CN103258609B - The preparation method of anisotropism nanometer rare earth permanent magnetic material - Google Patents
The preparation method of anisotropism nanometer rare earth permanent magnetic material Download PDFInfo
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Abstract
The invention discloses anisotropism nanometer rare earth permanent magnetic material and preparation method thereof, material is nano double phase structure and formula is RxFe100‑x‑y‑αBα‑θMyPθMaterial, in formula: R is Nd, Pr or Nd Pr alloy, M is one or more in Nb, V, Ta, Zr, Co, Mo, W, and the Hard Magnetic of described material is R mutually2Fe14B and have (00l) texture, soft magnetism is α Fe mutually.Preparation method is A, selects high purity iron, ferro-boron, ferrophosphorus, metal R as raw material, and obtaining alloy cast ingot by sensing or electric arc melting, described metal R selects neodymium, praseodymium or didymium alloy；Under B, vacuum condition, make annealing treatment 15 40 hours when 900 1200 DEG C；After alloy cast ingot after C, annealing crushes, under noble gas, remelting fast quenching obtains strip, pulverizes to obtain material of the present invention again after D, directly pulverizing or subsequent annealing.The material of the present invention has anisotropic character, i.e. soft magnetism is that α Fe, Hard Magnetic are mutually for R mutually2Fe14B and have (00l) texture, preparation method is simply, easily operate.
Description
Technical field
The invention belongs to permanent magnet material technical field, relate to a kind of rare earth permanent-magnetic material and preparation method thereof,
Particularly relate to a kind of anisotropism nanometer rare earth permanent magnetic material and preparation method thereof.
Background technology
In permanent magnet material, Nanocomposite permanent magnetism is by the Hard Magnetic phase of high-coercive force and high saturation and magnetic intensity
Soft magnetism is composited mutually, and both are compound tense in nanometer range, increases owing to exchange-coupling interaction produces remanent magnetism
Potent should so that Nanocomposite permanent magnet material has high theoretical magnetic energy product.Micromagnetics calculates and shows,
The maximum magnetic energy product of anisotropic Nanocomposite permanent magnet can reach 100MGOe, than having " permanent magnetism it
King " the theoretical maximum magnetic energy product of third generation rare earth permanent magnet sintered NdFeB of title exceed by about one time, be
The permanent magnet material that theoretical magnetic energy product known today is the highest.But, the most most researcheres obtain
Nanocomposite permanent magnet material is all isotropic, and its maximum magnetic energy product is generally at below 20MGOe.Cause
This, prepare and have the high-performance nano complex phase rare earth permanent magnetism material of high-performance anisotropic character and become
Realize the key that permanent magnetic material performance is broken through.
At present, the system of the single-phase magnet of anisotropy is mainly still continued to use in the research of anisotropy Nanocomposite permanent magnetism
Preparation Method, these methods mainly have thermal deformation method, dynamic oxidation-disproportionation-dehydrogenation-in conjunction with method (d-HDDR
Method), melt-quenching method etc..Thermal deformation method is to pay close attention to more preparation anisotropy Nanocomposite rare earth at present
A kind of method of permanent magnetism.But, this method is the harshest to technological requirement, and hot pressing is difficult to control to,
Therefore the anisotropy Nanocomposite permanent magnet anisotropisation degree prepared is the most relatively low, to performance
Lifting limited.Typically require super additionally, due to hot compression deformation method prepares anisotropy Nanocomposite permanent magnetism
Hot high pressure press forming device prepares hot compression deformation precast body, requires high to hot-press equipment, the most this
The development potentiality of technique is limited.
Dynamic oxidation-disproportionation-dehydrogenation-in conjunction with technique (d-HDDR method) is a kind of more ripe anisotropy
The preparation method of NdFeB single-phase permanent, but the method that there is no at present uses similar technique to prepare Nanocomposite
Permanent magnetism.
Melt-quenching method technique is relatively easy, the highest to equipment requirements, is current domestic production nano-magnetic powder
Main method.If able to use melt-quenching method to prepare high-performance anisotropy Nanocomposite magnetic
Powder, will produce great pushing effect to the development of permanent magnet material.But, at current alloy system
In the range of, the method that there is no uses melt-quenching method preparation to have the high-performance along direction of easy axis preferred orientation and receives
Rice complex phase rare earth permanent magnetism material.This is because in preparation process, preferable grain orientation process and crystal grain are long
Big process exists the most simultaneously, and while obtaining anisotropic material, the crystal grain within alloy has been sent out
Raw phenomenon of excessively growing up.Therefore, even if having obtained anisotropy alloy, but due to crystallite dimension
Grow up more than 100 the most hundreds of nanometers, that is out soft magnetism phase and the coupling range of Hard Magnetic phase, therefore
Alloy property not only can not get promoting, and there will be on the contrary and declines to a great extent.
