EP0499600A1 - Aimant permanent fritté ou une matière première pour cet aimant et son procédé de fabrication - Google Patents
Aimant permanent fritté ou une matière première pour cet aimant et son procédé de fabrication Download PDFInfo
- Publication number
- EP0499600A1 EP0499600A1 EP92890030A EP92890030A EP0499600A1 EP 0499600 A1 EP0499600 A1 EP 0499600A1 EP 92890030 A EP92890030 A EP 92890030A EP 92890030 A EP92890030 A EP 92890030A EP 0499600 A1 EP0499600 A1 EP 0499600A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- sse
- magnetic phase
- phase
- concentration
- grain
- 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
- 238000000034 method Methods 0.000 title claims abstract description 27
- 230000008569 process Effects 0.000 title claims abstract description 11
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 9
- 239000000696 magnetic material Substances 0.000 title description 5
- 230000005291 magnetic effect Effects 0.000 claims abstract description 59
- 239000000463 material Substances 0.000 claims abstract description 21
- 238000009792 diffusion process Methods 0.000 claims abstract description 17
- 230000000694 effects Effects 0.000 claims abstract description 6
- 239000000843 powder Substances 0.000 claims description 19
- 239000000654 additive Substances 0.000 claims description 18
- 229910045601 alloy Inorganic materials 0.000 claims description 10
- 239000000956 alloy Substances 0.000 claims description 10
- 238000005245 sintering Methods 0.000 claims description 10
- 230000000996 additive effect Effects 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 6
- 150000002910 rare earth metals Chemical class 0.000 claims description 5
- 229910002546 FeCo Inorganic materials 0.000 claims description 4
- 238000000137 annealing Methods 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 3
- 238000009826 distribution Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 238000002844 melting Methods 0.000 claims description 3
- 230000008018 melting Effects 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 238000005275 alloying Methods 0.000 claims description 2
- 238000005266 casting Methods 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- 239000012535 impurity Substances 0.000 claims description 2
- 238000005272 metallurgy Methods 0.000 claims description 2
- 238000000465 moulding Methods 0.000 claims description 2
- 239000000470 constituent Substances 0.000 claims 2
- 229910052738 indium Inorganic materials 0.000 claims 1
- 229910052751 metal Inorganic materials 0.000 claims 1
- 239000002184 metal Substances 0.000 claims 1
- 150000001247 metal acetylides Chemical class 0.000 claims 1
- 150000004767 nitrides Chemical class 0.000 claims 1
- 150000002902 organometallic compounds Chemical class 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 4
- 230000003247 decreasing effect Effects 0.000 abstract 1
- 239000012071 phase Substances 0.000 description 23
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 8
- 230000005415 magnetization Effects 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 4
- 230000007423 decrease Effects 0.000 description 4
- 229910052796 boron Inorganic materials 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 2
- 230000005290 antiferromagnetic effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000005294 ferromagnetic effect Effects 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 230000005298 paramagnetic effect Effects 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 238000012935 Averaging Methods 0.000 description 1
- 229910052692 Dysprosium Inorganic materials 0.000 description 1
- 229910000640 Fe alloy Inorganic materials 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- 229910052777 Praseodymium Inorganic materials 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 1
- 235000011837 pasties Nutrition 0.000 description 1
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000004627 transmission electron microscopy Methods 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
Images
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
- H01F1/0577—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 sintered
Definitions
- the invention relates to a sintered permanent magnet (material) according to the preamble of claim 1.
- the invention further relates to a method for producing permanent magnets (materials) according to the preamble of claim 6.
- Permanent magnets or permanent magnet materials made essentially of an alloy of iron (Fe), boron (B) and rare earths (SE) in the sintering process are preferably used when high coercive force, high remanence and / or large energy product are required.
- the component which forms or contains the magnetic phase of the SE2Fe14B type is melt-metallurgically produced and pulverized, which powder, optionally mixed with additives, is pressed into a green compact in the magnetic field and sintered, the sintered body optionally being subjected to at least one further heat treatment.
- EP-B1-0126802 discloses sintered permanent magnets of the Fe-B-R type (R means at least one SE element including Y), in which Fe can be partially replaced by Co.
- R means at least one SE element including Y
- Fe can be partially replaced by Co.
