CN103366941A - Method of producing sintered magnets with controlled structures and composition distribution - Google Patents
Method of producing sintered magnets with controlled structures and composition distribution Download PDFInfo
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- CN103366941A CN103366941A CN2013101145889A CN201310114588A CN103366941A CN 103366941 A CN103366941 A CN 103366941A CN 2013101145889 A CN2013101145889 A CN 2013101145889A CN 201310114588 A CN201310114588 A CN 201310114588A CN 103366941 A CN103366941 A CN 103366941A
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- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 17
- 238000004519 manufacturing process Methods 0.000 claims abstract description 14
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 26
- 238000005245 sintering Methods 0.000 claims description 23
- 229910001172 neodymium magnet Inorganic materials 0.000 claims description 17
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 239000007789 gas Substances 0.000 claims description 14
- 229910052742 iron Inorganic materials 0.000 claims description 12
- 229910052779 Neodymium Inorganic materials 0.000 claims description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 8
- 229910052796 boron Inorganic materials 0.000 claims description 8
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 claims description 8
- 150000002910 rare earth metals Chemical class 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 239000001257 hydrogen Substances 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- 238000007493 shaping process Methods 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 239000001307 helium Substances 0.000 claims description 4
- 229910052734 helium Inorganic materials 0.000 claims description 4
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 4
- 238000013467 fragmentation Methods 0.000 claims description 3
- 238000006062 fragmentation reaction Methods 0.000 claims description 3
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 1
- 230000005855 radiation Effects 0.000 abstract description 4
- 229910052692 Dysprosium Inorganic materials 0.000 description 20
- 229910052771 Terbium Inorganic materials 0.000 description 20
- 230000006872 improvement Effects 0.000 description 13
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 description 11
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 description 11
- 238000010438 heat treatment Methods 0.000 description 9
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- 239000002184 metal Substances 0.000 description 9
- 239000013078 crystal Substances 0.000 description 6
- 238000009768 microwave sintering Methods 0.000 description 6
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
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- 238000005516 engineering process Methods 0.000 description 3
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- 238000002844 melting Methods 0.000 description 3
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 229910052772 Samarium Inorganic materials 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
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- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
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Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/02—Making ferrous alloys by powder metallurgy
-
- 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
-
- 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
- H01F41/0266—Moulding; Pressing
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- 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
- H01F41/0293—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 diffusion of rare earth elements, e.g. Tb, Dy or Ho, into permanent magnets
-
- 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
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C2202/00—Physical properties
- C22C2202/02—Magnetic
-
- 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
Abstract
The invention provides a method of producing sintered magnets with controlled structures and composition distribution. A method of making a permanent magnet includes a step of providing an alloy powder comprising at least one rare earth element. The alloy powder is shaped and then exposed to microwave radiation or a pulsed electric current to form a sintered magnet.
Description
Technical field
Aspect at least one, the present invention relates to make the method for permanent magnet.
Background technology
Permanent magnet (PM) is widely used in the various device, comprises the traction electro-motor for hybrid power and motor vehicle.Sintering Nd-Fe-B (Nd-Fe-B) permanent magnet has extraordinary magnetic characteristic when low temperature.Yet, because Nd in the Nd-Fe-B permanent magnet
2Fe
14The low Curie temperature of B phase, magnetic remanent magnetism and coercivity be fast reducing along with the increase of temperature.The substitute Dy of Nd or Fe causes the increase of anisotropy field and coercivity in the known Nd-Fe-B magnet, and the reduction of saturation magnetization (C.S. Herget, Metal, Poed. Rep. V. 42, P.438 (1987); W. Rodewald, J. Less-Common Met., V111, P77 (1985); And D. Plusa, J. J. Wystocki, Less-Common Met. V. 133, P.231 (1987)).Convention be add in melting with before forming alloy heavy RE metal for example dysprosium (Dy) or terbium (Tb) in hybrid metal.But, Dy and Tb are very rare and expensive.Heavy RE only contains the Dy of the 2-7% that has an appointment, and only has in the world sub-fraction RE ore deposit to contain heavy RE.The price of Dy is sharply increasing in the recent period.Tb can provide the magnetic characteristic that can provide than Dy higher magnetic characteristic, but even also expensive more a lot of than Dy.