Summary of the invention
The technical problem to be solved in the present invention is, can only disposably obtain isotropism for prior art
Permanent magnet material and cannot obtaining has lacking of the Nanocomposite rare earth permanent-magnetic material of high-performance anisotropic character
Fall into, it is provided that it is that α Fe, Hard Magnetic are mutually for R mutually that one has anisotropic character, i.e. soft magnetism simultaneously2Fe14B
And there is the anisotropism nanometer rare earth permanent magnetic material of (00l) texture.
The present invention to solve the technical problem that further and be, it is provided that the operation simple, easy of a kind of technique, energy
Prepare the preparation method of the anisotropism nanometer rare earth permanent magnetic material of anisotropic character.
The technical solution adopted for the present invention to solve the technical problems is: a kind of anisotropy Nanocomposite is dilute
Soil permanent magnet material, is R for nano double phase structure and formulaxFe100-x-y-αBα-θMyPθMaterial, in formula: R
For Nd, Pr or Nd-Pr alloy, M is the one in Nb, V, Ta, Zr, Co, Mo, W or several
Kind, the Hard Magnetic of described anisotropism nanometer rare earth permanent magnetic material is R mutually2Fe14B and there is (00l)
Texture, soft magnetism is α Fe mutually.
The grain size of anisotropism nanometer rare earth permanent magnetic material is 10～90nm.
In described anisotropism nanometer rare earth permanent magnetic material, described x, y, α, θ meet: 7.0≤x≤11.0,
0≤y≤3、5.5≤α≤8.5、0.05≤θ≤0.3。
In described anisotropism nanometer rare earth permanent magnetic material, described x, y, α, θ are the most satisfied:
9.0≤x≤10.0、1≤y≤2、6.0≤α≤7.0、0.1≤θ≤0.2。
The preparation method of the first anisotropism nanometer rare earth permanent magnetic material, comprises the following steps:
A, melting ingot casting: selection high purity iron, ferro-boron, ferrophosphorus, metal R are as raw material, by sensing
Melting or electric arc melting obtain alloy cast ingot, and described metal R selects neodymium, praseodymium or didymium alloy；
B, annealing: under vacuum condition, make annealing treatment 15-40 hour when 900-1200 DEG C；
C, system band: after the alloy cast ingot after step B annealing crushes, under inert gas shielding, remelting
Fast quenching, obtains alloy thin band；
D, post processing: alloy thin band is directly pulverized, or alloy thin band subsequent annealing is pulverized again, obtain respectively
Anisotropy Nanocomposite rare earth permanent-magnetic material.
In the preparation method of the first anisotropism nanometer rare earth permanent magnetic material, described step A former
In material, high purity iron, ferro-boron, ferrophosphorus, the amount of metal R meet RxFe100-x-αBα-θPθ, wherein said x,
α, θ meet: 7.0≤x≤11.0,5.5≤α≤8.5,0.05≤θ≤0.3.
Wherein said x, α, θ are the most satisfied: 9.0≤x≤10.0,6.0≤α≤7.0,0.1≤θ≤0.2.
In the preparation method of the first anisotropism nanometer rare earth permanent magnetic material, in described step A,
Described electric arc melting is: be evacuated to 0.1 × 10-3Pa-2×10-3Pa, recoil noble gas is to reaching 0.2-1
Individual atmospheric pressure, then raw material is carried out electric arc melting.
In the preparation method of the first anisotropism nanometer rare earth permanent magnetic material, in described step A,
Described induction melting is: be evacuated to 0.1 × 10-3Pa-2×10-3Pa, recoil noble gas is to reaching 0.2-1
Individual atmospheric pressure, then raw material is carried out induction melting.
In the preparation method of the first anisotropism nanometer rare earth permanent magnetic material, in described remelting fast quenching,
Copper roller linear velocity is 20m/s to 24m/s.
The preparation method of the second anisotropism nanometer rare earth permanent magnetic material, comprises the following steps:
A, melting ingot casting: high purity iron, ferro-boron, ferrophosphorus, metal R, metal M are as raw material in selection,
Obtaining alloy cast ingot by induction melting or electric arc melting, described metal R selects neodymium, praseodymium or didymium alloy；
Described M metal is one or more in metal Nb, V, Ta, Zr, Co, Mo, W；
B, annealing: under vacuum condition, make annealing treatment 15-40 hour when 900-1200 DEG C；
C, system band: after the alloy cast ingot after step B annealing crushes, under inert gas shielding, remelting
Fast quenching, obtains alloy thin band；
D, post processing: alloy thin band is directly pulverized, or alloy thin band subsequent annealing is pulverized again, obtain respectively
Anisotropy Nanocomposite rare earth permanent-magnetic material；
In the raw material of described step A, the amount of all raw materials meets: RxFe100-x-y-αBα-θMyPθ, Qi Zhongsuo
State x, y, α, θ to meet: 7.0≤x≤11.0,0 ＜ y≤3,5.5≤α≤8.5,0.05≤θ≤0.3.
