CN106601401B - Preparation method of high abundance rare earth Sintered NdFeB magnet of crystal boundary sandwich construction regulation and control and products thereof - Google Patents

Preparation method of high abundance rare earth Sintered NdFeB magnet of crystal boundary sandwich construction regulation and control and products thereof Download PDF

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CN106601401B
CN106601401B CN201611150726.9A CN201611150726A CN106601401B CN 106601401 B CN106601401 B CN 106601401B CN 201611150726 A CN201611150726 A CN 201611150726A CN 106601401 B CN106601401 B CN 106601401B
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rare earth
crystal boundary
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powder
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CN106601401A (en
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张培
胡梅娟
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Institute of Materials of CAEP
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    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032Magnets 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
    • H01F1/04Magnets 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
    • H01F1/047Alloys characterised by their composition
    • H01F1/053Alloys characterised by their composition containing rare earth metals
    • H01F1/055Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/057Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
    • H01F1/0571Alloys 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
    • H01F1/0575Alloys 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
    • H01F1/0577Alloys 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
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00Apparatus 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
    • H01F41/02Apparatus 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
    • H01F41/0253Apparatus 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

Abstract

The invention discloses preparation method of high abundance rare earth Sintered NdFeB magnet of crystal boundary sandwich construction regulation and control and products thereof, purpose is that solution existing method can not realize the finely regulating to grain boundary structure, cause intercrystalline strengthening single effect, heavy rare earth serious waste of resources, and with the sharp increase of magnet dosage, the problem of by causing limited rare earth resources largely to consume.In the present invention, using pairing gold process and double sintering technology, the preparation of the high abundance rare earth Sintered NdFeB magnet of crystal boundary sandwich construction regulation and control is realized.Magnet prepared by the present invention has double principal phase structures, i.e., has Nd simultaneously2Fe14B principal phases and (La, Nd)2Fe14B/(Ce,Nd)2Fe14B principal phases;And Grain-Boundary Phase has high potential crystal boundary central core/heavy rare earth shell layer multi-layer grain boundary structure of heavy rare earth shell layer/rare earth containing high abundance.The present invention by the finely regulating to grain boundary structure, realizes comprehensive raising of magnet magnetic property and corrosion resistance, has higher application value and economic value on the basis of realizing high abundance rare earth and making full use of.

Description

The preparation method of the high abundance rare earth Sintered NdFeB magnet of crystal boundary sandwich construction regulation and control And products thereof
Technical field
The present invention relates to permanent-magnet material field, the high abundance rare earth sintering neodymium iron of specially a kind of crystal boundary sandwich construction regulation and control Preparation method of boron magnet and products thereof, i.e., a kind of high abundance rare earth sintered NdFeB magnetic of achievable crystal boundary sandwich construction regulation and control Preparation method of body and products thereof.
Background technology
Nd-Fe-B permanent magnet material has excellent magnetic property, is high-effect manufacture, small volume, magnetic function device in light weight The ideal material of part, it has been widely used in electric bicycle, electric motor of automobile, computer hard disc, electronic toy, electric tool etc. Product, and the field such as stereo set, communication product, consumer electronics, Medical Devices, household appliances, magnetic plant, its product shelves Secondary high, added value height, operation strategies are wide.Especially in the voice coil motor of computer hard disc driver(VCM)And motor (HDD), New-type electric machine, Magnetic resonance imaging(MRL)In application Deng core component, Nd-Fe-B permanent magnet material has irreplaceable Effect.
In recent years, the fast development of wind-power electricity generation and electric automobile, magnetic is had based on Nd-Fe-B permanent magnet material itself High, abundant raw material and lower-price characteristic, wind-power electricity generation and electric automobile field are in the demand of high-performance neodymium-iron-boron magnet Explosive increase.Therefore, neodymium iron boron industry is also considered as the Chaoyang industry of 21 century.
The principal phase of neodymium iron boron magnetic body is Nd2Fe14B Hard Magnetic phases, Grain-Boundary Phase are rich-Nd phase.Wherein, the composition of Grain-Boundary Phase, structure With distribution for magnet magnetic property, corrosion resistance and mechanical performance, having obviously influences.
At present, researcher mainly added by alloying, crystal boundary modified and grain boundary decision the methods of, realize to Grain-Boundary Phase Strengthen, so as to improve magnet performance.Existing method can not realize the finely regulating to grain boundary structure, cause intercrystalline strengthening effect list First, the problems such as heavy rare earth serious waste of resources.In addition, with the sharp increase of magnet dosage, limited rare earth resources turn into limitation neodymium The major issue of iron boron application.
Therefore, there is an urgent need to a kind of new method or material, to alleviate above mentioned problem.
