CN106910585B - A kind of Nd-Fe-B permanent magnet material and preparation method thereof and motor - Google Patents

A kind of Nd-Fe-B permanent magnet material and preparation method thereof and motor Download PDF

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CN106910585B
CN106910585B CN201510974491.4A CN201510974491A CN106910585B CN 106910585 B CN106910585 B CN 106910585B CN 201510974491 A CN201510974491 A CN 201510974491A CN 106910585 B CN106910585 B CN 106910585B
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邓小霞
陈波
吴波
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比亚迪股份有限公司
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Abstract

The present invention provides a kind of Nd-Fe-B permanent magnet materials, and containing neodymium iron boron bulk alloy and additive, the additive contains Rare-Earth Cobalt intermetallic compound, nitride and carbide.The present invention also provides a kind of method for preparing Nd-Fe-B permanent magnet material, this method includes the following steps: that (1) mixes neodymium iron boron bulk alloy with additive, and compression moulding under the conditions of magnetic field orientating obtains blank;The additive contains Rare-Earth Cobalt intermetallic compound, nitride and carbide;(2) blank is sintered and is tempered under vacuum or inert gas shielding.The present invention also provides the motor including Nd-Fe-B permanent magnet material as described above, which includes Nd-Fe-B permanent magnet material as described above.Through the above technical solutions, the present invention can be in the case where keeping remanent magnetism and magnetic energy product to be basically unchanged, enabling Nd-Fe-B permanent magnet material not only has improved mechanical property but also has the room temperature coercivity and high-temperature magnetic of raising.

Description

A kind of Nd-Fe-B permanent magnet material and preparation method thereof and motor

Technical field

The present invention relates to field of material technology, and in particular, to a kind of Nd-Fe-B permanent magnet material a kind of prepares neodymium iron boron forever The Nd-Fe-B permanent magnet material and a kind of motor that method, this method of magnetic material are prepared.

Background technique

Nd-Fe-B permanent magnet material has obtained rapidly because of its lower cost and excellent magnetic property since being born from nineteen eighty-three Development, application popularization to the fields such as space flight navigation, the energy, health care, computer, communication and auto industry.High-performance Nd-Fe-B permanent magnet material can be used as manufacture new-energy automobile power motor and specific type of electric machine rotor/stator main material Material.Since Nd-Fe-B permanent magnet material has the advantages that small in size, magnetic property is high, so using the motor phase of Nd-Fe-B permanent magnet material 1/2 can be reduced for ferrite permanent-magnet motor volume, weight reduces 60%, and power can improve 40%.Therefore, neodymium iron boron is forever Magnetic material have become the universal of equipment such as indispensable magnetic material, especially computer, communication in people's daily life and The high speed development of automobile motor keeps its application prospect more wide.

Nd-Fe-B permanent magnet material is with Nd2Fe14B intermetallic compound is the alloy of matrix, and intermetallic compound generally has There is the features such as crystal structure is complicated, and slip system is few, thus causes its toughness plasticity poor.The brittleness of this material leads to mechanical add Work difficulty often occurs peeling off in the production and use process, falls the problems such as corner, cracking, and it is required in anti-knock shock resistance The application that high field is closed is restricted.

The Curie temperature of Nd-Fe-B permanent magnet material is low, and the big disadvantage of temperature coefficient also seriously limits it under high temperature applicationss Application.The method for improving the high-temperature behavior of Nd-Fe-B permanent magnet material is mainly realized by improving coercivity, specifically, is led to The Curie temperature and coercivity of Sintered NdFeB magnet can be improved by crossing compound addition Co, Cu, Al, thus improve the thermostabilization of magnet Property, but the above-mentioned element of addition can all lead to the decline of magnet remanence and magnetic energy product.

As the application range of Nd-Fe-B permanent magnet material increasingly increases, comprehensive performance, such as agnetic property at room temperature m, thermostabilization The requirement of property, mechanical property etc. is higher and higher.The thermal stability of Nd-Fe-B permanent magnet material and intergranular microscopic structure are closely related, brilliant Boundary's rich-Nd phase is the key that Nd-Fe-B permanent magnet material obtains high-coercive force.However rich-Nd phase itself is mechanics reduction phase, is magnet Weakest link, therefore Nd-Fe-B permanent magnet material be easy from crystal boundary rich-Nd phase be broken, this is Sintered NdFeB magnet The main reason for brittle fracture.So improving the intensity of crystal boundary and toughness should be improves Sintered NdFeB magnet mechanical property Basic skills.

A large number of studies show that alloying element is added in Nd-Fe-B permanent magnet material by single alloyage, it can be further Improve coercivity and mechanical strength.The main reason is that this dvielement forms some cenotypes in intergranular and improves border structure.But It is that single alloyage addition alloying element is often added before molten alloy, alloying element not only enters intergranular, also enters main phase.Cause And coercivity is improved also along with the reduction of remanent magnetism and magnetic energy product.In order to be effectively improved the comprehensive performance of Nd-Fe-B permanent magnet material, It is extremely important to control reasonable layout of the alloying element in magnet.It is found by numerous studies, dual alloy method can be targetedly The characteristic for controlling Grain-Boundary Phase, makes border structure be significantly improved.In dual alloy method, according to a certain ratio with Grain-Boundary Phase by main phase Sintering, the compound addition of crystal boundary can improve crystal boundary structure and structure especially crystal edge region.Thus both guarantee Nd2Fe14B There is rich-Nd phase isolation around crystal grain, and reduces precipitation of the rich-Nd phase in main phase and the reunion at crystal boundary friendship corner, thus magnet Existing higher coercivity and thermal stability, and mechanical property with higher.But existing neodymium-iron-boron magnetic material also needs In the case where remanent magnetism and magnetic energy product remain unchanged, coercivity, thermal stability and mechanical property are further improved simultaneously.

