CN115331942B - Samarium cobalt magnet manufacturing method based on vacuum rapid hardening furnace - Google Patents
Samarium cobalt magnet manufacturing method based on vacuum rapid hardening furnace Download PDFInfo
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- CN115331942B CN115331942B CN202211029985.1A CN202211029985A CN115331942B CN 115331942 B CN115331942 B CN 115331942B CN 202211029985 A CN202211029985 A CN 202211029985A CN 115331942 B CN115331942 B CN 115331942B
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- 229910000938 samarium–cobalt magnet Inorganic materials 0.000 title claims abstract description 68
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 18
- 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 53
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 52
- 229910052802 copper Inorganic materials 0.000 claims abstract description 52
- 239000010949 copper Substances 0.000 claims abstract description 52
- 239000002994 raw material Substances 0.000 claims abstract description 51
- 239000000463 material Substances 0.000 claims abstract description 48
- 239000000843 powder Substances 0.000 claims abstract description 32
- 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
- 239000013589 supplement Substances 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 20
- 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
- 238000001816 cooling Methods 0.000 claims abstract description 14
- 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
- 238000000465 moulding Methods 0.000 claims abstract description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 48
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 32
- 238000010438 heat treatment Methods 0.000 claims description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 28
- 229910052757 nitrogen Inorganic materials 0.000 claims description 24
- 239000002245 particle Substances 0.000 claims description 20
- 229910052786 argon Inorganic materials 0.000 claims description 16
- 238000011049 filling Methods 0.000 claims description 16
- 229910052742 iron Inorganic materials 0.000 claims description 14
- 239000007789 gas Substances 0.000 claims description 11
- 239000013078 crystal Substances 0.000 claims description 10
- 238000000227 grinding Methods 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 8
- 230000001276 controlling effect Effects 0.000 claims description 7
- 238000011068 loading method Methods 0.000 claims description 7
- 238000002844 melting Methods 0.000 claims description 6
- 230000008018 melting Effects 0.000 claims description 6
- 239000000047 product Substances 0.000 claims description 6
- 238000000748 compression moulding Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 241001062472 Stokellia anisodon Species 0.000 claims description 4
- 239000003963 antioxidant agent Substances 0.000 claims description 4
- 230000003078 antioxidant effect Effects 0.000 claims description 4
- 238000005266 casting Methods 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
- 238000010008 shearing Methods 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 238000009461 vacuum packaging Methods 0.000 claims description 4
- 229910000640 Fe alloy Inorganic materials 0.000 claims description 3
- NDUKHFILUDZSHZ-UHFFFAOYSA-N [Fe].[Zr] Chemical compound [Fe].[Zr] NDUKHFILUDZSHZ-UHFFFAOYSA-N 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 3
- KPLQYGBQNPPQGA-UHFFFAOYSA-N cobalt samarium Chemical compound [Co].[Sm] KPLQYGBQNPPQGA-UHFFFAOYSA-N 0.000 abstract description 2
- 238000003825 pressing Methods 0.000 abstract 1
- 239000006104 solid solution Substances 0.000 abstract 1
- 238000007711 solidification Methods 0.000 description 9
- 230000008023 solidification Effects 0.000 description 9
- 229910045601 alloy Inorganic materials 0.000 description 7
- 239000000956 alloy Substances 0.000 description 7
- 238000009826 distribution Methods 0.000 description 3
- 238000005204 segregation Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- 230000005389 magnetism Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 241000276425 Xiphophorus maculatus Species 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 238000006467 substitution reaction 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
-
- 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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- Manufacturing & Machinery (AREA)
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- Crystallography & Structural Chemistry (AREA)
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- Hard Magnetic Materials (AREA)
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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 metal, cobalt metal, pure iron, electrolytic copper and zirconium sponge as smelting raw materials, and weighing samarium metal accounting for 1-2% of the mass of the smelting raw materials as burning loss supplement materials; smelting raw materials and burning-out supplementary materials into a crucible of a vacuum rapid hardening furnace to obtain molten metal, pouring the molten metal into a tundish, making the molten metal into a metal sheet at the bottom of the tundish, making the metal sheet into a samarium cobalt magnet melt-spun sheet after cooling, further crushing the samarium cobalt magnet melt-spun sheet into powder with the size of 4-6 mu m by a jaw crusher, a vacuum belt screen ball mill and an air flow mill, performing orientation press molding on the powder in a magnetic field, pressing the powder into a green body by a cold isostatic press, and making the green body into a samarium cobalt magnet after vacuum sintering, solid solution treatment and aging treatment; the method 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 2:17 type Sm-Co magnet has the characteristics of high magnetic performance, high Curie temperature (820 ℃), strong oxidation resistance, corrosion resistance and the like, and has an irreplaceable position in the fields of national defense industry, advanced technology, aviation, aerospace, navigation, high-precision instrument and meter and the like.
