CN108417378A - A kind of neodymium iron boron magnetic body and preparation method thereof containing dysprosium - Google Patents
A kind of neodymium iron boron magnetic body and preparation method thereof containing dysprosium Download PDFInfo
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- CN108417378A CN108417378A CN201810277194.8A CN201810277194A CN108417378A CN 108417378 A CN108417378 A CN 108417378A CN 201810277194 A CN201810277194 A CN 201810277194A CN 108417378 A CN108417378 A CN 108417378A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
- H01F41/0293—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets diffusion of rare earth elements, e.g. Tb, Dy or Ho, into permanent magnets
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
- H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
- H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
- H01F1/0577—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together sintered
Abstract
A kind of neodymium iron boron magnetic body containing dysprosium, forms through vacuum-sintering, and the content of dysprosium is 1 4wt% in the neodymium iron boron magnetic body.Preparation method includes：(1) dysprosium metal is put into a vacuum furnace, is passed through hydrogen, heat temperature raising; obtain dysprosium hydride; then ball milling or jet-stream wind wear into fine powder in nitrogen or inert gas shielding atmosphere, these fine powders are then put into drying in the glove box of argon gas atmosphere, obtain dysprosium hydride fine powder；(2) by fine powder, content is added in neodymium iron boron powder by mass percentage, is uniformly mixed；(3) mixed powder compression moulding under pulsed magnetic field and isostatic pressed obtains pressure embryo；(4) pressure embryo is placed in vacuum sintering furnace, is warming up to 1060 DEG C, vacuum-sintering, subsequent double annealing is cooling, and obtaining the present invention has the magnet of high-coercive force and higher residual magnetization.Easy to operate, process conditions are easy, and product quality is stablized, and rare earth alloy is low-consuming, and production cost is relatively low.
Description
Technical field
The present invention relates to a kind of Nd-Fe-B permanent magnet and preparation method thereof, especially a kind of neodymium iron boron magnetic body containing dysprosium and its
Preparation method.
Background technology
Rare-earth permanent magnet is growing day by day in the effect of various science and technology, and this trend is also continuing.Very much " green science and technology ", such as
Wind-power electricity generation, electric vehicle need a large amount of rare-earth permanent magnet, because this magnet has (the usually definition of maximum magnetic energy density
For (BH) max) and high coercivity.Sintered nd-fe-b magnet is such as sensed since excellent magnetic property is applied to many science and technology
Device, motor, engine etc..Sintered nd-fe-b magnet also plays an important roll in terms of mixing with pure electric automobile, it is required that
Magnet has high-coercive force, can apply to motor at high temperature.Mixing or the proper amount of heavy rare earth Dy energy of coating
Effectively improve the coercivity of Nd-Fe-B magnets.However, the fusing point of Dy (1407 DEG C) than sintering when formed rich Nd Grain-Boundary Phases (~
650 DEG C) fusing point want high more.Dy to Nd-Fe-B alloys are added in casting process and uniformly replace these elements, lead to coercive
Power increases, and also results in the intensity of magnetization and drastically reduces, thus reduces remanent magnetism.To improve its thermal stability, have by addition
Sintering and wetability low melting point Dy-Ni alloys realize improve Nd-Fe-B magnets coercivity without excessively reducing remanent magnetism, together
When obtained fully dense Nd-Fe-B magnets and accurate microstructure and desired magnetism.China Patent Publication No.：
CN104439232A, publication date：On March 25th, 2015, denomination of invention《The addition of dysprosium hydrogen compound improves Sintered NdFeB magnet and rectifys
The method and product of stupid power》, step is：Particle powder is made in Nd Fe B alloys by the hydrogen quick-fried method with airflow milling, is adopted
Particle powder is made in a brilliant phase dysprosium hydrogen compound with ball-milling method；The Grain-Boundary Phase particle powder prepared is added to Nd-Fe-B powder
In end；The alloy powder mixed carries out orientation compacting under magnetic field；The magnetic patch isostatic cool pressing that die mould is completed is at base, then very
Sky sintering finally obtains magnet.Used in the preparation method hydrogenation dysprosium grain size it is about smaller, be oxidized easily, and cost compared with
Height does not obtain ideal coercivity, needs to add more hydrogenation dysprosium.