- the elements are in due to the manufacturing process used the magnetic phase is homogeneously distributed and a heat or aging treatment of the sintered body is said to improve the magnetic values. If Fe is partially replaced by Co, this increases the Curie point or the Curie temperature (T c ) of the magnetic material, the coercive force of which, as is known to the person skilled in the art, however, decreases with increasing Co content, which also results in the energy product can be adversely affected.
- the invention has for its object to eliminate the disadvantages of the known RE-containing magnets (materials) and their manufacturing processes and to create sintered permanent magnets that have high saturation magnetization, high coercive force and large energy product with good temperature stability and high Curie point. It is also an object of the invention to provide a new and improved manufacturing method for magnets, with which high magnetic characteristics can be achieved and their scatter can be reduced.
- grains of the magnetic phase are surface-smoothed or their surface energy is reduced or minimized by diffusion molding in sinter-active or grain-connecting phases and have a diameter of at most 60 ⁇ m, but at least 3 ⁇ m.
- grain surfaces designed in this way energetically, a domain wall formation and / or shift at least made difficult, which generally leads to an improvement in the coercive force values.
- a corresponding grain size of the magnetic phase is of great importance because, as has been found, grain diameters of greater than 60 ⁇ m and less than 3 ⁇ m lead to a drop in the coercive force or the magnetic induction.
- a special feature of the new permanent magnet (material) according to the invention is a partial replacement of iron (Fe) by cobalt (Co) in the magnetic phase formed with boron (B) and light rare earths (LSE) and heavy rare earths (SSE) , where the average SSE content is set at a certain value depending on the concentration value of Co. It is known that Co contents cause a slight increase in magnetization and an increase in the Curie point, but the coercive force or magnetic inductance is reduced, which leads to a lower energy product (BH max ) of the magnet and thus to a deterioration in all of the magnetic properties.
- BH max lower energy product
- LSE magnetic moments of LSE, in particular the advantageously usable elements neodymium (Nd) and praseodymium (Pr), are aligned parallel to Fe or ferromagnetic and the SSE has an antiparallel direction to Fe or an antiferromagnetic direction of its have magnetic moments.
- SSE Dysprosium (Dy) has been shown to be particularly effective and advantageous because, among other things, the anisotropy field strength increases strongly due to the antiferro- magnetic coupling.
- the SSE content be at least 0.05 times the Co content because lower concentrations cause a reduction in the coercive force.
- SSE contents higher than 0.2 times the Co content lead to a decrease in the saturation magnetization.
- the local concentration of SSE atoms is also inhomogeneous across the cross-section of the grains, in particular increasing in the direction of the surface-smoothed grain boundary, domain wall formation and / or domain wall displacement is further reduced, as a result of which the coercive force and the result of the energy product are further increased .
- An at least 3 times higher concentration of SSE atoms in a range of at most 1 ⁇ m at the grain boundary has proven to be particularly effective.
- Another particularly important characteristic of the new permanent magnet according to the invention is a higher SSE content than the hard magnetic phase and / or a higher activity of the SSE at the diffusion temperature of the sinter-active or grain-connecting, essentially paramagnetic phase.
- Good magnetic values are preferably obtained if the SE concentration of this grain-connecting phase is greater by at least 25% and its SSE concentration by at least 90% than that of the magnetic phase on average.
- the hard magnetic phase of the type SE2 (FeCo) 14 B forming or containing component by melting and casting an alloy with 8 to 30 at.% SE, consisting of LSE and SSE, 2 to 28 at.% B , 3 to 25 at.% Co, remainder iron and optionally further alloying elements and impurities produced and to powder with a grain size crushed between 60 ⁇ m and 3 ⁇ m.
- Additives containing at least one SSE element, preferably to an extent of 5 to 15% by weight, are introduced into this powder and distributed homogeneously.
- additives In order to bring the surface of the powder grains and the additives into good contact with one another, it is necessary for solid additives to provide their particle diameter below 5 .mu.m or less than 15% of the diameter of the powder grains and, if appropriate, a further grinding process.
- the additives can also be introduced into the powder in liquid form, for example as SE compounds.
- the SS content as a function of the Co content is adjusted in a range from 0.02 to 0.19 times the Co content by the melt metallurgical route.
- the SSE content of the additive is intended to be at least 100% greater than that of the powder.
