CN115331942A - Method for manufacturing samarium-cobalt magnet based on vacuum rapid hardening furnace - Google Patents
Method for manufacturing samarium-cobalt magnet based on vacuum rapid hardening furnace Download PDFInfo
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- CN115331942A CN115331942A CN202211029985.1A CN202211029985A CN115331942A CN 115331942 A CN115331942 A CN 115331942A CN 202211029985 A CN202211029985 A CN 202211029985A CN 115331942 A CN115331942 A CN 115331942A
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- rapid hardening
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- hardening furnace
- cobalt magnet
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- 229910000938 samarium–cobalt magnet Inorganic materials 0.000 title claims abstract description 81
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 20
- 229910052751 metal Inorganic materials 0.000 claims abstract description 92
- 239000002184 metal Substances 0.000 claims abstract description 92
- 238000003723 Smelting Methods 0.000 claims abstract description 54
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 53
- 229910052802 copper Inorganic materials 0.000 claims abstract description 53
- 239000010949 copper Substances 0.000 claims abstract description 53
- 239000002994 raw material Substances 0.000 claims abstract description 46
- 239000013589 supplement Substances 0.000 claims abstract description 39
- 238000001816 cooling Methods 0.000 claims abstract description 31
- 239000000843 powder Substances 0.000 claims abstract description 31
- 238000005245 sintering Methods 0.000 claims abstract description 31
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229910052772 Samarium Inorganic materials 0.000 claims abstract description 28
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 claims abstract description 28
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 15
- 238000005303 weighing Methods 0.000 claims abstract description 13
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 12
- 239000010941 cobalt Substances 0.000 claims abstract description 12
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 12
- 230000032683 aging Effects 0.000 claims abstract description 11
- 239000006104 solid solution Substances 0.000 claims abstract description 10
- 238000000465 moulding Methods 0.000 claims abstract description 7
- 238000003825 pressing Methods 0.000 claims abstract description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 48
- 239000000463 material Substances 0.000 claims description 36
- 239000002245 particle Substances 0.000 claims description 33
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 30
- 238000010438 heat treatment Methods 0.000 claims description 28
- 229910052757 nitrogen Inorganic materials 0.000 claims description 24
- 229910052786 argon Inorganic materials 0.000 claims description 16
- 229910052742 iron Inorganic materials 0.000 claims description 14
- 239000013078 crystal Substances 0.000 claims description 10
- 238000011049 filling Methods 0.000 claims description 10
- 239000007789 gas Substances 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 7
- 241001062472 Stokellia anisodon Species 0.000 claims description 4
- 230000003064 anti-oxidating effect Effects 0.000 claims description 4
- 239000000314 lubricant Substances 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 4
- 238000007670 refining Methods 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 238000009461 vacuum packaging Methods 0.000 claims description 3
- 229910001093 Zr alloy Inorganic materials 0.000 claims 1
- 238000002844 melting Methods 0.000 claims 1
- 230000008018 melting Effects 0.000 claims 1
- 238000010008 shearing Methods 0.000 claims 1
- 239000007788 liquid Substances 0.000 abstract description 4
- KPLQYGBQNPPQGA-UHFFFAOYSA-N cobalt samarium Chemical compound [Co].[Sm] KPLQYGBQNPPQGA-UHFFFAOYSA-N 0.000 abstract description 2
- 229910045601 alloy Inorganic materials 0.000 description 7
- 239000000956 alloy Substances 0.000 description 7
- 238000007711 solidification Methods 0.000 description 7
- 230000008023 solidification Effects 0.000 description 7
- 238000005204 segregation Methods 0.000 description 3
- 238000009826 distribution Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 229910000640 Fe alloy Inorganic materials 0.000 description 1
- NDUKHFILUDZSHZ-UHFFFAOYSA-N [Fe].[Zr] Chemical compound [Fe].[Zr] NDUKHFILUDZSHZ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011362 coarse particle Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000010902 jet-milling Methods 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
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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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- 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
- H01F1/0555—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 pressed, sintered or bonded together
- H01F1/0557—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
The invention relates to the technical field of samarium cobalt permanent magnets and discloses a method for manufacturing a samarium cobalt magnet based on a vacuum rapid hardening furnace; respectively weighing samarium, cobalt, pure iron, electrolytic copper and sponge zirconium as smelting raw materials, and weighing samarium accounting for 1-2% of the smelting raw materials by mass as a burning loss supplement; putting a smelting raw material and a burning loss supplement into a crucible of a vacuum rapid hardening furnace, smelting into a metal liquid, pouring into a tundish, making the metal liquid into a metal sheet after the metal liquid is contacted with a water-cooled copper roller at the bottom of the tundish, cooling the metal sheet to prepare a samarium cobalt magnet throwing sheet, further crushing the samarium cobalt magnet throwing sheet into 4-6 mu m powder by a jaw crusher, a vacuum belt screen ball mill and an air flow mill, performing orientation pressing molding on the powder in a magnetic field, pressing the powder into a green body by a cold isostatic press, and performing vacuum sintering, solid solution treatment and aging treatment on the green body to prepare the samarium cobalt magnet; the invention has the advantages of increasing the thickness of the samarium cobalt magnet melt-spun piece and improving the magnet performance of the samarium cobalt magnet.