In the preparation method of the second anisotropism nanometer rare earth permanent magnetic material, described x, y, α, θ
The most satisfied: 9.0≤x≤10.0,1≤y≤2,6.0≤α≤7.0,0.1≤θ≤0.2.
In the preparation method of the second anisotropism nanometer rare earth permanent magnetic material, in described step A,
Described electric arc melting is: be evacuated to 0.1 × 10-3Pa-2×10-3Pa, recoil noble gas is to reaching 0.2-1
Individual atmospheric pressure, then raw material is carried out electric arc melting.
In the preparation method of the second anisotropism nanometer rare earth permanent magnetic material, in described step A,
Described induction melting is: be evacuated to 0.1 × 10-3Pa-2×10-3Pa, recoil noble gas is to reaching 0.2-1
Individual atmospheric pressure, then raw material is carried out induction melting.
In the preparation method of the second anisotropism nanometer rare earth permanent magnetic material, in described remelting fast quenching,
Copper roller linear velocity is 20m/s to 24m/s.
The Nanocomposite rare earth permanent-magnetic material of the present invention, is a kind of novel anisotropy Nanocomposite rare earth
Permanent magnet material, this material has the performance of uniqueness: for nano double phase structure and formula be
RxFe100-x-y-αBα-θMyPθMaterial, in formula: R is Nd, Pr or Nd-Pr alloy, M is Nb, V,
One or more in Ta, Zr, Co, Mo, W, described anisotropism nanometer rare earth permanent magnetic material
Hard Magnetic be R mutually2Fe14B and have (00l) texture, soft magnetism is α Fe mutually.The wherein material of the present invention
In at least while there is neodymium, praseodymium, ferrum, phosphorus, boron element so that the material of the present invention has above-mentioned characteristic,
The particularly existence of P elements, phosphorus is in the Nanocomposite permanent magnet material that the present invention provides indispensable one
Planting element, its role is to regulate and control the organizational structure of Hard Magnetic phase, induction produces (00l) texture, is formed respectively
Anisotropy magnet, makes the comprehensive magnetic of this material to be substantially improved.
In the material of the present invention, it is properly added some refractory metal elements M, these element M main
Effect is energy crystal grain thinning, can improve the magnetic property of material further.
In the method for the present invention, first use the mode of melting, cast alloy, anneal under vacuum the most again,
Then remelting fast quenching under inert gas shielding, obtains the material of the present invention finally by post processing.Above-mentioned
Preparation process can regulate and control the organizational structure of alloy, while making alloy grain be maintained at tens nanometers,
Alloy internal induction generation has the R of (00l) texture characteristic2Fe14B Hard Magnetic phase, and the α-Fe of soft magnetism phase
Exchange-coupling interaction after, material has anisotropy, along direction of easy axis magnetize time, material has height
Remanent magnetism and high-coercive force, can be applicable to prepare high-performance anisotropic bonded magnet.
The present invention is by adding P elements, adding rare earth element, especially after with the addition of P elements, a side
Face is greatly improved the Degree of Preferred Orientation of alloy grain so that (00l) texture is significantly strengthened；Separately
On the one hand in the size of alloy internal grain can be maintained at again tens nanometer range.I.e. it is simultaneously achieved edge
Direction of easy axis preferred orientation also keeps the size of alloy internal grain in tens nanometers so that obtain
Alloy material be anisotropic permanent-magnetic material, its magnetic property has obtained the biggest lifting.
Detailed description of the invention
In order to the technical characteristic of the present invention, purpose and effect are more clearly understood from, existing detailed description
The detailed description of the invention of the present invention.
A kind of anisotropism nanometer rare earth permanent magnetic material, for nano double phase structure and formula be
RxFe100-x-y-αBα-θMyPθMaterial, in formula: R is Nd, Pr or Nd-Pr alloy, M is Nb, V,
One or more in Ta, Zr, Co, Mo, W, the Hard Magnetic of described material is R mutually2Fe14B and having
(00l) texture, soft magnetism is α Fe mutually.Described x, y, α, θ meet: 7.0≤x≤11.0,0≤y≤3,
5.5≤α≤8.5、0.05≤θ≤0.3。
In described anisotropism nanometer rare earth permanent magnetic material, described x, y, α, θ are the most satisfied:
9.0≤x≤10.0、1≤y≤2、6.0≤α≤7.0、0.1≤θ≤0.2。
Wherein the grain size of anisotropism nanometer rare earth permanent magnetic material is 10～90nm.