The exemplary magnets that is used for the traction electro-motor of motor vehicle driven by mixed power contains the Dy of the 6-10wt% that has an appointment to satisfy desired magnetic characteristic.The conventional method of making magnet with Dy or Tb cause Dy or Tb by solid diffusion in magnet, be distributed on the crystal grain neutralization along crystal boundary mutually in.The Nd-Fe-B permanent magnet can be produced with powder metallurgical technique, and this comprises melting and thin strap continuous casting, hydrogenation broken (hydride and dehydrogenation compound), grinds (utilizing the nitrogen jet grinding), screening and the chemical composition of hybrid alloys powder to obtain expecting.Typical powder metallurgical technique is as follows: weigh under magnetic field and pressurize to realize powder alignment (vacuum-bag process), isostatic compaction, sintering and slaking are (for example, approximately 5-30 hour, approximately under 500-1100 degree centigrade, in a vacuum), and be machined to magnet pieces.At last, by (if necessary) such as phosphatization processing, electroless nickel plating (Ni), epoxy coatings magnet is carried out surface treatment.
The desired microstructure based on the magnet of Nd-Fe-B of sintering is Fe
14Nd
2B crystal grain, it (mainly is that Nd adds by some stable Fe of impurity by the rich Nd phase of nonferromagnetic ideally
4Nd
1.1B
4With Fe-Nd eutectic matrix mutually) isolation.Add Dy or Tb and cause forming very different ternary intercrystallines based on Fe, Nd and Dy or Tb mutually.These are positioned at territory, crystal boundary area and Fe mutually
14Nd
2The surface of B crystal grain.
Be coated with Dy or Tb(or their alloy of Nd-Fe-B powder) be used to make magnet, this causes the uneven distribution in magnet at Dy on the microcosmic and Tb.For example, compare with traditional handicraft, the amount of Dy and/or Tb can reduce approximately 20% or more, or approximately 30% or more, or approximately 40% or more, or approximately 50% or more, or approximately 60% or more, or approximately 70% or more, or approximately 80% or more, or approximately 90% or more, this depends on that surface powder is with respect to concentration in surface powder of the relative quantity of core powder and Dy or Ty, sintering plan (this affects Dy or the Ty diffusion in from the grain surface to the volume).This technique comprises the Nd-Fe-B based powders of utilizing Dy or Tb metal or alloy to coat to be used for the Nd-Fe-B permanent magnet of making sintering.The Nd-Fe-B based powders can coat by mechanical lapping, physical vapor deposition (PVD) or chemical vapor deposition (CVD).
Therefore, needing a kind of manufacturing permanent magnet, is the Innovative method of Nd-Fe-B base magnet specifically.
Summary of the invention
The present invention is by providing at least one embodiment the method for making permanent magnet to solve one or more problems of prior art.The method of making rare earth magnet comprises step: the alloy powder that comprises at least a rare earth element is provided.This alloy powder is formed and then is exposed to microwave to form sintered magnet.
In another embodiment, provide the method for making permanent magnet.The method of making rare earth magnet comprises step: the alloy powder that comprises neodymium, iron and boron is provided.This alloy powder is formed and then is exposed to microwave to form sintered magnet.
In another embodiment, provide the method for making permanent magnet.The method of making rare earth magnet comprises step: the alloy powder that comprises at least a rare earth element is provided.This alloy powder is formed and then is exposed to pulse current to form sintered magnet.
The invention provides following scheme:
Scheme
1.A kind of method of making rare earth magnet, the method comprises:
Alloy powder is provided, and this alloy powder comprises at least a rare earth element;
This alloy powder is shaped; And
This alloy powder is exposed to microwave to form sintered magnet.
