CN105070446A - High-performance cerium-neodymium-praseodymium cast sheet magnet and preparation method thereof - Google Patents
High-performance cerium-neodymium-praseodymium cast sheet magnet and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-performance cerium-neodymium-praseodymium cast sheet magnet and a preparation method thereof. The cast sheet magnet comprises, by weight, 4.0-5.0% of Pr, 17.0-19.0% of Nd, 6.5-7.5% of Ce, 0.8-1.2% of Gd, 0.9-1.3% of Ho, 0.95-1.05% of B, 0.5-1.0% of Al, 0.15-0.2% of Cu, 0.20-0.40% of Co and the balance Fe for supplement. The preparation method comprises the steps of cast sheet smelting, hydrogen decrepitation, air-current mill smashing, magnetic field orientation forming, isostatic pressing and sintering. According to the high-performance cerium-neodymium-praseodymium cast sheet magnet and the preparation method thereof, on one hand, the neodymium using amount is reduced, but it still can be guaranteed that the magnet has the excellent magnetism, and the neodymium resources are protected; on the other hand, no alpha-Fe crystal exists in cast sheet tissue due to the cast sheet smelting technology, cast sheets are broken more easily, and the production cycle is shortened.
Description
Technical field
The invention belongs to permanent magnetic material technical field, be specifically related to a kind of high-performance containing neodymium cerium praseodymium slab magnet and preparation method thereof.
Background technology
Nd-Fe-B rare earth permanent magnetic material, is the permanent magnetic material that the magnetic property that finds up to now is the strongest, and is more and more applied with its excellent magnetic property, be widely used in medical Magnetic resonance imaging, computer hard disc driver, sound equipment, mobile phone etc.; Along with energy-conservation and requirement that is low-carbon economy, Nd-Fe-B rare earth permanent magnetic material starts again at auto parts and components, household electrical appliance, energy-conservation and control motor, hybrid vehicle, and the field such as wind power generation, Aero-Space is applied, and causes its consumption increasing.
At present, China's neodymium iron boron output accounts for more than 60% of the whole world, estimate that its range of application following and the market demand will continuous enlargement, neodymium iron boron industry strengthens the demand of rare earth element nd, and annual about with the rise of the speed of amplification 20%, the permanent magnet of new generation seeking Nd requirement less is extremely urgent.
The manufacturing process of now conventional sintered Nd-Fe-B permanent magnet generally comprises: raw material preparation → ingot casting melting → broken powder process → die mould → sintering → timeliness → detection.Wherein in ingot casting melting step, the quality of slab tissue not only has impact to follow-up powder process, orientation, sintering process, and also has extreme influence to powder properties and final sintering magnetic property.Do not have excellent slab tissue, just can not produce high performance sintered permanent magnet, slab tissue is one of key technology of restriction magnet performance, and whether excellent slab tissue depend on the alloy composition of permanent magnet and content and ingot casting thickness to a great extent.At present, ingot casting thickness prepared by ingot casting smelting technology mostly is about 20mm, easily has α-Fe dendrite to separate out, because the plasticity of α-Fe dendrite is better, make ingot casting be difficult to fragmentation, bring inconvenience to follow-up pulverizing process, also need to extend sintering time to obtain uniform Nd2Fe14B crystal.
The reserves of occurring in nature cerium, holmium, cobalt element are far more than Nd element, and rare earth metal cerium, holmium, cobalt are lower than the rare earth metal Nd-Pr alloy market price, and thus CeHoCoFeB permanent-magnet alloy has obvious price advantage compared with (Pr, Nd) FeB permanent-magnet alloy.
Summary of the invention
The object of the present invention is to provide a kind of high-performance containing neodymium cerium praseodymium slab magnet and preparation method thereof; this magnet and preparation method thereof; decrease the use of neodymium on the one hand; and add cerium, holmium, cobalt composition; still can ensure that permanent magnet has excellent magnetic; thus saved cost, protect neodium resource.Slab smelting technology makes slab tissue not have α-Fe crystal on the other hand, and slab fragmentation is easier, and follow-up powder process is also easier, thus has saved manpower and materials, shortens the production cycle.
