CN104051104B - Nd-Fe-B permanent magnetic magnet and preparation method thereof - Google Patents
Nd-Fe-B permanent magnetic magnet and preparation method thereof Download PDFInfo
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- CN104051104B CN104051104B CN201410251254.0A CN201410251254A CN104051104B CN 104051104 B CN104051104 B CN 104051104B CN 201410251254 A CN201410251254 A CN 201410251254A CN 104051104 B CN104051104 B CN 104051104B
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- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 145
- -1 rare earth compound Chemical class 0.000 claims abstract description 135
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- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical group [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 claims description 66
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Abstract
The invention provides a kind of Nd-Fe-B permanent magnetic magnet and preparation method thereof, the Nd-Fe-B permanent magnetic magnet includes neodymium iron boron magnetic body and rare earth compound；The Nd-Fe-B permanent magnetic magnet is in layer structure；Composition layer containing the rare earth compound is the first composition layer, and it is the second composition layer, the first composition layer and the second composition alternately laminated arrangement of layer not contain the composition layer of rare earth compound；Rare earth compound is evenly distributed in the neodymium iron boron magnetic body described in the first composition layer.Nd-Fe-B permanent magnetic magnet of the invention forms multilayer rare earth compound barrier layer in the middle of neodymium iron boron magnetic body, magnet resistive rate is capable of achieving to increase substantially, rare earth compound is concentrated on into intermediate course simultaneously, influence of dystectic rare earth compound to adjacent two layers magnet structure is reduced.It is achieved thereby that in the case where magnet magnetic property is not decreased obviously, the resistivity of Nd-Fe-B permanent magnetic magnet is increased substantially.
Description
Technical field
The present invention relates to material manufacture field, more particularly to a kind of Nd-Fe-B permanent magnetic magnet and preparation method thereof.
Background technology
As third generation rare earth permanent-magnetic material, with neodymium iron boron (Nd2Fe14B) rare earth of phase structure and its similar structures is forever
Magnetic material is applied in hard disc of computer, Magnetic resonance imaging, hybrid vehicle, wind-power electricity generation etc. rapidly with its excellent performance
Field.At present, the neodymium iron boron yield of 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.Such as, average each hybrid vehicle needs 2-3kg neodymium iron boron based permanent magnetic materials,
And need 0.5-1t Nd-Fe-B permanent magnets per megawatt wind driven generator group.
Hot pressing/thermal deformation technique is to prepare high-performance, one of important method of theoretical density nanocrystalline rare-earth permanent magnetic material.By
There is nanocrystalline structure in magnet, therefore with preferable corrosion resistance, inoxidizability, become with good plasticity at high temperature
Shape ability；The preparation technology flow of hot-pressed magnets is short, low cost.
The Curie temperature of nanocrystalline neodymium iron boron permanent magnet prepared by hot pressing/thermal deformation technique, temperature coefficient are higher, high temperature
Under the conditions of when using the magnetic loss of energy it is larger.When motor, the relatively low hot pressing neodymium iron boron magnetic body of resistivity is easily because of vortex
Effect and produce amount of heat, if radiating not in time, can make magnet bulk temperature rise, so as to have a strong impact on the magnetic of magnet
Can, or even irreversible infringement can be caused to the magnetic property of magnet.
Current Domestic is outer to focus primarily upon a certain amount of electricity high of addition on improving the method for neodymium-iron-boron body resistivity
Resistance rate material.It is most common or by rare earth fluoride/rare earth oxide powder particle directly with magnetic be blended, carry out hot pressing/
Thermal deformation is made magnet, but be directly scattered in the non-magnetic phases such as rare earth fluoride/oxide in whole magnet by the method, easily
Defect is produced inside magnet, the influence to magnet magnetic property is very big, therefore magnetic property declines quickly.Also the document report having,
Directly magnetic is pre-processed, using the methods such as chemical deposition, sputter magnetic surface coating high resistivity SiO2 or
Rare earth fluoride, the resistivity of obtained magnet is of a relatively high, and magnetic property also has certain amplitude to decline, but mass disposal magnetic
Powder, it is not only less efficient, and high cost.Comprehensively apparently, the method for magnetic mixing or surface treatment can destroy magnetic
Hot-fluid becomes alignment capability, and the magnet degree of orientation is significantly reduced in thermal deformation process, reduces remanent magnetism.
The content of the invention
Based on above mentioned problem, the invention provides a kind of Nd-Fe-B permanent magnetic magnet and preparation method thereof, it can be significantly improved
The resistivity of Nd-Fe-B permanent magnetic magnet.
To reach above-mentioned technical purpose, the present invention is adopted the following technical scheme that：
A kind of Nd-Fe-B permanent magnetic magnet, including neodymium iron boron magnetic body and rare earth compound；The Nd-Fe-B permanent magnetic magnet is in layer
Shape structure；Composition layer containing the rare earth compound is the first composition layer, does not contain the composition of rare earth compound
Layer is the second composition layer, the first composition layer and the second composition alternately laminated arrangement of layer；
Rare earth compound is evenly distributed in the neodymium iron boron magnetic body described in the first composition layer.
Wherein in one embodiment, the rare earth compound is rare earth fluoride or rare earth oxide.
Wherein in one embodiment, the weight/mass percentage composition of rare earth compound is described in the Nd-Fe-B permanent magnetic magnet
0.0001% to 5.29%.
Wherein in one embodiment, the weight/mass percentage composition of rare earth compound is described in the first composition layer
0.001% to 63.8%.
Wherein in one embodiment, the rare earth compound in the first composition layer is in the form of sheets.
Wherein in one embodiment, it is described second composition layer quantity than described first composition layer quantity more than one layer.
