CN103824668B - Low-weight rare earth high-coercivity sintered neodymium-iron-boron magnet and production method thereof - Google Patents
Low-weight rare earth high-coercivity sintered neodymium-iron-boron magnet and production method thereof Download PDFInfo
- Publication number
- CN103824668B CN103824668B CN201410020883.2A CN201410020883A CN103824668B CN 103824668 B CN103824668 B CN 103824668B CN 201410020883 A CN201410020883 A CN 201410020883A CN 103824668 B CN103824668 B CN 103824668B
- Authority
- CN
- China
- Prior art keywords
- rare earth
- micropowder
- earth element
- hours
- kinds
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Hard Magnetic Materials (AREA)
Abstract
The invention relates to the technical field of rare earth neodymium-iron-boron permanent magnet material, in particular to a low-weight rare earth high-coercivity sintered neodymium-iron-boron magnet and a production method thereof. Composition of the low-weight rare earth high-coercivity sintered neodymium-iron-boron magnet is expressed as: Re Alpha Fe(100-Alpha-Beta-NuB Beta)MNu. The production method includes: mixing alloy powder and rare earth micro powder, pressing the mixture under the orientation field with intensity not smaller than 1.5T to obtain a blank; sintering at the temperature of 1050-1120 DEG C to obtain low-weight rare earth high-coercivity sintered neodymium-iron-boron magnet. The rare earth neodymium-iron-boron permanent magnet material produced by the method and products of the material have well uniform properties, heavy rare earth consumption is low, and coercivity is high.
Description
Technical field
The present invention relates to a kind of rare-earth Nd-Fe-B permanent magnetic material technical field, be specifically related to a kind of low heavy rare earth high-coercive force Sintered NdFeB magnet and preparation method thereof.
Background technology
Rare-earth Nd-Fe-B permanent magnetic material is the third generation rare earth permanent magnet functional material of the invention early 1980s, its excellent magnetic property with high remanent magnetism, high-coercive force and high energy product is that other permanent magnet material cannot replace, therefore it is widely used in all fields of national economies such as the energy, traffic, machinery, electronics and becomes one of important foundation material supporting contemporary electronic information industry, guide electronic product to energy-saving and environmental protection, efficient, light direction development.The most also using the consumption per capita of rare-earth Nd-Fe-B permanent magnetic material as weighing one of people of other countries' living standard important symbol with up-to-dateness.
In the prior art, mainly use heavy rare earth element Dy, Tb, Ho for obtaining high-coercive force, and the compound interpolation of the element such as other non-rare earth metal Nb, Cu, Al, Ga, Ti, V, Mn, Zn, Zr, W, Si, Sn, Cr, Mo.And heavy rare earth element Dy, Tb, Ho belong to scarce resource and relatively costly, it is unfavorable for protecting effective utilization of non-renewable resources, too increases production cost simultaneously.Although using the combination process that low oxygen process, micropowder technique or hypoxia combine with micropowder to fully demonstrate the magnetic property characteristic of material itself, also the purpose reducing heavy rare earth element usage amount can be played, but for now, because of by many restrictions of process equipment in large-scale production process, in China still in test and exploratory stage.
As Patent No. 8510978 Japan Patent, the Japan Patent of Patent No. 99801229.7 and Patent No. 200510084295.6 Japan Patent all have employed interpolation heavy rare earth element Dy, Tb, Ho to obtain the performance of high-coercive force, this can not change the degree of dependence to heavy rare earth element Dy, Tb, Ho.
Summary of the invention
The present invention is directed to current rare-earth Nd-Fe-B permanent magnetic material high-coercive force to heavy rare earth element Dy, Tb, the present situation of the dependence of Ho, a kind of low heavy rare earth high-coercive force Sintered NdFeB magnet and preparation method thereof is provided, by production process using rare earth element powder the richest neodymium of Fe-B rare-earth permanent magnet is carried out effective compensation mutually to make up the loss of the rare-earth Nd-Fe-B permanent magnet richness neodymium phase caused in process of production, thus in preparation process, reduce the usage amount of heavy rare earth element and obtain producing excellent low heavy rare earth high-coercive force Nd-Fe-B rare earth permanent magnetic material of performance concordance and products thereof in batches.
In order to reach foregoing invention purpose, the present invention by the following technical solutions:
A kind of low heavy rare earth high-coercive force Sintered NdFeB magnet, its constituent is ReαFe100-α-β-γBβMγ；
Re is rare earth element, including selected from La, Ce, Pr, Nd, Pm, Sm, Eu,Gd 、One or more element in Tb, Dy, Tb, Ho, Er, Tm, Yb, Lu, Y and Sc；
M is addition element, including the element of one or more in Ti, V, Cr, Ni, Zn, Ga, Ge, Al, Zr, Nb, Co, Cu, Ag, Sn, W, Pb, Bi and Pd；
Fe is Fe and inevitable impurity；
α, β and γ are the atom percentage content of each element, wherein: 12≤α≤18,5.3≤β≤6.5,0.1≤γ≤8.
