellet for extrusion molding. In this case, it is more preferable to set it to 20 to 35 mass%.
  • the magnet powder has a substantially spherical particle size for the following reason. When magnet powder is manufactured by HDDR treatment or d-HDR treatment, the obtained particle shape is greatly affected by the alloy structure before the treatment. In the early stages of the hydrogenation process of HDDR treatment and in the low-temperature hydrogenation process of d-HDDR treatment, if the alloy absorbs hydrogen, it causes volume expansion and breaks mainly at fragile grain boundaries.
  • the magnet alloy when the magnet alloy is made of a structure such as an ingot, the crystal structure at the center becomes equiaxed grain shape, and the crystal structure at the end becomes dendrite shape.
  • the crystallization or precipitation of the primary crystal, Hi-Fe is suppressed by the presence of the B-rich phase, so that the dendritic crystal structure formed at the end is also fine.
  • the structure made of the magnet alloy of the present invention is subjected to the HDDR treatment or the d-HDDR treatment, one crystal grain becomes almost one substantially spherical particle from the center of the structure.
  • a plurality of dendritic crystals are obtained as one substantially spherical particle from the end.
  • the constituent particles of the magnet powder are much more spherical than the magnet powder obtained by the conventional melt-span method or the like.
  • the use of the magnet powder obtained as described above not only excels in magnetic properties, but also enables low-cost production of a bonded magnet due to its excellent powdering properties.
  • the bonded magnet is obtained through a mixing step of mixing the above-mentioned isotropic magnet powder or anisotropic magnet powder with a binder, and a molding step of molding the mixed powder obtained by the mixing step.
  • the binder include a metal binder and the like in addition to the organic binder described above.
  • an organic binder such as a resin binder is generally used.
  • the resin used for the resin binder may be a thermosetting resin or a thermoplastic resin.
  • the mixing step may be a kneading step of kneading the magnet powder and the resin binder.
  • the molding process includes compression molding, injection molding, and extrusion molding.
  • anisotropic magnetic powder is formed in a magnetic field.
  • a thermosetting resin is used as the resin binder, a heating (curing) process is performed during the molding process or after the molding process.
  • La has the highest oxidation potential among rare earth elements, La
  • the magnet powder and the hard magnet containing manganese are suppressed from being oxidized and exhibit extremely excellent corrosion resistance.
  • the addition form of La for example, the following three forms can be considered.
  • the corrosion resistance and the like of the magnetic powder and the hard magnet can be improved. Therefore, in the present invention, the form of addition of La is not particularly considered.
  • La be present on the surface of the constituent particles of the magnet powder or in the vicinity thereof. . Therefore, it is more advantageous to mix La-based material after or during the production of the magnet powder and to diffuse La or the like into the surface or inside of the magnet powder, rather than including La in the magnet alloy from the beginning. is there.
  • the magnet powder obtained after the dehydrogenation step is mixed with a La-based material comprising at least one of La alone, a La alloy and a La compound.
  • a La-based material comprising at least one of La alone, a La alloy and a La compound.
  • the La mixture is heated to 673-1123 K to perform a diffusion heat treatment step of diffusing La on the surface and inside of the magnet powder, and the obtained isotropic magnet powder is 100 at% in total. It is preferable to contain La in a range of 0.001 to 1.0 at%.
  • This hydride (HFeBHx) is obtained by removing hydrogen from the RH 2 phase that has undergone three-phase decomposition in the hydrogenation step; and re-combining the polycrystal in which the crystal orientation of the Fe 2 B phase has been transferred, d- Obtained after the first evacuation step of HDDR processing.
  • the method for producing an anisotropic magnet powder of the present invention further comprises the step of adding a La simple substance, a La alloy, a La compound or a hydride thereof to the RFeB-based hydride obtained after the first evacuation step.
  • the second evacuation step is a step of removing hydrogen from the La treated material after the diffusion heat treatment step, or simultaneously performing the second evacuation step after the diffusion heat treatment step, or After the process, a diffusion heat treatment process is performed.