Wherein in one embodiment, the first composition layer is at least one layer, and the second composition layer is at least two-layer,
The thickness of all first composition layers is equal, and the thickness of all second composition layers is equal.
Wherein in one embodiment, the rare earth element in described rare earth compound is neodymium, dysprosium, terbium or praseodymium.
The present invention also provides a kind of preparation method of Nd-Fe-B permanent magnetic magnet, comprises the following steps：
(1) mixture is configured：Rare earth compound powder and NdFeB magnetic powder are mixed to prepare mixture, then by the mixing
Thing is divided into N parts；The weight/mass percentage composition of rare earth compound described in the mixture is 0.001% to 63.8%；
(2) raw material is prepared：Weigh a certain amount of NdFeB magnetic powder and the NdFeB magnetic powder is divided into N+1 parts；
(3) it is die-filling：The mixture that the NdFeB magnetic powder and step (1) that step (2) is obtained are obtained alternately is fitted into mould
And flatten；
(4) hot-pressing processing：The mould that the filling that step (3) is obtained is finished is put into vacuum induction hot press carries out heat
Pressure, hot pressing temperature be 500 DEG C to 850 DEG C, the heating-up time be 5 minutes to 10 minutes, pressure be 100MPa to 500MPa, compacting and
Soaking time is 1 minute to 3 minutes；The hot-pressed magnets with layer structure can be obtained；
(5) thermal deformation field：Thermal deformation processing is carried out to the hot-pressed magnets that step (4) is obtained, you can obtain with stratiform
The Nd-Fe-B permanent magnetic magnet of structure.
Wherein in one embodiment, in step (1), described rare earth compound powder mixes with the NdFeB magnetic powder
Be by the rare earth compound and the NdFeB magnetic powder in mortar it is finely ground after uniformly mix.
Wherein in one embodiment, in step (1), described rare earth compound powder mixes with the NdFeB magnetic powder
It is to be placed in the absolute ethyl alcohol suspension for being dispersed with rare earth compound by by NdFeB magnetic powder, and after the uniform mixing of ultrasonic disperse
The mixture is dried to obtain, and the drying process is carried out in vacuum drying oven.
Wherein in one embodiment, the detailed process of the thermal deformation field of the step (5) is：
The obtained hot-pressed magnets with layer structure of step (4) are put into thermal deformation mould, control temperature 700~
850 DEG C, the heating-up time is 5~10 minutes, is warmed up to insulation after preset temperature and opens hydraulic system after 0.5~5 minute, is slowly applied
Plus-pressure, makes magnet at the uniform velocity deform, and prepares the magnet time for 2~3 minutes, and magnet is incubated 10~30 seconds after the completion of preparing, then
Room temperature was cooled in 20~30 minutes.
Wherein in one embodiment, the NdFeB magnetic powder is Nano crystal neodymium, boron magnetic.
Compared with prior art, the advantage of the invention is that：Nd-Fe-B permanent magnetic magnet of the invention is in thermal deformation neodymium iron boron
Multilayer rare earth compound barrier layer is formed in the middle of magnet, magnet resistive rate is capable of achieving and is increased substantially, while by rare earth compound
Intermediate course is concentrated on, influence of dystectic rare earth compound to adjacent two layers magnet structure is reduced.It is achieved thereby that in magnetic
In the case that body magnetic property is not decreased obviously, the resistivity of Nd-Fe-B permanent magnetic magnet is increased substantially.
Brief description of the drawings
Fig. 1 is the overall structure diagram of one embodiment of Nd-Fe-B permanent magnetic magnet of the invention；
Fig. 2 is the scanning backscattered figure of one embodiment of Nd-Fe-B permanent magnetic magnet of the invention；
Fig. 3 is the overall structure diagram of the one embodiment in the preparation method of Nd-Fe-B permanent magnetic magnet of the invention；
Fig. 4 is the overall structure diagram of another embodiment of preparation method of Nd-Fe-B permanent magnetic magnet of the invention.
Specific 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 is described.It should be noted that in the case where not conflicting, the feature in embodiment and embodiment in the application can phase
Mutually combination.
The invention provides a kind of Nd-Fe-B permanent magnetic magnet in layer structure, its composition includes neodymium iron boron magnetic body and rare earth
Compound, the neodymium iron boron magnetic body is in layer structure in its macrostructure, and its composition layer includes two kinds, and one kind is included containing dilute
The composition layer of earth compounds, another kind is free from constituting layer by rare earth compound；Composition layer containing rare earth compound is by dilute
Earth compounds and neodymium iron boron magnetic body are constituted, and are not contained and only contain neodymium iron boron magnetic body in the composition layer of rare earth compound.Containing dilute
The composition layer of earth compounds and the composition alternately laminated setting of layer for not containing rare earth compound, the i.e. composition containing rare earth compound
Other composition layers of the both sides of layer are the composition layer for not containing rare earth compound；See on the whole, rare earth compound is not
It is evenly distributed in whole Nd-Fe-B permanent magnetic magnet, but in the single composition layer middle rare earth compound containing rare earth compound
It is equally distributed.
As shown in figure 1, Nd-Fe-B permanent magnetic magnet is layer structure, its composition layer is divided into two kinds, and one kind is to contain rare earth
First composition layer 100 of compound 110, another kind is free from constituting layer 200, the first composition layer 100 by the second of rare earth compound
Layer structure is formed with the second alternately laminated setting of composition layer 200.And rare earth compound 110 is evenly distributed on the first composition layer
In 100.