Description
Technical Field
The invention belongs to the technical field of samarium cobalt permanent magnets, and relates to a method for manufacturing a samarium cobalt magnet based on a vacuum rapid hardening furnace.
Background
The type 2.
At present, the production process of the 2. The alloy ingot prepared by vacuum induction smelting has the advantages that the thickness of the ingot is large, the thickness of a commonly used plate-shaped ingot is 8-50 mm, the size of a solidification structure crystal grain is generally 20-100 mu m, and the size of the alloy ingot crystal grain is large, so that if the alloy ingot is prepared by using an air flow mill, the production efficiency is extremely low, the size and the distribution of powder are poor, and the economical efficiency is poor. Meanwhile, the component segregation in the thick solidification structure is serious, and the magnetic performance is further reduced; when the alloy melt-spun sheet is prepared by using a conventional vacuum rapid hardening furnace, the thickness of the melt-spun sheet is usually 0.2-0.5 mm, although the segregation of components of a solidification structure is small, the grain size of the solidification structure is 2-5 mu m, and because the grains are too thin, a single jet milling powder body contains a plurality of solidification grains, the orientation degree of a magnet is reduced, the remanence is reduced, and the performance of the magnet is seriously influenced.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a method for manufacturing the samarium cobalt magnet based on the vacuum rapid hardening furnace, wherein the formula of the samarium cobalt magnet and the preparation process of the melt-spun piece are organically combined, so that the thickness and the grain diameter of the melt-spun piece of the samarium cobalt magnet are increased, and the performance of the samarium cobalt magnet prepared by the melt-spun piece of the samarium cobalt magnet is improved.
The invention is realized by the following technical scheme:
a method for manufacturing a samarium cobalt magnet based on a vacuum rapid hardening furnace comprises the following steps by mass percent:
s1, weighing 24-27% of metal samarium, 40-50% of metal cobalt, 18-25% of pure iron, 4-10% of electrolytic copper and 2-5% of sponge zirconium as smelting raw materials, and weighing 1-2% of metal samarium in mass of the smelting raw materials as a burning loss supplement;
s2, filling the smelting raw materials and the burning loss supplement into a crucible of a vacuum rapid hardening furnace; controlling a vacuum rapid hardening furnace to smelt the smelting raw material and the burning loss supplement material into molten metal;
s3, controlling the crucible in the vacuum rapid hardening furnace to incline, pouring molten metal in the crucible into a tundish at a speed of 800-2000 g/S, and enabling the depth of the molten metal in the tundish to be 70-120 mm;
the water-cooled copper roller rotates at a linear speed of 0.5-1.1 m/s, molten metal in the tundish is in contact with the surface of the water-cooled copper roller and then is solidified and crystallized to form a metal sheet, and the metal sheet is taken out from the tundish when the water-cooled copper roller rotates and is primarily cooled on the water-cooled copper roller;
the metal sheet slides into the rotary water-cooling disc from the surface of the water-cooling copper roller, and is rapidly cooled by the rotary water-cooling disc to prepare a samarium-cobalt magnet melt-spun sheet with the thickness of 0.50-2.0 mm and the grain size of a solidified tissue of 3-15 mu m;
s4, after cooling the samarium-cobalt magnet melt-spun piece to 60 ℃, opening an air discharge valve of the vacuum rapid hardening furnace, and standing for 30min to discharge the samarium-cobalt magnet melt-spun piece;
s5, placing the samarium-cobalt magnet melt-spun piece in a jaw crusher, and carrying out coarse crushing under the protection of nitrogen to prepare melt-spun piece particles with the particle size of 5-20 mm;
s6, putting the melt-spun sheet particles with the particle size of 5-20 mm into a vacuum ball mill with a sieve, vacuumizing, and then filling argon or nitrogen for secondary crushing, wherein the particle size of the coarse powder particles of the melt-spun sheet is 0.1-0.6 mm after crushing;
s7, adding 1-3 per mill of anti-oxidation lubricant RH-1 in percentage by mass into the coarse powder particles of the melt-spun sheets with the particle size of 0.1-0.6 mm, filling argon or nitrogen into a sealed mixer, stirring and mixing for 0.5-1 h to prepare middle broken materials, adding the middle broken materials into a grinding chamber of an airflow mill, enabling the middle broken materials to mutually collide, shear and grind under the drive of supersonic speed power medium gas sprayed from a nozzle of the airflow mill, crushing the middle broken materials into powder, and adjusting the rotating speed of a grading wheel to enable the particle size of the powder to be 4-6 mu m; adding the powder into a mixer, and mixing for 2-3 h;
s8, carrying out orientation pressing molding on the powder in a magnetic field with the magnetic field intensity of 1200-2400 KA/m, carrying out vacuum packaging after molding, and keeping the pressure for 10-120 seconds at 180-220 MPa by using a cold isostatic press to prepare a green body;
s9, placing the green body into a vacuum sintering furnace, continuously vacuumizing, slowly heating to 1190-1220 ℃, introducing argon gas to keep the pressure in the vacuum sintering furnace at 0-0.015 MPa, and carrying out heat preservation sintering for 70-120 min;
adjusting the temperature in the vacuum sintering furnace to 1150-1190 ℃ to perform solid solution treatment on the green body, wherein the treatment time is 1-20 h; after the solid solution treatment is finished, rapidly cooling the green body in the vacuum sintering furnace to room temperature by a cooling fan;
heating the temperature in the vacuum sintering furnace to 820-870 ℃, and carrying out aging treatment on the green body for 1-20 hours;
after the aging treatment is finished, the temperature in the vacuum sintering furnace is reduced to 350-450 ℃ at the speed of 0.5-1 ℃/min, the temperature is kept for 1-5 h, and the samarium cobalt magnet can be prepared by taking out the samarium cobalt magnet after being cooled to room temperature.