The content of the invention
The goal of the invention of the present invention is:The finely regulating to grain boundary structure can not be realized for existing method, causes crystalline substance Boundary strengthens single effect, heavy rare earth serious waste of resources, and with the sharp increase of magnet dosage, by causing, limited rare earth resources are big The problem of amount consumption, there is provided a kind of preparation method of the high abundance rare earth Sintered NdFeB magnet of crystal boundary sandwich construction regulation and control and its Product.In the present invention, using pairing gold process and double sintering technology, the high abundance rare earth that crystal boundary sandwich construction regulates and controls is realized The preparation of Sintered NdFeB magnet.Magnet prepared by the present invention has double principal phase structures, i.e., has Nd simultaneously2Fe14B principal phases and (La,Nd)2Fe14B/(Ce,Nd)2Fe14B principal phases;And Grain-Boundary Phase has the high potential of heavy rare earth shell layer/rare earth containing high abundance brilliant Boundary's central core/heavy rare earth shell layer multi-layer grain boundary structure.The present invention is led on the basis of realizing high abundance rare earth and making full use of The finely regulating to grain boundary structure is crossed, realizes comprehensive raising of magnet magnetic property and corrosion resistance.Wherein, double principal phase structures The deterioration of principal phase magnetic property can be suppressed, being distributed in the heavy rare earth shell layer on main phase grain border has higher magnetocrystalline different Property field, therefore, it is possible to suppress the magnetic domain of the crystal boundary weakness zone in opposing magnetic field reversion, and then improve magnet coercivity and height Temperature stability.Meanwhile heavy rare earth shell layer is only distributed in main phase grain border, is seldom diffused into principal phase and crystal boundary central area, Heavy rare earth dosage is greatly reduced, reduces magnet generation cost.And the shape of the high potential crystal boundary central core of the rare earth containing high abundance Into then further improving the dosage of light rare earth, while reduce Grain-Boundary Phase and Nd2Fe14The difference in Electrode Potential of B principal phases, reduce electricity Chemical attack driving force, hence it is evident that improve the corrosion resistance of magnet.
To achieve these goals, the present invention adopts the following technical scheme that:
The preparation method of the high abundance rare earth Sintered NdFeB magnet of crystal boundary sandwich construction regulation and control, comprises the following steps:
(1)Low rare-earth Nd-Fe-B main-phase alloy powder A1, the MM of rare earth containing high abundance neodymium iron boron main-phase alloy powder A2 are taken respectively, Low rare-earth Nd-Fe-B main-phase alloy powder A1, the MM of rare earth containing high abundance neodymium iron boron main-phase alloy powder A2 and low melting point heavy rare earth is brilliant Boundary reconstruct alloyed powder R1xM1yMixing, obtains the first mixture, and the first mixture is heated into the reconstruct of low melting point heavy rare earth crystal boundary closes Bronze R1xM1yMore than fusing point, and heating-up temperature is less than 1100 DEG C, makes low rare-earth Nd-Fe-B main-phase alloy A1, main-phase alloy A2 brilliant Grain edge forms the heavy rare earth shell layer of high magnetocrystalline anisotropy, obtains intermediate;
(2)By step(1)After the intermediate of preparation is broken, gained powder and the low melting point high potential containing high abundance rare earth Crystal boundary reconstruct alloy MMaM2bMixing, obtains the second mixture, after the second mixture is carried out into magnetic field orientating shaping, carries out successively Sintering, heat treatment, produce product.
The MM is the one or more in La, Ce.
The particle mean size of the low rare-earth Nd-Fe-B main-phase alloy powder A1 is less than 5 μm, and rare earth element content is less than 29 Wt.%, Nd2Fe14B phases proportion is more than 95 %.
The neodymium iron boron main-phase alloy powder A2 of the MM of rare earth containing high abundance particle mean size is less than 5 μm, high abundance therein Rare earth MM accounts for 3 more than wt.% of main-phase alloy powder A2 gross masses.
High abundance rare earth MM accounts for the wt.% of 3 wt.% of main-phase alloy powder A2 gross masses ~ 20.
The low melting point heavy rare earth crystal boundary reconstruct alloyed powder R1xM1yIn, R1 is one kind in lanthanide series metal Gd, Tb, Dy, Ho Or a variety of, the one or more in M1 O, F, H, Cu, Ni, Fe, Co, Sn, Ti, Nb, Zr, x, y are respectively R1, M1 atom hundred Fraction, x scope are 5 ~ 80, x and y's and be 100.
The low melting point heavy rare earth crystal boundary reconstruct alloyed powder R1xM1yFusing point be less than 900 DEG C.
The low melting point high potential crystal boundary reconstruct alloy MMaM2bIn, MM is one or both of lanthanide series metal La, Ce, M2 is the one or more in high standard noble potential metal Cu, Ni, Fe, Co, and a, b are respectively MM and M2 atomic percentage, a model Enclose for 5 ~ 80, a and b's and be 100.
The low melting point heavy rare earth crystal boundary reconstruct alloyed powder R1xM1y, low melting point high potential crystal boundary reconstruct alloyed powder MMaM2b Granularity be 0.1-100 μm.
The step(2)In, after the second mixture is carried out into magnetic field orientating shaping, it is sintered, sintering temperature 950- 1100 DEG C, sintering time 2-5h, two-stage heat treatment is then carried out, one-level heat treatment temperature is 850-950 DEG C, and soaking time is 1-5h, two level heat treatment temperature are 300-600 DEG C, soaking time 1-5h, produce product.
Using the product prepared by preceding method.
In terms of intercrystalline strengthening mechanism, the coercivity of magnet is improved, it is necessary to form a floor height magnetocrystalline on main phase grain border Anisotropic heavy rare earth shell layer;And improve the corrosion resistance of magnet, then need to be centrally formed high potential stabilization in crystal boundary Grain-Boundary Phase;The continuity of Grain-Boundary Phase is improved, it is necessary to reduce Grain-Boundary Phase fusing point, and improve its wetability with principal phase.
At present, Grain-Boundary Phase is often studied its fusing point, magnetocrystalline anisotropy field and the change of corrosion potential as an entirety Change, the finely regulating to grain boundary structure can not be realized, the problems such as causing intercrystalline strengthening single effect, heavy rare earth serious waste of resources Occur.In addition, with the sharp increase of magnet dosage, limited rare earth resources turn into the major issue of limitation neodymium iron boron magnetic body application. And during rare earth mining, the association product as rare earth Nd such as the high abundance rare earth Las of rich reserves, Ce, because its 2:14:1 The theoretical magnetic property of phase is less than Nd2Fe14B does not obtain enough attention and utilization, causes the waste of high abundance rare earth resources.
