CN106409456A - Rare earth permanent magnet preparation process for improving magnetic property - Google Patents
Rare earth permanent magnet preparation process for improving magnetic property Download PDFInfo
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- CN106409456A CN106409456A CN201610739202.7A CN201610739202A CN106409456A CN 106409456 A CN106409456 A CN 106409456A CN 201610739202 A CN201610739202 A CN 201610739202A CN 106409456 A CN106409456 A CN 106409456A
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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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- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Hard Magnetic Materials (AREA)
- Manufacturing Cores, Coils, And Magnets (AREA)
- Powder Metallurgy (AREA)
Abstract
The present invention relates to a rare earth permanent magnet preparation process for improving a magnetic property, belonging to the technical field of preparation of rare earth magnetic materials. The preparation process mainly comprises the steps of preparing raw materials, smelting, pouring, hydrogen decrepitating, airflow grinding to obtain powder, magnetic field orienting and press molding, and sintering and tempering. The particle size of the powder obtained through airflow grinding is 1.5-4 [mu]m. A powder concentration ratio, D90/D10, is 4-5. The rare earth permanent magnet preparation process for improving the magnetic property uses a powder metallurgy method. The process conditions of all steps are controlled, specifically, the alloy component and microstructure, oxygen, grain refinement, magnetic field orientation, sintering and tempering are controlled. All the steps are interlocked, and each step prepares for the next step. Through adoption of the method, the formula cost is not increased, and further, the magnetic property is improved based on improvement of the preparation process. The stability of the high performance rare earth permanent magnet is improved, so that the rare earth permanent magnet can further cater to high-end application fields.
Description
Technical field
The present invention relates to a kind of rare earth permanent magnet preparation technology, more particularly, to a kind of rare earth permanent magnet preparation work improving magnetic property
Skill, belongs to rareearth magnetic material preparing technical field.
Background technology
The utilization of rare earth permanent magnet, rises to mobile phone, new forms of energy from simple loudspeaker, toy, bag buckle etc. use
The high-end fields such as automobile, servomotor.And in mobile phone, new-energy automobile, servomotor, especially mobile phone with it is desirable to magnetic
Product made from steel specification is little, magnetic property is high.At present, the magnet steel in high-end handsets is all using 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 also improves continuous.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, only leans on the adjustment of formula
It has been extremely difficult to the effect that magnetic property is greatly improved.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, reaches the effect of magnetic property raising by the improvement of production technology, thus improving the stability of high-performance rare-earth permanent-magnetic,
Better meet the needs in high-end utilization field.
Content of the invention
The purpose of the present invention is for the above-mentioned problems in the prior art it is proposed that a kind of do not increase formulation cost
Under the premise of improve magnet magnetic property, especially high performance magnetic improve rare earth permanent magnet preparation technology.
The purpose of the present invention can be realized by following technical proposal：A kind of rare earth permanent magnet preparation work improving magnetic property
Skill, mainly includes that dispensing, melting, cast, hydrogen is broken, airflow milling powder, magnetic field orientating and compressing, sintering and be tempered, described
The powder particles that airflow milling powder obtains are 1.5-4 μm, and wherein powder concentration degree D90/D10 ratio is 4-5.
In the present invention, powder concentration degree D90/D10 refers to 90% maximum particle size in powder and 10% powder maximum particle size value
Ratio, D90/D10 ratio is less, and the concordance of powder is better.
It is 4-5 that the present invention controls powder particles and powder concentration degree D90/D10 ratio, and the granularity of powder is got over and concentrated, and burns
The Grain-Boundary Phase of knot blank is more consistent with principal phase, and the sintering temperature of magnet is relatively low, the internal density relative equilibrium of magnet, concordance
High, magnet rich neodymium distributed mutually equilibrium, this is more beneficial for improving the coercivity of magnet, that is, improve the resistance to elevated temperatures of magnet.
Preferably, the raw material chosen during described dispensing is more than 99.9% high pure raw material or pure raw material, reduce miscellaneous
The bringing into of matter.
In a kind of rare earth permanent magnet preparation technology of above-mentioned raising magnetic property, described airflow milling powder is in anti-oxidation gas
Carry out under protection.