Further, in the step S3, a contact line between the inner bottom surface of the tundish and the outer circumferential surface of the water-cooled copper roller is marked as an x line, and an axial lead of the water-cooled copper roller is marked as a y line; the included angle between the plane of the x line and the y line and the horizontal plane passing through the y line is marked as alpha, and the alpha is 26-35 degrees.
Further, the water temperature at the water inlet of the water-cooling copper roller is 30-35 ℃, and the water temperature at the water outlet of the water-cooling copper roller is 55-70 ℃.
Further, in the S1, 24.7% of metal samarium, 47% of metal cobalt, 21% of pure iron, 4.9% of electrolytic copper and 2.4% of sponge zirconium are weighed as smelting raw materials in percentage by mass;
weighing samarium metal accounting for 1.2 percent of the mass of the smelting raw materials as a burning loss supplement.
Further, in S1, the pure iron and the sponge zirconium may also be a zirconium-iron alloy.
Further, in the step S2, the electrolytic copper and the sponge zirconium are placed at the bottom of the crucible, the metal cobalt and the pure iron are placed in the middle of the crucible, and the metal samarium in the smelting raw material and the metal samarium in the burning loss supplement are both placed at the top of the crucible.
Further, in S2, the specific steps of smelting the smelting raw material and the burnout supplement material into molten metal in the vacuum rapid hardening furnace are as follows:
continuously introducing nitrogen into the vacuum rapid hardening furnace, and continuously vacuumizing to keep the internal vacuum degree of the vacuum rapid hardening furnace at 1000-2000 Pa, wherein the nitrogen introduction and vacuumizing time is 30-50 min to remove the smelting raw materials, the burning loss supplement materials and the water on the inner surface of the crucible;
continuously vacuumizing to 610-1000 Pa, heating the smelting raw material and the burning loss supplement material in the crucible by using medium-frequency heating power of 40-60 KW, and simultaneously increasing the heating power at the speed of 2-4 KW/min to further remove the smelting raw material, the burning loss supplement material, the water on the surface of the crucible and the crystal water on the crucible;
when the temperature in the vacuum rapid hardening furnace is raised to 800 ℃, argon is continuously filled into the vacuum rapid hardening furnace, so that the vacuum degree in the vacuum rapid hardening furnace is kept between-0.035 MPa and-0.025 MPa, and the smelting volatilization loss of metal samarium is reduced;
when the temperature in the vacuum rapid hardening furnace is raised to 1400 ℃, the heating power of the vacuum rapid hardening furnace is reduced to 170-210 KW after the metal is liquefied and cleared, and the smelting raw material and the burning loss supplement are smelted into molten metal after refining for 18-26 min.
Further, in S3, when the temperature in the vacuum rapid hardening furnace is reduced to 1350 ℃, the heating power is reduced to 145-165 KW, the inclination of the crucible in the vacuum rapid hardening furnace is controlled, molten metal in the crucible is poured into the tundish at the speed of 800-2000 g/S, and the depth of the molten metal in the tundish is 70-120 mm.
Further, in S7, the supersonic motive medium gas is nitrogen.
Further, in S3, a baffle plate for preventing molten metal from rushing forward during pouring of the crucible is disposed between the crucible and the tundish.
Compared with the prior art, the invention has the following beneficial technical effects:
in the technical scheme of the invention, a samarium cobalt magnet alloy melt-spun sheet is prepared by a vacuum rapid hardening furnace, the melt-spun sheet is further crushed into 4-6 mu m superfine powder by a jaw crusher, a vacuum ball mill with a sieve and an airflow mill, the powder is pressed into a green body by a cold isostatic press after being oriented and molded in a magnetic field, and the green body is subjected to vacuum sintering, solid solution treatment and aging treatment to prepare the samarium cobalt magnet; when the samarium cobalt magnet alloy melt-spun piece is prepared, the pouring speed of the molten metal is increased to 800-2000 g/s, the depth of the molten metal in the tundish is increased to h = 70-120 mm, and the linear velocity of a water-cooling copper roller is reduced to 0.5-1.1 m/s; the temperature of a water inlet of the water-cooling copper roller is increased to 30-35 ℃, the temperature of a water outlet is reduced to 55-70 ℃, the temperature when metal liquid is poured is increased to 1350 ℃, so that the thickness of the prepared samarium-cobalt magnet melt-spun piece is increased, the thickness of the prepared samarium-cobalt magnet melt-spun piece is 0.5-2.0 mm, and the grain size of a solidification structure is 3-15 mu m; the problems that the thickness of a melt-spun sheet prepared by using a vacuum rapid hardening furnace in the current production process is 0.2-0.5 mm, so that crystal grains in a samarium-cobalt magnet melt-spun sheet are too thin, and the magnet performance is poor are solved; and the problems of large thickness and coarse grains (the thickness of the cast ingot is 8-50 mm, the grain size is 20-100 mu m), long time consumption in the crushing process, low efficiency, reduced magnetism caused by serious segregation of solidification structure components and the like can be solved.
