CN105321645A - Nanocrystalline thermal deformation rare-earth permanent magnet material with high coercivity and preparation method of nanocrystalline thermal deformation rare-earth permanent magnet material - Google Patents
Nanocrystalline thermal deformation rare-earth permanent magnet material with high coercivity and preparation method of nanocrystalline thermal deformation rare-earth permanent magnet material Download PDFInfo
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- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 44
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000000463 material Substances 0.000 title abstract description 7
- 239000000654 additive Substances 0.000 claims abstract description 50
- 230000000996 additive effect Effects 0.000 claims abstract description 46
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 20
- 239000000956 alloy Substances 0.000 claims abstract description 20
- 239000000843 powder Substances 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 17
- 150000004767 nitrides Chemical class 0.000 claims abstract description 5
- 239000000696 magnetic material Substances 0.000 claims description 36
- 238000002156 mixing Methods 0.000 claims description 23
- 238000003856 thermoforming Methods 0.000 claims description 11
- 230000008569 process Effects 0.000 claims description 10
- 230000001681 protective effect Effects 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000011159 matrix material Substances 0.000 claims description 8
- 229910052684 Cerium Inorganic materials 0.000 claims description 6
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 6
- 229910052779 Neodymium Inorganic materials 0.000 claims description 6
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 6
- 229910052771 Terbium Inorganic materials 0.000 claims description 6
- 229910052746 lanthanum Inorganic materials 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 5
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 238000009826 distribution Methods 0.000 claims description 4
- 230000000737 periodic effect Effects 0.000 claims description 4
- 238000010791 quenching Methods 0.000 claims description 4
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- 239000000126 substance Substances 0.000 claims description 4
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- 229910052733 gallium Inorganic materials 0.000 claims description 3
- 238000009413 insulation Methods 0.000 claims description 3
- 230000014759 maintenance of location Effects 0.000 claims description 3
- 238000002844 melting Methods 0.000 abstract description 5
- 230000008018 melting Effects 0.000 abstract description 5
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Abstract
The invention relates to a preparation method of a nanocrystalline thermal deformation rare-earth permanent magnet material with high coercivity. The method comprises the steps as follows: (1) alloy powder and a high melting point additive are respectively provided, wherein the high melting point additive is at least one of refractory carbide, nitride and oxide; (2) the alloy powder and the high melting point additive are mixed evenly to obtain mixed magnetic powder, wherein the mass ratio of the high melting point additive in the mixed magnetic powder is greater than or equal to 0.01% and is smaller than or equal to 10%; and (3) hot press molding and thermal deformation molding are sequentially carried out on the mixed magnetic powder, so as to obtain the nanocrystalline thermal deformation rare-earth permanent magnet material with high coercivity. The invention further provides the nanocrystalline thermal deformation rare-earth permanent magnet material with high coercivity.
Description
Technical field
The present invention relates to rare earth permanent magnet technical field, particularly relate to a kind of have excellent magnetic can rare earth permanent-magnetic material and preparation method thereof.
Background technology
The permanent magnetic material that rare earth permanent-magnetic material is the intermetallic compound that formed with thulium and magnesium-yttrium-transition metal is matrix.Nd-Fe-B permanent magnet (also claiming NdFeB permanent magnet) is the permanent magnetic material that current magnetic property is the highest.Nd-Fe-B permanent magnet is widely used in social production, life and the field such as national defence and space flight, becomes the critical function material supporting social progress.
Thermal deformation method and sintering process is mainly contained in the preparation method of NdFeB permanent magnetic material.Compared with sintering process, thermal deformation method has that rare-earth usage is low, corrosion resistance good and be easy to realize the advantages such as newly net forming.The permanent magnetic material that thermal deformation obtains is primarily of Nd
2fe
14b principal phase and rich-Nd phase composition.The magnetic property of heat distortion magnet, especially remanent magnetism and magnetic energy product, depend on the degree of main phase grain along c-axis orientation.Rich-Nd phase, except possessing at crystal grain wetting in deformation process, modifies the effect of grain boundary, the obvious characteristic of self nonferromagnetic can also be utilized to reduce the alternate exchange-coupling interaction of Hard Magnetic, thus improve coercive force.