The technical scheme is that by using rare earth element powder the richest effectively neodymium of Fe-B rare-earth permanent magnet to carry out effective compensation mutually to make up the loss of the rare-earth Nd-Fe-B permanent magnet richness neodymium phase caused in process of production in process of production, thus in preparation process, reduce the usage amount of heavy rare earth element and obtain producing excellent low heavy rare earth high-coercive force Nd-Fe-B rare earth permanent magnetic material of performance concordance and products thereof in batches.
Preferably, described rare earth element is one or more in La, Ce, Pr, Nd, Dy and Tb.
Preferably, 15≤α≤18.
Preferably, 5.8≤β≤6.2.
Preferably, 2≤γ≤3.
The preparation method of a kind of low heavy rare earth high-coercive force Sintered NdFeB magnet, comprises the following steps:
1) use Mechanical Crushing or the hydrogen quick-fried airflow milling mode that adds that Nd-Fe-B rare earth permanent magnetic material alloy is crushed, prepare the mean diameter Nd-Fe-B rare earth permanent magnetic material alloy powder in 2.5-5.0 μm；
2) rare earth element micropowder is obtained the mean diameter rare earth micropowder in 1.5-3.6 μm by all kinds of crushing process；Crushing process comprises Mechanical Crushing technique (as ball mill crushing, airflow milling crush), the crushing process of physico-chemical process (as hydrogen crushes) and machinery and adds physico-chemical process broken (add air-flow gall broken as hydrogen is broken) etc.；
3) above-mentioned prepared rare earth micropowder is joined in Nd-Fe-B rare earth permanent magnetic material alloy powder according to the percentage by weight of 0.3%-5%, mix homogeneously；
4) by mixed alloy powder compressing blank in the alignment magnetic field of magnetic field intensity >=1.5T；
5) molded blank is put into vacuum sintering furnace and carries out high temperature sintering, sintering temperature 1050 DEG C-1120 DEG C, sintering time 1.0-6.0 hour, and carry out temper, prepare low heavy rare earth high-coercive force Sintered NdFeB magnet.
Preferably, described step 5) tempering process uses 460 DEG C of-530 DEG C of constant temperature 2-5 hour.
Preferably, described step 5) tempering process uses double tempering, is specially first 890 DEG C of-920 DEG C of constant temperature 1.5-3 hour, then 480 DEG C of-520 DEG C of constant temperature 2-5 hour.
Nd Fe B alloys system blank after molding is will be by principal phase (Nd after above-mentioned technique2Fe14B), rich-Nd phase, rare earth micropowder (one or more in La, Ce, Pr, Nd, Dy, Tb) and minimal amount of rich B phase (Nd1.1Fe4B4) composition, rare earth micropowder is present between the gap of principal phase granule.The fusing point of principal phase is about 1185 DEG C, and rare earth micropowder typically begins to dissolve when 700 DEG C ~ 800 DEG C, therefore the Nd Fe B alloys system principal phase by solid-state and the Nd-rich phase (being made up of rare earth micropowder and rich-Nd phase) of fusing under sintering temperature state, and Nd-rich phase is flowed by liquid phase, molecular thermalmotion penetrates into the gap between powder particle.When two powder particles are deposited in the liquid phase simultaneously, and when having preferable wellability between liquid phase and solid phase particles, two intergranular liquid phase surfaces to liquid phase curving thus produce a capillarity attraction, under the effect of this suction, even if two granules are mutually drawn close strengthens again liquid phase rare earth element to the infiltration within granule simultaneously, thus form the most complete Nd-rich phase, compensate in melting, powder process, the process loss of NdFeB material Nd-rich phase in molding and sintering process, inherently improve the anisotropy field of main phase grain surface layer, the magnetic hardening of main phase grain boundary region is caused to improve the coercivity of material.
The present invention compared with prior art, provides the benefit that: prepare that Nd-Fe-B rare earth permanent magnetic material and products thereof consistency of performance is excellent, heavy rare earth consumption is low and has high-coercive force.Use this method can replace heavy rare earth element with part LREE in the preparation process of Sintered NdFeB magnet product; reduce the usage amount of heavy rare earth element Dy and Tb; and the coercivity of resulting materials and be not less than with other process produce material; thus reduce the usage amount inherently comparing rare heavy rare earth element in rare earth element, effective utilization of protection non-renewable resources.
Detailed description of the invention
Below by specific embodiment, technical scheme is further described explanation.
If without specified otherwise, the raw material employed in embodiments of the invention is raw material commonly used in the art, and the method employed in embodiment is the conventional method of this area.