To sum up, the current urgent problem of sintered neodymium iron boron material is concentrated mainly on following two aspects:1)Magnet Coercivity is low, and corrosion resistance is poor;2)High abundance rare earth La, Ce etc. are not fully used because intrinsic magnetic property is poor.
For the problem of neodymium iron boron magnetic body coercivity is low, corrosion resistance is poor, researcher mainly by alloying addition and Crystal boundary modified and reconstruct method realizes reinforcing to Grain-Boundary Phase, so as to improve the coercivity of Sintered NdFeB magnet and anticorrosive Performance.
Many researchers have studied the oligo-element alloying such as Al, Co, Cu, Ga, P, Cr, Ti, Zr, Pb, to improve magnet Decay resistance;These elements can chemically react with Nd, Fe in Grain-Boundary Phase or B element, generate relatively stable Grain-Boundary Phase, suppress corrosion and dissolving of the Grain-Boundary Phase in corrosive environment, so as to prevent coming off and magnetic device for main phase grain Failure.Although melting addition metal or alloy can form relatively stable Grain-Boundary Phase in crystal boundary, improving magnetic to a certain degree The corrosion resistance of body;But the element of melting addition typically has part and enters Nd2Fe14B principal phases, part substitute rare earth Nd or Transition-metal Fe, cause the decline of the intrinsic performance of magnet.Meanwhile some nonmagnetic elements enter principal phase and magnetic dilution can be caused to make With reducing the remanent magnetism and maximum magnetic energy product of magnet.
Crystal boundary modified and reconstruct refers to prepare Nd-Fe-B magnetics and crystal boundary addition powder respectively, and by mechanical mixture by two Kind powder is well mixed, the method for carrying out compacting sintering afterwards.Using crystal boundary adding method, can taking human as the crystalline substance that adds of design Boundary's modified powder, and follow-up sintering process temperature is typically at 1050-1100 DEG C or so, well below smelting temperature.Therefore, phase Added than melting, its additive can concentrate on Grain-Boundary Phase, and can try one's best it is few be diffused into principal phase, so as to maximum limit The additive that plays of degree improves the effect of Grain-Boundary Phase.It is different that addition heavy rare earth alloy can form high magnetocrystalline in magnet grain boundaries The heavy rare earth shell of property, so as to improve the coercivity of magnet;And high potential alloy is added, chemical property can be formed in grain boundaries Stable Grain-Boundary Phase, reduce principal phase and Grain-Boundary Phase potential difference, so as to improve magnet corrosion resistance.
However, research before is studied using Grain-Boundary Phase as an entirety, crystal boundary is strengthened by different methods, The finely regulating to crystal boundary internal structure is not realized, so as to cause unnecessary waste.It is for example, brilliant in heavy rare earth alloy Boundary is modified and reconstruct in, heavy rare earth shell that main phase grain border is formed can effectively improve magnet coercivity, and remaining big portion Divide heavy rare earth element to concentrate on crystal boundary central area, cause unnecessary waste.Meanwhile reconstruct magnetic in high potential alloy crystal boundary In body, grain boundaries form continuous stable Grain-Boundary Phase, and the intrinsic corrosion resistance of magnet greatly improved, but in order to reduce into This, heavy rare earth element is not contained in general high potential reconstruct alloy, so being lifted to coercivity little.At present, can not also realize It is substantially improved while neodymium iron boron magnetic body coercivity and corrosion resistance.
Think that the reason for causing above mentioned problem is mainly after inventor's analysis, it is brilliant under current process conditions Boundary's composition and structure can not realize finely regulating, can't control the magnetic reversal farmland forming core field of crystal boundary, grain boundary potentials and steady simultaneously It is qualitative, and the magnetic exchange coupling effect between main phase grain.
Meanwhile in order to solve the problem of rare earth Nd shortage, high abundance rare earth La, the Ce wastings of resources, the present invention is main to be used The mode such as double principal phase technologies and crystal boundary addition high abundance rare earth, to improve the utilization rate of La, Ce high abundance rare earth.Double principal phase structures Refer in neodymium iron boron magnetic body, while there is Nd2Fe14B principal phases and (La, Nd)2Fe14B/(Ce,Nd)2Fe14B principal phases, two-phase Between produce magnetic exchange coupling effect, magnetocrystalline anisotropy fieldH ARelatively low (La, Nd)2Fe14B/(Ce,Nd)2Fe14B principal phases are brilliant Grain border is due to foringH AHigher Nd2Fe14B shells, improve the coercivity of magnet.Therefore, double principal phases in the present invention Structure compensate for the shortcomings that intrinsic magnetic property of high abundance rare earth is poor.
In addition, thinking after inventor's research, the high potential alloy of crystal boundary addition high abundance rare earth can reduce principal phase and crystal boundary The potential difference of phase, improve the corrosion resistance of magnet.Containing for low melting point is designed by alloy phase diagram and metal master electrode potential The high potential alloy of high abundance rare earth, prepares neodymium iron boron magnetic body using pairing gold process afterwards, can realize high abundance rare earth collection In grain boundary area purpose, while corrosion resistance is improved, because high abundance rare earth is mainly distributed on grain boundaries, do not have Principal phase largely is diffused into, so as to keep the higher magnetic property of magnet.