The coercive force that Fuerst and the Brewer research discovery nonmagnetic Zn of grain boundaries and the buffer action of Cu element partly can improve magnet (refers to FuerstCD, BrewerEG.Enhancedcoercivitiesindie-upsetNd-Fe-Bmagnetswi thdiffusion-alloyedadditives (Zn, Cu, andNi) .AppliedPhysicsLetters.1990,56:2252-2254.).The advantage that the people such as K.Hono utilize three-dimensional atom probe to characterize at microregion element, have studied heat distortion magnet crystal boundary fine structure, think that heat distortion magnet grain boundaries contains the Fe of high level, there is stronger ferromagnetism, and utilize grain boundary decision technology to introduce nonmagnetic elements, reduce the ferromagnetism of Grain-Boundary Phase, form stronger domain wall pinning effect, coercive force is significantly promoted and (refers to LiuJ, Sepehri-AminH, OhkuboT, HiokiK, HattoriA, SchreflT, andHonoK.EffectOfNdcontentonthemicrostructureandcoercivi tyofhot-deformedNd-Fe-Bpermanentmagnets.ActaMaterialia, 2013, 61:5387-5399, Sepehri-AminH, OhkuboT, NagashimaS, YanoM, ShojiT, KatoA, SchreflT, andHonoK.High-coercivityultrafine-grainedanisotropicNd-F e-BmagnetsprocessedbyhotdeformationandtheNd-Cugrainbound arydiffusionprocess [J] .ActaMaterialia, 2013,61:6622-6634.).
But the rich-Nd phase added due to grain boundary decision increases, make the Nd of magnet
2fe
14b principal phase reduces, although the magnet that thermal deformation technique obtains has high coercive force, remanent magnetism reduces obviously, causes the comprehensive magnetic of magnet energy poor.
Summary of the invention
In view of this, necessaryly provide a kind of there is rare earth permanent-magnetic material of magnetic property excellence and preparation method thereof.
The invention provides the preparation method of the nanocrystalline thermal deformation rare earth permanent-magnetic material of a kind of high-coercive force, it comprises the following steps:
(1) provide alloy powder and high-melting-point additive respectively, wherein said high-melting-point additive is at least one in the carbide of infusibility, nitride, oxide;
(2) evenly obtained mixing magnetic with described high-melting-point additives mixed by described alloy powder, wherein, the mass ratio described in described mixing magnetic shared by high-melting-point additive is more than or equal to 0.01% and is less than or equal to 10%;
(3) described mixing magnetic is carried out hot-forming and thermoforming successively, obtain the nanocrystalline thermal deformation rare earth permanent-magnetic material of high-coercive force.
Wherein, described high-melting-point additive is WC, SiC, BN, ZrO
2, Al
2o
3, SiO
2in at least one.
Wherein, the mass ratio described in described mixing magnetic shared by high-melting-point additive is 0.1% ~ 5%.
Wherein, the chemical formula of described alloy powder is Re by mass percentage
xfe
100-x-y-zm
yb
z, wherein Re is one or more in Nd, Pr, Dy, Tb, La, Ce, and M is one or more in Al, Co, Cu, Ga, 20≤x≤40,0≤y≤10,0.7≤z≤1.5.
Wherein, the particle diameter of described high-melting-point additive is 10 nanometer ~ 1 micron.
Wherein, step (3) in described mixing magnetic is carried out hot-forming being specially: mixing magnetic is put into the first mould; in vacuum environment or protective atmosphere, the first temperature is heated to mixing magnetic; and the first pressure is applied to the first mould; obtain hot-pressed magnets; wherein, described first temperature is 600 DEG C ~ 750 DEG C, and described first pressure is 100MPa ~ 250MPa.
Wherein, the vacuum degree of described vacuum environment is not less than 1 × 10
-2pa.
Wherein, step (3) described in thermoforming be that described hot-pressed magnets is put into the second mould; in vacuum environment or protective atmosphere, the second temperature is heated to described hot-pressed magnets; again the second pressure is applied to hot-pressed magnets; described hot-pressed magnets is carried out distortion that degree of deformation is 30% ~ 95%; obtain heat distortion magnet, wherein said second temperature is 750 DEG C ~ 900 DEG C, and described second pressure is 30MPa ~ 100MPa.