The existing 2:17 type samarium cobalt magnet production process mainly adopts a powder metallurgy process to manufacture, and the main process method adopted by alloying is that an alloy cast ingot is manufactured by a vacuum induction furnace and an alloy melt-spun sheet is manufactured by a vacuum rapid hardening furnace. The alloy cast ingot prepared by vacuum induction smelting is characterized in that the thickness of the cast ingot is larger, the thickness of a common platy cast ingot is 8-50 mm, the size of crystal grains of a solidification structure is generally 20-100 mu m, and the size of the crystal grains of the alloy cast ingot is coarse, if air flow grinding is used for powder preparation, the production efficiency is extremely low, the size and the distribution of powder are poor, and the economical efficiency is poor due to the large crushing ratio. Meanwhile, the coarse solidification structure has serious component segregation, so that the magnetic performance is further reduced; when the conventional vacuum rapid hardening furnace is used for preparing the alloy melt-spun sheet, the thickness of the melt-spun sheet is usually 0.2-0.5 mm, and although the segregation of the solidification structure components is small, the grain size of the solidification structure is 2-5 mu m, and the grains are too fine, so that a single airflow powder body easily contains a plurality of solidification grains, the magnet orientation degree is reduced, the residual magnetism is reduced, and the magnet performance is seriously affected.
Disclosure of Invention
The technical problem solved by the invention is to provide the samarium cobalt magnet manufacturing method based on the vacuum rapid hardening furnace, which organically combines the formulation of the samarium cobalt magnet and the preparation process of the melt-spun piece, 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 samarium cobalt magnet manufacturing method based on a vacuum rapid hardening furnace 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 by mass of the smelting raw materials as burning loss supplement materials;
s2, loading smelting raw materials and burning loss supplementary materials into a crucible of a vacuum rapid hardening furnace; controlling a vacuum rapid hardening furnace to smelt the smelting raw materials and the burning loss supplementary materials into molten metal;
s3, controlling the inclination of a crucible in the vacuum rapid hardening furnace, 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, after the molten metal in the tundish contacts with the surface of the water-cooled copper roller, the molten metal is solidified and crystallized to form a metal sheet, and the metal sheet is taken out of the tundish when the water-cooled copper roller rotates and is initially cooled on the water-cooled copper roller;
the metal sheet slides from the surface of the water-cooled copper roller to the rotary water-cooled disc, and is rapidly cooled by the rotary water-cooled disc to prepare a samarium cobalt magnet melt-spun sheet with the thickness of 0.50-2.0 mm and the size of 3-15 mu m of solidified structure grains;
s4, after cooling the samarium cobalt magnet melt-spun piece to 60 ℃, opening a vacuum rapid hardening furnace air release valve, and standing for 30min to obtain the product;
s5, placing the samarium cobalt magnet melt-spun pieces in a jaw crusher, and performing coarse crushing under the protection of nitrogen to prepare melt-spun piece particles with the granularity of 5-20 mm;
s6, loading the melt-spun sheet particles with the granularity of 5-20 mm into a vacuum belt screen ball mill, vacuumizing, filling argon or nitrogen for secondary crushing, and enabling the particle size of the melt-spun sheet coarse powder particles to be 0.1-0.6 mm after crushing;
s7, adding an antioxidant lubricant RH-1 with the mass percentage concentration of 1-3%o into the coarse powder particles of the melt-spun sheet with the granularity of 0.1-0.6 mm, filling argon or nitrogen into a sealed mixer, stirring and mixing for 0.5-1 h to prepare a middle broken material, adding the middle broken material into a grinding chamber of an airflow pulverizer, mutually colliding, shearing and grinding the middle broken material under the drive of supersonic speed power medium gas sprayed by a nozzle of the airflow pulverizer, crushing the middle broken material into powder, and adjusting the rotating speed of a classification wheel to enable the granularity of the powder to be 4-6 mu m; adding the powder into a mixer, and mixing for 2-3 hours;
