CN103794355B - A kind of preparation method of the neodymium iron boron magnetic body with high-Curie-point - Google Patents
A kind of preparation method of the neodymium iron boron magnetic body with high-Curie-point Download PDFInfo
- Publication number
- CN103794355B CN103794355B CN201410064216.4A CN201410064216A CN103794355B CN 103794355 B CN103794355 B CN 103794355B CN 201410064216 A CN201410064216 A CN 201410064216A CN 103794355 B CN103794355 B CN 103794355B
- Authority
- CN
- China
- Prior art keywords
- magnet
- magnetic
- sintering
- curie
- glass tube
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 229910001172 neodymium magnet Inorganic materials 0.000 title claims abstract description 12
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 title claims abstract description 9
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000005245 sintering Methods 0.000 claims abstract description 17
- 239000000843 powder Substances 0.000 claims abstract description 15
- 229910052779 Neodymium Inorganic materials 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 7
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 6
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000004381 surface treatment Methods 0.000 claims abstract description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 54
- 229910052786 argon Inorganic materials 0.000 claims description 27
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 16
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 13
- 229910052802 copper Inorganic materials 0.000 claims description 13
- 239000010949 copper Substances 0.000 claims description 13
- 238000005266 casting Methods 0.000 claims description 12
- 230000005684 electric field Effects 0.000 claims description 12
- 239000007789 gas Substances 0.000 claims description 10
- 229910045601 alloy Inorganic materials 0.000 claims description 9
- 239000000956 alloy Substances 0.000 claims description 9
- 229910052742 iron Inorganic materials 0.000 claims description 9
- 238000002844 melting Methods 0.000 claims description 9
- 230000008018 melting Effects 0.000 claims description 9
- 238000012545 processing Methods 0.000 claims description 9
- 229910000640 Fe alloy Inorganic materials 0.000 claims description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 239000001257 hydrogen Substances 0.000 claims description 8
- 229910052739 hydrogen Inorganic materials 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 238000012986 modification Methods 0.000 claims description 8
- 230000004048 modification Effects 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 8
- 238000010792 warming Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 229910001021 Ferroalloy Inorganic materials 0.000 claims description 6
- 238000009413 insulation Methods 0.000 claims description 6
- MTRJKZUDDJZTLA-UHFFFAOYSA-N iron yttrium Chemical compound [Fe].[Y] MTRJKZUDDJZTLA-UHFFFAOYSA-N 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- 238000005496 tempering Methods 0.000 claims description 5
- 229910000604 Ferrochrome Inorganic materials 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- 238000013019 agitation Methods 0.000 claims description 4
- 238000007605 air drying Methods 0.000 claims description 4
- 239000012670 alkaline solution Substances 0.000 claims description 4
- 229910021538 borax Inorganic materials 0.000 claims description 4
- 238000006356 dehydrogenation reaction Methods 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 238000009792 diffusion process Methods 0.000 claims description 4
- 230000000694 effects Effects 0.000 claims description 4
- 230000005674 electromagnetic induction Effects 0.000 claims description 4
- 238000007499 fusion processing Methods 0.000 claims description 4
- 230000006698 induction Effects 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 238000003754 machining Methods 0.000 claims description 4
- -1 manganeisen Inorganic materials 0.000 claims description 4
- 238000003801 milling Methods 0.000 claims description 4
- BDDGCXUIIBADED-UHFFFAOYSA-N neodymium Chemical compound [Nd].[Nd].[Nd].[Nd] BDDGCXUIIBADED-UHFFFAOYSA-N 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 239000002002 slurry Substances 0.000 claims description 4
- 239000004328 sodium tetraborate Substances 0.000 claims description 4
- 235000010339 sodium tetraborate Nutrition 0.000 claims description 4