Scheme
2.Such as scheme 1 described method, the shaping of wherein said alloy powder is by alloy powder being placed in the mould under the magnetic field to realize the powder magnetic alignment.
Scheme
3.Such as scheme 1 described method, wherein this alloy powder is at shaping or pressurized afterwards.
Scheme
4.Such as scheme 1 described method, also be included in be exposed to before the microwave or during make alloy powder contact gas.
Scheme
5.Such as scheme 4 described methods, wherein said gas comprises the composition that is selected from by helium, argon gas, hydrogen, nitrogen and their group that constitutes.
Scheme
6.Such as scheme 5 described methods, wherein said alloy powder is hydrogenated fragmentation.
Scheme
7.Such as scheme 1 described method, wherein said microwave has from about 1 to about 6kw power stage with from about 300MHz to the about frequency of 300GHz.
Scheme
8.Such as scheme 1 described method, wherein this alloy powder comprises neodymium, iron and boron.
Scheme
9.Such as scheme 8 described methods, wherein this alloy powder also comprises the composition that is selected from by dysprosium, terbium and their group that constitutes.
Scheme
10.Such as scheme 9 described methods, wherein this alloy powder comprises dysprosium and/or the terbium with non-uniform Distribution.
Scheme
11.Such as scheme 10 described methods, wherein said dysprosium and/or terbium coat this alloy powder.
Scheme
12.Such as scheme 1 described method, wherein this alloy powder comprises samarium and iron.
Scheme
13.Such as scheme 12 described methods, wherein said sintered magnet comprises the Sm-Fe-N magnetic domain.
Scheme
14.A kind of method of making neodymium-iron-boron magnet, the method comprises:
Alloy powder is provided, and this alloy powder comprises neodymium, iron and boron;
Be shaped and this alloy powder that pressurizes; And
This alloy powder is exposed to microwave to form the sintering neodymium-iron-boron magnet.
Scheme
15.Such as scheme 14 described methods, also be included in be exposed to before the microwave or during make alloy powder contact gas.
Scheme
16.Such as scheme 15 described methods, wherein said gas comprises the composition that is selected from by helium, argon gas, hydrogen, nitrogen and their group that constitutes.
Scheme
17.Such as scheme 15 described methods, wherein said microwave have from about 300MHz to about 300GHz frequency and from approximately 1 to the about power stage of 6kw.
Scheme
18.Such as scheme 14 described methods, wherein this alloy powder also comprises the composition that is selected from by dysprosium, terbium and their group that constitutes.
Scheme
19.A kind of method of making rare earth magnet, the method comprises:
Alloy powder is provided, and this alloy powder comprises at least a rare earth element;
This alloy powder is shaped; And
This alloy powder is exposed to pulse current.
Scheme
20.Such as scheme 19 described methods, wherein said pulse current is from approximately 100 to approximately 10000 amperes.
Scheme
21.Such as scheme 19 described methods, wherein said pulse current has pulse duration and 1 from about 1ms to about 300ms to the about time out of 50ms.
Description of drawings
Exemplary embodiment of the present invention will be by specific descriptions and accompanying drawing and by comprehend, in the accompanying drawing:
Fig. 1 is that explanation uses microwave to make the flow chart of the method for permanent magnet;
Fig. 2 is the schematic diagram of microwave sintering device;
Fig. 3 is that explanation uses microwave to make the flow chart of the method for permanent magnet; And
Fig. 4 is the schematic diagram of pulse electric current sintering device of the method for execution graph 3.
Embodiment
Specifically with reference to the at present preferred composition of the present invention, embodiment and method, this has consisted of the present optimal mode of the present invention of putting into practice known for inventor now.Accompanying drawing is not necessarily drawn in proportion.But, it should be understood that the disclosed embodiments only are examples of the present invention, the present invention can implement by different alternative forms.Therefore, disclosed detail should not be interpreted as determinately in this paper, and only is for the representative basis of any aspect of the present invention and/or is that instruction those skilled in the art utilize representative basis of the present invention in every way.