A kind of low heavy rare earth high-coercive force Sintered NdFeB magnet, its constituent is ReαFe100-α-β-γBβMγ；
Re is rare earth element, including selected from La, Ce, Pr, Nd, Pm, Sm, Eu,Gd 、One or more element in Tb, Dy, Tb, Ho, Er, Tm, Yb, Lu, Y and Sc；
M is addition element, including the element of one or more in Ti, V, Cr, Ni, Zn, Ga, Ge, Al, Zr, Nb, Co, Cu, Ag, Sn, W, Pb, Bi and Pd；
Fe is Fe and inevitable impurity；
α, β and γ are the atom percentage content of each element, wherein: 12≤α≤18,5.3≤β≤6.5,0.1≤γ≤8.
Described rare earth element is one or more in La, Ce, Pr, Nd, Dy and Tb.
15≤α≤18,5.8≤β≤6.2,2≤γ≤3.
The preparation method of a kind of low heavy rare earth high-coercive force Sintered NdFeB magnet, comprises the following steps:
1) use Mechanical Crushing or the hydrogen quick-fried airflow milling mode that adds that Nd-Fe-B rare earth permanent magnetic material alloy is crushed, prepare the mean diameter Nd-Fe-B rare earth permanent magnetic material alloy powder in 2.5-5.0 μm；Nd-Fe-B rare earth permanent magnetic material alloy, by mentioned component requirement, uses casting technique or rapid hardening thin slice technique to prepare；
2) rare earth element micropowder is obtained the mean diameter rare earth micropowder in 1.5-3.6 μm by all kinds of crushing process；
3) above-mentioned prepared rare earth micropowder is joined in Nd-Fe-B rare earth permanent magnetic material alloy powder according to the percentage by weight of 0.3%-5%, mix homogeneously；
4) by mixed alloy powder compressing blank in the alignment magnetic field of magnetic field intensity >=1.5T；
5) molded blank is put into vacuum sintering furnace and carries out high temperature sintering, sintering temperature 1050 DEG C-1120 DEG C, sintering time 1.0-6.0 hour, and carry out temper, prepare low heavy rare earth high-coercive force Sintered NdFeB magnet；Tempering process uses once tempering: 460 DEG C of-530 DEG C of constant temperature 2-5 hour, or double tempering: first 890 DEG C of-920 DEG C of constant temperature 1.5-3 hour, then 480 DEG C of-520 DEG C of constant temperature 2-5 hour.
Scheme combination 1:
It is Nd by composition10Dy2FeRemainingB5.3M0.1(at%) rare-earth Nd-Fe-B permanent magnetic material alloy, is prepared by technical scheme: carries out dispensing by mentioned component and prepares Nd-Fe-B permanent magnet material alloy with rapid hardening thin slice technique；Use that hydrogen is broken to be added airflow milling mode and crush rare-earth Nd-Fe-B permanent magnetic material alloy, prepare the mean diameter alloy powder in 2.5 μm.
The rare earth element micropowder adding air-flow grinding process acquisition mean diameter in 1.5 μm is broken by hydrogen, prepared various rare earth element micropowders are added in Nd-Fe-B rare earth permanent magnetic material alloy powder by different percentage compositions in pulverizing process, and carries out batch mixing and enable rare earth micropowder to be mixed into uniformly in Nd-Fe-B rare earth permanent magnetic material alloy powder；Mixed powder is compressing 41.5 × 50 × 42.3(mm in the alignment magnetic field of >=1.6T) square blank；Blank is put into high vacuum sintering furnace, sinters 4.0 hours at 1100 DEG C, be tempered 2 hours and 510 DEG C of second annealings 3.5 hours 890 DEG C of one-levels, prepared sintered magnet；Take Φ 10 × 10(mm) standard specimen five only carry out magnetism testing.
Scheme example 1: the interpolation percentage composition of rare earth element micropowder is 0%；The magnetic property testing result of gained sintered magnet: Hcj=27.73-28.26kOe.
Embodiment 2: the interpolation percentage composition of rare earth element micropowder is 0.3%, rare earth element used is Nd；The magnetic property testing result of gained sintered magnet: Hcj=27.86-28.50kOe；.
Embodiment 3: the interpolation percentage composition of rare earth neodymium micropowder is 1.0%, rare earth element used is Nd；The magnetic property testing result of gained sintered magnet: Hcj=28.81-29.49kOe.
Embodiment 4: the interpolation percentage composition of rare earth neodymium micropowder is 2.0%, rare earth element used is Nd；The magnetic property testing result of gained sintered magnet: Hcj=29.45-30.27kOe.
Embodiment 5: the interpolation percentage composition of rare earth neodymium micropowder is 3.0%, rare earth element used is Nd；The magnetic property testing result of gained sintered magnet: Hcj=30.05-31.49kOe.
Embodiment 6: the interpolation percentage composition of rare earth neodymium micropowder is 5.0%, rare earth element used is Nd；The magnetic property testing result of gained sintered magnet: Hcj=28.85-29.70kOe.
