CN104575920B - Rare-earth permanent magnet and preparation method thereof - Google Patents
Rare-earth permanent magnet and preparation method thereof Download PDFInfo
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- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 105
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 103
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 229910052779 Neodymium Inorganic materials 0.000 claims abstract description 13
- 229910052692 Dysprosium Inorganic materials 0.000 claims abstract description 5
- 229910052691 Erbium Inorganic materials 0.000 claims abstract description 5
- 229910052688 Gadolinium Inorganic materials 0.000 claims abstract description 5
- 229910052689 Holmium Inorganic materials 0.000 claims abstract description 5
- 229910052771 Terbium Inorganic materials 0.000 claims abstract description 5
- 229910052775 Thulium Inorganic materials 0.000 claims abstract description 5
- 229910052769 Ytterbium Inorganic materials 0.000 claims abstract description 5
- 229910052802 copper Inorganic materials 0.000 claims abstract description 5
- 229910052733 gallium Inorganic materials 0.000 claims abstract description 5
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 5
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 5
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 5
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 5
- 239000000843 powder Substances 0.000 claims description 24
- 229910045601 alloy Inorganic materials 0.000 claims description 23
- 239000000956 alloy Substances 0.000 claims description 23
- 239000002994 raw material Substances 0.000 claims description 20
- 230000005291 magnetic effect Effects 0.000 claims description 19
- 238000002844 melting Methods 0.000 claims description 10
- 230000008018 melting Effects 0.000 claims description 10
- 238000005245 sintering Methods 0.000 claims description 10
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 8
- 229910052737 gold Inorganic materials 0.000 claims description 8
- 239000010931 gold Substances 0.000 claims description 8
- 230000006698 induction Effects 0.000 claims description 8
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- 235000012054 meals Nutrition 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- 238000000465 moulding Methods 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- 239000003963 antioxidant agent Substances 0.000 claims description 3
- 230000003078 antioxidant effect Effects 0.000 claims description 3
- 238000000498 ball milling Methods 0.000 claims description 3
- 238000005266 casting Methods 0.000 claims description 3
- 238000007731 hot pressing Methods 0.000 claims description 3
- 238000003801 milling Methods 0.000 claims description 3
- 238000010791 quenching Methods 0.000 claims description 3
- 230000000171 quenching effect Effects 0.000 claims description 3
- 238000005496 tempering Methods 0.000 claims description 3
- -1 HRE La Inorganic materials 0.000 claims description 2
- 238000007670 refining Methods 0.000 claims 1
- 229910052777 Praseodymium Inorganic materials 0.000 abstract description 9
- 238000006467 substitution reaction Methods 0.000 abstract description 6
- 229910052684 Cerium Inorganic materials 0.000 abstract description 5
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 abstract description 4
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 abstract description 4
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical group [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 abstract description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 26
- 239000000126 substance Substances 0.000 description 21
- 229910001172 neodymium magnet Inorganic materials 0.000 description 12
- 238000001228 spectrum Methods 0.000 description 11
- 239000013078 crystal Substances 0.000 description 8
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 239000000696 magnetic material Substances 0.000 description 5
- 230000005389 magnetism Effects 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 230000008878 coupling Effects 0.000 description 3
- 238000010168 coupling process Methods 0.000 description 3
- 238000005859 coupling reaction Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
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- 238000010183 spectrum analysis Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000007792 addition Methods 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000005984 hydrogenation reaction Methods 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 230000005415 magnetization Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 1
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 1
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 1
- 235000007926 Craterellus fallax Nutrition 0.000 description 1
- 240000007175 Datura inoxia Species 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 1
- 239000005642 Oleic acid Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000013068 control sample Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 238000002595 magnetic resonance imaging Methods 0.000 description 1
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- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000005298 paramagnetic effect Effects 0.000 description 1
- 239000002907 paramagnetic material Substances 0.000 description 1
- 230000005408 paramagnetism Effects 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
- H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
- H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
- H01F1/0577—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together sintered
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/16—Ferrous alloys, e.g. steel alloys containing copper
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
- H01F41/0273—Imparting anisotropy
Abstract
The invention provides a kind of rare-earth permanent magnet and preparation method thereof, the general molecular formula of the mass ratio of the rare-earth permanent magnet is MMa‑ bHREbFeeBdTMc；Wherein, MM represents (LRE1‑xCex), and x and 1 x are mass ratio, LRE is one or both of Pr, Nd, the one or more in HRE La, Y, Gd, Tb, Dy, Ho, Er, Yb, Tm, the one or more in TM Al, Cu, Mn, Ga, Nb, Zr, and 0.24≤x≤0.6,27≤a≤36,0≤b≤10,0≤c≤3, the a d c d of 0.8≤d≤1.5, e=100；The principal phase of the rare-earth permanent magnet is 2 14 1 phases, in addition, Nd-rich phase and CeFe also be present2Phase.Rare-earth permanent magnet of the present invention and preparation method thereof, a part of cerium substitution praseodymium or neodymium are used so that the cost of the rare-earth permanent magnet declines to a great extent, and keeps higher coercivity.
