CN102347126B - High-performance sintered neodymium-iron-boron (Nd-Fe-B) rare-earth permanent magnet material and manufacturing method thereof - Google Patents
High-performance sintered neodymium-iron-boron (Nd-Fe-B) rare-earth permanent magnet material and manufacturing method thereof Download PDFInfo
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- 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
- H01F1/0572—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 with a protective layer
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- C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
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- 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
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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
Abstract
The invention discloses a high-performance sintered neodymium-iron-boron (Nd-Fe-B) rare-earth permanent magnet material and a manufacturing method thereof. The manufacturing method comprises the following steps: firstly, casting R-iron-boron-aluminum (R-Fe-B-Al) into a rapidly solidified alloy plate (R represents one and/or several of rare-earth elements containing Nd) by adopting a vacuum rapid solidifying process, then, coating a metal penetrant comprising the component Ra-Al or Ra-Al-X [the Ra represents dysprosium (Dy) and/or terbium (Tb), and the X represents one or several of cobalt, copper, gallium and zirconium (Co, Cu, Ga and Zr) elements] to the surface of the alloy plate, and heating to enable the metal penetrant to penetrate into the crystal boundary of the rapidly solidified alloy plate. A replacement reaction happens between the Ra in the penetrant entering the crystal boundary of the rapidly solidified alloy plate and the Nd and/or praseodymium (Pr) in the main phase of the alloy plate to form an Rh2(Fe, Al)14B phase with high content of the Dy and/or the Tb (the Rh represents that the content of the Dy and/or the Tb is higher than that of the Dy and/or the Tb in the R), and the positions of part of Fe atoms are replaced by Al atoms to encircle the double-main phase structure of an R2Fe14B phase. The high-performance sintered neodymium-iron-boron (Nd-Fe-B) rare-earth permanent magnet material disclosed by the invention is capable of effectively improving a coercive force and obviously reducing the use level of rare earth, and simultaneously, is also capable of improving the corrosion resistance of a magnet.
Description
Technical field
The invention belongs to permanent magnetic material field, particularly relate to a kind of high performance sintered neodymium-iron-boron rare earth permanent-magnetic material and manufacture method
Background technology
Nd-Fe-B rare earth permanent magnetic material, since coming out, has more and more been applied with its good magnetic property, is widely used in medical Magnetic resonance imaging, computer hard disc driver, sound equipment, mobile phone etc.; Along with energy-conservation and requirement low-carbon economy, the field application such as Nd-Fe-B rare earth permanent magnetic material starts again the motor at car electrics, household electrical appliance, energy-saving electric machine, hybrid vehicle, wind power generating motor.
Nineteen eighty-two, first SUMITOMO CHEMICAL particulate metal company disclosed the Japan Patent 1,622,492 of neodymium iron boron, and this patent has disclosed the new neodymium iron boron compound that exists to have high magnetic property first.Its composition is R-Fe-B-M, and R is one or more in the rare earth that comprises Nd here, and Fe is transiting group metal elements Fe, and B represents nonmetalloid B, and M is one or more of any element that can find on the periodic table of elements.Production technology adopts powder metallurgical technique, first adopts vacuum melting furnace, and under vacuum or protection gas, founding becomes alloy pig; Then make by operations such as powder process, pressing under magnetic field, sintering the third generation rare earth permanent-magnetic material that is called as Nd-Fe-B rare-earth permanent magnet.Compared with second generation rare earth permanent-magnetic material SmCo, replace cobalt with iron, low price many, and magnetic energy product is several times of second generation rare earth permanent magnet.People thereupon to this material carry out study widely and start application.Soon, the structure of this compound is just identified, and principal phase is R
2fe
14b phase, Grain-Boundary Phase is by rich R phase and B phase composition.The people such as Hadijtanayis studies and confirms that principal phase is Tetragonal crystal structure subsequently, and measures Nd
2fe
14b phase lattice constant is a=0.8792, c=1.2177; Dy
2fe
14the lattice constant of B phase is a=0.8757, c=1.1990.
June nineteen ninety-five SUMITOMO CHEMICAL particulate metal company again to U. S. application a patent with Tetragonal crystal structure that the principal phase of quite being disputed on is made up of Fe-Co-B-R, principal phase is containing Co patent.For distinguishing previous patent, this patent clearly proposes not comprise that Co is zero.This patent has disclosed principal phase and has had Tetragonal crystal structure, its lattice constant a
0approximately 0.88nm, c
0approximately 1.2nm.And in principal phase, replace part Fe with Co, Curie temperature does not contain Fe-B-R or the Fe-B-R-M of Co higher than principal phase.