The present invention forms multilayer rare earth compound barrier layer in the middle of heat distortion magnet, by increasing rare earth compound significantly
Degree improves the resistivity of magnet, while rare earth compound is concentrated on the present invention intermediate course of heat distortion magnet, as far as possible
Reduce influence of dystectic compound to its adjacent sets stratification, it is achieved thereby that situation about not being decreased obviously in magnetic property
Under, the effect that the resistivity of Nd-Fe-B permanent magnetic magnet is increased substantially.The rare earth compound of high resistivity is insulator, in magnet
After being internally formed layer structure, scattering of the electronics in transmitting procedure is increased, so that perpendicular to layer structure direction
Resistivity is increased substantially.Simultaneously as rare earth fluoride fusing point is (1400 DEG C or so) high, deformation is difficult at 800-900 DEG C,
So as to influence the deformation orientation of rare earth compound particle surrounding grains, magnet entirety texture is destroyed.So by rare earth compound
It is confined in very thin layer, it can be greatly reduced grain deformation orientation in adjacent layer and overall texture are formed.Magnet magnetic
Principal phase and its texture can be mostly come from, texture is destroyed and is reduced, magnet magnetic property will maintain a preferable numerical value.
Preferably, used as a kind of embodiment, the rare earth compound is rare earth fluoride or rare earth oxide.This reality
The rare earth in example is applied for neodymium, dysprosium, terbium or praseodymium, described rare earth fluoride and rare earth oxide are the fluoride of neodymium, dysprosium, terbium or praseodymium
And oxide
Preferably, as a kind of embodiment, the quality hundred of rare earth compound described in whole Nd-Fe-B permanent magnetic magnet
Content is divided to be 0.0001% to 5.29%.
Preferably, as a kind of embodiment, rare earth chemical combination described in the first composition layer 100 containing rare earth compound
The weight/mass percentage composition of thing is 0.001% to 63.8%.Preferably, the quality percentage of rare earth compound described in the first composition layer
Content is preferably 11% to 63.8%.
Preferably, as a kind of embodiment, referring to Fig. 2, first composition containing the rare earth compound 110
The rare earth compound 110 in layer 100 is distributed in the neodymium iron boron magnetic body in the form of sheets.Rare earth in first composition layer 100
The resistivity of compound is high, and these rare earth compounds divide in the form of sheets in the presence of pressure, temperature etc. between neodymium iron boron particles
Cloth.Most last layer and bottom in Fig. 2 are the second composition layer, and middle one layer is the first composition layer, white in the first composition layer
Color part is rare earth compound.
Preferably, used as a kind of embodiment, the quantity of the second composition layer 200 is than the described first composition layer 100
Many one layers of quantity.Ground floor and last layer are the second composition layer i.e. in Nd-Fe-B permanent magnetic magnet.Referring to Fig. 1, this implementation
Nd-Fe-B permanent magnetic magnet in example, ground floor is that the second composition layer 200 and last layer are not comprising rare earth compound the
Two composition layers.The second composition layer that ground floor and last layer are set to not contain rare earth compound is easy to mechanical grinding, is contained
Slightly weakened by the first mechanical strength for constituting layer of rare earth compound, be unfavorable for polishing.
Preferably, used as a kind of embodiment, the thickness of each group stratification can be with equal, it is also possible to.The present embodiment
In it is all first composition layers 100 thickness it is equal, it is all second composition layers 200 thickness it is also equal.But first composition layer and
The variable thickness of the second composition layer is fixed equal.
The preparation method of above-mentioned Nd-Fe-B permanent magnetic magnet, comprises the following steps：
(1) mixture is configured：Rare earth compound powder and NdFeB magnetic powder are mixed to prepare mixture, then by the mixing
Thing is divided into N parts；The mass percent of rare earth compound described in the mixture is 0.001% to 63.8%；In the present embodiment
N parts of mixture be equivalent.
(2) raw material is prepared：Weigh a certain amount of NdFeB magnetic powder and the NdFeB magnetic powder is divided into N+1 parts；This implementation
N+1 parts of NdFeB magnetic powder in example is equivalent.
(3) it is die-filling：The mixture that the NdFeB magnetic powder and step (1) that step (2) is obtained are obtained alternately is fitted into mould
And flatten；Concrete operation step is to be firstly added a NdFeB magnetic powder in a mold, strikes closely knit by the NdFeB magnetic powder and puts down
After paving is uniform；Evenly laid out one layer of mixture on this layer of neodymium-iron-boron bisque, so alternates tiling compacting, Zhi Daopu again
Untill upper last layer of NdFeB magnetic powder.
(4) hot-pressing processing：The mould that the filling that step (3) is obtained is finished is put into vacuum induction hot press carries out heat
Pressure, hot pressing temperature be 500 DEG C to 850 DEG C, the heating-up time be 5 minutes to 10 minutes, pressure be 100MPa to 500MPa, compacting and
Soaking time is 1 minute to 3 minutes；The hot-pressed magnets with layer structure can be obtained；Vacuum induction heat in the present embodiment
It is evacuated down to higher than 9*10 when press is used-2Pa。
(5) thermal deformation field：Thermal deformation processing is carried out to the hot-pressed magnets that step (4) is obtained, you can obtain with stratiform
The Nd-Fe-B permanent magnetic magnet of structure.
As shown in figure 3, step (3) can be carried out with pressure direction with the composition vertical mould of layer, now NdFeB magnetic powder
Alternately it is fitted into hot pressing die and paves with mixture part, pressure direction is vertical with mould；Or step (3) as shown in Figure 4
Can be carried out in the pressure direction mould parallel with composition layer, concrete operation method is to place papery dividing plate in a mold, then
NdFeB magnetic powder and mixture are filled in interlayer respectively respectively, extract papery dividing plate out, now pressure direction is put down with composition layer
OK.Neodymium-iron-boron bisque and the alternate sandwich construction of mixture layer can be formed on pressure at right angle direction.
