CN109599237A - A kind of method that impact system prepares samarium-cobalt permanent-magnetic material - Google Patents

A kind of method that impact system prepares samarium-cobalt permanent-magnetic material Download PDF

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Publication number
CN109599237A
CN109599237A CN201811541259.1A CN201811541259A CN109599237A CN 109599237 A CN109599237 A CN 109599237A CN 201811541259 A CN201811541259 A CN 201811541259A CN 109599237 A CN109599237 A CN 109599237A
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magnetic material
vacuum
nano particle
permanent
alloy
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CN201811541259.1A
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王群华
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032Magnets 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
    • H01F1/04Magnets 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
    • H01F1/047Alloys characterised by their composition
    • H01F1/053Alloys characterised by their composition containing rare earth metals
    • H01F1/055Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/058Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IVa elements, e.g. Gd2Fe14C
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032Magnets 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
    • H01F1/04Magnets 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
    • H01F1/047Alloys characterised by their composition
    • H01F1/053Alloys characterised by their composition containing rare earth metals
    • H01F1/055Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/0555Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 pressed, sintered or bonded together
    • H01F1/0557Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 pressed, sintered or bonded together sintered

Abstract

The invention discloses a kind of methods that impact system prepares samarium-cobalt permanent-magnetic material, adjust SmCo using doping5The ingredient of alloy obtains big alloying component degree of supercooling, and cooperates high speed rapid quenching technique, obtains the anisotropy SmCo of fine grain size5;The present invention combines chemosetting and photocuring, shortens curing time, improves the curing rate of magnetic material, to improve the shaping rate of product, promotes the preparation efficiency of magnetic material.

