CN103794355A - Method for preparing neodymium iron boron magnet with high Curie point - Google Patents
Method for preparing neodymium iron boron magnet with high Curie point Download PDFInfo
- Publication number
- CN103794355A CN103794355A CN201410064216.4A CN201410064216A CN103794355A CN 103794355 A CN103794355 A CN 103794355A CN 201410064216 A CN201410064216 A CN 201410064216A CN 103794355 A CN103794355 A CN 103794355A
- Authority
- CN
- China
- Prior art keywords
- magnet
- under
- magnetic
- sintering
- melt
- 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.)
- Granted
Links
- 229910001172 neodymium magnet Inorganic materials 0.000 title claims abstract description 12
- 238000000034 method Methods 0.000 title claims abstract description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000000843 powder Substances 0.000 claims abstract description 17
- 238000005245 sintering Methods 0.000 claims abstract description 16
- 229910052742 iron Inorganic materials 0.000 claims abstract description 10
- 229910052779 Neodymium Inorganic materials 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
- 229910045601 alloy Inorganic materials 0.000 claims description 13
- 239000000956 alloy Substances 0.000 claims description 13
- 229910052802 copper Inorganic materials 0.000 claims description 13
- 239000010949 copper Substances 0.000 claims description 13
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 12
- 239000003708 ampul Substances 0.000 claims description 12
- 238000005266 casting Methods 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 12
- 230000005684 electric field Effects 0.000 claims description 12
- 239000001257 hydrogen Substances 0.000 claims description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims description 12
- 238000002844 melting Methods 0.000 claims description 12
- 230000008018 melting Effects 0.000 claims description 12
- 238000012545 processing Methods 0.000 claims description 12
- 239000010453 quartz Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 239000007789 gas Substances 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- 229910000640 Fe alloy Inorganic materials 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 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
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 claims description 7
- 229910001021 Ferroalloy Inorganic materials 0.000 claims description 6
- 230000006698 induction Effects 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
- 239000000696 magnetic material Substances 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 5
- 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
- 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
- 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
- 239000000155 melt Substances 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
- 238000010791 quenching Methods 0.000 claims description 4
- 230000000171 quenching effect Effects 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
- 238000005507 spraying Methods 0.000 claims description 4
- 239000000463 material Substances 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 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
- 229910052804 chromium Inorganic materials 0.000 abstract description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 abstract 1
- 239000011651 chromium Substances 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 5
- 229910052772 Samarium Inorganic materials 0.000 description 4
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 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
- 238000000465 moulding Methods 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
- 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
- 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
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 230000005389 magnetism Effects 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
- 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
- 238000002156 mixing Methods 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 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 invention relates to a method for preparing a neodymium iron boron magnet with a high Curie point. The atom molecular formula of magnet permanent materials adopted in the magnet is as follows: (LawYxNd1-w-x) a (Fel-y-zMnyCrz) 100-a-b-c Bb Fc, 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, and c=0.3-0.5. The method includes the steps of permanent magnet powder manufacturing, blank manufacturing, sintering and surface treatment. According to the magnet prepared through the method, neodymium is replaced by adding lanthanum and yttrium, so the cost is lowered; the Curie point of the materials is improved by adding chromium and iron, and finally the coercivity of the magnet is further improved through surface treatment. Thus, the magnet is more suitable for being used at high-temperature environments.
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.The challenge of environmental problem recently has made the range of application of these magnets expand to industrial equipment, electric automobile and wind-driven generator from household electrical appliance.Require further to improve the performance of Nd-Fe-B magnet.
But the Curie temperature of Nd-Fe-B permanent magnetic material is not high, generally, below 130 ℃, magnetic flux density is not high simultaneously, because this two classes magnetic material exists defect and causes coercive force not high in crystallization process.Existing prior art proposes, and take existing neodymium iron boron magnetic body as matrix, adds some auxiliary elements and improve Curie temperature and the coercive force of neodymium iron boron magnetic body.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, and price is improving constantly.