Technical scheme of the present invention is: a kind of high-performance is containing neodymium cerium praseodymium slab magnet and preparation method thereof, and the described component containing neodymium cerium praseodymium slab magnet and weight percentage are Pr:4.0 ~ 5.0%, Nd:17.0 ~ 19.0%, Ce:6.5 ~ 7.5%, Gd:0.8 ~ 1.2%, Ho:0.9 ~ 1.3%, B:0.95 ~ 1.05%, Al:0.5 ~ 1.0%, Cu:0.15 ~ 0.20%, Co:0.20 ~ 0.40%, surplus Fe supplement;
The component and the weight percentage that also preferably contain neodymium cerium praseodymium slab magnet are:
Pr:4.5%, Nd:18.0%, Ce:7.0%, Gd:1.0%, Ho:1.1%, B:1.00%, Al:0.8%, Cu:0.18%, Co:0.30%, surplus Fe supplements;
Prepare this preparation method containing neodymium cerium praseodymium slab magnet to comprise the following steps:
1) slab melting: the raw metal of proportioning is in proportion dropped into vacuum induction rapid hardening slab stove, vacuumize, melting at 800 ~ 1000 DEG C, be heated to metal Pr when starting to melt, be filled with high-purity argon gas, through ultrasonic mixing after raw metal melts, when after the conjunctiva of alloy molten solution surface, be poured on the water-cooled copper rod of rotation, through being cooled to the slab that thickness is 0.25 ~ 0.35mm fast;
2) hydrogen is pulverized: by step 1) slab that obtains drops into hydrogen crushing furnace, and dehydrogenation at 450 ~ 560 DEG C, obtains the alloying pellet of 100 ~ 110 μm;
3) airflow milling is pulverized: by step 2) alloying pellet that obtains adds in airflow milling under nitrogen protection, is ground into the alloy powder of 3.4 ~ 4.4 μm through airflow milling;
4) magnetic field orientating is shaping: by step 3) alloy powder that obtains drops into Magnetic field press, and oriented moulding under the magnetic field of 1.9T, obtains pressed compact;
5) isostatic pressed: will through step 4) shaping after pressed compact, reinstall in the high pressure chest of isostatic pressing machine, under the pressure of 190-200MPa, keep 10-20s;
6) sinter: will through step 5) pressed compact drop in vacuum sintering furnace, vacuumize, at 1080 ~ 1150 DEG C, constant temperature 2.5 ~ 3.5 hours; One-level temperature is 880 ~ 1000 DEG C, constant temperature 1.5 ~ 2.5 hours; Second annealing temperature is 500 ~ 600 DEG C, constant temperature 2.5 ~ 4.5 hours; Finally obtain sintered magnet.
7) detect: the magnetic parameter of test products.
Adopt alloy component of the present invention to be raw material, adopt this slab smelting technology, excellent slab tissue can be obtained, slab thickness is 0.25 ~ 0.35mm, the appearance of α-Fe crystal can be suppressed completely, be conducive to the carrying out of follow-up powder process, orientation, sintering, and high performance permanent magnet can be obtained.
Described step 1) in, raw metal also can mix through electromagnetic agitation after melting.
Described step 6) in sintering temperature be 1120 DEG C, constant temperature 3 hours; One-level temperature is 920 DEG C, constant temperature 2 hours; Second annealing temperature is 550 DEG C, constant temperature 3 hours.
Beneficial effect of the present invention is:
(1) decrease the use of neodymium, be only 17.0 ~ 19.0%, and.By cerium, holmium, the cobalt composition of suitable dose of adulterating, still can ensure that permanent magnet has excellent magnetic, thus save cost, protect neodium resource.
(2) slab smelting technology makes slab tissue not have α-Fe crystal, and slab fragmentation is easier, and follow-up powder process is also easier, thus has saved manpower and materials, shortens the production cycle.
