EP0848397B1 - Procédé de fabrication d'un composant magnétique en alliage magnétique doux à base de fer ayant une structure nanocristalline - Google Patents
Procédé de fabrication d'un composant magnétique en alliage magnétique doux à base de fer ayant une structure nanocristalline Download PDFInfo
- Publication number
- EP0848397B1 EP0848397B1 EP97402667A EP97402667A EP0848397B1 EP 0848397 B1 EP0848397 B1 EP 0848397B1 EP 97402667 A EP97402667 A EP 97402667A EP 97402667 A EP97402667 A EP 97402667A EP 0848397 B1 EP0848397 B1 EP 0848397B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- temperature
- magnetic
- crystallization
- heat treatment
- annealing
- 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.)
- Expired - Lifetime
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Classifications
-
- 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
- H01F41/0206—Manufacturing of magnetic cores by mechanical means
- H01F41/0213—Manufacturing of magnetic circuits made from strip(s) or ribbon(s)
- H01F41/0226—Manufacturing of magnetic circuits made from strip(s) or ribbon(s) from amorphous ribbons
-
- 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
- H01F1/12—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 soft-magnetic materials
- H01F1/14—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 soft-magnetic materials metals or alloys
- H01F1/147—Alloys characterised by their composition
- H01F1/153—Amorphous metallic alloys, e.g. glassy metals
- H01F1/15333—Amorphous metallic alloys, e.g. glassy metals containing nanocrystallites, e.g. obtained by annealing
-
- 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
- H01F1/12—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 soft-magnetic materials
- H01F1/14—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 soft-magnetic materials metals or alloys
- H01F1/147—Alloys characterised by their composition
- H01F1/153—Amorphous metallic alloys, e.g. glassy metals
- H01F1/15341—Preparation processes therefor
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S977/00—Nanotechnology
- Y10S977/70—Nanostructure
- Y10S977/832—Nanostructure having specified property, e.g. lattice-constant, thermal expansion coefficient
- Y10S977/833—Thermal property of nanomaterial, e.g. thermally conducting/insulating or exhibiting peltier or seebeck effect
Definitions
- the present invention relates to the manufacture of magnetic components in soft magnetic alloy based on iron having a nanocrystalline structure.
- Nanocrystalline magnetic materials are well known and have been described, in particular, in European patent applications EP 0 271 657 and EP 0 299 498. These are iron-based alloys, containing more than 60 at% (atoms%) of iron, copper, silicon, boron, and possibly at least one element taken among niobium, tungsten, tantalum, zirconium, hafnium, titanium and molybdenum, cast in the form of amorphous ribbons and then subjected to a treatment which causes extremely fine crystallization (the crystals have less 100 nanometers in diameter). These materials have magnetic properties particularly suitable for the manufacture of soft magnetic cores for electrotechnical devices such as earth leakage circuit breakers.
- hysteresis (Br / Bm ⁇ 0.5), i.e. a coated hysteresis cycle (Br / Bm ⁇ 0.3); Br / Bm being the ratio of remanent magnetic induction to magnetic induction Max.
- Round hysteresis cycles are obtained when treatment thermal consists of a simple annealing at a temperature between 500 ° C and 600 ° C.
- the lying hysteresis cycles are obtained when the treatment thermal includes at least one annealing under magnetic field, this annealing can be the annealing intended to cause the formation of nanocrystals.
- Nanocrystalline ribbons, or more precisely, magnetic components produced with these ribbons have a drawback which limits their use. This drawback is insufficient stability of the magnetic properties when the temperature rises above room temperature. This stability insufficient results in unreliability of circuit breaker operation differentials fitted with such magnetic cores.
- the object of the present invention is to remedy this drawback by providing a means for manufacturing magnetic cores from material nanocrystalline having magnetic properties whose temperature stability is significantly improved.
- the thermal relaxation treatment can be a maintenance for a time between 0.1 and 10 hours, at a temperature between 250 ° C and 480 ° C.