Except pointing out clearly in example or in other place, all numerical quantities of the amount of Indicator Reaction in this manual and/or the material of use or condition should be understood to modify with the word " approximately " of describing in the wide region of the present invention.Usually the preferably practice in described numerical limits.And unless clear and definite opposite indication is arranged: percentage, " part " and ratio all are by weight; To describe a group or a class material be suitable for the given purpose relevant with the present invention or preferably mean this group or such member in any two or more mixture be suitable or preferred too; Composition when with chemical wording the description of composition being referred to any compound that specifies in adding specification to, and not necessarily get rid of chemical interaction between the ingredients of a mixture after mixing; Definition first time of acronym or other abbreviation be applicable to identical abbreviation in this article whole follow-up use and make necessary modification after be suitable for the normal grammatical variants of the abbreviation of initial definition; And, unless clear and definite opposite explanation is arranged, the measurement of character be by before or after the similar technology that is used for same nature quoted determine.
Concrete parts and/or condition it will also be appreciated that the specific embodiment and the method that the invention is not restricted to the following describes, because can change certainly.And term used herein only is used for describing the purpose of specific embodiment of the present invention and is absolutely not as determinate.
Also must be noted that when using in this specification and appended claim, singulative " ", " one " and " being somebody's turn to do " comprise the denoted object of plural number, unless clearly make other indication in the context.For example, parts mentioning singulative are to be intended to comprise a plurality of parts.
Various embodiment of the present invention provides the method for sintering with the permanent magnet of controlled macrostructure (for example porousness and powder particle size and distribution) and microstructure (mutually various and basis).These embodiment comprise microwave sintering method and electric current sintering method.Processed magnet comprises Nd-Fe-B base magnet and Sm-Fe-N(Sm-Fe-N) basic magnet.
With reference to Fig. 1, provide explanation to make the flow chart of the method for permanent magnet.The method comprises provides alloy powder 10, and this alloy powder comprises at least a rare earth element.Alloy powder 10 is formed in mould 12 and then is exposed to microwave 14 to form sintered magnet 16.In a modification, alloy powder 10 comprises neodymium, iron and boron.In further improving, alloy powder 10 also comprises the composition that is selected from by dysprosium, terbium and their group that constitutes.In another further improvement, dysprosium and/or terbium have distribution heterogeneous.The name of submitting on January 14th, 2011 is called the U.S. Patent application 13/007 of " Method Of Making Nd-Fe-B Sintered Magnets With Dy Or Tb " (identical with the present inventor), 203 have described the method for magnet and manufacturing magnet, this magnet uses Dy or the Tb of much less by coating the core magnetic powder particles by physical vapour deposition (PVD) with rich Dy or Tb coating than the magnet that those use conventional method to make, but has obtained similar magnetic characteristic.This patent is incorporated this paper hereby by reference in full into.In a kind of improvement, disclosed alloy powder is used in the embodiment of the invention in this patent.In another improved, alloy powder 10 comprised samarium and iron, and they contact with nitrogen in sintering process.In a kind of modification, sintered magnet 16 comprises the Sm-Fe-N magnetic domain after this.