Embodiment
Embodiment 1
Get and containing the component of neodymium cerium praseodymium slab magnet and weight percentage be: Pr:4.0 ~ 5.0%, Nd:17.0 ~ 19.0%, Ce:6.5 ~ 7.5%, Gd:0.8 ~ 1.2%, Ho:0.9 ~ 1.3%, B:0.95 ~ 1.05%, Al:0.5 ~ 1.0%, Cu:0.15 ~ 0.2%, Co:0.20 ~ 0.40%, surplus Fe supplement;
Prepare this preparation method containing neodymium cerium praseodymium slab magnet to comprise the following steps:
1) slab melting: the raw metal of proportioning is in proportion dropped into vacuum induction rapid hardening slab stove, vacuumize, melting at 800 ~ 1000 DEG C, be heated to metal Pr when starting to melt, be filled with high-purity argon gas, through ultrasonic mixing after raw metal melts, when after the conjunctiva of alloy molten solution surface, be poured on the water-cooled copper rod of rotation, through being cooled to the slab that thickness is 0.25 ~ 0.35mm fast;
2) hydrogen is pulverized: by step 1) slab that obtains drops into hydrogen crushing furnace, and dehydrogenation at 450 ~ 560 DEG C, obtains the alloying pellet of 100 ~ 110 μm;
3) airflow milling is pulverized: by step 2) alloying pellet that obtains adds in airflow milling under nitrogen protection, is ground into the alloy powder of 3.4 ~ 4.4 μm through airflow milling;
4) magnetic field orientating is shaping: by step 3) alloy powder that obtains drops into Magnetic field press, and oriented moulding under the magnetic field of 1.9T, obtains pressed compact;
5) isostatic pressed: will through step 4) shaping after pressed compact, reinstall in the high pressure chest of isostatic pressing machine, under the pressure of 190-200MPa, keep 10-20s;
6) sinter: will through step 5) pressed compact drop in vacuum sintering furnace, vacuumize, at 1080 ~ 1150 DEG C, constant temperature 2.5 ~ 3.5 hours; One-level temperature is 880 ~ 1000 DEG C, constant temperature 1.5 ~ 2.5 hours; Second annealing temperature is 500 ~ 600 DEG C, constant temperature 2.5 ~ 4.5 hours; Finally obtain sintered magnet;
7) detect: the magnetic parameter of test products.
After testing, its key technical indexes reaches following parameter:
Remanent magnetism (Br) 1.17 ~ 1.22T
Magnetic induction coercive force (Hcb) >=860Ka/m
HCJ (Hcj) >=955Ka/m
Maximum magnetic energy product (BH) max:264 ~ 288KJ/m
3
Embodiment 2
Get and containing the component of neodymium cerium praseodymium slab magnet and weight percentage be:
Pr:4.5%, Nd:18%, Ce:7%, Gd:1.0%, Ho:1.1%, B:1.0%, Al:0.8%, Cu:0.18%, Co:0.3%, surplus Fe supplements;
Prepare this preparation method containing neodymium cerium praseodymium slab magnet to comprise the following steps:
1) slab melting: the raw metal of proportioning is in proportion dropped into vacuum induction rapid hardening slab stove, vacuumize, melting at 800 ~ 1000 DEG C, be heated to metal Pr when starting to melt, be filled with high-purity argon gas, through ultrasonic mixing after raw metal melts, when after the conjunctiva of alloy molten solution surface, be poured on the water-cooled copper rod of rotation, through being cooled to the slab that thickness is 0.25 ~ 0.35mm fast;
2) hydrogen is pulverized: by step 1) slab that obtains drops into hydrogen crushing furnace, and dehydrogenation at 450 ~ 560 DEG C, obtains the alloying pellet of 100 ~ 110 μm;
3) airflow milling is pulverized: by step 2) alloying pellet that obtains adds in airflow milling under nitrogen protection, is ground into the alloy powder of 3.4 ~ 4.4 μm through airflow milling;
4) magnetic field orientating is shaping: by step 3) alloy powder that obtains drops into Magnetic field press, and oriented moulding under the magnetic field of 1.9T, obtains pressed compact;
5) isostatic pressed: will through step 4) shaping after pressed compact, reinstall in the high pressure chest of isostatic pressing machine, under the pressure of 190-200MPa, keep 10-20s;
6) sinter: will through step 5) pressed compact drop in vacuum sintering furnace, vacuumize, at 1120 DEG C, constant temperature 3 hours; One-level temperature is 920 DEG C, constant temperature 2 hours; Second annealing temperature is 550 DEG C, constant temperature 3 hours; Finally obtain sintered magnet;
7) detect: the magnetic parameter of test products.