Comparative example 1: be Nd by composition9.5Dy2.5FeRemainingB5.3M0.1(at%) rare-earth Nd-Fe-B permanent magnetic material alloy；It is not added with rare earth micropowder by upper method and prepares the sample of same specification size, the magnetic property testing result of gained sintered magnet: Hcj=30.34-31.57.
The performance of embodiment 1-6 and comparative example 1 collects and is shown in Table 1；
Table 1
| Project | Adding proportion (%) | Addition element | Addition element ratio | Hcj(kOe) |
| Embodiment 1 | 0 | —— | —— | 27.73-28.26 |
| Embodiment 2 | 0.3 | Nd | 1 | 27.86-28.50 |
| Embodiment 3 | 1.0 | Nd | 1 | 28.81-29.49 |
| Embodiment 4 | 2.0 | Nd | 1 | 29.45-30.27 |
| Embodiment 5 | 3.0 | Nd | 1 | 30.05-31.49 |
| Embodiment 6 | 5.0 | Nd | 1 | 28.85-29.70 |
| Comparative example 1 | —— | —— | —— | 30.34-31.57 |
Scheme combination 2:
It is Nd by composition17Dy1FeRemainingB6.5M8(at%) rare-earth Nd-Fe-B permanent magnetic material alloy, is wherein prepared by technical scheme: carries out dispensing by mentioned component and prepares Nd-Fe-B permanent magnet material alloy with rapid hardening thin slice technique；Use that hydrogen is broken to be added airflow milling mode and crush rare-earth Nd-Fe-B permanent magnetic material alloy, prepare the mean diameter alloy powder in 5.0 μm.
The rare earth element micropowder adding air-flow grinding process acquisition mean diameter in 3.6 μm is broken by hydrogen, prepared various rare earth element micropowders are added in Nd-Fe-B rare earth permanent magnetic material powder by different percentage compositions in pulverizing process, and carries out batch mixing and enable rare earth micropowder to be mixed into uniformly in Nd-Fe-B rare earth permanent magnetic material powder；Mixed powder is compressing 41.5 × 50 × 42.3(mm in the alignment magnetic field of >=2.0T) square blank；Blank is put into high vacuum sintering furnace, sinters 6.0 hours at 1120 DEG C, be tempered 5 hours at 480 DEG C, prepare sintered magnet；Take Φ 10 × 10(mm) standard specimen five only carry out magnetism testing.
Embodiment 7: the interpolation percentage composition of rare earth element micropowder is 2.8%, rare earth element used is bis-kinds of admixed finepowders of Pr, Nd (mixed proportion is Pr:Nd=3:7)；The magnetic property testing result of gained sintered magnet: Hcj=26.38-26.70kOe.
Embodiment 8: the interpolation percentage composition of rare earth element micropowder is 2.8%, rare earth element used is bis-kinds of admixed finepowders of Ce, Pr (mixed proportion is Ce:Pr=5:5)；The magnetic property testing result of gained sintered magnet: Hcj=25.78-26.32kOe.
Embodiment 9: the interpolation percentage composition of rare earth element micropowder is 2.8%, rare earth element used is tri-kinds of admixed finepowders of Ce, Pr, Nd (mixed proportion is Ce:Pr:Nd=2:2:6)；The magnetic property testing result of gained sintered magnet: Hcj=26.08-26.42kOe.
Embodiment 10: the interpolation percentage composition of rare earth element micropowder is 2.8%, rare earth element used is tri-kinds of admixed finepowders of Pr, Nd, Dy (mixed proportion is Pr:Nd:Dy=5:2:3)；The magnetic property testing result of gained sintered magnet: Hcj=27.78-28.12kOe.
Embodiment 11: the interpolation percentage composition of rare earth element micropowder is 2.8%, rare earth element used is tetra-kinds of admixed finepowders of La, Pr, Nd, Tb (mixed proportion is La:Pr:Nd:Tb=5:2:2:1)；The magnetic property testing result of gained sintered magnet: Hcj=26.30-26.74kOe.
Embodiment 12: the interpolation percentage composition of rare earth element micropowder is 2.8%, rare earth element used is tetra-kinds of admixed finepowders of La, Ce, Pr, Nd (mixed proportion is La:Ce:Pr:Nd=4:1:2:3)；The magnetic property testing result of gained sintered magnet: Hcj=25.14-25.61kOe.
Comparative example 2: the interpolation percentage composition of rare earth element micropowder is 0%；The magnetic property testing result of gained sintered magnet: Hcj=22.80-23.26kOe.
