EP0478674A1 - Method for preparing permanent magnets based on neodymium-iron-boron. - Google Patents
Method for preparing permanent magnets based on neodymium-iron-boron.Info
- Publication number
- EP0478674A1 EP0478674A1 EP19900910143 EP90910143A EP0478674A1 EP 0478674 A1 EP0478674 A1 EP 0478674A1 EP 19900910143 EP19900910143 EP 19900910143 EP 90910143 A EP90910143 A EP 90910143A EP 0478674 A1 EP0478674 A1 EP 0478674A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- alloy
- neodymium
- iron
- atoms
- copper
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
- H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
- H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
- H01F1/0576—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together pressed, e.g. hot working
Definitions
- the present invention relates to a new improved process for the preparation of high performance permanent magnets based on Neodymium-Iron-Boron. It relates more particularly to a process for manufacturing permanent magnets by the technical process known as wrought.
- mechanical working means a mechanical treatment applied to a metal alloy and intended to cause refinement of the constituent grains of the alloy.
- the wrought is then defined by its wrought rate.
- the mechanical treatments liable to induce corroya ⁇ ge are essentially forging, hammering, rolling, spinning, vibro-compaction (compaction by vibra ⁇ tion), etc.
- Praseodymium is much rarer on the earth's surface than Neodymium, hence the cost price of magnets based on Praseodymium much higher (typically in a ratio of 5 to 1 compared to Neodymium).
- the present invention relates to a perfected process for the preparation of high performance permanent magnets from a solid alloy containing a mixture based on Fer-Boron and Neodymium which, for a temperature range, has a inside which said alloy is in two phases, one solid and fragile and the other liquid, a process which consists of:
- the present invention consists in replacing, in a solid alloy based on Neodymium-Iron-Boron, some of the Iron and / or Neodymium atoms with Copper atoms, and then subjecting this alloy to a treatment hot working. While the use of copper was known per se with a view to improving certain magnetic properties, on the other hand, it was clearly shown that the use of copper in an iron-boron alloy of rare earth, in which rare earth was Neodymium did not make it possible to obtain permanent magnets with high magnetic properties.
- the alloy comprises from 0.5 to 4 atomic% of Cui ⁇ vre; it has in fact been found that if the atomic amount of copper is less than 0.5%, a fall in the magnetic properties of the magnet thus produced is observed. In other words, there was no noticeable improvement compared to the magnets obtained according to the method described in European patent EP-A-0 269 667. On the other hand, if the amount of copper exceeds 4 atomic%, the remanence is affected due to the decrease in the amount of magnetic material;
- the alloy contains from 1 to 2.5 atomic% of copper, preferably 2%;
- the alloy based on Neodymium-Iron-Boron-Copper also carries Dysprosium (Dy); - Dysprosium is present at a rate of 0.5% to 2 atomic%.
- the installation according to the invention comprises an anvil (1), on which rests a retaining ring (2), surrounded by an enclosure glass (3), defining a sealed chamber (4), connected to the inlet (5) of a source of argon not shown.
- the top of the chamber has an opening (6) through which the hammer (7) of the exterior impact assembly (8) can pass, by means of a seal sealing (9).
- the sample (10) rests on the anvil (1) inside the ring (2) in which the hammer (7) slides.
- the glass enclosure (3) is surrounded by induction coils (11).
- a massive sample is prepared (washer, cylin ⁇ dre, molded ..., shot) in an alloy constituted by a mixture of Iron, Neodymium, Boron and Aluminum.
- the atomic concentration for 100 alloy atoms of the different elements is:
- An annealing is then carried out under neutral gas, or possibly under vacuum, at a temperature of 650 ° C.
- the magnetic element thus obtained has an intrinsic coercive field of 756 kilo-amperes per meter (756 kA / m) and a residual induction of 0.8 Tesla.
- the internal energy obtained in this case is of the order of 103.5 kilojoules per cubic meter (103.5 kJ / m 3 ).
- Example 2 The element obtained has in known manner a quadratic crystal structure.
- Example 2 The element obtained has in known manner a quadratic crystal structure.
- Example 1 is repeated but in which the two aluminum atoms are replaced by two cobalt atoms.
- the sample is subjected to the same treatment.