Invention content
The object of the present invention is to provide the higher neodymium iron boron magnetic body containing dysprosium of a kind of coercivity and residual magnetization, the magnet
Rare-earth usage is less, magnet reasonable in internal structure, while the present invention also provides a kind of preparation method of the magnet, this method techniques
Simplicity, easy to operate, product quality is stablized, and production cost is relatively low.
Technical solution of the invention is：A kind of neodymium iron boron magnetic body containing dysprosium, forms, feature exists through vacuum-sintering
In：The content of dysprosium is 1-4wt% in the neodymium iron boron magnetic body.
The content of dysprosium is 2-3wt% in the neodymium iron boron magnetic body.
The preparation method of a kind of neodymium iron boron magnetic body containing dysprosium of the present invention, it is characterised in that include the following steps：
(1) dysprosium metal is put into a vacuum furnace, is passed through hydrogen, vacuum pressure 10-5-10-8Bar is heated to 350-
500 DEG C, dysprosium hydride is obtained, medium is then made with hexamethylene in nitrogen or inert gas shielding atmosphere, by dysprosium hydride ball
Wear into 3-7 microns of fine powder, or in nitrogen or inert gas shielding atmosphere using jet-stream wind mill by dysprosium hydride ball milling at
These fine powders are then put into drying in the glove box of argon gas atmosphere, obtain dysprosium hydride fine powder by 3-7 microns of fine powder；
(2) by the dysprosium hydride fine powder prepared in step (1), content is added in neodymium iron boron powder by mass percentage,
It is uniformly mixed；
(3) by step (2) by after evenly mixing powder magnetic induction intensity 1.8-6T pulsed magnetic field and 1000-
1400kg/cm2Isostatic pressed under compression moulding, obtain pressure embryo；
(4) pressure embryo is placed in vacuum sintering furnace, rises to 1010 DEG C with the heating rate of 600-800 DEG C/h, then 50-
The heating rate of 150 DEG C/h rises to 1060 DEG C, and vacuum-sintering 2-4 hours is then annealed 1-2 hours at 900 DEG C, respectively 650
DEG C double annealing 1-2 hours, it is cooling, finally obtain neodymium iron boron magnetic body.
In the step (1), the vacuum drying oven pressure is 10-8Bar, temperature are 450 DEG C.
In the step (1), by dysprosium hydride ball milling at 4 microns of fine powder.
In the step (3), the pulsed magnetic field and 1200kg/cm2 of powder after evenly mixing in magnetic induction intensity 4.5T
Isostatic pressed under compression moulding.
In the step (4), 1010 DEG C are risen to the heating rate of 700 DEG C/h, then extremely with the heating rate of 100 DEG C/h
1060℃。
It in the step (4), first anneals 1 hour at 900 DEG C, then in 650 DEG C of double annealings 1 hour.
Compared with prior art the beneficial effects of the invention are as follows：
1. simple process, rationally.Low melting point Dy hydride is in nitrogen or inert gas shielding atmosphere through ball milling or injection
It is added to after airflow milling in Nd-Fe-B micro mists and is sintered, process conditions is easy, applying pulse magnetic field, isostatic pressing
And vacuum-sintering is easy to operate, product quality is stablized, and production cost is relatively low.
2. cost-effective.Heavy rare earth element resource is limited, expensive, can effectively reduce its dosage using this method, add
Add micro heavy rare earth element to can be obtained high-coercive force and higher residual magnetization, energy saving and optimization " nucleocapsid " structure with
Minimize valuable Dy dosages.