- 239000007921 spray Substances 0.000 claims description 4
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 3
- 229910052737 gold Inorganic materials 0.000 claims description 3
- 239000010931 gold Substances 0.000 claims description 3
- 230000005389 magnetism Effects 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 238000010791 quenching Methods 0.000 claims description 2
- 230000000171 quenching effect Effects 0.000 claims description 2
- 210000001367 artery Anatomy 0.000 claims 1
- 238000002347 injection Methods 0.000 claims 1
- 239000007924 injection Substances 0.000 claims 1
- 239000000155 melt Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 9
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052727 yttrium Inorganic materials 0.000 abstract description 3
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 abstract description 3
- 239000003708 ampul Substances 0.000 description 6
- 239000010453 quartz Substances 0.000 description 6
- 229910052772 Samarium Inorganic materials 0.000 description 4
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000011572 manganese Substances 0.000 description 3
- 238000005507 spraying Methods 0.000 description 3
- 229910052692 Dysprosium Inorganic materials 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000006247 magnetic powder Substances 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 150000002910 rare earth metals Chemical class 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 229910052688 Gadolinium Inorganic materials 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 229910052771 Terbium Inorganic materials 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 230000036760 body temperature Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Hard Magnetic Materials (AREA)
- Manufacturing Cores, Coils, And Magnets (AREA)
Abstract
The present invention relates to a kind of preparation method of the neodymium iron boron magnetic body with high-Curie-point, this magnet adopts the permanent-magnet material of following atom and molecule formula: (LawYxNd1-w-x）a（Fe1-y-zMnyCrz）100-a-b-cBbFc, wherein w=0.12-0.14, x=0.25-0.32, y=0.12-0.27, z=0.07-0.09, a=26-28, b=4.5-5.6, c=0.3-0.5, the method comprises the steps: that (1) makes permanent-magnet powder, (2) base, (3) sintering, (4) surface treatment. Magnet prepared by this method, use lanthanum and yttrium to replace neodymium to reduce costs by interpolation, improve the curie point of material by adding Cr and F, finally further improve the coercivity of magnet by surface treatment, make magnet of the present invention be more suitable for using for hot environment.
Description
Affiliated technical field
The present invention relates to a kind of preparation method of the neodymium iron boron magnetic body with high-Curie-point.
Background technology
Rely on excellent magnetic property, the range of application of Nd-Fe-B permanent magnet constantly increases. Nearest environmental problemChallenge has made the range of application of these magnets expand to industrial equipment, electric automobile and wind-force from household electrical appliance to send outMotor. Require further to improve the performance of Nd-Fe-B magnet.
But the Curie temperature of Nd-Fe-B permanent-magnet material is not high, generally, below 130 DEG C, magnetic flux density is not simultaneouslyHeight, because there is defect and cause coercivity not high in this two classes magnetic material in crystallization process. Existing prior artPropose, taking existing neodymium iron boron magnetic body as matrix, the Curie who adds some auxiliary elements and improve neodymium iron boron magnetic bodyTemperature and coercivity. But that adds all includes the element that dysprosium, gadolinium, terbium, samarium etc. belong to heavy rare earth substantially,And this class rare earth material is along with protection and the management of country to resource, price is improving constantly.
In this case, what should consider is the use amount that how can reduce counterweight rare-earth-type material, comes realNow can meet under the prerequisite of performance, reduce production costs.
Summary of the invention
The invention provides a kind of preparation method of the neodymium iron boron magnetic body with high-Curie-point, use the method to prepareMagnet still has good magnetic property under high-temperature work environment.