For example, patent document CN201110161367.8 is disclosed, a kind of rare-earth fluoride nano particle doping preparation is high to be rectified The preparation method of stupid power neodymium iron boron magnetic body.Entered in female powder using rare-earth fluoride nano powder particle is added in micro mist, and it is same The single alloy of sample ingredient is improved compared to performance, but coercivity increase rate appoints so deficiency.In another example patent document CN201210266800.9 discloses a kind of nanometer of toughening neodymium-iron-boron magnetic material and preparation method, it is mentioned that in neodymium iron boron crystalline substance Nano-complex Grain-Boundary Phase is formed in boundary, is realized and is utilized SH grades of rare earth permanent-magnetic materials of M, H grades of preparations without heavy rare earth doping, it is therein Nanometer additive includes the alloy of Al, Cu, Cr, Fe, Zn, Nb, Co, Ga composition;During the sintering process, nano powder is formed with main phase Crystal boundary, is greatly improved coercivity, while the machining property of product is also improved, but the Neodymium iron boron magnetic material Expect that mechanical property is still to be improved.

Summary of the invention

In order to further improve the coercive of Nd-Fe-B permanent magnet material simultaneously in the case where remanent magnetism and magnetic energy product remain unchanged Power, thermal stability and mechanical property, the present invention provides a kind of Nd-Fe-B permanent magnet materials, a kind of Nd-Fe-B permanent magnet material for preparing The Nd-Fe-B permanent magnet material and a kind of motor that method, this method are prepared.

It was found by the inventors of the present invention that preparing Nd-Fe-B permanent magnet material using specific additive, neodymium iron boron can be made The border structure and tissue of permanent-magnet material have all obtained apparent improvement, to make Nd-Fe-B permanent magnet material in remanent magnetism and magnetic energy product In the case where remaining unchanged, not only there is good coercivity and high-temperature behavior, but also there is the mechanical property improved, result in The present invention.

On the one hand, the present invention provides a kind of Nd-Fe-B permanent magnet material, which contains neodymium iron boron main body Alloy and additive, wherein the additive contains Rare-Earth Cobalt intermetallic compound, nitride and carbide;Relative to 100 weights The neodymium iron boron bulk alloy of part is measured, the content of the Rare-Earth Cobalt intermetallic compound is 0.005-5 parts by weight, the nitridation The content of object is 0.005-3 parts by weight, and the content of the carbide is 0.005-2 parts by weight.

On the other hand, the present invention also provides a kind of methods for preparing Nd-Fe-B permanent magnet material, wherein under this method includes It states step: (1) mixing neodymium iron boron bulk alloy with additive, compression moulding under the conditions of magnetic field orientating obtains blank;It is described Additive contains Rare-Earth Cobalt intermetallic compound, nitride and carbide;(2) by the blank in vacuum or inert gas shielding Under be sintered and be tempered;Wherein, relative to the neodymium iron boron bulk alloy of 100 parts by weight, change between the Rare-Earth Cobalt metal The dosage for closing object is 0.005-5 parts by weight, and the dosage of the nitride is 0.005-3 parts by weight, and the dosage of the carbide is 0.005-2 parts by weight.

On the other hand, the present invention also provides the Nd-Fe-B permanent magnet materials being prepared according to method as described above.

In another aspect, the present invention also provides a kind of motors, wherein the motor includes Nd-Fe-B permanent magnetic material as described above Material.

Through the above technical solutions, the present invention can keep remanent magnetism (Br) and magnetic energy product (BH)maxThe case where being basically unchanged Under, enabling Nd-Fe-B permanent magnet material not only has improved mechanical property but also has the room temperature coercivity and high-temperature magnetic of raising.

Specific embodiment

Detailed description of the preferred embodiments below.It should be understood that described herein specific Embodiment is merely to illustrate and explain the present invention, and is not intended to restrict the invention.

On the one hand, the present invention provides a kind of Nd-Fe-B permanent magnet material, which contains neodymium iron boron main body Alloy and additive, wherein the additive contains Rare-Earth Cobalt intermetallic compound, nitride and carbide;Relative to 100 weights The neodymium iron boron bulk alloy of part is measured, the content of the Rare-Earth Cobalt intermetallic compound is 0.005-5 parts by weight, the nitridation The content of object is 0.005-3 parts by weight, and the content of the carbide is 0.005-2 parts by weight.

Wherein, Rare-Earth Cobalt intermetallic compound is mainly distributed on grain boundary, so that the crystallization magnetic on main phase grain surface is each Anisotropy increases, and the generation of anti-magnetic domain is suppressed, and the coercivity of entire magnet all effectively improves, and improves magnet High-temperature magnetic energy.