3. the addition of low melting point Dy hydride can increase substantially magnet coercivity.At the method for the invention
Reason, with DyH3Amount increases to 4wt% from 1wt%, and coercivity is increased to 1738kA/m from 690kA/m.The present invention is for using
High-coercive force rare earth permanent magnet motor (such as electric vehicle, the commercial Applications such as wind-driven generator) Effec-tive Function has critical work
With.
4. this low melting point Dy hydride can limit excessive Dy and be diffused into NdFeB Hard Magnetic discrete phases, the intensity of magnetization is prevented
Drastically reduce.On the other hand, low melting point Dy hydrogen compounds addition in sintering process for realize optimization microstructure and
It is magnetic helpful.
Specific implementation mode
With reference to specific implementation row, the present invention is further described, but the present invention is not limited to following embodiments.
Embodiment 1
Dysprosium metal is put into a vacuum furnace, is passed through hydrogen, vacuum pressure 10-8Bar is heated to 450 DEG C, obtains dysprosium hydrogen
Then compound makees medium in nitrogen or inert gas shielding atmosphere with hexamethylene, dysprosium hydride ball milling is thin at 3 microns
These fine powders are then put into drying in the glove box of argon gas atmosphere, obtain dysprosium hydride fine powder by powder；The DyH that will be prepared3Add
It is added to Nd13.5Fe79.75B6.75In powder, adding proportion is Nd13.5Fe79.75B6.75The 2.5% of powder quality, equably with DyH3
Powder is uniformly mixed；Pulsed magnetic field and 1200kg/cm of the powder after evenly mixing in magnetic induction intensity 4.5T will be passed through2Etc. quiet
Pressure, compression moulding obtain pressure embryo；Pressure embryo is placed in vacuum sintering furnace, 1010 DEG C are risen to the heating rate of 700 DEG C/h,
Then the heating rate of 100 DEG C/h rises to 1060 DEG C, carries out under vacuum-sintering 2 hours, then anneals 1 hour at 900 DEG C respectively,
In 650 DEG C of double annealings 1 hour, Sintered NdFeB magnet is finally obtained.
Embodiment 2
The DyH that will be prepared3It is added to Nd13.5Fe79.75B6.75In powder, DyH3Adding proportion be
Nd13.5Fe79.75B6.75The 3% of powder quality, then prepare neodymium iron boron magnetic body as a comparison in fact with 1 identical technique of same embodiment
It tests.
Comparative example 1
It is prepared for undoped with DyH using technique same as Example 13The Nd of powder particle13.5Fe79.75B6.75As right
Than experiment.
The magnetic property of four kinds of magnets is measured using ferrometer, the items time performance indicator of prepared magnet is listed in Table 1 below.
1 embodiment 1 of table, embodiment 2, with comparison 1 magnet magnetic property of row comparison
It these results suggest that for the identical sintered Nd of ingredient13.5Fe79.75B6.75For magnet, added using the present invention
DyH3Magnet prepared by powder particle is significantly improved than the coercivity of undoped magnet, and remanent magnetism is not reduced substantially.
Embodiment 3
Dysprosium metal is put into a vacuum furnace, is passed through hydrogen, vacuum pressure 10-5Bar is heated to 400 DEG C, obtains dysprosium hydrogen
Compound then in nitrogen or inert gas shielding atmosphere using jet-stream wind mill by dysprosium hydride ball milling at 4 microns of fine powder,
These fine powders are then put into drying in the glove box of argon gas atmosphere, obtain dysprosium hydride fine powder；The DyH that will be prepared3Addition
To Nd10Fe80B10In powder, adding proportion is Nd10Fe80B10The 2% of powder quality, equably with DyH3Powder is uniformly mixed；
Pulsed magnetic field and 1200kg/cm of the powder after evenly mixing in magnetic induction intensity 1.8T will be passed through2Under isostatic pressed, it is pressed into
Type obtains pressure embryo；Pressure embryo is placed in vacuum sintering furnace, rises to 1010 DEG C with the heating rate of 700 DEG C/h, then 100 DEG C/h
Heating rate rise to 1060 DEG C, vacuum-sintering carries out 2-4 hours, then anneals 1 hour at 900 DEG C respectively, secondary at 650 DEG C
Annealing 1 hour, finally obtains Sintered NdFeB magnet.