- the relaxation heat treatment can also consist of a progressive heating from room temperature to a temperature greater than 450 ° C, at a heating rate between 30 ° C / hour and 300 ° C / hour between 250 ° C and 450 ° C.
- At least one annealing constituting the heat treatment can be carried out under magnetic field.
- This process applies more particularly to soft magnetic alloys with iron base having a nanocrystalline structure, the chemical composition of which is such that Si ⁇ 14%.
- the alloy may have low levels of impurities provided by raw materials or resulting from production.
- the amorphous ribbon is obtained in a manner known per se by solidification very fast liquid alloy, poured, for example, on a cooled wheel.
- the magnetic core blanks are also manufactured known in itself, by winding the ribbon on a mandrel, cutting it and fixing its end by a welding point, in order to obtain small toroids of rectangular section.
- the blanks are first subjected to a so-called "relaxation" annealing, at a temperature below the temperature of onset of crystallization of the amorphous strip, and preferably between 250 ° C and 480 ° C, then an annealing of crystallization which may or may not be carried out under magnetic field, and possibly be followed by annealing at lowest temperature under magnetic field.
- This annealing of relaxation had for advantage of significantly reducing the sensitivity of magnetic properties nuclei at temperature.
- the inventors have also found that the annealing of relaxation prior to crystallization annealing had the added benefit of reduce the dispersion of the magnetic properties of the nuclei observed on mass production.
- the crystallization annealing is intended to precipitate in the matrix amorphous nanocrystals of size less than 100 nanometers, preferably between 10 and 20 nanometers. This very fine crystallization makes it possible to obtain the desired magnetic properties.
- the crystallization annealing consists of a maintaining at a temperature higher than the temperature at the start of crystallization and lower than the onset temperature of the secondary phases which deteriorate the magnetic properties.
- the annealing temperature of crystallization is between 500 ° C and 600 ° C, but it can be optimized for each ribbon, for example, by determining by tests the temperature which leads to maximum magnetic permeability.
- the annealing temperature of crystallization can then be chosen equal to this temperature, or, better, be chosen to be about 30 ° C higher.
- crystallization annealing can be carried out under a transverse magnetic field.
- the crystallization treatment can also be supplemented by annealing at a temperature below the crystallization start temperature, for example towards 400 ° C, carried out under transverse magnetic field.
- the heat treatment of the blanks magnetic component include a relaxation annealing, a crystallization possibly carried out under magnetic field, and, possibly, an additional annealing carried out under magnetic field.
- the relaxation annealing which precedes the crystallization annealing, and which can be performed both on the amorphous tape itself and on the component blank magnetic, can consist in maintaining a constant temperature during a time which preferably should be between 0.1 and 10 hours.
- This annealing can also consist of a gradual rise in temperature, which precedes, by example, crystallization annealing, and which must be done at a rate of rise in temperature between 30 ° C / h and 300 ° C / h, at least between 250 ° C and 450 ° C; preferably the rate of temperature rise should be around 100 ° C / h.
- the series of blanks of magnetic cores A2 and B2 have, for comparison, been treated in accordance with the prior art by a single crystallization annealing for 3 hours at 530 ° C.
- the maximum magnetic permeability at 50 Hz was measured at different temperatures between - 25 ° C and + 100 ° C, and it was expressed as a% of the maximum magnetic permeability at 50 Hz at 20 ° C.
- the first example relates to toroidal magnetic cores produced from ribbons 20 ⁇ m thick and 10 mm wide obtained by direct quenching on a cooled wheel, of an alloy of composition (in at%) Fe 73.5 Si 13.5 B 9 Cu 1 Nb 3 . After quenching on a wheel, it was checked by X-ray that the ribbon was completely amorphous. The ribbon was then separated into three sections, one, A, remained as it was, the other two, B and C, were subjected to relaxation annealing, for one, B, 1 hour at 400 ° C, for the other, C, 1 hour at 450 ° C.