Wherein, addition nitride can replenish stomata present in preparation process into sintered Nd-Fe-B permanent magnetic material and lack It falls into, increases the compactness and continuity of magnet.To improve the mechanical property of magnet.For fragile material, the particle energy of addition The extension and propagation for inhibiting crackle, are equivalent to strengthening and toughening, this is similar to particle humidification in composite material.The nitride At grain boundary, improve the uniformity of crystal boundary, refine crystal grain, pinning crystal boundary inhibits magnetic reversal farmland to generate, can significantly improve The mechanical property and coercivity and high-temperature magnetic energy of neodymium iron boron magnetic body.

Wherein, nano-carbide can make insensitive to the influence of sintering temperature in Growing Process of Crystal Particles, pass through phase After the sintering of long period, the magnetic property difference of the Nd-Fe-B permanent magnet material of different sintered locations can be made to reduce, it is brilliant in magnet The distribution of boundary's phase is more uniform, to substantially eliminate the phenomenon that main phase grain directly contacts, makes irregularly growing up for crystal grain Inhibited, so that main phase grain be hindered to grow up, prevent the forming core on magnetic reversal farmland and grow up, while being reduced between main phase grain It directly contacts, reduces the exchange-coupling interaction between main phase grain, to effectively improve the mechanical property of Nd-Fe-B permanent magnet material Energy and magnetic property.

Additive containing Rare-Earth Cobalt intermetallic compound, nitride and carbide of the invention can make Neodymium iron boron magnetic The distribution of the Grain-Boundary Phase of material is more uniform, pinning crystal boundary, inhibits irregularly growing up for crystal grain, direct between reduction main phase grain Exchange-coupling interaction between contact and main phase grain, increases the compactness and continuity of magnet;Thus make sintered NdFeB magnetic Material obtains the mechanical property and improved magnetism for having both raising.

Wherein, in order in the case where remanent magnetism and magnetic energy product remain unchanged, Nd-Fe-B permanent magnet material is further improved simultaneously Coercivity, thermal stability and mechanical property, it is preferable that it is described dilute relative to the neodymium iron boron bulk alloy of 100 parts by weight The content of native cobalt intermetallic compound is 0.01-2.5 parts by weight, and the content of the nitride is 0.01-1.6 parts by weight, described The content of carbide is 0.01-1 parts by weight.

Wherein, particularly preferred a kind of embodiment according to the present invention, the neodymium iron boron main body relative to 100 parts by weight Alloy, the content of the Rare-Earth Cobalt intermetallic compound are 1.5-2 parts by weight, and the content of the nitride is 0.8-1.5 weight Part, the content of the carbide is 0.5-0.8 parts by weight.In the case where the preferred embodiment, neodymium iron boron of the invention is forever Magnetic material has both very excellent magnetic property and mechanical property.

Wherein, in order in the case where remanent magnetism and magnetic energy product remain unchanged, Nd-Fe-B permanent magnet material is further improved simultaneously Coercivity, thermal stability and mechanical property, it is preferable that the average grain diameter of the Rare-Earth Cobalt intermetallic compound be 0.5-6 μm, Further preferably 1-3 μm;The average grain diameter of the nitride is 5-40nm, further preferably 10-30nm;The carbide Average grain diameter be 10-100nm, further preferably 30-80nm.In the preferred embodiment, it is preferred that average grain diameter model Enclosing can make the degree of oxidation of the Rare-Earth Cobalt intermetallic compound and cost are effectively reduced, and facilitate described The coercivity of Rare-Earth Cobalt intermetallic compound improvement Nd-Fe-B permanent magnet material;Preferred average particle size range can make the nitrogen Compound, which is more advantageous to, replenishes stomata present in matrix and defect;Preferred average particle size range can make the carbide more Be conducive to the intergranular structure of the mechanical property for improving Nd-Fe-B permanent magnet material and magnetic property.

Wherein, the Rare-Earth Cobalt intermetallic compound refers to the chemical combination formed between thulium and cobalt metal element Object can be RCo5Rare-Earth Cobalt intermetallic compound, R2Co17Rare-Earth Cobalt intermetallic compound and RCo7Rare-Earth Cobalt intermetallic At least one of object.Wherein, the nitride refers to the compound that nitrogen is formed with other elements of-trivalent and non-hydrogen, can To be selected from metal nitride and/or non-metal nitride;The carbide refers to carbon with other elements of negative valency and non-hydrogen The compound of formation can be selected from metal carbides and/or non-metallic carbide.

Wherein, R is rare earth element, can be selected from La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Y At least one of with Sc.The particularly preferred Rare-Earth Cobalt intermetallic compound is selected from GdCo5、YCo5And SmCo5In at least one Kind.Wherein, GdCo5Compound has very high anisotropy, YCo5Also there is high magnetocrystalline anisotropy constant (k1=5.7 ×106J/m3) and quite high saturation magnetization (u0Ms=1.06T), SmCo5It is high, full with good temp characteristic, Curie temperature With the intensity of magnetization it is big, with temperature and environmental change stability be good and good reliability the characteristics of, coercivity H can achieve 1194- 3184kA/m(15-40kOe);It is particularly conducive to improve the comprehensive performance of Nd-Fe-B permanent magnet material.