Embodiment 4
The DyH that will be prepared3It is added to Nd10Fe80B10In powder, DyH3Adding proportion be Nd10Fe80B10Powder quality
3.2%, then prepare neodymium iron boron magnetic body with 1 identical technique of same embodiment and test as a comparison.
Comparative example 2
It is prepared for undoped with DyH using technique same as Example 33The Nd of powder particle10Fe80B10It is real as a comparison
It tests.
The magnetic property of four kinds of magnets is measured using ferrometer, the items time performance indicator of prepared magnet is listed in Table 1 below.
1 embodiment 3 of table, embodiment 4 are compared with 2 magnet magnetic property of comparative example
It these results suggest that for the identical sintered Nd of ingredient10Fe80B10For magnet, DyH is added using the present invention3Powder
The magnet of last particle preparation is significantly improved than the coercivity of undoped magnet, and remanent magnetism does not change substantially.
Embodiment 5
Dysprosium metal is put into a vacuum furnace, is passed through hydrogen, vacuum pressure 10-7Bar is heated to 500 DEG C, obtains dysprosium hydrogen
Then compound makees medium in nitrogen or inert gas shielding atmosphere with hexamethylene, dysprosium hydride ball milling is thin at 5 microns
These fine powders are then put into drying in the glove box of argon gas atmosphere, obtain dysprosium hydride fine powder by powder；The DyH that will be prepared3Add
It is added to Nd12.5Fe81.5B6In powder, adding proportion is Nd12.5Fe81.5B6The 2.5% of powder quality, equably with DyH3Powder is mixed
It closes uniform.By powder after evenly mixing magnetic induction intensity 2T pulsed magnetic field and 1000kg/cm2Under isostatic pressed, it is pressed into
Type obtains pressure embryo；Pressure embryo is placed in vacuum sintering furnace, rises to 1010 DEG C with the heating rate of 700 DEG C/h, then 100 DEG C/h
Heating rate rise to 1060 DEG C, vacuum-sintering carries out 2-4 hours, then anneals 1 hour at 900 DEG C respectively, secondary at 650 DEG C
Annealing 1.5 hours, finally obtains Sintered NdFeB magnet.
Embodiment 6
Dysprosium metal is put into a vacuum furnace, is passed through hydrogen, vacuum pressure 10-6Bar is heated to 490 DEG C, obtains dysprosium hydrogen
Compound, then in nitrogen or inert gas shielding atmosphere using jet-stream wind mill by dysprosium hydride ball milling at 6 microns of fine powder,
These fine powders are then put into drying in the glove box of argon gas atmosphere, obtain dysprosium hydride fine powder；The DyH that will be prepared3Addition
To Nd10Fe80B10In powder, adding proportion is Nd10Fe80B10The 2.7% of powder quality, equably with DyH3Powder mixing is equal
It is even；By powder after evenly mixing magnetic induction intensity 3T pulsed magnetic field and 1400kg/cm2Under isostatic pressed, compression moulding obtains
To pressure embryo；Pressure embryo is placed in vacuum sintering furnace, rises to 1010 DEG C with the heating rate of 800 DEG C/h, then the heating of 150 DEG C/h
Rate rises to 1060 DEG C, and vacuum-sintering carries out 2-4 hours, then anneals 1.5 hours at 900 DEG C respectively, in 650 DEG C of double annealings
1 hour, finally obtain Sintered NdFeB magnet.