With reference to Fig. 2, provide the schematic diagram of the microwave sintering device that is used to form rare-earth permanent magnet.Microwave sintering device 20 comprises microwave generator 22, and it provides microwave to agglomerating chamber 24.Microwave generator 22 provides microwave to recirculator 26, and recirculator 26 can provide and be radiated R-H tuner 28.Microwave sintering device 20 arrives the approximately frequencies operations of 300GHz with 300MHZ usually, and power stage is in the 1-6kW scope.In a kind of improvement, microwave has from approximately 2 to about 3GHz(for example, frequency 2.45GHz).After this microwave is provided to agglomerating chamber 24.Microwave sintering device 20 also comprises water load 30, microwave generator be energized but radiation when not being provided to agglomerating chamber 24 this radiation can be imported into water load 30.Alloy powder 10 is maintained in the mould 32, and mould 32 centers on (batch system) by insulated ceramic shell 34.In another modification, insulated ceramic shell can be replaced by the alumina tube that insulate with ceramic insulation.The major function of insulation is to be kept at the heat that produces in the magnet part.In the green powder part 10 of overcompression also can be placed in the ceramic shell (container) or frame, thereby they are by the thermal radiation heating from heated ceramic shell.Pyrometer 36 is used for the temperature at sintering process monitoring alloy powder 10.The IR transducer and/or the band sheath thermocouple that are placed with near the surface of sample also can be used to monitor temperature.In a kind of improvement, alloy powder 10 has been realized from approximately 500 to about 1600 degrees centigrade temperature.In a kind of improvement, alloy powder 10 has been realized from approximately 500 to about 1200 degrees centigrade temperature.In another improves, control length from approximately 1 minute be from about 1 to 1000 centigrade per minute to approximately 10 hours and heating and cooling speed.Gas (for example, argon gas, helium, nitrogen, hydrogen etc.) is introduced by gas system 40.In a kind of improvement, alloy powder 10 contacts with gas before being exposed to microwave and/or in the process.Vacuum system 42 is used to gas pumped and/or keep agglomerating chamber 24 and is in approximately 10
-4Pa or larger vacuum degree.
Aforesaid microwave process provide a kind of satisfy with potential lower cost produce trickle microstructure, the method for the requirement of high density and better characteristic more.It has produced than the better mechanical performance of traditional treatment method and has produced trickleer crystallite dimension.The shape of porousness (if present) is very different from the shape that is realized by the conventional sintering method.The powder metal component of Microwave Treatment is expected to produce the porousness of rounded edge, thereby produces higher ductility and toughness.Microwave-metal interaction is desired also more complicated than the people who works hard on the spot.There are many factors all to help significantly total microwave heating of powdered-metal.The distribution of the microwave energy in the size and dimension of magnet part, the cavity and the magnetic field of electromagnetic radiation are important to heating and the sintering of powdered-metal all.
With reference to Fig. 3, provide explanation to make the flow chart of the method for permanent magnet by pulse electric current sintering (PECS).Pulse electric current sintering is also known as spark plasma sintering (SPS) or field assisted sintering technology (FAST).PECS has adopted pulsed D C electric current to come electric conduction of heating powder compact part by Joule heating.This DC heating mode allows to use very high heating and cooling speed, make it possible to realize the sintering temperature lower than conventional sintering technique, improved densification in grain growth, promoted solid diffusion, allowed in the full densification product of Magnaglo, to have kept the intrinsic property of this Magnaglo.The method comprises provides alloy powder 10, and this alloy powder comprises at least a rare earth element.Alloy powder 10 be formed and be positioned in stamping parts 52,54 and punch die 58,60 between.After this alloy powder 10 is exposed to from the pulse current in source 62 to form sintered magnet 64.
With reference to Fig. 4, provide the signal explanation of pulse electric current sintering system.Sintering system 70 comprises vacuum chamber 72, and alloy powder 10 is sintered in this chamber.Sintering system 70 comprises stamping parts 74 and lower stamping parts 76, they two usually have graphite or metal to form.Sintering system 70 comprises that also it also is made of metal usually be used to the punch die 78 that holds alloy powder 10.Shown in arrow 80,82, power is applied to alloy powder 10.Pulsed D C power supply 84 is used to the apply pulse electric current to alloy powder 10.In a kind of improvement, pulse current be from approximately 100 to approximately 10000 amperes and have from about 1ms to about 300ms pulse duration and from 1 to the about time out of 50ms.Vacuum degree is approximately 10 in a kind of improvement
-4Pa or larger.