Description
Technical field
The present invention relates to material manufacture field, more particularly to a kind of rare-earth permanent magnet and preparation method thereof.
Background technology
As third generation rare earth permanent-magnetic material, there is neodymium iron boron（Nd2Fe14B）The rare earth of phase structure and its similar structures is forever
Magnetic material is applied rapidly in hard disc of computer, Magnetic resonance imaging, hybrid vehicle, wind-power electricity generation etc. with its excellent performance
Field.At present, the neodymium iron boron yield in China occupies more than the 80% of the world, and this is mainly due in hybrid vehicle and wind
The heavy demand in the fields such as power generating.For example average each hybrid vehicle needs 2-3kg neodymium iron boron based permanent magnetic materials,
And need 0.5-1t neodymium iron boron base permanent magnets per megawatt wind driven generator group.
Although neodymium iron boron base permanent magnet has a wide range of applications, the rare earth element fancy price such as neodymium or praseodymium causes
Low and middle-grade permanent magnets remains in that higher price.This undoubtedly limits the application of Nd-Fe-B permanent magnet.It is well known that
Storage number is relevant in the world with it for the height of rare earth price, compared to neodymium or praseodymium, content compared with the cerium of horn of plenty have compared with
Low price.Thus, substitute Pr/Nd using the Rare-Earth Ce of high abundance, it is possible to prepare cheap neodymium iron boron base permanent magnet.But
Ce2Fe14B saturation magnetization and anisotropy field is compared with Nd2Fe14B's is low, and the remanent magnetism of magnet can be caused after Ce additions and is rectified
Stupid power reduces.Therefore, prepare satisfaction application and the permanent magnet containing high level Ce turns into current technological difficulties and focus.
The content of the invention
Based on above mentioned problem, the invention provides a kind of rare-earth permanent magnet and preparation method thereof, reduces rare earth permanent magnet material
The cost of material, meanwhile, maintain higher coercivity.
To reach above-mentioned technical purpose, the present invention adopts the following technical scheme that：
A kind of rare-earth permanent magnet, the quality of the rare-earth permanent magnet are MM than general molecular formulaa-bHREbFeeBdTMc；Wherein,
MM represents (LRE1-xCex), and x and 1-x are one or both of mass ratio, LRE Pr, Nd, HRE La, Y, Gd, Tb,
One or more in Dy, Ho, Er, Yb, Tm, the one or more in TM Al, Cu, Mn, Ga, Nb, Zr, and 0.24≤x≤
0.6,27≤a≤36,0≤b≤10,0≤c≤3,0.8≤d≤1.5, e=100-a-d-c-d；The principal phase of the rare-earth permanent magnet
For 2-14-1 phases, in addition, Nd-rich phase and CeFe also be present2Phase.
In one of the embodiments, the CeFe2Distributed mutually is in the grain boundaries in the rare earth permanent magnet body.
In one of the embodiments, 0.24≤x≤0.32.
A kind of preparation method of rare-earth permanent magnet, comprises the following steps：
（1）Configure raw material：According to MMa-bHREbFeeBdTMcQuality proportioning, configure a certain amount of gold containing respective element
Category or alloy raw material；
（2）Prepare initial alloy：By step（1）By rapid hardening, fast quenching or sense after obtained metal or alloy raw material mixing
Melting is answered to prepare the initial alloy that form is rapid-hardening flake, rapid tempering belt or ingot casting；
（3）Prepare alloyed powder：By step（2）Obtained initial alloy hydrogen is broken or Mechanical Crushing by way of crush
Into corase meal, described corase meal is then worn into fine powder by way of airflow milling or ball milling, obtains alloyed powder；
（4）Prepare magnet green compact：By step（3）Obtained alloyed powder is placed in the mould of definite shape, Ran Hou
Oriented moulding under magnetic fields, and magnet green compact are obtained after isostatic pressed is handled；
（5）Prepare magnet blank：By step（4）Obtained magnet green compact be placed in vacuum drying oven at a certain temperature sintering or
Hot pressing 1-4h, obtain magnet blank；
（6）Prepare rare-earth permanent magnet：By step（5）In obtained magnet blank carry out vacuum heat, you can obtain dilute
Native permanent magnet.
In one of the embodiments, step（2）In, initial alloy, the temperature of induction melting are prepared using induction melting
1410 DEG C of ＜.
In one of the embodiments, step（3）In the obtained particle mean size of alloyed powder be 3-5 μm.