Embodiment 7
Dysprosium metal is put into a vacuum furnace, is passed through hydrogen, vacuum pressure 10-5Bar is heated to 380 DEG C, obtains dysprosium hydrogen
Then compound makees medium in nitrogen or inert gas shielding atmosphere with hexamethylene, dysprosium hydride ball milling is thin at 7 microns
These fine powders are then put into drying in the glove box of argon gas atmosphere, obtain dysprosium hydride fine powder by powder；The DyH that will be prepared3Add
It is added to Nd12.5Fe81.5B6In powder, adding proportion is Nd12.5Fe81.5B6The 2.8% of powder quality, equably with DyH3Powder is mixed
It closes uniform；By powder after evenly mixing magnetic induction intensity 4T pulsed magnetic field and 1200kg/cm2Under isostatic pressed, it is pressed into
Type obtains pressure embryo；Pressure embryo is placed in vacuum sintering furnace, rises to 1010 DEG C with the heating rate of 700 DEG C/h, then 100 DEG C/h
Heating rate rise to 1060 DEG C, 1060 DEG C of vacuum-sinterings carry out 2-4 hours, then anneal 2 hours at 900 DEG C respectively, 650
DEG C double annealing 1 hour, finally obtains Sintered NdFeB magnet.
Embodiment 8
Dysprosium metal is put into a vacuum furnace, is passed through hydrogen, vacuum pressure 10-7Bar is heated to 370 DEG C, obtains dysprosium hydrogen
Compound, it is using jet-stream wind mill that dysprosium hydride ball milling is thin at 5 microns then or in nitrogen or inert gas shielding atmosphere
These fine powders are then put into drying in the glove box of argon gas atmosphere, obtain dysprosium hydride fine powder by powder；The DyH that will be prepared3Add
It is added to Nd12.5Fe81.5B6In powder, adding proportion is Nd10Fe80B10The 1% of powder quality, equably with DyH3Powder mixing is equal
It is even；By powder after evenly mixing magnetic induction intensity 5T pulsed magnetic field and 1400kg/cm2Under isostatic pressed, compression moulding obtains
To pressure embryo；Pressure embryo is placed in vacuum sintering furnace, rises to 1010 DEG C with the heating rate of 700 DEG C/h, then the heating of 100 DEG C/h
Rate rises to 1060 DEG C, and vacuum-sintering carries out 2-4 hours, then anneals 1 hour at 900 DEG C respectively, in 650 DEG C of double annealings 2
Hour, the final sintered NdFeB magnetic that obtains is kicked.
Embodiment 9
Dysprosium metal is put into a vacuum furnace, is passed through hydrogen, vacuum pressure 10-7Bar is heated to 420 DEG C, obtains dysprosium hydrogen
Then compound makees medium in nitrogen or inert gas shielding atmosphere with hexamethylene, dysprosium hydride ball milling is thin at 4 microns
These fine powders are then put into drying in the glove box of argon gas atmosphere, obtain dysprosium hydride fine powder by powder；The DyH that will be prepared3Add
It is added to Nd12.5Fe81.5B6In powder, adding proportion is Nd12Fe81.5B6The 4% of powder quality, equably with DyH3Powder mixing is equal
It is even；By powder after evenly mixing magnetic induction intensity 6T pulsed magnetic field and 1300kg/cm2Under isostatic pressed, compression moulding obtains
To pressure embryo；Pressure embryo is placed in vacuum sintering furnace, rises to 1010 DEG C with the heating rate of 600 DEG C/h, then the heating of 50 DEG C/h
Rate rises to 1060 DEG C, and vacuum-sintering carries out 2-4 hours, then anneals 1.5 hours at 900 DEG C respectively, in 650 DEG C of double annealings
2 hours, finally obtain Sintered NdFeB magnet.
Embodiment 10
Dysprosium metal is put into a vacuum furnace, is passed through hydrogen, vacuum pressure 10-8Bar is heated to 450 DEG C, obtains dysprosium hydrogen
Compound, then in nitrogen or inert gas shielding atmosphere using jet-stream wind mill by dysprosium hydride ball milling at 6 microns of fine powder,
These fine powders are then put into drying in the glove box of argon gas atmosphere, obtain dysprosium hydride fine powder；The DyH that will be prepared3Addition
To Nd12.5Fe81.5B6In powder, adding proportion is Nd12.5Fe81.5B6The 1.5% of powder quality, equably with DyH3Powder mixes
Uniformly；By powder after evenly mixing magnetic induction intensity 4.8T pulsed magnetic field and 1100kg/cm2Under isostatic pressed, it is pressed into
Type obtains pressure embryo；Pressure embryo is placed in vacuum sintering furnace, rises to 1010 DEG C with the heating rate of 600 DEG C/h, then 150 DEG C/h
Heating rate rise to 1060 DEG C, vacuum-sintering carries out 2-4 hours, then anneals 2 hours at 900 DEG C respectively, secondary at 650 DEG C
Annealing 1.5 hours, finally obtains Sintered NdFeB magnet.
