CN104599801A - Rare earth permanent magnetic material and preparation method thereof - Google Patents
Rare earth permanent magnetic material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a rare earth permanent magnetic material and a preparation method of the rare earth permanent magnetic material. The rare earth permanent magnetic material mainly comprises, by weight, 28-35% of PrNd, 0-5% of Dy or Tb or 0-5% of Dy and Tb, 1.0% of B, 0.01-10% of M and the balance being Fe, wherein M contains one or more elements of titanium, tin, zirconium, copper, cobalt, niobium, aluminum, manganese, gallium, chromium, nickel, zinc and magnesium, and when copper, cobalt, niobium and aluminum exist, Co accounts for 0-3%, Al accounts for 0.2-1.5%, Nb accounts for 0-0.5%, and Cu accounts for 0-0.2%. By controlling the content of hydrogen and oxygen and compound addition of microelements of a magnet, the rare earth permanent magnetic material achieves good sintered neodymium-iron-boron performance, good machining performance, good pressing and bending strength and other characteristics, and has the advantages of being low in heavy rare earth consumption, high in coercivity, excellent, low in cost, efficient in production, stable in quality and good in product quality controllability.
Description
Technical field
The present invention relates to a kind of permanent magnet and preparation method thereof, particularly a kind of there is good HCJ, consistency of performance is strong, machinability good, bending resistance compressive property is strong rare-earth permanent magnet and preparation method thereof.
Background technology
Rare earth permanent magnet, as emerging magnetic material, especially sintered NdFeB, has unprecedented high energy product, and after nineteen eighty-three is found, industry plays great function in new-energy automobile, wind-driven generator, servomotor, sound equipment motor etc.After 2000, along with the utilization of getting rid of band, hydrogen breaks technique, the magnetic property of sintered NdFeB significantly improves, according to domestic and international laboratory data, the remanent magnetism magnetic property of sintered NdFeB in 2005 reaches Br1.55T, having reached theoretical sintered NdFeB peak performance is 96.27% of remanent magnetism Br1.61T, but still Distance Theory value is comparatively large to determine the leading indicator coercive force (Hcj) of product serviceability temperature, is only 12% of theoretical value.How improving the coercive force of magnet, to better meet neodymium iron boron use at high operating temperatures, is the key that we break through at present.
Traditional Sintered NdFeB magnet technique is more the HCJ improving magnet by adding the less element such as heavy rare earth dysprosium, terbium of content improving in magnet working temperature.The anisotropy field HA of Dy2Fe14B is about 12000KA/m, and higher than the HA5600KA/m of Nd2Fe14B about 2.14 times, the HA of terbium is more obvious.A large amount of interpolations of the heavy rare earth such as dysprosium, terbium, although the HCJ of magnet significantly can be improved, but the magnetic polarization of Dy2Fe14B and Tb2Fe14B magnet is lower, the JS of Nd2Fe14B is 1.6T and the JS of Dy2Fe14B is only 0.71T, and a large amount of interpolations of the heavy rare earth such as dysprosium terbium cause the hydraulic performance declines such as the Br of neodymium iron boron obvious.And the heavy rare earth such as dysprosium terbium belongs to scarce resource, cost of winning is high, resource-constrained.Therefore, the use amount reducing the heavy rare earth such as dysprosium terbium while improving magnet working temperature is the key subjects needing us to solve.
For the requirement reducing or do not use the heavy rare earth such as dysprosium, terbium, a large amount of technological innovations and equipment research and development are carried out at present both at home and abroad, as reduced powder granularity, dysprosium diffusion etc.By the use of novel technique and new equipment, the HCJ of Sintered NdFeB magnet is greatly improved, but bring new problem thereupon: reduce that powder granularity easily causes that superfine powder is on the high side, product oxidation, inside and outside oxygen content be unbalanced, sintering time temperature control improper cause grain growth, fragility significantly increases, machinability is poor, product is easily fragmented into the problems such as product rate is low, and the thickness of dysprosium diffusion technology to product has certain restriction, oozes dysprosium and spread and be not easy equilibrium, easily occur the problems such as magnet thermal deformation.
Summary of the invention
For solving the problem, the invention discloses a kind of rare-earth permanent magnet and preparation method thereof, is a kind ofly have low heavy rare earth, high-coercive force, have excellent conforming high-performance rare-earth permanent-magnetic body.