Hereinafter above-mentioned anisotropism nanometer rare earth permanent magnetic material and preparation method are described in detail.
Embodiment 1:
A kind of anisotropism nanometer rare earth permanent magnetic material is: Nd7Fe87.5B5.45P0.05, this material has
Nano double phase structure, the Hard Magnetic of described material is R mutually2Fe14B and have (00l) texture, soft magnetism is α Fe mutually.
This material is less due to the rare earth element contained, and therefore cost is relatively low.
The preparation method of anisotropism nanometer rare earth permanent magnetic material: comprise the following steps:
A, melting ingot casting: choose ingot iron, technical pure neodymium, technical pure ferro-boron, technical pure ferrophosphorus, press
According to Nd7Fe87.5B5.45P0.05In each element atomic ratio weigh raw material.Load weighted raw material is put into electric arc melt
In furnace, it is evacuated to 1 × 10-3Pa, then recoil high-purity argon gas to stove internal gas pressure is 0.5 atmospheric pressure, adopts
Uniform with the mode melting of electric arc melting.Electric arc melting is that prior art does not repeats them here.
B, annealing: by the alloy after the melting of step A under vacuum, make annealing treatment 15 when 1200 DEG C
Hour；Fritter it is broken into after annealing；
C, system band: put in fast melt-quenching stove, remelting fast quenching under inert gas shielding, copper roller linear velocity
For 22m/s, obtain the strip of anisotropism nanometer rare earth permanent magnetic material；
D, post processing: the strip that step C prepares is optimal fast quenching thin strap, directly uses airflow crash
After obtain anisotropism nanometer rare earth permanent magnetic material.This material is not required to further Crystallizing treatment, can be straight
Connect for preparing bonded permanent magnet.
Detection: use the superconducting quantum interference device (SQUID) strip to preparing to carry out magnetic property measurement.
Testing conditions: applied field strengths is 4T, chooses when applying magnetic field along vertical strip surface direction and moves back
The magnetic factor is 0.75, and choosing demagnetizing factor when applying magnetic field along parallel stripes surface direction is 0.
Testing result is:
Along vertical strip surface direction: Br=1.05,iHc=417kA/m, (BH)max=120kJ/m3,
Along parallel stripes surface direction: Br=1.0,iHc=380kA/m, (BH)max=98kJ/m3。
Above-mentioned data show: this material has anisotropic character, and vertical strip surface direction is this material
Direction of easy axis, this side up, this permanent magnet material has higher magnetic property；Simultaneously as rare earth
Content is less, thus Hard Magnetic Phase Proportion is slightly lower, and this makes material HCJ slightly lower.
Embodiment 2:
A kind of anisotropism nanometer rare earth permanent magnetic material is: Nd11Fe79.5B8.2Zr1P0.3, this material has
Having nano double phase structure, the Hard Magnetic of described material is R mutually2Fe14B and have (00l) texture, soft magnetism is mutually
α–Fe.Carrying of interpolation due to Zr element so that alloy grain is refined, beneficially material property
Rise.
The preparation method of anisotropism nanometer rare earth permanent magnetic material: comprise the following steps:
A, melting ingot casting: choose ingot iron, technical pure neodymium, industrial pure zirconium, technical pure ferro-boron, industry
Pure ferrophosphorus, according to Nd11Fe79.5B8.2Zr1P0.3In each element atomic ratio weigh raw material.By load weighted former
Material is put in arc-melting furnace, is evacuated to 1 × 10-3Pa, then recoil high-purity argon gas to stove internal gas pressure is 0.5
Individual atmospheric pressure, the mode melting using electric arc melting is uniform.
B, annealing: by the alloy after the melting of step A under vacuum, make annealing treatment 40 when 900 DEG C
Hour；Homogenizing annealing be broken into fritter after annealing；
C, system band: the alloy after Po Sui is put in fast melt-quenching stove, remelting fast quenching under inert gas shielding,
Copper roller linear velocity is 20m/s, obtains the strip of anisotropism nanometer rare earth permanent magnetic material.
D, post processing: the strip that step C prepares is optimal fast quenching thin strap, directly uses airflow crash
After obtain anisotropism nanometer rare earth permanent magnetic material.This material is not required to further Crystallizing treatment, can be straight
Connect for preparing bonded permanent magnet.
Detection: use the superconducting quantum interference device (SQUID) strip to preparing to carry out magnetic property measurement.
Testing conditions: applied field strengths is 4T, chooses when applying magnetic field along vertical strip surface direction and moves back
The magnetic factor is 0.75, and choosing demagnetizing factor when applying magnetic field along parallel stripes surface direction is 0.