Wherein, step (3) in after thermoforming step, also comprise the step of temper; the process of described temper is specially: in vacuum environment or protective atmosphere, described heat distortion magnet be heated to the 3rd temperature and be incubated; and terminate rear quenching chilling in insulation; wherein the 3rd temperature is 500 DEG C ~ 800 DEG C; temperature retention time is 1 hour ~ 10 hours, during heating heating rate be 5 DEG C/min ~ 20 DEG C/min.
The present invention also provides a kind of high-coercive force adopting above-mentioned preparation method to obtain nanocrystalline thermal deformation rare earth permanent-magnetic material, and it is by matrix phase Re
2fe
14b, Grain-Boundary Phase and high-melting-point infusibility additive form, and wherein Re is one or more in Nd, Pr, Dy, Tb, La, Ce, matrix phase Re
2fe
14b is flaky nanocrystalline, and the length of described flaky nanocrystalline is 200 nanometer ~ 500 nanometers, and thickness is 50 nanometer ~ 100 nanometers, and described high-melting-point infusibility additive is ribbon periodic distribution.
Compared with prior art, nanocrystalline thermal deformation rare earth permanent-magnetic material of high-coercive force provided by the invention and preparation method thereof has the following advantages: first, due to the addition of infusibility high-melting-point additive, it not easily melts in hot pressing and thermal deformation process, this high-melting-point additive is uniformly distributed, and thus can suppress coarse grain zone and Re
2fe
14growing up of B crystal grain, makes the Re formed
2fe
14the size of B crystal grain is relatively little (being less than 1 micron), i.e. Re
2fe
14the size of B crystal grain close to single-domain critical size, the thus easier stabilisation of magnetic domain, and generation or the expansion of reverse domain occur hardly, this is conducive to improving coercive force; The second, the mass ratio shared by described high-melting-point additive is more than or equal to 0.01 and is less than or equal to 10%, thus can not cause serious harm to the remanent magnetism of the magnet obtained, and makes its coercive force obtain larger raising simultaneously.This preparation method is easy to operation and industrialization.The comprehensive magnetic of the nanocrystalline thermal deformation rare earth permanent-magnetic material of the described high-coercive force obtained can be excellent.
Accompanying drawing explanation
Fig. 1 is ESEM (SEM) photo of the nanocrystalline thermal deformation rare earth permanent-magnetic material of high-coercive force that embodiment 2 obtains.
Fig. 2 is backscattered electron imagine (BSE) photo of the nanocrystalline thermal deformation rare earth permanent-magnetic material of high-coercive force that embodiment 2 obtains.
Following specific embodiment will further illustrate the present invention in conjunction with above-mentioned accompanying drawing.
Embodiment
Below will be described further nanocrystalline thermal deformation rare earth permanent-magnetic material of high-coercive force provided by the invention and preparation method thereof.
The invention provides the preparation method of the nanocrystalline thermal deformation rare earth permanent-magnetic material of a kind of high-coercive force, it comprises following step:
S1, provides alloy powder and high-melting-point additive respectively, and wherein said high-melting-point additive is at least one in the carbide of infusibility, nitride, oxide;
S2, evenly obtains mixing magnetic with described high-melting-point additives mixed by described alloy powder, and wherein, the mass ratio described in described mixing magnetic shared by high-melting-point additive is more than or equal to 0.01 and is less than or equal to 10%; And
S3, carries out hot-forming and thermoforming successively by described mixing magnetic, obtains the nanocrystalline thermal deformation rare earth permanent-magnetic material of high-coercive force.
In step sl, the chemical formula of described alloy powder is Re by mass percentage
xfe
100-x-y-zm
yb
z, wherein Re is one or more in Nd, Pr, Dy, Tb, La, Ce, and M is one or more in Al, Co, Cu, Ga, 20≤x≤40,0≤y≤10,0.7≤z≤1.5.Described alloy powder can be commercially available product, also can be homemade.Described alloy powder prepares by following method:
A () is prepared burden according to the ratio of element each in alloy powder;
B (), also carries out melting under an inert atmosphere by the raw material prepared mixing, obtains foundry alloy;
C (), is injected into water-cooled running roller and carries out fast quenching, make rapid tempering belt by foundry alloy; And
D (), carries out Mechanical Crushing by described rapid tempering belt, obtain alloy powder.