Embodiment 11
Dysprosium metal is put into a vacuum furnace, is passed through hydrogen, vacuum pressure 10-58bar is heated to 460 DEG C, obtains dysprosium
Then hydride makees medium in nitrogen or inert gas shielding atmosphere with hexamethylene, dysprosium hydride ball milling is thin at 6 microns
These fine powders are then put into drying in the glove box of argon gas atmosphere, obtain dysprosium hydride fine powder by powder；The DyH that will be prepared3Add
It is added to Nd10Fe80B10In powder, adding proportion is Nd10Fe80B10The 1.6% of powder quality, equably with DyH3Powder mixing is equal
It is even；By powder after evenly mixing magnetic induction intensity 3.5T pulsed magnetic field and 1200kg/cm2Under isostatic pressed, compression moulding,
Obtain pressure embryo；Pressure embryo is placed in vacuum sintering furnace, rises to 1010 DEG C with the heating rate of 700 DEG C/h, then the liter of 150 DEG C/h
Warm rate rises to 1060 DEG C, and vacuum-sintering carries out 2-4 hours, then anneals 1 hour at 900 DEG C respectively, in 650 DEG C of double annealings
1 hour, finally obtain Sintered NdFeB magnet.
Embodiment 12
Dysprosium metal is put into a vacuum furnace, is passed through hydrogen, vacuum pressure 10-8Bar is heated to 430 DEG C, obtains dysprosium hydrogen
Compound, then in nitrogen or inert gas shielding atmosphere using jet-stream wind mill by dysprosium hydride ball milling at 5 microns of fine powder,
These fine powders are then put into drying in the glove box of argon gas atmosphere, obtain dysprosium hydride fine powder；The DyH that will be prepared3Addition
To Nd12.5Fe81.5B6In powder, adding proportion is Nd12Fe81.5B6The 3.6% of powder quality, equably with DyH3Powder mixing is equal
It is even；By powder after evenly mixing magnetic induction intensity 2.5T pulsed magnetic field and 1200kg/cm2Under isostatic pressed, compression moulding,
Obtain pressure embryo；Pressure embryo is placed in vacuum sintering furnace, rises to 1010 DEG C with the heating rate of 800 DEG C/h, then the liter of 150 DEG C/h
Warm rate rises to 1060 DEG C, and vacuum-sintering carries out 2-4 hours, then anneals 1 hour at 900 DEG C respectively, in 650 DEG C of double annealings
1 hour, finally obtain Sintered NdFeB magnet.
Embodiment 13
Dysprosium metal is put into a vacuum furnace, is passed through hydrogen, vacuum pressure 10-6Bar is heated to 400 DEG C, obtains dysprosium hydrogen
Then compound makees medium in nitrogen or inert gas shielding atmosphere with hexamethylene, dysprosium hydride ball milling is thin at 7 microns
These fine powders are then put into drying in the glove box of argon gas atmosphere, obtain dysprosium hydride fine powder by powder；The DyH that will be prepared3Add
It is added to Nd12.5Fe81.5B6In powder, adding proportion is Nd12.5Fe81.5B6The 3.5% of powder quality, equably with DyH3Powder is mixed
It closes uniform；By powder after evenly mixing magnetic induction intensity 5.5T pulsed magnetic field and 1300kg/cm2Under isostatic pressed, compacting
Molding obtains pressure embryo；Pressure embryo is placed in vacuum sintering furnace, 1010 DEG C are risen to the heating rate of 700 DEG C/h, then 150 DEG C/
The heating rate of h rises to 1060 DEG C, and vacuum-sintering carries out 2-4 hours, then anneals 1 hour at 900 DEG C respectively, at 650 DEG C two
Secondary annealing 1 hour, finally obtains Sintered NdFeB magnet.