In one of the embodiments, step（3）In, a small amount of antioxidant is added when preparing alloyed powder.
In one of the embodiments, step（4）In, the density of the magnet green compact is 2.8-4.5g/cm3。
In one of the embodiments, step（5）In, 1050 DEG C of sintering temperature ＜.
In one of the embodiments, in step（6）In, the process of vacuum heat is divided into two-stage, the temperature of the first order
For 860-940 DEG C, 1-4h is incubated, the temperature of the second level is 420-560 DEG C, is incubated 1-4h.
Rare-earth permanent magnet provided by the invention, a part of cerium substitution praseodymium or neodymium are used, from the aspect of cost, with market
Upper existing Nd-Fe-B permanent magnet is compared, and cost declines to a great extent；From the aspect of magnetic property, the permanent magnet remains in that higher
Coercivity and larger magnetic energy product.The preparation method of the present invention, has successfully prepared a kind of rare-earth permanent magnet, ensure that and prepare
Rare-earth permanent magnet there is higher coercivity, it is met many applications.
Brief description of the drawings
The X ray diffracting spectrum of Fig. 1 rare-earth permanent magnets of the present invention, wherein,（a）-（c）Respectively reference examples 1-3's is dilute
The X ray diffracting spectrum of native permanent magnet,（d）-（f）The respectively X ray diffracting spectrum of embodiment 1-3 rare-earth permanent magnet；
The X ray diffracting spectrum of Fig. 2 rare-earth permanent magnets of the present invention, wherein,（a）-（c）Respectively reference examples 4-6's is dilute
The X ray diffracting spectrum of native permanent magnet,（d）-（f）The respectively X ray diffracting spectrum of embodiment 4-6 rare-earth permanent magnet；
Fig. 3 is the back scattering stereoscan photograph of the rare-earth permanent magnet of the present invention, wherein（a）、（b）、（c）、（d）Respectively
Reference examples 5, embodiment 4, embodiment 5, the stereoscan photograph of embodiment 6；
Fig. 4 is that the rare-earth permanent magnet of reference examples 5 is reported in the energy spectrum analysis of triangle grain boundaries；
Fig. 5 is that the rare-earth permanent magnet of embodiment 4 is reported in the energy spectrum analysis of triangle grain boundaries；
Fig. 6 is the micro-structure diagram of the rare-earth permanent magnet of the embodiment of the present invention 1.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Site preparation describes.It should be noted that in the case where not conflicting, the feature in embodiment and embodiment in the application can phase
Mutually combination.
Referring to Fig. 1 to Fig. 6, the invention provides a kind of rare-earth permanent magnet, the quality of the rare-earth permanent magnet compares general molecular formula
For MMa-bHREbFeeBdTMc；Wherein, MM represents (LRE1-xCex), and x and 1-x are mass ratio, one kind in LRE Pr, Nd
Or two kinds, the one or more in HRE La, Y, Gd, Tb, Dy, Ho, Er, Yb, Tm, in TM Al, Cu, Mn, Ga, Nb, Zr
One or more, and 0.24≤x≤0.6,27≤a≤36,0≤b≤10,0≤c≤3,0.8≤d≤1.5, e=100-a-d-c-
d.The principal phase of the rare-earth permanent magnet is 2-14-1 phases, in addition, Nd-rich phase and CeFe also be present2Phase.One embodiment wherein
In, CeFe2Distributed mutually is especially distributed across triangle grain boundaries in the grain boundaries in rare earth permanent magnet body.Preferably, the present invention's
In rare-earth permanent magnet, Ce substitution Pr or Nd mass ratio 0.24≤x≤0.32.Under the substitution content, rare-earth permanent magnet
With of a relatively high coercivity and larger remanent magnetism, many practical applications can be met, and because Ce contents are more, so
Greatly save the cost of rare-earth permanent magnet.
The rare-earth permanent magnet of the present invention, a part of Ce substitutions Pr or Nd is used, and CeFe is formed in crystalline phase2Phase.By
In CeFe2It is mutually that one kind is at room temperature paramagnetic phase, it is mainly distributed on crystal boundary, can strengthen that 2-14-1 is alternate to be gone
Magnetic coupling interaction, so as to the coercivity of enhancing magnet, it compensate for causing because Ce is entered in 2-14-1 phases to a certain extent
The anisotropy field of magnet reduces the defects of coercivity declines caused by.Simultaneously as Ce addition so that of the invention
Compared with the existing Nd-Fe-B permanent magnet of in the market, cost declines to a great extent rare-earth permanent magnet.