Described high-melting-point additive is at least one in the carbide of infusibility, nitride, oxide.Concrete, described high-melting-point additive is WC, SiC, BN, ZrO
2, Al
2o
3, SiO
2in at least one.The particle diameter of described high-melting-point additive is 10 nanometer ~ 1 micron.Consider that the particle diameter of additive is less, more easily spread, and do not hinder stream to become, do not affect the formation of texture, the particle diameter of described high-melting-point additive is preferably 10 nanometer ~ 100 nanometers.By adding high-melting-point additive, and coarse grain zone and Re can be suppressed in follow-up thermoforming process
2fe
14growing up of B crystal grain, makes the Re obtained
2fe
14b crystallite dimension is less, thus the coercive force of the nanocrystalline thermal deformation rare earth permanent-magnetic material of the high-coercive force obtained is excellent.
In step s 2, by by described alloy powder and described high-melting-point additives mixed, described high-melting-point additive is uniformly distributed in described alloy powder.Described mixing can be carried out in three-dimensional material mixer.Mass ratio described in described mixing magnetic shared by high-melting-point additive is preferably 0.1% ~ 5%, to avoid when the mass ratio shared by described high-melting-point additive is too high, the stream of magnet can be hindered to become, and then affect the formation of texture, and high-melting-point additive is namagnetic substance, the too high meeting of shared mass ratio makes remanent magnetism reduce; And mass ratio shared by described high-melting-point additive too low time, skewness, does not have the effect of suppression.
In step s3, loose mixing magnetic can be formed the hot-pressed magnets with certain density and intensity by hot press forming technology.In described thermoforming technique, hot-pressed magnets under high moderate pressure effect, Re
2t
14b phase crystal grain, by dissolving-mass transfer-recrystallization process, forms the sheet flaky nanocrystalline along the consistent orientation of easy magnetizing axis c-axis, thus the nanocrystalline thermal deformation rare earth permanent-magnetic material of the high-coercive force obtained has excellent magnetic property.
Concrete, to be describedly hot-formingly specially: mixing magnetic is put into the first mould, is not less than 1 × 10 at protective atmosphere or vacuum degree
-2be heated to the first temperature to mixing magnetic in the vacuum environment of Pa, and apply the first pressure to the first mould, obtain hot-pressed magnets, wherein, described first temperature is 600 DEG C ~ 750 DEG C, and described first pressure is 100MPa ~ 250MPa.Preferably, described first temperature is 650 DEG C ~ 680 DEG C, and described first pressure is 170MPa ~ 220MPa.
Described thermoforming is that hot-pressed magnets is put into the second mould; in vacuum environment or protective atmosphere, the second temperature is heated to described hot-pressed magnets; again the second pressure is applied to hot-pressed magnets; described hot-pressed magnets is carried out distortion that degree of deformation is 30% ~ 95%; obtain heat distortion magnet; wherein said second temperature is 750 DEG C ~ 900 DEG C, and described second pressure is 30MPa ~ 100MPa.Preferably, described second temperature is 800 DEG C ~ 850 DEG C, and described second pressure is 30MPa ~ 70MPa.
The step of a temper is also comprised after thermoforming step.The process of described temper is specially: in vacuum environment or protective atmosphere, described heat distortion magnet be heated to the 3rd temperature and be incubated; and terminate rear quenching chilling in insulation; wherein the 3rd temperature is 500 DEG C ~ 800 DEG C; temperature retention time is 1 hour ~ 10 hours, during heating heating rate be 5 DEG C/min ~ 20 DEG C/min.It should be noted that, in the process of temper, the atom in described heat distortion magnet spreads gradually, and composition becomes branch's generation change to a certain degree mutually with crystal grain, but grain morphology and size do not change substantially.