After testing, its key technical indexes reaches following parameter:
Remanent magnetism (Br) 1.22 ~ 1.27T
Magnetic induction coercive force (Hcb) >=900Ka/m
HCJ (Hcj) >=955Ka/m
Maximum magnetic energy product (BH) max:288 ~ 312KJ/m
3
Embodiment 3
Get and containing the component of neodymium cerium praseodymium slab magnet and weight percentage be:
Pr:4.0%, Nd:17.0%, Ce:7.5%, Gd:1.2%, Ho:0.9%, B:1.05%, Al:0.5%, Cu:0.15%, Co:0.40%, surplus Fe supplements;
Prepare this preparation method containing neodymium cerium praseodymium slab magnet to comprise the following steps:
1) slab melting: the raw metal of proportioning is in proportion dropped into vacuum induction rapid hardening slab stove, vacuumize, melting at 850 ~ 1050 DEG C, be heated to metal Pr when starting to melt, be filled with high-purity argon gas, through electromagnetic agitation mixing after raw metal melts, when after the conjunctiva of alloy molten solution surface, be poured on the water-cooled copper rod of rotation, through being cooled to the slab that thickness is 0.25 ~ 0.35mm fast;
2) hydrogen is pulverized: by step 1) slab that obtains drops into hydrogen crushing furnace, and dehydrogenation at 450 ~ 560 DEG C, obtains the alloying pellet of 100 ~ 110 μm;
3) airflow milling is pulverized: by step 2) alloying pellet that obtains adds in airflow milling under nitrogen protection, is ground into the alloy powder of 3.4 ~ 4.4 μm through airflow milling;
4) magnetic field orientating is shaping: by step 3) alloy powder that obtains drops into Magnetic field press, and oriented moulding under the magnetic field of 1.9T, obtains pressed compact;
5) isostatic pressed: will through step 4) shaping after pressed compact, reinstall in the high pressure chest of isostatic pressing machine, under the pressure of 190-200MPa, keep 10-20s;
6) sinter: will through step 5) pressed compact drop in vacuum sintering furnace, vacuumize, at 1080 DEG C, constant temperature 3 hours; One-level temperature is 880 DEG C, constant temperature 2 hours; Second annealing temperature is 600 DEG C, constant temperature 3 hours; Finally obtain sintered magnet;
7) detect: the magnetic parameter of test products.
