EP0712532B1 - alliage SmFeTa à adjonction de 4-5 at% Ta et le procédé de sa préperation - Google Patents
alliage SmFeTa à adjonction de 4-5 at% Ta et le procédé de sa préperation Download PDFInfo
- Publication number
- EP0712532B1 EP0712532B1 EP95907498A EP95907498A EP0712532B1 EP 0712532 B1 EP0712532 B1 EP 0712532B1 EP 95907498 A EP95907498 A EP 95907498A EP 95907498 A EP95907498 A EP 95907498A EP 0712532 B1 EP0712532 B1 EP 0712532B1
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- Prior art keywords
- alloy
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- addition
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 43
- 239000000956 alloy Substances 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 15
- 229910052715 tantalum Inorganic materials 0.000 title claims description 14
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 68
- 229910052742 iron Inorganic materials 0.000 claims abstract description 16
- 238000002360 preparation method Methods 0.000 claims abstract description 15
- 239000000463 material Substances 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 10
- 230000005294 ferromagnetic effect Effects 0.000 claims abstract description 5
- 238000002844 melting Methods 0.000 claims description 5
- 230000008018 melting Effects 0.000 claims description 3
- 229910001362 Ta alloys Inorganic materials 0.000 claims description 2
- 230000008020 evaporation Effects 0.000 claims description 2
- 238000001704 evaporation Methods 0.000 claims description 2
- 230000005291 magnetic effect Effects 0.000 abstract description 9
- 238000000137 annealing Methods 0.000 abstract description 8
- 238000006902 nitrogenation reaction Methods 0.000 abstract description 5
- 150000001875 compounds Chemical class 0.000 abstract description 4
- 230000004048 modification Effects 0.000 abstract description 4
- 238000012986 modification Methods 0.000 abstract description 4
- 150000004767 nitrides Chemical class 0.000 abstract description 4
- 230000005298 paramagnetic effect Effects 0.000 abstract description 4
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 4
- 150000002910 rare earth metals Chemical class 0.000 abstract description 4
- 229910052723 transition metal Inorganic materials 0.000 abstract description 4
- 150000003624 transition metals Chemical class 0.000 abstract description 4
- 229910000765 intermetallic Inorganic materials 0.000 abstract description 3
- 230000007774 longterm Effects 0.000 abstract description 3
- 238000005275 alloying Methods 0.000 abstract description 2
- 229910052719 titanium Inorganic materials 0.000 description 4
- 229910052772 Samarium Inorganic materials 0.000 description 3
- 210000001787 dendrite Anatomy 0.000 description 3
- 229910001068 laves phase Inorganic materials 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910001172 neodymium magnet Inorganic materials 0.000 description 3
- 229910052758 niobium Inorganic materials 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000000875 corresponding effect Effects 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 229910052735 hafnium Inorganic materials 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 description 2
- 229910052720 vanadium Inorganic materials 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- 229910052684 Cerium Inorganic materials 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 238000012790 confirmation Methods 0.000 description 1
- 229910052802 copper Inorganic materials 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
- 239000013078 crystal Substances 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 239000003302 ferromagnetic material Substances 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000009862 microstructural analysis Methods 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical group [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 229910052725 zinc Inorganic materials 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
-
- 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
- H01F1/059—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and Va elements, e.g. Sm2Fe17N2
- H01F1/0596—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and Va elements, e.g. Sm2Fe17N2 of rhombic or rhombohedral Th2Zn17 structure or hexagonal Th2Ni17 structure
Definitions
- the invention relates to the Sm 2 Fe 17 alloy with Ta addition, and to the process for producing this alloy, which is suitable as the basic material for the preparation of permanent magnets based on nitrides of intermetallic compounds of rare earth and transition metals.
- Nitrides of binary intermetallic compounds between rare earths in the following text designated as RE, and transition metals, in the following text designated as TM, thus Sm 2 Fe 17 N x , are new ferromagnetic materials, first discovered by Coey J. M. D. and Sun H., published in J. Mag. Magn. Mat. 87, (1990), L251 (1). The preparation of these materials is described in the European applications EP 369097, EP 453270, EP 538643, EP 493019 and Canadian applications CA 2040686, CA 2058283.
- JP-A-05 25 592 a rare earth magnet materials are described, having a composition of general formula R X Fe (1-X-Y-Z) M Y C Z and in which R 2 Fe 17 type tetragonal crystal constitutes the main phase, where said R comprises rare earth metal which includes at least one of Sm, Ce, Nd and Pr, M comprises at least one of Ti, Zr, Hf, V, Nb, Ta, Cr, Mo, W, Mn, Nl, Pd, Cu, Ag, Zn, Mg, B, Al, Ga, In, Si ans Sn in defined ranges of quantities.
- the material obtained has to be heat treated at 1000°C for 12 hours because of component segregation.