Drawings
FIG. 1 is a schematic view of the structure of a water-cooled copper roller, a crucible and a tundish in the present invention;
FIG. 2 is a distribution plot of the solidified structure grains of the #1 samarium-cobalt magnet melt spun tab of example 1;
FIG. 3 is a graph of the solidified structure grains of a #2 samarium cobalt magnet slinger blade of example 1;
reference numerals: 1 is the crucible, 2 is keeping off the class board, 3 is the centre package, 4 is water-cooling copper roller, 5 is the x line, 6 is the y line, and 7 is samarium cobalt magnet melt-spun piece.
Detailed Description
The present invention will now be described in further detail with reference to the attached drawings, which are illustrative, but not limiting, of the present invention.
The invention discloses a method for manufacturing a samarium cobalt magnet based on a vacuum rapid hardening furnace, which comprises the following steps in percentage by mass:
s1, weighing 24-27% of metal samarium, 40-50% of metal cobalt, 18-25% of pure iron, 4-10% of electrolytic copper and 2-5% of sponge zirconium as smelting raw materials, and weighing 1-2% of metal samarium in mass of the smelting raw materials as a burning loss supplement;
specifically, 24.7% of metal samarium, 47% of metal cobalt, 21% of pure iron, 4.9% of electrolytic copper and 2.4% of sponge zirconium are weighed as smelting raw materials; weighing samarium metal accounting for 1.2 percent of the mass of the smelting raw materials as a burning loss supplement;
the pure iron and the sponge zirconium can also be ferrozirconium alloy;
s2, putting the smelting raw materials and the burning loss supplement into a crucible 1 of a vacuum rapid hardening furnace;
specifically, electrolytic copper and sponge zirconium are placed at the bottom of a crucible 1, metal cobalt and pure iron are placed in the middle of the crucible 1, and metal samarium in a smelting raw material and metal samarium in a burning loss supplement are both placed at the top of the crucible 1;
controlling a vacuum rapid hardening furnace to smelt the smelting raw material and the burning loss supplement material into molten metal;
specifically, the method for smelting the smelting raw material and the burning loss supplement material into molten metal by the vacuum rapid hardening furnace comprises the following specific steps:
continuously introducing nitrogen into the vacuum rapid hardening furnace, and continuously vacuumizing to keep the internal vacuum degree of the vacuum rapid hardening furnace at 1000-2000 Pa, wherein the nitrogen introduction and vacuumizing time is 30-50 min to remove the smelting raw materials, the burning loss supplement materials and the water on the inner surface of the crucible 1; continuously vacuumizing to 610-1000 Pa, heating the smelting raw material and the burning loss supplement material in the crucible 1 by using medium-frequency heating power of 40-60 KW, and simultaneously increasing the heating power at the speed of 2-4 KW/min to further remove the smelting raw material, the burning loss supplement material, the water on the surface of the crucible 1 and the crystal water on the surface of the crucible 1; when the temperature in the vacuum rapid hardening furnace is raised to 800 ℃, argon is continuously filled into the vacuum rapid hardening furnace, so that the vacuum degree in the vacuum rapid hardening furnace is kept between-0.035 MPa and-0.025 MPa, and the smelting volatilization loss of metal samarium is reduced; when the temperature in the vacuum rapid hardening furnace is raised to 1400 ℃, the heating power of the vacuum rapid hardening furnace is reduced to 170-210 KW after the metal is liquefied and cleared, and the smelting raw material and the burning loss supplement are smelted into molten metal after refining for 18-26 min;
s3, controlling the crucible 1 in the vacuum rapid hardening furnace to incline, pouring molten metal in the crucible 1 into the tundish 3 at the speed of 800-2000 g/S, and enabling the depth of the molten metal in the tundish 3 to be 70-120 mm; a baffle plate 2 for preventing molten metal from rushing forwards during crucible pouring is arranged between the crucible 1 and the tundish 3;
specifically, when the temperature in the vacuum rapid hardening furnace is reduced to 1350 ℃, the heating power is reduced to 145-165 KW, the crucible 1 in the vacuum rapid hardening furnace is controlled to incline, the molten metal in the crucible 1 is poured into the tundish 3 at the speed of 800-2000 g/s, and the depth of the molten metal in the tundish 3 is 70-120 mm;
the water-cooled copper roller 4 rotates at a linear speed of 0.5-1.1 m/s, the molten metal in the tundish 3 is in contact with the surface of the water-cooled copper roller 4 and then is solidified and crystallized to form a metal sheet, and the metal sheet is taken out from the tundish 3 when the water-cooled copper roller 4 rotates and is primarily cooled on the water-cooled copper roller 4;
specifically, a contact line between the inner bottom surface of the tundish 3 and the outer circular surface of the water-cooled copper roller 4 is marked as an x line 5, and an axial lead of the water-cooled copper roller 4 is marked as a y line 6;
the included angle between the plane of the x line 5 and the y line 6 and the horizontal plane passing through the y line 6 is marked as alpha which is 26-35 degrees.