s8, carrying out orientation compression molding on the powder in a magnetic field with the magnetic field strength of 1200-2400 KA/m, vacuum packaging after molding, and maintaining the pressure for 10-120 seconds under 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 ℃, filling argon gas to keep the pressure in the vacuum sintering furnace at 0-0.015 MPa, and performing heat preservation and sintering for 70-120 min;
the temperature in the vacuum sintering furnace is regulated to 1150-1190 ℃ to carry out solution treatment on the green body, and the treatment time is 1-20 h; after the solution treatment is completed, 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 completed, the temperature in the vacuum sintering furnace is reduced to 350-450 ℃ at the speed of 0.5-1 ℃/min, then the temperature is kept for 1-5 h, and the mixture is rapidly cooled to room temperature and discharged from the furnace, thus obtaining the samarium cobalt magnet.
In the step 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 axis of the water-cooled copper roller is marked as a y line; and the included angle between the plane where the x-ray and the y-ray are positioned and the horizontal plane passing through the y-ray is denoted as alpha, and the alpha is 26-35 degrees.
Further, the water temperature at the water inlet of the water-cooled copper roller is 30-35 ℃, and the water temperature at the water outlet of the water-cooled copper roller is 55-70 ℃.
Further, in the step S1, 24.7% of metal samarium, 47% of metal cobalt, 21% of pure iron, 4.9% of electrolytic copper and 2.4% of zirconium sponge are weighed as smelting raw materials in percentage by mass;
weighing samarium metal accounting for 1.2% of the mass of the smelting raw material as a burning loss supplement.
Further, in S1, the pure iron and the sponge zirconium may be zirconium-iron alloy.
Further, in the step S2, electrolytic copper and sponge zirconium are placed at the bottom of the crucible, metallic cobalt and pure iron are placed at the middle of the crucible, and both the metallic samarium in the smelting raw material and the metallic samarium in the burning loss supplement are placed at the top of the crucible.
Further, in the step S2, the specific steps of smelting the smelting raw material and the burning loss supplementary material into molten metal by the vacuum rapid hardening furnace are as follows:
continuously introducing nitrogen into the vacuum rapid hardening furnace, and continuously vacuumizing to keep the vacuum degree in the vacuum rapid hardening furnace at 1000-2000 Pa, wherein the duration of introducing nitrogen and vacuumizing is 30-50 min so as to remove water on the inner surfaces of the smelting raw materials, the burning-loss supplementary materials and the crucible;
continuously vacuumizing to 610-1000 Pa, heating the smelting raw material and the burning loss supplement material in the crucible with intermediate frequency heating power of 40-60 KW, and simultaneously lifting the heating power at a speed of 2-4 KW/min to further remove water on the smelting raw material, the burning loss supplement material and the crucible surface and crystal water on the smelting raw material and the burning loss supplement material;
continuously filling argon into the vacuum rapid hardening furnace when the temperature in the vacuum rapid hardening furnace is increased to 800 ℃ so as to keep the vacuum degree in the vacuum rapid hardening furnace at-0.035 MPa to-0.025 MPa, thereby reducing the melting volatilization loss of the metal samarium;
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 cleaned, and the smelting raw material and the burning loss supplement are smelted into molten metal after refining for 18-26 min.
Further, in the step 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 a crucible in the vacuum rapid hardening furnace is controlled, the molten metal in the crucible is poured into a tundish at a 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 power medium gas is nitrogen.
Further, in S3, a baffle plate for preventing molten metal from rushing forward during pouring of the crucible is provided between the crucible and the tundish.