Mainly consisting of (by weight percentage, wt%) of rare earth permanent-magnetic material disclosed by the invention, PrNd 28-35%; In Dy or Tb, one or both add up to 0-5%; B 1.0%; M 0.01-10%, surplus is Fe, and wherein M element is one or more in titanium, tin, zirconium, copper, cobalt, niobium, aluminium, manganese, gallium, chromium, nickel, zinc, magnesium, and when copper, cobalt, niobium, aluminium exist, Co 0-3%; Al 0.2-1.5%; Nb 0-0.5%; Cu 0-0.2%.
Preferred as one; M element is for add by nano-powder; described nano-powder is in one or both electrode assemblies protected in nitrogen or argon gas (keeping nitrogen or argon shield constant pressure), the powder of size 10 ~ 100 nanometer adopting arc process to prepare.
Preferred as one, rare earth permanent-magnetic material is average grain size is 2.5 ~ 3.5 μm, and smallest particles >=1 μm, the largest particles≤20 μm, preferred the largest particles≤10 μm.
Preferred as one, rare earth permanent-magnetic material rare earth elements Pr, Nd, Dy, Tb total amount proportion is 29-35%.
The preparation method of rare earth permanent-magnetic material disclosed by the invention, a, is configured at high melt in vacuum rapid hardening furnace according to the aforementioned various raw material by rare earth permanent-magnetic material, b, the alloy liquid that step a melting obtains obtains chilling slab by 0 ~ 35 DEG C of water-cooled copper roller quick-cooling and (thus impels chilling slab to generate the column crystal evenly penetrating in a large number the scope of freedom from copper roller contact-making surface, paste the column crystal forming core point distance 2 ~ 100 μm of roll surface), chilling slab is stirred well to Homogeneous cooling and obtains alloy casting piece (column crystal of alloy casting piece is evenly distributed in aqueous cold plate, forming core point is intensive, alloy casting piece gauge is 0.05-0.5mm thus makes alloy casting piece institutional framework without α Fe with without amorphous state, rich neodymium Entropy density deviation is even, there is good crystalline structure), the alloy casting piece that c, step b obtain is through hydrogen fragmentation, airflow milling, compression molding, magnetization, demagnetization, vacuum packaging, isostatic pressed compacting, vacuum-sintering and reprocessing thus obtain finished product.Magnet after being suppressed by isostatic pressed is put into oxygen content and is divested vacuum bag lower than the guard box of 500ppm and (namely keeping environment oxygen content lower than 500ppm) to load sintering basin to be sintered under remaining on same environment.Guard box can with sintering furnace disjunctor, also can split.Can select after hydrogen fragmentation in technical solution of the present invention that dehydrogenation is carried out to powder as required and carry out compression molding again, not dehydrogenation also can be selected directly to carry out compression molding.Hydrogen content >=500PPm contained by magnet powder after hydrogen fragmentation, can adopt dehydrogenation 1 ~ 10 hour of heating after hydrogen fragmentation, also can adopt not dehydrogenation mode airflow milling powder.Magnet controls oxygen content in powder by the inert gas such as nitrogen or argon gas in airflow milling powder process; guard box oxygen content 0 ~ 2000ppm is controlled during compression molding compacting; adopt oxygen content lower than the guard box of 500ppm after isostatic pressed; protection magnet enters sintering furnace, and after controlling sintering, the difference of oxygen content oxygen content inside and outside 200 ~ 1200ppm preferably 400 ~ 800ppm, single magnet of magnet is less than 500ppm and is preferably less than 200ppm, hydrogen content at 1 ~ 100ppm.The average crystal grain particle diameter of magnet is 3 ~ 8 μm, preferably 4 ~ 6 μm (being detected by the TM3030 scanning electron microscope analysis of Hitachi).
Magnetic airflow milling made adds in moulding press mould weigh up weight by regulation in the sealed environment of the inert gas shielding such as nitrogen or argon gas after.Press can adopt die cavity to fix, upper push-down head compacting.Also die cavity independent assortment can be used, the pattern of left and right compacting.Forming magnetic field field intensity must be greater than 1.5T, and the temperature of forming seal protective device is between 0 ~ 37 DEG C, and oxygen content 0 ~ 2000ppm, powder first carries out magnetizing orientation in a mold, then carries out being pressed into 3.5 ~ 4.5g/cm
3magnet, finally by press, magnet is demagnetized.Magnet after demagnetization carries out vacuum packaging in forming seal protective device, prevents oxygen from entering.Magnet after vacuum uses isostatic pressed compacting, and pressure 150 ~ 200Mpa, pressurize was taken out after 1 ~ 3 minute, and the density of magnet is at 4.0 ~ 5.0g/cm
3.