Testing result is:
Along vertical strip surface direction: Br=1.05,iHc=590kA/m, (BH)max=140kJ/m3,
Along parallel stripes surface direction: Br=1.05,iHc=520kA/m, (BH)max=115kJ/m3。
Above-mentioned data show: this material has anisotropic character, and vertical strip surface direction is this material
Direction of easy axis, this side up, this permanent magnet material has higher magnetic property.
Embodiment 3:
A kind of anisotropism nanometer rare earth permanent magnetic material is: Nd7.5Pr2Fe82.5B6.4Nb1.5P0.1, this material
Material has nano double phase structure, and the Hard Magnetic of described material is R mutually2Fe14B and there is (00l) texture, soft magnetism
It is α Fe mutually.Due to the interpolation of Nb element, on the one hand alloy grain is refined, beneficially material
The lifting of material performance；On the other hand the thermostability of material is improved.
The preparation method of anisotropism nanometer rare earth permanent magnetic material: comprise the following steps:
A, melting ingot casting: choose ingot iron, technical pure didymium alloy, technical pure ferro-niobium, technical pure boron
Ferrum, technical pure ferrophosphorus, according to Nd7.5Pr2Fe82.5B6.4Nb1.5P0.1In each element atomic ratio weigh raw material.
Load weighted raw material is put in arc-melting furnace, is evacuated to 1 × 10-3Pa, then recoil high-purity argon gas is extremely
Stove internal gas pressure is 0.5 atmospheric pressure, and the mode melting using electric arc melting is uniform.
B, annealing: by the alloy after the melting of step A under vacuum, make annealing treatment 20 when 1000 DEG C
Hour；Homogenizing annealing be broken into fritter after annealing；
C, system band: the alloy after Po Sui is put in fast melt-quenching stove, remelting fast quenching under inert gas shielding,
Copper roller linear velocity is 22m/s, obtains the strip of anisotropism nanometer rare earth permanent magnetic material.
D, post processing: the strip that step C prepares is optimal fast quenching thin strap, after direct gas flow is broken
To anisotropism nanometer rare earth permanent magnetic material.This material is not required to further Crystallizing treatment, can directly use
In preparing bonded permanent magnet.
Detection: use the superconducting quantum interference device (SQUID) strip to preparing to carry out magnetic property measurement.
Testing conditions: applied field strengths is 4T, chooses when applying magnetic field along vertical strip surface direction and moves back
The magnetic factor is 0.75, and choosing demagnetizing factor when applying magnetic field along parallel stripes surface direction is 0.
Testing result is:
Along vertical strip surface direction: Br=1.05,iHc=570kA/m, (BH)max=230kJ/m3,
Along parallel stripes surface direction: Br=1.05,iHc=490kA/m, (BH)max=135kJ/m3。
Above-mentioned data show: this material has anisotropic character, and vertical strip surface direction is this material
Direction of easy axis, this side up, this permanent magnet material has higher magnetic property.Meanwhile, Nb element
Interpolation can crystal grain thinning, will not hinder again the formation of (00l) texture, therefore material property promotes bigger.
Embodiment 4:
A kind of anisotropism nanometer rare earth permanent magnetic material is: Nd9Fe84B6.4Ta 0.5P0.1, this material has
Having nano double phase structure, the Hard Magnetic of described material is R mutually2Fe14B and have (00l) texture, soft magnetism is mutually
α–Fe.Carrying of interpolation due to Ta element so that alloy grain is refined, beneficially material property
Rise.
The preparation method of anisotropism nanometer rare earth permanent magnetic material: comprise the following steps:
A, melting ingot casting: choose ingot iron, technical pure neodymium, technical pure ferro-boron, technical pure tantalum, industry
Pure ferrophosphorus, according to Nd9Fe84B6.4Ta0.5P0.1In each element atomic ratio weigh raw material.By load weighted former
Material is put in arc-melting furnace, is evacuated to 1 × 10-3Pa, then recoil high-purity argon gas to stove internal gas pressure is 0.5
Individual atmospheric pressure, the mode melting using electric arc melting is uniform.
B, annealing: by the alloy after the melting of step A under vacuum, make annealing treatment 30 when 1100 DEG C
Hour；Homogenizing annealing be broken into fritter after annealing；
C, system band: the alloy after Po Sui is put in fast melt-quenching stove, remelting fast quenching under inert gas shielding,
Copper roller linear velocity is 23m/s, obtains the strip of anisotropism nanometer rare earth permanent magnetic material.
D, post processing: the strip that step C prepares is optimal fast quenching thin strap, directly uses airflow crash
After obtain anisotropism nanometer rare earth permanent magnetic material.This material is not required to further Crystallizing treatment, can be straight
Connect for preparing bonded permanent magnet.