In this case, what should consider is the use amount that how can reduce counterweight rare-earth-type material, realizes under the prerequisite that can meet performance, reduces 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, the magnet that uses the method to prepare still has good magnetic property under high-temperature work environment.
To achieve these goals, the preparation method of a kind of neodymium iron boron magnetic body with high-Curie-point provided by the invention, this magnet adopts the permanent magnetic material of following atom and molecule formula: (La
wy
xnd
1-w-x)
a(Fe
1-y-zmn
ycr
z)
100-a-b-cb
bf
c, 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 being mixed, raw material after taking in entering vacuum electromagnetic induction furnace, melts under argon gas atmosphere, concrete fusion process is as follows: carry out vacuum melting take neodymium and iron atom ratio as the mode of 1: 2, then add yttrium iron alloy, lanthanum ferroalloy, manganeisen, ferrochrome, ferric flouride and borax to melt again by composition, finally add the iron of the surplus of calculating by proportioning, ingot casting after melting;
Bottom being put into, opens on ingot casting the quartz glass tube of aperture; and be placed in the vacuum spray to cast stove with impulse electric field and pulsed magnetic field apparatus; water cooled copper mould is placed in lower end at quartz ampoule; ingot casting induction melting under high-purity argon gas protection becomes liquid; then electrode is inserted in melt; apply impulse electric field, carry 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/cm
2, pulse duration 10-50 μ s, processing time 35-50s, with after-applied pulsed magnetic field, the magnetic line of force, through copper mold cavity, is then opened the air valve being connected with quartz ampoule, melt injects fast copper mold cavity by the aperture of quartz ampoule bottom under the effect of spraying air pressure, the cold rapid-hardening flake that makes of speed;
Above-mentioned rapid-hardening flake band, after adding the reactor of hydrogen crushing furnace to vacuumize, is poured to hydrogen and carries out the broken dehydrogenation processing of hydrogen and be 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/cm
2pressure by this fine powder compacting, under the magnetic field of 16-19kOe, be orientated simultaneously, make blank;
(3) sintering
Molded blank is put under argon shield to sintering furnace and carried out sintering, be first warming up to 640-660 ℃ with 5-10 ℃/min, insulation 3-4h, is then warming up to 1000-1060 ℃ of sintering 4-5h with 10-15 ℃/min, after double tempering, is 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 Dy
42co
56powder and average grain diameter are the Tb of 1 μ m
4o
7ratio with weight ratio 1: 1-2 is mixed, this mixture of powders is combined with deionized water with weight fraction 30-40% and forms slurry, under the condition of ultrasonic agitation, above-mentioned magnet body is immersed to 15-20 second, magnet body is taken out, and use immediately heated air drying, then at 850-890 ℃, in argon atmospher, carry out DIFFUSION TREATMENT 5-7h, rear quenching, obtains product.
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 coercive force of magnet by surface treatment, make magnet of the present invention be more suitable for using for hot environment.
Embodiment
Embodiment mono-
This magnet of the present embodiment adopts the permanent magnetic material of following atom and molecule formula: (La
0.12y
0.25nd
0.37)
26(Fe
0.81mn
0.12cr
0.07)
69.4b
4.5f
0.3.
Take raw material by proportioning, after being mixed, raw material after taking in entering vacuum electromagnetic induction furnace, melts under argon gas atmosphere, concrete fusion process is as follows: carry out vacuum melting take neodymium and iron atom ratio as the mode of 1: 2, then add yttrium iron alloy, lanthanum ferroalloy, manganeisen, ferrochrome, ferric flouride and borax to melt again by composition, finally add the iron of the surplus of calculating by proportioning, ingot casting after melting.