Wherein, the nitride can be selected from AlN3、TiBN、Mg2N3、Ga3N2, in ZrN, GeN, SiBN, VN, BN and TiN At least one;It is particularly advantageous since these nitride of TiBN, SiBN and ZrN also do not decompose at a high temperature of 3000 degrees Celsius In improve Nd-Fe-B permanent magnet material comprehensive performance, it is preferred that the nitride in TiBN, SiBN and ZrN one Kind.

The carbide can be selected from TaC, NbC, V2C5, CrC, WC, TiC, NiC, HfC, SiC, BC and Al2C3In extremely Few one kind.Due to NbC, NiC and Cr2C3These carbide also do not decompose at a high temperature of 3000 degrees Celsius, are particularly conducive to improve The comprehensive performance of Nd-Fe-B permanent magnet material, it is preferred that the carbide is selected from NbC, NiC and Cr2C3One of.

Wherein, the additive can be dispersed in the neodymium iron boron bulk alloy.Wherein, the neodymium iron boron main body Alloy can be that can be used in preparing the various neodymium iron boron bulk alloys of Nd-Fe-B permanent magnet material, such as can have formula (1) institute The composition shown:

Ra(Fe1-xCox)100-a-b-cMcBbFormula (1)

Wherein, a, b, c and x respectively indicate weight percent, 26≤a≤35;0.9≤b≤1.3;0≤c≤1.5;0≤x ≤10;R is selected from least one of Pr, Nd, La, Ce, Gd, Dy, Tb and Ho;M be selected from Al, Cu, Ti, V, Cr, Zr, Hf, Mn, At least one of Nb, Sn, Mo, Ga and Si.

On the other hand, the present invention also provides a kind of methods for preparing Nd-Fe-B permanent magnet material, wherein under this method includes It states step: (1) mixing neodymium iron boron bulk alloy with additive, compression moulding under the conditions of magnetic field orientating obtains blank;It is described Additive contains Rare-Earth Cobalt intermetallic compound, nitride and carbide;(2) by the blank in vacuum or inert gas shielding Under be sintered and be tempered;Wherein, relative to the neodymium iron boron bulk alloy of 100 parts by weight, change between the Rare-Earth Cobalt metal The dosage for closing object is 0.005-5 parts by weight, and the dosage of the nitride is 0.005-3 parts by weight, and the dosage of the carbide is 0.005-2 parts by weight.

Wherein, mode neodymium iron boron bulk alloy mixed with additive can be known to those skilled in the art, can Uniformly to be mixed in batch mixer.In the preferred case, can also add when neodymium iron boron bulk alloy powder is mixed with additive Add lubricant.The lubricant is conventional lubricants, type, dosage and the usage of lubricant by those skilled in the art public affairs Know, be not particularly limited, such as: can be used oleic acid, stearic acid and their salt, polyalcohol, polyethylene glycol, sorbierite and Mixture of anhydro sorbitol and glyceryl stearate etc. is used as lubricant;The neodymium iron boron bulk alloy of opposite 100 parts by weight, institute The dosage for stating lubricant can be 0.03-0.15 parts by weight.

Wherein, in order in the case where remanent magnetism and magnetic energy product remain unchanged, Nd-Fe-B permanent magnet material is further improved simultaneously Coercivity, thermal stability and mechanical property, it is preferable that it is described dilute relative to the neodymium iron boron bulk alloy of 100 parts by weight The dosage of native cobalt intermetallic compound is 0.01-2.5 parts by weight, and the dosage of the nitride is 0.01-1.6 parts by weight, described The dosage of carbide is 0.01-1 parts by weight.

Wherein, particularly preferred a kind of embodiment according to the present invention, the neodymium iron boron main body relative to 100 parts by weight Alloy, the dosage of the Rare-Earth Cobalt intermetallic compound are 1.5-2 parts by weight, and the dosage of the nitride is 0.8-1.5 weight Part, the dosage of the carbide is 0.5-0.8 parts by weight.In the case where the preferred embodiment, neodymium iron boron of the invention is forever Magnetic material has both very excellent magnetic property and mechanical property.

Wherein, in order in the case where remanent magnetism and magnetic energy product remain unchanged, Nd-Fe-B permanent magnet material is further improved simultaneously Coercivity, thermal stability and mechanical property, it is preferable that the average grain diameter of the Rare-Earth Cobalt intermetallic compound be 0.5-6 μm, Further preferably 1-3 μm;The average grain diameter of the nitride is 5-40nm, further preferably 10-30nm;The carbide Average grain diameter be 10-100nm, further preferably 30-80nm.

Wherein, the Rare-Earth Cobalt intermetallic compound refers to the chemical combination formed between thulium and cobalt metal element Object can be RCo5Rare-Earth Cobalt intermetallic compound, R2Co17Rare-Earth Cobalt intermetallic compound and RCo7Rare-Earth Cobalt intermetallic At least one of object;The nitride is selected from metal nitride and/or non-metal nitride;The carbide is selected from metal carbon Compound and/or non-metallic carbide.