The water temperature at the water inlet of the water-cooled copper roller 4 is 30-35 ℃, and the water temperature at the water outlet of the water-cooled copper roller 4 is 55-70 ℃;
the metal sheet slides into the rotary water-cooling disc from the surface of the water-cooling copper roller 4, and is rapidly cooled by the rotary water-cooling disc to prepare a samarium-cobalt magnet melt-spun sheet 7 with the thickness of 0.50-2.0 mm and the grain size of a solidified tissue of 3-15 mu m;
s4, after cooling the samarium-cobalt magnet melt-spun piece 7 to 60 ℃, opening an air release valve of the vacuum rapid hardening furnace, and standing for 30min to discharge;
s5, placing the samarium-cobalt magnet melt-spun piece 7 in a jaw crusher, and carrying out coarse crushing under the protection of nitrogen to prepare melt-spun piece particles with the particle size of 5-20 mm;
s6, putting the melt-spun sheet particles with the particle size of 5-20 mm into a vacuum ball mill with a sieve, vacuumizing, and then filling argon or nitrogen for secondary crushing, wherein the particle size of the coarse powder particles of the melt-spun sheet is 0.1-0.6 mm after crushing;
s7, adding 1-3 per mill of anti-oxidation lubricant RH-1 in percentage by mass into the coarse powder particles of the melt-spun sheets with the particle size of 0.1-0.6 mm, filling argon or nitrogen into a sealed mixer, stirring and mixing for 0.5-1 h to prepare middle broken materials, adding the middle broken materials into a grinding chamber of an airflow mill, enabling the middle broken materials to mutually collide, shear and grind under the drive of supersonic speed power medium gas sprayed from a nozzle of the airflow mill, crushing the middle broken materials into powder, and adjusting the rotating speed of a grading wheel to enable the particle size of the powder to be 4-6 mu m; adding the powder into a mixer, and mixing for 2-3 h;
specifically, the supersonic speed power medium gas is nitrogen;
s8, carrying out orientation pressing molding on the powder in a magnetic field with the magnetic field intensity of 1200-2400 KA/m, carrying out vacuum packaging after molding, and keeping the pressure for 10-120 seconds at 180-220 MPa by using a cold isostatic press to prepare a green body;
s9, placing the green body into a vacuum sintering furnace, continuously vacuumizing, slowly heating to 1190-1220 ℃, introducing argon gas to keep the pressure in the vacuum sintering furnace at 0-0.015 MPa, and carrying out heat preservation sintering for 70-120 min;
adjusting the temperature in the vacuum sintering furnace to 1150-1190 ℃ to perform solid solution treatment on the green body, wherein the treatment time is 1-20 h; after the solid solution treatment is finished, rapidly cooling the green body in the vacuum sintering furnace to room temperature by a cooling fan;
heating the temperature in the vacuum sintering furnace to 820-870 ℃, and carrying out aging treatment on the green body for 1-20 hours;
after the aging treatment is finished, the temperature in the vacuum sintering furnace is reduced to 350-450 ℃ at the speed of 0.5-1 ℃/min, the temperature is kept for 1-5 h, and the samarium cobalt magnet can be prepared by taking out the samarium cobalt magnet after being cooled to room temperature.
Specific examples are given below.
Example 1:
preparing two samarium cobalt magnets according to the following steps, and recording the two samarium cobalt magnets as a #1 samarium cobalt magnet and a #2 samarium cobalt magnet;
the method comprises the following steps of:
s1, weighing 24.7% of metal samarium, 47% of metal cobalt, 21% of pure iron, 4.9% of electrolytic copper and 2.4% of sponge zirconium as smelting raw materials; weighing samarium metal accounting for 1.2 percent of the mass of the smelting raw materials as a burning loss supplement;
s2, placing electrolytic copper and sponge zirconium at the bottom of the crucible 1, placing metal cobalt and pure iron in the middle of the crucible 1, and placing metal samarium in the smelting raw materials and metal samarium in the burning loss supplement material at the top of the crucible 1; controlling a vacuum rapid hardening furnace to smelt the smelting raw material and the burning loss supplement material into molten metal;
specifically, nitrogen is continuously introduced into the vacuum rapid hardening furnace, and continuous vacuum pumping is carried out, so that the internal vacuum degree is kept at 2000Pa, and the nitrogen introduction and vacuum pumping time is 35min, so as to remove the smelting raw materials, the burning loss supplement materials and the water on the inner surface of the crucible 1; continuously vacuumizing to 610Pa, heating the smelting raw material and the burning supplement material in the crucible 1 by using 40KW of medium-frequency heating power, and simultaneously increasing the heating power at the speed of 3KW/min to further remove the smelting raw material, the burning supplement material, the water on the surface of the crucible 1 and the crystal water on the surface of the crucible 1; when the temperature in the vacuum rapid hardening furnace is raised to 800 ℃, argon is continuously filled into the vacuum rapid hardening furnace, so that the vacuum degree in the vacuum rapid hardening furnace is kept at-0.035 MPa, and the smelting volatilization loss of metal samarium is reduced; when the temperature in the vacuum rapid hardening furnace is raised to 1400 ℃, the heating power of the vacuum rapid hardening furnace is reduced to 190KW after the metal is liquefied and cleared, and the smelting raw material and the burning loss supplement are smelted into molten metal after refining for 25 min;