Present invention also offers a kind of preparation method of above-mentioned rare-earth permanent magnet, comprise the following steps：
（1）Configure raw material：According to MMa-bHREbFeeBdTMcQuality proportioning, configure a certain amount of gold containing respective element
Category or alloy raw material, wherein, MM represents (LRE1-xCex), and x and 1-x are mass ratio, one kind or two in LRE Pr, Nd
Plant, the one or more in HRE La, Y, Gd, Tb, Dy, Ho, Er, Yb, Tm, one kind in TM Al, Cu, Mn, Ga, Nb, Zr
Or it is several, and 0.24≤x≤0.6,27≤a≤36,0≤b≤10,0≤c≤3,0.8≤d≤1.5, e=100-a-d-c-d.It is excellent
Selection of land, the raw material of rare earth element is mixed rare earth alloy, it is, for example, possible to use containing in tri- kinds of elements of Ce, Pr, Nd at least two
The alloy of element, which reduces the separation process of rare earth, so as to avoid energy consumption and the environmental pollution in separation process.
（2）Prepare initial alloy：By step（1）By rapid hardening, fast quenching or sense after obtained metal or alloy raw material mixing
Melting is answered to prepare the initial alloy that form is rapid-hardening flake, rapid tempering belt or ingot casting.Preferably, initial close is prepared using induction melting
Gold, 1410 DEG C of the temperature ＜ of induction melting.
（3）Prepare alloyed powder：By step（2）Obtained initial alloy hydrogen is broken or Mechanical Crushing by way of crush
Into corase meal, then by way of airflow milling or ball milling by corase meal wear into fine powder, alloyed powder is made.Preferably, obtain
The particle mean size of the alloyed powder arrived is 3-5 μm.It is preferred that a small amount of antioxidant, such as isopropyl can be added when preparing alloyed powder
Alcohol and oleic acid, to prevent the oxidation of alloyed powder.
（4）Prepare magnet green compact：By step（3）Obtained alloyed powder is placed in the mould of definite shape, then in magnetic
Oriented moulding under field action, and magnet green compact are obtained after isostatic pressed is handled.Preferably, the density of magnet green compact is
2.8-4.5g/cm3。
（5）Prepare magnet blank：By step（4）Obtained magnet green compact be placed in vacuum drying oven at a certain temperature sintering or
Hot pressing 1-4h time, obtain magnet blank.As a kind of embodiment, magnet green compact are placed in vacuum drying oven in ＜ 1050
DEG C temperature below sintering 1-4h.At this temperature, the 2-14-1 phases rich in Ce will not melt and destroy the degree of orientation of magnet and then
Influence the remanent magnetism of magnet.
（6）Prepare rare-earth permanent magnet：By step（5）In obtained magnet blank carry out vacuum heat, you can obtain dilute
Native permanent magnet.Preferably, the process of vacuum heat is divided into two-stage, and the temperature of the first order is 860-940 DEG C, is incubated 1-4h,
The temperature of the second level is 420-560 DEG C, is incubated 1-4h.By heat treatment, the optimization in structure can be carried out to rare-earth permanent magnet,
It is distributed its crystal boundary more continuous, crystal boundary is apparent.
The preparation method of the present invention, has successfully prepared a kind of rare-earth permanent magnet, ensure that the rare-earth permanent magnet prepared
With higher coercivity and larger magnetic energy product, many applications can be met.
Two groups of experiments are elaborated to rare earth permanent-magnetic material of the present invention and preparation method thereof below, first group is pair
1-3 and embodiment 1-3 as usual；Second group is reference examples 4-6 and embodiment 4-6.
Reference examples 1
A kind of rare-earth permanent magnet, its quality are (Pr than chemical formula0.2Nd0.8)27.5Dy3Fe68.3Al0.1Cu0.1B1, the rare earth
Ce is free of in permanent magnet, its preparation method is as follows：
S100：Each raw material is prepared according to the amount that gross mass is 2.5kg, wherein, raw material uses Pr0.2Nd0.8(mass ratio) closes
Gold, pure Fe, pure Al, pure Cu, Dy79.7Fe20.3（Mass ratio）Alloy and B19.4Fe80.6（Mass ratio）Alloy.
S200：It is placed on after the raw material configured in S100 is mixed in vacuum induction rapid hardening furnace, is evacuated to 2 × 10-2Pa,
300Torr argon gas is then charged with, melting is carried out at 1400-1410 DEG C and is poured into a mould, prepares the rapid hardening that thickness is 300 μm
Piece.
S300：The rapid-hardening flake that S200 is obtained is placed in the broken stove of hydrogen and crushed by hydrogenation treatment, and shattering process is true to take out
Empty-to be filled with hydrogen-suction hydrogen-dehydrogenation-cooling, desorption temperature is at 300-800 DEG C.