Still with reference to Fig. 4, the metal of sintering system 70 partly has resistance so that generate very rapidly direct projection heat when electric current is employed.Therefore, the control time can only be one minute.Because PCES is direct heating means, so stop crystal structure to be changed by the quick rising of temperature.And, by using the pulse current method, can promote the combination of powder particle border surface and the temperature of the powder that do not raise significantly.As a result, but sintered magnet powder and its magnetic characteristic of not demoting.And, can improve density by using the servo pressurization with Loading Control able to programme.In order to promote the Even Sintering behavior, the temperature gradient in the sample is minimized.The parameter that affects the Temperature Distribution in the magnetic part comprises conductivity, the die wall thickness of material and is used for stoping the existence of the graphite paper of the direct contact between the magnetic part (if needs and be used for electrically contacting between all parts of assurance).FEM (finite element) model can be used to assess thermal gradient in the PECS process according to the geometric parameter of physical material character, different piece and pulse current input.Depend on the electrical property of described part, the electric current in working portion and Temperature Distribution are fully different.In the situation that current-carrying part, pulsed D C electric current Main Current is crossed this part and is only had sub-fraction to flow through punch die.
In a modification of the present embodiment, the permanent magnet of the present embodiment has the non-uniform Distribution of dysprosium and/or terbium.For example, in a kind of improvement, permanent magnet comprises a plurality of zones, and neodymium, iron and boron magnetic domain are coated with the layer that comprises dysprosium and/or terbium in these zones.In a kind of improvement, this coating has from about 100nm to about 100 microns thickness.In another kind improves, this coating have from approximately 5 microns to about 70 microns thickness.In another improves, this coating have from approximately 10 microns to about 50 microns thickness.In a kind of improvement, the powder that is wrapped by is formed by alloy powder 10 is put into mould 22.Alloy powder 10 is usually at shaping or pressurized afterwards.Usually, permanent magnet comprise the total weight that accounts for this permanent magnet from approximately 0.01 to approximately dysprosium and/or the terbium of 8 percentage by weights.But, the surface concentration of dysprosium and/or terbium can be coating layer total weight approximately 5 to about 50 percentage by weights.
In the modification of above-described embodiment, the alloy powder that uses in microwave and PECS method can followingly form.To contain the alloy melting of neodymium, iron and boron and cast to make slice by spinning.After this alloy slice is hydrogenated fragmentation by this alloy of hydrogenation.Usually, this step is approximately finished until alloy is broken under 1 to 5atm the pressure in the hydrogen stove.After this this alloy usually in a vacuum at elevated temperatures (for example 300 to 600 degrees centigrade) by dehydrogenation 1 to 10 hour.The result of hydrogenation and dehydrogenation is that this alloy is ground into meal, and it has the particle mean size from 0.1mm to 4mm usually.After this meal is pulverized (grinding by the nitrogen spray is refreshing) to make start powder.In a kind of improvement, alloy powder can mix to regulate chemical composition and optionally sieving with the second alloy powder.In a kind of improvement, after this alloy powder is wrapped by the layer that contains Dy and/or Tb by mechanical lapping, physical gas-phase deposition or chemical vapour deposition (CVD).After this resulting powder that is wrapped by can randomly be sieved.At last, form permanent magnet by above-mentioned technique.
Although illustrated and described embodiments of the invention, should not be considered as these embodiment diagram and described of the present invention all may form.Or rather, the word that uses in the specification is descriptive but not determinate word, and it should be understood that and can carry out various changes without departing from the spirit and scope of the present invention.
Claims (10)
1. method of making rare earth magnet, the method comprises:
Alloy powder is provided, and this alloy powder comprises at least a rare earth element;
This alloy powder is shaped; And
This alloy powder is exposed to microwave to form sintered magnet.
2. the method for claim 1, the shaping of wherein said alloy powder are by alloy powder being placed in the mould under the magnetic field to realize the powder magnetic alignment.
3. the method for claim 1, wherein this alloy powder is at shaping or pressurized afterwards.
4. the method for claim 1, also be included in be exposed to before the microwave or during make alloy powder contact gas.