To achieve these goals, the preparation side of a kind of neodymium iron boron magnetic body with high-Curie-point provided by the inventionMethod, this magnet adopts the permanent-magnet material of following molecular formula: (LawYxNd1-w-x)a(Fe1-y-zMnyCrz)100-a-b-cBbFc, wherein w=0.12-0.14, x=0.25-0.32, y=0.12-0.27, z=0.07-0.09, a=26-28,B=4.5-5.6, c=0.3-0.5, the method comprises the steps:
(1) make permanent-magnet powder
Take raw material by proportioning, after the raw material after taking is mixed, under argon gas atmosphere, put into vacuum electromagnetic induction furnaceMelt, concrete fusion process is as follows: carry out vacuum melting taking neodymium and iron atom ratio as the mode of 1: 2,Then add yttrium iron alloy, lanthanum ferroalloy, manganeisen, ferrochrome, ferric flouride and borax by compositionMelt again, finally add the iron of the surplus of calculating by proportioning, ingot casting after melting;
Ingot casting is put into bottom and open the quartz glass tube of aperture, and be placed in impulse electric field and pulsed magnetic field dressIn the vacuum spray to cast stove of putting, place water cooled copper mould in the lower end of quartz glass tube, ingot casting is under high-purity argon gas protectionInduction melting becomes liquid, then electrode is inserted in melt, applies impulse electric field, carries out electro-pulse modification processing;When alloy melt electro-pulse modification is processed, the impulse electric field parameter of employing is: pulse frequency 1000-1500Hz,Pulse current peak density 240-350A/cm2, pulse width 10-50 μ s, processing time 35-50s, executes subsequentlyAdd pulsed magnetic field, the magnetic line of force, through copper mold cavity, is then opened the air valve being connected with quartz glass tube, meltUnder the effect of spraying air pressure, inject fast copper mold cavity by the aperture of quartz glass tube bottom, cold the making of speedRapid-hardening flake;
Above-mentioned rapid-hardening flake, after adding the reactor of hydrogen crushing furnace to vacuumize, is poured to hydrogen and carries out the broken dehydrogenation of hydrogenProcessing is cooled to after room temperature, takes out and is placed in airflow milling, makes the magnetic that particle diameter is 10-20 μ m;
(2) base
In argon shield atmosphere, in argon atmospher, with 1.5-2 ton/cm2Pressure by this magnetic compacting, simultaneouslyUnder the magnetic field of 16-19kOe, be orientated, make blank;
(3) sintering
Molded blank is put under argon shield to sintering furnace and carried out sintering, be first warming up to 5-10 DEG C/min640-660 DEG C, insulation 3-4h, is then warming up to 1000-1060 DEG C of sintering 4-5h, two with 10-15 DEG C/minAfter inferior tempering, be down to room temperature;
(4) surface treatment
Use successively alkaline solution, deionized water, acid solution and washed with de-ionized water machining to obtain magnet body,And dry, obtain magnet body, for subsequent use;
By alloy Dy42Co56Powder and average grain diameter are the Tb of 1 μ m4O7With the ratio of weight ratio 1: 1-2After mixing, obtain mixture of powders, this mixture of powders is tied with weight fraction 30-40% and deionized waterClose formation slurry, under the condition of ultrasonic agitation, above-mentioned magnet body is immersed to 15-20 second, by magnet originallyBody takes out, and uses immediately heated air drying, then at 850-890 DEG C, in argon atmospher, carries out DIFFUSION TREATMENT5-7h, rear quenching, obtains product.
Magnet prepared by this method, uses lanthanum and yttrium to replace neodymium to reduce costs by interpolation, by adding CrImprove the curie point of material with F, finally further improve the coercivity of magnet by surface treatment, make thisThe magnet of invention is more suitable for using for hot environment.
Detailed description of the invention
Embodiment mono-
This magnet of the present embodiment adopts the permanent-magnet material of following molecular formula: (La0.12Y0.25Nd0.63)26(Fe0.81Mn0.12Cr0.07)69.2B4.5F0.3。
Take raw material by proportioning, after the raw material after taking is mixed, under argon gas atmosphere, put into vacuum electromagnetic induction furnaceMelt, concrete fusion process is as follows: carry out vacuum melting taking neodymium and iron atom ratio as the mode of 1: 2,Then add yttrium iron alloy, lanthanum ferroalloy, manganeisen, ferrochrome, ferric flouride and borax by compositionMelt again, finally add the iron of the surplus of calculating by proportioning, ingot casting after melting.
Ingot casting is put into bottom and open the quartz glass tube of aperture, and be placed in impulse electric field and pulsed magnetic field dressIn the vacuum spray to cast stove of putting, place water cooled copper mould in the lower end of quartz ampoule, ingot casting induction under high-purity argon gas protectionBe fused into liquid, then electrode inserted in melt, apply impulse electric field, carry out electro-pulse modification processing. CloseWhen gold melt electro-pulse modification is processed, the impulse electric field parameter of employing is: pulse frequency 1000Hz, Pulse ElectricStream peak density 240A/cm2, pulse width 10 μ s, processing time 50s, with after-applied pulsed magnetic field, magneticThe line of force, through copper mold cavity, is then opened the air valve being connected with quartz ampoule, and melt is spraying under the effect of air pressureAperture by quartz ampoule bottom injects copper mold cavity fast, the cold rapid-hardening flake that makes of speed.
