CN107887091A - A kind of neodymium iron boron magnetic body containing dysprosium and its method for preparation - Google Patents
A kind of neodymium iron boron magnetic body containing dysprosium and its method for preparation Download PDFInfo
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- 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
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- H01F1/053—Alloys characterised by their composition containing rare earth metals
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- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
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- 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
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- 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
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Abstract
A kind of method that the present invention provides neodymium iron boron magnetic body containing dysprosium and its preparation, magnet forms by mass percentage is：Pr：5~8%；Nd：19~21%；Dy：4~5%；B：0.9~1.0%；Al：0.1~0.9%；Cu：0.1~0.2%；Zr：0.1~0.15%；Surplus is Fe.The preparation method of the present invention is included in the broken process of the hydrogen after slab melting adds fritter Dy Fe alloys again, powder Dy in final sintering is replaced with Pr and/or Nd, is enclosed in around principal phase, and form Nd-rich phase on principal phase border.Preparation method of the present invention significantly improves the coercivity and corrosion resistance of neodymium iron boron magnetic body, reduces magnet high temperature demagnetizing factor in the case where reducing heavy rare earth use ratio.
Description
Technical field
The present invention relates to magnet preparing technical field, the method for more particularly to a kind of neodymium iron boron magnetic body containing dysprosium and its preparation.
Background technology
Nineteen eighty-two, Japanese Scientists Masato Sagawa are found that a kind of new rare earth permanent-magnetic material-neodymium iron boron
Nd2Fe14B, there is excellent comprehensive magnetic energy as sintered Nd-Fe-B permanent magnetic material prepared by principal phase using the material, just promote
The fields such as electronics, electric machinery, Medical Instruments, packaging, hardware machinery, computer, Aero-Space, ocean engineering and Chemical Engineering
Technology rapid development.
In recent years as Nd-Fe-B rare earth permanent magnetic material application market is constantly widened with going deep into, to sintered Nd-Fe-B permanent magnetic material
Requirement more and more higher, should performance it is high, cost is low again.Lot of domestic and foreign scholar carries out one after another prepares high-performance, low cost
The research of Nd-Fe-B rare earth permanent magnetic material.
In conventional method, high-coercive force product is prepared, need to add more heavy rare earth during dispensing, to reach coercivity lifting
Purpose, but the influence brought therewith, it is the loss of remanent magnetism.In conventional method, heavy rare earth is largely combined with B, Fe, without very
Good formation Nd-rich phase, it is impossible to which formation causes to improve coercitive preferable crystal boundary condition, i.e. Nd-rich phase is enclosed in principal phase week
Enclose.
And as rare earth price rapidly rises, in addition conventional method prepare neodymium iron boron magnetic body, heavy rare earth ratio is big, greatly
The big production cost for adding sintered NdFeB motor magnet, but invention is studied in order to reduce production cost, do not changing work
In the case of skill, the properties of product degradation that the heavy rare earth in dispensing is produced is reduced merely.Meanwhile motor product pair
The requirement that high temperature subtracts magnetic is higher, and the high temperature demagnetizing factor of existing neodymium iron boron magnetic body is still too high.
The content of the invention
It is an object of the invention to overcome drawbacks described above, there is provided one kind can reduce production cost while improve magnet coercive
The neodymium iron boron magnetic body containing dysprosium of power and its method for preparation.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention is：
The present invention provides a kind of neodymium iron boron magnetic body containing dysprosium, and the neodymium iron boron magnetic body containing dysprosium forms by mass percentage is：Pr：
5~8%；Nd：19~21%；Dy：4~5%；B：0.9~1.0%；Al：0.1~0.9%；Cu：0.1~0.2%；Zr：0.1
~0.15%；Surplus is Fe.