Wherein, R is rare earth element, can be selected from La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Y At least one of with Sc.The particularly preferred Rare-Earth Cobalt intermetallic compound is selected from GdCo5、YCo5And SmCo5In at least one Kind.

Wherein, the nitride can be selected from AlN3、TiBN、Mg2N3、Ga3N2, in ZrN, GeN, SiBN, VN, BN and TiN At least one;Preferably, the nitride is selected from one of TiBN, SiBN and ZrN.

Wherein, the carbide can be selected from TaC, NbC, V2C5, CrC, WC, TiC, NiC, HfC, SiC, BC and Al2C3In At least one.Preferably, the carbide is selected from NbC, NiC and Cr2C3One of.

Wherein, the additive can be dispersed in the neodymium iron boron bulk alloy.Wherein, the neodymium iron boron main body Alloy can be that can be used in preparing the various neodymium iron boron bulk alloys of Nd-Fe-B permanent magnet material, such as can have formula (1) institute The composition shown:

Ra(Fe1-xCox)100-a-b-cMcBbFormula (1)

Wherein, a, b, c and x respectively indicate weight percent, 26≤a≤35;0.9≤b≤1.3;0≤c≤1.5;0≤x ≤ 10, surplus is Fe and impurity;R is selected from least one of Pr, Nd, La, Ce, Gd, Dy, Tb and Ho;M be selected from Al, Cu, Ti, V, at least one of Cr, Zr, Hf, Mn, Nb, Sn, Mo, Ga and Si.

Wherein, the condition of the magnetic field orientating can be conventional use of condition in Nd-Fe-B permanent magnet material, such as can be with It include: magnetic induction intensity can be 1-3T, preferably 1.5-2.8T;The condition of compression moulding may include: that pressure can be 140-250MPa is preferably 150-220MPa, and it is preferably 60-180s that the pressing time, which can be 50-200s,.The present invention is excellent Choosing uses higher alignment magnetic field, is more preferably orientated consistent magnet convenient for being made, and is conducive to improve coercivity.

Wherein, the condition of sintering may include: that sintering temperature can be for 1000-1250 DEG C, and preferably 1020-1100 DEG C, Sintering time can be 1.5-7.5 hours, preferably 2-7 hours;The condition of tempering may include: in 880 DEG C of -920 DEG C of progress Level-one tempering, and 2-5h is kept, then in 460 DEG C of -550 DEG C of progress second annealings, and keep 2-5h.Wherein, it is tempered by two-stage Processing is conducive to Nd-Fe-B permanent magnet material and obtains good microstructure.

Wherein it is possible to which blank is placed in sintering furnace, it is sintered under conditions of vacuum or inert gas shielding.The burning Cavity is equipped in freezing of a furnace, the cricoid molybdenum filament of cavity inner wall at certain intervals is surround, and energization makes molybdenum filament generate heat, then with heat radiation Form be applied on blank, blank is heated, the blank, that is, die mould block, shape is with required Nd-Fe-B permanent magnet Processing external form be reference, it is general be square;The inert gas can be any gas for being not involved in reaction, preferably zero One or more of race's elemental gas.

The neodymium iron boron bulk alloy can be neodymium iron boron bulk alloy ingot casting or neodymium iron boron rapid hardening thin slice, can pass through quotient Industry purchase, can also make by oneself, and manufacturing process is neodymium iron boron bulk alloy to be carried out melting by component, and be made of casting technique Neodymium iron boron bulk alloy ingot casting, or neodymium iron boron bulk alloy rapid hardening thin slice is made using rapid setting sheet process.

Wherein, the method that ingot casting is made in the casting technique can be the various methods being able to use, such as can will melt Alloy molten solution after refining is cast in water-cooled copper mold, obtains ingot casting after cooling.Preferably, before cooling, to the neodymium of melting Iron boron bulk alloy under inert gas protection, 1040 DEG C -1090 DEG C at a temperature of carry out 6h-12h homogenization heat treatment, And coarse crushing is carried out, because, if cooling velocity is not fast enough, will lead to the precipitation of α-Fe under existing cooling condition, and lead to It crosses using heat treatment, making α-Fe, the long period keeps at a higher temperature, reacts, further generates dilute with boron, rare earth Unmanufactured iron boron phase, to eliminate α-Fe;And coarse crushing is then played the role of accelerating cooling velocity.

Wherein, the method that rapid hardening thin slice is made in the rapid setting sheet process can be the various methods being able to use, such as Alloy molten solution after melting can be poured onto the copper roller surface of rotation, water flowing is cooling on the inside of copper roller, copper roller surface linear velocity 1-2.5m/s or so, alloy molten solution form rapid hardening thin slice after cooling down rapidly.

Wherein, this method can also include: to be crushed ingot casting shape and/or the laminar neodymium iron boron bulk alloy of rapid hardening With powder processed, the neodymium iron boron bulk alloy of powdery is obtained, then can be mixed the neodymium iron boron bulk alloy of powdery with the additive It closes.