The present invention also provides a kind of high-coercive force adopting above-mentioned preparation method to obtain nanocrystalline thermal deformation rare earth permanent-magnetic material, and it is by matrix phase Re
2fe
14b, Grain-Boundary Phase and high-melting-point infusibility additive form, and wherein Re is one or more in Nd, Pr, Dy, Tb, La, Ce.Matrix phase Re
2fe
14b is flaky nanocrystalline.Described high-melting-point infusibility additive is ribbon periodic distribution.The length of described flaky nanocrystalline is 200 nanometer ~ 500 nanometers, and thickness is 50 nanometer ~ 100 nanometers.
Nanocrystalline thermal deformation rare earth permanent-magnetic material of high-coercive force provided by the invention and preparation method thereof has the following advantages: first, due to the addition of infusibility high-melting-point additive, it not easily melts in hot pressing and thermal deformation process, this high-melting-point additive is uniformly distributed, and thus can suppress coarse grain zone and Re
2fe
14growing up of B crystal grain, makes the Re formed
2fe
14the size of B crystal grain is relatively little (being less than 1 micron), i.e. Re
2fe
14the size of B crystal grain close to single-domain critical size, the thus easier stabilisation of magnetic domain, and generation or the expansion of reverse domain occur hardly, this is conducive to improving coercive force; The second, the mass ratio shared by described high-melting-point additive is more than or equal to 0.01 and is less than or equal to 10%, thus can not cause serious harm to the remanent magnetism of the magnet obtained, and makes its coercive force obtain larger raising simultaneously.This preparation method is easy to operation and industrialization.The comprehensive magnetic of the nanocrystalline thermal deformation rare earth permanent-magnetic material of the described high-coercive force obtained can be excellent.
Below, will further illustrate in conjunction with specific embodiments.
Embodiment 1 to 9
Be Nd at composition
30ga
0.5fe
bal.co
4b
1alloy powder in add the high-melting-point additive that granularity is 10 nanometer-50 nanometers respectively, and to mix.Addition and the kind of high-melting-point additive refer to table 1.
By mixed powder induction heating in vacuum environment, when temperature is upgraded to 200 DEG C, start to apply the first pressure to the first mould, and maximum temperature controls to be 670 DEG C, obtain hot-pressed magnets, the time being wherein raised to maximum temperature from room temperature is 5 minutes ~ 6 minutes, and the first pressure is 150MPa, and in hot pressing, vacuum degree is not less than 5 × 10
-2pa.
Hot pressing blank is put into the second mould that diameter is larger, in argon gas atmosphere, induction heating is carried out to hot-pressed magnets, described hot-pressed magnets is carried out distortion that degree of deformation is 70%.After temperature reaches maximum temperature 830 DEG C, be incubated 1 minute, then apply the second pressure, obtain heat distortion magnet.Wherein, the time being raised to maximum temperature from room temperature is 6 minutes ~ 7 minutes, and the second pressure is 50MPa.
At room temperature carry out test magnetic property to the heat distortion magnet obtained, test result is in table 1.Wherein, B
rrepresent remanent magnetism, unit is kGs; H
cjrepresent coercive force, unit is kOe; (BH)
mrepresent magnetic energy product, unit is MGOe.
Embodiment 10 to 14
Respectively the heat distortion magnet of embodiment 1, embodiment 2, embodiment 3, embodiment 5 and embodiment 6 is placed in vacuum environment, 700 DEG C of tempering 2 hours.After cooling, measure the magnetic property of magnet according to the mode of embodiment 1, the results are shown in Table 2.
Comparative example
This preparation method is substantially the same manner as Example 1, and difference is, does not add high-melting-point additive.
At room temperature carry out test magnetic property to the heat distortion magnet obtained, test result is in table 1.
The magnetic property of the nanocrystalline thermal deformation rare earth permanent-magnetic material of high-coercive force of table 1 embodiment 1 ~ 9, comparative example
As can be seen from Table 1, a certain amount of dystectic carbide powder is added helpful, especially obvious with embodiment 2 effect for the coercive force promoting rare-earth permanent magnet.For analyzing the microscopic pattern of embodiment 2 rare-earth permanent magnet better, also SEM (see Fig. 1) and BSE (see Fig. 2) being carried out to the rare-earth permanent magnet of embodiment 2 and analyzing.As shown in Figure 1, rare-earth permanent magnet is by Nd
2fe
14b matrix phase forms, Nd
2fe
14b phase crystal grain mostly is flaky nanocrystalline, the equiax crystal that yet existence part is not out of shape.Described flaky nanocrystalline is of a size of nanoscale, and its length is about 250 ~ 400nm, and thickness is about 50 ~ 100nm.As seen from Figure 2, WC is ribbon periodic distribution, and WC is mainly distributed in bar band gap, thus inhibits coarse grain zone and Nd
2fe
14the growth of B phase crystal grain, and then improve the coercive force of rare-earth permanent magnet.