Compared with the prior art, the invention has the following beneficial technical effects:
according to the technical scheme, a samarium cobalt magnet alloy melt-spun sheet is prepared through a vacuum rapid hardening furnace, the melt-spun sheet is further crushed into fine powder with the diameter of 4-6 mu m by a jaw crusher, a vacuum belt screen ball mill and an air flow mill, the powder is subjected to orientation compression molding in a magnetic field and then is pressed into a green body by a cold isostatic press, and the green body is subjected to vacuum sintering, 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 molten metal is increased to 800-2000 g/s, the depth of the molten metal in a tundish is increased to h=70-120 mm, and the linear speed of a water-cooled copper roller is reduced to 0.5-1.1 m/s; the temperature of the water-cooling copper roller water inlet is increased to 30-35 ℃, the temperature of the water outlet is reduced to 55-70 ℃, and the temperature of the casting molten metal is increased to 1350 ℃ so as to increase the thickness of the prepared samarium cobalt magnet melt-spun sheet, so that the thickness of the prepared samarium cobalt magnet melt-spun sheet is 0.5-2.0 mm, and the size of the crystal grain of a solidification structure is 3-15 mu m; solves the problems of too fine grains and poor magnet performance of the samarium cobalt magnet melt-spun sheet prepared by using a vacuum rapid hardening furnace in the current production process, wherein the thickness of the melt-spun sheet is 0.2-0.5 mm; the problems of overlarge thickness of the metal cast ingot, coarse grains (the thickness of the cast ingot is 8-50 mm, and the grain size is 20-100 mu m), long time consumption, low efficiency, magnetic reduction caused by serious segregation of solidification structure components and the like in the crushing process can be solved.
Drawings
FIG. 1 is a schematic diagram of the water-cooled copper roll, crucible, tundish of the present invention;
FIG. 2 is a graph of the solidification structure grain distribution of the #1 samarium cobalt magnet melt-spun sheet of example 1;
FIG. 3 is a graph of the solidification structure grain distribution of the #2 samarium cobalt magnet melt-spun sheet of example 1;
reference numerals: 1 is a crucible, 2 is a baffle plate, 3 is a tundish, 4 is a water-cooled copper roller, 5 is an x-ray, 6 is a y-ray, and 7 is a samarium cobalt magnet melt-spun piece.
Detailed Description
The invention will now be described in further detail with reference to the accompanying drawings, which illustrate but do not limit the invention.
The invention discloses a samarium cobalt magnet manufacturing method 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 by mass of the smelting raw materials as burning loss supplement materials;
specifically, 24.7% of samarium metal, 47% of cobalt metal, 21% of pure iron, 4.9% of electrolytic copper and 2.4% of zirconium sponge are weighed as smelting raw materials; weighing samarium metal accounting for 1.2% of the mass of the smelting raw material as a burning loss supplement;
the pure iron and the sponge zirconium can also be zirconium-iron alloy;
s2, loading smelting raw materials and burning loss supplementary materials into a crucible 1 of a vacuum rapid hardening furnace;
specifically, electrolytic copper and zirconium sponge are placed at the bottom of a crucible 1, metallic cobalt and pure iron are placed in the middle of the crucible 1, and metallic samarium in smelting raw materials and metallic samarium in burning-out supplementary materials are all placed at the top of the crucible 1;
controlling a vacuum rapid hardening furnace to smelt the smelting raw materials and the burning loss supplementary materials into molten metal;
specifically, the vacuum rapid hardening furnace comprises the following specific steps of smelting raw materials and burning loss supplementary materials into molten metal:
continuously introducing nitrogen into the vacuum rapid hardening furnace, and continuously vacuumizing to keep the vacuum degree in the vacuum rapid hardening furnace at 1000-2000 Pa, wherein the duration of introducing nitrogen and vacuumizing is 30-50 min so as to remove the smelting raw materials, the burning-loss supplementary 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 with intermediate frequency heating power of 40-60 KW, and simultaneously lifting the heating power at a speed of 2-4 KW/min to further remove water on the smelting raw material, the burning loss supplement material and the crucible 1 and crystal water on the smelting raw material and the burning loss supplement material; continuously filling argon into the vacuum rapid hardening furnace when the temperature in the vacuum rapid hardening furnace is increased to 800 ℃ so as to keep the vacuum degree in the vacuum rapid hardening furnace at-0.035 MPa to-0.025 MPa, thereby reducing the melting volatilization loss of the metal samarium; 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 cleaned, and the smelting raw material and the burning loss supplement are smelted into molten metal after refining for 18-26 min;