Preferably, as a kind of embodiment, in step (1), described rare earth compound powder and the neodymium iron boron
Magnetic mixing be by the rare earth compound and the NdFeB magnetic powder in mortar it is finely ground after uniformly mix.
Preferably, as a kind of embodiment, in step (1), described rare earth compound powder and the neodymium iron boron
Magnetic is combined by being placed in NdFeB magnetic powder in the absolute ethyl alcohol suspension for being dispersed with rare earth compound, and ultrasonic disperse is equal
The mixture is dried to obtain after even mixing, and the drying process is carried out in vacuum drying oven.
Preferably, used as a kind of embodiment, the detailed process of the thermal deformation field of the step (5) is：
The obtained hot-pressed magnets with layer structure of step (4) are put into thermal deformation mould, control temperature 700~
850 DEG C, heating-up time of room temperature to preset temperature is 5~10 minutes, is warmed up to insulation after preset temperature and is opened after 0.5~5 minute
Hydraulic system is opened, slowly applies pressure, magnet is at the uniform velocity deformed, prepare the magnet time for 2~3 minutes, after the completion of prepared by magnet
Insulation 10~30 seconds, then cooled to room temperature in 20~30 minutes.
Preferably, used as a kind of embodiment, the NdFeB magnetic powder is Nano crystal neodymium, boron magnetic.Preferably fast quenching
Magnetic or HDDR magnetics.
The present invention is described in further detail below in conjunction with specific embodiment.
Embodiment one
(1) 446.9mg NdF accurately are weighed3Powder, and with 3.5g Nano crystal neodymium, borons magnetic in being ground well in mortar.
(2) 40g Nano crystal neodymium, boron magnetics are weighed and is divided into 2 equal portions, portion is put into the mould of internal diameter 18mm, first colds pressing close
It is real, the uniform mixed powder of grinding is added, it is evenly laid out on NdFeB magnetic powder, finally spread another Nano crystal neodymium, boron magnetic
Powder.
(3) whole mould is put into vacuum induction hot press, and is evacuated to 4 × 10-2Below Pa is simultaneously maintained low true
It is empty.Induction heating system heating is opened, while opening hydraulic system is pressurized to 5.8MPa, the pressure that will act on mould is maintained
In 100MPa.At the uniform velocity it is warmed up to 670 DEG C from room temperature, 5 minutes used times, keeping temperature and pressure 1 minute at 670 DEG C.Hot pressing is complete
Into rear rapid closing induction heating system and hydraulic system, and argon gas being poured repeatedly and being vacuumized, dropping to room temperature from the highest temperature uses
When 20-30 minutes.Hot-pressed magnets wire cutting is cut into the magnet of a diameter of 13mm, then outer surface is polished with cylindrical sanding machine
Totally.
(4) hot-pressed magnets are put into the mould that internal diameter is 24mm, 4 × 10 is evacuated down in advance-2Below Pa, then pours
Argon gas, as protective gas, 850 DEG C is at the uniform velocity warming up to from room temperature to 1 × 102Pa, and the heating-up time is 6 minutes, after reaching 850 DEG C
Insulation 60 seconds.Hydraulic system is opened, slow pressurization maintains magnet at the uniform velocity deformation, after the completion of thermal deformation, is gradually pressurized to 5MPa,
The pressure that maintenance is applied on mould is 50MPa, and heat-insulation pressure keeping rapid closing presure and heating system after 30 seconds, thermal deformation are completed
It is the Nd-Fe-B permanent magnetic magnet that can obtain layer structure for 30 minutes to be reduced to the room temperature time from the highest temperature afterwards.
The weight/mass percentage composition that the present embodiment middle rare earth compound accounts for whole neodymium iron boron magnetic body is 1.02%, the first composition layer
The weight/mass percentage composition of middle rare earth compound is 11.32%.
To recycle wire cutting that the circle of lower diameter 6mm is cut from magnet after the Nd-Fe-B permanent magnetic magnet demoulding of step (5)
Post, magnetism testing measures B-H instrument using permanent-magnet material, and test temperature is room temperature.
Likewise, on Nd-Fe-B permanent magnetic magnet from after the demoulding 2 × 2 × 6mm of the lower size of cutting cuboid, edge long
Pressure direction, resistivity measurement uses comprehensive physical test system (PPMS), and test temperature is room temperature.
Comparative example one
Accurately weigh 446.9mg NdF3Powder, and with 43.5g Nano crystal neodymium, borons magnetic in being ground well in mortar.This implementation
Example middle rare earth compound is evenly distributed in whole neodymium iron boron magnetic body, and rare earth compound accounts for the quality hundred of whole neodymium iron boron magnetic body
Content is divided to be 1.02%.
Performance test methods are with embodiment one.
Embodiment two
(1) 893.1mg NdF accurately are weighed3Powder, and with 3.5g Nano crystal neodymium, borons magnetic in being ground well in mortar.
(2) 40g Nano crystal neodymium, boron magnetics are weighed and is divided into 2 equal portions, portion is put into the mould of internal diameter 18mm, first colds pressing close
It is real, the uniform mixed powder of grinding is added, it is evenly laid out on magnetic, finally spread another Nano crystal neodymium, boron magnetic.
Other steps are with reference to embodiment one.
The weight/mass percentage composition that the present embodiment middle rare earth compound accounts for whole neodymium iron boron magnetic body is 2.01%, the first composition layer
The weight/mass percentage composition of middle rare earth compound is 20.33%.