Nineteen ninety-five, Japanese three moral metal company have replaced by vacuum rapid hardening technique the vacuum ingot casting process always using.Day disclosure special permission: Unexamined Patent 9-155507 has disclosed principle and the key technology of this technology.Raw material is smelted into alloy under vacuum state and inert gas shielding, and molten alloy to water cooled rolls, under water cooled rolls quick cooling, becomes alloy sheet by the alloy rapid hardening of melting by trough casting; Can control the size, size uniform of crystal grain because rapid hardening slab technique has, without advantages such as α-iron, from 1997, this technology was applied fast, Chinese patent: ZL97217372.2, ZL01141410.3 are disclosed is also this technology.
As everyone knows, neodymium iron boron is mainly by principal phase R
2fe
14b and Grain-Boundary Phase (rich neodymium phase and boron-rich phase) composition.Principal phase R
2fe
14b shared ratio in material is larger, and magnetic property is just higher; Accordingly, the content of rare earth will approach the content of principal phase as far as possible.In the time that rare earth reduces, easily form again α-iron, do not reach the principal phase requirement of design.Grain-Boundary Phase can not form again liquid-phase sintering very little.Nineteen ninety, in the international rare earth permanent magnet that the people such as Otsuki E hold at a Regensburg and application meeting, two alloyages are proposed, by principal phase direct ratio composition molten alloy, be called as the first alloy, then by composition melting second alloy of the Grain-Boundary Phase of rich neodymium phase and boron-rich phase composition; Two kinds of alloys can be used respectively the melting of vacuum rapid hardening technique, after melting, mix by a certain percentage, and follow-up technique is identical with other technique.In order to improve the coercive force of magnet, have people in the rare earth R of the second alloy mainly taking Dy, Tb as main.
Chinese patent ZL200610089124.7 discloses the people such as the Yue Ming of Beijing University of Technology and has done second-phase with nanometer Dy, Tb powder, with the technology of first-phase mixing manufacture high-coercive force neodymium iron boron.Under the same conditions, saved the consumption of heavy rare earth.
The inventor, by research and probe, has obtained a kind of high performance sintered neodymium-iron-boron Rare earth permanent-magnet material and its preparation method of corrosion-resistant, low heavy rare earth consumption.
Compared with prior art; one of advantage of the present invention is adding of Dy and/or Tb; to infiltrate agent by metal to infiltrate along crystal boundary; and replace with Pr and/or Nd; be enclosed in principal phase around, improving the coercitive while, less to the reduction of magnetic energy product; significantly reduce the consumption of heavy rare earth, protected tellurian scarce resource.
Compared with prior art, another advantage of the present invention is adding of Al, Co, Cu, Ga, Zr, is to infiltrate agent by metal to infiltrate along crystal boundary, and is retained in crystal boundary, has reduced the probability that enters principal phase.Improve magnetic property, improved again the corrosion resistance of crystal boundary, thereby also improved the corrosion resistance of magnet.
Summary of the invention
A kind of high performance sintered neodymium-iron-boron rare earth permanent-magnetic material and manufacture method, its master alloying is made up of the R-Fe-B-Al alloy that adds a small amount of metal element A l, and R represent one in the rare earth element that comprises Nd and/or multiple here.First adopting vacuum rapid hardening technique, described R-Fe-B-Al founding is become to rapid hardening alloy sheet, is then that (Ra represents Dy and/or Tb here for Ra-Al or Ra-Al-X by composition; X represents one or more in Co, Cu, Ga, Zr element) metal infiltrate agent and be coated to the surface of alloy sheet, then heating penetrates in the crystal boundary of described rapid hardening alloy sheet; Penetrate into the Ra in the infiltration agent in the crystal boundary of rapid hardening alloy sheet and the Nd in alloy sheet principal phase and/or Pr displacement reaction occurs, form the Rh of high Dy and/or Tb content
2(Fe, Al)
14(Rh represents that the content of Dy and/or Tb is higher than the content of the Dy in R and/or Tb to B phase here; The position of part Fe atom is replaced by Al atom) encirclement R
2fe
14two principal phase structures of B phase.What Fe, the B in crystal boundary had also forms new Rh with Dy and/or Tb
2(Fe, Al)
14b phase.
Infiltrate in agent at Ra-Al or Ra-Al-X metal, the adding of Al reduced Ra-Al-X metal and infiltrate the fusing point of agent, increased mobility and wettability, be conducive to Ra-Al-X metal and infiltrate the infiltration of agent, therefore, Al is essential element.