  • the anisotropic magnet powder obtained by such a method contains La of 0.001 to 1.0 at% when the whole is 100 at%.
  • the diffusion heat treatment step is a step of diffusing (or coating) La on the surface and inside of the RF eB-based magnet powder or: RF eB-based hydride.
  • This diffusion heat treatment step may be performed after the La-based material is mixed, or may be performed simultaneously with the mixing. If the treatment temperature is lower than 673 K, the La-based material is unlikely to be in a liquid phase and diffusion treatment is difficult. On the other hand, when the temperature exceeds 1123K, crystal grains such as RFeB-based magnet powder are grown, and iHc is reduced, so that it is not possible to sufficiently improve the corrosion resistance and the like (reduce the permanent demagnetization rate).
  • the processing time is preferably 0.5 to 5 hours.
  • the La-based material is as described above, but its form does not matter. However, from the viewpoint of efficiently and surely performing the manufacturing process of the magnet powder, it is preferable that they are in the form of powder.
  • the La alloy or the La compound is preferably an alloy or a compound (including an intermetallic compound) of La with a transition metal element (TM).
  • TM transition metal element
  • LaCo, LaNd Co, LaDyCo and the like are suitable because it can also increase the Curie point of the magnet powder. 6547
  • ingots (magnet alloys) having the compositions listed in Samples 1 to 10 in Table 1 or Table 2 were produced by melting. Further, as comparative examples, ingots having the compositions shown in Samples C1 to C6 in each table were produced by melting. The ingots produced are each about 3 ⁇ kg.
  • Table 1 and Table 2 differ in the treatment applied to each sample (ingot). That is, Table 1 shows a case where each sample was subjected to HDR treatment, and the magnetic powder shown in Table 1 is an isotropic magnet powder obtained through the treatment. The bonded magnets shown in Table 1 were manufactured from the isotropic magnet powder. Hereinafter, these are referred to as Example 1.
  • Table 2 shows the case where each sample was subjected to d-HDDR treatment.
  • the magnetic powder shown in Table 2 is an anisotropic magnet powder obtained by the treatment.
  • the bonded magnet shown in Table 2 was manufactured from the anisotropic magnet powder. Hereinafter, these are referred to as Example 2. [5].
  • the magnetic powders shown in Table 1 were applied to ingots with alloy compositions of Sample No. -1 to 10 and C1 to C6 without any heat treatment for homogenization. It was manufactured by subjecting it to HDDR treatment. That is, heat treatment was performed for 360 minutes in a hydrogen gas atmosphere consisting of the temperature and hydrogen pressure shown in Table 1 (hydrogenation step). Subsequently, vacuum was evacuated with a rotary pump and a diffusion pump for 60 minutes, followed by cooling in a vacuum atmosphere of 1 O ⁇ Pa or less (dehydrogenation step). In this way, about 10 kg of magnetic powder was produced per batch.
  • the magnetic powders shown in Table 2 were also subjected to a low-temperature hydrogenation process and a high-temperature hydrogenation without injecting any homogenizing heat treatment to ingots having the alloy compositions of samples No. 1 to 10 and C 1 to C6. It was manufactured by performing d-HDD R treatment consisting of a process, a first exhaust process, and a second exhaust process. That is, in a hydrogen gas atmosphere at room temperature and a hydrogen pressure of 100 kPa, hydrogen was sufficiently absorbed by each sample alloy (low-temperature hydrogenation i). Next, heat treatment was performed for 480 minutes in a hydrogen gas atmosphere at the temperature and hydrogen pressure shown in Table 2 (high-temperature hydrogenation process).
  • an epoxy resin (3 wt%) previously dissolved in bushnon was mixed with each magnetic powder. Then, the vacuum was evaporated to evaporate the non-metal, and pellets for bonded magnets were produced.