After testing, its key technical indexes reaches following parameter:
Remanent magnetism (Br) 1.22 ~ 1.27T
Magnetic induction coercive force (Hcb) >=900Ka/m
HCJ (Hcj) >=955Ka/m
Maximum magnetic energy product (BH) max:288 ~ 312KJ/m
3
Embodiment 4
Get and containing the component of neodymium cerium praseodymium slab magnet and weight percentage be:
Pr:5.0%, Nd:19.0%, Ce:6.5%, Gd:0.8%, Ho:0.9%, B:1.05%, Al:0.5%, Cu:0.2%, Co:0.20%, surplus Fe supplements;
Prepare this preparation method containing neodymium cerium praseodymium slab magnet to comprise the following steps:
1) slab melting: the raw metal of proportioning is in proportion dropped into vacuum induction rapid hardening slab stove, vacuumize, melting at 1000 DEG C, be heated to metal Pr when starting to melt, be filled with high-purity argon gas, through ultrasonic mixing after raw metal melts, when after the conjunctiva of alloy molten solution surface, be poured on the water-cooled copper rod of rotation, through being cooled to the slab that thickness is 0.25 ~ 0.35mm fast;
2) hydrogen is pulverized: by step 1) slab that obtains drops into hydrogen crushing furnace, and dehydrogenation at 560 DEG C, obtains the alloying pellet of 100 ~ 110 μm;
3) airflow milling is pulverized: by step 2) alloying pellet that obtains adds in airflow milling under nitrogen protection, is ground into the alloy powder of 3.4 ~ 4.4 μm through airflow milling;
4) magnetic field orientating is shaping: by step 3) alloy powder that obtains drops into Magnetic field press, and oriented moulding under the magnetic field of 1.9T, obtains pressed compact;
5) isostatic pressed: will through step 4) shaping after pressed compact, reinstall in the high pressure chest of isostatic pressing machine, under the pressure of 190-200MPa, keep 10-20s;
6) sinter: will through step 5) pressed compact drop in vacuum sintering furnace, vacuumize, at 1150 DEG C, constant temperature 2.5 hours; One-level temperature is 880 DEG C, constant temperature 2.5 hours; Second annealing temperature is 600 DEG C, constant temperature 4.5 hours; Finally obtain sintered magnet;
7) detect: the magnetic parameter of test products.
After testing, its key technical indexes reaches following parameter:
Remanent magnetism (Br) 1.22 ~ 1.27T
Magnetic induction coercive force (Hcb) >=900Ka/m
HCJ (Hcj) >=955Ka/m
Maximum magnetic energy product (BH) max:288 ~ 312KJ/m
3
Embodiment 5
Get and containing the component of neodymium cerium praseodymium slab magnet and weight percentage be: Pr:4.0%, Nd:19.0%, Ce:6.5%, Gd:1.2%, Ho:0.9%, B:1.05%, Al:0.5%, Cu:0.15%, Co:0.40%, surplus Fe supplement;
Prepare this preparation method containing neodymium cerium praseodymium slab magnet to comprise the following steps:
1) slab melting: the raw metal of proportioning is in proportion dropped into vacuum induction rapid hardening slab stove, vacuumize, melting at 800 DEG C, be heated to metal Pr when starting to melt, be filled with high-purity argon gas, through electromagnetic agitation mixing after raw metal melts, when after the conjunctiva of alloy molten solution surface, be poured on the water-cooled copper rod of rotation, through being cooled to the slab that thickness is 0.25 ~ 0.35mm fast;
2) hydrogen is pulverized: by step 1) slab that obtains drops into hydrogen crushing furnace, and dehydrogenation at 450 DEG C, obtains the alloying pellet of 100 ~ 110 μm;
3) airflow milling is pulverized: by step 2) alloying pellet that obtains adds in airflow milling under nitrogen protection, is ground into the alloy powder of 3.4 ~ 4.4 μm through airflow milling;
4) magnetic field orientating is shaping: by step 3) alloy powder that obtains drops into Magnetic field press, and oriented moulding under the magnetic field of 1.9T, obtains pressed compact;
5) isostatic pressed: will through step 4) shaping after pressed compact, reinstall in the high pressure chest of isostatic pressing machine, under the pressure of 190-200MPa, keep 10-20s;
6) sinter: will through step 5) pressed compact drop in vacuum sintering furnace, vacuumize, at 1080 DEG C, constant temperature 3.5 hours; One-level temperature is 1000 DEG C, constant temperature 1.5 hours; Second annealing temperature is 500 DEG C, constant temperature 2.5 hours; Finally obtain sintered magnet;
7) detect: the magnetic parameter of test products.
After testing, its key technical indexes reaches following parameter:
After testing, its key technical indexes reaches following parameter:
Remanent magnetism (Br) 1.22 ~ 1.27T
Magnetic induction coercive force (Hcb) >=900Ka/m
HCJ (Hcj) >=955Ka/m
Maximum magnetic energy product (BH) max:288 ~ 312KJ/m
3
Above content is in conjunction with concrete preferred implementation further description made for the present invention; can not assert that the specific embodiment of the present invention is only limitted to this; for general technical staff of the technical field of the invention; without departing from the inventive concept of the premise; some simple deduction or replace can also be made, all should be considered as belonging to the present invention by submitted to claims determination scope of patent protection.