In the time that Ra-Al-X metal infiltration agent contains Elements C o, Co replacement of fe in crystal boundary, Fe is combined with Ra, B and is formed new principal phase Rh
2(Fe, Al)
14b phase, thus, has increased the content of principal phase, and due in crystal boundary, Co is more corrosion-resistant than Fe again, has improved the decay resistance of magnet.In the time that the content of Co in magnet is greater than 3%wt, Co can enter principal phase, and at this moment the remanent magnetism of magnet and coercive force can reduce, but can improve the Curie temperature of magnet.
When Ra-Al-X metal infiltrates agent while containing element Cu, Cu is present in crystal boundary, is conducive to improve the coercive force of magnet, especially, with the interpolation of combining of Co, obviously improves coercive force.The content of Cu in magnet is less than 0.3%wt.Too much Cu can enter principal phase, obviously reduces coercive force and the remanent magnetism of magnet.
In the time containing Ga in Ra-Al-X metal infiltration agent, Ga is present in crystal boundary, improves the lubrification of crystal boundary, restrains growing up of crystal grain, is beneficial to improving coercive force and thermal stability.
In the time containing Zr in Ra-Al-X metal infiltration agent, Zr is also present in crystal boundary, and the abnormal growth of restriction crystal grain is beneficial to stablizing follow-up sintering process.
When Ra-Al-X metal infiltrates while containing two or more in Co, Cu, Ga, Zr in agent, performance is better than adding separately, and especially four kinds add simultaneously, best performance.Combine and add, be conducive to infiltration, optimization crystal boundary that metal infiltrates agent, be also conducive to new Rh
2(Fe, Al)
14b forms mutually, and restriction abnormal grain growth.
Find that after deliberation the infiltration capacity 1%-10%wt of Ra-Al or Ra-Al-X metal infiltration agent, for best, in the time that infiltration capacity is less than 1%wt, cannot bring into play the effect of metal infiltration agent; When infiltrating when agent is greater than 10%wt, metal infiltrates difficulty, overlong time, and practical value is little.
Find after testing Rh
2(Fe, Al)
14b also has tetragonal structure, wherein a mutually
0be about 0.87nm; c
0be about 1.19nm, compare R
2fe
14the a of B phase
0little.R
2fe
14b phase crystallite dimension is at 5-50 μ m; Rh
2(Fe, Al)
14b is enclosed in R
2fe
14the skin of B, thickness is less than 30 μ m.
Further research is found, before metallic cementation or in metallic cementation process, passes into hydrogen, is conducive to the infiltration of metal infiltration agent.Therefore, before metallic cementation or in metallic cementation process, can pass into hydrogen.
After metallic cementation, adopt conventional production method, complete the operations such as airflow milling powder, pressing under magnetic field, sintering timeliness.In process of production, oxygen content, powder process granularity and sintering temperature are larger on the impact of production high-performance magnet.
Adopt the magnet produced of said method, there is the structure similar to rapid hardening alloy sheet after metallic cementation.Remain Rh
2(Fe, Al)
14b is enclosed in R
2fe
14the skin of B, just Rh
2(Fe, Al)
14b embracing layer has the trend of thickening.
Ra-Al or Ra-Al-X metal are infiltrated to the method that agent is coated to alloy sheet surface and have physical vaporous deposition, chemical vapour deposition technique.Also having a kind of method is first Ra-Al or Ra-Al-X to be smelted into alloy, then makes particle mean size and is less than 3 μ m powder, then powder coating is arrived to the surface of rapid hardening alloy sheet.In coating process, can add solvent.
Embodiment
Further illustrate remarkable result of the present invention below by the contrast of embodiment.
In the following example, metal infiltration agent manufacture method is: first Ra-Al or Ra-Al-X raw metal are melted under vacuum condition, be then filled with argon gas vacuum degree is reduced to-below 0.2MPa.Be incubated after 40 minutes, be cast in water-cooled film tool cooling, after 1 hour take out, then alloy is made to the alloy powder that particle mean size is 2.2 μ m.Content according to the form below is coated to the surface of alloy sheet.The composition of alloy sheet and metal infiltrate the composition of agent and also list in following form.
In the following example, the production technology of magnet is as follows: the temperature of metallic cementation is 900 DEG C; Be incubated 8 hours, then cooling with stove; The particle mean size of airflow milling powder is 3.5 μ m; The field intensity of pressing under magnetic field is 1.9T, and pressure is 22MPa; Sintering temperature is 1080 DEG C, is incubated 3 hours.Specimen size is 30 × 30 × 20mm, and 20 is magnetic field orientating direction.