In a kind of rare earth permanent magnet preparation technology of above-mentioned raising magnetic property, described melting adopts vacuum to be less than 1Pa
Ultrahigh vacuum heating melting.
In a kind of rare earth permanent magnet preparation technology of above-mentioned raising magnetic property, adopt during the rejection tablet cooling that described cast obtains
With copper roller chilling.
Preferably, described copper roller is through surface polishing, the cooling water temperature of copper roller is 0-20 DEG C.
Preferably, the thickness of rejection tablet that described cast obtains is between 0.15～0.3mm, the column crystal of rejection tablet uniformly divides
Cloth, no alpha ferrite and amorphous state, rejection tablet oxygen content is less than 100ppm.
The optimization of alloying component and its microstructure is the key of high performance sintered NdFeB permanent magnet, so the present invention
Not only adopt high pure raw material or pure raw material in material blending process, reduce the introducing of impurity as far as possible.Meanwhile, what cast obtained gets rid of
Through copper roller chilling during piece cooling, to obtain column crystal arrangement fine and closely woven neat, no alpha ferrite and amorphous rejection tablet.In addition, with getting rid of
The reduction of piece thickness, the thermograde between the scope of freedom and patch roll surface reduces, the very fine homogeneous of the tissue within rejection tablet, averagely
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 alpha ferrite dendrite is complete
Full suppression.
In a kind of rare earth permanent magnet preparation technology of above-mentioned raising magnetic property, described magnetic field orientating with compressing when adopt
Produced with alloy mold, mould adopts high-purity iron material in the oriented surface being close to press, adopts non-magnet material, mould in other faces
Non-magnetic alloy thin slice is inlayed in tool oriented surface both sides.Such that it is able to improve press magnetic field orientating field equilibrium degree it is ensured that magnet
All directions orientation is uniformly complete.
In a kind of rare earth permanent magnet preparation technology of above-mentioned raising magnetic property, described magnetic field orientating and compressing process
The control oxygen technique of middle employing oxygen content 0～1000ppm.
In a kind of rare earth permanent magnet preparation technology of above-mentioned raising magnetic property, carbon fiber in described sintering process, is adopted to burn
Knot 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
Card magnet will not lead to magnet deformation after sintering process because of sintering basin deformation.In addition, carbon fiber has certain hole, permissible
Ensure that in sintered NdFeB high-temperature sintering process, entrained antioxidant and other atmosphere distribute, do not affect magnet.And
The magnet performance that commonly used ferrum in prior art sinters the yielding bending of basin, extraneous bad atmosphere easily affects in box, no
Method is reached carbon fiber and sinters the effect of basin it is impossible to be reached the effect of magnetic property raising by the improvement of production technology.
In a kind of rare earth permanent magnet preparation technology of above-mentioned raising magnetic property, in described sintering process, vacuum is less than
4.2*10-2Pa, the temperature of sintering is 1000～1100 DEG C, and the time of sintering is 4-6h.
In a kind of rare earth permanent magnet preparation technology of above-mentioned raising magnetic property, described tempering includes once being tempered and secondary
Tempering, the described temperature being once tempered is 850-950 DEG C, and the time is 1-3h；The temperature of described double tempering is 450-550 DEG C,
Time is 2-5h.
The present invention improve magnetic property rare earth permanent magnet preparation technology adopt powder metallurgic method, including all steps be one
Individual system engineering, all linked with one another, each step will lay the first stone for next step, once a step is not reaching to require,
The magnetic property of the magnet made cannot effectively improve, or even the magnet made is waste product.It is each that the present invention passes through control
The process conditions of step, control including alloying component and microstructure, control oxygen, crystal grain refinement control, magnetic field orientating controls, sintering
And the control of tempering, so that the magnetic property of magnet is improved.
Compared with prior art, the present invention, on the premise of not increasing formulation cost, is reached by the improvement of production technology
The effect that magnetic property improves, thus improving the stability of high-performance rare-earth permanent-magnetic, better meets the needs in high-end utilization field.
Specific embodiment
The following is the specific embodiment of the present invention, technical scheme is further described, but the present invention is simultaneously
It is not limited to these embodiments.