- the role of Cobalt is essentially to increase the Curie temperature, therefore the temperature of use of the permanent magnets thus produced.
- Example 1 is repeated but in which the basic alloy is no more than a ternary mixture of Neodymium, Iron and Boron.
- the atomic composition for 100 atoms of the mixture is:
- the intrinsic coercive field obtained is then 600 kA / m and the residual induction of 0.9 Tesla.
- the internal energy obtained is in this case close to 95.5 kJ / m 3 .
- Permanent magnets are then produced by the process known as "hot pressing".
- the production process and the composition of the base alloy are described in the publication (SHIMODA et al) mentioned above J.Appl. Phy. 64 (10). This example and the following two are given for comparison.
- the atomic percentage composition of the basic mixture is: - 17 Praseodymium atoms
- the intrinsic coercive field obtained is 800kA / m and the residual induction of 1.25 Tesla.
- the internal energy obtained is 288 kJ / m 3 .
- centesimal composition of the initial mixture is:
- the intrinsic coercive field obtained is 230kA / m and the residual induction of 0.19 Tesla.
- the internal energy obtained is 72.8 kJ / m 3 .
- the intrinsic coercive field obtained is 950 kA / m and the residual induction of 1.01 Tesla. In this way, an internal energy close to 200 kJ / m 3 is obtained. This gives excellent permanent anistropic magnets with very high performance.
- the intrinsic coercive field obtained is 835kA / m for a residual induction of 1.15 Tesla.
- the internal magnetic energy obtained is then 238 kJ / m 3 .
- the magnetic properties obtained are slightly lower than the two previous examples, in fact there is an intrinsic coercive field of 800 kA / m for a residual induction of 1 Tesla, the internal magnetic energy obtained being 159 kJ / m 3 .
- the intrinsic coercive field obtained is then 835 kA / m for a residual induction of 0.95 Tesla.
- the maximum internal energy obtained is 243 kJ / m 3 . It is therefore observed in the context of the strict use of the four elements Neodymium-Iron-Boron-Copper, that the maximum of the magnetic properties is located for a centesimal atomic concentration of Copper close to 2.
- the temperature of the wrought is at least equal to 500 ° C. in order to be situated at least at the level of the melting of the Neodymium-Copper eutectic. However, it was found that around 800 ° C., the results were appreciably the best. These different results are grouped in the following table.
- Dysprosium at a rate of 0.5 to 2 atomic%, in particular in the context of the use of these magnets at higher temperatures. Indeed, the latter makes it possible to increase the coercivity therefore the operating temperature of the magnets obtained.
- the process according to the invention has many advantages over the process mentioned in the preamble.
- the cost price of such magnets can be reduced by a factor of 5.
- this process using a Neodymium-Iron-Boron-Copper base mixture makes it possible to obtain permanent magnets of reduced cost, with high magnetic performance, and capable of being produced in quantity. easily.
Landscapes
- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Hard Magnetic Materials (AREA)
Abstract
Procédé pour la préparation d'aimants permanents à partir d'un alliage massif contenant un mélange à base de Néodyme-Fer-Bore qui, pour une gamme de température, présente un domaine à l'intérieur duquel ledit alliage se trouve sous deux phases, l'une solide et fragile et l'autre liquide, caractérisé en ce qu'il consiste: à substituer partiellement des atomes de fer et/ou de néodyme dudit alliage par des atomes de cuivre, puis, à corroyer le nouvel alliage ainsi réalisé à une température comprise dans ladite gamme de température, pour obtenir un taux de corroyage d'au moins dix, de manière à affiner les grains constitutifs de l'alliage en particules de quelques micromètres; et enfin, à soumettre l'alliage ainsi corroyé à un traitement de recuit et/ou de revenu.Process for the preparation of permanent magnets from a solid alloy containing a mixture based on Neodymium-Iron-Boron which, for a temperature range, has a range within which said alloy is in two phases, one solid and fragile and the other liquid, characterized in that it consists in: partially replacing iron and / or neodymium atoms of said alloy with copper atoms, then, to correct the new alloy thus produced to a temperature included in said temperature range, in order to obtain a wrought rate of at least ten, so as to refine the grains constituting the alloy into particles of a few micrometers; and finally, to subject the alloy thus wrought to an annealing and / or tempering treatment.