- Permanent magnets based on the Sm 2 Fe 17 N 3 -x ternary interstitial phase with a rhombohedral Th 2 Zn 17 - type structure are considered to be competitive with the well-known Nd-Fe-B based magnets.
- the intrinsic properties of Sm 2 Fe 17 N 3-x include a higher Curie temperature (Tc) for 100 to 200°C and anisotropy field (Ha), and a slightly lover magnetisation saturation (Ms).
- Sm 2 Fe 17 binary phase which is used for production of the Sm 2 Fe 17 N 3-x interstitial temary compound through a gas-phase interstitial modification process, forms through a peritectic reaction between primary crystallised iron and Sm- rich liquid: L(liquid) + Fe -> Sm 2 Fe 17 .
- Free iron especially, unless removed by a subsequent isothermal homogenization treatment, reduces the coercivity of the Sm 2 Fe 17 nitride produced when used for permanent magnets.
- the usual methods for creating an alloy without soft magnetic phases are either high temperature-long term annealing of the samarium-rich cast alloy (five days at 1050°C) or through the phase modification with the addition of a third alloying element (from the group of transition metals).
- the phase relation can be influenced by the addition of the third element, which modifies the crystallization and prevents the primary crystallization of free iron and leads to a two phase structure consisting of Sm 2 Fe 17 phase and one paramagnetic intermediate Laves phase.
- the elements Ti and Nb as elements which influence the phase relations, and is published in the open literature Reinch B., Grieb B., Henig E. T., Petzow G., IEEE Trans. Magn., 28, (1992), 2832 and Platts A. E., Harris I. R., Coey J. M. D., J. Alloys Comp., (1992), 251
- the purpose and the aim of the invention relates to the Sm Fe Ta alloy with 4-5 at% Ta addition and to the process for producing this alloy with the corresponding properties.
- the production of the alloy should be cheap and comparatively easy.
- Tantalum forms a Pauli paramagnetic TaFe2 intermediate hexagonal Laves phase with iron, as described in the patent claims.
- the preparation of as -cast alloy which contains a minimal quantity of free iron and other ferromagnetic phases is enabled.
- the as -cast alloy is suitable for the nitrogenation procedure without any subsequent annealing process.
- the nitrogenated alloy is suitable as a basic material for the preparation of a new generation of permanent magnets of Sm 2 Fe 17 N x type.
- the alloy which contains a minimum quantity of free iron and other ferromagnetic phases, which diminish the hard magnetic coercivity of Sm 2 Fe 17 alloy, is produced.
- the amount of soft magnetic phases is low enough that for the preparation of Sm 2 Fe 17 alloy suitable for the nitrogenation and production of Sm 2 Fe 17 N x , high temperature annealing can be avoided.
- the alloy with the composition Sm 2 Fe 17-x Ta x is produced by arc melting in an inert atmosphere of Ar purified with Ti as a getter.
- Microstructural analysis shows phase compositional changes, which are dependent upon the increasing Ta content of the alloys of nominal composition Sm 2 Fe 17-x Ta x .
- Fig. 1 which shows the microstructure of the tantalum -free alloy, we can see the normal appearance of the as -cast state of the nominally stoichiometric Sm 2 Fe 17 alloy. Dendrites of primary crystallised iron (black) are surrounded by peritecticaly formed Sm 2 Fe 17 phase (grey) with some Sm -rich phase which was identified as SmFe 2 (white).
- microstructural morphology is typical for the as -cast alloy of stoichiometric composition with dendrites of primary recrystallised iron, surrounded by peritecticaly formed Sm 2 Fe 17 phase and partly with the Sm -rich phase, identified as SmFe 2 phase, detrimental for the magnetic properties and which can be removed by the known method of high temperature long term annealing.
- Figure 2 shows the microstructure of the alloy with a nominal composition of 5 at.% of Ta. No iron dendrites are observed and the microstructure consists of a mixture of only Sm 2 Fe 17 (grey) and Tafe 2 (white) phases.
- Fig. 4 shows thermomagnetic curves normalised to the Curie temperature of the Sm 2 Fe 17 phase for the alloys with a) 1% Ta, b) 2% Ta and c) 4% Ta. Thermomagnetic analysis also shows the increase in the Curie temperature as a function of the Ta concentration in the Sm 2 Fe 17 phase.
- the invention relates to the preparation of the cast alloy with a minimum amount of free iron and/or other soft magnetic phases, which is suitable for further nitrogenation without high temperature long term annealing.
- the as -cast alloy is suitable for the preparation of the Sm 2 Fe 17-x Ta x N 3-y compound.
- the most important advantage of the invention is the cheaper preparation procedure of the alloy.
- Ta addition is a new solution to the problem of the appearance of soft ferromagnetic phases which deteriorate the hard magnetic properties of the alloy.