Embodiment 1：
Using present invention process and conventionally produced N48 product：
Dispensing：
Melting, cast：First surface polishing is carried out to the copper roller of vacuum melting furnace, then by various 99.9% high-purity former materials
Material loads in vacuum rapid hardening smelting furnace after directly mixing by formulation weight requirement, vacuum rapid hardening smelting furnace is evacuated down to and is less than
During 0.1Pa, start melting of heating, when material is rubescent in stove, is filled with argon, and rises high temperature, 1440 DEG C of smelting temperature, until former material
Material melts completely, and refine was poured into a mould after 10 minutes, and during cast, the cooling water temperature of copper roller is then shut off power supply for 10 DEG C, waits to get 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, is passed through hydrogen, 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 less than 60 DEG C.
Airflow milling powder：Powder after the completion of dehydrogenation is added 0.1% protective agent mix and blend 1 hour, put into oxygen and contain
Amount is that the high pure nitrogen protection air-flow mill less than 10ppm carries out powder processed, controls powder particle mean size (laser particle analyzer) to exist
Between 1.5～4 μm, D90/D10 is between 4～5.Mix grinding this batch of powder in stainless steel cylinder under high pure nitrogen protection,
Add 0.1% gasoline during batch mixing：0.05% protective agent carries out 2h stirring it is ensured that batch mixing is uniform.Wherein, protective agent is by containing electron
The Organic substance of group, borate and gasoline composition, the Organic substance containing electron donating group accounts for the 30% of protective agent cumulative volume, borate
Account for the 20% of protective agent cumulative volume, gasoline accounts for the 50% of protective agent cumulative volume.
Magnetic field orientating with compressing：The powder being stirred is weighed by predetermined weight, puts in nitrogen protection closing press,
Produced using alloy mold, mould adopts high-purity iron material in the oriented surface being close to press, adopts non-magnet material in other faces,
Non-magnetic alloy thin slice is inlayed in mould oriented surface both sides, controls oxygen content 0～500ppm, is orientated two in 40mm air gap 2T magnetic field
Secondary, then re-compacted, Vacuum Package after demagnetization, then the green compact of Vacuum Package are carried out isostatic pressed 150～200Mpa, pressurize 1～3
Take out after minute.
Sintering：Green compact are protected in nitrogen, load in carbon fiber sintering basin after oxygen content 0～300ppm glove box stripping oil,
Put in sintering furnace and be less than 4.2*10 in vacuum-2Pa, temperature sinter 5 hours at being 1055 DEG C, are once tempered 2h at 900 DEG C,
500 DEG C of tempering were taken out after 3 hours, and Sintered NdFeB magnet operation completes.
By above operation and conventionally produced N48 Sintered NdFeB magnet, after surface grinding, according to GB/T3217 forever
Magnetic (Hard Magnetic) magnetism of material test method regulation is detected, magnetic property is：
By production technology of the present invention, the remanent magnetism of product improves 0.017T, substantially increases product especially high-performance and produces
The performance of product.
Embodiment 2：
Using present invention process and conventionally produced 45H product：
Dispensing：
Melting：First surface polishing is carried out to the copper roller of vacuum melting furnace, then by various more than 99.9% high-purity former materials
Material loads in vacuum rapid hardening smelting furnace after directly mixing by formulation weight requirement, vacuum rapid hardening smelting furnace is evacuated down to and is less than
During 0.1Pa, start melting of heating, when material is rubescent in stove, is filled with argon, and rises high temperature, 1450 DEG C of smelting temperature, until former material
Material melts completely, and refine was poured into a mould after 10 minutes, and during cast, the cooling water temperature of copper roller is then shut off power supply for 10 DEG C, waits to get 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, is passed through hydrogen, after product inhales hydrogen completely, be warming up to 550～600
DEG C, carry out dehydrogenation within 6～9 hours, the powder after dehydrogenation is come out of the stove when being cooled to less than 60 DEG C.