While in order to realize that high abundance rare earth makes full use of, keep even improving the magnetic property and corrosion resistance of magnet Can, the present invention uses following design principle:1)With double principal phase structures, by the interaction between principal phase, the magnetic of magnet is kept Performance;2)Main phase grain border forms heavy rare earth shell layer, improves the coercivity and heat endurance of magnet;3)Crystal boundary center be containing High abundance rare earth high potential Grain-Boundary Phase, improve the corrosion resistance of magnet.
Based on this, the present invention provides a kind of preparation of the high abundance rare earth Sintered NdFeB magnet of crystal boundary sandwich construction regulation and control Method and products thereof, this method mainly comprise the following steps.
In the present invention, first, the Nd-Fe-B principal phases powder of low content of rare earth and the neodymium iron boron master containing high abundance rare earth are prepared Be harmonious bronze.Wherein, the method that the Nd-Fe-B principal phase powder A1 of low content of rare earth is quickly cooled down using melting and rejection tablet, is first made Strip, then by the way that hydrogen is quick-fried and air-flow grinding process, obtain the principal phase powder that average particle size particle size is less than 5 μm.The MM of rare earth containing high abundance Main-phase alloy powder use alloyage process, addition part high abundance rare earth substitution rare earth Nd, formation has (La, Nd)2Fe14B/ (Ce,Nd)2Fe14The alloy of B principal phases, and by the way that hydrogen is quick-fried and air-flow grinding process, obtain the principal phase that average particle size particle size is less than 5 μm Powder.Wherein, the particle mean size of low rare-earth Nd-Fe-B main-phase alloy powder A1 powder is less than 5 μm(Particle diameter may range from 0.01 ~ 5 μ m), rare earth element content is less than 29 wt.%, Nd2Fe14B phases proportion is more than 95 %.The MM of rare earth containing high abundance(MM=La、Ce One or both of)Neodymium iron boron main-phase alloy powder A2 particle mean size be less than 5 μm(Particle diameter may range from 0.01 ~ 5 μ m), high abundance rare earth MM therein accounts for 3 more than wt.% of main-phase alloy powder A2 gross masses(Can be 3 ~ 20 wt.%).The present invention In, signified high abundance rare earth is primarily referred to as La, Ce, and both mixtures.
Secondly, low melting point heavy rare earth crystal boundary reconstruct alloyed powder is prepared.It is low according to enthalpy of mixing between alloy phase diagram, element, design Fusing point heavy rare earth crystal boundary reconstructs the composition of alloy, generally eutectic composition, using vacuum arc melting or vacuum induction melting, Alloy pig is prepared, followed by modes such as ball milling or airflow millings, by alloy breaks down into the powder that granularity is 0.1-100 μm, Produce low melting point heavy rare earth crystal boundary reconstruct alloyed powder R1xM1y.Low melting point heavy rare earth crystal boundary reconstruct alloyed powder R1xM1yIn, R1 is lanthanum It is the one or more in metal Gd, Tb, Dy, Ho, one kind or more in M1 O, F, H, Cu, Ni, Fe, Co, Sn, Ti, Nb, Zr Kind, x, y are respectively R1, M1 atomic percentage, wherein, 5≤x≤80,20≤y≤95.Alloyed powder R1xM1y fusing point is less than 900℃。
Then, the low melting point high potential crystal boundary reconstruct alloyed powder of the rare earth containing high abundance is prepared.According between alloy phase diagram, element Enthalpy of mixing and metal master electrode potential, alloying component is designed, using vacuum arc melting or vacuum induction melting, is prepared Alloy pig, followed by modes such as ball milling or airflow millings, by alloy breaks down into the powder that granularity is 0.1-100 μm, produce eutectic Point high potential crystal boundary reconstruct alloy MMaM2b.Wherein, a and b is MM and M atomic percentage respectively, wherein, 5≤a≤80,20≤ B≤95, alloyed powder MMaM2bFusing point be less than 900 DEG C, the granularity of powder is 0.1-100 μm.
Again by low rare-earth Nd-Fe-B main-phase alloy powder A1, the MM of rare earth containing high abundance neodymium iron boron main-phase alloy powder A2 and eutectic Point heavy rare earth crystal boundary reconstruct alloyed powder R1xM1yMixing, obtains the first mixture, the first mixture is heated into low melting point heavy rare earth Crystal boundary reconstruct alloyed powder R1xM1yMore than fusing point, and heating-up temperature is less than 1100 DEG C so that crystal boundary reconstruct powder melts and is uniformly distributed Around main phase grain, reacted in heat treatment process with principal phase, make low rare-earth Nd-Fe-B main-phase alloy A1, main-phase alloy The higher heavy rare earth shell layer of A2 crystal edges generation magnetocrystalline anisotropy field, and then magnet coercivity is improved, obtain intermediate.
Finally, after the intermediate of preparation is crushed, gained powder and the low melting point high potential crystal boundary containing high abundance rare earth Reconstruct alloy MMaM2bUniformly mixing, obtains the second mixture, after the second mixture is carried out into magnetic field orientating shaping, carries out successively Sintering, heat treatment, are prepared the high abundance rare earth Sintered NdFeB magnet with multilayer grain boundary structure.
Wherein, treated intermediate powder and the low melting point high potential crystal boundary reconstruct alloyed powder magnetic containing high abundance rare earth After the oriented moulding of field, sintered at 950-1100 DEG C, be incubated 2-5 hours, be then heat-treated, one-level heat treatment temperature is 850-950 DEG C, soaking time is 1-5 hours, and two level heat treatment temperature is 300-600 DEG C, and soaking time is 1-5 hours.