Bottom being put into, opens on ingot casting the quartz glass tube of aperture; and be placed in the vacuum spray to cast stove with impulse electric field and pulsed magnetic field apparatus; water cooled copper mould is placed in lower end at quartz ampoule; ingot casting induction melting under high-purity argon gas protection becomes liquid; then electrode is inserted in melt; apply impulse electric field, carry out electro-pulse modification processing.When alloy melt electro-pulse modification is processed, the impulse electric field parameter of employing is: pulse frequency 1000Hz, pulse current peak density 240A/cm
2, pulse duration 10 μ s, processing time 50s, with after-applied pulsed magnetic field, the magnetic line of force, through copper mold cavity, is then opened the air valve being connected with quartz ampoule, melt injects fast copper mold cavity by the aperture of quartz ampoule bottom under the effect of spraying air pressure, the cold rapid-hardening flake that makes of speed.
Above-mentioned rapid-hardening flake band, after adding the reactor of hydrogen crushing furnace to vacuumize, is poured to hydrogen and carries out the broken dehydrogenation processing of hydrogen and be cooled to after room temperature, take out and be placed in airflow milling, make the magnetic that particle diameter is 10-20 μ m.
In argon shield atmosphere, in argon atmospher, with 1.5 tons/cm
2pressure by this fine powder compacting, under the magnetic field of 16-19kOe, be orientated simultaneously, make blank.
Molded blank is put under argon shield to sintering furnace and carried out sintering, be first warming up to 640 ℃ with 5 ℃/min, insulation 4h, is then warming up to 1000 ℃ of sintering 5h with 10 ℃/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 Dy
42co
56powder and average grain diameter are the Tb of 1 μ m
4o
7mix with the weight ratio ratio of 1: 1, this mixture of powders is combined with deionized water with weight fraction 30% and forms slurry, under the condition of ultrasonic agitation, above-mentioned magnet body is immersed to 15 seconds, magnet body is taken out, and use immediately heated air drying, then at 850 ℃, in argon atmospher, carry out DIFFUSION TREATMENT 7h, rear quenching, obtains product.
Embodiment bis-
This magnet of the present embodiment adopts the permanent magnetic material of following atom and molecule formula: (La
0.14y
0.32nd
0.54)
28(Fe
0.64mn
0.27cr
0.09)
65.9b
5.6f
0.5, 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 being mixed, raw material after taking in entering vacuum electromagnetic induction furnace, melts under argon gas atmosphere, concrete fusion process is as follows: carry out vacuum melting take neodymium and iron atom ratio as the mode of 1: 2, then add yttrium iron alloy, lanthanum ferroalloy, manganeisen, ferrochrome, ferric flouride and borax to melt again by composition, finally add the iron of the surplus of calculating by proportioning, ingot casting after melting.
Bottom being put into, opens on ingot casting the quartz glass tube of aperture; and be placed in the vacuum spray to cast stove with impulse electric field and pulsed magnetic field apparatus; water cooled copper mould is placed in lower end at quartz ampoule; ingot casting induction melting under high-purity argon gas protection becomes liquid; then electrode is inserted in melt; apply impulse electric field, carry out electro-pulse modification processing.When alloy melt electro-pulse modification is processed, the impulse electric field parameter of employing is: pulse frequency 1500Hz, pulse current peak density 350A/cm
2, pulse duration 50 μ s, processing time 35s, with after-applied pulsed magnetic field, the magnetic line of force, through copper mold cavity, is then opened the air valve being connected with quartz ampoule, melt injects fast copper mold cavity by the aperture of quartz ampoule bottom under the effect of spraying air pressure, the cold rapid-hardening flake that makes of speed.
Above-mentioned rapid-hardening flake band, after adding the reactor of hydrogen crushing furnace to vacuumize, is poured to hydrogen and carries out the broken dehydrogenation processing of hydrogen and be cooled to after room temperature, take out and be placed in airflow milling, make the magnetic that particle diameter is 10-20 μ m.
In argon shield atmosphere, in argon atmospher, with 2 tons/cm
2pressure by this fine powder compacting, under the magnetic field of 19kOe, be orientated simultaneously, make blank.