The performance of embodiment 7-12 and comparative example 2 collects and is shown in Table 2；
Table 2
| Project | Adding proportion (%) | Addition element | Addition element ratio | Hcj(kOe) |
| Embodiment 7 | 2.8 | Pr:Nd | 3:7 | 26.38-26.70 |
| Embodiment 8 | 2.8 | Ce:Pr | 5:5 | 25.78-26.32 |
| Embodiment 9 | 2.8 | Ce:Pr:Nd | 2:2:6 | 26.08-26.42 |
| Embodiment 10 | 2.8 | Pr:Nd:Dy | 5:2:3 | 27.78-28.12 |
| Embodiment 11 | 2.8 | La: Pr:Nd:Tb | 5:2:2:1 | 26.30-26.74 |
| Embodiment 12 | 2.8 | La:Ce:Pr:Nd | 4:1:2:3 | 25.14-25.61 |
| Comparative example 2 | —— | —— | —— | 22.80-23.26 |
Scheme combination 3:
It is Nd by composition13.4Dy0.4FeRemainingB5.8M4(at%) rare-earth Nd-Fe-B permanent magnetic material alloy, is wherein prepared by technical scheme: carries out dispensing by mentioned component and prepares Nd-Fe-B permanent magnet material alloy with rapid hardening thin slice technique；Use that hydrogen is broken to be added airflow milling mode and crush rare-earth Nd-Fe-B permanent magnetic material alloy, prepare the mean diameter alloy powder in 3.2 μm.
The rare earth element micropowder adding air-flow grinding process acquisition mean diameter in 2.5 μm is broken by hydrogen, prepared various rare earth element micropowders are added in Nd-Fe-B rare earth permanent magnetic material powder by different percentage compositions in pulverizing process, and carries out batch mixing and enable rare earth micropowder to be mixed into uniformly in Nd-Fe-B rare earth permanent magnetic material powder；Mixed powder is compressing 41.5 × 50 × 42.3(mm in the alignment magnetic field of >=1.5T) square blank；Blank is put into high vacuum sintering furnace, sinters 4.0 hours at 1080 DEG C, be tempered 2.2 hours and 510 DEG C of second annealings 4.0 hours 900 DEG C of one-levels, prepared sintered magnet；Take Φ 10 × 10(mm) standard specimen five only carry out magnetism testing.
Embodiment 13: the interpolation percentage composition of rare earth element micropowder is 0%；The magnetic property testing result of gained sintered magnet: Hcj=18.32-18.85kOe.
Embodiment 14: the interpolation percentage composition of rare earth element micropowder is 0.5%, rare earth element used is bis-kinds of admixed finepowders of Pr, Nd (mixed proportion is Pr:Nd=4:6)；The magnetic property testing result of gained sintered magnet: Hcj=18.88-19.30kOe.
Embodiment 15: the interpolation percentage composition of rare earth element micropowder is 1.0%, rare earth element used is bis-kinds of admixed finepowders of Pr, Nd (mixed proportion is Pr:Nd=4:6)；The magnetic property testing result of gained sintered magnet: Hcj=19.38-19.70kOe.
Embodiment 16: the interpolation percentage composition of rare earth element micropowder is 1.5%, rare earth element used is bis-kinds of admixed finepowders of Pr, Nd (mixed proportion is Pr:Nd=4:6)；The magnetic property testing result of gained sintered magnet: Hcj=19.90-20.43kOe.
Embodiment 17: the interpolation percentage composition of rare earth element micropowder is 2.0%, rare earth element used is bis-kinds of admixed finepowders of Pr, Nd (mixed proportion is Pr:Nd=4:6)；The magnetic property testing result of gained sintered magnet: Hcj=20.40-20.86kOe.
Embodiment 18: the interpolation percentage composition of rare earth element micropowder is 2.5%, rare earth element used is bis-kinds of admixed finepowders of Pr, Nd (mixed proportion is Pr:Nd=4:6)；The magnetic property testing result of gained sintered magnet: Hcj=21.02-21.44kOe.
Comparative example 3: be Nd by composition13.2Dy0.8FeRemainingB5.8M3 .58(at%) rare-earth Nd-Fe-B permanent magnetic material alloy；It is not added with rare earth micropowder by upper method and prepares the sample of same specification size, the magnetic property testing result of gained sintered magnet: Hcj=21.22-21.57kOe.