Embodiment 1
Ra-Al metal infiltrates agent, during not containing Co, Cu, Ga, Zr.Compared with prior art (comparative example), along with the increase of metal infiltration agent, the magnetic property of magnet increases, and especially coercive force increases significantly; Infiltrate in agent at metal, while replacing Dy with Tb, coercive force increase is more obvious.What table 1 provided is metal infiltrates agent composition, metal infiltrate the composition of the content of agent in corresponding alloy sheet and corresponding alloy sheet.Table 2 is magnetic property and decay resistances that corresponding table 1 is numbered.Wherein B00 is numbered the comparative example of prior art.
Table 1:
Note: wt% represents percentage by weight
Table 2
Embodiment 2
When in Ra-Al-X metal infiltration agent, X is Co, along with the increase of metal infiltration agent, the magnetic property of magnet improves thereupon, but weightless obviously minimizing.Metal infiltrates composition, the infiltration capacity parameter of metal infiltration agent in alloy sheet of agent and alloy sheet and lists table 3 in; Corresponding performance is listed table 4 in.
Table 3:
Note: wt% represents percentage by weight
Table 4
Embodiment 3
When in Ra-Al-X metal infiltration agent, X is Co, Cu, can be found out by table 5 and table 6, along with the increase of metal infiltration agent, the magnetic property of magnet improves, but weightless obviously minimizing.
Table 5:
Note: wt% represents percentage by weight
Table 6
Embodiment 4
When in Ra-Al-X metal infiltration agent, X is Co, Cu, Ga, can be found out by table 7 and table 8, along with the increase of metal infiltration agent, the magnetic property of magnet improves, but weightless obviously minimizing.
Table 7:
Note: wt% represents percentage by weight
Table 8
Embodiment 5
When in Ra-Al-X metal infiltration agent, X is Co, Cu, Ga, Zr, can be found out by table 9 and table 10, along with the increase of metal infiltration agent, the magnetic property of magnet improves, but weightless obviously minimizing.
Table 9:
Note: wt% represents percentage by weight
Table 10
Claims (2)
1. the manufacture method of a high performance sintered neodymium-iron-boron rare earth permanent-magnetic material, its master alloying is made up of the R-Fe-B-Al alloy that adds a small amount of metal element A l, R represents a kind of and/or multiple in the rare earth element that comprises Nd, it is characterized in that, first adopt vacuum rapid hardening technique, R-Fe-B-Al founding is become to rapid hardening alloy sheet; Then the metal that is Ra-Al-X by composition infiltrates agent and penetrates in the crystal boundary of rapid hardening alloy sheet, and Ra represents Dy and/or Tb; X represents one or more in Co, Cu, Ga, Zr element, and the infiltration capacity that the metal that composition is Ra-Al-X infiltrates agent is less than 10% of alloy sheet weight; Penetrate into the Ra in the infiltration agent in the crystal boundary of rapid hardening alloy sheet and the Nd in alloy sheet principal phase and/or Pr displacement reaction occurs, form the Rh of high Dy and/or Tb content
2(Fe, Al)
14b surrounds R mutually
2fe
14two principal phase structures of B phase, Rh represents that the content of Dy and/or Tb is higher than the content of the Dy in R and/or Tb; The position of part Fe atom is replaced by Al atom; Then, produce performance Nd Fe B sintered magnet through airflow milling powder, pressing under magnetic field, sintering and timeliness operation; Adopt the magnet produced of said method, there is the structure identical with rapid hardening alloy sheet after metallic cementation, remain Rh
2(Fe, Al)
14b is enclosed in R
2fe
14the skin of B, Rh
2(Fe, Al)
14b thickening;
Involutory gold plaque carries out passing into hydrogen in metallic cementation process; Rh in alloy sheet after metallic cementation
2(Fe, Al)
14b has tetragonal structure mutually, wherein lattice constant a
0be about 0.87nm; c
0be about 1.19nm, compare R
2fe
14the lattice constant a of B phase
0little; R
2fe
14b phase crystallite dimension is at 5-50 μ m; Rh
2(Fe, Al)
14b is enclosed in R
2fe
14the skin of B, thickness is less than 30nm; Composition is that the metal of Ra-Al-X infiltrates X in agent and represents Co, Cu, Ga, Zr, and metal infiltrates agent and is made up of Ra-Al-Co-Cu-Ga-Zr.
2. method according to claim 1, is characterized in that: when the involutory gold plaque of metal infiltration agent that composition is Ra-Al-X carries out metallic cementation and oozes after-baking, metallic cementation temperature range is 500-1100 DEG C.
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PCT/CN2011/074855 WO2012013086A1 (en) | 2010-07-30 | 2011-05-30 | High performance sintered ndfeb magnet and manufacturing method of the same |
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