Above-mentioned rapid-hardening flake, after adding the reactor of hydrogen crushing furnace to vacuumize, is poured to hydrogen and carries out the broken dehydrogenation of hydrogenProcessing is cooled to after room temperature, takes out and is placed in airflow milling, makes the magnetic that particle diameter is 10-20 μ m.
In argon shield atmosphere, in argon atmospher, with 1.5 tons/cm2Pressure by this magnetic powder compacting, simultaneouslyUnder the magnetic field of 16-19kOe, be orientated, make blank.
Molded blank is put under argon shield to sintering furnace and is carried out sintering, be first warming up to 640 DEG C with 5 DEG C/min,Insulation 4h, is then warming up to 1000 DEG C of sintering 5h with 10 DEG C/min, after double tempering, is down to room temperature.
Use successively alkaline solution, deionized water, acid solution and washed with de-ionized water machining to obtain magnet body,And dry, obtain magnet body, for subsequent use; By alloy Dy42Co56Powder and average grain diameter are the Tb of 1 μ m4O7Mix with the weight ratio ratio of 1: 1, this mixture of powders is tied with weight fraction 30% and deionized waterClose formation slurry, under the condition of ultrasonic agitation, above-mentioned magnet body is immersed to 15 seconds, by magnet bodyTake out, and use immediately heated air drying, then at 850 DEG C, in argon atmospher, carry out DIFFUSION TREATMENT 7h, after quenchFire, obtains product.
Embodiment bis-
This magnet of the present embodiment adopts the permanent-magnet material of following molecular formula: (La0.14Y0.32Nd0.54)28(Fe0.64Mn0.27Cr0.09)65.9B5.6F0.5, wherein w=0.14, x=0.32, y=0.27, z=0.09, a=28,b＝5.6，c＝0.5。
Take raw material by proportioning, after the raw material after taking is mixed, under argon gas atmosphere, put into vacuum electromagnetic induction furnaceMelt, concrete fusion process is as follows: carry out vacuum melting taking neodymium and iron atom ratio as the mode of 1: 2,Then add yttrium iron alloy, lanthanum ferroalloy, manganeisen, ferrochrome, ferric flouride and borax by compositionMelt again, finally add the iron of the surplus of calculating by proportioning, ingot casting after melting.
Ingot casting is put into bottom and open the quartz glass tube of aperture, and be placed in impulse electric field and pulsed magnetic field dressIn the vacuum spray to cast stove of putting, place water cooled copper mould in the lower end of quartz ampoule, ingot casting induction under high-purity argon gas protectionBe fused into liquid, then electrode inserted in melt, apply impulse electric field, carry out electro-pulse modification processing. CloseWhen gold melt electro-pulse modification is processed, the impulse electric field parameter of employing is: pulse frequency 1500Hz, Pulse ElectricStream peak density 350A/cm2, pulse width 50 μ s, processing time 35s, with after-applied pulsed magnetic field, magneticThe line of force, through copper mold cavity, is then opened the air valve being connected with quartz ampoule, and melt is spraying under the effect of air pressureAperture by quartz ampoule bottom injects copper mold cavity fast, the cold rapid-hardening flake that makes of speed.
Above-mentioned rapid-hardening flake, after adding the reactor of hydrogen crushing furnace to vacuumize, is poured to hydrogen and carries out the broken dehydrogenation of hydrogenProcessing is cooled to after room temperature, takes out and is placed in airflow milling, makes the magnetic that particle diameter is 10-20 μ m.
In argon shield atmosphere, in argon atmospher, with 2 tons/cm2Pressure by this magnetic powder compacting, exist simultaneouslyUnder the magnetic field of 19kOe, be orientated, make blank.
Molded blank is put under argon shield to sintering furnace and carried out sintering, be first warming up to 10 DEG C/min660 DEG C, insulation 3h, is then warming up to 1060 DEG C of sintering 4h with 15 DEG C/min, after double tempering, is down to chamberTemperature.
Use successively alkaline solution, deionized water, acid solution and washed with de-ionized water machining to obtain magnet body,And dry, obtain magnet body, for subsequent use; By alloy Dy42Co56Powder and average grain diameter are the Tb of 1 μ m4O7Mix with the weight ratio ratio of 1: 2, this mixture of powders is tied with weight fraction 40% and deionized waterClose formation slurry, under the condition of ultrasonic agitation, above-mentioned magnet body is immersed to 20 seconds, by magnet bodyTake out, and use immediately heated air drying, then at 890 DEG C, in argon atmospher, carry out DIFFUSION TREATMENT 5h, after quenchFire, obtains product.