S400：The powder after crushing will be hydrogenated in S300 and prepares particle mean size at 3 μm or so by stream of nitrogen gas mill
Powder.
S500：By the magnetic obtained in S300 under 1800kA/m magnetic fields oriented moulding, the then isostatic pressed under 200Mpa
Processing, it is 2-4g/cm to obtain density3Magnet green compact.
S600：The magnet green compact obtained in S500 are sintered in a vacuum furnace, sintering temperature is 1040-1045 DEG C, sintering
Time is 2h, obtains magnet blank.
S700：The magnet blank obtained in S600 is subjected to two level Technology for Heating Processing, it is true at 900 DEG C and 480 DEG C respectively
Sky heat treatment 2h, obtains rare-earth permanent magnet.
Reference examples 2
A kind of rare-earth permanent magnet, quality are [(Pr than chemical formula0.2Nd0.8)92Ce8]27.5Dy3Fe68.3Al0.1Cu0.1B1, root
Understand that the Pr/Nd for having 8wt.% is substituted by Ce according to the chemical formula.
S100：Each raw material is prepared according to the amount that gross mass is 2.5kg, wherein, raw material uses Pr0.2Nd0.8(mass ratio) closes
Gold, metal Ce, pure Fe, pure Al, pure Cu, Dy79.7Fe20.3（Mass ratio）Alloy and B19.4Fe80.6（Mass ratio）Alloy.
Remaining step obtains rare-earth permanent magnet with reference examples 1.
Reference examples 3
A kind of rare-earth permanent magnet, quality are [(Pr than chemical formula0.2Nd0.8)84Ce16]27.5Dy3Fe68.3Al0.1Cu0.1B1, by
This chemical formula understands that the Pr/Nd for having 16wt.% is substituted by Ce.Preparation method according to reference examples 2 prepares the rare-earth permanent magnet.
Embodiment 1
A kind of rare-earth permanent magnet, quality are [(Pr than chemical formula0.2Nd0.8)76Ce24]27.5Dy3Fe68.3Al0.1Cu0.1B1, by
This chemical formula understands that the Pr/Nd for having 24wt.% is substituted by Ce.Preparation method according to reference examples 2 prepares the rare-earth permanent magnet.
Fig. 6 is the micro-structure diagram of the rare-earth permanent magnet of embodiment 1, and as seen from the figure, the rare-earth permanent magnet includes 2-14-
1 phase, CeFe2Phase and Nd-rich phase, wherein, CeFe2The triangle grain boundaries being mutually distributed mainly in rare earth permanent magnet body.
Embodiment 2
A kind of rare-earth permanent magnet, quality are [(Pr than chemical formula0.2Nd0.8)68Ce32]27.5Dy3Fe68.3Al0.1Cu0.1B1, by
This chemical formula understands that the Pr/Nd for having 32wt.% is substituted by Ce.Preparation method according to reference examples 2 prepares the rare-earth permanent magnet.
Embodiment 3
A kind of rare-earth permanent magnet, quality are [(Pr than chemical formula0.2Nd0.8)40Ce60]27.5Dy3Fe68.3Al0.1Cu0.1B1, by
This chemical formula understands that the Pr/Nd for having 60wt.% is substituted by Ce.Preparation method according to reference examples 2 prepares the rare-earth permanent magnet.
Fig. 1 is the X ray diffracting spectrum of first group of rare-earth permanent magnet, in this group of sample,（a）For the diffraction of reference examples 1
Collection of illustrative plates, it is blank control sample, Cheng Xiangwei 2-14-1 phases.（b）-（f）To mix the diffracting spectrum of Ce rare-earth permanent magnet, in Ce
When substituting Pr/Nd percentage to be 8wt.% and 16wt.%, do not occur CeFe2Diffraction maximum；With increasing for Ce contents, in Ce
When substituting Pr/Nd percentage to be 24wt.%, there is CeFe2Diffraction maximum；Continue to increase with Ce contents, occur more apparent
CeFe2Diffraction maximum, and in the range of 24wt.%-60wt.%, CeFe2Diffraction maximum gradually strengthen, illustrate in this scope
It is interior, with increasing for Ce contents, CeFe2Content in rare-earth permanent magnet gradually increases.Meanwhile it can be seen by diffracting spectrum
Go out, from（a）-（f）, diffraction peak to wide-angle offset, illustrate that Ce enters the lattice of 2-14-1 phases, cause lattice constant to become
It is small.
Table 1 is the magnetic performance test data of reference examples 1-3 and embodiment 1-3 rare-earth permanent magnet, wherein, Br is represented
Remanent magnetism, Hcj represent coercivity, BHmaxRepresent maximum magnetic energy product.