Comparative example two
Accurately weigh 893.1mg NdF3Powder, and with 43.5g Nano crystal neodymium, borons magnetic in being ground well in mortar.This implementation
Example middle rare earth compound is evenly distributed in whole neodymium iron boron magnetic body, and rare earth compound accounts for the quality hundred of whole neodymium iron boron magnetic body
Content is divided to be 2.01%.
Performance test methods are with embodiment one.
Embodiment three
(1) 1785.9mg NdF accurately are weighed3Powder, and with 3.5g Nano crystal neodymium, borons magnetic in being ground well in mortar.
(2) 40g Nano crystal neodymium, boron magnetics are weighed and is divided into 2 equal portions, portion is put into the mould of internal diameter 18mm, first colds pressing close
It is real, the uniform mixed powder of grinding is added, it is evenly laid out on magnetic, finally spread another Nano crystal neodymium, boron magnetic.
Other steps are with reference to embodiment one.
The weight/mass percentage composition that the present embodiment middle rare earth compound accounts for whole neodymium iron boron magnetic body is 3.94%, the first composition layer
The weight/mass percentage composition of middle rare earth compound is 33.79%.
Comparative example three
Accurately weigh 1785.9mg NdF3Powder, and with 43.5g Nano crystal neodymium, borons magnetic in being ground well in mortar.This reality
A middle rare earth compound is applied to be evenly distributed in whole neodymium iron boron magnetic body, and rare earth compound accounts for the quality of whole neodymium iron boron magnetic body
Percentage composition is 3.94%.
Performance test methods are with embodiment one.
Example IV
(1) 2350mg NdF accurately are weighed3Powder, and with 3.5g Nano crystal neodymium, borons magnetic in being ground well in mortar；By NdF3
5 equal portions are divided into the mixed powder of Nano crystal neodymium, boron magnetic；
(2) 40g Nano crystal neodymium, boron magnetics are weighed and is divided into 6 equal portions, a magnetic is put into the mould of internal diameter 18mm, it is first cold
Densification reality, adds a mixed powder, evenly laid out on magnetic, so alternately until spreading last portion Nano crystal neodymium, boron
Magnetic.
Other steps are with reference to embodiment one.
The weight/mass percentage composition that the present embodiment middle rare earth compound accounts for whole neodymium iron boron magnetic body is 5.12%, the first composition layer
The weight/mass percentage composition of middle rare earth compound is 40.2%.
Comparative example four
Accurately weigh 2350mg NdF3Powder, and with 43.5g Nano crystal neodymium, borons magnetic in being ground well in mortar.This implementation
Example middle rare earth compound is evenly distributed in whole neodymium iron boron magnetic body, and rare earth compound accounts for the quality hundred of whole neodymium iron boron magnetic body
Content is divided to be 5.12%.
Performance test methods are with embodiment one.
Embodiment five
(1) 2350mg NdF accurately are weighed3Powder, and with 1.333g Nano crystal neodymium, borons magnetic in being ground well in mortar；Will
NdF35 equal portions are divided into the mixed powder of Nano crystal neodymium, boron magnetic；
(2) 40.7g Nano crystal neodymium, boron magnetics are weighed and is divided into 6 equal portions, a magnetic is put into the mould of internal diameter 18mm, first
Cold pressing closely knit, add a mixed powder, it is evenly laid out on magnetic, so alternately until spreading last a nanocrystalline neodymium iron
Boron magnetic powder.
Other steps are with reference to embodiment one.
The weight/mass percentage composition that the present embodiment middle rare earth compound accounts for whole neodymium iron boron magnetic body is 5.29%, the first composition layer
The weight/mass percentage composition of middle rare earth compound is 63.8%.
Comparative example five
Accurately weigh 2350mg NdF3Powder, and with 42.033g Nano crystal neodymium, borons magnetic in being ground well in mortar.This reality
A middle rare earth compound is applied to be evenly distributed in whole neodymium iron boron magnetic body, and rare earth compound accounts for the quality of whole neodymium iron boron magnetic body
Percentage composition is 5.29%.
Performance test methods are with embodiment one.
Embodiment six
(1) 893.4mg NdF accurately are weighed3Powder, and with 3.5g Nano crystal neodymium, borons magnetic in being ground well in mortar, will
NdF32 equal portions are divided into the mixture of Nano crystal neodymium, boron magnetic；
(2) weigh 40g Nano crystal neodymium, boron magnetics to classify in three categories part, a magnetic is put into the mould of internal diameter 18mm, it is first cold
Densification reality, adds a mixed powder, evenly laid out on magnetic, so alternately until spreading last portion Nano crystal neodymium, boron
Magnetic.
Other steps are with reference to embodiment one.
The weight/mass percentage composition that the present embodiment middle rare earth compound accounts for whole neodymium iron boron magnetic body is 2.01%, the first composition layer
The weight/mass percentage composition of middle rare earth compound is 20.33%.
Embodiment seven
(1) 893.4mg NdF accurately are weighed3Powder, and with 3.5g Nano crystal neodymium, borons magnetic in being ground well in mortar, will
NdF33 equal portions are divided into the mixture of Nano crystal neodymium, boron magnetic；
(2) 40g Nano crystal neodymium, boron magnetics are weighed and is divided into 4 equal portions, a magnetic is put into the mould of internal diameter 18mm, it is first cold
Densification reality, adds a mixed powder, evenly laid out on magnetic, so alternately until spreading last portion Nano crystal neodymium, boron
Magnetic.
Other steps are with reference to embodiment one.