To sum up, the invention provides a kind of high abundance rare earth Sintered NdFeB magnet of achievable crystal boundary sandwich construction regulation and control Preparation method, the present invention prepares the multilayer grain boundary structure for meeting to require, is advantageous to by the finely regulating to grain boundary structure Magnet prepare and use during, maintain the stability of the sandwich construction, and study the sandwich construction to magnet magnetic property, anti- The influencing mechanism of corrosive nature, and the research of this respect is rarely reported at present.
As shown in Fig. 2 give the high potential crystal boundary center in the present invention with heavy rare earth shell layer/rare earth containing high abundance The Sintered NdFeB magnet structural representation of layer/heavy rare earth shell layer multi-layer grain boundary structure.The magnet has double principal phase structures, together When there is the heavy rare earth shell layer of high magnetocrystalline anisotropy on main phase grain border, to contain high abundance rare earth at crystal boundary center High potential crystal boundary central core.The present invention utilizes high abundance rare earth and a small amount of heavy rare earth, and preparing grain boundary structure can finely regulating High-performance neodymium-iron-boron magnet, there is higher application value.
The magnet prepared to the present invention is measured, and measurement result shows, the present invention has the sintering of crystal boundary sandwich construction Coercivity can reach 16 more than kOe to neodymium iron boron magnetic body at room temperature, and heavy rare earth addition is less than 1 wt.%;In 3.5 wt.% chlorinations Corrosion potential in sodium water solution is higher than -0.80V, corrodes 96 in the environment of 120 DEG C, 2 atmospheric pressure and 100% relative humidity The weight loss of hour is less than 0.78mg/cm2.In the present invention, the formation of heavy rare earth shell layer substantially increases the magnetocrystalline of Grain-Boundary Phase Anisotropy fieldH A, and then improve the coercivity of magnetH cj, the formation of high potential crystal boundary central core substantially reduces Grain-Boundary Phase And Nd2Fe14The potential difference of B principal phases, i.e. electrochemical corrosion driving force, and then improve the corrosion resistance of magnet;Meanwhile Gao Feng A large amount of uses of degree rare earth greatly reduce production cost, and the magnetic property of magnet does not occur corruptions.
Brief description of the drawings
Examples of the present invention will be described by way of reference to the accompanying drawings, wherein:
Fig. 1 is traditional sintered NdFeB structural representation.
Fig. 2 is the structural representation that the present invention prepares magnet.
Embodiment
All features disclosed in this specification, or disclosed all methods or during the step of, except mutually exclusive Feature and/or step beyond, can combine in any way.
Any feature disclosed in this specification, unless specifically stated otherwise, can be equivalent by other or with similar purpose Alternative features are replaced.I.e., unless specifically stated otherwise, each feature is an example in a series of equivalent or similar characteristics .
Embodiment 1
The present embodiment comprises the following steps.
(1)Prepare the Nd-Fe-B principal phases powder of low content of rare earth and the neodymium iron boron principal phase powder containing high abundance rare earth
When preparing the Nd-Fe-B principal phase powder of low content of rare earth, the method that is quickly cooled down using melting and rejection tablet, neodymium iron is made Boron rapid hardening thin slice.Then, by the way that hydrogen is quick-fried and air-flow grinding process, the low content of rare earth that average particle size particle size is about 3.8 μm is obtained Nd-Fe-B principal phase powder.
Prepare the neodymium iron boron principal phase powder containing high abundance rare earth, composition Nd12.3FebalB6.1(Nd10.3La2.0) FebalB3.1.The method quickly cooled down using melting and rejection tablet, neodymium iron boron rapid hardening thin slice is made.Then, by the way that hydrogen is quick-fried and airflow milling Technique, obtain the neodymium iron boron principal phase powder containing high abundance rare earth that average particle size particle size is about 3.8 μm.
(2)Prepare low melting point heavy rare earth crystal boundary reconstruct alloy
According to enthalpy of mixing between alloy phase diagram, element, design low melting point heavy rare earth crystal boundary reconstruct alloying component, it is desirable in alloy Containing more heavy rare earth element, while fusing point is relatively low, can be melted in heat treatment process and be evenly distributed on main phase grain week Enclose.
Inventor have selected Dy-Ni binary eutectics point components D y69Ni31(Atomic percent)Reconstructed as heavy rare earth crystal boundary Alloy, its fusing point are 693 DEG C.Afterwards, the La-Co binary containing high abundance rare earth is have selected according to the standard electrode potential of metal Eutectic composition La69Co31(Atomic percent)Alloy is reconstructed as high potential crystal boundary, its fusing point is 500 DEG C.Then, electricity is passed through Arc melting is prepared for two kinds of crystal boundary reconstruct alloy pigs, and is prepared for the alloy powder that granularity is about 1.7 μm by ball milling.
(3)Prepare product
It is 1 in mass ratio by low rare-earth Nd-Fe-B main-phase alloy powder and the neodymium iron boron principal phase powder containing high abundance rare earth:1 Ratio uniform is mixed, and mixed powder and heavy rare earth crystal boundary then are reconstructed into alloyed powder Dy69Ni31Uniformly mixing, obtains the first mixing Thing, by the first mixture at 800 DEG C vacuum heat 2 hours, obtain intermediate.Obtained intermediate powder is crushed, divided Dissipate, and with high potential alloyed powder La69Co31Uniformly mixing, obtains the second mixture.Wherein, low rare earth principal phase powder(I.e. low rare earth The mixture of neodymium iron boron main-phase alloy powder and neodymium iron boron principal phase powder containing high abundance rare earth):Heavy rare earth crystal boundary reconstructs alloyed powder Dy69Ni31:High potential alloyed powder La69Co31Mass ratio be 97:1:2.By the second mixture under 1.6 T, 200 MPa, carry out Magnetic field orientating is molded, and is sintered at 1070 DEG C 4 hours, is then heat-treated 2 hours at 890 DEG C afterwards, then at 400 DEG C at heat Reason 2 hours, being made has double principal phase structures, while has the high potential crystal boundary center of heavy rare earth shell layer/rare earth containing high abundance The neodymium iron boron magnetic body of layer/heavy rare earth shell layer multi-layer grain boundary structure.