Table 1
| Numbering | Ce/LRE(%) | Br(kGs) | Hcj(kOe) | （BH）max(MGOe) |
| Reference examples 1 | 0 | 13.23 | 19.21 | 42.80 |
| Reference examples 2 | 8 | 13.07 | 16.72 | 41.43 |
| Reference examples 3 | 16 | 12.92 | 14.99 | 40.21 |
| Embodiment 1 | 24 | 12.44 | 16.72 | 36.37 |
| Embodiment 2 | 32 | 12.08 | 15.78 | 34.28 |
| Embodiment 3 | 60 | 11.33 | 11.33 | 29.07 |
Reference examples 1-3 is observed, after mixing Ce in rare-earth permanent magnet, the remanent magnetism of magnet declines, and coercivity reduces, and with
The rise of Ce contents, it is due to lattice that Ce enters 2-14-1 phases that the coercivity of rare-earth permanent magnet, which reduces this, causes the phase
Caused by saturation magnetization, anisotropy field reduce.
Reference examples 3 and the magnetic performance data of embodiment 1-3 rare-earth permanent magnet are observed, with the increase of Ce contents, rare earth
The phenomenon for first raising and reducing again occurs in the value of permanent magnet coercive force.This is due to as Ce contents increase, in rare-earth permanent magnet
There is CeFe2Caused by phase.CeFe2It is a kind of phase for being shown as paramagnetic material at room temperature, is distributed on crystal boundary, can strengthens
2-14-1 it is alternate remove magnetic coupling interaction, so as to enhancing magnet coercivity；But after the rise to a certain extent of Ce concentration, due to
CeFe2Caused by coercitive rise be not enough to make up due to the defects of anisotropy field caused by Ce reduces.Therefore, coercivity
Value the phenomenon for first raising and reducing again occurs.Meanwhile Pr/Nd weight/mass percentage composition is substituted to be 24wt.%-32wt.% in Ce
When, rare-earth permanent magnet has more excellent magnetic performance, can meet many applications, and within this range, Ce percentage contains
Amount is higher, and therefore, the cost of overall rare-earth permanent magnet substantially reduces.
Reference examples 4
A kind of rare-earth permanent magnet, its quality are (Pr than chemical formula0.2Nd0.8)30.5Fe68.3Al0.1Cu0.1B1, the rare earth permanent magnet
Body Ce percentage composition is 0wt.%, and its preparation method is as follows：
S100：Each raw material is prepared according to the amount that gross mass is 2.5kg, wherein, raw material uses Pr0.2Nd0.8(mass ratio) closes
Gold, pure Cu, pure Al, pure Fe, B19.4Fe80.6（Mass ratio）Alloy.
S200：It is placed on after the raw material configured in S100 is mixed in vacuum induction rapid hardening furnace, is evacuated to 2 × 10-2Pa,
300Torr argon gas is then charged with, melting is carried out at 1390-1400 DEG C and is poured into a mould, prepares the rapid hardening that thickness is 300 μm
Piece.
S300：The rapid-hardening flake that S200 is obtained is placed in the broken stove of hydrogen and crushed by hydrogenation treatment, and shattering process is true to take out
Empty-to be filled with hydrogen-suction hydrogen-dehydrogenation-cooling, desorption temperature is at 300-800 DEG C.
S400：The powder after crushing will be hydrogenated in S300 and prepares particle mean size at 3 μm or so by stream of nitrogen gas mill
Powder.
S500：By the magnetic obtained in S300 under 1800kA/m magnetic fields oriented moulding, the then isostatic pressed under 200Mpa
Processing, it is 3-4g/cm to obtain density3Magnet green compact.
S600：The magnet green compact obtained in S500 are sintered in a vacuum furnace, sintering temperature is 1020-1040 DEG C, sintering
Time is 2h, obtains magnet blank.
S700：The magnet blank obtained in S600 is subjected to two level Technology for Heating Processing, it is true at 900 DEG C and 500 DEG C respectively
Sky heat treatment 2h, obtains rare-earth permanent magnet.
Reference examples 5
A kind of rare-earth permanent magnet, quality are [(Pr than chemical formula0.2Nd0.8)92Ce8]30.5Fe68.3Al0.1Cu0.1B1, according to this
Chemical formula understands that the Pr/Nd for having 8wt.% is substituted by Ce.
S100：Each raw material is prepared according to the amount that gross mass is 2.5kg, wherein, raw material uses Pr0.2Nd0.8(mass ratio) closes
Gold, metal Ce, pure Al, pure Fe, pure Cu, B19.4Fe80.6（Mass ratio）Alloy.
Remaining step obtains rare-earth permanent magnet with reference examples 4.