The weight/mass percentage composition that the present embodiment middle rare earth compound accounts for whole neodymium iron boron magnetic body is 2.01%, the first composition layer
The weight/mass percentage composition of middle rare earth compound is 20.33%.
Embodiment eight
(1) 2350mg NdF accurately are weighed3Powder, and with 3.5g Nano crystal neodymium, borons magnetic in being ground well in mortar, by NdF3
2 equal portions are divided into the mixture of Nano crystal neodymium, boron magnetic；
(2) weigh 40g Nano crystal neodymium, boron magnetics to classify in three categories part, a magnetic is put into the mould of internal diameter 18mm, it is first cold
Densification reality, adds a mixed powder, evenly laid out on magnetic, so alternately until spreading last portion Nano crystal neodymium, boron
Magnetic.
Other steps are with reference to embodiment one.
The weight/mass percentage composition that the present embodiment middle rare earth compound accounts for whole neodymium iron boron magnetic body is 5.12%, the first composition layer
The weight/mass percentage composition of middle rare earth compound is 40.1%.
Embodiment nine
(1) 2350mg NdF accurately are weighed3Powder, and with 3.5g Nano crystal neodymium, borons magnetic in being ground well in mortar；
(2) 40g Nano crystal neodymium, boron magnetics are weighed and is divided into 2 equal portions, a magnetic is put into the mould of internal diameter 18mm, it is first cold
Densification reality, adds a mixed powder, evenly laid out on magnetic, then spreads most another Nano crystal neodymium, boron magnetic.
Other steps are with reference to embodiment one.
The weight/mass percentage composition that the present embodiment middle rare earth compound accounts for whole neodymium iron boron magnetic body is 5.12%, the first composition layer
The weight/mass percentage composition of middle rare earth compound is 40.1%.
Comparative example one
Without rare earth compound in the present embodiment, other conditions reference implementation example one.
The magnetic property of neodymium-iron-boron magnet prepared by each embodiment of table 1, electric property compare
Increased as can be seen that adding the resistivity of the Nd-Fe-B permanent magnetic magnet obtained after rare earth compound by upper table, and
With the increase of rare earth compound content, resistivity value is consequently increased.
Various embodiments above is identical with the percentage composition of corresponding comparative example's middle rare earth compound, by each implementation
The contrast of example embodiment in contrast is this it appears that the stratiform Nd-Fe-B permanent magnetic magnet prepared using the method for the present invention
Resistivity is greatly increased, and its magnetic property is not decreased obviously.
From embodiment one to embodiment five it can be seen that the increase of the content with rare earth compound, stratiform Nd-Fe-B permanent magnetic
Magnet is higher relative to the percentage that the resistivity of existing Nd-Fe-B permanent magnetic magnet is improved.
Embodiment two, embodiment six are identical with the content of the middle rare earth compound of embodiment seven, but the number of plies is different；Embodiment
4th, embodiment eight is identical with the content of the middle rare earth compound of embodiment nine, but the number of plies is different.Can be with according to above-mentioned experimental result
Find out, when the percentage composition of rare earth compound is higher, the number of plies is more, it is more that its resistivity is improved.
Embodiment ten
(1) 893.7mg DyF accurately are weighed3Powder, and with 3.5g Nano crystal neodymium, borons magnetic in being ground well in mortar.
(2) 40g Nano crystal neodymium, boron magnetics are weighed and is divided into 2 equal portions, portion is put into the mould of internal diameter 18mm, first colds pressing close
It is real, the uniform mixed powder of grinding is added, it is evenly laid out on magnetic, finally spread another Nano crystal neodymium, boron magnetic.
Other steps are with reference to embodiment one.The resistivity of the Nd-Fe-B permanent magnetic magnet obtained in the present embodiment is 430 μ Ω
cm.
The weight/mass percentage composition that the present embodiment middle rare earth compound accounts for whole neodymium iron boron magnetic body is 2.01%, the first composition layer
The weight/mass percentage composition of middle rare earth compound is 20.33%.
Embodiment 11
(1) 893.4mg Dy accurately are weighed2O3Powder, and with 3.5g Nano crystal neodymium, borons magnetic in being ground well in mortar.
(2) 40g Nano crystal neodymium, boron magnetics are weighed and is divided into 2 equal portions, portion is put into the mould of internal diameter 18mm, first colds pressing close
It is real, the uniform mixed powder of grinding is added, it is evenly laid out on magnetic, finally spread another Nano crystal neodymium, boron magnetic.
Other steps are with reference to embodiment one.The resistivity of the Nd-Fe-B permanent magnetic magnet obtained in the present embodiment is 208 μ Ω
cm.The weight/mass percentage composition that the present embodiment middle rare earth compound accounts for whole neodymium iron boron magnetic body is 2.01%, dilute in the first composition layer
The weight/mass percentage composition of earth compounds is 20.33%.
Embodiment 12
(1) 893.4mg Pr accurately are weighed2O3Powder, and with 3.5g Nano crystal neodymium, borons magnetic in being ground well in mortar, will
Pr2O32 equal portions are divided into the mixture of Nano crystal neodymium, boron magnetic；
(2) weigh 40g Nano crystal neodymium, boron magnetics to classify in three categories part, a magnetic is put into the mould of internal diameter 18mm, it is first cold
Densification reality, adds a mixed powder, evenly laid out on magnetic, so alternately until spreading last portion Nano crystal neodymium, boron
Magnetic.
Other steps are with reference to embodiment one.The resistivity of the Nd-Fe-B permanent magnetic magnet obtained in the present embodiment is 205 μ Ω
cm.The weight/mass percentage composition that the present embodiment middle rare earth compound accounts for whole neodymium iron boron magnetic body is 2.01%, dilute in the first composition layer
The weight/mass percentage composition of earth compounds is 20.33%.