5. method as claimed in claim 4, wherein said gas comprises the composition that is selected from by helium, argon gas, hydrogen, nitrogen and their group that constitutes.
6. method as claimed in claim 5, wherein said alloy powder is hydrogenated fragmentation.
7. the method for claim 1, wherein said microwave have from about 1 to about 6kw power stage with from about 300MHz to the about frequency of 300GHz.
8. the method for claim 1, wherein this alloy powder comprises neodymium, iron and boron.
9. method of making neodymium-iron-boron magnet, the method comprises:
Alloy powder is provided, and this alloy powder comprises neodymium, iron and boron;
Be shaped and this alloy powder that pressurizes; And
This alloy powder is exposed to microwave to form the sintering neodymium-iron-boron magnet.
10. method of making rare earth magnet, the method comprises:
Alloy powder is provided, and this alloy powder comprises at least a rare earth element;
This alloy powder is shaped; And
This alloy powder is exposed to pulse current.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US13/440,482 | 2012-04-05 | ||
| US13/440,482 US20130266473A1 (en) | 2012-04-05 | 2012-04-05 | Method of Producing Sintered Magnets with Controlled Structures and Composition Distribution |
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| Publication Number | Publication Date |
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| CN103366941A true CN103366941A (en) | 2013-10-23 |
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| CN2013101145889A Pending CN103366941A (en) | 2012-04-05 | 2013-04-03 | Method of producing sintered magnets with controlled structures and composition distribution |
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| US (1) | US20130266473A1 (en) |
| JP (1) | JP2013219353A (en) |
| CN (1) | CN103366941A (en) |
| DE (1) | DE102013205769A1 (en) |
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| CN104715878A (en) * | 2013-12-17 | 2015-06-17 | 现代自动车株式会社 | NdFeB PERMANENT MAGNET AND METHOD FOR PRODUCING THE SAME |
| CN105845301A (en) * | 2015-08-13 | 2016-08-10 | 北京中科三环高技术股份有限公司 | Rare earth permanent magnet and preparation method of rare earth permanent magnet |
| CN108555240A (en) * | 2017-11-30 | 2018-09-21 | 深圳粤网节能技术服务有限公司 | A kind of microwave casting method |
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| EP2722855A1 (en) * | 2012-10-19 | 2014-04-23 | Siemens Aktiengesellschaft | Nd-Fe-B permanent magnet without Dysprosium, rotor assembly, electromechanical transducer, wind turbine |
| US9276731B2 (en) * | 2013-08-08 | 2016-03-01 | Qualcomm Incorporated | N-phase signal transition alignment |
| ES2543652B1 (en) * | 2013-12-30 | 2016-03-01 | Universidad De Sevilla | Method for powder metallurgy manufacturing |
| KR101633252B1 (en) * | 2014-12-23 | 2016-06-27 | 주식회사 포스코 | Preparation method of high energy magnet |
| DE102015012412A1 (en) * | 2015-09-25 | 2017-03-30 | Wilo Se | Apparatus and method for producing annular permanent magnets |
| CN111128541B (en) * | 2019-12-27 | 2022-01-04 | 广西科学院 | Microwave sintering method of neodymium iron boron magnet |
| CN111554505B (en) * | 2020-05-26 | 2022-12-20 | 合肥夸夫超导科技有限公司 | Preparation method of PbMo6S8 superconducting wire |
| CN112458384B (en) * | 2020-11-25 | 2022-08-02 | 浙江炜烨晶体纤维有限公司 | Adopt polycrystal mullite fibre heat retaining discharge plasma sintering mould |
| CN113333759B (en) * | 2021-03-31 | 2023-04-18 | 宁波同创强磁材料有限公司 | Recycling method of phosphated neodymium iron boron waste |
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Also Published As
| Publication number | Publication date |
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| JP2013219353A (en) | 2013-10-24 |
| US20130266473A1 (en) | 2013-10-10 |
| DE102013205769A1 (en) | 2013-10-10 |
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