s3, controlling the inclination of the crucible 1 in the vacuum rapid hardening furnace, pouring molten metal in the crucible 1 into the tundish 3 at a 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 forward during the casting of the crucible 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 inclination of a crucible 1 in the vacuum rapid hardening furnace is controlled, the molten metal in the crucible 1 is poured into a tundish 3 at a 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, after the molten metal in the tundish 3 contacts with the surface of the water-cooled copper roller 4, the molten metal is solidified and crystallized to form a metal sheet, and the metal sheet is carried out of the tundish 3 when the water-cooled copper roller 4 rotates and is initially cooled on the water-cooled copper roller 4;
specifically, 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 axis line of the water-cooled copper roller 4 is marked as a y line 6;
the included angle between the plane of the x-ray 5 and the y-ray 6 and the horizontal plane passing through the y-ray 6 is denoted as alpha, and the alpha 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 from the surface of the water-cooled copper roller 4 to the rotary water-cooled disc, and is rapidly cooled by the rotary water-cooled disc to prepare a samarium cobalt magnet melt-spun sheet 7 with the thickness of 0.50-2.0 mm and the size of the solidified structure crystal grain of 3-15 mu m;
s4, after cooling the samarium cobalt magnet melt-spun piece 7 to 60 ℃, opening a vacuum rapid hardening furnace air release valve, and standing for 30min to obtain the product;
s5, placing the samarium cobalt magnet melt-spun piece 7 in a jaw crusher, and performing coarse crushing under the protection of nitrogen to prepare melt-spun piece particles with the granularity of 5-20 mm;
s6, loading the melt-spun sheet particles with the granularity of 5-20 mm into a vacuum belt screen ball mill, vacuumizing, filling argon or nitrogen for secondary crushing, and enabling the particle size of the melt-spun sheet coarse powder particles to be 0.1-0.6 mm after crushing;
s7, adding an antioxidant lubricant RH-1 with the mass percentage concentration of 1-3%o into the coarse powder particles of the melt-spun sheet with the granularity of 0.1-0.6 mm, filling argon or nitrogen into a sealed mixer, stirring and mixing for 0.5-1 h to prepare a middle broken material, adding the middle broken material into a grinding chamber of an airflow pulverizer, mutually colliding, shearing and grinding the middle broken material under the drive of supersonic speed power medium gas sprayed by a nozzle of the airflow pulverizer, crushing the middle broken material into powder, and adjusting the rotating speed of a classification wheel to enable the granularity of the powder to be 4-6 mu m; adding the powder into a mixer, and mixing for 2-3 hours;
specifically, the supersonic speed power medium gas is nitrogen;
s8, carrying out orientation compression molding on the powder in a magnetic field with the magnetic field strength of 1200-2400 KA/m, vacuum packaging after molding, and maintaining the pressure for 10-120 seconds under 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 ℃, filling argon gas to keep the pressure in the vacuum sintering furnace at 0-0.015 MPa, and performing heat preservation and sintering for 70-120 min;
the temperature in the vacuum sintering furnace is regulated to 1150-1190 ℃ to carry out solution treatment on the green body, and the treatment time is 1-20 h; after the solution treatment is completed, 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 completed, the temperature in the vacuum sintering furnace is reduced to 350-450 ℃ at the speed of 0.5-1 ℃/min, then the temperature is kept for 1-5 h, and the mixture is rapidly cooled to room temperature and discharged from the furnace, thus obtaining the samarium cobalt magnet.
Specific examples are given below.