Embodiment 13
(1) 893.4mg Pr F accurately are weighed3Powder, and with 3.5g Nano crystal neodymium, borons magnetic in being ground well in mortar, will
Pr F33 equal portions are divided into the mixture of Nano crystal neodymium, boron magnetic；
(2) 40g Nano crystal neodymium, boron magnetics are weighed and is divided into 4 equal portions, a magnetic is put into the mould of internal diameter 18mm, it is first cold
Densification reality, adds a mixed powder, evenly laid out on magnetic, so alternately until spreading last portion Nano crystal neodymium, boron
Magnetic.
Other steps are with reference to embodiment one.The resistivity of the Nd-Fe-B permanent magnetic magnet obtained in the present embodiment is 410 μ Ω
cm。
The weight/mass percentage composition that the present embodiment middle rare earth compound accounts for whole neodymium iron boron magnetic body is 2.01%, the first composition layer
The weight/mass percentage composition of middle rare earth compound is 20.33%.
Embodiment 14
(1) 1785.9mg TbF accurately are weighed3Powder, and with 3.5g Nano crystal neodymium, borons magnetic in being ground well in mortar.
(2) 40g Nano crystal neodymium, boron magnetics are weighed and is divided into 2 equal portions, portion is put into the mould of internal diameter 18mm, first colds pressing close
It is real, the uniform mixed powder of grinding is added, it is evenly laid out on magnetic, finally spread another Nano crystal neodymium, boron magnetic.
Other steps are with reference to embodiment one.The resistivity of the Nd-Fe-B permanent magnetic magnet obtained in the present embodiment is 420 μ Ω
cm。
The weight/mass percentage composition that the present embodiment middle rare earth compound accounts for whole neodymium iron boron magnetic body is 3.94%, the first composition layer
The weight/mass percentage composition of middle rare earth compound is 33.78%.
Embodiment 15
(1) 1785.9mg Tb accurately are weighed2O3Powder, and with 3.5g Nano crystal neodymium, borons magnetic in being ground well in mortar.
(2) 40g Nano crystal neodymium, boron magnetics are weighed and is divided into 2 equal portions, portion is put into the mould of internal diameter 18mm, first colds pressing close
It is real, the uniform mixed powder of grinding is added, it is evenly laid out on magnetic, finally spread another Nano crystal neodymium, boron magnetic.
Other steps are with reference to embodiment one.The resistivity of the Nd-Fe-B permanent magnetic magnet obtained in the present embodiment is 212 μ Ω
cm。
The weight/mass percentage composition that the present embodiment middle rare earth compound accounts for whole neodymium iron boron magnetic body is 3.94%, the first composition layer
The weight/mass percentage composition of middle rare earth compound is 33.78%.
Embodiment 16
(1) 1785.9mg Nd accurately are weighed2O3Powder, and with 3.5g Nano crystal neodymium, borons magnetic in being ground well in mortar.
(2) 40g Nano crystal neodymium, boron magnetics are weighed and is divided into 2 equal portions, portion is put into the mould of internal diameter 18mm, first colds pressing close
It is real, the uniform mixed powder of grinding is added, it is evenly laid out on magnetic, finally spread another Nano crystal neodymium, boron magnetic.
Other steps are with reference to embodiment one.The resistivity of the Nd-Fe-B permanent magnetic magnet obtained in the present embodiment is 310 μ Ω
cm。
The weight/mass percentage composition that the present embodiment middle rare earth compound accounts for whole neodymium iron boron magnetic body is 3.94%, the first composition layer
The weight/mass percentage composition of middle rare earth compound is 33.78%.
Embodiment described above only expresses several embodiments of the 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 guarantor of the invention
Shield scope.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (15)
1. a kind of Nd-Fe-B permanent magnetic magnet, it is characterised in that including neodymium iron boron magnetic body and rare earth compound；The Nd-Fe-B permanent magnetic
Magnet is in layer structure；Composition layer containing the rare earth compound is the first composition layer, does not contain the composition of rare earth compound
Layer is the second composition layer, the first composition layer and the second composition alternately laminated arrangement of layer；
Rare earth compound is evenly distributed in the neodymium iron boron magnetic body described in the first composition layer, in the first composition layer
The weight/mass percentage composition of the rare earth compound is 11% to 63.8%；
The rare earth compound in the first composition layer is distributed in the form of sheets, and the rare earth compound concentrates on the first composition layer
In.
2. Nd-Fe-B permanent magnetic magnet according to claim 1, it is characterised in that rare earth described in the first composition layer
The weight/mass percentage composition of compound is 20.33% to 63.8%.
3. Nd-Fe-B permanent magnetic magnet according to claim 1, it is characterised in that rare earth described in the first composition layer
The weight/mass percentage composition of compound is 40.1% to 63.8%.
4. Nd-Fe-B permanent magnetic magnet according to claim 1, it is characterised in that the rare earth compound is rare earth fluoride
Or rare earth oxide.
5. Nd-Fe-B permanent magnetic magnet according to claim 1, it is characterised in that dilute described in the Nd-Fe-B permanent magnetic magnet
The weight/mass percentage composition of earth compounds is 0.0001% to 5.29%.
6. the Nd-Fe-B permanent magnetic magnet according to claim 1 to 5 any one, it is characterised in that the second composition layer
Quantity than described first composition layer quantity more than one layer.
7. Nd-Fe-B permanent magnetic magnet according to claim 6, it is characterised in that the first composition layer is at least a layer,
The second composition layer is at least two-layer, and the thickness of all first composition layers is equal, the thickness of all second composition layers
Degree is equal.