Description

A kind of method that impact system prepares samarium-cobalt permanent-magnetic material
Technical field
The present invention relates to magnetic material manufacturing fields, and in particular to a kind of method that impact system prepares samarium-cobalt permanent-magnetic material.
Background technique
Rare earth permanent-magnetic material refers to alloy that rare earth metal and magnesium-yttrium-transition metal are formed through permanent magnetism made of certain technique Material.Rare earth permanent-magnetic material is a kind of highest permanent-magnet material of currently known comprehensive performance, the magnetic that it is used than 90th century The magnetic property of steel is more than 100 times high, and much than ferrite, alnico superior performance, the magnetic property than expensive platinum cobalt alloy is also high One times.Due to the use of rare earth permanent-magnetic material, permanent magnet devices are not only promoted to miniaturization, improve the performance of product, And promote the generation of certain particular devices, so rare earth permanent-magnetic material one occurs, cause greatly to pay attention to immediately, develop extremely fast Speed.Rare earth permanent-magnetic material is applied widely in fields such as machinery, electronics, instrument and medical treatment.
SmCo5Rare earth permanent-magnetic material has high magnetic property and high-curie temperature, and especially operating temperature is at 180-250 DEG C When above, which still has high magnetic energy product, coercivity and remanent magnetism, is therefore widely used in aerospace, national defence troops Work, microwave device, communication, Medical Devices, instrument and meter, wind-power electricity generation, various magnetic driving devices, sensor, magnetic processor, The industries such as high-end motor.
SmCo5The traditional preparation methods of rare earth permanent-magnetic material are powder metallurgic method, and technical process includes alloy melting, system Powder, magnetic field compression moulding, sintering and heat treatment etc..It is formed by magnetic field orientating, the alloy of preparation has strong magnetic anisotropy And magnetic property.But the preparation process is complex.
3D printing is for belonging to new technology, in 3D gel print magnetic material product process in the molding of magnetic material It is middle that it is carried out to solidify in printing using chemical method, but since chemosetting needs the regular hour, air exercise printing The size of product has certain limitations, if the printing larger product of product size continues since product is not fully cured in print procedure Material is accumulated above the printable layer not being fully cured to cause the defects of collapsing and deforming, so that the shaping rate of printing product It is low.
Summary of the invention
The present invention provides a kind of method that impact system prepares samarium-cobalt permanent-magnetic material, adjusts SmCo using doping5Alloy Ingredient obtains big alloying component degree of supercooling, and cooperates high speed rapid quenching technique, obtains the anisotropy of fine grain size SmCo5;The present invention combines chemosetting and photocuring, shortens curing time, improves the curing rate of magnetic material, thus The shaping rate of product is improved, the preparation efficiency of magnetic material is promoted.
To achieve the goals above, above-mentioned purpose is realized, the present invention provides a kind of impact systems to prepare samarium-cobalt permanent-magnetic material Method, the samarium-cobalt permanent-magnetic material main body by following components press general formula: Sm (Co1-yTiy)5-xSix, wherein y=0.03-0.1, x= 0.2-0.5;
This method comprises the following steps:
(1) each element is weighed according to above-mentioned general formula carry out ingredient;
(2) ingredient is placed in smelting furnace, at least up to 5 × 10 is vacuumized in furnace-3Pa;Then, helium injection gas to furnace pressure is 50-80kPa;It is warming up to 1300-1450 DEG C of fusing, is cast in water cooled copper mould after stirring, refining stand-by;
(3) obtained alloy cast ingot is crushed, is fitted into vacuum and gets rid of in the quartz ampoule in machine, quartz ampoule bottom end nozzle diameter is 0.5-0.8mm gets rid of after the cavity with machine vacuumizes vacuum, protective gas is filled with into cavity;It connects vacuum and gets rid of band electromechanical source, The alloy in fused quartz pipe is heated, meanwhile, control quartz ampoule bottom end nozzle to copper roller surface distance is 1-5mm, adjusts vacuum Band machine copper roller revolving speed is got rid of, makes copper roller revolving speed 55-65m/s, mother alloy melt is ejected on the copper roller of rotation, obtain each to different Property SmCo5Type rare earth permanent-magnetic material strip;Strip cracker is worn into nano particle;
Both (4) 2- methacrylic chloride and photosensitive resin are mixed with volume ratio 1:(3-6) first, stirring 50-80min makes It is uniformly mixed and obtains mixed liquor, add above-mentioned nano particle, the volume ratio of mixed liquor and nano particle is 1:(1.5-3), and 30-60min is stirred to be uniformly mixed;
(5) the silicates dispersing agent of 1-3wt% is added, the initiator potassium persulfate of 0.2-0.5wt% continues to stir 80- 100min is mixed thoroughly slurry, and wherein nano particle accounts for the 55%-65vol% of slurry volume fraction, phosphoric acid For 500-800Pa.s;
(6) obtained slurry is fitted into the syringe of gel printer, print speed 15-20mm/s, every one layer of completion is beaten Print, spraying device will spray one layer of misty catalyst to print surface, and whole printing process carries out ultraviolet light irradiation;
(7) obtained green body dry 20-30h at 70-85 DEG C will be printed, dry green body 900- in a vacuum will be passed through 1050 DEG C are sintered, and sintering time 10-20h obtains permanent-magnet material.
Iron-based soft magnetic composite cores prepared by the present invention have following advantages:
(1) SmCo is adjusted using doping5The ingredient of alloy obtains big alloying component degree of supercooling, and cooperates high speed fast quenching work Skill obtains the anisotropy SmCo of fine grain size5
(2) present invention combines chemosetting and photocuring, shortens curing time, improves the curing rate of magnetic material, from And the shaping rate of product is improved, promote the preparation efficiency of magnetic material.
Specific embodiment
Embodiment one
The samarium-cobalt permanent-magnetic material main body of the present embodiment presses general formula: Sm (Co by following components0.97Ti0.03)4.8Si0.2
Each element, which is weighed, according to above-mentioned general formula carries out ingredient;Ingredient is placed in smelting furnace, at least up to 5 are vacuumized in furnace ×10-3Pa;Then, helium injection gas to furnace pressure is 50kPa;1300 DEG C of fusings are warming up to, are cast to water-cooled copper after stirring, refining It is stand-by in mould.
Obtained alloy cast ingot is crushed, vacuum is fitted into and gets rid of in the quartz ampoule in machine, quartz ampoule bottom end nozzle diameter is 0.5mm gets rid of after the cavity with machine vacuumizes vacuum, protective gas is filled with into cavity;It connects vacuum and gets rid of band electromechanical source, heating Alloy in fused quartz pipe, meanwhile, control quartz ampoule bottom end nozzle to copper roller surface distance is 1-5mm, and adjustment vacuum gets rid of band Machine copper roller revolving speed makes copper roller revolving speed 55-65m/s, mother alloy melt is ejected on the copper roller of rotation, anisotropy is obtained SmCo5Type rare earth permanent-magnetic material strip.Strip cracker is worn into nano particle.
2- methacrylic chloride and photosensitive resin are mixed with volume ratio 1:3 first, stirring 50min makes the two mixing equal It is even to obtain mixed liquor, add above-mentioned nano particle, the volume ratio of mixed liquor and nano particle is 1:1.5, and stirs 30- 60min is uniformly mixed;The silicates dispersing agent of 1wt% is added, the initiator potassium persulfate of 0.2wt% continues to stir 80min is mixed thoroughly slurry, and wherein nano particle accounts for the 55% of slurry volume fraction, phosphoric acid 500a.s.
Obtained slurry is fitted into the syringe of gel printer, print speed 15mm/s, one layer of printing of every completion, Spraying device will spray one layer of misty catalyst to print surface, and whole printing process carries out ultraviolet light irradiation;It will beat Obtained green body dry 20h at 70 DEG C is printed, will be sintered for 900 DEG C in a vacuum by dry green body, sintering time For 10h, permanent-magnet material is obtained.
Embodiment two
The samarium-cobalt permanent-magnetic material main body of the present embodiment presses general formula: Sm (Co by following components0.9Ti0.1)4.5Si0.5
Each element, which is weighed, according to above-mentioned general formula carries out ingredient;Ingredient is placed in smelting furnace, at least up to 5 are vacuumized in furnace ×10-3Pa;Then, helium injection gas to furnace pressure is 80kPa;1450 DEG C of fusings are warming up to, are cast to water-cooled copper after stirring, refining It is stand-by in mould.
Obtained alloy cast ingot is crushed, vacuum is fitted into and gets rid of in the quartz ampoule in machine, quartz ampoule bottom end nozzle diameter is 0.8mm gets rid of after the cavity with machine vacuumizes vacuum, protective gas is filled with into cavity;It connects vacuum and gets rid of band electromechanical source, heating Alloy in fused quartz pipe, meanwhile, control quartz ampoule bottom end nozzle to copper roller surface distance is 5mm, and adjustment vacuum gets rid of band machine Copper roller revolving speed makes copper roller revolving speed 65m/s, mother alloy melt is ejected on the copper roller of rotation, anisotropy SmCo is obtained5Type Rare earth permanent-magnetic material strip.Strip cracker is worn into nano particle.
2- methacrylic chloride and photosensitive resin are mixed with volume ratio 1:6 first, stirring 80min makes the two mixing equal It is even to obtain mixed liquor, add above-mentioned nano particle, the volume ratio of mixed liquor and nano particle is 1:3, and stirs 60min mixing Uniformly;The silicates dispersing agent of 3wt% is added, the initiator potassium persulfate of 0.5wt% continues stirring 100min and to expect Slurry is mixed thoroughly, and wherein nano particle accounts for the 65vol% of slurry volume fraction, phosphoric acid 800Pa.s.
Obtained slurry is fitted into the syringe of gel printer, print speed 20mm/s, one layer of printing of every completion, Spraying device will spray one layer of misty catalyst to print surface, and whole printing process carries out ultraviolet light irradiation;It will beat Obtained green body dry 30h at 85 DEG C is printed, will be sintered for 1050 DEG C in a vacuum by dry green body, sintering time For 20h, permanent-magnet material is obtained.
Comparative example
Match SmCo is molten for alloy, the alloy prepared will be melted and be put into the porose quartz test tube in bottom of vacuum chamber, recycled three times It vacuumizes and enters high-purity Ar gas with reversely charging;Fusion alloying is heated using applications of high frequency electromagnetic method, then Ar gas is filled with quartz test tube to melt Melt aspect product to be blown on the runner of rotation into alloy thin band;Gained alloy thin band is protected 400 DEG C under the conditions of under Ar gas shielded Temperature 1 hour, then cools to the furnace and comes out of the stove at room temperature.Permanent-magnet material is cast in remelting.
The permanent-magnet material of embodiment 1-2 and comparative example to same shape and size carries out magnetism testing, 25 DEG C into The coercivity of row test, (1) material is measured using KM-Ot ype List-Koerzimeter coercivity instrument;(2) remanent magnetization Intensity uses static magnetic performance measuring instrument, is saturation induction density of the magnetic induction intensity under 800A/m as alloy using magnetic field Bs.Test result is shown: the coercivity of embodiment 1-2 relatively example rises 10% or more, remanent magnetization relatively example Improve 12% or more.