  • a similar pellet made from flake shaped MQP-B (manufactured by Magnequench In Yuichi National) manufactured by meltsbinning was also prepared. Then, the pellet was pressure-formed into a 7 mm cubic shape while being oriented in a magnetic field of 2.5 T to obtain a bonded magnet.
  • the magnetic powder was classified to a particle size of 75 to 106 m. Using the classified magnetic powder, it is molded so that the demagnetizing factor becomes 0.2, and after orientation in a magnetic field, it is magnetized at 4.57 MAm- and VSM (manufactured by Riken Electronics Sales Co., Ltd., BH-525H) The (BH) max and iHc were measured by means of. The results are shown in Tables 1 and 2.
  • the B amount is preferably 10.8 to 15 at% as described in the present invention.
  • ternary isotropic magnetic powder obtained by subjecting an alloy ingot differing only in the composition of B to HDDR treatment under the same conditions are shown in Table 1 in Examples (Sample Nos. 1 and 2) and Comparative Examples (Sample Nos. Comparison with C1 to C3) reveals the following.
  • the amount of B is small or large as in the comparative example, specifically, if the amount of B is out of the range of 10.8 to 15 at%, the maximum energy product (BH) max of the magnetic powder decreases. . In contrast, in the embodiment where there is a B amount within that range, 70 k Jm_ 3 more than big (BH) max is obtained. Thus, the peak value of (BH) max exists in the range of B: 10.8 to 15 at%.
  • the coercive force i He of the magnetic powder shows a tendency to increase as the B content increases.
  • the increasing tendency of iHc becomes very slow, and when the B content is 10.8 to: L5 at%, iHc is sufficient. Is obtained.
  • the (BH) max is about the same as that of the bonded magnet composed of MQP-B, but the iHc is about 5 We also know that it has improved by 0%.
  • ternary anisotropic magnetic powder obtained by subjecting an alloy ingot differing only in the composition of B to d-HDD R treatment under the same conditions and the examples shown in Table 2 (Sample Nos. 1 and 2) and Comparative Examples (Samples No. .C 1 to C 3), the following can be understood.
  • the maximum energy product (BH) max of the magnetic powder decreases when the B content is outside the range of 10.8 to 15 at%, even if the B content is small or large as in the comparative example.
  • a (BH) max as large as 210 kJm- 3 or more is obtained.
  • the peak value of (BH) max exists in the range of B: 10.8 to 15a1:%.
  • the coercive force i He of the magnetic powder shows a tendency to increase as the B content increases. However, in the range where the B content is 10.8 at% or more, the increasing tendency of iHc becomes very slow, and sufficient iHc is obtained when the B content is 10.8 to 15 at%. .
  • the intrinsic coercive force i Hc of the isotropic magnetic powder obtained by subjecting the ingots of sample Nos. 2 and 6 shown in Table 1 to HDD R treatment and the time of the hydrogenation step of the HDD R treatment (180 to 1 '800 minutes). Except for the time of the hydrogenation step, the production conditions of each magnetic powder are the same as in the HDDR treatment described in Example 1. Also, the method of measuring magnetic properties This is the same as in the first and second embodiments. Table 3 shows the results thus obtained.
  • D Specific coercive force iHc of anisotropic magnetic powder obtained by subjecting ingots of sample Nos. 2 and 6 shown in Table 2 to HDD R treatment, and d—time of high-temperature hydrogenation step in HDD R treatment ( 180-1800 minutes).
  • each magnetic powder is the same as those of the d-HDDR treatment described in Example 2.
  • the method for measuring the magnetic properties is also the same as in Examples 1 and 2. Table 4 shows the results thus obtained.
  • the fluidity and bulk density of the pellet were measured according to JIS Z8041 (JIS standard).
  • the fluidity and the bulk density were improved by about 20% and 10%, respectively, as compared with the case of the reference sample. This is considered to be because the particle shape of each magnetic powder of this example is close to spherical.