The present invention also provides a kind of preparation method of the above-mentioned neodymium iron boron magnetic body containing dysprosium, comprises the following steps：
Step 1：Prepare raw metal：Pr-Nd alloys, Dy-Fe alloys, B-Fe alloys, Zr-Fe alloys, Al, Cu and Fe,
The raw metal has the elemental constituent of following element percentage example：Pr：5~8%；Nd：19~21%；Dy：4~5%；B：
0.9~1.0%；Al：0.1~0.9%；Cu：0.1~0.2%；Zr：0.1~0.15%；Surplus is Fe；
Under vacuum, Pr-Nd alloys, B-Fe alloys, Zr-Fe alloys, Al, Cu and Fe melting are made into thickness is
0.25~0.30mm slab；
Step 2：By Dy-Fe alloy raw materials, 3cm~5cm fritter is cut into, together with the slab then obtained with step 1
Put into hydrogen crushing furnace, the dehydrogenation under the conditions of 500~750 DEG C after the broken disproportionated reaction of hydrogen, obtain hydrogen flour material and alloying pellet；
Step 3：The hydrogen flour material and alloying pellet that step 2 is obtained carry out powder processed under nitrogen protection, obtain 3~5 μm
Alloy powder, then mixed with antioxidant, lubricant and gasoline, obtain fine powder；
Step 4：Step 3 gained fine powder is put into Magnetic field press, under nitrogen protection and under more than 1.9T magnetic field intensity
Oriented moulding obtains pressed compact；
Step 5：Pressed compact after step 4 is molded is put into isostatic pressing machine, is kept under 18~20MPa pressure
10-20s；
Step 6：By in the pressed compact input vacuum sintering furnace handled by step 5, vacuumize, in 1040~1090 DEG C of conditions
Lower sintering, constant temperature keep 4~5h；
Step 7：Product after step 6 the is sintered Ageing Treatment 2h in 900~920 DEG C of environment under vacuum, so
4.5~5.5h of Ageing Treatment obtains target product in 450~520 DEG C of environment under vacuum afterwards.
The beneficial effects of the present invention are：(1) for the relatively conventional method of the inventive method, the use of heavy rare earth is reduced
Amount, has saved production cost；(2) the inventive method makes powder most by adding fritter Dy-Fe alloys in breaking process in hydrogen again
Dy replaces with Pr and/or Nd during sintering eventually, is enclosed in around principal phase, and forms Nd-rich phase on principal phase border, significantly
The coercivity and corrosion resistance of magnet are improved, meanwhile, it is smaller on remanent magnetism influence, also reduce magnet high temperature demagnetizing factor；(3) originally
The coercivity and corrosion resistance of invention magnet are good, and high temperature demagnetizing factor is low.
Embodiment
To describe the technology contents of the present invention, construction feature, the objects and the effects in detail, below in conjunction with embodiment
It is explained in detail.
The design of most critical of the present invention is：Production cost is reduced by reducing the use ratio of Dy-Fe alloys, together
When, add fritter Dy-Fe alloys again in hydrogen breaks process, powder Dy in final sintering is replaced with Pr and/or Nd, wrap
Be trapped among around principal phase, and principal phase border formed Nd-rich phase to improve the coercivity of magnet, meanwhile, on remanent magnetism influence compared with
It is small.
The present invention provides a kind of neodymium iron boron magnetic body containing dysprosium, and the neodymium iron boron magnetic body containing dysprosium forms by mass percentage is：
Pr：5~8%；Nd：19~21%；Dy：4~5%；B：0.9~1.0%；Al：0.1~0.9%；Cu：0.1~
0.2%；Zr：0.1~0.15%；Surplus is Fe.
It was found from foregoing description, the beneficial effects of the present invention are：The coercivity and corrosion resistance of magnet of the present invention are good, high
Warm demagnetizing factor is low, and production cost is lower.
Further, the neodymium iron boron magnetic body containing dysprosium forms by mass percentage is：Pr：19.5~20.5%；Nd：6~
7%；Dy：4~4.5%；B：0.9~1.0%；Al：0.6~0.8%；Cu：0.1~0.2%；Zr：0.1~0.15%；Surplus
For Fe.
Further, the neodymium iron boron magnetic body containing dysprosium forms by mass percentage is：Pr：20.1%；Nd：6.7%；Dy：
4.2%；B：0.95%；Al：0.7%；Cu：0.2%；Zr：0.1%；Surplus is Fe.