Description
Claims
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
AT90910143T ATE91564T1 (en) | 1989-06-23 | 1990-06-21 | PROCESS FOR THE MANUFACTURE OF PERMANENT MAGNETS BASED ON NEODYMIUM-IRON-BORON. |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR8908657 | 1989-06-23 | ||
FR8908657A FR2648948B1 (en) | 1989-06-23 | 1989-06-23 | IMPROVED PROCESS FOR THE PREPARATION OF HIGH PERFORMANCE PERMANENT MAGNETS BASED ON NEODYME-FER-BORE |
Publications (2)
Publication Number | Publication Date |
---|---|
EP0478674A1 true EP0478674A1 (en) | 1992-04-08 |
EP0478674B1 EP0478674B1 (en) | 1993-07-14 |
Family
ID=9383235
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP90910143A Expired - Lifetime EP0478674B1 (en) | 1989-06-23 | 1990-06-21 | Method for preparing permanent magnets based on neodymium-iron-boron |
Country Status (6)
Country | Link |
---|---|
US (1) | US5356489A (en) |
EP (1) | EP0478674B1 (en) |
JP (1) | JPH05503810A (en) |
DE (1) | DE69002236T2 (en) |
FR (1) | FR2648948B1 (en) |
WO (1) | WO1991000602A1 (en) |
Families Citing this family (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR2779267B1 (en) * | 1998-05-28 | 2000-08-11 | Rhodia Chimie Sa | PROCESS FOR PREPARING A MAGNETIC MATERIAL BY FORGING AND MAGNETIC MATERIAL IN POWDER FORM |
US6277211B1 (en) * | 1999-09-30 | 2001-08-21 | Magnequench Inc. | Cu additions to Nd-Fe-B alloys to reduce oxygen content in the ingot and rapidly solidified ribbon |
CN104766717B (en) * | 2014-01-07 | 2018-12-07 | 中国科学院宁波材料技术与工程研究所 | A method of improving sintered Nd-Fe-B permanent magnet magnetic property |
CN105097261B (en) * | 2015-08-20 | 2018-06-26 | 京磁新材料有限公司 | A kind of sintering method of neodymium iron boron magnetic body |
CN106392077B (en) * | 2016-10-09 | 2019-03-19 | 中国核动力研究设计院 | A kind of preparation method of high-boron stainless steel plate |
Family Cites Families (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO1988006797A1 (en) * | 1987-03-02 | 1988-09-07 | Seiko Epson Corporation | Rare earth element-iron base permanent magnet and process for its production |
CA1269029A (en) * | 1986-01-29 | 1990-05-15 | Peter Vernia | Permanent magnet manufacture from very low coercivity crystalline rare earth-transition metal-boron alloy |
FR2598949B1 (en) * | 1986-05-23 | 1989-08-04 | Centre Nat Rech Scient | PROCESS FOR THE PREPARATION OF FINELY DIVIDED CRYSTALS FROM A METAL ALLOY, IN PARTICULAR FOR THE PREPARATION OF PERMANENT MAGNETS |
-
1989
- 1989-06-23 FR FR8908657A patent/FR2648948B1/en not_active Expired - Fee Related
-
1990
- 1990-06-21 WO PCT/FR1990/000452 patent/WO1991000602A1/en active IP Right Grant
- 1990-06-21 US US07/777,547 patent/US5356489A/en not_active Expired - Fee Related
- 1990-06-21 EP EP90910143A patent/EP0478674B1/en not_active Expired - Lifetime
- 1990-06-21 JP JP2509401A patent/JPH05503810A/en active Pending
- 1990-06-21 DE DE90910143T patent/DE69002236T2/en not_active Expired - Fee Related
Non-Patent Citations (1)
Title |
---|
See references of WO9100602A1 * |
Also Published As
Publication number | Publication date |
---|---|
FR2648948B1 (en) | 1993-12-31 |
JPH05503810A (en) | 1993-06-17 |
DE69002236D1 (en) | 1993-08-19 |
DE69002236T2 (en) | 1993-10-28 |
WO1991000602A1 (en) | 1991-01-10 |
EP0478674B1 (en) | 1993-07-14 |
FR2648948A1 (en) | 1990-12-28 |
US5356489A (en) | 1994-10-18 |
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