The magnetic property of the nanocrystalline thermal deformation rare earth permanent-magnetic material of high-coercive force of table 2 embodiment 10 ~ 14
From table 1 and table 2, after temper time, the magnetic property of the magnet of embodiment 10 ~ 14 all improves, and especially obvious with embodiment 10, embodiment 11, its remanent magnetism Br and coercive force have certain increase.This is because temper accelerates the diffusion of high-melting-point additive, and they are distributed more uniformly, thus better suppress coarse grain zone and Re
2fe
14growing up of B crystal grain.
The explanation of above embodiment just understands method of the present invention and core concept thereof for helping.It should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention, can also carry out some improvement and modification to the present invention, these improve and modify and also fall in the protection range of the claims in the present invention.
To the above-mentioned explanation of the disclosed embodiments, professional and technical personnel in the field are realized or uses the present invention.To be apparent for those skilled in the art to the multiple amendment of these embodiments, General Principle as defined herein can without departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention can not be restricted to these embodiments shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (10)
1. a preparation method for the nanocrystalline thermal deformation rare earth permanent-magnetic material of high-coercive force, it comprises the following steps:
(1) provide alloy powder and high-melting-point additive respectively, wherein said high-melting-point additive is at least one in the carbide of infusibility, nitride, oxide;
(2) evenly obtained mixing magnetic with described high-melting-point additives mixed by described alloy powder, wherein, the mass ratio described in described mixing magnetic shared by high-melting-point additive is more than or equal to 0.01% and is less than or equal to 10%;
(3) described mixing magnetic is carried out hot-forming and thermoforming successively, obtain the nanocrystalline thermal deformation rare earth permanent-magnetic material of high-coercive force.
2. the preparation method of the nanocrystalline thermal deformation rare earth permanent-magnetic material of high-coercive force as claimed in claim 1, it is characterized in that, described high-melting-point additive is WC, SiC, BN, ZrO
2, Al
2o
3, SiO
2in at least one.
3. the preparation method of the nanocrystalline thermal deformation rare earth permanent-magnetic material of high-coercive force as claimed in claim 1, it is characterized in that, the mass ratio described in described mixing magnetic shared by high-melting-point additive is 0.1% ~ 5%.
4. the preparation method of the nanocrystalline thermal deformation rare earth permanent-magnetic material of high-coercive force as claimed in claim 1, it is characterized in that, the chemical formula of described alloy powder is Re by mass percentage
xfe
100-x-y-zm
yb
z, wherein Re is one or more in Nd, Pr, Dy, Tb, La, Ce, and M is one or more in Al, Co, Cu, Ga, 20≤x≤40,0≤y≤10,0.7≤z≤1.5.
5. the preparation method of the nanocrystalline thermal deformation rare earth permanent-magnetic material of high-coercive force as claimed in claim 1, it is characterized in that, the particle diameter of described high-melting-point additive is 10 nanometer ~ 1 micron.
6. the preparation method of the nanocrystalline thermal deformation rare earth permanent-magnetic material of high-coercive force as claimed in claim 1; it is characterized in that; step (3) in described mixing magnetic is carried out hot-forming being specially: mixing magnetic is put into the first mould; in vacuum environment or protective atmosphere, the first temperature is heated to mixing magnetic; and the first pressure is applied to the first mould, obtain hot-pressed magnets, wherein; described first temperature is 600 DEG C ~ 750 DEG C, and described first pressure is 100MPa ~ 250MPa.
7. the preparation method of the nanocrystalline thermal deformation rare earth permanent-magnetic material of high-coercive force as claimed in claim 6, it is characterized in that, the vacuum degree of described vacuum environment is not less than 1 × 10
-2pa.