- the second example relates to toroidal magnetic cores produced from ribbons 20 ⁇ m thick and 10 mm wide obtained by direct quenching on a cooled wheel, of an alloy of composition (in at%) Fe 73 Si 15 B 8 Cu 1 Nb 3 .
- ribbons 20 ⁇ m thick and 10 mm wide obtained by direct quenching on a cooled wheel, of an alloy of composition (in at%) Fe 73 Si 15 B 8 Cu 1 Nb 3 .
- the ribbon two batches of 300 toroids with an internal diameter of 11 mm and an external diameter of 15 mm were produced using automatic winding machines. The batches were then treated in ovens with neutral atmosphere. A control batch A was only subjected to a 1 hour crystallization annealing at 530 ° C.
- the second batch was treated in accordance with the invention: a relaxation annealing of 1 hour at 400 ° C. was first carried out, then a crystallization annealing of 1 hour at 530 ° C.
- the toroids were put in a box
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Electromagnetism (AREA)
- Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Soft Magnetic Materials (AREA)
- Thin Magnetic Films (AREA)
- Hard Magnetic Materials (AREA)
- Powder Metallurgy (AREA)
- Manufacturing Of Steel Electrode Plates (AREA)
Description
- on fabrique avec l'alliage magnétique un ruban amorphe,
- avec le ruban on fabrique une ébauche de composant magnétique,
- et on soumet le composant magnétique à un traitement thermique de cristallisation comprenant au moins un recuit de cristallisation à une température comprise entre 500°C et 600°C pendant un temps de maintien compris entre 0,1 et 10 heures, afin de provoquer la formation de nanocristaux, et, avant d'effectuer le traitement thermique de cristallisation, on réalise un traitement thermique de relaxation à une température inférieure à la température de début de recristallisation de l'alliage amorphe.
- de 0,1 à 3 at %, et de préférence, de 0,5 à 1,5 at % de cuivre ;
- de 0,1 à 30 at %, et, de préférence, de 2 à 5 at % d'au moins un élément pris parmi le niobium, le tungstène, le tantale, le zirconium, le hafnium, le titane, et le molybdène ; de préférence, la teneur en niobium est comprise entre 2 et 4 at % ;
- du silicium et du bore, la somme des teneurs en ces éléments étant comprise entre 5 et 30 at %, et, de préférence, entre 15 et 25 at % ; la teneur en bore pouvant aller jusqu'à 25 at %, et, de préférence, étant comprise entre 5 et 14 at % ; la teneur en silicium pouvant atteindre 30 at %, et, de préférence, étant comprise entre 12 et 17 at %.
échantillon | - 25°C | - 5°C | 20°C | 80°C | 100°C |
A1 (inv) | 100 % | 102 % | 100 % | 93 % | 86 % |
A2 (comp) | 102 % | 103 % | 100 % | 87 % | 78 % |
B1 (inv) | 97 % | 98 % | 100 % | 88 % | 78 % |
B2 (comp) | 98 % | 99 % | 100 % | 75 % | 60 % |
échantillon | traitement relaxation | champ coercitif (mOe) | perméabilité max à 50 Hz |
A | sans | 6,1 | 650 000 |
B | 1 h à 400 °C | 5,2 | 690 000 |
C | 1 h à 450 °C | 5,1 | 760 000 |
échantillon | Trait relax | ch coercitif (mOe) | Br / Bm | perm max à 50 Hz |
A | sans | 5 | 0,12 | 200 000 |
B | 1 h à 400 °C | 3,8 | 0,08 | 215 000 |
C | 1 h à 450 °C | 3,4 | 0,07 | 205 000 |
traitement | perméabilité max à 50 Hz moyenne | perméabilité max à 50 Hz écart type |
sans relaxation (lot A) | 585 000 | 28 000 |
avec relaxation (lot B) | 615 000 | 20 000 |