Claims (1)

1. a kind of method that impact system prepares samarium-cobalt permanent-magnetic material, which presses general formula: Sm by following components (Co1-yTiy)5-xSix, wherein y=0.03-0.1, x=0.2-0.5;
This method comprises the following steps:
(1) each element is weighed according to above-mentioned general formula carry out ingredient;
(2) ingredient is placed in smelting furnace, at least up to 5 × 10 is vacuumized in furnace-3Pa;Then, helium injection gas to furnace pressure is 50-80kPa;It is warming up to 1300-1450 DEG C of fusing, is cast in water cooled copper mould after stirring, refining stand-by;
(3) obtained alloy cast ingot is crushed, is fitted into vacuum and gets rid of in the quartz ampoule in machine, quartz ampoule bottom end nozzle diameter is 0.5-0.8mm gets rid of after the cavity with machine vacuumizes vacuum, protective gas is filled with into cavity;It connects vacuum and gets rid of band electromechanical source, The alloy in fused quartz pipe is heated, meanwhile, control quartz ampoule bottom end nozzle to copper roller surface distance is 1-5mm, adjusts vacuum Band machine copper roller revolving speed is got rid of, makes copper roller revolving speed 55-65m/s, mother alloy melt is ejected on the copper roller of rotation, obtain each to different Property SmCo5Type rare earth permanent-magnetic material strip;Strip cracker is worn into nano particle;
Both (4) 2- methacrylic chloride and photosensitive resin are mixed with volume ratio 1:(3-6) first, stirring 50-80min makes It is uniformly mixed and obtains mixed liquor, add above-mentioned nano particle, the volume ratio of mixed liquor and nano particle is 1:(1.5-3), and 30-60min is stirred to be uniformly mixed;
(5) the silicates dispersing agent of 1-3wt% is added, the initiator potassium persulfate of 0.2-0.5wt% continues to stir 80- 100min is mixed thoroughly slurry, and wherein nano particle accounts for the 55%-65vol% of slurry volume fraction, phosphoric acid For 500-800Pa.s;
(6) obtained slurry is fitted into the syringe of gel printer, print speed 15-20mm/s, every one layer of completion is beaten Print, spraying device will spray one layer of misty catalyst to print surface, and whole printing process carries out ultraviolet light irradiation;
(7) obtained green body dry 20-30h at 70-85 DEG C will be printed, dry green body 900- in a vacuum will be passed through 1050 DEG C are sintered, and sintering time 10-20h obtains permanent-magnet material.
CN201811541259.1A 2018-12-17 2018-12-17 A kind of method that impact system prepares samarium-cobalt permanent-magnetic material Pending CN109599237A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113637180A (en) * 2020-05-11 2021-11-12 清华-伯克利深圳学院筹备办公室 Optically anisotropic hydrogel, preparation method thereof, production system thereof and optical device

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107610856A (en) * 2017-10-22 2018-01-19 苏州南尔材料科技有限公司 A kind of preparation method with ceramic layer samarium-cobalt permanent-magnetic material
CN107803505A (en) * 2017-10-22 2018-03-16 苏州南尔材料科技有限公司 A kind of 3d printings prepare the preparation method of Mn-Bi-Al permanent-magnet material
CN108899151A (en) * 2018-06-17 2018-11-27 苏州诺弘添恒材料科技有限公司 A kind of preparation method of the samarium cobalt permanent magnet body of surface treatment

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107610856A (en) * 2017-10-22 2018-01-19 苏州南尔材料科技有限公司 A kind of preparation method with ceramic layer samarium-cobalt permanent-magnetic material
CN107803505A (en) * 2017-10-22 2018-03-16 苏州南尔材料科技有限公司 A kind of 3d printings prepare the preparation method of Mn-Bi-Al permanent-magnet material
CN108899151A (en) * 2018-06-17 2018-11-27 苏州诺弘添恒材料科技有限公司 A kind of preparation method of the samarium cobalt permanent magnet body of surface treatment

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113637180A (en) * 2020-05-11 2021-11-12 清华-伯克利深圳学院筹备办公室 Optically anisotropic hydrogel, preparation method thereof, production system thereof and optical device
CN113637180B (en) * 2020-05-11 2023-12-05 清华-伯克利深圳学院筹备办公室 Optically anisotropic hydrogel, preparation method, production system thereof and optical device

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Application publication date: 20190409