Wherein, the broken method can be for the quick-fried method of hydrogen or by being crushed crusher machine, and the condition of the quick-fried method of hydrogen can To include: the hydrogen pressure in 0.5-2.2Mpa, inhaling hydrogen 1-5h (can hear the cracker of neodymium iron boron cast ingot or rapid hardening thin slice, together When can detecte the temperature of container and constantly increasing, this be neodymium iron boron cast ingot or rapid hardening thin slice inhale hydrogen after form hydride and quick-fried Split), then 500-600 DEG C at a temperature of, dehydrogenase 35-10h.

Wherein, the method for being crushed rare earth permanent-magnetic material ingot casting or rapid hardening thin slice by crusher can be various The method being able to use carries out coarse crushing for example, by using jaw crusher, then by being crushed in the progress of middle crusher.

Wherein, the maneuver of powder processed can be the various methods being able to use, such as may include: by broken neodymium iron Boron bulk alloy is mixed with antioxidant, is then milled into the fine powder that average grain diameter can be 2.5-4.5 μm by air-flow;Phase For the broken neodymium iron boron bulk alloy of 100 parts by weight, the additive amount of the antioxidant can be 0.03-1.5 weight Part.The type and usage of antioxidant are known to those skilled in the art, such as: can selected from polyethylene oxide alkyl ethers, One or more of polyethylene oxide list fatty ester, polyethylene oxide alkylene ether.

On the other hand, the present invention also provides the Nd-Fe-B permanent magnet materials being prepared according to method as described above.

In another aspect, the present invention also provides a kind of motors, wherein the motor includes Nd-Fe-B permanent magnetic material as described above Material.The structure of motor of the invention can be various permanent magnet motor structures, which is characterized in that the permanent magnetism material in motor of the invention Material includes Nd-Fe-B permanent magnet material as described above.

Preparation method of the invention is described further below by embodiment.

Embodiment

NdFeB material is prepared in accordance with the following steps:

According to component melting neodymium iron boron bulk alloy shown in table 1, neodymium iron boron master is then made using rapid casting technique The laminar neodymium iron boron bulk alloy of rapid hardening, is then carried out that hydrogen is broken and airflow milling powder by body alloy rapid hardening thin slice, actual conditions Referring to table 2.Then the neodymium iron boron bulk alloy of powdery is mixed with additive, compression moulding under the conditions of magnetic field orientating obtains Then the blank is sintered and is tempered under vacuum or inert gas shielding, obtains Nd-Fe-B permanent magnet material by blank, tool Concrete conditions in the establishment of a specific crime is referring to table 3 and table 4.

Using China National Measuring Science Research Inst. permanent-magnet material magnetic property measuring system NIM10000H and NIM200C to The Nd-Fe-B permanent magnet material C1 arrived carries out remanent magnetism, magnetic energy product and the coercitive measurement of normal high temperature.Group's public affairs are newly thought carefully using Shenzhen The universal testing machine CMT5105 of department carries out Mechanics Performance Testing to above-mentioned Nd-Fe-B permanent magnet material.Measurement result As shown in table 4.

Table 1

Alloy Composition
Alloy 1 Pr8Nd19.5Dy4.5Fe60.9Co5B1.2Al0.5Cu0.2Ga0.2
Alloy 2 Nd17.5La2Ho7Fe62.2Co10B1.3
Alloy 3 Nd20Ce2Ho4Fe61.8Co9.8B0.9Hf0.4Ti0.5Cu0.6
Alloy 4 Pr26Gd4Dy5Fe62.56Co0.5B0.94V0.2Sn0.3Si0.2Zr0.3
Alloy 5 Nd28.8La2Tb3.7Fe63.8Co0B1.3Nb0.1Si0.1Al0.2
Alloy 6 Pr20Ce2Ho5Fe61.38Co9.5B0.92Cr0.3Al0.7Mn0.2
Alloy 7 Pr24.7Gd4Ho5.3Fe63.31Co0.8B1.29Mo0.2Sn0.4

Table 2

Table 3

Table 4

In table 2-4, embodiment 1-16 represents Nd-Fe-B permanent magnet material of the invention, and D1-D28 represents the neodymium iron for comparison B permanent magnetic material;In table 2, the parts by weight of the dosage of antioxidant are that the neodymium iron boron bulk alloy of opposite 100 parts by weight calculates; In table 2, the ingot casting in embodiment 8, which refers to, is made neodymium iron boron bulk alloy ingot casting using casting technique, then, protects in inert gas Under shield, 1050 DEG C at a temperature of carry out the homogenization heat treatment of 6h, and carry out coarse crushing;In table 4, Rare-Earth Cobalt intermetallic Dosage part of object, nitride and carbide is the value for the parts by weight that the neodymium iron boron bulk alloy of opposite 100 parts by weight calculates;Table 4 In, the partial size of Rare-Earth Cobalt intermetallic compound refers to that average grain diameter, unit are micron;The partial size of nitride and carbide refers to flat Equal partial size, unit are nanometer;In table 4, "-" expression is not added, and Br refers to remanent magnetism, unit kGs;HcjRefer to coercivity, unit For kOe;BH is (BH)maxAbbreviation, refer to magnetic energy product, unit MGsOe;Hcj* refer to the high temperature coercivity at 180 DEG C, unit For kOe;σfRefer to bending strength, unit MPa.