Detection: use the superconducting quantum interference device (SQUID) strip to preparing to carry out magnetic property measurement.
Testing conditions: applied field strengths is 4T, chooses when applying magnetic field along vertical strip surface direction and moves back
The magnetic factor is 0.75, and choosing demagnetizing factor when applying magnetic field along parallel stripes surface direction is 0.
Testing result is:
Along vertical strip surface direction: Br=1.05,iHc=580kA/m, (BH)max=170kJ/m3,
Along parallel stripes surface direction: Br=1.05,iHc=510kA/m, (BH)max=125kJ/m3。
Above-mentioned data show: this material has anisotropic character, and vertical strip surface direction is this material
Direction of easy axis, this side up, this permanent magnet material has higher magnetic property.
Embodiment 5:
A kind of anisotropism nanometer rare earth permanent magnetic material is: Nd10Fe81.5B6.8V1.5P0.2, this material has
Having nano double phase structure, the Hard Magnetic of described material is R mutually2Fe14B and have (00l) texture, soft magnetism is mutually
α–Fe.The lifting of the interpolation due to V element so that alloy grain is refined, beneficially material property.
The preparation method of anisotropism nanometer rare earth permanent magnetic material: comprise the following steps:
A, melting ingot casting: choose ingot iron, technical pure neodymium, technical pure ferro-boron, technical pure vanadium iron, work
The pure ferrophosphorus of industry, according to Nd10Fe81.5B6.8V1.5P0.2In each element atomic ratio weigh raw material.By load weighted
Raw material is put in arc-melting furnace, is evacuated to 1 × 10-3Pa, then recoil high-purity argon gas to stove internal gas pressure is
0.5 atmospheric pressure, the mode melting using electric arc melting is uniform.
B, annealing: by the alloy after the melting of step A under vacuum, make annealing treatment 32 when 950 DEG C
Hour；Homogenizing annealing after being broken into fritter after annealing；
C, system band: the alloy after Po Sui is put in fast melt-quenching stove, remelting fast quenching under inert gas shielding,
Copper roller linear velocity is that 24m/s obtains strip.
D, post processing: the strip that step C prepares was melt spun alloy strip, need to carry out crystalline substance further
Annealing processes.Annealing is carried out in vacuum resistance furnace, is evacuated to 1 × 10-4Pa, is brought rapidly up
To 700 DEG C, pulverize after insulation 10min and obtain anisotropism nanometer rare earth permanent magnetic material.
Detection: use the superconducting quantum interference device (SQUID) strip to preparing to carry out magnetic property measurement.
Testing conditions: applied field strengths is 4T, chooses when applying magnetic field along vertical strip surface direction and moves back
The magnetic factor is 0.75, and choosing demagnetizing factor when applying magnetic field along parallel stripes surface direction is 0.
Testing result is:
Along vertical strip surface direction: Br=1.01,iHc=590kA/m, (BH)max=180kJ/m3；
Along parallel stripes surface direction: Br=0.95,iHc=482kA/m, (BH)max=115kJ/m3。
Above-mentioned data show: this material has anisotropic character, and vertical strip surface direction is this material
Direction of easy axis, this side up, this permanent magnet material has higher magnetic property.
Embodiment 6:
A kind of anisotropism nanometer rare earth permanent magnetic material is: Nd9.5Fe83.5B6.3W0.5P0.2, this material
Having nano double phase structure, the Hard Magnetic of described material is R mutually2Fe14B and there is (00l) texture, soft magnetism phase
For α Fe.Interpolation due to W element so that alloy grain is refined, beneficially material property
Promote.
The preparation method of anisotropism nanometer rare earth permanent magnetic material: comprise the following steps:
A, melting ingot casting: choose ingot iron, technical pure neodymium, technical pure ferro-boron, technical pure ferrotungsten, work
The pure ferrophosphorus of industry, according to Nd9.5Fe83.5B6.3W0.5P0.2In each element atomic ratio weigh raw material, load weighted
Raw material is put in arc-melting furnace, is evacuated to 1 × 10-3Pa, then recoil high-purity argon gas to stove internal gas pressure is
0.5 atmospheric pressure, the mode melting using electric arc melting is uniform.
B, annealing: by the alloy after the melting of step A under vacuum, make annealing treatment 25 when 1050 DEG C
Hour；Homogenizing annealing be broken into fritter after annealing；
C, system band: the alloy after Po Sui is put in fast melt-quenching stove, remelting fast quenching under inert gas shielding,
Copper roller linear velocity is that 24m/s obtains strip.