Comparative example
Prepare burden according to atomic percentage conc: 25% neodymium, 1% cobalt, 1.5% silicon, 2% manganese, 10%Boron and the iron of surplus, 0.1% Dy-Fe alloy wherein in Dy-Fe alloy dysprosium account for weight percentage be 5%,0.5% samarium ferroalloy wherein in samarium ferroalloy samarium account for weight percentage be 5%, 1.5% yttrium iron alloy itsIn middle yttrium iron alloy, to account for weight percentage be 10% to yttrium. To in feed metal induction furnace, melt, after fusing1550 DEG C of refinings 30 minutes, the then cooling alloy pig that is cast into constant weight and shape. Subsequently, by alloyIngot joins in spun furnace, under inert atmosphere (as argon gas) protection at the temperature of 1350 DEG C～1450 DEG CSpun furnace in eddy-current heating remelting, obtain alloy molten solution. Aperture by this alloy molten solution through crucible bottom nozzleThe water-cooled copper roller or the molybdenum roller surface moment that are ejected into High Rotation Speed solidify, and cooling velocity can reach 104～106K/s,Form amorphous or crystallite metal alloy strip. Wherein the wheel border line speed of water-cooled wheel is about 20～30m/s.The alloy thin band obtaining is placed in to disintegrating machine, under the protection of argon gas, through broken, and crosses 40 mesh sieves;By the powder after screening again under argon shield, heat treatment 10 minutes under 600 DEG C～700 DEG C conditions,Obtain final magnetic. Utilize Magnetic field press, by the powder that mixes under the magnetic field of 1.7T, be orientated toType, then pass through isostatic cool pressing, moulding pressed compact is placed in to vacuum sintering furnace, little at 1075 DEG C of sintered heat insulatings 3Time, 890 DEG C of one-level tempering insulations 2 hours, 560 DEG C of second annealing insulations 3 hours, obtain sintering magneticBody.
Embodiment 1-2 to same shape and size and the permanent-magnet of comparative example carry out magnetism testing, testCondition is: condition 1: under the indoor environment that temperature is 25 DEG C, test; Condition 2: it is 60 DEG C that magnet is placed in to temperatureEnvironment under test after 100h, measure maximum magnetic energy product (BH)maxAnd coercivity. Test result is aobviousShow: the maximum magnetic energy product relative conditon 1 in condition 2 of the embodiment 1-2 10-15% that only declines, coercivity onlyDecline 9-12%, and comparative example declines and exceedes 26%, coercivity at the maximum magnetic energy product relative conditon 1 of condition 2Only decline and exceed 22%.
Claims (1)
1. have a preparation method for the neodymium iron boron magnetic body of high-Curie-point, this magnet adopts the permanent magnetism of following molecular formulaMaterial: (LawYxNd1-w-x)a(Fe1-y-zMnyCrz)100-a-b-cBbFc, wherein w=0.12-0.14, x=0.25-0.32,Y=0.12-0.27, z=0.07-0.09, a=26-28, b=4.5-5.6, c=0.3-0.5, the method comprises the steps:
(1) make permanent-magnet powder
Take raw material by proportioning, after the raw material after taking is mixed, under argon gas atmosphere, put into vacuum electromagnetic induction furnace and carry outFusing, concrete fusion process is as follows: carry out vacuum melting taking neodymium and iron atom ratio as the mode of 1: 2, thenAdd yttrium iron alloy, lanthanum ferroalloy, manganeisen, ferrochrome, ferric flouride and borax to enter again by compositionRow melts, and finally adds the iron of the surplus of calculating by proportioning, ingot casting after melting;
Ingot casting is put into bottom and open the quartz glass tube of aperture, and be placed in impulse electric field and pulsed magnetic field apparatusIn vacuum spray to cast stove, place water cooled copper mould in the lower end of quartz glass tube, ingot casting induction under high-purity argon gas protectionBe fused into liquid, then electrode inserted in melt, apply impulse electric field, carry out electro-pulse modification processing; CloseWhen gold melt electro-pulse modification is processed, the impulse electric field parameter of employing is: pulse frequency 1000-1500Hz, arteries and veinsRush current peak density 240-350A/cm2, pulse width 10-50 μ s, processing time 35-50s, with after-appliedPulsed magnetic field, the magnetic line of force, through copper mold cavity, is then opened the air valve being connected with quartz glass tube, and melt existsUnder the effect of injection air pressure, inject fast copper mold cavity by the aperture of quartz glass tube bottom, the cold speed that makes of speedSolidifying sheet;