Example 1:
two samarium cobalt magnets, designated #1 and #2, were prepared according to the following procedure;
the method comprises the following steps in percentage by mass:
s1, weighing 24.7% of samarium metal, 47% of cobalt metal, 21% of pure iron, 4.9% of electrolytic copper and 2.4% of zirconium sponge as smelting raw materials; weighing samarium metal accounting for 1.2% of the mass of the smelting raw material as a burning loss supplement;
s2, placing electrolytic copper and zirconium sponge at the bottom of the crucible 1, placing metallic cobalt and pure iron in the middle of the crucible 1, and placing both the metallic samarium in the smelting raw material and the metallic 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 materials and the burning loss supplementary materials into molten metal;
specifically, continuously introducing nitrogen into the vacuum rapid hardening furnace, and continuously vacuumizing to keep the vacuum degree in the furnace at 2000Pa, wherein the duration of introducing nitrogen and vacuumizing is 35min so as to remove the smelting raw materials, the burning-out supplementary materials and the water on the inner surface of the crucible 1; continuously vacuumizing to 610Pa, heating the smelting raw material and the burning loss supplement material in the crucible 1 with 40KW of medium-frequency heating power, and simultaneously lifting the heating power at a speed of 3KW/min to further remove water on the smelting raw material, the burning loss supplement material and the surface of the crucible 1 and crystal water on the smelting raw material and the burning loss supplement material; continuously filling argon into the vacuum rapid hardening furnace when the temperature in the vacuum rapid hardening furnace is increased to 800 ℃ so as to keep the vacuum degree in the vacuum rapid hardening furnace at-0.035 MPa, thereby reducing the melting volatilization loss of the metal samarium; when the temperature in the vacuum rapid hardening furnace is raised to 1400 ℃, reducing the heating power of the vacuum rapid hardening furnace to 190KW after the metal is liquefied and cleaned, and smelting the smelting raw materials and the burning loss supplementary materials 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 inclination of a crucible 1 in the vacuum rapid hardening furnace is controlled, molten metal in the crucible 1 is poured into a tundish 3 at a 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 forward during the casting of the crucible is arranged between the crucible 1 and the tundish 3;
the water-cooled copper roller 4 rotates at a linear speed of 0.7m/s, after the molten metal in the tundish 3 contacts with the surface of the water-cooled copper roller 4, the molten metal solidifies and crystallizes to form a metal sheet, and when the water-cooled copper roller 4 rotates, the metal sheet is carried out of the tundish 3 and is initially cooled on the water-cooled copper roller 4;
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 axis 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, 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 from the surface of the water-cooled copper roller 4 to the rotary water-cooled disc, and the samarium cobalt magnet melt-spun sheet 7 is manufactured after the metal sheet is rapidly cooled by the rotary water-cooled disc;
s4, after cooling the samarium cobalt magnet melt-spun piece 7 to 60 ℃, opening a vacuum rapid hardening furnace air release valve, and standing for 30min to obtain the product;
s5, placing the samarium cobalt magnet melt-spun piece 7 in a jaw crusher, and performing coarse crushing under the protection of nitrogen to prepare melt-spun piece particles with the granularity of 15 mm;
s6, loading the melt-spun sheet particles with the granularity of 15mm into a vacuum belt screen ball mill, vacuumizing, filling argon or nitrogen for secondary crushing, and enabling the particle size of the melt-spun sheet coarse powder particles to be 0.6mm after crushing;
s7, adding an antioxidant lubricant RH-1 with the mass percentage concentration of 1-3 per mill into the coarse powder particles of the melt-spun sheet with the granularity of 0.6mm, filling argon or nitrogen into a sealed mixer, stirring and mixing for 1h to prepare a medium broken material, adding the medium broken material into a grinding chamber of an airflow pulverizer, mutually colliding, shearing and grinding the medium broken material under the drive of supersonic speed power medium gas, namely nitrogen, sprayed out by a nozzle of the airflow pulverizer, crushing the medium broken material into powder, and adjusting the rotating speed of a classification wheel to enable the granularity of the powder to be 4.5 mu m; adding the powder into a mixer, and mixing for 2 hours;
s8, carrying out orientation compression molding on the powder in a magnetic field with the magnetic field strength of 1350KA/m, vacuum packaging after molding, and maintaining the pressure for 60 seconds under 209MPa 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 1200 ℃, filling argon gas to keep the pressure in the vacuum sintering furnace at 0.015MPa, and performing heat preservation and sintering for 70min;
adjusting the temperature in the vacuum sintering furnace to 1180 ℃ to carry out solution treatment on the green body for 6 hours; after the solution treatment is completed, 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 for 18 hours;
and after the aging treatment is finished, the temperature in the vacuum sintering furnace is reduced to 400 ℃ at the speed of 0.8 ℃/min, the temperature is kept for 2 hours, and the mixture is rapidly cooled to room temperature and discharged from the furnace, so that the samarium cobalt magnet can be manufactured.