- a green compact is pressed from the material formed from powder with the additives and is preferably sintered in a vacuum or, if appropriate, in a protective gas atmosphere at high temperature.
- the additives become at least partially liquid or pasty, essentially envelop the grains and act as a sinter-active or grain-connecting agent which largely fills the edges and fissures in and between the grains.
- the sintering temperature is selected so high for a short time that the sintering agent is given a sufficient degree of liquid to in particular fill or envelop the fissures and sharp-edged concave cavities of the grain surfaces.
- the sintered body is subjected to a diffusion treatment or diffusion annealing at a temperature below the sintering temperature with a temperature between 600 and 1100 ° C. and a period of 1 to 12 hours.
- the sinter-active or grain-connecting phase or mass has a sufficient degree of strength for shape stabilization.
- a Diffusion treatment of the sintered body which can be directly connected to the sintering, achieves surface structures and concentration profiles of atoms which are advantageous for the grains for the magnetic properties.
- the surfaces of the grains forming or containing the hard magnetic phase which are made sharp-edged by the comminution process, are smoothed because the edges or tips represent energetic irregularities and an increased atom diffusion takes place in these areas.
- a shaping of the grains or a largely directed atom diffusion brings about a reduction or minimization of their surface energy. Due to smoothed surfaces with reduced energy of the grains from the hard magnetic phase, a new formation of domain walls, which preferably occurs at the tips and edges, is effectively reduced in relation to the change in direction of the magnetic moments, and thus the coercive force of the magnets is increased.
- a certain grain size specified above and a sufficient filling, in particular the fissures and sharp-edged concave cavities of the grain surfaces with sinter-active mass or phase are important.
- SSE atoms Due to the set difference in concentration of SSE atoms in the hard magnetic phase and the grain-connecting, largely paramagnetic phase, SSE atoms also penetrate into the magnetocrystalline phase during the diffusion treatment. Because in the case of elements diffused in, such as AL, for example, a rapid, essentially immediate, concentration equalization takes place, it was surprising that SSE atoms at the grain boundaries or in the region near the grain boundaries can be enriched to at least 3 times the content and one inhomogeneous concentration of SSE atoms can be formed in the grains. It is important to choose the diffusion treatment parameters in such a way that the thickness of the area of the increased SSE concentration is set to at least 0.05 ⁇ m, but at most 1 ⁇ m. Smaller strengths cause only an insignificant further reduction in the formation of domain walls and / or domain wall mobility, thus a slight increase in coercive force; greater strengths reduce the achievable saturation magnetization and reduce the energy product of the permanent magnet.
- Table 1 shows the magnetic values of reference magnets (materials) with different compositions.
- the respective starting material was produced by melt metallurgy and ground into powder. Under the influence of a magnetic field, the powder was pressed into a green body, which was sintered, heat-treated and magnetized.
- the composition and the measured magnetic values of the permanent magnet bodies are given under the designations A to F in Table 1.
- the permanent magnets (materials) according to the invention are listed under numbers 1 to 14 in Table 2.
- the analytical determinations were carried out by transmission electron microscopy (TEM).
- TEM transmission electron microscopy
- the SSE content in the magnetic phase on average was determined by averaging from point and area measurements over the grain cross section.
- the Co content and the magnetic field strength or magnetization are increased by the Co content and, as has been shown, the coercive force or induction is kept at high values as a result of the further measures, which synergistically brings about an increased energy product .
- conventional magnets largely without Co content, high coercive forces become low at low Curie temperatures and at high Co content high magnetization achieved at high Curie temperatures.
- the magnetic energy product is relatively low in both cases.