8. the preparation method of the nanocrystalline thermal deformation rare earth permanent-magnetic material of high-coercive force as claimed in claim 6; it is characterized in that; step (3) described in thermoforming be that described hot-pressed magnets is put into the second mould; in vacuum environment or protective atmosphere, the second temperature is heated to described hot-pressed magnets; again the second pressure is applied to hot-pressed magnets; described hot-pressed magnets is carried out distortion that degree of deformation is 30% ~ 95%; obtain heat distortion magnet; wherein said second temperature is 750 DEG C ~ 900 DEG C, and described second pressure is 30MPa ~ 100MPa.
9. the preparation method of the nanocrystalline thermal deformation rare earth permanent-magnetic material of high-coercive force as claimed in claim 1; it is characterized in that; step (3) in after thermoforming step, also comprise the step of temper; the process of described temper is specially: in vacuum environment or protective atmosphere, described heat distortion magnet be heated to the 3rd temperature and be incubated; and terminate rear quenching chilling in insulation; wherein the 3rd temperature is 500 DEG C ~ 800 DEG C; temperature retention time is 1 hour ~ 10 hours, during heating heating rate be 5 DEG C/min ~ 20 DEG C/min.
10. adopt the nanocrystalline thermal deformation rare earth permanent-magnetic material of high-coercive force that preparation method obtains as described in any one of claim 1 ~ 9, it is by matrix phase Re
2fe
14b, Grain-Boundary Phase and high-melting-point infusibility additive form, and wherein Re is one or more in Nd, Pr, Dy, Tb, La, Ce, matrix phase Re
2fe
14b is flaky nanocrystalline, and the length of described flaky nanocrystalline is 200 nanometer ~ 500 nanometers, and thickness is 50 nanometer ~ 100 nanometers, and described high-melting-point infusibility additive is ribbon periodic distribution.
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|---|---|---|---|
| CN201510834685.4A CN105321645B (en) | 2015-11-25 | 2015-11-25 | High-coercivity nanocrystalline thermal deformation rare earth permanent magnet material and preparation method thereof |
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| CN107557551A (en) * | 2017-10-27 | 2018-01-09 | 华北理工大学 | A kind of preparation method of samarium iron nitrogen series permanent magnetic material |
| CN109473248A (en) * | 2018-11-21 | 2019-03-15 | 重庆科技学院 | A kind of NdCeFeB anisotropic permanent magnet and preparation method thereof |
| CN110534280A (en) * | 2019-09-23 | 2019-12-03 | 广西科技大学 | A kind of preparation method of the performance Nd Fe B sintered magnet based on crystal boundary addition |
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| CN105702405A (en) * | 2016-04-29 | 2016-06-22 | 湖北工程学院 | Nano composite NdFeB (neodymium iron boron) permanent magnetic material and preparation method |
| CN106252011A (en) * | 2016-08-29 | 2016-12-21 | 浙江东阳东磁稀土有限公司 | The compound interpolation of a kind of Grain-Boundary Phase improves the coercitive method of sintered NdFeB |
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| CN114203430A (en) * | 2016-09-23 | 2022-03-18 | 日东电工株式会社 | Sintered body for forming rare earth sintered magnet and method for producing same |
| CN107464647A (en) * | 2017-09-29 | 2017-12-12 | 中国科学院宁波材料技术与工程研究所 | High microcosmic uniformity thermal deformation nanocrystalline rare-earth permanent magnetic material and preparation method thereof |
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| CN107557551A (en) * | 2017-10-27 | 2018-01-09 | 华北理工大学 | A kind of preparation method of samarium iron nitrogen series permanent magnetic material |
| CN107557551B (en) * | 2017-10-27 | 2019-08-23 | 华北理工大学 | A kind of preparation method of samarium iron nitrogen series permanent magnetic material |
| CN109473248A (en) * | 2018-11-21 | 2019-03-15 | 重庆科技学院 | A kind of NdCeFeB anisotropic permanent magnet and preparation method thereof |
| CN110534280A (en) * | 2019-09-23 | 2019-12-03 | 广西科技大学 | A kind of preparation method of the performance Nd Fe B sintered magnet based on crystal boundary addition |
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