Above-mentioned rapid-hardening flake, after adding the reactor of hydrogen crushing furnace to vacuumize, is poured to hydrogen and carries out the broken dehydrogenation processing of hydrogenBe cooled to after room temperature, take out and be placed in airflow milling, make the magnetic that particle diameter is 10-20 μ m;
(2) base
In argon shield atmosphere, in argon atmospher, with 1.5-2 ton/cm2Pressure by this magnetic compacting, exist simultaneouslyUnder the magnetic field of 16-19kOe, be orientated, make blank;
(3) sintering
Molded blank is put under argon shield to sintering furnace and carried out sintering, be first warming up to 5-10 DEG C/min640-660 DEG C, insulation 3-4h, is then warming up to 1000-1060 DEG C of sintering 4-5h, two with 10-15 DEG C/minAfter inferior tempering, be down to room temperature;
(4) surface treatment
Use successively alkaline solution, deionized water, acid solution and washed with de-ionized water machining to obtain magnet body, andDry, obtain magnet body, for subsequent use;
By alloy Dy42Co56Powder and average grain diameter are the Tb of 1 μ m4O7Ratio with weight ratio 1: 1-2 is carried outAfter mixing, obtain mixture of powders, this mixture of powders is combined to shape with weight fraction 30-40% with deionized waterForm slurry is immersed 15-20 second by above-mentioned magnet body under the condition of ultrasonic agitation, and magnet body is gotGo out, and use heated air drying immediately, then at 850-890 DEG C, in argon atmospher, carry out DIFFUSION TREATMENT 5-7h,Rear quenching, obtains product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410064216.4A CN103794355B (en) | 2014-02-25 | 2014-02-25 | A kind of preparation method of the neodymium iron boron magnetic body with high-Curie-point |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410064216.4A CN103794355B (en) | 2014-02-25 | 2014-02-25 | A kind of preparation method of the neodymium iron boron magnetic body with high-Curie-point |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103794355A CN103794355A (en) | 2014-05-14 |
| CN103794355B true CN103794355B (en) | 2016-05-18 |
Family
ID=50669922
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410064216.4A Active CN103794355B (en) | 2014-02-25 | 2014-02-25 | A kind of preparation method of the neodymium iron boron magnetic body with high-Curie-point |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103794355B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP7167665B2 (en) * | 2018-11-29 | 2022-11-09 | トヨタ自動車株式会社 | Rare earth magnet and manufacturing method thereof |
| CN113921263A (en) * | 2021-11-10 | 2022-01-11 | 赣州市钜磁科技有限公司 | Preparation method of sintered neodymium-iron-boron permanent magnet material containing lanthanum and yttrium |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1649046A (en) * | 2004-01-26 | 2005-08-03 | Tdk株式会社 | Forming method in magnetic field, and method for producing rare-earth sintered magnet |
| CN102568729A (en) * | 2012-01-10 | 2012-07-11 | 福州大学 | Method for preparing bulk composite nanocrystalline rare earth permanent magnetic material |
| CN102667978A (en) * | 2009-10-10 | 2012-09-12 | 株式会社丰田中央研究所 | Rare earth magnet material and method for producing the same |
| CN103280288A (en) * | 2013-06-25 | 2013-09-04 | 李超 | Manufacturing method of high-coercivity samarium-cobalt-based permanent magnet materials |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002038245A (en) * | 2000-07-27 | 2002-02-06 | Hitachi Metals Ltd | Rare earth alloy powder for rermanent magnet and method for manufacturing rare earth permanent magnet |
-
2014
- 2014-02-25 CN CN201410064216.4A patent/CN103794355B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1649046A (en) * | 2004-01-26 | 2005-08-03 | Tdk株式会社 | Forming method in magnetic field, and method for producing rare-earth sintered magnet |
| CN102667978A (en) * | 2009-10-10 | 2012-09-12 | 株式会社丰田中央研究所 | Rare earth magnet material and method for producing the same |