Landscapes
- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Hard Magnetic Materials (AREA)
- Powder Metallurgy (AREA)
- Manufacturing Cores, Coils, And Magnets (AREA)
- Compounds Of Iron (AREA)
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| AT287/91 | 1991-02-11 | ||
| AT0028791A AT398861B (de) | 1991-02-11 | 1991-02-11 | Gesinterter permanentmagnet(-werkstoff) sowie verfahren zu dessen herstellung |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| EP0499600A1 true EP0499600A1 (fr) | 1992-08-19 |
| EP0499600B1 EP0499600B1 (fr) | 1994-11-23 |
Family
ID=3486534
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP92890030A Expired - Lifetime EP0499600B1 (fr) | 1991-02-11 | 1992-02-10 | Aimant permanent fritté ou une matière première pour cet aimant et son procédé de fabrication |
Country Status (6)
| Country | Link |
|---|---|
| EP (1) | EP0499600B1 (fr) |
| AT (2) | AT398861B (fr) |
| CZ (1) | CZ281161B6 (fr) |
| DE (1) | DE59200795D1 (fr) |
| HU (1) | HU213284B (fr) |
| PL (1) | PL169844B1 (fr) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE4331563A1 (de) * | 1992-09-18 | 1994-03-24 | Hitachi Metals Ltd | Nd-Fe-B-Sintermagnete |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0265006A1 (fr) * | 1986-10-13 | 1988-04-27 | Koninklijke Philips Electronics N.V. | Méthode de fabrication d'un aimant permanent |
| EP0126802B1 (fr) * | 1983-05-25 | 1988-12-14 | Sumitomo Special Metals Co., Ltd. | Procédé de fabrication d'un aimant permanant |
| EP0344542A2 (fr) * | 1988-06-03 | 1989-12-06 | Masato Sagawa | Aimant fritté de Nd-Fe-B et son procédé de fabrication |
| EP0389626A1 (fr) * | 1988-06-03 | 1990-10-03 | Mitsubishi Materials Corporation | AIMANT FRITTE A BASE D'UN ALLIAGE DE B-Fe-ELEMENTS DE TERRES RARES ET PROCEDE DE PRODUCTION |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA1316375C (fr) * | 1982-08-21 | 1993-04-20 | Masato Sagawa | Materiaux magnetiques et aimants permanents |
| AT393177B (de) * | 1989-04-28 | 1991-08-26 | Boehler Gmbh | Permanentmagnet(-werkstoff) sowie verfahren zur herstellung desselben |
-
1991
- 1991-02-11 AT AT0028791A patent/AT398861B/de not_active IP Right Cessation
-
1992
- 1992-02-10 PL PL92293427A patent/PL169844B1/pl unknown
- 1992-02-10 AT AT92890030T patent/ATE114383T1/de not_active IP Right Cessation
- 1992-02-10 CZ CS92392A patent/CZ281161B6/cs unknown
- 1992-02-10 HU HU9200403A patent/HU213284B/hu not_active IP Right Cessation
- 1992-02-10 EP EP92890030A patent/EP0499600B1/fr not_active Expired - Lifetime
- 1992-02-10 DE DE59200795T patent/DE59200795D1/de not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0126802B1 (fr) * | 1983-05-25 | 1988-12-14 | Sumitomo Special Metals Co., Ltd. | Procédé de fabrication d'un aimant permanant |
| EP0265006A1 (fr) * | 1986-10-13 | 1988-04-27 | Koninklijke Philips Electronics N.V. | Méthode de fabrication d'un aimant permanent |
| EP0344542A2 (fr) * | 1988-06-03 | 1989-12-06 | Masato Sagawa | Aimant fritté de Nd-Fe-B et son procédé de fabrication |
| EP0389626A1 (fr) * | 1988-06-03 | 1990-10-03 | Mitsubishi Materials Corporation | AIMANT FRITTE A BASE D'UN ALLIAGE DE B-Fe-ELEMENTS DE TERRES RARES ET PROCEDE DE PRODUCTION |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE4331563A1 (de) * | 1992-09-18 | 1994-03-24 | Hitachi Metals Ltd | Nd-Fe-B-Sintermagnete |
Also Published As
| Publication number | Publication date |
|---|---|
| DE59200795D1 (de) | 1995-01-05 |
| HU9200403D0 (en) | 1992-04-28 |
| AT398861B (de) | 1995-02-27 |
| PL293427A1 (en) | 1992-10-19 |
| HU213284B (en) | 1997-04-28 |
| PL169844B1 (pl) | 1996-09-30 |
| CZ39292A3 (en) | 1993-12-15 |
| HUT64108A (en) | 1993-11-29 |
| EP0499600B1 (fr) | 1994-11-23 |
| ATA28791A (de) | 1994-06-15 |
| CZ281161B6 (cs) | 1996-07-17 |
| ATE114383T1 (de) | 1994-12-15 |
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