Reference examples 6
A kind of rare-earth permanent magnet, mass ratio are chemical formula [(Pr0.2Nd0.8)84Ce16]30.5Fe68.3Al0.1Cu0.1B1, thus
Chemical formula understands that the Pr/Nd for having 16wt.% is substituted by Ce.Preparation method according to reference examples 5 prepares the rare-earth permanent magnet.
Embodiment 4
A kind of rare-earth permanent magnet, quality compare chemical formula：[(Pr0.2Nd0.8)76Ce24]30.5Fe68.3Al0.1Cu0.1B1, thus change
Formula understands that the Pr/Nd for having 24wt.% is substituted by Ce.Preparation method according to reference examples 5 prepares the rare-earth permanent magnet.
Embodiment 5
A kind of rare-earth permanent magnet, quality are [(Pr than chemical formula0.2Nd0.8)68Ce32]30.5Fe68.3Al0.1Cu0.1B1, thus
Chemical formula understands that the Pr/Nd for having 32wt.% is substituted by Ce.Preparation method according to reference examples 5 prepares the rare-earth permanent magnet.
Embodiment 6
A kind of rare-earth permanent magnet, quality are [(Pr than chemical formula0.2Nd0.8)40Ce60]30.5Fe68.3Al0.1Cu0.1B1, thus
Chemical formula understands that the Pr/Nd for having 60wt.% is substituted by Ce.Preparation method according to reference examples 5 prepares the rare-earth permanent magnet.
Fig. 2 is the X ray diffracting spectrum of second group of rare-earth permanent magnet, and table 2 is its magnetic performance test data.By Fig. 2 and
Table 2 can find second group of rare-earth permanent magnet and first group of similar experimental phenomena and experiment conclusion, not repeat one by one here.Together
When, contrast Tables 1 and 2 can be found, the rare-earth permanent magnet added after Dy has higher compared with the rare-earth permanent magnet for being not added with Dy
Coercivity and magnetic energy product, show as more excellent magnetic performance.
Table 2
| Numbering | Ce/LRE(%) | Br(kGs) | Hcj(kOe) | （BH）max(MGOe) |
| Reference examples 4 | 0 | 13.64 | 13.03 | 44.42 |
| Reference examples 5 | 8 | 13.43 | 9.65 | 41.45 |
| Reference examples 6 | 16 | 13.12 | 9.01 | 39.23 |
| Embodiment 4 | 24 | 12.67 | 13.33 | 37.01 |
| Embodiment 5 | 32 | 12.30 | 12.29 | 34.04 |
| Embodiment 6 | 60 | 11.28 | 7.01 | 26.80 |
Fig. 3 is magnet back scattering stereoscan photograph, wherein（a）、（b）、（c）、（d）Respectively reference examples 5, embodiment 4,
The stereoscan photograph of embodiment 5, embodiment 6.Gray area in figure is 2-14-1 phases, and triangle grain boundaries contain more
CeFe2Phase.It can be found by figure, due to there is CeFe2The presence of phase, the crystal boundary phase structure of magnet gradually become more, and crystal boundary is gradually clear.
Fig. 4 is that reference examples 5 are reported in the energy spectrum analysis of triangle grain boundaries, and Fig. 5 is power spectrum of the embodiment 4 in triangle grain boundaries
Analysis report.As seen from the figure, substantial amounts of Ce and Fe elements are contained in the triangle grain boundaries of rare earth permanent-magnetic material, and Ce/Fe is approached
1/2, this result confirms CeFe2The presence of phase, while also illustrate CeFe2Mutually it is easily collected on the triangle crystal boundary of rare-earth permanent magnet
Place.
The rare-earth permanent magnet of the present invention, a part of Ce substitutions Pr or Nd is used, and CeFe is formed in crystalline phase2Phase.By
In CeFe2It is mutually that one kind is shown as paramagnetism phase at room temperature, is distributed on crystal boundary, the alternate degaussing couplings of 2-14-1 can be strengthened
Cooperation is used, and so as to the coercivity of enhancing magnet, compensate for a certain extent because Ce enters Nd2Fe14Cause 2- in B phases
14-1 phases anisotropy field reduces the defects of coercivity reduces caused by.Simultaneously as Ce use so that of the invention
Compared with the existing Nd-Fe-B permanent magnet of in the market, cost declines to a great extent rare-earth permanent magnet.