D, post processing: the strip that step C prepares was melt spun alloy strip, need to carry out crystalline substance further
Annealing processes.Annealing is carried out in vacuum resistance furnace, is evacuated to 1 × 10-4Pa, is brought rapidly up
To 700 DEG C, pulverize after insulation 10min and obtain anisotropism nanometer rare earth permanent magnetic material.
Detection: use the superconducting quantum interference device (SQUID) strip to preparing to carry out magnetic property measurement.
Testing conditions: applied field strengths is 4T, chooses when applying magnetic field along vertical strip surface direction and moves back
The magnetic factor is 0.75, and choosing demagnetizing factor when applying magnetic field along parallel stripes surface direction is 0.
Testing result is:
Along vertical strip surface direction: Br=1.01,iHc=520kA/m, (BH)max=170kJ/m3；
Along parallel stripes surface direction: Br=0.95,iHc=482kA/m, (BH)max=115kJ/m3。
Above-mentioned data show: this material has anisotropic character, and vertical strip surface direction is this material
Direction of easy axis, this side up, this permanent magnet material has higher magnetic property.
Embodiment 7:
A kind of anisotropism nanometer rare earth permanent magnetic material is: Pr8Fe85.5Co0.5B5.9P0..1, this material has
Having nano double phase structure, the Hard Magnetic of described material is R mutually2Fe14B and have (00l) texture, soft magnetism is mutually
α–Fe.The effect added except playing crystal grain thinning of Co, also advantageously improves the corrosion resistance of material
Energy.
The preparation method of anisotropism nanometer rare earth permanent magnetic material: comprise the following steps:
A, melting ingot casting: choose ingot iron, technical pure praseodymium, technical pure ferro-boron, technical pure cobalt, industry
Pure ferrophosphorus, according to r8Fe85.5Co0.5B5.9P0..1In each element atomic ratio weigh raw material, load weighted raw material
Put in induction melting furnace, be evacuated to 1 × 10-3Pa, then recoil high-purity argon gas to stove internal gas pressure is 0.5
Individual atmospheric pressure, the mode melting using induction melting is uniform.Induction melting is prior art, at this no longer
Repeat.
B, annealing: by the alloy after the melting of step A under vacuum, make annealing treatment 37 when 980 DEG C
Hour；Homogenizing annealing after being broken into fritter after annealing；
C, system band: the alloy after Po Sui is put in fast melt-quenching stove, remelting fast quenching under inert gas shielding,
Copper roller linear velocity is that 24m/s obtains strip.
D, post processing: the strip that step C prepares was melt spun alloy strip, need to carry out crystalline substance further
Annealing processes.Annealing is carried out in vacuum resistance furnace, is evacuated to 1 × 10-4Pa, is brought rapidly up
To 700 DEG C, pulverize after insulation 10min and obtain anisotropism nanometer rare earth permanent magnetic material.
Detection: use the superconducting quantum interference device (SQUID) strip to preparing to carry out magnetic property measurement.
Testing conditions: applied field strengths is 4T, chooses when applying magnetic field along vertical strip surface direction and moves back
The magnetic factor is 0.75, and choosing demagnetizing factor when applying magnetic field along parallel stripes surface direction is 0.
Testing result is:
Along vertical strip surface direction: Br=1.01,iHc=590kA/m, (BH)max=180kJ/m3；
Along parallel stripes surface direction: Br=0.95,iHc=482kA/m, (BH)max=115kJ/m3。
Above-mentioned data show: this material has anisotropic character, and vertical strip surface direction is this material
Direction of easy axis, this side up, this permanent magnet material has higher magnetic property.
Embodiment 8:
A kind of anisotropism nanometer rare earth permanent magnetic material is: Nd11Fe80.5B8.2P0.3, this material has to be received
Rice double structure, the Hard Magnetic of described material is R mutually2Fe14B and have (00l) texture, soft magnetism is α Fe mutually.
The preparation method of anisotropism nanometer rare earth permanent magnetic material: comprise the following steps:
A, melting ingot casting: choose ingot iron, technical pure neodymium, technical pure ferro-boron, technical pure ferrophosphorus, press
According to Nd11Fe80.5B8.2P0.3In each element atomic ratio weigh raw material, arc-melting furnace put into by load weighted raw material
In, it is evacuated to 1 × 10-3Pa, then recoil high-purity argon gas to stove internal gas pressure is 0.5 atmospheric pressure, uses electricity
The mode melting of arc melting is uniform.