s3, when the temperature in the vacuum rapid hardening furnace is reduced to 1350 ℃, the heating power is reduced to 150KW, the crucible 1 in the vacuum rapid hardening furnace is controlled to incline, molten metal in the crucible 1 is poured into the tundish 3 at the speed of 950 g/S, and the depth of the molten metal in the tundish 3 is 80mm; a baffle plate 2 for preventing molten metal from rushing forwards during pouring of the crucible is arranged between the crucible 1 and the tundish 3;
the water-cooled copper roller 4 rotates at the linear speed of 0.7m/s, the molten metal in the tundish 3 is in contact with the surface of the water-cooled copper roller 4, then the molten metal is solidified and crystallized to form a metal sheet, and the metal sheet is taken out from the tundish 3 when the water-cooled copper roller 4 rotates and is primarily cooled on the water-cooled copper roller 4;
wherein, the contact line between the inner bottom surface of the tundish 3 and the outer circular surface of the water-cooled copper roller 4 is marked as an x line 5, and the axial lead of the water-cooled copper roller 4 is marked as a y line 6;
the included angles between the plane where the x line 5 and the y line 6 are located and the horizontal plane passing through the y line 6 are marked as alpha, and the alpha is 28 degrees;
the water temperature at the water inlet of the water-cooled copper roller 4 is 30 ℃, and the water temperature at the water outlet of the water-cooled copper roller 4 is 70 ℃;
the metal sheet slides into the rotary water-cooling disc from the surface of the water-cooling copper roller 4, and is rapidly cooled by the rotary water-cooling disc to form a samarium-cobalt magnet melt-spun piece 7;
s4, after cooling the samarium-cobalt magnet melt-spun piece 7 to 60 ℃, opening an air release valve of the vacuum rapid hardening furnace, and standing for 30min to discharge;
s5, placing the samarium-cobalt magnet melt-spun piece 7 in a jaw crusher, and carrying out coarse crushing under the protection of nitrogen to prepare melt-spun piece particles with the particle size of 15 mm;
s6, putting the melt-spun sheet particles with the particle size of 15mm into a vacuum ball mill with a sieve, vacuumizing, and then filling argon or nitrogen for secondary crushing, wherein the particle size of coarse particles of the melt-spun sheet is 0.6mm after crushing;
s7, adding 1-3 per mill of anti-oxidation lubricant RH-1 in percentage by mass into the coarse powder particles of the melt-spun sheets with the particle size of 0.6mm, filling argon or nitrogen into a sealed mixer, stirring and mixing for 1 hour to prepare middle broken materials, adding the middle broken materials into a grinding chamber of an airflow grinding machine, enabling the middle broken materials to collide, shear and grind with supersonic speed power medium gas sprayed out of a nozzle of the airflow grinding machine under the drive of the nitrogen, enabling the middle broken materials to be crushed into powder, and adjusting the rotating speed of a grading wheel to enable the particle size of the powder to be 4.5 mu m; adding the powder into a mixer, and mixing for 2 hours;
s8, the powder is oriented and pressed in a magnetic field with the magnetic field intensity of 1350KA/m for forming, and after forming, the powder is packaged in vacuum and is kept for 60 seconds under 209MPa through a cold isostatic press to prepare a green body;
s9, placing the green body into a vacuum sintering furnace, continuously vacuumizing, slowly heating to 1200 ℃, introducing argon to keep the pressure in the vacuum sintering furnace at 0.015MPa, and carrying out heat preservation sintering for 70min;
adjusting the temperature in the vacuum sintering furnace to 1180 ℃ to perform solid solution treatment on the green body, wherein the treatment time is 6 hours; after the solid solution treatment is finished, rapidly cooling the green body in the vacuum sintering furnace to room temperature by a cooling fan;
heating the temperature in the vacuum sintering furnace to 850 ℃, and carrying out aging treatment on the green body, wherein the treatment time is 18 hours;
and after the aging treatment is finished, reducing the temperature in the vacuum sintering furnace to 400 ℃ at the speed of 0.8 ℃/min, preserving the heat for 2h, and quickly cooling to room temperature to discharge the samarium cobalt magnet.
The thickness and the grain size of a #1 samarium-cobalt magnet melt-spun piece and a #2 samarium-cobalt magnet melt-spun piece manufactured in a vacuum rapid hardening furnace are measured, the average thickness of the #1 samarium-cobalt magnet melt-spun piece and the #2 samarium-cobalt magnet melt-spun piece is 0.85mm, and the average grain size is 11.215 micrometers.