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- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Hard Magnetic Materials (AREA)
Abstract
Procédé de production d'un alliage Sm2Fe17 à adjonction de Ta, sans recuit prolongé et onéreux à haute température. L'alliage coulé est suitable comme matière initiale dans la préparation d'aimants permanents à base de nitrures de composés intermétalliques de métaux des terres rares et d'éléments de transition. Le procédé permet la préparation d'un alliage coulé à deux phases, à savoir une phase Sm2Fe17 utilisable dans la nitration en vue d'obtenir une phase Sm2Fe17N3-x magnétique dure, et une pahse hexagonale TaFe2 paramagnétique. On obtient un changement de phase par adjonction d'un troisième élément d'alliage. Le Ta remplace le Fe dans la composition nominale Sm2Fe17. La teneur en fer ou en d'autres phases ferromagnétiques est inférieure à 0,5 % en poids. On a mis au point la préparation d'un alliage coulé renfermant une quantité minimale de fer libre et/ou d'autres phases magnétiques douces, et pouvant subir une nitration supplémentaire sans recuit prolongé à haute température. L'alliage coulé est utilisable dans la préparation du composé Sm2Fe17-xTaxN3-y.
Claims (2)
- Alliage contenant Sm-Fe-Ta convenable comme matériau de base pour la préparation d'aimants permanents de type Sm2Fe17-xN3-x,
caractérisé par l'addition de 4 at% à 5 at% de Ta élémentaire à du Sm élémentaire introduit en un excès de 10 jusqu'à 30% en poids et du Fe élémentaire, pour obtenir une composition nominale Sm2Fe17-xTax et qui est traitée pour fournir l'alliage coulé contenant deux phases principales Sm2Fe17 et TaFe2, avec des quantités minimales de fer libre et d'autres phases ferromagnétiques. - Procédé pour la production de l'alliage contenant Sm-Fe-Ta suivant la revendication 1,
caractérisé en ce que ce procédé comprend les étapes d'alliage de Fe et de Ta, après quoi du Sm est ajouté en un excès de 10 jusqu'à 30% en poids par rapport à la composition nominale Sm2Fe17-xTax pour compenser des pertes par évaporation, l'addition de Ta étant comprise entre 4 et 5 at% et que cet alliage Sm-Fe-Ta est au moins refondu à trois reprises, où cette fusion est une fusion à l'arc dans une atmosphère d'Ar purifié avec Ti.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SI9300422 | 1993-08-06 | ||
| SI9300422A SI9300422A (sl) | 1993-08-06 | 1993-08-06 | Zlitina Sm<SUB>2<\SUB>Fe<SUB>17<\SUB> z dodatkom Ta in postopek za njeno pripravo |
| PCT/SI1994/000014 WO1995004996A1 (fr) | 1993-08-06 | 1994-08-05 | ALLIAGE Sm2Fe17 A ADJONCTION DE Ta ET SON PROCEDE DE PREPARATION |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| EP0712532A1 EP0712532A1 (fr) | 1996-05-22 |
| EP0712532B1 true EP0712532B1 (fr) | 1997-05-02 |
Family
ID=20431230
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP95907498A Expired - Lifetime EP0712532B1 (fr) | 1993-08-06 | 1994-08-05 | alliage SmFeTa à adjonction de 4-5 at% Ta et le procédé de sa préperation |
Country Status (5)
| Country | Link |
|---|---|
| EP (1) | EP0712532B1 (fr) |
| DE (1) | DE69402988T2 (fr) |
| DK (1) | DK0712532T3 (fr) |
| SI (1) | SI9300422A (fr) |
| WO (1) | WO1995004996A1 (fr) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3751084B2 (ja) * | 1996-08-30 | 2006-03-01 | 本田技研工業株式会社 | 複合磁歪材料およびその製造方法 |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0525592A (ja) * | 1991-07-15 | 1993-02-02 | Minebea Co Ltd | 希土類磁石材料 |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3057448B2 (ja) * | 1988-05-26 | 2000-06-26 | 信越化学工業株式会社 | 希土類永久磁石 |
-
1993
- 1993-08-06 SI SI9300422A patent/SI9300422A/sl unknown
-
1994
- 1994-08-05 DE DE69402988T patent/DE69402988T2/de not_active Expired - Fee Related
- 1994-08-05 WO PCT/SI1994/000014 patent/WO1995004996A1/fr not_active Ceased
- 1994-08-05 DK DK95907498.0T patent/DK0712532T3/da active
- 1994-08-05 EP EP95907498A patent/EP0712532B1/fr not_active Expired - Lifetime
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0525592A (ja) * | 1991-07-15 | 1993-02-02 | Minebea Co Ltd | 希土類磁石材料 |
Also Published As
| Publication number | Publication date |
|---|---|
| EP0712532A1 (fr) | 1996-05-22 |
| DE69402988T2 (de) | 1997-09-25 |
| WO1995004996A1 (fr) | 1995-02-16 |
| DE69402988D1 (de) | 1997-06-05 |
| DK0712532T3 (da) | 1997-11-03 |
| SI9300422A (sl) | 1993-12-31 |
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