Molded blank is put under argon shield to sintering furnace and carried out sintering, be first warming up to 660 ℃ with 10 ℃/min, insulation 3h, is then warming up to 1060 ℃ of sintering 4h with 15 ℃/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 Dy
42co
56powder and average grain diameter are the Tb of 1 μ m
4o
7mix with the weight ratio ratio of 1: 2, this mixture of powders is combined with deionized water with weight fraction 40% and forms slurry, under the condition of ultrasonic agitation, above-mentioned magnet body is immersed to 20 seconds, magnet body is taken out, and use immediately heated air drying, then at 890 ℃, in argon atmospher, carry out DIFFUSION TREATMENT 5h, rear quenching, 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 wherein in yttrium iron alloy yttrium to account for weight percentage be 10%.To in feed metal induction furnace, melt, after fusing 1550 ℃ of refinings 30 minutes, the then cooling alloy pig that is cast into constant weight and shape.Subsequently, alloy pig is joined in spun furnace, induction heating remelting in the spun furnace under inert atmosphere (as argon gas) protection at the temperature of 1350 ℃～1450 ℃, obtains alloy molten solution.This alloy molten solution is solidified to water-cooled copper roller or the molybdenum roller surface moment of High Rotation Speed through the small hole injection of crucible bottom nozzle, and cooling rate can reach 104～106K/s, forms 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, under 600 ℃～700 ℃ conditions, heat treatment 10 minutes, can obtain final magnetic.Utilize Magnetic field press, by in powder oriented moulding under the magnetic field of 1.7T of mixing, pass through again isostatic cool pressing, moulding pressed compact is placed in to vacuum sintering furnace, 1075 ℃ of sintered heat insulatings 3 hours, 890 ℃ of one-level tempering insulations 2 hours, 560 ℃ of second annealing insulations 3 hours, obtain sintered magnet.
Embodiment 1-2 to same shape and size and the permanent-magnet of comparative example carry out magnetism testing, and test condition is: condition 1: under the indoor environment that temperature is 25 ℃, test; Condition 2: it is to test after 100h under the environment of 60 ℃ that magnet is placed in to temperature, measures maximum magnetic energy product (BH)
maxand coercive force.Test result shows: the maximum magnetic energy product relative conditon 1 in condition 2 of the embodiment 1-2 10-15% that only declines, and the coercive force 9-12% that only declines, and comparative example declines at the maximum magnetic energy product relative conditon 1 of condition 2 and exceedes 26%, coercive force only declines and exceedes 22%.
Claims (1)
1. have a preparation method for the neodymium iron boron magnetic body of high-Curie-point, this magnet adopts the permanent magnetic material of following atom and molecule formula: (La
wy
xnd
1-w-x)
a(Fe
1-y-zmn
ycr
z)
100-a-b-cb
bf
c, 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 being mixed, raw material after taking in entering vacuum electromagnetic induction furnace, melts under argon gas atmosphere, concrete fusion process is as follows: carry out vacuum melting take neodymium and iron atom ratio as the mode of 1: 2, then add yttrium iron alloy, lanthanum ferroalloy, manganeisen, ferrochrome, ferric flouride and borax to melt again by composition, finally add the iron of the surplus of calculating by proportioning, ingot casting after melting;
Bottom being put into, opens on ingot casting the quartz glass tube of aperture; and be placed in the vacuum spray to cast stove with impulse electric field and pulsed magnetic field apparatus; water cooled copper mould is placed in lower end at quartz ampoule; ingot casting induction melting under high-purity argon gas protection becomes liquid; then electrode is inserted in melt; apply impulse electric field, carry 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/cm
2, pulse duration 10-50 μ s, processing time 35-50s, with after-applied pulsed magnetic field, the magnetic line of force, through copper mold cavity, is then opened the air valve being connected with quartz ampoule, melt injects fast copper mold cavity by the aperture of quartz ampoule bottom under the effect of spraying air pressure, the cold rapid-hardening flake that makes of speed;
Above-mentioned rapid-hardening flake band, after adding the reactor of hydrogen crushing furnace to vacuumize, is poured to hydrogen and carries out the broken dehydrogenation processing of hydrogen and be 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/cm