| CN102568729A (en) * | 2012-01-10 | 2012-07-11 | 福州大学 | Method for preparing bulk composite nanocrystalline rare earth permanent magnetic material |
| CN103280288A (en) * | 2013-06-25 | 2013-09-04 | 李超 | Manufacturing method of high-coercivity samarium-cobalt-based permanent magnet materials |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103794355A (en) | 2014-05-14 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107316726B (en) | A kind of preparation method of sintered samarium cobalt magnet | |
| CN104576028A (en) | Methods for manufacturing cerium-rich anisotropy nano-crystalline rare-earth permanent magnets | |
| CN103014477B (en) | Method for smelting iron-based nanocrystalline master alloy | |
| CN108335819A (en) | A kind of sintering magnetic composite and preparation method thereof | |
| CN102568729B (en) | Method for preparing bulk composite nanocrystalline rare earth permanent magnetic material | |
| CN108389676A (en) | A kind of temperature tolerance permanent-magnet material and preparation method thereof | |
| CN108962528A (en) | A kind of magnetic material and preparation method thereof with high-temperature stability | |
| CN103794354A (en) | Preparation method of neodymium iron boron sintered magnet | |
| CN105869816A (en) | Mischmetal-mixed neodymium iron boron hot-pressed and hot-deformed magnet and manufacturing method thereof | |
| CN108517455B (en) | Nanocrystalline rare earth permanent magnetic material with double-main-phase structure and preparation method thereof | |
| CN102360702A (en) | Simple and convenient functional magnetic material block and preparation method thereof | |
| CN103632835A (en) | Rapid forming method of high-performance Nd-Fe-B magnetic body | |
| CN112216460B (en) | Nanocrystalline neodymium-iron-boron magnet and preparation method thereof | |
| CN103794355B (en) | A kind of preparation method of the neodymium iron boron magnetic body with high-Curie-point | |
| CN103000324A (en) | Sintered rare earth permanent magnetic material and preparation method thereof | |
| CN105006327A (en) | High-performance Gd containing cast sheet magnet and preparation method thereof | |
| CN108806910A (en) | Improve the coercitive method of neodymium-iron-boron magnetic material | |
| CN103632834A (en) | Preparation method of high-performance anisotropic Nd-Fe-B magnetic body | |
| CN103824669B (en) | A kind of μ 90 iron tantnickel powder core material and preparation method thereof | |
| CN103779065B (en) | A kind of preparation method of rare earth permanent magnet magnet ring | |
| CN105913989B (en) | High remanent magnetism material and preparation method | |
| CN105070448A (en) | High-performance cerium-containing cast sheet magnet and preparation method thereof | |
| CN105070447A (en) | High-performance holmium-containing cast sheet magnet and preparation method thereof | |
| CN109326404A (en) | A kind of neodymium-iron-boron magnetic material and preparation method | |
| CN103489556B (en) | Hemimorphic square loop sintered ferrite rotor magnetite and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C41 | Transfer of patent application or patent right or utility model | ||
| CB03 | Change of inventor or designer information |
Inventor after: Ying Zhongliang Inventor before: Liu Yang |
|
| COR | Change of bibliographic data | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20160422 Address after: 321016 No. 589 Longtan Road, autumn street, Wucheng District, Zhejiang, Jinhua Applicant after: ZHEJIANG ACTIVETECH COMPUTER TECHNOLOGY Co.,Ltd. Address before: 518000 Guangdong Province, Shenzhen city Longgang District cloth Road Park four building 12 unit 1805 A Applicant before: Liu Yang |
|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20240819 Address after: Building 6, No. 888 Jinde Road, Jiangdong Town, Jindong District, Jinhua City, Zhejiang Province 321042 Patentee after: Zhejiang Huachuang New Energy Commercial Vehicle Co.,Ltd. Country or region after: China Address before: No. 589 Longtan Road, Qiubin Street, Wucheng District, Jinhua City, Zhejiang Province, 321016 Patentee before: ZHEJIANG ACTIVETECH COMPUTER TECHNOLOGY Co.,Ltd. Country or region before: China |
|
| TR01 | Transfer of patent right |