Traitement | ch coercitif (mOe) | Br / Bm | perm à 5mOe à 50 Hz |
sans relaxation (lot A) | 5,2 | 0,08 | 117 000 |
avec relaxation (lot B) | 4,3 | 0,06 | 124 000 |
Claims (6)
- Procédé de fabrication d'un composant magnétique en alliage magnétique doux à base de fer ayant une structure nanocristalline dont la composition chimique comprend, en atomes %, Fe ≥ 60% 0,1 % ≤ Cu ≤ 3 %, 0 % ≤ B ≤ 25 %, 0 % ≤ Si ≤ 30 %, et au moins un élément pris parmi le niobium, le tungstène, le tantale, le zirconium, le hafnium, le titane, et le molybdène en des teneurs comprises entre 0,1 % et 30 %, le reste étant des impuretés résultant de l'élaboration, la composition satisfaisant en outre la relation 5 % ≤ Si + B ≤ 30 %, selon lequel :on fabrique avec l'alliage magnétique un ruban amorphe,avec le ruban, on fabrique une ébauche de composant magnétique par enroulement du ruban magnétique autour d'un mandrin de façon à former un tore,et on soumet le composant magnétique à un traitement thermique de cristallisation comprenant au moins un recuit de cristallisation à une température comprise entre 500°C et 600°C pendant un temps de maintien compris entre 0,1 et 10 heures, afin de provoquer la formation de nanocristaux, caractérisé en ce que, avant le traitement thermique de cristallisation on effectue un traitement thermique de relaxation à une température inférieure à la température de début de cristallisation de l'alliage amorphe.
- Procédé selon la revendication 1 caractérisé en ce que le traitement thermique de relaxation est un maintien pendant un temps compris entre 0,1 et 10 heures, à une température comprise entre 250 °C et 480 °C.
- Procédé selon la revendication 1 caractérisé en ce que le traitement thermique de relaxation consiste en un chauffage progressif depuis la température ambiante jusqu'à une température supérieure à 450 °C, à une vitesse de chauffage comprise entre 30 °C/heure et 300 °C/heure entre 250 °C et 450 °C.
- Procédé selon l'une quelconque des revendications 1 à 3 caractérisé en ce que le recuit de cristallisation est effectué sous champ magnétique.
- Procédé selon l'une quelconque des revendications 1 à 4 caractérisé en ce que on effectue en outre un recuit complémentaire sous champ magnétique à une température inférieure à la température de début de cristallisation.
- Procédé selon l'une quelconque des revendications 1 à 5 caractérisé en ce que la composition chimique de l'alliage est telle que Si ≤ 14 %.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR9615197A FR2756966B1 (fr) | 1996-12-11 | 1996-12-11 | Procede de fabrication d'un composant magnetique en alliage magnetique doux a base de fer ayant une structure nanocristalline |
FR9615197 | 1996-12-11 |
Publications (2)
Publication Number | Publication Date |
---|---|
EP0848397A1 EP0848397A1 (fr) | 1998-06-17 |
EP0848397B1 true EP0848397B1 (fr) | 2002-09-18 |
Family
ID=9498537
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP97402667A Expired - Lifetime EP0848397B1 (fr) | 1996-12-11 | 1997-11-07 | Procédé de fabrication d'un composant magnétique en alliage magnétique doux à base de fer ayant une structure nanocristalline |
Country Status (18)
Country | Link |
---|---|
US (1) | US5911840A (fr) |
EP (1) | EP0848397B1 (fr) |
JP (1) | JPH10195528A (fr) |