Airflow milling powder：Powder after the completion of dehydrogenation is added 0.1% protective agent mix and blend 1.5 hours, put into oxygen
Content is that the high pure nitrogen protection air-flow mill less than 20ppm carries out powder processed, controls powder particle mean size (laser particle analyzer)
Between 1.5～4 μm, D90/D10 is between 4～5.Mixed in stainless steel cylinder under high pure nitrogen protection by grinding this batch of powder
Close, during batch mixing, add 0.08% gasoline：0.06% protective agent carries out 1h stirring it is ensured that batch mixing is uniform.Wherein, protective agent is by containing giving
The Organic substance of electron group, borate and gasoline composition, the Organic substance containing electron donating group accounts for the 30% of protective agent cumulative volume, boron
Acid esters accounts for the 20% of protective agent cumulative volume, and gasoline accounts for the 50% of protective agent cumulative volume.
Magnetic field orientating with compressing：The powder being stirred is weighed by predetermined weight, puts in nitrogen protection closing press,
Produced using alloy mold, mould adopts high-purity iron material in the oriented surface being close to press, adopts non-magnet material in other faces,
Non-magnetic alloy thin slice is inlayed in mould oriented surface both sides, controls oxygen content 0～600ppm, is orientated two in 40mm air gap 2T magnetic field
Secondary, then re-compacted, Vacuum Package after demagnetization, then the green compact of Vacuum Package are carried out isostatic pressed 150～200Mpa, pressurize 1～3
Take out after minute.
Sintering：Green compact are protected in nitrogen, load in carbon fiber sintering basin after oxygen content 0～300ppm glove box stripping oil,
Put in sintering furnace and be less than 4.2*10 in vacuum-2Pa, temperature are to sinter 5 hours under 1060 DEG C of sintering temperature, at 900 DEG C one
Secondary tempering 2h, 520 DEG C of tempering were taken out after 3 hours, and Sintered NdFeB magnet operation completes.
The 45H Sintered NdFeB magnet producing by above operation and conventional processes, after surface grinding, according to GB/T3217 forever
Magnetic (Hard Magnetic) magnetism of material test method regulation is detected, magnetic property is：
By same formula various processes above, the remanent magnetism of present invention process product improves 0.023T, greatly improves
The performance of product.
Embodiment 3：
Using present invention process and conventionally produced 42SH product：
Dispensing：
Melting：First surface polishing is carried out to the copper roller of vacuum melting furnace, then by various more than 99.9% high-purity former materials
Material loads in vacuum rapid hardening smelting furnace after directly mixing by formulation weight requirement, vacuum rapid hardening smelting furnace is evacuated down to and is less than
During 0.1Pa, start melting of heating, when material is rubescent in stove, is filled with argon, and rises high temperature, 1455 DEG C of smelting temperature, until former material
Material melts completely, and refine was poured into a mould after 10 minutes, and during cast, the cooling water temperature of copper roller is then shut off power supply for 8 DEG C, waits to get 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, is passed through hydrogen, after product inhales hydrogen completely, be warming up to 520～600
DEG C, carry out dehydrogenation within 6～9 hours, the powder after dehydrogenation is come out of the stove when being cooled to less than 60 DEG C.
Airflow milling powder：Powder after the completion of dehydrogenation is added 0.1% protective agent mix and blend 1.5 hours, put into oxygen
Content is that the high pure nitrogen protection air-flow mill less than 25ppm carries out powder processed, controls powder particle mean size (laser particle analyzer)
Between 1.5～4 μm, D90/D10 is between 4～5.Mixed in stainless steel cylinder under high pure nitrogen protection by grinding this batch of powder
Close, during batch mixing, add 0.1% gasoline：0.05% protective agent carries out 1.5h stirring it is ensured that batch mixing is uniform.Wherein, protective agent is by containing
The Organic substance of electron donating group, borate and gasoline composition, the Organic substance containing electron donating group accounts for the 30% of protective agent cumulative volume,
Borate accounts for the 20% of protective agent cumulative volume, and gasoline accounts for the 50% of protective agent cumulative volume.
Magnetic field orientating with compressing：The powder being stirred is weighed by predetermined weight, puts in nitrogen protection closing press,
Produced using alloy mold, mould adopts high-purity iron material in the oriented surface being close to press, adopts non-magnet material in other faces,
Non-magnetic alloy thin slice is inlayed in mould oriented surface both sides, controls oxygen content 0～700ppm, is orientated two in 40mm air gap 2T magnetic field
Secondary, then re-compacted, Vacuum Package after demagnetization, then the green compact of Vacuum Package are carried out isostatic pressed 150～200Mpa, pressurize 1～3
Take out after minute.