The performance of embodiment 13-18 and comparative example 3 collects and is shown in Table 3；
Table 3
| Project | Adding proportion (%) | Addition element | Addition element ratio | Hcj(kOe) |
| Embodiment 13 | 0 | —— | —— | 18.32-18.85 |
| Embodiment 14 | 0.5 | Pr:Nd | 4:6 | 18.88-19.30 |
| Embodiment 15 | 1.0 | Pr:Nd | 4:6 | 19.38-19.70 |
| Embodiment 16 | 1.5 | Pr:Nd | 4:6 | 19.90-20.43 |
| Embodiment 17 | 2.0 | Pr:Nd | 4:6 | 20.40-20.86 |
| Embodiment 18 | 2.5 | Pr:Nd | 4:6 | 21.02-21.44 |
| Comparative example 3 | 0 | —— | —— | 21.22-21.57 |
Claims (3)
1. one kind low heavy rare earth high-coercive force Sintered NdFeB magnet preparation method, it is characterised in that concretely comprise the following steps:
(1) in terms of atomic number percentage composition, by name component Nd10Dy2Fe82.6B5.3M0.1Dispensing also prepares Nd-Fe-B permanent magnet material alloy with rapid hardening thin slice technique, and wherein M is addition element, including the element of one or more in Ti, V, Cr, Ni, Zn, Ga, Ge, Al, Zr, Nb, Co, Cu, Ag, Sn, W, Pb, Bi and Pd；
(2) use that hydrogen is broken to be added airflow milling mode and crush Nd-Fe-B permanent magnet material alloy, prepare the mean diameter alloy powder in 2.5 μm；
(3) broken the rare earth element micropowder adding air-flow grinding process acquisition mean diameter in 1.5 μm by hydrogen, rare earth element micropowder is Nd micropowder；
(4) after carrying out batch mixing in adding rare earth element micropowder to alloy powder according to the percentage by weight of 0.3%, 1.0%, 2.0%, 3.0% or 5.0%, by mixed powder square blank of compressing 41.5mm × 50mm × 42.3mm in the alignment magnetic field of >=1.6T；
(5) square blank is put into high vacuum sintering furnace, sinter 4.0 hours at 1100 DEG C, be tempered 2 hours and 510 DEG C of second annealings 3.5 hours 890 DEG C of one-levels, prepared sintered magnet.
2. one kind low heavy rare earth high-coercive force Sintered NdFeB magnet preparation method, it is characterised in that concretely comprise the following steps:
(1) in terms of atomic number percentage composition, by name component Nd17Dy1Fe67.5B6.5M8Dispensing also prepares Nd-Fe-B permanent magnet material alloy with rapid hardening thin slice technique, and wherein M is addition element, including the element of one or more in Ti, V, Cr, Ni, Zn, Ga, Ge, Al, Zr, Nb, Co, Cu, Ag, Sn, W, Pb, Bi and Pd；
(2) use that hydrogen is broken to be added airflow milling mode and crush Nd-Fe-B permanent magnet material alloy, prepare the mean diameter alloy powder in 5.0 μm；
(3) broken the rare earth element micropowder adding air-flow grinding process acquisition mean diameter in 3.6 μm by hydrogen, wherein, rare earth element micropowder is bis-kinds of admixed finepowders of Pr, Nd, and mixed proportion is Pr:Nd=3:7；Or rare earth element micropowder is bis-kinds of admixed finepowders of Ce, Pr, mixed proportion is Ce:Pr=5:5；Or rare earth element micropowder is tri-kinds of admixed finepowders of Ce, Pr, Nd, mixed proportion is Ce:Pr:Nd=2:2:6；Or rare earth element micropowder is tri-kinds of admixed finepowders of Pr, Nd, Dy, mixed proportion is Pr:Nd:Dy=5:2:3；Or rare earth element micropowder is tetra-kinds of admixed finepowders of La, Pr, Nd, Tb, mixed proportion is La:Pr:Nd:Tb=5:2:2:1；Or rare earth element micropowder is tetra-kinds of admixed finepowders of La, Ce, Pr, Nd, mixed proportion is La:Ce:Pr:Nd=4:1:2:3；
(4) after carrying out batch mixing in adding rare earth element micropowder to alloy powder according to the percentage by weight of 2.8%, by mixed powder square blank of compressing 41.5mm × 50mm × 42.3mm in the alignment magnetic field of >=2.0T；
(5) square blank is put into high vacuum sintering furnace, sinter 6.0 hours at 1120 DEG C, be tempered 5 hours at 480 DEG C, prepare sintered magnet.