Claims (8)
1. a kind of neodymium iron boron magnetic body containing dysprosium, forms through vacuum-sintering, it is characterised in that：Dysprosium contains in the neodymium iron boron magnetic body
Amount is 1-4wt%.
2. a kind of neodymium iron boron magnetic body containing dysprosium according to claim 1, it is characterised in that：Dysprosium in the neodymium iron boron magnetic body
Content is 2-3wt%.
3. a kind of preparation method of the neodymium iron boron magnetic body containing dysprosium described in claims 1 or 2, it is characterised in that include the following steps：
（1）Dysprosium metal is put into a vacuum furnace, is passed through hydrogen, vacuum pressure 10-5 -10-8 Bar is heated to 350-500
DEG C, obtain dysprosium hydride, medium is then made with hexamethylene in nitrogen or inert gas shielding atmosphere, by dysprosium hydride ball milling at
3-7 microns of fine powder, or use jet-stream wind mill that dysprosium hydride ball milling is micro- at 3-7 in nitrogen or inert gas shielding atmosphere
These fine powders are then put into drying in the glove box of argon gas atmosphere, obtain dysprosium hydride fine powder by the fine powder of rice；
（2）By step（1）In the dysprosium hydride fine powder for preparing content is added in neodymium iron boron powder by mass percentage, mixing
Uniformly；
（3）By step（2）By powder after evenly mixing magnetic induction intensity 1.8-6T pulsed magnetic field and 1000-1400
kg/cm2Isostatic pressed under compression moulding, obtain pressure embryo；
（4）Pressure embryo is placed in vacuum sintering furnace, 1010 DEG C are risen to the heating rate of 600-800 DEG C/h, then 50-150 DEG C/
The heating rate of h rises to 1060 DEG C, and vacuum-sintering 2-4 hours is then annealed 1-2 hours at 900 DEG C respectively, secondary at 650 DEG C
Annealing 1-2 hours, it is cooling, finally obtain neodymium iron boron magnetic body.
4. a kind of preparation method of the neodymium iron boron magnetic body containing dysprosium according to claim 3, it is characterised in that：The step（1）
In, the vacuum drying oven pressure is 10-8Bar, temperature are 450 DEG C.
5. a kind of preparation method of the neodymium iron boron magnetic body containing dysprosium according to claim 3, it is characterised in that：The step（1）
In, by dysprosium hydride ball milling at 4 microns of fine powder.
6. a kind of preparation method of the neodymium iron boron magnetic body containing dysprosium according to claim 3, it is characterised in that：The step（3）
In, the pulsed magnetic field and 1200 kg/cm of powder after evenly mixing in magnetic induction intensity 4.5T2Isostatic pressed under compression moulding.
7. a kind of preparation method of the neodymium iron boron magnetic body containing dysprosium according to claim 3, it is characterised in that：The step（4）
In, 1010 DEG C are risen to the heating rate of 700 DEG C/h, then with the heating rate of 100 DEG C/h to 1060 DEG C.
8. a kind of preparation method of neodymium iron boron magnetic body containing dysprosium, it is characterised in that：The step（4）In, first moved back at 900 DEG C
Fire 1 hour, then in 650 DEG C of double annealings 1 hour.
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| CN107403675A (en) * | 2017-07-25 | 2017-11-28 | 廊坊京磁精密材料有限公司 | A kind of preparation method of high thermal stability neodymium iron boron magnetic body |
| WO2017210957A1 (en) * | 2016-06-08 | 2017-12-14 | 浙江东阳东磁稀土有限公司 | Method for manufacturing rare-earth permanent magnetic material |
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