After measured, the obtained neodymium iron boron magnetic body with double principal phases and multilayer grain boundary structure of the present embodiment, its coercivity are 16.78 kOe, corrosion potential of the magnet in 25 DEG C, 3.5 wt.% sodium chloride solutions are -0.771 V;Magnet is at 120 DEG C, 2 In the environment of atmospheric pressure and 100% relative humidity, the weight loss of corrosion 96 hours is 0.65 mg/cm2
Embodiment 2
The present embodiment comprises the following steps.
(1)Prepare the Nd-Fe-B principal phases powder of low content of rare earth and the neodymium iron boron principal phase powder containing high abundance rare earth
The Nd-Fe-B principal phase powder of low content of rare earth, and the neodymium iron boron principal phase powder containing high abundance rare earth are prepared first(Composition For Nd12.3FebalB6.1(Nd10.3Ce2.0)FebalB3.1).The method quickly cooled down using melting and rejection tablet, neodymium iron boron speed is made Solidifying thin slice.Then, by the way that hydrogen is quick-fried and air-flow grinding process, two kinds of principal phase powder that average particle size particle size is about 3.8 μm are obtained.
(2)Prepare low melting point heavy rare earth crystal boundary reconstruct alloy
According to enthalpy of mixing between alloy phase diagram, element, design low melting point heavy rare earth crystal boundary reconstruct alloying component, it is desirable in alloy Containing more heavy rare earth element, while fusing point is relatively low, can be melted in heat treatment process, and is evenly distributed on main phase grain week Enclose.
The present embodiment have selected y-Ni binary eutectics point components D y71.5Fe28.5(Atomic percent)As heavy rare earth crystal boundary weight Structure alloy, its fusing point are 890 DEG C.Afterwards, the La-Co binary containing high abundance rare earth is selected according to the standard electrode potential of metal Eutectic composition La69Co31(Atomic percent)Alloy is reconstructed as high potential crystal boundary, its fusing point is 500 DEG C.Then, electricity is passed through Arc melting is prepared for two kinds of crystal boundary reconstruct alloy pigs, and is prepared for the alloy powder that granularity is about 1.7 μm by ball milling.
(3)Prepare product
It is 1 in mass ratio by the Nd-Fe-B principal phases powder of low content of rare earth and the neodymium iron boron principal phase powder containing high abundance rare earth: 1 ratio uniform mixing, then reconstructs alloyed powder Dy by mixed powder and heavy rare earth crystal boundary71.5Fe28.5Uniformly mixing, obtains first Mixture, by the first mixture at 800 DEG C vacuum heat 2 hours, obtain intermediate.Obtained intermediate powder is broken It is broken, scattered, and with high potential alloyed powder La69Co31Uniformly mixing, obtains the second mixture.Wherein, low rare earth principal phase powder:Weight is dilute Native crystal boundary reconstruct alloyed powder Dy69Ni31:High potential crystal boundary reconstruct alloy La69Co31Mass ratio be 96:2:2.By the second mixture Under 1.6 T, 200 MPa, magnetic field orientating shaping is carried out, is sintered 4 hours at 1070 DEG C afterwards, then at 890 DEG C at heat Reason 2 hours, then be heat-treated at 400 DEG C to be made for 2 hours there are pair principal phase structures, while there is heavy rare earth shell layer/contain Gao Feng Spend the neodymium iron boron magnetic body of high potential crystal boundary central core/heavy rare earth shell layer multi-layer grain boundary structure of rare earth.
After measured, the obtained neodymium iron boron magnetic body with double principal phases and multilayer grain boundary structure of the present embodiment, its coercivity are 18.46 kOe, corrosion potential of the magnet in 25 DEG C, 3.5 wt.% sodium chloride solutions are -0.777 V;Magnet is at 120 DEG C, 2 The weight loss corroded in the environment of atmospheric pressure and 100% relative humidity 96 hours is 0.68 mg/cm2
Embodiment 3
The present embodiment comprises the following steps.
(1)Prepare the Nd-Fe-B principal phases powder of low content of rare earth and the neodymium iron boron principal phase powder containing high abundance rare earth
The Nd-Fe-B principal phase powder of low content of rare earth, and the neodymium iron boron principal phase powder containing high abundance rare earth are prepared first(Composition For Nd12.3FebalB6.1(Nd9.3La3.0)FebalB3.1).The method quickly cooled down using melting and rejection tablet, neodymium iron boron speed is made Solidifying thin slice.Then, two kinds of principal phase powder that average particle size particle size is about 3.8 μm are obtained with air-flow grinding process by the way that hydrogen is quick-fried.
(2)Prepare low melting point heavy rare earth crystal boundary reconstruct alloy
According to enthalpy of mixing between alloy phase diagram, element, design low melting point heavy rare earth crystal boundary reconstruct alloying component, it is desirable in alloy Containing more heavy rare earth element, while fusing point is relatively low, can be melted in heat treatment process and be evenly distributed on main phase grain week Enclose.