The thickness and grain size of the #1 samarium cobalt magnet melt-spun piece and the #2 samarium cobalt magnet melt-spun piece which are manufactured in the 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 mu m.
The magnetic properties of the #1 and #2 samarium cobalt magnets prepared by the above steps, namely, the residual magnetism (Br), intrinsic coercive force (Hcj) and maximum magnetic energy product ((BH) max) of the #1 and #2 samarium cobalt magnets were measured using an ATM-4 magnetic properties meter in a room temperature environment (20 ℃); and calculates the improvement ratio of the magnetic properties 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 technology. (let(s) stand (s))Residual magnetic property Br of the samarium cobalt magnet manufactured by using a common vacuum rapid hardening furnace process: 1.12T, intrinsic coercivity Hcj:1433kA/m, maximum magnetic energy product (BH) max:239KJ/m 3 )
The specific data are as follows:
to sum up, the #1 and #2 samarium cobalt magnets prepared according to example 1, wherein the average thickness of the #1 and #2 samarium cobalt magnet melt-spun pieces 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 thickness of the samarium cobalt magnet melt-spun piece prepared by the technical scheme is increased, the average crystal size is improved, and the influence of the too thin melt-spun piece and the too fine crystal grain on the performance of the samarium cobalt magnet is reduced;
as shown in the table above, the performance of the samarium cobalt magnet prepared by vacuum sintering, solution treatment and aging treatment is greatly improved compared with that of the samarium cobalt magnet produced by the common process.
The embodiments given above are preferred examples for realizing the present invention, and the present invention is not limited to the above-described embodiments. Any immaterial additions and substitutions made by those skilled in the art according to the technical features of the technical scheme of the invention are all within the protection scope of the invention.
Claims (9)
1. The samarium cobalt magnet manufacturing method based on the 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 by mass of the smelting raw materials as burning loss supplement materials;
s2, loading smelting raw materials and burning loss supplementary materials into a crucible of a vacuum rapid hardening furnace; controlling a vacuum rapid hardening furnace to smelt the smelting raw materials and the burning loss supplementary materials into molten metal;
s3, controlling the inclination of a crucible in the vacuum rapid hardening furnace, increasing the temperature of a water inlet of a water-cooled copper roller to 30-35 ℃ and the temperature of a water outlet of the water-cooled copper roller to 55-70 ℃, increasing the temperature of molten metal in the crucible to 1350 ℃, pouring the 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, after the molten metal in the tundish contacts with the surface of the water-cooled copper roller, the molten metal is solidified and crystallized to form a metal sheet, and the metal sheet is taken out of the tundish when the water-cooled copper roller rotates and is initially cooled on the water-cooled copper roller;
the metal sheet slides from the surface of the water-cooled copper roller to the rotary water-cooled disc, and is rapidly cooled by the rotary water-cooled disc to prepare a samarium cobalt magnet melt-spun sheet with the thickness of 0.50-2.0 mm and the size of 3-15 mu m of solidified structure grains;
s4, after cooling the samarium cobalt magnet melt-spun piece to 60 ℃, opening a vacuum rapid hardening furnace air release valve, and standing for 30min to obtain the product;
s5, placing the samarium cobalt magnet melt-spun pieces in a jaw crusher, and performing coarse crushing under the protection of nitrogen to prepare melt-spun piece particles with the granularity of 5-20 mm;
s6, loading the melt-spun sheet particles with the granularity of 5-20 mm into a vacuum belt screen ball mill, vacuumizing, filling argon or nitrogen for secondary crushing, and enabling the particle size of the melt-spun sheet coarse powder particles to be 0.1-0.6 mm after crushing;
s7, adding an antioxidant lubricant RH-1 with the mass percentage concentration of 1-3%o into the coarse powder particles of the melt-spun sheet with the granularity of 0.1-0.6 mm, filling argon or nitrogen into a sealed mixer, stirring and mixing for 0.5-1 h to prepare a middle broken material, adding the middle broken material into a grinding chamber of an airflow pulverizer, mutually colliding, shearing and grinding the middle broken material under the drive of supersonic speed power medium gas sprayed by a nozzle of the airflow pulverizer, crushing the middle broken material into powder, and adjusting the rotating speed of a classification wheel to enable the granularity of the powder to be 4-6 mu m; adding the powder into a mixer, and mixing for 2-3 hours;
s8, carrying out orientation compression molding on the powder in a magnetic field with the magnetic field strength of 1200-2400 KA/m, vacuum packaging after molding, and maintaining the pressure for 10-120 seconds under 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 ℃, filling argon gas to keep the pressure in the vacuum sintering furnace at 0-0.015 MPa, and performing heat preservation and sintering for 70-120 min;
the temperature in the vacuum sintering furnace is regulated to 1150-1190 ℃ to carry out solution treatment on the green body, and the treatment time is 1-20 h; after the solution treatment is completed, 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 completed, the temperature in the vacuum sintering furnace is reduced to 350-450 ℃ at the speed of 0.5-1 ℃/min, then the temperature is kept for 1-5 h, and the mixture is rapidly cooled to room temperature and discharged from the furnace, thus obtaining the samarium cobalt magnet.