Claims (5)
1. containing a neodymium cerium praseodymium slab magnet, it is characterized in that: slab magnet component and weight percentage are: Pr:4.0 ~ 5.0%, Nd:17.0 ~ 19.0%, Ce:6.5 ~ 7.5%, Gd:0.8 ~ 1.2%, Ho:0.9 ~ 1.3%, B:0.95 ~ 1.05%, Al:0.5 ~ 1.0%, Cu:0.15 ~ 0.20%, Co:0.20 ~ 0.40%, surplus Fe supplement.
2. a kind of containing neodymium cerium praseodymium slab magnet according to claim 1, it is characterized in that: slab magnet component and weight percentage are: Pr:4.5%, Nd:18.0%, Ce:7.0%, Gd:1.0%, Ho:1.1%, B:1.00%, Al:0.8%, Cu:0.18%, Co:0.30%, surplus Fe supplement.
3. prepare a kind of method containing neodymium cerium praseodymium slab magnet described in claim 1 or 2, comprise the following steps:
1) slab melting: the raw metal of proportioning is in proportion dropped into vacuum induction rapid hardening slab stove, vacuumize, melting at 800 ~ 1000 DEG C, be heated to metal Pr when starting to melt, be filled with high-purity argon gas, through ultrasonic mixing after raw metal melts, when after the conjunctiva of alloy molten solution surface, be poured on the water-cooled copper rod of rotation, through being cooled to the slab that thickness is 0.25 ~ 0.35mm fast;
2) hydrogen is pulverized: by step 1) slab that obtains drops into hydrogen crushing furnace, and dehydrogenation at 450 ~ 560 DEG C, obtains the alloying pellet of 100 ~ 110 μm;
3) airflow milling is pulverized: by step 2) alloying pellet that obtains adds in airflow milling under nitrogen protection, is ground into the alloy powder of 3.4 ~ 4.4 μm through airflow milling;
4) magnetic field orientating is shaping: by step 3) alloy powder that obtains drops into Magnetic field press, and oriented moulding under the magnetic field of 1.9T, obtains pressed compact;
5) isostatic pressed: will through step 4) shaping after pressed compact, reinstall in the high pressure chest of isostatic pressing machine, under the pressure of 190-200MPa, keep 10-20s;
6) sinter: will through step 5) pressed compact drop in vacuum sintering furnace, vacuumize, at 1080 ~ 1150 DEG C, constant temperature 2.5 ~ 3.5 hours; One-level temperature is 880 ~ 1000 DEG C, constant temperature 1.5 ~ 2.5 hours; Second annealing temperature is 500 ~ 600 DEG C, constant temperature 2.5 ~ 4.5 hours; Finally obtain sintered magnet.
4. a kind of preparation method containing neodymium cerium praseodymium slab magnet according to claim 3, is characterized in that: described step 1) in, raw metal mixes through electromagnetic agitation after melting.
5. a kind of preparation method containing neodymium cerium praseodymium slab magnet according to claim 3, is characterized in that: described step 6) in sintering temperature be 1120 DEG C, constant temperature 3 hours; One-level temperature is 920 DEG C, constant temperature 2 hours; Second annealing temperature is 550 DEG C, constant temperature 3 hours.
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| CN109065312A (en) * | 2018-09-13 | 2018-12-21 | 上海交通大学 | Neodymium iron boron magnetic body containing cerium and its heat treatment process and purposes |
| CN110257724A (en) * | 2019-07-16 | 2019-09-20 | 宁德市星宇科技有限公司 | A kind of preparation method of the neodymium iron boron magnetic body containing lanthanum and cerium |
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| CN110257724B (en) * | 2019-07-16 | 2020-05-22 | 宁德市星宇科技有限公司 | Preparation method of neodymium-iron-boron magnet containing lanthanum and cerium |
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Application publication date: 20151118 |