Measuring the magnetic properties of the #1 samarium-cobalt magnet and the #2 samarium-cobalt magnet prepared by the steps by using an ATM-4 magnetic property measuring instrument in a room temperature environment (20 ℃), namely measuring the remanence (Br), the intrinsic coercive force (Hcj) and the maximum energy product ((BH) max) of the #1 samarium-cobalt magnet and the #2 samarium-cobalt magnet; and calculating the lifting rate of the magnetic performance of the #1 samarium-cobalt magnet and the #2 samarium-cobalt magnet compared with the samarium-cobalt magnet produced by the common vacuum rapid hardening furnace process. (the residual magnetic property Br of the samarium cobalt magnet produced by the common vacuum rapid hardening furnace process is 1.12T, the intrinsic coercive force Hcj is 1433kA/m, and the maximum magnetic energy product (BH) max is 239KJ/m 3 )
The specific data are as follows:
in summary, the #1 samarium cobalt magnet and the #2 samarium cobalt magnet were prepared according to example 1, wherein the average thickness of the #1 samarium cobalt magnet melt-spun piece and the #2 samarium cobalt magnet melt-spun piece was 0.85mm and the average grain size was 11.215 μm; the thickness of the melt-spun sheet prepared by the common melt-spun process is 0.2-0.5 mm, and the grain size is 2-5 mu m; the samarium cobalt magnet melt-spun piece prepared by the technical scheme of the invention has increased thickness, improved average crystal size and reduced influence of over-thin melt-spun piece and over-fine crystal grains on the performance of the samarium cobalt magnet;
as shown in the table, the performances of the samarium cobalt magnet prepared by vacuum sintering, solution treatment and aging treatment are greatly improved compared with the performances of the samarium cobalt magnet produced by the common process.
The embodiments given above are preferable examples for implementing the present invention, and the present invention is not limited to the above-described embodiments. Any non-essential addition or replacement made by a person skilled in the art according to the technical features of the technical solution of the present invention is within the scope of the present invention.
Claims (10)
1. A method for manufacturing a samarium cobalt magnet based on a vacuum rapid hardening furnace is characterized by comprising the following steps of:
s1, weighing 24-27% of metal samarium, 40-50% of metal cobalt, 18-25% of pure iron, 4-10% of electrolytic copper and 2-5% of sponge zirconium as smelting raw materials, and weighing 1-2% of metal samarium in mass of the smelting raw materials as a burning loss supplement;
s2, filling the smelting raw materials and the burning loss supplement materials into a crucible of a vacuum rapid hardening furnace; controlling a vacuum rapid hardening furnace to smelt the smelting raw material and the burning loss supplement into molten metal;
s3, controlling the crucible in the vacuum rapid hardening furnace to incline, pouring molten metal in the crucible into a tundish at the speed of 800-2000 g/S, and enabling the depth of the molten metal in the tundish to be 70-120 mm;
the water-cooled copper roller rotates at a linear speed of 0.5-1.1 m/s, molten metal in the tundish is in contact with the surface of the water-cooled copper roller and then is solidified and crystallized to form a metal sheet, and the metal sheet is taken out from the tundish when the water-cooled copper roller rotates and is primarily cooled on the water-cooled copper roller;
the metal sheet slides into the rotary water-cooling disc from the surface of the water-cooling copper roller, and is rapidly cooled by the rotary water-cooling disc to prepare a samarium-cobalt magnet melt-spun sheet with the thickness of 0.50-2.0 mm and the size of solidified structure crystal grains of 3-15 mu m;
s4, after cooling the samarium-cobalt magnet melt-spun piece to 60 ℃, opening an air release valve of the vacuum rapid hardening furnace, and standing for 30min to discharge;
s5, placing the samarium-cobalt magnet melt-spun piece in a jaw crusher, and carrying out coarse crushing under the protection of nitrogen to prepare melt-spun piece particles with the particle size of 5-20 mm;
s6, putting the melt-spun sheet particles with the particle size of 5-20 mm into a vacuum ball mill with a sieve, vacuumizing, and then filling argon or nitrogen for secondary crushing, wherein the particle size of the coarse powder particles of the melt-spun sheet is 0.1-0.6 mm after crushing;
s7, adding 1-3 per mill of anti-oxidation lubricant RH-1 in percentage by mass into 0.1-0.6 mm-granularity melt-spun sheet coarse powder particles, filling argon or nitrogen into a sealed mixer, stirring and mixing for 0.5-1 h to prepare middle broken materials, adding the middle broken materials into a grinding chamber of a jet mill, mutually colliding, shearing and grinding the middle broken materials under the drive of supersonic power medium gas sprayed by a nozzle of the jet mill, crushing the middle broken materials into powder, and adjusting the rotating speed of a grading wheel to ensure that the granularity of the powder is 4-6 mu m; adding the powder into a mixer, and mixing for 2-3 h;
s8, carrying out orientation pressing molding on the powder in a magnetic field with the magnetic field intensity of 1200-2400 KA/m, carrying out vacuum packaging after molding, and keeping the pressure for 10-120 seconds at 180-220 MPa by using a cold isostatic press to prepare a green body;
s9, placing the green body into a vacuum sintering furnace, continuously vacuumizing and slowly heating to 1190-1220 ℃, introducing argon to keep the pressure in the vacuum sintering furnace at 0-0.015 MPa, and carrying out heat preservation and sintering for 70-120 min;
adjusting the temperature in the vacuum sintering furnace to 1150-1190 ℃ to perform solid solution treatment on the green body, wherein the treatment time is 1-20 h; after the solid solution treatment is finished, rapidly cooling the green body in the vacuum sintering furnace to room temperature through a cooling fan;
heating the temperature in the vacuum sintering furnace to 820-870 ℃, and carrying out aging treatment on the green body for 1-20 hours;
after the aging treatment is finished, the temperature in the vacuum sintering furnace is reduced to 350-450 ℃ at the speed of 0.5-1 ℃/min, the temperature is kept for 1-5 h, and the samarium cobalt magnet can be prepared by taking out the samarium cobalt magnet after being cooled to room temperature.