3. one kind low heavy rare earth high-coercive force Sintered NdFeB magnet preparation method, it is characterised in that concretely comprise the following steps:
(1) in terms of atomic number percentage composition, by name component Nd13.4Dy0.4Fe76.4B5.8M4Dispensing also prepares Nd-Fe-B permanent magnet material alloy with rapid hardening thin slice technique, and wherein M is addition element, including the element of one or more in Ti, V, Cr, Ni, Zn, Ga, Ge, Al, Zr, Nb, Co, Cu, Ag, Sn, W, Pb, Bi and Pd；
(2) use that hydrogen is broken to be added airflow milling mode and crush Nd-Fe-B permanent magnet material alloy, prepare the mean diameter alloy powder in 3.2 μm；
(3) broken the rare earth element micropowder adding air-flow grinding process acquisition mean diameter in 2.5 μm by hydrogen, wherein, rare earth element micropowder is bis-kinds of admixed finepowders of Pr, Nd, and mixed proportion is Pr:Nd=4:6；
(4) after carrying out batch mixing in adding rare earth element micropowder to alloy powder according to the percentage by weight of 0.5%, 1.0%, 1.5%, 2.0% or 2.5%, by mixed powder square blank of compressing 41.5mm × 50mm × 42.3mm in the alignment magnetic field of >=1.5T；
(5) square blank is put into high vacuum sintering furnace, sinter 4.0 hours at 1080 DEG C, be tempered 2.2 hours and 510 DEG C of second annealings 4.0 hours 900 DEG C of one-levels, prepared sintered magnet.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410020883.2A CN103824668B (en) | 2014-01-17 | 2014-01-17 | Low-weight rare earth high-coercivity sintered neodymium-iron-boron magnet and production method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410020883.2A CN103824668B (en) | 2014-01-17 | 2014-01-17 | Low-weight rare earth high-coercivity sintered neodymium-iron-boron magnet and production method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103824668A CN103824668A (en) | 2014-05-28 |
| CN103824668B true CN103824668B (en) | 2017-01-11 |
Family
ID=50759672
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410020883.2A Active CN103824668B (en) | 2014-01-17 | 2014-01-17 | Low-weight rare earth high-coercivity sintered neodymium-iron-boron magnet and production method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103824668B (en) |
Families Citing this family (25)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104217832B (en) * | 2014-08-08 | 2017-01-18 | 江苏北斗绿迅新能源科技有限公司 | Composite magnetic material for photovoltaic inverter and preparation method thereof |
| CN104313645B (en) * | 2014-10-28 | 2017-08-08 | 苏州萨伯工业设计有限公司 | The preparation facilities and preparation technology of Mo-bearing granitoid material |
| CN104342721A (en) * | 2014-10-28 | 2015-02-11 | 南京萨伯工业设计研究院有限公司 | Device and process for preparing rare-earth permanent-magnet material |
| CN104308160A (en) * | 2014-10-28 | 2015-01-28 | 南京萨伯工业设计研究院有限公司 | Rare-earth alloy permanent magnet material preparation device and technique |
| CN105225782A (en) * | 2015-07-31 | 2016-01-06 | 浙江东阳东磁稀土有限公司 | A kind of Sintered NdFeB magnet without heavy rare earth and preparation method thereof |
| CN105427994B (en) * | 2015-12-16 | 2018-04-06 | 浙江东阳东磁稀土有限公司 | A kind of corrosion resistant rich lanthanum cerium Sintered NdFeB magnet and manufacture method |
| CN106783129A (en) * | 2016-12-21 | 2017-05-31 | 包头稀土研究院 | The preparation method of low heavy rare earth high-coercive force neodymium iron boron magnetic body |
| CN106783128B (en) * | 2016-12-21 | 2019-06-21 | 包头稀土研究院 | The method for preparing low heavy rare earth high-coercive force neodymium iron boron magnetic body |
| CN106676310A (en) * | 2017-03-07 | 2017-05-17 | 龙岩紫荆创新研究院 | Ag-Cu-Sn grain boundary diffusion additive and NdFeB magnet containing same |
| CN108109799A (en) * | 2017-12-01 | 2018-06-01 | 程桂平 | The preparation method of generator permanent magnet |
| CN108109798A (en) * | 2017-12-01 | 2018-06-01 | 程桂平 | The preparation method of transformer permanent magnet |
| CN108597708A (en) * | 2018-04-12 | 2018-09-28 | 江苏柯普斯磁业有限公司 | A kind of high performance sintered neodymium-iron-boron and manufacturing method |
| CN108831654A (en) * | 2018-07-10 | 2018-11-16 | 浙江英洛华磁业有限公司 | A method of improving properties of sintered ndfeb magnets |
| CN109727742A (en) * | 2019-01-23 | 2019-05-07 | 宁波合盛磁业有限公司 | A kind of low heavy rare earth NdFeB material and preparation method thereof |
| CN110111961B (en) * | 2019-03-12 | 2024-03-12 | 宁波雄海稀土速凝技术有限公司 | Preparation method of high-coercivity neodymium-iron-boron magnet and neodymium-iron-boron magnet |
| CN111883327A (en) * | 2020-06-11 | 2020-11-03 | 包头稀土研究院 | Low-heavy rare earth content high-coercivity permanent magnet and method for preparing composite gold |
| CN114388251A (en) * | 2020-10-16 | 2022-04-22 | 赣州市东磁稀土有限公司 | Rare earth neodymium iron boron magnetic material and compression molding method thereof |