B, annealing: by the alloy after the melting of step A under vacuum, make annealing treatment 22 when 1150 DEG C
Hour；Fritter it is broken into after annealing；
C, system band: put in fast melt-quenching stove, remelting fast quenching under inert gas shielding, copper roller linear velocity
For 20m/s, obtain the strip of anisotropism nanometer rare earth permanent magnetic material；
D, post processing: the strip that step C prepares is optimal fast quenching thin strap, directly uses airflow crash
After obtain anisotropism nanometer rare earth permanent magnetic material.This material is not required to further Crystallizing treatment, can be straight
Connect for preparing bonded permanent magnet.
Detection: use the superconducting quantum interference device (SQUID) strip to preparing to carry out magnetic property measurement.
Testing conditions: applied field strengths is 4T, chooses when applying magnetic field along vertical strip surface direction and moves back
The magnetic factor is 0.75, and choosing demagnetizing factor when applying magnetic field along parallel stripes surface direction is 0.
Testing result is:
Along vertical strip surface direction: Br=1.05,iHc=517kA/m, (BH)max=130kJ/m3,
Along parallel stripes surface direction: Br=1.0,iHc=380kA/m, (BH)max=108kJ/m3。
Above-mentioned data show: this material has anisotropic character, and vertical strip surface direction is this material
Direction of easy axis, this side up, this permanent magnet material has higher magnetic property.
Claims (5)
1. the preparation method of an anisotropism nanometer rare earth permanent magnetic material, it is characterised in that include
Following steps:
A, melting ingot casting: select high purity iron, ferro-boron, ferrophosphorus, metal R as raw material, melted by sensing
Refining or electric arc melting obtain alloy cast ingot, and described metal R selects neodymium, praseodymium or didymium alloy；
B, annealing: under vacuum condition, make annealing treatment 15-40 hour when 900-1200 DEG C；
C, system band: after the alloy cast ingot after step B annealing crushes, under inert gas shielding, remelting
Fast quenching, obtains alloy thin band；In described remelting fast quenching, copper roller linear velocity is 20m/s-24m/s；
D, post processing: alloy thin band is directly pulverized, or alloy thin band subsequent annealing is pulverized again, obtain respectively
Anisotropy Nanocomposite rare earth permanent-magnetic material；
In the raw material of described step A, high purity iron, ferro-boron, ferrophosphorus, the amount of metal R meet
RxFe100-x-αBα-θPθ, wherein said x, α, θ meet: 7.0≤x≤11.0,5.5≤α≤8.5,
0.05≤θ≤0.3。
The preparation method of anisotropism nanometer rare earth permanent magnetic material the most according to claim 1,
It is characterized in that, in described step A, described electric arc melting is: be evacuated to 0.1 × 10-3Pa
-2×10-3Pa, recoil noble gas is to reaching 0.2-1 atmospheric pressure, then raw material is carried out electric arc melting.
The preparation method of anisotropism nanometer rare earth permanent magnetic material the most according to claim 1,
It is characterized in that, in described step A, described induction melting is: be evacuated to 0.1 × 10-3Pa
-2×10-3Pa, recoil noble gas is to reaching 0.2-1 atmospheric pressure, then raw material is carried out induction melting.
4. the preparation method of an anisotropism nanometer rare earth permanent magnetic material, it is characterised in that include
Following steps:
A, melting ingot casting: select high purity iron, ferro-boron, ferrophosphorus, metal R, metal M as raw material, lead to
Crossing induction melting or electric arc melting obtains alloy cast ingot, described metal R selects neodymium, praseodymium or didymium to close
Gold；Described M metal is one or more in metal Nb, V, Ta, Zr, Co, Mo, W；
B, annealing: under vacuum condition, make annealing treatment 15-40 hour when 900-1200 DEG C；
C, system band: after the alloy cast ingot after step B annealing crushes, under inert gas shielding, remelting
Fast quenching, obtains alloy thin band；In described remelting fast quenching, copper roller linear velocity is 20m/s-24m/s；
D, post processing: alloy thin band is directly pulverized, or alloy thin band subsequent annealing is pulverized again, obtain respectively
Anisotropy Nanocomposite rare earth permanent-magnetic material；
In the raw material of described step A, the amount of all raw materials meets: RxFe100-x-y-αBα-θMyPθ, Qi Zhongsuo
State x, y, α, θ to meet: 7.0≤x≤11.0,0 ＜ y≤3,5.5≤α≤8.5,0.05≤θ≤0.3.
The preparation method of anisotropism nanometer rare earth permanent magnetic material the most according to claim 4,
It is characterized in that, in described step A, described electric arc melting is: be evacuated to 0.1 × 10-3Pa
-2×10-3Pa, recoil noble gas is to reaching 0.2-1 atmospheric pressure, then raw material is carried out electric arc melting；
Described induction melting is: be evacuated to 0.1 × 10-3Pa-2×10-3Pa, recoil noble gas is to reaching 0.2-1
Individual atmospheric pressure, then raw material is carried out induction melting.
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