The present invention also provides a kind of preparation method of the above-mentioned neodymium iron boron magnetic body containing dysprosium, comprises the following steps：
Step 1：Prepare raw metal：Pr-Nd alloys, Dy-Fe alloys, B-Fe alloys, Zr-Fe alloys, Al, Cu and Fe,
The raw metal has the elemental constituent of following element percentage example：Pr：5~8%；Nd：19~21%；Dy：4~5%；B：
0.9~1.0%；Al：0.1~0.9%；Cu：0.1~0.2%；Zr：0.1~0.15%；Surplus is Fe；
Under vacuum, Pr-Nd alloys, B-Fe alloys, Zr-Fe alloys, Al, Cu and Fe melting are made into thickness is
0.25~0.30mm slab；
Step 2：By Dy-Fe alloy raw materials, 3cm~5cm fritter is cut into, together with the slab then obtained with step 1
Put into hydrogen crushing furnace, (pressure gauge of equipment shows that pressure is constant, then represents disproportionated reaction and terminate) exists after the broken disproportionated reaction of hydrogen
Dehydrogenation under the conditions of 500~750 DEG C, obtain hydrogen flour material and alloying pellet；
Step 3：The hydrogen flour material and alloying pellet that step 2 is obtained carry out powder processed under nitrogen protection, obtain 3~5 μm
Alloy powder, then mixed with antioxidant, lubricant and gasoline, obtain fine powder；
Step 4：Step 3 gained fine powder is put into Magnetic field press, under nitrogen protection and under more than 1.9T magnetic field intensity
Oriented moulding obtains pressed compact；
Step 5：Pressed compact after step 4 is molded is put into isostatic pressing machine, is kept under 18~20MPa pressure
10-20s；
Step 6：By in the pressed compact input vacuum sintering furnace handled by step 5, vacuumize, in 1040~1090 DEG C of conditions
Lower sintering, constant temperature keep 4~5h；
Step 7：Product after step 6 the is sintered Ageing Treatment 2h in 900~920 DEG C of environment under vacuum, so
4.5~5.5h of Ageing Treatment obtains target product in 450~520 DEG C of environment under vacuum afterwards.
The present invention operation principle be：The electron spectrum point of the sintered NdFeB rare-earth permanent magnet material prepared from conventional method
Analysis has fcc structure as can be seen that magnet crystal boundary center is rich-Nd phase, and B content is low, and O, Nd content are high, thickness 5-10nm,
It is relevant with the Nd contents of magnet, it is change.There is unusual contrast Grain-Boundary Phase both sides, and its thickness is 10-20nm, its Nd content compared with
Height, O and C content are higher, form the transition region between Grain-Boundary Phase and principal phase, i.e. frontier district.The composition of frontier district deviates principal phase (2:
14:1) composition, structure is also imperfect, i.e., defective, turns into defect area, and anisotropy field is low, in the presence of magnetic reversal field,
The area easily forms magnetic reversal farmland core, therefore the coercivity of magnet made from conventional method is bad.And the present invention breaks process in hydrogen
Middle addition Dy-Fe alloys, compared to Dy-Fe alloys are directly added directly in fusion process, the dosage of heavy rare earth can be saved, is reduced
Production cost, meanwhile, after Dy-Fe alloys crush with slab hydrogen, 3~5 μm of fine powder is worn into by airflow milling, by three-dimensional blender
Machine, Dy-Fe alloys fine powder and slab fine powder are well mixed, carry out shaping compacting, last sintered timeliness, in sintering process
In, Dy replaces with Pr and/or Nd, is enclosed in around principal phase, improve it is coercitive simultaneously, reduction to magnetic energy product compared with
It is few, the dosage of heavy rare earth is substantially reduced, improves the corrosion resistance of magnet.
It was found from foregoing description, the beneficial effects of the present invention are：(1) for the relatively conventional method of the inventive method, drop
The low usage amount of heavy rare earth, has saved production cost；(2) the inventive method by adding fritter Dy- again in breaking process in hydrogen
Fe alloys, powder Dy in final sintering is replaced with Pr and/or Nd, be enclosed in around principal phase, and on principal phase border
Nd-rich phase is formed, significantly improves the coercivity and corrosion resistance of magnet, meanwhile, it is smaller on remanent magnetism influence, also reduce magnetic
Body high temperature demagnetizing factor.
Further, the concrete operations of step 1 are：Raw metal in addition to Dy-Fe is put into vacuum induction speed in proportion
Solidifying slab stove, is vacuumized, and after melting to raw metal thawing under the conditions of 1000~1450 DEG C after electromagnetic agitation is uniform, is poured
Onto the water-cooled copper roller of rotation, the rotating speed that adjusts water-cooled copper roller is that to obtain thickness be 0.25~0.30mm to 2300~2700r/min
Slab.
Further, the concrete operations of step 3 are：The hydrogen flour material and alloying pellet that step 2 is obtained are protected in nitrogen
Under be added in airflow milling, 3~5 μm of alloy powder is ground into through airflow milling, by alloy powder, antioxidant, lubricant and
Gasoline is placed in powder material tank together, and powder material tank then is placed on into stirring more than 3h on three-dimensional material mixer.
Further, the temperature of dehydrogenation is 650 DEG C in step 2；In step 6, the temperature of sintering is 1070 DEG C, and constant temperature is kept
5h。
Further, Pr mass percent is 20.8~27.59% in the Pr-Nd alloys；In the Dy-Fe alloys
Dy mass percent is 80%；B mass percent is the quality hundred of Zr in 18%, Zr-Fe alloys in the B-Fe alloys
Divide than being 65%.
Embodiment 1
A kind of neodymium iron boron magnetic body containing dysprosium, the neodymium iron boron magnetic body containing dysprosium forms by mass percentage is：Pr：5%；Nd：
19%；Dy：4%；B：0.9%；Al：0.1%；Cu：0.1%；Zr：0.1%；Fe：70.8%；
The preparation method of above-mentioned magnet comprises the following steps：
Step 1：Prepare raw metal：Pr-Nd alloys, Dy-Fe alloys, B-Fe alloys, Zr-Fe alloys, Al, Cu and Fe,
Wherein, Pr is added in the form of Pr-Nd alloys, and Pr mass percent is 20.83% in Pr-Nd alloys；Dy is with Dy-Fe alloys
Form add, Dy mass percent is 80% in Dy-Fe alloys；B is added in the form of B-Fe alloys, B in B-Fe alloys
Mass percent for 18%, Zr is added in the form of Zr-Fe alloys, Zr mass percent is 65% in Zr-Fe alloys, its
His raw material is analytically pure metal.To ensure that each alloying element content is stable in product, need to estimate the actual damage of raw material in advance
Consumption, actual each material quality of weighing are：Pr-Nd alloys：24kg, Dy-Fe alloy：5kg, B-Fe alloy：5kg, Zr-Fe alloy：
0.154kg, Al：0.1kg, Cu:0.1kg, Fe:65.646kg；
By Pr-Nd alloys, B-Fe alloys, Zr-Fe alloys, Al, Cu and Fe input vacuum induction rapid hardening slab stove, take out true
Sky, after melting to raw metal thawing under the conditions of 1000 DEG C after electromagnetic agitation is uniform, it is poured into the water-cooled copper roller of rotation,
The rotating speed for adjusting water-cooled copper roller is 2700r/min, obtains the slab that thickness is 0.25mm；
Step 2：By Dy-Fe alloy raw materials, 3cm fritter is cut into, hydrogen is put into together with the slab then obtained with step 1
In broken stove, the dehydrogenation under the conditions of 500 DEG C after the broken disproportionated reaction of hydrogen, hydrogen flour material and alloying pellet are obtained；
Step 3：Hydrogen flour material and alloying pellet that step 2 obtains are added in airflow milling under nitrogen protection, through gas
Stream milling is broken into 3 μm of alloy powder, alloy powder, antioxidant, lubricant and gasoline is placed in powder material tank together, then
Powder material tank is placed on stirring more than 3h on three-dimensional material mixer；
Step 4：By step 3 gained fine powder put into Magnetic field press, under nitrogen protection (oxygen content is not higher than 1000ppm) and
Oriented moulding obtains pressed compact under 1.9T magnetic field intensity；
Step 5：Pressed compact after step 4 is molded is put into isostatic pressing machine, and 20s is kept under 19.5MPa pressure；
Step 6：By in the pressed compact input vacuum sintering furnace handled by step 5, vacuumize, burnt under the conditions of 1040 DEG C
Knot, constant temperature keep 5h；
Step 7：Product after step 6 the is sintered Ageing Treatment 2h in 900 DEG C of environment under vacuum, then true
Ageing Treatment 5.5h obtains target product in 450 DEG C of environment under empty condition.
Detection：The magnetic parameter of test product, the results are shown in Table 1.
Embodiment 2
A kind of neodymium iron boron magnetic body containing dysprosium, the neodymium iron boron magnetic body containing dysprosium forms by mass percentage is：Pr：8%；Nd：
21%；Dy：5%；B：1.0%；Al：0.9%；Cu：0.2%；Zr：0.15%；Fe：63.75%；
The preparation method of above-mentioned magnet comprises the following steps：
Step 1：Prepare raw metal：Pr-Nd alloys, Dy-Fe alloys, B-Fe alloys, Zr-Fe alloys, Al, Cu and Fe,
Wherein, Pr is added in the form of Pr-Nd alloys, and Pr mass percent is 27.59% in Pr-Nd alloys；Dy is with Dy-Fe alloys
Form add, Dy mass percent is 80% in Dy-Fe alloys；B is added in the form of B-Fe alloys, B in B-Fe alloys
Mass percent for 18%, Zr is added in the form of Zr-Fe alloys, Zr mass percent is 65% in Zr-Fe alloys, its
His raw material is analytically pure metal.To ensure that each alloying element content is stable in product, need to estimate the actual damage of raw material in advance
Consumption, actual each material quality of weighing are：Pr-Nd alloys：29kg, Dy-Fe alloy：6.25kg, B-Fe alloy：5.556kg Zr-
Fe alloys：0.2308kg, Al：0.9kg, Cu:0.2kg, Fe:57.8632kg；
By Pr-Nd alloys, B-Fe alloys, Zr-Fe alloys, Al, Cu and Fe input vacuum induction rapid hardening slab stove, take out true
Sky, after melting to raw metal thawing under the conditions of 1000 DEG C after electromagnetic agitation is uniform, it is poured into the water-cooled copper roller of rotation,
The rotating speed for adjusting water-cooled copper roller is 2300r/min, obtains the slab that thickness is 0.30mm；
Step 2：By Dy-Fe alloy raw materials, 5cm fritter is cut into, hydrogen is put into together with the slab then obtained with step 1
In broken stove, the dehydrogenation under the conditions of 750 DEG C after the broken disproportionated reaction of hydrogen, hydrogen flour material and alloying pellet are obtained；
Step 3：Hydrogen flour material and alloying pellet that step 2 obtains are added in airflow milling under nitrogen protection, through gas
Stream milling is broken into 5 μm of alloy powder, alloy powder, antioxidant, lubricant and gasoline is placed in powder material tank together, then
Powder material tank is placed on stirring more than 3h on three-dimensional material mixer；
Step 4：By step 3 gained fine powder put into Magnetic field press, under nitrogen protection (oxygen content is not higher than 1000ppm) and
Oriented moulding obtains pressed compact under 2.0T magnetic field intensity；
Step 5：Pressed compact after step 4 is molded is put into isostatic pressing machine, and 10s is kept under 20.5MPa pressure；
Step 6：By in the pressed compact input vacuum sintering furnace handled by step 5, vacuumize, burnt under the conditions of 1090 DEG C
Knot, constant temperature keep 4.5h；
Step 7：Product after step 6 the is sintered Ageing Treatment 2h in 900 DEG C of environment under vacuum, then true
Ageing Treatment 4h obtains target product in 520 DEG C of environment under empty condition.
Detection：The magnetic parameter of test product, the results are shown in Table 1.
Embodiment 3
A kind of neodymium iron boron magnetic body containing dysprosium, the neodymium iron boron magnetic body containing dysprosium forms by mass percentage is：Pr：6.7%；Nd：
20.1%；Dy：4.2%；B：0.95%；Al：0.7%；Cu：0.2%；Zr：0.1%；Fe：67.05%；
The preparation method of above-mentioned magnet comprises the following steps：
Step 1：Prepare raw metal：Pr-Nd alloys, Dy-Fe alloys, B-Fe alloys, Zr-Fe alloys, Al, Cu and Fe,
Wherein, Pr is added in the form of Pr-Nd alloys, and Pr mass percent is 25% in Pr-Nd alloys；Dy is with Dy-Fe alloys
Form adds, and Dy mass percent is 80% in Dy-Fe alloys；B is added in the form of B-Fe alloys, B in B-Fe alloys
Mass percent is that 18%, Zr is added in the form of Zr-Fe alloys, and Zr mass percent is 65% in Zr-Fe alloys, other
Raw material is analytically pure metal.To ensure that each alloying element content is stable in product, need to estimate raw material active loss in advance,
Reality weighs each material quality：Pr-Nd alloys：26.8kg, Dy-Fe alloy：5.25kg, B-Fe alloy：5.278kg Zr-Fe
Alloy：0.1538kg, Al：0.7kg, Cu:0.2kg, Fe:61.6182kg；
By Pr-Nd alloys, B-Fe alloys, Zr-Fe alloys, Al, Cu and Fe input vacuum induction rapid hardening slab stove, take out true
Sky, after melting to raw metal thawing under the conditions of 1435 DEG C after electromagnetic agitation is uniform, it is poured into the water-cooled copper roller of rotation,
The rotating speed for adjusting water-cooled copper roller is 2700r/min, obtains the slab that thickness is 0.25mm；
Step 2：By Dy-Fe alloy raw materials, 4.5cm fritter is cut into, is put into together with the slab then obtained with step 1
In hydrogen crushing furnace, the dehydrogenation under the conditions of 500 DEG C after the broken disproportionated reaction of hydrogen, hydrogen flour material and alloying pellet are obtained；
Step 3：Hydrogen flour material and alloying pellet that step 2 obtains are added in airflow milling under nitrogen protection, through gas
Stream milling is broken into 4.5 μm of alloy powder, alloy powder, antioxidant, lubricant and gasoline is placed in powder material tank together, so
Powder material tank is placed on stirring more than 3h on three-dimensional material mixer afterwards；
Step 4：By step 3 gained fine powder put into Magnetic field press, under nitrogen protection (oxygen content is not higher than 1000ppm) and
Oriented moulding obtains pressed compact under 1.95T magnetic field intensity；
Step 5：Pressed compact after step 4 is molded is put into isostatic pressing machine, and 15s is kept under 20MPa pressure；
Step 6：By in the pressed compact input vacuum sintering furnace handled by step 5, vacuumize, burnt under the conditions of 1070 DEG C
Knot, constant temperature keep 5h；
Step 7：Product after step 6 the is sintered Ageing Treatment 2h in 910 DEG C of environment under vacuum, then true
Ageing Treatment 5h obtains target product in 485 DEG C of environment under empty condition.
Detection：The magnetic parameter of test product, the results are shown in Table 1.
Comparative example
A kind of preparation method of neodymium iron boron magnetic body containing dysprosium, comprises the following steps：
Step 1：Prepare raw metal：Pr-Nd alloys, Dy-Fe alloys, B-Fe alloys, Zr-Fe alloys, Al, Cu and Fe,
Wherein, Pr is added in the form of Pr-Nd alloys, and Pr mass percent is 25% in Pr-Nd alloys；Dy is with Dy-Fe alloys
Form adds, and Dy mass percent is 80% in Dy-Fe alloys；B is added in the form of B-Fe alloys, B in B-Fe alloys
Mass percent is that 18%, Zr is added in the form of Zr-Fe alloys, and Zr mass percent is 65% in Zr-Fe alloys, other
Raw material is analytically pure metal.To ensure that each alloying element content is stable in product, need to estimate raw material active loss in advance,
Reality weighs each material quality：Pr-Nd alloys：26.8kg, Dy-Fe alloy：6.25kg, B-Fe alloy：5.278kg Zr-Fe
Alloy：0.1538kg, Al：0.7kg, Cu:0.2kg, Fe:60.6182kgkg；
By Pr-Nd alloys, Dy-Fe alloys, B-Fe alloys, Zr-Fe alloys, Al, Cu and Fe input vacuum induction rapid hardening casting
Piece stove, is vacuumized, and after melting to raw metal thawing under the conditions of 1435 DEG C after electromagnetic agitation is uniform, is poured into the water of rotation
On cold copper roller, the rotating speed for adjusting water-cooled copper roller is 2700r/min, obtains the slab that thickness is 0.25mm；
Step 2：In the slab input hydrogen crushing furnace that step 1 is obtained, taken off after the broken disproportionated reaction of hydrogen under the conditions of 500 DEG C
Hydrogen, obtain hydrogen flour material and alloying pellet；
Step 3：Hydrogen flour material and alloying pellet that step 2 obtains are added in airflow milling under nitrogen protection, through gas
Stream milling is broken into 4.5 μm of alloy powder, alloy powder, antioxidant, lubricant and gasoline is placed in powder material tank together, so
Powder material tank is placed on stirring more than 3h on three-dimensional material mixer afterwards；
Step 4：By step 3 gained fine powder put into Magnetic field press, under nitrogen protection (oxygen content is not higher than 1000ppm) and
Oriented moulding obtains pressed compact under 1.95T magnetic field intensity；
Step 5：Pressed compact after step 4 is molded is put into isostatic pressing machine, and 15s is kept under 20MPa pressure；
Step 6：By in the pressed compact input vacuum sintering furnace handled by step 5, vacuumize, burnt under the conditions of 1070 DEG C
Knot, constant temperature keep 5h；
Step 7：Product after step 6 the is sintered Ageing Treatment 2h in 910 DEG C of environment under vacuum, then true
Ageing Treatment 5h obtains target product in 485 DEG C of environment under empty condition.
Detection：The magnetic parameter of test product, the results are shown in Table 1.
The parameter of the 1~embodiment of embodiment 3 of table 1 and comparative example product.
As shown in Table 1, the inventive method can significantly improve HCJ and squareness, reduce high temperature and subtract magnetic
Rate, performance are more preferable.
In summary, neodymium iron boron magnetic body containing dysprosium provided by the invention and its method for preparation, the inventive method are relatively conventional
For method, the usage amount of heavy rare earth is reduced, has saved production cost；The inventive method by adding again in breaking process in hydrogen
Fritter Dy-Fe alloys, powder Dy in final sintering is replaced with Pr and/or Nd, be enclosed in around principal phase, and in master
Phase boundray forms Nd-rich phase, significantly improves the coercivity and corrosion resistance of magnet, meanwhile, it is smaller on remanent magnetism influence, also drop
Low magnet high temperature demagnetizing factor；The coercivity and corrosion resistance of magnet of the present invention are good, and high temperature demagnetizing factor is low.
Embodiments of the invention are the foregoing is only, are not intended to limit the scope of the invention, it is every to utilize this hair
The equivalent structure or equivalent flow conversion that bright description is made, or directly or indirectly it is used in other related technology necks
Domain, it is included within the scope of the present invention.
Claims (8)
1. a kind of neodymium iron boron magnetic body containing dysprosium, it is characterised in that the neodymium iron boron magnetic body containing dysprosium forms by mass percentage is：
Pr：5~8%；Nd：19~21%；Dy：4~5%；B：0.9~1.0%；Al：0.1~0.9%；Cu：0.1~0.2%；
Zr：0.1~0.15%；Surplus is Fe.
2. neodymium iron boron magnetic body containing dysprosium according to claim 1, it is characterised in that the neodymium iron boron magnetic body containing dysprosium presses quality hundred
Divide than composition and be：Pr：19.5~20.5%；Nd：6~7%；Dy：4~4.5%；B：0.9~1.0%；Al：0.6~0.8%；
Cu：0.1~0.2%；Zr：0.1~0.15%；Surplus is Fe.
3. neodymium iron boron magnetic body containing dysprosium according to claim 1, it is characterised in that the neodymium iron boron magnetic body containing dysprosium presses quality hundred
Divide than composition and be：Pr：20.1%；Nd：6.7%；Dy：4.2%；B：0.95%；Al：0.7%；Cu：0.2%；Zr：0.1%；It is remaining
Measure as Fe.
4. the preparation method of a kind of neodymium iron boron magnetic body containing dysprosium, it is characterised in that comprise the following steps：
Step 1：Prepare raw metal：Pr-Nd alloys, Dy-Fe alloys, B-Fe alloys, Zr-Fe alloys, Al, Cu and Fe, it is described
Raw metal has the elemental constituent of following element percentage example：Pr：5~8%；Nd：19~21%；Dy：4~5%；B：0.9
~1.0%；Al：0.1~0.9%；Cu：0.1~0.2%；Zr：0.1~0.15%；Surplus is Fe；
Under vacuum, by Pr-Nd alloys, B-Fe alloys, Zr-Fe alloys, Al, Cu and Fe melting be made thickness for 0.25~
0.30mm slab；
Step 2：Dy-Fe alloys are cut into 3~5cm fritter, hydrogen crushing furnace is put into together with the slab then obtained with step 1
In, the dehydrogenation under the conditions of 500~750 DEG C after the broken disproportionated reaction of hydrogen, obtain hydrogen flour material and alloying pellet；
Step 3：The hydrogen flour material and alloying pellet that step 2 is obtained carry out powder processed under nitrogen protection, obtain 3~5 μm of conjunction
Bronze end, then mixes with antioxidant, lubricant and gasoline, obtains fine powder；
Step 4：Step 3 gained fine powder is put into Magnetic field press, is orientated under nitrogen protection and under more than 1.9T magnetic field intensity
Shaping obtains pressed compact；
Step 5：Pressed compact after step 4 is molded is put into isostatic pressing machine, and 10- is kept under 18~20MPa pressure
20s；
Step 6：By in the pressed compact input vacuum sintering furnace handled by step 5, vacuumize, burnt under the conditions of 1040~1090 DEG C
Knot, constant temperature keep 4~5h；
Step 7：Product after step 6 is sintered Ageing Treatment 2h, Ran Hou in 900~920 DEG C of environment under vacuum
4.5~5.5h of Ageing Treatment obtains target product in 450~520 DEG C of environment under vacuum condition.
5. the preparation method of high-performance neodymium iron boron magnetic body containing dysprosium according to claim 4, it is characterised in that the tool of step 1
Gymnastics conduct：Raw metal in addition to Dy-Fe is put into vacuum induction rapid hardening slab stove in proportion, vacuumized, 1000~
After melting is melted to raw metal under the conditions of 1450 DEG C after electromagnetic agitation is uniform, it is poured into the water-cooled copper roller of rotation, adjusts
The rotating speed of water-cooled copper roller is that 2300~2700r/min obtains the slab that thickness is 0.25~0.30mm.
6. the preparation method of high-performance neodymium iron boron magnetic body containing dysprosium according to claim 4, it is characterised in that the tool of step 3
Gymnastics conduct：Hydrogen flour material and alloying pellet that step 2 obtains are added in airflow milling under nitrogen protection, are milled through air-flow
3~5 μm of alloy powder is broken into, alloy powder is placed in powder material tank together with antioxidant, lubricant and gasoline, then will
Powder material tank is placed on stirring more than 3h on three-dimensional material mixer.
7. the preparation method of high-performance neodymium iron boron magnetic body containing dysprosium according to claim 4, it is characterised in that taken off in step 2
The temperature of hydrogen is 650 DEG C；In step 6, the temperature of sintering is 1070 DEG C, and constant temperature keeps 5h.
8. the preparation method of high-performance neodymium iron boron magnetic body containing dysprosium according to claim 4, it is characterised in that the Pr-Nd
Pr mass percent is 20.8~27.59% in alloy；Dy mass percent is 80% in the Dy-Fe alloys；It is described
B mass percent is 18% in B-Fe alloys, Zr mass percent is 65% in Zr-Fe alloys.
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