8. Nd-Fe-B permanent magnetic magnet according to claim 1, it is characterised in that the rare earth unit in described rare earth compound
Element is neodymium, dysprosium, terbium or praseodymium.
9. a kind of preparation method of Nd-Fe-B permanent magnetic magnet as described in claim 1 to 8 any one, it is characterised in that bag
Include following steps：
（1）Configuration mixture：Rare earth compound powder and NdFeB magnetic powder are mixed to prepare mixture, then the mixture is divided
It is N parts；The weight/mass percentage composition of rare earth compound described in the mixture is 11% to 63.8%；
（2）Prepare raw material：Weigh a certain amount of NdFeB magnetic powder and the NdFeB magnetic powder is divided into N+1 parts；
（3）It is die-filling：By step（2）The NdFeB magnetic powder and step for obtaining（1）The mixture for obtaining alternately is fitted into mould and presses
It is flat；
（4）Hot-pressing processing：By step（3）The mould that the filling for obtaining is finished carries out hot pressing in being put into vacuum induction hot press, heat
Pressure temperature is 500 DEG C to 850 DEG C, and the heating-up time is 5 minutes to 10 minutes, and pressure is 100MPa to 500MPa, suppresses and is incubated
Time is 1 minute to 3 minutes；The hot-pressed magnets with layer structure can be obtained；
（5）Thermal deformation field：To step（4）The hot-pressed magnets for obtaining carry out thermal deformation processing, you can obtain with layer structure
Nd-Fe-B permanent magnetic magnet,
Wherein, the rare earth compound is distributed in the form of sheets, and the rare earth compound is concentrated in the layer of mixture formation.
10. preparation method according to claim 9, it is characterised in that rare earth compound described in the first composition layer
Weight/mass percentage composition be 20.33% to 63.8%.
11. preparation methods according to claim 9, it is characterised in that rare earth compound described in the first composition layer
Weight/mass percentage composition be 40.1% to 63.8%.
12. preparation methods according to claim 9, it is characterised in that step（1）In, described rare earth compound powder
Mix with the NdFeB magnetic powder be by the rare earth compound and the NdFeB magnetic powder in mortar it is finely ground after uniformly mix.
13. preparation methods according to claim 9, it is characterised in that step（1）In, described rare earth compound powder
In being combined by being placed in NdFeB magnetic powder the absolute ethyl alcohol suspension for being dispersed with rare earth compound with the NdFeB magnetic powder,
And the mixture is dried to obtain after the uniform mixing of ultrasonic disperse, and the drying process is carried out in vacuum drying oven.
14. preparation methods according to claim 9, it is characterised in that the step（5）Thermal deformation field specific mistake
Cheng Wei：
By step（4）The obtained hot-pressed magnets with layer structure are put into thermal deformation mould, and control temperature is 700 ~ 850
DEG C, the heating-up time is 5 ~ 10 minutes, is warmed up to insulation after preset temperature and opens hydraulic system after 0.5 ~ 5 minute, slow to apply
Pressure, makes magnet at the uniform velocity deform, and prepares the magnet time for 2 ~ 3 minutes, and magnet is incubated 10 ~ 30 seconds after the completion of preparing, Ran Hou
Room temperature is cooled in 20 ~ 30 minutes.
15. preparation methods according to claim 9, it is characterised in that the NdFeB magnetic powder is Nano crystal neodymium, boron magnetic
Powder.
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| CN105118605A (en) * | 2015-08-28 | 2015-12-02 | 锦州汉拿电机有限公司 | Motor, transformer core and manufacturing method thereof |
| CN108630366B (en) * | 2017-03-17 | 2020-09-08 | 中国科学院宁波材料技术与工程研究所 | Rare earth permanent magnet and preparation method thereof |
| DE102017223268A1 (en) * | 2017-12-19 | 2019-06-19 | Robert Bosch Gmbh | Method for producing a magnetic material, magnetic material, hard magnet, electric motor, starter and generator |
| CN108962580B (en) * | 2018-06-28 | 2020-06-30 | 宁波招宝磁业有限公司 | Preparation method of dysprosium-infiltrated/terbium neodymium iron boron magnet |
| CN109065314B (en) * | 2018-09-07 | 2020-10-27 | 京磁材料科技股份有限公司 | Method for preparing high-coercivity magnet |
| CN110136953B (en) * | 2019-06-17 | 2022-04-26 | 江苏科技大学 | Preparation method of composite neodymium iron boron magnet with coercivity gradient distribution characteristic |
| CN111223623B (en) * | 2020-01-31 | 2022-04-05 | 厦门钨业股份有限公司 | Large-thickness neodymium iron boron magnetic steel and preparation method thereof |
| CN113451036B (en) * | 2021-04-09 | 2022-10-25 | 宁波科田磁业有限公司 | High-coercivity and high-resistivity neodymium-iron-boron permanent magnet and preparation method thereof |
| CN113996791B (en) * | 2021-09-27 | 2023-05-02 | 宁波金鸡强磁股份有限公司 | Manufacturing method of high-performance hot-pressing neodymium-iron-boron magnetic ring |
| CN114141469B (en) * | 2021-11-10 | 2023-04-11 | 钢铁研究总院 | High-resistivity rare earth hot-pressed permanent magnet and preparation method thereof |
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| JP2006344854A (en) * | 2005-06-10 | 2006-12-21 | Mitsubishi Materials Pmg Corp | Rare earth magnet having high strength and high resistance |
| CN101859639A (en) * | 2010-07-06 | 2010-10-13 | 烟台正海磁性材料股份有限公司 | R-Fe-B series magnet of gradient resistance and production method thereof |
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