  • Heat treatment was performed in a hydrogen gas atmosphere of 1-1 OkPa for 160 minutes (first evacuation step). Finally, evacuate with a rotary pump and a diffusion pump for 60 minutes,
  • a bonded magnet was produced in the same manner as in Examples 1 and 2, and its (BH) max was measured. Then, the value obtained by dividing the measured (BH) max by the raw material cost (raw material cost, melting and manufacturing cost) subjected to d-HDDR processing is plotted as cost performance.
  • a bonded magnet was prepared in the same manner as in Sample 6, and the (BH) max was measured.
  • Figure 3 also shows the value obtained by dividing the measured (BH) max by the cost of the raw material subjected to d_HDDR processing (raw material cost, melting cost, and homogenization heat treatment cost). .
  • Example 1 The alloy ingots of samples No. 1 and No. 6 in Table 1 were subjected to the same HDR treatment as in Example 1 to produce isotropic magnetic powder.
  • This isotropic magnetic powder was mixed with La80 Co20 alloy powder (La-based material) (mixing step) and heated (diffusion heat treatment step) to obtain sample Nos. 11 to 15 and 15 shown in Tables 5 and 6.
  • Magnetic powders of Sample Nos. 16 and 17 were obtained.
  • the composition of each sample shown in Tables 5 and 6 is based on the ICP after the diffusion heat treatment step.
  • Table 5 also shows the diffusion heat treatment conditions for each sample.
  • the diffusion heat treatment conditions in Table 6 are all 1073 Kx lhr.
  • the mixing step and the diffusion heat treatment process all 10- 2 P a following Performed in a lower vacuum atmosphere.
  • Table 6 also shows, as an example, the magnetic properties of the isotropic magnet powder of sample No. 16, 16 and the bonded magnet using the same. The measuring method is as described above.
  • the La 80 Co 20 alloy is an alloy of La: 80 at% and Co: 20 at%, and is melted similarly to the case of the magnet alloy (ingot) of the first embodiment.
  • the powder was obtained by crushing the ingot by a hydrogen crushing method and pulverizing the powder by a vibration mill, and the average particle size was 10 im.
  • a 7 mm square isotropic bonded magnet was produced in the same manner as in Example 1. Using this bonded magnet, the permanent demagnetization rate was measured. Permanent demagnetization rate is calculated from the difference between the initial magnetic flux of the bonded magnet and the magnetic flux obtained by re-magnetizing after holding for 1000 hours in the atmosphere of 1 ° C or 80 ° C for 1000 hours. It is the ratio to the magnetic flux. The magnetization was performed in 1. IMAZm (45 kO e). A flux meter was used to measure the magnetic flux. Tables 5 and 6 show the permanent demagnetization rates obtained in this way.
  • the isotropic bonded magnets according to the present invention have low permanent demagnetization ratio, excellent heat resistance, and high practicality.
  • a small permanent demagnetization rate means that it has excellent corrosion resistance and little aging.
  • the permanent demagnetization rate is as low as less than 10%. In the case of 8 CTCx 1000 hours, the permanent demagnetization rate is as small as about 5%.
  • the permanent magnetic susceptibility was as high as about 1 ⁇ % at 80 ° C for 1000 hours, and as high as about 15% at 100 ° C for 1000 hours. It is getting higher.
  • isotropically produced by rapid solidification method Table 5 also shows the permanent demagnetization rate of the powder (MQP-B).
  • the magnetic properties of the magnetic powder and the bonded magnets were equivalent to the results shown in Table 1 of the examples, or were reduced by only about 7 to 8% at the maximum, and were at a level with no practical problems. .
  • Example 7 (RF eB hydride) was obtained.
  • the same La80Co0.2 alloy powder as in Example 7 was mixed with the NdFeB powder (mixing step) and heated (diffusion heat treatment step). In connection with this, the same second exhaust process as in Example 2 was performed.
  • Tables 7 and 8 show magnetic powders of Sample Nos. 11 to 15 and Samples No. 16 and 17 shown in Tables 7 and 8 .