The present embodiment selection Dy-Ni binary eutectic point components Ds y69Ni31(Atomic percent)Reconstructed as heavy rare earth crystal boundary Alloy, its fusing point are 693 DEG C.Afterwards, the La-Co binary containing high abundance rare earth is selected to be total to according to the standard electrode potential of metal Fisheye composition La69Co31(Atomic percent)Alloy is reconstructed as high potential crystal boundary, its fusing point is 500 DEG C.Then, electric arc is passed through Melting is prepared for two kinds of crystal boundary reconstruct alloy pigs, and is prepared for the alloy powder that granularity is about 1.7 μm by ball milling.
(3)Prepare product
It is 1 in mass ratio by the Nd-Fe-B principal phases powder of low content of rare earth and the neodymium iron boron principal phase powder containing high abundance rare earth: 1 ratio uniform mixing, then reconstructs alloyed powder Dy by mixed powder and heavy rare earth crystal boundary69Ni31Uniformly mixing, it is mixed to obtain first Compound, by the first mixture at 800 DEG C vacuum heat 2 hours, obtain intermediate.Obtained intermediate powder is crushed, It is scattered, and with high potential alloyed powder La69Co31Uniformly mixing, obtains the second mixture.Wherein, low rare earth principal phase powder:Heavy rare earth Grain boundary alloys powder:The mass ratio of high potential grain boundary alloys powder is 96:2:2.By the second mixture under 1.6 T, 200 MPa, enter Row magnetic field orientating is molded, and is sintered at 1070 DEG C 4 hours, is then heat-treated 2 hours at 890 DEG C afterwards, then the heat at 400 DEG C Processing is made for 2 hours has double principal phase structures, while has the high potential crystal boundary center of heavy rare earth shell layer/rare earth containing high abundance The neodymium iron boron magnetic body of layer/heavy rare earth shell layer multi-layer grain boundary structure.
After measured, the obtained neodymium iron boron magnetic body with double principal phases and multilayer grain boundary structure of the present embodiment, its coercivity are 18.12 kOe, corrosion potential of the magnet in 25 DEG C, 3.5 wt.% sodium chloride solutions are -0.784 V;Magnet is at 120 DEG C, 2 The weight loss corroded in the environment of atmospheric pressure and 100% relative humidity 96 hours is 0.69 mg/cm2
Embodiment 4
The present embodiment comprises the following steps.
(1)Prepare the Nd-Fe-B principal phases powder of low content of rare earth and the neodymium iron boron principal phase powder containing high abundance rare earth
The Nd-Fe-B principal phase powder of low content of rare earth, and the neodymium iron boron principal phase powder containing high abundance rare earth are prepared first(Composition For Nd12.3FebalB6.1(Nd9.3La2.0Ce1.0)FebalB3.1).The method quickly cooled down using melting and rejection tablet, neodymium iron is made Boron rapid hardening thin slice.Then, two kinds of principal phase powder that average particle size particle size is about 3.8 μm are obtained with air-flow grinding process by the way that hydrogen is quick-fried.
(2)Prepare low melting point heavy rare earth crystal boundary reconstruct alloy
According to enthalpy of mixing between alloy phase diagram, element, design low melting point heavy rare earth crystal boundary reconstruct alloying component, it is desirable in alloy Containing more heavy rare earth element, while fusing point is relatively low, can be melted in heat treatment process and be evenly distributed on main phase grain week Enclose.
Inventor selects Dy-Ni binary eutectic point components Ds y71.5Fe28.5(Atomic percent)Reconstructed as heavy rare earth crystal boundary Alloy, its fusing point are 890 DEG C.Afterwards, the La-Co binary containing high abundance rare earth is selected to be total to according to the standard electrode potential of metal Fisheye composition La69Co31(Atomic percent)Alloy is reconstructed as high potential crystal boundary, its fusing point is 500 DEG C.Then, electric arc is passed through Melting is prepared for two kinds of crystal boundary reconstruct alloy pigs, and is prepared for the alloy powder that granularity is about 1.7 μm by ball milling.
(3)Prepare product
It is 4 in mass ratio by the Nd-Fe-B principal phases powder of low content of rare earth and the neodymium iron boron principal phase powder containing high abundance rare earth: 6 ratio uniform mixing, then reconstructs alloyed powder Dy by mixed powder and heavy rare earth crystal boundary71.5Fe28.5Uniformly mixing, obtains first Mixture, by the first mixture at 800 DEG C vacuum heat 2 hours, obtain intermediate.Obtained intermediate powder is broken It is broken, scattered, and with high potential alloyed powder La69Co31Uniformly mixing, obtains the second mixture.Wherein, low rare earth principal phase powder:Weight is dilute Native grain boundary alloys powder:The mass ratio of high potential grain boundary alloys powder is 96:2:2.Second mixture is mixed after powder in 1.6 T, 200 Under MPa, magnetic field orientating shaping is carried out, sinters at 1070 DEG C 4 hours, is then heat-treated 2 hours at 890 DEG C afterwards, then It is heat-treated 2 hours at 400 DEG C, being made has double principal phase structures, while has the height electricity of heavy rare earth shell layer/rare earth containing high abundance The neodymium iron boron magnetic body of position crystal boundary central core/heavy rare earth shell layer multi-layer grain boundary structure.
After measured, the obtained neodymium iron boron magnetic body with double principal phases and multilayer grain boundary structure of the present embodiment, its coercivity are 17.88 kOe, corrosion potential of the magnet in 25 DEG C, 3.5 wt.% sodium chloride solutions are -0.790 V.Magnet is at 120 DEG C, 2 The weight loss corroded in the environment of atmospheric pressure and 100% relative humidity 96 hours is 0.75 mg/cm2
The invention is not limited in foregoing embodiment.The present invention, which expands to, any in this manual to be disclosed New feature or any new combination, and disclose any new method or process the step of or any new combination.