2pressure by this fine powder compacting, under the magnetic field of 16-19kOe, be orientated simultaneously, make blank;
(3) sintering
Molded blank is put under argon shield to sintering furnace and carried out sintering, be first warming up to 640-660 ℃ with 5-10 ℃/min, insulation 3-4h, is then warming up to 1000-1060 ℃ of sintering 4-5h with 10-15 ℃/min, after double tempering, is 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 Dy
42co
56powder and average grain diameter are the Tb of 1 μ m
4o
7ratio with weight ratio 1: 1-2 is mixed, this mixture of powders is combined with deionized water with weight fraction 30-40% and forms slurry, under the condition of ultrasonic agitation, above-mentioned magnet body is immersed to 15-20 second, magnet body is taken out, and use immediately heated air drying, then at 850-890 ℃, 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 true CN103794355A (en) | 2014-05-14 |
| CN103794355B 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) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111243805A (en) * | 2018-11-29 | 2020-06-05 | 丰田自动车株式会社 | Rare earth magnet and method for producing same |
| 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 (5)
| 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 |
| 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 |
-
2014
- 2014-02-25 CN CN201410064216.4A patent/CN103794355B/en active Active
Patent Citations (5)
| 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 |
| 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 |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111243805A (en) * | 2018-11-29 | 2020-06-05 | 丰田自动车株式会社 | Rare earth magnet and method for producing same |
| CN111243805B (en) * | 2018-11-29 | 2022-02-25 | 丰田自动车株式会社 | Rare earth magnet and method for producing same |
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103794355B (en) | 2016-05-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP7220301B2 (en) | Neodymium-iron-boron magnet material, raw material composition, manufacturing method, and application | |
| 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 | |
| CN108335819A (en) | A kind of sintering magnetic composite and preparation method thereof | |
| CN102969112B (en) | Rare earth permanent magnet powder and preparation method thereof and magnet prepared therefrom and magnetic device | |
| CN103014477B (en) | Method for smelting iron-based nanocrystalline master alloy | |
| CN108389676A (en) | A kind of temperature tolerance permanent-magnet material and preparation method thereof | |
| CN103545079A (en) | Double-principal-phase yttrium-contained permanent magnet and preparing method of double-principal-phase yttrium-contained permanent magnet | |
| CN108962528A (en) | A kind of magnetic material and preparation method thereof with high-temperature stability | |
| CN102568729B (en) | Method for preparing bulk composite nanocrystalline rare earth permanent magnetic material | |
| CN103794354A (en) | Preparation method of neodymium iron boron sintered magnet | |
| CN104851543A (en) | Preparing method of anticorrosion samarium cobalt-based permanent magnet material | |
| CN104599802A (en) | Rare earth permanent magnetic material and preparation method thereof | |
| CN103632835A (en) | Rapid forming method of high-performance Nd-Fe-B magnetic body | |
| CN105006327A (en) | High-performance Gd containing cast sheet magnet and preparation method thereof | |
| CN103000324A (en) | Sintered rare earth permanent magnetic material and preparation method thereof | |
| CN104846255B (en) | A kind of preparation method of yttrium iron based permanent magnetic material | |
| CN103794355B (en) | A kind of preparation method of the neodymium iron boron magnetic body with high-Curie-point | |
| CN103824669B (en) | A kind of μ 90 iron tantnickel powder core material and preparation method thereof | |
| CN108806910A (en) | Improve the coercitive method of neodymium-iron-boron magnetic material | |
| CN109326404A (en) | A kind of neodymium-iron-boron magnetic material and preparation method | |
| CN105913989B (en) | High remanent magnetism material and preparation method | |
| KR102589893B1 (en) | Method for preparing sintered magnet and sintered magnet | |
| CN103489556B (en) | Hemimorphic square loop sintered ferrite rotor magnetite and preparation method thereof | |
| KR102399418B1 (en) | Manufacturing method of sintered magnetic and sintered magnetic manufactured by the same |
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 |