  • the composition of each sample shown in Tables 7 and 8 is a value analyzed by ICP after the second evacuation step, as in Example 7.
  • Table 7 also shows the diffusion heat treatment conditions for each sample.
  • the diffusion heat treatment conditions in Table 8 are all 107 Kl hr.
  • the mixing step and the diffusion heat treatment step was performed in all 1 0- 2 P a time in a vacuum atmosphere.
  • Table 8 also shows, as an example, the magnetic properties of the anisotropic magnet powders of Sample Nos. 16 and 17, and the bonded magnets using the same. The measuring method and the like are as described above.
  • Tables 7 and 8 also show the permanent demagnetization rates obtained in the same manner as in Example 7.

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Abstract

L'invention concerne un alliage utilisé dans un aimant lié, caractérisé en ce qu'il comprend du fer (Fe) comme composant primaire, 12 à 16 % en poids atomique d'un élément des terres rares (R) comprenant de l'yttrium (Y) et 10,8 à 15 % en poids atomique de bore (B). La poudre d'aimant produite par soumission de l'alliage d'aimant précité à un traitement d-HDDR ou analogue peut fournir des pastilles alimentant plus facilement un moule afin de former un aimant lié, ce qui permet de réduire un aimant lié présentant d'excellentes caractéristiques magnétiques à un coût réduit.
PCT/JP2002/006547 2002-04-09 2002-06-28 Alliage utilise dans un aimant lie, poudre d'aimant isotrope et anisotrope et son procede de production, et aimant lie WO2003085147A1 (fr)

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AU2002346234A AU2002346234A1 (en) 2002-04-09 2002-06-28 Alloy for use in bonded magnet, isotropic magnet powder and anisotropic magnet powder and method for production thereof, and bonded magnet
US10/182,724 US6955729B2 (en) 2002-04-09 2002-06-28 Alloy for bonded magnets, isotropic magnet powder and anisotropic magnet powder and their production method, and bonded magnet
JP2003582322A JP3565513B2 (ja) 2002-04-09 2002-06-28 ボンド磁石用合金、等方性磁石粉末および異方性磁石粉末とそれらの製造方法並びにボンド磁石

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006173170A (ja) * 2004-12-13 2006-06-29 Ricoh Co Ltd 圧縮成形用磁性粉、圧縮成形用磁石コンパウンド、長尺磁石成形体、マグネットローラ、現像剤担持体、現像装置、及び、画像形成装置
EP3514807A1 (fr) 2018-01-22 2019-07-24 Nichia Corporation Procédé de production d'un composite pour aimants lié, et composite pour aimants liés
EP3675143A1 (fr) 2018-12-28 2020-07-01 Nichia Corporation Procédé de préparation d'un aimant lié et aimant lié

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JPH06128610A (ja) * 1992-09-02 1994-05-10 Sumitomo Special Metals Co Ltd 永久磁石用異方性希土類合金粉末の製造方法
JPH07188704A (ja) * 1993-12-27 1995-07-25 Showa Denko Kk 希土類永久磁石用合金粉末及びその製造法
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006173170A (ja) * 2004-12-13 2006-06-29 Ricoh Co Ltd 圧縮成形用磁性粉、圧縮成形用磁石コンパウンド、長尺磁石成形体、マグネットローラ、現像剤担持体、現像装置、及び、画像形成装置
JP4571852B2 (ja) * 2004-12-13 2010-10-27 株式会社リコー 圧縮成形用磁性粉、圧縮成形用磁石コンパウンド、長尺磁石成形体、マグネットローラ、現像剤担持体、現像装置、及び、画像形成装置
EP3514807A1 (fr) 2018-01-22 2019-07-24 Nichia Corporation Procédé de production d'un composite pour aimants lié, et composite pour aimants liés
EP3675143A1 (fr) 2018-12-28 2020-07-01 Nichia Corporation Procédé de préparation d'un aimant lié et aimant lié

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