2. The method for manufacturing the samarium cobalt magnet based on the vacuum rapid hardening furnace according to claim 1, wherein in S3, the contact line between the inner bottom surface of the tundish and the outer circular surface of the water-cooled copper roller is marked as an x line, and the axial lead of the water-cooled copper roller is marked as a y line; the included angle between the plane of the x line and the y line and the horizontal plane passing through the y line is recorded as alpha which is 26-35 degrees.
3. The method for manufacturing the samarium cobalt magnet based on the vacuum rapid hardening furnace according to claim 1, wherein the water temperature at the water inlet of the water-cooled copper roller is 30 ℃ to 35 ℃ and the water temperature at the water outlet of the water-cooled copper roller is 55 ℃ to 70 ℃.
4. The method for manufacturing the samarium cobalt magnet based on the vacuum rapid hardening furnace according to claim 1, characterized in that in the S1, 24.7% of metal samarium, 47% of metal cobalt, 21% of pure iron, 4.9% of electrolytic copper and 2.4% of sponge zirconium are weighed as smelting raw materials by mass percentage;
weighing samarium metal accounting for 1.2 percent of the mass of the smelting raw materials as a burning loss supplement.
5. The method of manufacturing a samarium cobalt magnet based on a vacuum rapid hardening furnace of claim 1, wherein in S1, the pure iron and the zirconium sponge can also be a zircaloy.
6. The method of making a samarium cobalt magnet based on a vacuum rapid hardening furnace of claim 1 wherein in S2 electrolytic copper and sponge zirconium are placed at the bottom of the crucible, metallic cobalt and pure iron are placed in the middle of the crucible, and metallic samarium in the melting feed and metallic samarium in the burnout supplement are both placed at the top of the crucible.
7. The method for manufacturing the samarium cobalt magnet based on the vacuum rapid hardening furnace according to claim 1, wherein in the step S2, the vacuum rapid hardening furnace is used for smelting raw materials and burning loss supplement materials into molten metal by the specific steps of:
continuously introducing nitrogen into the vacuum rapid hardening furnace, and continuously vacuumizing to keep the internal vacuum degree of the vacuum rapid hardening furnace at 1000-2000 Pa, wherein the nitrogen introduction and vacuumizing time is 30-50 min to remove the smelting raw materials, the burning loss supplement materials and the water on the inner surface of the crucible;
continuously vacuumizing to 610-1000 Pa, heating the smelting raw material and the burning loss supplement material in the crucible by using medium-frequency heating power of 40-60 KW, and simultaneously increasing the heating power at the speed of 2-4 KW/min to further remove the smelting raw material, the burning loss supplement material, the water on the surface of the crucible and the crystal water on the crucible;
when the temperature in the vacuum rapid hardening furnace is raised to 800 ℃, argon is continuously filled into the vacuum rapid hardening furnace, so that the vacuum degree in the vacuum rapid hardening furnace is kept between-0.035 MPa and-0.025 MPa, and the smelting volatilization loss of metal samarium is reduced;
when the temperature in the vacuum rapid hardening furnace is raised to 1400 ℃, the heating power of the vacuum rapid hardening furnace is reduced to 170-210 KW after the metal is liquefied and cleared, and the smelting raw material and the burning loss supplement are smelted into molten metal after refining for 18-26 min.
8. The manufacturing method of the samarium cobalt magnet based on the vacuum rapid hardening furnace according to claim 1, wherein in the step S3, when the temperature in the vacuum rapid hardening furnace is reduced to 1350 ℃, the heating power is reduced to 145 to 165KW, the inclination of the crucible in the vacuum rapid hardening furnace is controlled, the molten metal in the crucible is poured into the tundish at a speed of 800 to 2000 g/S, and the depth of the molten metal in the tundish is 70 to 120mm.
9. The method of making a samarium cobalt magnet based on a vacuum rapid hardening furnace of claim 1, wherein in S7 the supersonic motive medium gas is nitrogen.
10. The method for manufacturing the samarium cobalt magnet based on the vacuum rapid hardening furnace according to claim 1, wherein in S3, a baffle plate for preventing molten metal from rushing forward during pouring of the crucible is arranged between the crucible and the tundish.
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| CN106298138A (en) * | 2016-11-10 | 2017-01-04 | 包头天和磁材技术有限责任公司 | The manufacture method of rare-earth permanent magnet |
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Denomination of invention: A Method for Manufacturing Samarium Cobalt Magnets Based on Vacuum Rapid Solidification Furnace Effective date of registration: 20230927 Granted publication date: 20230526 Pledgee: Bank of China Limited Xi'an High tech Development Zone Sub branch Pledgor: XI'AN XIGONGDA SIQIANG TECHNOLOGY Co.,Ltd. Registration number: Y2023980059733 |