It can be seen that Nd-Fe-B permanent magnet material of the invention according to the data in table 4, relative to not adding Rare-Earth Cobalt metal Between one of compound, nitride and carbide or a variety of technical solutions, Nd-Fe-B permanent magnet material can be made in remanent magnetism (Br) and magnetic energy product (BH)maxCoercivity (H with higher in the case where being held essentially constantcj) also, high temperature coercivity obtain Very big improvement, bending strength are also greatly improved.Also, in the neodymium iron boron main body preferably with respect to 100 parts by weight Alloy, the content of the Rare-Earth Cobalt intermetallic compound are 1.5-2 parts by weight, and the content of the nitride is 0.8-1.5 weight Part, in the case that the content of the carbide is 0.5-0.8 parts by weight, the synthesis of Nd-Fe-B permanent magnet material can be further increased Performance.

The preferred embodiment of the present invention has been described above in detail, still, during present invention is not limited to the embodiments described above Detail within the scope of the technical concept of the present invention can be with various simple variants of the technical solution of the present invention are made, this A little simple variants all belong to the scope of protection of the present invention.

It is further to note that specific technical features described in the above specific embodiments, in not lance In the case where shield, can be combined in any appropriate way, in order to avoid unnecessary repetition, the present invention to it is various can No further explanation will be given for the combination of energy.

In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally The thought of invention, it should also be regarded as the disclosure of the present invention.

Claims (23)