Sintering：Green compact are protected in nitrogen, load in carbon fiber sintering basin after oxygen content 0～300ppm glove box stripping oil,
Put in sintering furnace and be less than 4.2*10 in vacuum-2Pa, temperature are to sinter 5 hours under 1055 DEG C of sintering temperature, at 900 DEG C one
Secondary tempering 2h, 520 DEG C of tempering were taken out after 3 hours, and Sintered NdFeB magnet operation completes.
The 42SH Sintered NdFeB magnet producing by above operation and conventional processes, after surface grinding, according to GB/T3217
Permanent magnetism (Hard Magnetic) magnetism of material test method regulation is detected, magnetic property is：
By same formula various processes above, the remanent magnetism of the product that present invention process produces improves 0.021T, greatly
Improve greatly the performance of product.
In above-described embodiment and its alternative, sintering temperature can also for 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 for 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 for 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 explanation for example to present invention spirit.The affiliated technology of the present invention is led
The technical staff in domain can be made various modifications or supplement or substituted using similar mode to described specific embodiment, but simultaneously
Do not deviate by the spirit of the present invention or surmount scope defined in appended claims.
Although the present invention has been made a detailed description and has been cited with some specific embodiments, skilled to this area
For technical staff, as long as it is obvious for can making various changes without departing from the spirit and scope of the present invention or revise.
Claims (9)
1. a kind of rare earth permanent magnet preparation technology improving magnetic property, mainly includes that dispensing, melting, cast, hydrogen is broken, air-flow grinds
Powder, magnetic field orientating and compressing, sintering and tempering are it is characterised in that the powder particles that described airflow milling powder obtains are
1.5-4 μm, wherein powder concentration degree D90/D10 ratio is 4-5.
2. a kind of rare earth permanent magnet preparation technology improving magnetic property according to claim 1 is it is characterised in that described air-flow
Powder-grinding is carried out under anti-oxidation gas shield.
3. a kind of rare earth permanent magnet preparation technology improving magnetic property according to claim 1 is it is characterised in that described melting
Melting is heated using the ultrahigh vacuum that vacuum is less than 1Pa.
4. a kind of rare earth permanent magnet preparation technology improving magnetic property according to claim 1 is it is characterised in that described cast
Copper roller chilling is adopted during the rejection tablet cooling obtaining.
5. a kind of rare earth permanent magnet preparation technology improving magnetic property according to claim 1 is it is characterised in that described magnetic field
Produced using alloy mold when being orientated and be compressing, mould adopts high-purity iron material in the oriented surface being close to press, in other
Face adopts non-magnet material, and non-magnetic alloy thin slice is inlayed in mould oriented surface both sides.
6. according to claim 1 or 5 a kind of rare earth permanent magnet preparation technology improving magnetic property it is characterised in that described
Magnetic field orientating with compressing during using oxygen content 0～1000ppm control oxygen technique.
7. a kind of rare earth permanent magnet preparation technology improving magnetic property according to claim 1 is it is characterised in that described sintering
During using carbon fiber sinter basin.
8. a kind of rare earth permanent magnet preparation technology of the raising magnetic property according to claim 1 or 7 is it is characterised in that described
In sintering process, vacuum is less than 4.2*10-2Pa, the temperature of sintering is 1000～1100 DEG C, and the time of sintering is 4-6h.
9. a kind of rare earth permanent magnet preparation technology improving magnetic property according to claim 1 is it is characterised in that described tempering
Including once tempering and double tempering, the described temperature being once tempered is 850-950 DEG C, and the time is 1-3h；Described double tempering
Temperature be 450-550 DEG C, the time be 2-5h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610739202.7A CN106409456B (en) | 2016-08-26 | 2016-08-26 | A kind of rare earth permanent magnet preparation process improving magnetic property |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610739202.7A CN106409456B (en) | 2016-08-26 | 2016-08-26 | A kind of rare earth permanent magnet preparation process improving magnetic property |
Publications (2)
| Publication Number | Publication Date |
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| CN106409456A true CN106409456A (en) | 2017-02-15 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112927911A (en) * | 2019-12-06 | 2021-06-08 | 宁波科宁达工业有限公司 | Preparation method of magnet |
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