KR (1) | KR19980064039A (fr) |
CN (1) | CN1134034C (fr) |
AT (1) | ATE224582T1 (fr) |
AU (1) | AU731520B2 (fr) |
CZ (1) | CZ293837B6 (fr) |
DE (1) | DE69715575T2 (fr) |
ES (1) | ES2184047T3 (fr) |
FR (1) | FR2756966B1 (fr) |
HK (1) | HK1010938A1 (fr) |
HU (1) | HU216168B (fr) |
PL (1) | PL184208B1 (fr) |
SK (1) | SK284008B6 (fr) |
TR (1) | TR199701599A3 (fr) |
TW (1) | TW561193B (fr) |
ZA (1) | ZA9710780B (fr) |
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US5252144A (en) * | 1991-11-04 | 1993-10-12 | Allied Signal Inc. | Heat treatment process and soft magnetic alloys produced thereby |
DE69408916T2 (de) * | 1993-07-30 | 1998-11-12 | Hitachi Metals Ltd | Magnetkern für Impulsübertrager und Impulsübertrager |
US5611871A (en) * | 1994-07-20 | 1997-03-18 | Hitachi Metals, Ltd. | Method of producing nanocrystalline alloy having high permeability |
-
1996
- 1996-12-11 FR FR9615197A patent/FR2756966B1/fr not_active Expired - Fee Related
-
1997
- 1997-11-07 AT AT97402667T patent/ATE224582T1/de not_active IP Right Cessation
- 1997-11-07 DE DE69715575T patent/DE69715575T2/de not_active Expired - Fee Related
- 1997-11-07 ES ES97402667T patent/ES2184047T3/es not_active Expired - Lifetime
- 1997-11-07 EP EP97402667A patent/EP0848397B1/fr not_active Expired - Lifetime
- 1997-11-13 TW TW086116891A patent/TW561193B/zh not_active IP Right Cessation
- 1997-11-14 AU AU45199/97A patent/AU731520B2/en not_active Ceased
- 1997-11-28 SK SK1618-97A patent/SK284008B6/sk unknown
- 1997-12-01 ZA ZA9710780A patent/ZA9710780B/xx unknown
- 1997-12-09 CZ CZ19973983A patent/CZ293837B6/cs not_active IP Right Cessation
- 1997-12-10 HU HUP9702383A patent/HU216168B/hu not_active IP Right Cessation
- 1997-12-10 CN CNB971253668A patent/CN1134034C/zh not_active Expired - Fee Related
- 1997-12-11 KR KR1019970067847A patent/KR19980064039A/ko not_active Application Discontinuation
- 1997-12-11 US US08/989,083 patent/US5911840A/en not_active Expired - Fee Related
- 1997-12-11 PL PL97323663A patent/PL184208B1/pl not_active IP Right Cessation
- 1997-12-11 JP JP9362223A patent/JPH10195528A/ja not_active Withdrawn
- 1997-12-11 TR TR97/01599A patent/TR199701599A3/tr unknown
-
1998
- 1998-11-17 HK HK98112053A patent/HK1010938A1/xx not_active IP Right Cessation
Also Published As
Publication number | Publication date |
---|---|
CN1134034C (zh) | 2004-01-07 |
SK161897A3 (en) | 1998-12-02 |
TR199701599A2 (xx) | 2000-07-21 |
AU731520B2 (en) | 2001-03-29 |
HU216168B (hu) | 1999-04-28 |
HK1010938A1 (en) | 1999-07-02 |
ES2184047T3 (es) | 2003-04-01 |
FR2756966B1 (fr) | 1998-12-31 |
HUP9702383A3 (en) | 1998-08-28 |
JPH10195528A (ja) | 1998-07-28 |
FR2756966A1 (fr) | 1998-06-12 |
KR19980064039A (ko) | 1998-10-07 |
DE69715575D1 (de) | 2002-10-24 |
CZ398397A3 (cs) | 1998-07-15 |
ATE224582T1 (de) | 2002-10-15 |
EP0848397A1 (fr) | 1998-06-17 |
DE69715575T2 (de) | 2003-05-22 |
CN1185012A (zh) | 1998-06-17 |
TR199701599A3 (tr) | 2000-07-21 |
PL184208B1 (pl) | 2002-09-30 |
HUP9702383A2 (hu) | 1998-07-28 |
SK284008B6 (sk) | 2004-07-07 |
PL323663A1 (en) | 1998-06-22 |
ZA9710780B (en) | 1998-06-12 |
AU4519997A (en) | 1998-06-18 |
TW561193B (en) | 2003-11-11 |
CZ293837B6 (cs) | 2004-08-18 |
US5911840A (en) | 1999-06-15 |
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