2. The method for manufacturing the samarium cobalt magnet based on the vacuum rapid hardening furnace according to claim 1, wherein in the step 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 x line, and the axis of the water-cooled copper roller is marked as y line; and the included angle between the plane where the x-ray and the y-ray are positioned and the horizontal plane passing through the y-ray is denoted as alpha, and the alpha 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 in the step 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% of the mass of the smelting raw material as a burning loss supplement.
4. The method for manufacturing samarium cobalt magnets based on a vacuum rapid hardening furnace according to claim 1, wherein in S1, pure iron and sponge zirconium may be zirconium-iron alloy.
5. The method for manufacturing the samarium-cobalt magnet based on the vacuum rapid hardening furnace according to claim 1, wherein in the step S2, electrolytic copper and zirconium sponge are placed at the bottom of a crucible, metallic cobalt and pure iron are placed at the middle of the crucible, and metallic samarium in smelting raw materials and metallic samarium in burning loss supplement are placed at the top of the crucible.
6. The method for manufacturing the samarium cobalt magnet based on the vacuum rapid hardening furnace according to claim 1, wherein in S2, the specific steps of melting the melting raw material and the burning loss supplement into molten metal by the vacuum rapid hardening furnace are as follows:
continuously introducing nitrogen into the vacuum rapid hardening furnace, and continuously vacuumizing to keep the vacuum degree in the vacuum rapid hardening furnace at 1000-2000 Pa, wherein the duration of introducing nitrogen and vacuumizing is 30-50 min so as to remove water on the inner surfaces of the smelting raw materials, the burning-loss supplementary materials and the crucible;
continuously vacuumizing to 610-1000 Pa, heating the smelting raw material and the burning loss supplement material in the crucible with intermediate frequency heating power of 40-60 KW, and simultaneously lifting the heating power at a speed of 2-4 KW/min to further remove water on the smelting raw material, the burning loss supplement material and the crucible surface and crystal water on the smelting raw material and the burning loss supplement material;
continuously filling argon into the vacuum rapid hardening furnace when the temperature in the vacuum rapid hardening furnace is increased to 800 ℃ so as to keep the vacuum degree in the vacuum rapid hardening furnace at-0.035 MPa to-0.025 MPa, thereby reducing the melting volatilization loss of the metal samarium;
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 cleaned, and the smelting raw material and the burning loss supplement are smelted into molten metal after refining for 18-26 min.
7. The method according to claim 1, wherein 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, the molten metal in the crucible is poured into the tundish at a speed of 800-2000 g/S, and the depth of the molten metal in the tundish is made to be 70-120 mm.
8. The method for manufacturing a samarium cobalt magnet based on a vacuum rapid hardening furnace according to claim 1, wherein in S7, the supersonic dynamic medium gas is nitrogen.
9. The method according to claim 1, wherein in S3, a baffle plate for preventing molten metal from being pushed forward during casting of the crucible is provided between the crucible and the tundish.
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