Embodiment described above only expresses the several embodiments of the present invention, and its description is more specific and detailed, but simultaneously
Therefore the limitation to the scope of the claims of the present invention can not be interpreted as.It should be pointed out that for one of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the guarantor of the present invention
Protect scope.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (8)
1. a kind of rare-earth permanent magnet, it is characterised in that the quality of the rare-earth permanent magnet is MM than general molecular formulaa- bHREbFeeBdTMc；
Wherein, MM represents (LRE1-xCex), and x and 1-x are one or both of mass ratio, LRE Pr, Nd, HRE La,
Y, the one or more in Gd, Tb, Dy, Ho, Er, Yb, Tm, the one or more in TM Al, Cu, Mn, Ga, Nb, Zr, and
0.24≤x≤0.32,27≤a≤36,0 ＜ b≤10,0 ＜ c≤3,0.8≤d≤1.5, e=100-a-c-d；
The principal phase of the rare-earth permanent magnet is 2-14-1 phases, in addition, Nd-rich phase and CeFe also be present2Phase；
The CeFe2Distributed mutually is in the grain boundaries in the rare earth permanent magnet body.
2. a kind of preparation method of rare-earth permanent magnet as claimed in claim 1, it is characterised in that comprise the following steps：
(1) raw material is configured：According to MMa-bHREbFeeBdTMcQuality proportioning, configure a certain amount of metal or conjunction containing respective element
Golden raw material；
(2) initial alloy is prepared：The metal or alloy raw material that step (1) is obtained is molten by rapid hardening, fast quenching or sensing after mixing
The initial alloy that form is rapid-hardening flake, rapid tempering belt or ingot casting is prepared in refining；
(3) alloyed powder is prepared：By the initial alloy that step (2) obtains hydrogen is broken or Mechanical Crushing by way of be broken into it is thick
Powder, described corase meal is then worn into fine powder by way of airflow milling or ball milling, obtains alloyed powder；
(4) magnet green compact are prepared：The alloyed powder that step (3) obtains is placed in the mould of definite shape, then made in magnetic field
With lower oriented moulding, and magnet green compact are obtained after isostatic pressed is handled；
(5) magnet blank is prepared：The magnet green compact that step (4) obtains are placed in vacuum drying oven sintering or hot pressing at a certain temperature
1-4h, obtain magnet blank；
(6) rare-earth permanent magnet is prepared：The magnet blank obtained in step (5) is subjected to vacuum heat, you can obtain rare earth forever
Magnet.
3. preparation method according to claim 2, it is characterised in that in step (2), initial close is prepared using induction melting
Gold, 1410 DEG C of the temperature ＜ of induction melting.
4. preparation method according to claim 2, it is characterised in that the particle mean size of the alloyed powder obtained in step (3)
For 3-5 μm.
5. preparation method according to claim 2, it is characterised in that in step (3), added when preparing alloyed powder a small amount of
Antioxidant.
6. preparation method according to claim 2, it is characterised in that in step (4), the density of the magnet green compact is
2.8-4.5g/cm3。
7. preparation method according to claim 2, it is characterised in that in step (5), 1050 DEG C of sintering temperature ＜.
8. preparation method according to claim 2, it is characterised in that in step (6), the process of vacuum heat is divided into
Two-stage, the temperature of the first order is 860-940 DEG C, is incubated 1-4h, the temperature of the second level is 420-560 DEG C, is incubated 1-4h.
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| CN107578869B (en) * | 2016-07-05 | 2020-03-17 | 中国科学院物理研究所 | Mixed rare earth-iron-based permanent magnet material and preparation method and application thereof |
| JP2020095989A (en) * | 2017-03-30 | 2020-06-18 | Tdk株式会社 | Rare earth magnet and rotary machine |
| CN108922710B (en) | 2018-07-18 | 2020-03-20 | 钢铁研究总院 | High-toughness high-coercivity Ce-containing sintered rare earth permanent magnet and preparation method thereof |
| CN110148507B (en) * | 2019-05-23 | 2020-10-16 | 钢铁研究总院 | Grain boundary diffusion cerium magnet containing REFE2 phase and preparation method thereof |
| CN111223628B (en) * | 2020-02-26 | 2022-02-01 | 厦门钨业股份有限公司 | Neodymium-iron-boron magnet material, raw material composition, preparation method and application |
| CN114823028A (en) * | 2022-05-27 | 2022-07-29 | 广州北创磁材科技有限公司 | Low-cost high-coercivity neodymium iron boron alloy and preparation method thereof |
| CN115274242A (en) * | 2022-08-30 | 2022-11-01 | 烟台东星磁性材料股份有限公司 | Cerium-added RE-T-B-M series sintered neodymium-iron-boron magnet |
| CN115831519B (en) * | 2023-02-14 | 2023-05-12 | 宁波守正磁电有限公司 | Sintered NdFeB permanent magnet |
| CN116110707B (en) * | 2023-02-28 | 2023-08-15 | 宁波新越磁性科技有限公司 | Sintered Nd-Fe-B permanent magnet and preparation method thereof |
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