Claims (12)

1. the preparation method of the high abundance rare earth Sintered NdFeB magnet of crystal boundary sandwich construction regulation and control, it is characterised in that including such as Lower step:
(1)Low rare-earth Nd-Fe-B main-phase alloy powder A1, the MM of rare earth containing high abundance neodymium iron boron main-phase alloy powder A2 are taken respectively, will be low Rare-earth Nd-Fe-B main-phase alloy powder A1, the MM of rare earth containing high abundance neodymium iron boron main-phase alloy powder A2 and low melting point heavy rare earth crystal boundary weight Structure alloyed powder R1xM1yMixing, obtains the first mixture, and the first mixture is heated into low melting point heavy rare earth crystal boundary reconstruct alloyed powder R1xM1yMore than fusing point, and heating-up temperature is less than 1100 DEG C, makes low rare-earth Nd-Fe-B main-phase alloy A1, main-phase alloy A2 crystal grain side Edge forms the heavy rare earth shell layer of high magnetocrystalline anisotropy, obtains intermediate;
(2)By step(1)After the intermediate of preparation is broken, gained powder and the low melting point high potential crystal boundary containing high abundance rare earth Reconstruct alloy MMaM2bMixing, obtains the second mixture, after the second mixture is carried out into magnetic field orientating shaping, be sintered successively, Heat treatment, produces product.
2. the preparation method of the high abundance rare earth Sintered NdFeB magnet of crystal boundary sandwich construction regulation and control according to claim 1, Characterized in that, the MM is the one or more in La, Ce.
3. the preparation method of the high abundance rare earth Sintered NdFeB magnet of crystal boundary sandwich construction regulation and control according to claim 1, Characterized in that, the particle mean size of the low rare-earth Nd-Fe-B main-phase alloy powder A1 is less than 5 μm, rare earth element content is less than 29 Wt.%, Nd2Fe14B phases proportion is more than 95 %.
4. the preparation method of the high abundance rare earth Sintered NdFeB magnet of crystal boundary sandwich construction regulation and control according to claim 1, Characterized in that, the neodymium iron boron main-phase alloy powder A2 of the MM of rare earth containing high abundance particle mean size is less than 5 μm, Gao Feng therein Degree rare earth MM accounts for 3 more than wt.% of main-phase alloy powder A2 gross masses.
5. the system of the high abundance rare earth Sintered NdFeB magnet regulated and controled according to any one of the claim 1-4 crystal boundary sandwich constructions Preparation Method, it is characterised in that the low melting point heavy rare earth crystal boundary reconstruct alloyed powder R1xM1yIn, R1 be lanthanide series metal Gd, Tb, Dy, One or more in Ho, the one or more in M1 O, F, H, Cu, Ni, Fe, Co, Sn, Ti, Nb, Zr, x, y be respectively R1, M1 atomic percentage, x scope are 5 ~ 80, x and y's and be 100.
6. the preparation method of the high abundance rare earth Sintered NdFeB magnet of crystal boundary sandwich construction regulation and control according to claim 5, Characterized in that, the low melting point heavy rare earth crystal boundary reconstruct alloyed powder R1xM1yFusing point be less than 900 DEG C.
7. the high abundance rare earth Sintered NdFeB magnet regulated and controled according to any one of claim 1-4,6 the crystal boundary sandwich construction Preparation method, it is characterised in that the low melting point high potential crystal boundary reconstruct alloy MMaM2bIn, MM is in lanthanide series metal La, Ce One or two, M2 are the one or more in high standard noble potential metal Cu, Ni, Fe, Co, and a, b are respectively MM and M2 atom Percentage, a scope are 5 ~ 80, a and b's and be 100.
8. the preparation method of the high abundance rare earth Sintered NdFeB magnet of crystal boundary sandwich construction regulation and control according to claim 5, Characterized in that, the low melting point high potential crystal boundary reconstruct alloy MMaM2bIn, MM is one kind or two in lanthanide series metal La, Ce Kind, M2 is the one or more in high standard noble potential metal Cu, Ni, Fe, Co, and a, b are respectively MM and M2 atomic percentage, a Scope be 5 ~ 80, a and b's and be 100.
9. the preparation method of the high abundance rare earth Sintered NdFeB magnet of crystal boundary sandwich construction regulation and control according to claim 1, Characterized in that, the low melting point heavy rare earth crystal boundary reconstruct alloyed powder R1xM1y, low melting point high potential crystal boundary reconstruct alloyed powder MMaM2bGranularity be 0.1-100 μm.
10. the high abundance rare earth sintered NdFeB magnetic regulated and controled according to any one of claim 1-4,6,9 the crystal boundary sandwich construction The preparation method of body, it is characterised in that the step(2)In, after the second mixture is carried out into magnetic field orientating shaping, burnt Knot, sintering temperature are 950-1100 DEG C, sintering time 2-5h, then carry out two-stage heat treatment, one-level heat treatment temperature is 850-950 DEG C, soaking time 1-5h, two level heat treatment temperature is 300-600 DEG C, soaking time 1-5h, produces product.
11. the preparation method of the high abundance rare earth Sintered NdFeB magnet of crystal boundary sandwich construction regulation and control according to claim 5, Characterized in that, the step(2)In, after the second mixture is carried out into magnetic field orientating shaping, it is sintered, sintering temperature is 950-1100 DEG C, sintering time 2-5h, two-stage heat treatment is then carried out, one-level heat treatment temperature is 850-950 DEG C, during insulation Between be 1-5h, two level heat treatment temperature is 300-600 DEG C, soaking time 1-5h, produces product.
12. the product prepared using any one of preceding claims 1-11 methods described.
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