| CN112670047B (en) * | 2020-12-11 | 2023-02-03 | 东莞市嘉达磁电制品有限公司 | High-temperature-resistant neodymium-iron-boron magnet and preparation method thereof |
| CN112768167A (en) * | 2020-12-23 | 2021-05-07 | 宁波科星材料科技有限公司 | Preparation method of neodymium iron boron permanent magnet |
| CN112992461B (en) * | 2021-03-17 | 2023-05-30 | 福建省长汀金龙稀土有限公司 | R-T-B magnet and preparation method thereof |
| CN113571280B (en) * | 2021-07-23 | 2024-02-13 | 包头天和磁材科技股份有限公司 | Neodymium-iron-boron magnet coarse powder auxiliary agent, preparation method and application thereof, and preparation method of magnet |
| CN113782289A (en) * | 2021-08-03 | 2021-12-10 | 宁波可可磁业股份有限公司 | Low (no) heavy rare earth high-coercivity sintered neodymium-iron-boron magnet and preparation method thereof |
| CN114499080B (en) * | 2022-01-28 | 2024-02-23 | 中国科学院赣江创新研究院 | Composite permanent magnet steel and manufacturing method thereof |
| CN114864264B (en) * | 2022-05-16 | 2023-06-30 | 安徽吉华新材料有限公司 | Preparation process of low-weight rare earth high-coercivity rare earth neodymium-iron-boron permanent magnet |
| CN117373767A (en) * | 2022-06-30 | 2024-01-09 | 浙江东阳东磁稀土有限公司 | Modified sintered NdFeB permanent magnet material and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101320609A (en) * | 2008-03-21 | 2008-12-10 | 浙江大学 | Grain boundary phase-reconstructed high-corrosion resistance Sintered NdFeB magnet and preparation method thereof |
| CN101872668A (en) * | 2009-04-23 | 2010-10-27 | 北京中科三环高技术股份有限公司 | Sintered NdFeB rear-earth permanent magnet with fine magnetization characteristic and manufacturing method thereof |
-
2014
- 2014-01-17 CN CN201410020883.2A patent/CN103824668B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101320609A (en) * | 2008-03-21 | 2008-12-10 | 浙江大学 | Grain boundary phase-reconstructed high-corrosion resistance Sintered NdFeB magnet and preparation method thereof |
| CN101872668A (en) * | 2009-04-23 | 2010-10-27 | 北京中科三环高技术股份有限公司 | Sintered NdFeB rear-earth permanent magnet with fine magnetization characteristic and manufacturing method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103824668A (en) | 2014-05-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103824668B (en) | Low-weight rare earth high-coercivity sintered neodymium-iron-boron magnet and production method thereof | |
| CN106128673B (en) | A kind of Sintered NdFeB magnet and preparation method thereof | |
| CN101364465B (en) | Permanent magnetic RE material and preparation thereof | |
| CN102956336B (en) | A kind of method preparing the sintered Nd-Fe-B permanent magnetic material of compound interpolation gadolinium, holmium and yttrium | |
| CN100394518C (en) | Method for preparing high coercive force sintering rare-earth-iron-p permanent magnetic material | |
| CN101315825B (en) | Fire resistant permanent magnet alloy and manufacturing method thereof | |
| WO2014101247A1 (en) | Method for preparing sintered neodymium-iron-boron magnet | |
| CN104575920B (en) | Rare-earth permanent magnet and preparation method thereof | |
| CN109585113A (en) | A kind of preparation method of Sintered NdFeB magnet | |
| CN103956244A (en) | Preparation method for high-coercivity sintered neodymium-iron-boron | |
| CN105427994A (en) | Corrosion-resistant lanthanum-cerium-rich sintered neodymium iron boron magnet and preparation method | |
| CN107958760B (en) | Rare earth permanent magnetic material and preparation method thereof | |
| CN112086255A (en) | High-coercivity and high-temperature-resistant sintered neodymium-iron-boron magnet and preparation method thereof | |
| CN106409458B (en) | A kind of motor composite permanent-magnetic material and preparation method thereof | |
| CN113838622A (en) | High-coercivity sintered neodymium-iron-boron magnet and preparation method thereof | |
| CN109585109A (en) | A kind of mischmetal permanent magnet and preparation method thereof | |
| CN112712986B (en) | Low-temperature coefficient Sm2Co17Molded sintered magnet and method for producing same | |
| CN110853857B (en) | Alloy containing Ho and/or Gd, rare earth permanent magnet, raw materials, preparation method and application | |
| CN116612956A (en) | Cerium-containing neodymium-iron-boron magnet with core-shell structure and preparation method and application thereof | |
| EP4156213A1 (en) | A high temperature resistant magnet and a method thereof | |
| KR102513836B1 (en) | Method of manufacturing multiple main phase magnet and multiple main phase magnet therefrom | |
| CN108831648A (en) | The method of spray drying preparation performance Nd Fe B sintered magnet | |
| CN103740959A (en) | Alloy additive for preparing double high neodymium-iron-boron material and application method thereof | |
| CN114823027A (en) | High-boron neodymium-iron-boron permanent magnet material and preparation method thereof | |
| CN111883327A (en) | Low-heavy rare earth content high-coercivity permanent magnet and method for preparing composite gold |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |