CN106409456B - A kind of rare earth permanent magnet preparation process improving magnetic property - Google Patents
A kind of rare earth permanent magnet preparation process improving magnetic property Download PDFInfo
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- CN106409456B CN106409456B CN201610739202.7A CN201610739202A CN106409456B CN 106409456 B CN106409456 B CN 106409456B CN 201610739202 A CN201610739202 A CN 201610739202A CN 106409456 B CN106409456 B CN 106409456B
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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
- H01F1/0573—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 obtained by reduction or by hydrogen decrepitation or embrittlement
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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
- H01F1/0576—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 pressed, e.g. hot working
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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
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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
- H01F41/0266—Moulding; Pressing
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- Crystallography & Structural Chemistry (AREA)
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- Manufacturing Cores, Coils, And Magnets (AREA)
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Abstract
The present invention relates to a kind of rare earth permanent magnet preparation processes improving magnetic property, belong to rareearth magnetic material preparing technical field.The preparation process includes mainly broken dispensing, melting, cast, hydrogen, airflow milling powder, magnetic field orientating and compression moulding, sintering and tempering, wherein the powder particles that airflow milling powder obtains are 1.5 4 μm, and powder concentration degree D90/D10 ratios are 45.The present invention improves the rare earth permanent magnet preparation process of magnetic property using powder metallurgic method, by the process conditions for controlling each step, including alloying component and microstructure control, control oxygen, crystal grain refinement control, magnetic field orientating control, sintering and the control of tempering, all linked with one another, each step will be that next step lays the first stone.Therefore, the present invention can be achieved the effect that magnetic property is improved by the improvement of production technology, to improve the stability of high-performance rare-earth permanent-magnetic, better meet the high-end needs with field under the premise of not increasing formulation cost.
Description
Technical field
The present invention relates to a kind of rare earth permanent magnet preparation processes more particularly to a kind of rare earth permanent magnet improving magnetic property to prepare work
Skill belongs to rareearth magnetic material preparing technical field.
Background technology
The utilization of rare earth permanent magnet is promoted from the utilizations such as simple loudspeaker, toy, bag buckle to mobile phone, new energy
The high-end fields such as automobile, servo motor.And the utilization in mobile phone, new-energy automobile, servo motor, especially mobile phone, it is desirable that magnetic
Steel product specification is small, magnetic property is high.Currently, the magnet steel in high-end handsets uses the highest trade mark in sintered NdFeB performance,
But the rapid advances of the high-end industry such as mobile phone, the requirement to magnetic property are also constantly improving.With the progress of production technology, pass
The remanent magnetism of the rare earth permanent-magnetic materials such as the sintered NdFeB of system has basically reached the limit of batch production, the only adjustment by being formulated
It has been extremely difficult to the effect that magnetic property greatly improves.In this regard, being badly in need of a kind of system improving rare earth permanent-magnetic material magnetic property of research and development
Standby technique achievees the effect that magnetic property improves by the improvement of production technology, to improve the stability of high-performance rare-earth permanent-magnetic,
Better meet the high-end needs with field.
Invention content
The purpose of the present invention is be directed to the above-mentioned problems in the prior art, it is proposed that a kind of not increase formulation cost
Under the premise of improve magnet magnetic property, especially high performance magnetic improve rare earth permanent magnet preparation process.
Object of the invention can be realized by the following technical scheme：A kind of rare earth permanent magnet preparation work improving magnetic property
Skill, includes mainly broken dispensing, melting, cast, hydrogen, airflow milling powder, magnetic field orientating and compression moulding, sintering and tempering, described
The powder particles that airflow milling powder obtains are 1.5-4 μm, and wherein powder concentration degree D90/D10 ratios are 4-5.
Powder concentration degree D90/D10 refers to 90% maximum particle size in powder and 10% powder maximum particle size value in the present invention
Ratio, D90/D10 ratios are smaller, and the consistency of powder is better.
It is 4-5 that the present invention, which controls powder particles and powder concentration degree D90/D10 ratios, and the granularity of powder is more concentrated, and is burnt
The Grain-Boundary Phase for tying blank is more consistent with main phase, and the sintering temperature of magnet is relatively low, magnet internal density relative equilibrium, consistency
High, magnet rich neodymium distributed mutually is balanced, this is more advantageous to the coercivity for improving magnet, that is, improves the high temperature resistance of magnet.
Preferably, the raw material chosen when the dispensing is 99.9% or more high pure raw material or pure raw material, reduce miscellaneous
Matter is brought into.
In a kind of rare earth permanent magnet preparation process of above-mentioned raising magnetic property, the airflow milling powder is in anti-oxidation gas
Protection is lower to be carried out.
In a kind of rare earth permanent magnet preparation process of above-mentioned raising magnetic property, the melting is less than 1Pa using vacuum degree
Ultrahigh vacuum heat melting.
In a kind of rare earth permanent magnet preparation process of above-mentioned raising magnetic property, described pour into a mould when obtained rejection tablet cools down is adopted
With copper roller chilling.
Preferably, the copper roller is by surface polishing treatment, the cooling water temperature of copper roller is 0-20 DEG C.
Preferably, the thickness for pouring into a mould obtained rejection tablet is between 0.15~0.3mm, the column crystal of rejection tablet uniformly divides
Cloth, without α iron and amorphous state, rejection tablet oxygen content is less than 100ppm.
The optimization of alloying component and its microstructure is the key that high performance sintered NdFeB permanent magnet, so of the invention
High pure raw material or pure raw material are not only used in material blending process, reduce the introducing of impurity to the greatest extent.Meanwhile that pours into a mould gets rid of
Pass through copper roller chilling when piece cools down, with obtain column crystal arrangement it is fine and closely woven it is neat, without α iron and amorphous rejection tablet.In addition, with getting rid of
The reduction of piece thickness, the temperature gradient between the scope of freedom and patch roll surface reduce, and the tissue inside rejection tablet is very fine uniformly, average
The thickness of flake crystalline crystal grain is 2.5-3.0 μm, and rich-Nd phase is evenly distributed between main phase grain, and the precipitation of α iron dendrite is complete
It is complete to inhibit.
In a kind of rare earth permanent magnet preparation process of above-mentioned raising magnetic property, adopted when the magnetic field orientating is with compression moulding
It is produced with alloy mold, mold uses high-purity iron material in the oriented surface for being close to press, and non-magnet material, mould are used in other faces
Inlay non-magnetic alloy thin slice in tool oriented surface both sides.So as to improve press magnetic field orientating field equilibrium degree, it is ensured that magnet
All directions are orientated uniformly complete.
In a kind of rare earth permanent magnet preparation process of above-mentioned raising magnetic property, the magnetic field orientating and compression moulding process
The middle control oxygen technique using 0~1000ppm of oxygen content.
In a kind of rare earth permanent magnet preparation process of above-mentioned raising magnetic property, burnt using carbon fiber in the sintering process
Tie basin.Because density is relatively low after sintering and molding neodymium iron boron, green compact are relatively soft, and carbon fiber sintering basin itself will not deform, Ke Yibao
Magnet deforms after card magnet will not lead to sintering process because of the deformation of sintering basin.It, can be in addition, carbon fiber has certain hole
Ensure that entrained antioxidant and other atmosphere distribute in sintered NdFeB high-temperature sintering process, do not influence magnet.And
The bad atmosphere of the yielding bending of iron sintering basin, the external world that are commonly used in the prior art easily influences the magnet performance in box, nothing
Method achievees the effect that carbon fiber is sintered basin, can not achieve the effect that magnetic property is improved by the improvement of production technology.
In a kind of rare earth permanent magnet preparation process of above-mentioned raising magnetic property, vacuum degree is less than in the sintering process
4.2*10-2The temperature of Pa, sintering are 1000~1100 DEG C, and the time of sintering is 4-6h.
In a kind of rare earth permanent magnet preparation process of above-mentioned raising magnetic property, the tempering includes primary tempering and secondary
Tempering, the temperature being once tempered are 850-950 DEG C, time 1-3h；The temperature of the double tempering is 450-550 DEG C,
Time is 2-5h.
The present invention improve magnetic property rare earth permanent magnet preparation process use powder metallurgic method, including all steps be one
A system engineering, all linked with one another, each step will lay the first stone for next step, once a step does not reach requirement,
The magnetic property of manufactured magnet cannot effectively improve or even manufactured magnet is waste product.The present invention is each by controlling
The process conditions of step, including alloying component and microstructure control, control oxygen, crystal grain refinement control, magnetic field orientating control, sintering
And the control of tempering, so that the magnetic property of magnet is improved.
Compared with prior art, the present invention is reached under the premise of not increasing formulation cost by the improvement of production technology
The effect that magnetic property improves better meets the high-end needs with field to improve the stability of high-performance rare-earth permanent-magnetic.
Specific implementation mode
The following is specific embodiments of the present invention, and technical scheme of the present invention will be further described, but the present invention is simultaneously
It is not limited to these embodiments.
Embodiment 1：
Use present invention process and conventionally produced N48 products：
Dispensing：
Melting, cast：Surface polishing is carried out to the copper roller of vacuum melting furnace first, then by various 99.9% high-purity former materials
Material is fitted into after directly being mixed by formulation weight requirement in vacuum rapid hardening smelting furnace, and vacuum rapid hardening smelting furnace is evacuated down to and is less than
When 0.1Pa, starts to heat melting, when material is rubescent in stove, be filled with argon gas, and increase temperature, 1440 DEG C of smelting temperature, until former material
Material melts completely, and refining is poured into a mould after ten minutes, and the cooling water temperature of copper roller is 10 DEG C and is then shut off power supply when cast, waits getting rid of
Piece is come out of the stove when being less than 80 DEG C, and rejection tablet average thickness is 0.25mm.
Hydrogen is broken：Rejection tablet is positioned in hydrogen crushing furnace, hydrogen is passed through, be warming up to after rejection tablet inhales hydrogen completely 550~600 DEG C, 6
Carry out dehydrogenation within~9 hours, the powder after dehydrogenation is come out of the stove when being cooled to 60 DEG C or less.
Airflow milling powder：The protective agent of powder addition 0.1% after the completion of dehydrogenation is mixed 1 hour, oxygen is put into and contains
Amount carries out powder processed for the high pure nitrogen protection air-flow mill less than 10ppm, and control powder average particle size (laser particle analyzer) exists
Between 1.5~4 μm, D90/D10 is between 4~5.This batch of powder will be ground to mix in stainless steel cylinder under high pure nitrogen protection,
0.1% gasoline is added when batch mixing：0.05% protective agent carries out 2h stirrings, ensures that batch mixing is uniform.Wherein, protective agent is by containing electron
Organic matter, borate and the gasoline of group form, and the organic matter containing electron donating group accounts for the 30% of protective agent total volume, borate
The 20% of protective agent total volume is accounted for, gasoline accounts for the 50% of protective agent total volume.
Magnetic field orientating and compression moulding：The powder being stirred is weighed by predetermined weight, is put into nitrogen protection closing press,
It being produced using alloy mold, mold uses high-purity iron material in the oriented surface for being close to press, and non-magnet material is used in other faces,
Non-magnetic alloy thin slice is inlayed in mold oriented surface both sides, controls 0~500ppm of oxygen content, two are orientated in the magnetic fields 40mm air gap 2T
It is secondary, then re-compacted, Vacuum Package after demagnetization, then the green compact of Vacuum Package are subjected to 150~200Mpa of isostatic pressed, pressurize 1~3
It is taken out after minute.
Sintering：Green compact are fitted into after nitrogen protection, oxygen content 0~300ppm glove boxes stripping oil in carbon fiber sintering basin,
It is put into sintering furnace and is less than 4.2*10 in vacuum degree-2Pa, temperature are to be sintered 5 hours at 1055 DEG C, and 2h are once tempered at 900 DEG C,
500 DEG C tempering 3 hours after take out, Sintered NdFeB magnet process complete.
By the above process and conventionally produced N48 Sintered NdFeB magnets, after surface grinding, forever according to GB/T3217
Magnetic (Hard Magnetic) magnetic properties of material testing method regulation is detected, and magnetic property is：
The remanent magnetism of production technology through the invention, product improves 0.017T, substantially increases product especially high-performance and produces
The performance of product.
Embodiment 2：
Use present invention process and conventionally produced 45H products：
Dispensing：
Melting：Surface polishing is carried out to the copper roller of vacuum melting furnace first, then by various 99.9% or more high-purity former materials
Material is fitted into after directly being mixed by formulation weight requirement in vacuum rapid hardening smelting furnace, and vacuum rapid hardening smelting furnace is evacuated down to and is less than
When 0.1Pa, starts to heat melting, when material is rubescent in stove, be filled with argon gas, and increase temperature, 1450 DEG C of smelting temperature, until former material
Material melts completely, and refining is poured into a mould after ten minutes, and the cooling water temperature of copper roller is 10 DEG C and is then shut off power supply when cast, waits getting rid of
Piece is come out of the stove when being less than 80 DEG C, and rejection tablet average thickness is 0.24mm.
Hydrogen is broken：Alloy rejection tablet is positioned in hydrogen crushing furnace, hydrogen is passed through, 550~600 are warming up to after product inhales hydrogen completely
DEG C, carry out dehydrogenation within 6~9 hours, the powder after dehydrogenation comes out of the stove when being cooled to 60 DEG C or less.
Airflow milling powder：The protective agent of powder addition 0.1% after the completion of dehydrogenation is mixed 1.5 hours, oxygen is put into
Content is that the high pure nitrogen protection air-flow mill less than 20ppm carries out powder processed, control powder average particle size (laser particle analyzer)
Between 1.5~4 μm, D90/D10 is between 4~5.This batch of powder will be ground to mix in stainless steel cylinder under high pure nitrogen protection
It closes, when batch mixing adds 0.08% gasoline：0.06% protective agent carries out 1h stirrings, ensures that batch mixing is uniform.Wherein, protective agent by contain to
Organic matter, borate and the gasoline of electron group form, and the organic matter containing electron donating group accounts for the 30% of protective agent total volume, boron
Acid esters accounts for the 20% of protective agent total volume, and gasoline accounts for the 50% of protective agent total volume.
Magnetic field orientating and compression moulding：The powder being stirred is weighed by predetermined weight, is put into nitrogen protection closing press,
It being produced using alloy mold, mold uses high-purity iron material in the oriented surface for being close to press, and non-magnet material is used in other faces,
Non-magnetic alloy thin slice is inlayed in mold oriented surface both sides, controls 0~600ppm of oxygen content, two are orientated in the magnetic fields 40mm air gap 2T
It is secondary, then re-compacted, Vacuum Package after demagnetization, then the green compact of Vacuum Package are subjected to 150~200Mpa of isostatic pressed, pressurize 1~3
It is taken out after minute.
Sintering：Green compact are fitted into after nitrogen protection, oxygen content 0~300ppm glove boxes stripping oil in carbon fiber sintering basin,
It is put into sintering furnace and is less than 4.2*10 in vacuum degree-2It is sintered 5 hours under Pa, the sintering temperature that temperature is 1060 DEG C, at 900 DEG C one
Secondary tempering 2h, 520 DEG C tempering 3 hours after take out, Sintered NdFeB magnet process complete.
By the 45H Sintered NdFeB magnets that the above process and conventional processes produce, after surface grinding, forever according to GB/T3217
Magnetic (Hard Magnetic) magnetic properties of material testing method regulation is detected, and magnetic property is：
By the above same formula various processes, the remanent magnetism of present invention process product improves 0.023T, greatly improves
The performance of product.
Embodiment 3：
Use present invention process and conventionally produced 42SH products：
Dispensing：
Melting：Surface polishing is carried out to the copper roller of vacuum melting furnace first, then by various 99.9% or more high-purity former materials
Material is fitted into after directly being mixed by formulation weight requirement in vacuum rapid hardening smelting furnace, and vacuum rapid hardening smelting furnace is evacuated down to and is less than
When 0.1Pa, starts to heat melting, when material is rubescent in stove, be filled with argon gas, and increase temperature, 1455 DEG C of smelting temperature, until former material
Material melts completely, and refining is poured into a mould after ten minutes, and the cooling water temperature of copper roller is 8 DEG C and is then shut off power supply when cast, waits getting rid of
Piece is come out of the stove when being less than 80 DEG C, and rejection tablet average thickness is 0.26mm.
Hydrogen is broken：Alloy rejection tablet is positioned in hydrogen crushing furnace, hydrogen is passed through, 520~600 are warming up to after product inhales hydrogen completely
DEG C, carry out dehydrogenation within 6~9 hours, the powder after dehydrogenation comes out of the stove when being cooled to 60 DEG C or less.
Airflow milling powder：The protective agent of powder addition 0.1% after the completion of dehydrogenation is mixed 1.5 hours, oxygen is put into
Content is that the high pure nitrogen protection air-flow mill less than 25ppm carries out powder processed, control powder average particle size (laser particle analyzer)
Between 1.5~4 μm, D90/D10 is between 4~5.This batch of powder will be ground to mix in stainless steel cylinder under high pure nitrogen protection
It closes, when batch mixing adds 0.1% gasoline：0.05% protective agent carries out 1.5h stirrings, ensures that batch mixing is uniform.Wherein, protective agent is by containing
Organic matter, borate and the gasoline of electron donating group form, and the organic matter containing electron donating group accounts for the 30% of protective agent total volume,
Borate accounts for the 20% of protective agent total volume, and gasoline accounts for the 50% of protective agent total volume.
Magnetic field orientating and compression moulding：The powder being stirred is weighed by predetermined weight, is put into nitrogen protection closing press,
It being produced using alloy mold, mold uses high-purity iron material in the oriented surface for being close to press, and non-magnet material is used in other faces,
Non-magnetic alloy thin slice is inlayed in mold oriented surface both sides, controls 0~700ppm of oxygen content, two are orientated in the magnetic fields 40mm air gap 2T
It is secondary, then re-compacted, Vacuum Package after demagnetization, then the green compact of Vacuum Package are subjected to 150~200Mpa of isostatic pressed, pressurize 1~3
It is taken out after minute.
Sintering：Green compact are fitted into after nitrogen protection, oxygen content 0~300ppm glove boxes stripping oil in carbon fiber sintering basin,
It is put into sintering furnace and is less than 4.2*10 in vacuum degree-2It is sintered 5 hours under Pa, the sintering temperature that temperature is 1055 DEG C, at 900 DEG C one
Secondary tempering 2h, 520 DEG C tempering 3 hours after take out, Sintered NdFeB magnet process complete.
By the 42SH Sintered NdFeB magnets that the above process and conventional processes produce, after surface grinding, according to GB/T3217
Magnetic test method for permanent magnetic (hard magnetic) material regulation is detected, and magnetic property is：
By the above same formula various processes, the remanent magnetism of the product of present invention process production improves 0.021T, greatly
The big performance for improving product.
In above-described embodiment and its alternative, sintering temperature can also be 1000 DEG C, 1010 DEG C, 1020 DEG C, 1030
DEG C, 1040 DEG C, 1050 DEG C, 1065 DEG C, 1070 DEG C, 1080 DEG C, 1090 DEG C, 1100 DEG C, the time can also be 4h, 6h.
In above-described embodiment and its alternative, the temperature that is once tempered can also be 850 DEG C, 860 DEG C, 870 DEG C,
880 DEG C, 890 DEG C, 910 DEG C, 920 DEG C, 930 DEG C, 940 DEG C, 950 DEG C, the time can also be 1h, 3h.
In above-described embodiment and its alternative, the temperature of double tempering can also be 450 DEG C, 460 DEG C, 470 DEG C,
480 DEG C, 490 DEG C, 510 DEG C, 530 DEG C, 540 DEG C, 550 DEG C, the time can also be 2h, 4h, 5h.
Specific embodiment described herein is only an example for the spirit of the invention.Technology belonging to the present invention is led
The technical staff in domain can do various modifications or supplement to described specific embodiment or substitute by a similar method, but simultaneously
The spirit or beyond the scope defined by the appended claims of the present invention is not deviated by.
It is skilled to this field although present invention has been described in detail and some specific embodiments have been cited
For technical staff, as long as it is obvious that can make various changes or correct without departing from the spirit and scope of the present invention.
Claims (7)
- Include mainly that dispensing, melting, cast, hydrogen is broken, air-flow is ground 1. a kind of rare earth permanent magnet preparation process improving magnetic property Powder, magnetic field orientating and compression moulding, sintering and tempering, which is characterized in that the powder particles that the airflow milling powder obtains are 1.5-4 μm, wherein powder concentration degree D90/D10 ratios are 4-5；The magnetic field orientating is given birth to when compression moulding using alloy mold Production, mold use high-purity iron material in the oriented surface for being close to press, and non-magnet material, mold oriented surface both sides are used in other faces Inlay non-magnetic alloy thin slice；Basin is sintered using carbon fiber in the sintering process.
- 2. a kind of rare earth permanent magnet preparation process improving magnetic property according to claim 1, which is characterized in that the air-flow Powder-grinding carries out under anti-oxidation gas shield.
- 3. a kind of rare earth permanent magnet preparation process improving magnetic property according to claim 1, which is characterized in that the melting Ultrahigh vacuum using vacuum degree less than 1Pa heats melting.
- 4. a kind of rare earth permanent magnet preparation process improving magnetic property according to claim 1, which is characterized in that the cast Copper roller chilling is used when obtained rejection tablet cooling.
- 5. a kind of rare earth permanent magnet preparation process improving magnetic property according to claim 1, which is characterized in that the magnetic field The control oxygen technique for being orientated and using 0~1000ppm of oxygen content during compression moulding.
- 6. a kind of rare earth permanent magnet preparation process improving magnetic property according to claim 1, which is characterized in that the sintering Vacuum degree is less than 4.2*10 in the process-2The temperature of Pa, sintering are 1000~1100 DEG C, and the time of sintering is 4-6h.
- 7. a kind of rare earth permanent magnet preparation process improving magnetic property according to claim 1, which is characterized in that the tempering Including being once tempered and double tempering, the temperature being once tempered is 850-950 DEG C, time 1-3h；The double tempering Temperature be 450-550 DEG C, time 2-5h.
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| CN201610739202.7A CN106409456B (en) | 2016-08-26 | 2016-08-26 | A kind of rare earth permanent magnet preparation process improving magnetic property |
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| CN201610739202.7A CN106409456B (en) | 2016-08-26 | 2016-08-26 | A kind of rare earth permanent magnet preparation process improving magnetic property |
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| CN106409456A CN106409456A (en) | 2017-02-15 |
| CN106409456B true CN106409456B (en) | 2018-09-07 |
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| CN114188114A (en) * | 2021-11-15 | 2022-03-15 | 福建省长汀金龙稀土有限公司 | Sintered neodymium-iron-boron magnet material and preparation method and application thereof |
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| CN101178962A (en) * | 2007-09-18 | 2008-05-14 | 横店集团东磁股份有限公司 | Non-pressure preparation method of rare-earth-iron-boron sintered magnetic material |
| CN101850421A (en) * | 2010-06-23 | 2010-10-06 | 宁波永久磁业有限公司 | Molding device for NdFeB materials |
| CN201760594U (en) * | 2010-09-06 | 2011-03-16 | 宁德市星宇科技有限公司 | NdFeB molding die with uniform orientation magnetic field |
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| CN102110507B (en) * | 2010-12-16 | 2012-10-17 | 麦格昆磁（天津）有限公司 | Ultrafine particle neodymium iron boron magnetic powder |
| CN104174857B (en) * | 2014-09-03 | 2018-03-09 | 京磁材料科技股份有限公司 | A kind of air-flow Flour milling method of neodymium iron boron magnetic body |
| CN105261473A (en) * | 2015-11-05 | 2016-01-20 | 宁波同创强磁材料有限公司 | Method for sintering neodymium-iron-boron magnet |
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| CN101850421A (en) * | 2010-06-23 | 2010-10-06 | 宁波永久磁业有限公司 | Molding device for NdFeB materials |
| CN201760594U (en) * | 2010-09-06 | 2011-03-16 | 宁德市星宇科技有限公司 | NdFeB molding die with uniform orientation magnetic field |
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