1. a kind of Nd-Fe-B permanent magnet material, which contains neodymium iron boron bulk alloy and additive, and feature exists In the additive contains Rare-Earth Cobalt intermetallic compound, nitride and carbide;The neodymium iron relative to 100 parts by weight The content of boron bulk alloy, the Rare-Earth Cobalt intermetallic compound is 0.005-5 parts by weight, and the content of the nitride is 0.005-3 parts by weight, the content of the carbide are 0.005-2 parts by weight.
2. Nd-Fe-B permanent magnet material according to claim 1, wherein the neodymium iron boron main body relative to 100 parts by weight Alloy, the content of the Rare-Earth Cobalt intermetallic compound are 0.01-2.5 parts by weight, and the content of the nitride is 0.01-1.6 Parts by weight, the content of the carbide are 0.01-1 parts by weight.
3. Nd-Fe-B permanent magnet material according to claim 2, wherein the neodymium iron boron main body relative to 100 parts by weight Alloy, the content of the Rare-Earth Cobalt intermetallic compound are 1.5-2 parts by weight, and the content of the nitride is 0.8-1.5 weight Part, the content of the carbide is 0.5-0.8 parts by weight.
4. Nd-Fe-B permanent magnet material described in any one of -3 according to claim 1, wherein the Rare-Earth Cobalt intermetallic The average grain diameter of object is 0.5-6 μm;The average grain diameter of the nitride is 5-40nm;The average grain diameter of the carbide is 10- 100nm。
5. Nd-Fe-B permanent magnet material according to claim 4, wherein the average grain diameter of the Rare-Earth Cobalt intermetallic compound It is 1-3 μm;The average grain diameter of the nitride is 10-30nm;The average grain diameter of the carbide is 30-80nm.
6. Nd-Fe-B permanent magnet material described in any one of -3 and 5 according to claim 1, wherein between the Rare-Earth Cobalt metal Compound is RCo5Rare-Earth Cobalt intermetallic compound, R2Co17Rare-Earth Cobalt intermetallic compound and RCo7Rare-Earth Cobalt intermetallic compound At least one of;The nitride is selected from metal nitride and/or non-metal nitride;The carbide is selected from metallic carbide Object and/or non-metallic carbide, R is in La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Y and Sc It is at least one.
7. Nd-Fe-B permanent magnet material according to claim 6, wherein the nitride is selected from AlN3、TiBN、Mg2N3、 Ga3N2, at least one of ZrN, GeN, SiBN, VN, BN and TiN;The carbide is selected from TaC, NbC, V2C5、CrC、WC、 TiC, NiC, HfC, SiC, BC and Al2C3At least one of.
8. Nd-Fe-B permanent magnet material described in any one of -3,5 and 7 according to claim 1, wherein the additive is uniform It is scattered in the neodymium iron boron bulk alloy, the neodymium iron boron bulk alloy has to be formed shown in formula (1):
Ra(Fe1-xCox)100-a-b-cMcBbFormula (1)
Wherein, a, b, c and x respectively indicate weight percent, 26≤a≤35;0.9≤b≤1.3;0≤c≤1.5;0≤x≤10; R is selected from least one of Pr, Nd, La, Ce, Gd, Dy, Tb and Ho;M be selected from Al, Cu, Ti, V, Cr, Zr, Hf, Mn, Nb, Sn, At least one of Mo, Ga and Si.
9. a kind of method for preparing Nd-Fe-B permanent magnet material, which is characterized in that this method includes the following steps:
(1) neodymium iron boron bulk alloy is mixed with additive, compression moulding under the conditions of magnetic field orientating obtains blank;It is described to add Agent is added to contain Rare-Earth Cobalt intermetallic compound, nitride and carbide;
(2) blank is sintered and is tempered under vacuum or inert gas shielding;
Wherein, relative to the neodymium iron boron bulk alloy of 100 parts by weight, the dosage of the Rare-Earth Cobalt intermetallic compound is 0.005-5 parts by weight, the dosage of the nitride are 0.005-3 parts by weight, and the dosage of the carbide is 0.005-2 weight Part.
10. described relative to the neodymium iron boron bulk alloy of 100 parts by weight according to the method described in claim 9, wherein The dosage of Rare-Earth Cobalt intermetallic compound is 0.01-2.5 parts by weight, and the dosage of the nitride is 0.01-1.6 parts by weight, institute The dosage for stating carbide is 0.01-1 parts by weight.
11. described relative to the neodymium iron boron bulk alloy of 100 parts by weight according to the method described in claim 10, wherein The dosage of Rare-Earth Cobalt intermetallic compound is 1.5-2 parts by weight, and the dosage of the nitride is 0.8-1.5 parts by weight, the carbon The dosage of compound is 0.5-0.8 parts by weight.
12. the method according to any one of claim 9-11, wherein the Rare-Earth Cobalt intermetallic compound is averaged Partial size is 0.5-6 μm;The average grain diameter of the nitride is 5-40nm;The average grain diameter of the carbide is 10-100nm.
13. according to the method for claim 12, wherein the average grain diameter of the Rare-Earth Cobalt intermetallic compound is 1-3 μm; The average grain diameter of the nitride is 10-30nm;The average grain diameter of the carbide is 30-80nm.
14. the method according to any one of claim 9-11 and 13, wherein the Rare-Earth Cobalt intermetallic compound is RCo5Rare-Earth Cobalt intermetallic compound, R2Co17Rare-Earth Cobalt intermetallic compound and RCo7In Rare-Earth Cobalt intermetallic compound at least It is a kind of;The nitride is selected from metal nitride and/or non-metal nitride;The carbide be selected from metal carbides and/or Non-metallic carbide, R in La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Y and Sc at least one Kind.
15. according to the method for claim 14, wherein the nitride is selected from AlN3、TiBN、Mg2N3、Ga3N2、ZrN、 At least one of GeN, SiBN, VN, BN and TiN;The carbide is selected from TaC, NbC, V2C5、CrC、WC、TiC、NiC、HfC、 SiC, BC and Al2C3At least one of.
16. the method according to any one of claim 9-11,13 and 15, wherein the additive is dispersed in In the neodymium iron boron bulk alloy, the neodymium iron boron bulk alloy has to be formed shown in formula (1):
Ra(Fe1-xCox)100-a-b-cMcBbFormula (1)
Wherein, a, b, c and x respectively indicate weight percent, 26≤a≤35;0.9≤b≤1.3;0≤c≤1.5;0≤x≤10, Surplus is Fe and impurity;R is selected from least one of Pr, Nd, La, Ce, Gd, Dy, Tb and Ho;M be selected from Al, Cu, Ti, V, Cr, At least one of Zr, Hf, Mn, Nb, Sn, Mo, Ga and Si.
17. the method according to any one of claim 9-11,13 and 15, wherein the condition packet of the magnetic field orientating It includes: magnetic induction intensity 1.5-2.8T;The condition of compression moulding includes: that pressure is 150-220MPa, pressing time 60- 180s。
18. the method according to any one of claim 9-11,13 and 15, wherein the condition of sintering includes: sintering temperature Degree is 1020-1100 DEG C, and sintering time is 2-7 hours;The condition of tempering include: in 880 DEG C of -920 DEG C of progress level-one tempering, and 2-5h is kept, then in 460 DEG C of -550 DEG C of progress second annealings, and keeps 2-5h.
19. the method according to any one of claim 9-11,13 and 15, wherein this method further include: by ingot casting shape And/or the laminar neodymium iron boron bulk alloy of rapid hardening carries out powder broken and processed, obtains the neodymium iron boron bulk alloy of powdery, then will The neodymium iron boron bulk alloy of powdery is mixed with the additive.
20. according to the method for claim 19, wherein the broken method is the quick-fried method of hydrogen or is broken by crusher It is broken, the condition of the quick-fried method of hydrogen include: 0.5-2.2Mpa hydrogen depress, inhale hydrogen 1-5h, then 500-600 DEG C at a temperature of, Dehydrogenase 35-10h.
21. according to the method for claim 19, wherein the operation of powder processed includes: by broken neodymium iron boron bulk alloy It is mixed with antioxidant, the fine powder that average grain diameter is 2.5-4.5 μm is then milled by air-flow;Relative to 100 parts by weight Broken neodymium iron boron bulk alloy, the additive amount of the antioxidant is 0.03-1.5 parts by weight.
22. the Nd-Fe-B permanent magnet material that method described in any one of claim 9-21 is prepared.
23. a kind of motor, which is characterized in that the motor include neodymium iron boron described in any one of claim 1-8 and 22 forever Magnetic material.
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CN102299000A (en) * 2010-06-26 2011-12-28 比亚迪股份有限公司 The method of preparing a permanent magnet material and NdFeB
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US5486240A (en) * 1994-04-25 1996-01-23 Iowa State University Research Foundation, Inc. Carbide/nitride grain refined rare earth-iron-boron permanent magnet and method of making
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