Preferred as one, in step c, vacuum-sintering also comprises dehydrogenating technology, and dehydrogenating technology comprises step I, the magnet after isostatic pressed compacting is carried out preliminary dehydrogenation and removal of impurities in 1 ~ 3 hour 250 ~ 350 DEG C of insulations; The magnet of step II, tentatively dehydrogenation and removal of impurities removes rich neodymium phase hydrogen for 1 ~ 5 hour 450 ~ 600 DEG C of insulations, and the magnet oxygen content after process is 200 ~ 1000ppm, and more preferably oxygen content is 400 ~ 800ppm; The difference of the inside and outside oxygen content of single magnet is less than 500ppm, and more preferably the difference of the inside and outside oxygen content of single magnet is less than 200ppm; Magnet hydrogen content is 1 ~ 100ppm.The anti-oxidation of performance in process of production in order to improve magnet, magnet itself is also containing a large amount of hydrogen.Now part hydrogen can be free in magnet space, can cause that magnet cracks, fragility increases, processability is poor, here free hydrogen, impurity and the rich neodymium phase hydrogen in magnet effectively can be removed by twice dehydrogenating technology, thus quality stability and the processability of magnet can be improved to a great extent, effectively improve rate of finished products.
Preferred as one, in step c, post-processing step is after high temperature 1000 ~ 1080 DEG C sinters 1-10 hour, cooling and sequentially through the tempering of 1 ~ 3 hour when 850 ~ 950 DEG C, is cooled to less than 80 DEG C after the double tempering of 2 ~ 5 hours when 450 ~ 550 DEG C and comes out of the stove.
Preferred as one, in step b, chilling slab is for being congeal into after rejection tablet in 0 ~ 35 DEG C of water-cooled copper roller rapidly in temperature, is incubated 600 ~ 900 DEG C and obtains for 1 ~ 30 minute.
Preferred as one, in step c, magnetized field strength is greater than 1.5T, and forming temperature is between 0 ~ 37 DEG C.
Preferred as one, in step c, after vacuum-sintering, the oxygen content of magnet is at 200 ~ 1200ppm, and hydrogen content is at 1 ~ 100ppm, and wherein the difference of the inside and outside oxygen content of single magnet is less than 500ppm.
R-Fe-B (R represents rare earth element) RE permanent magnetic alloy sheet is meeting and hydrogen generation hydrogen abstraction reaction in the atmosphere of hydrogen:
R2Fe14B+Hx＝R2Fe14BHx-△H1
R+Hy＝RNdHy-△H2
Because RFeB alloy sheet is fragile material, percentage elongation is almost nil, and fracture strength is very low, and the regional area forming hydride during hydrogenation produces volumetric expansion and internal stress, thus forms single crystal grain.By this principle, hydrogen can be imported in airtight stainless steel cask with alloy sheet generation hydrogenation, make the hydrogen comminuted powder of hydrogen content >=500PPm.Because protium has anti-oxidation function, therefore, the hydrogen content of hydrogen flour reservation >=500PPm is favourable to magnet performance.
In order to the anti-oxidation of the performance improving magnet, magnet itself is also containing a large amount of hydrogen.Part hydrogen can be free in magnet space, causes magnet to crack, fragility increases, processability is poor.Before sintering high temperature, carry out Dehydroepiandrosterone derivative just seem particularly necessary.
Rare earth magnet disclosed by the invention has lower oxygen content, has good crystal boundary structure and average crystal grain simultaneously.Magnet can obtain the HCJ of higher than common process about 10%, thus reduces the use amount of heavy rare earth dysprosium terbium etc., and protium is departed from substantially, oxygen content is balanced inside and outside magnet, and the machinability of magnet itself is good, and qualification rate is high.
Embodiment
Below in conjunction with embodiment, illustrate the present invention further, following embodiment should be understood and be only not used in for illustration of the present invention and limit the scope of the invention.
Mainly consisting of (by weight percentage, wt%) of rare earth permanent-magnetic material disclosed by the invention, PrNd 28-35%; In Dy or Tb, one or both add up to 0-5%; B 1.0%; M 0.01-10%, surplus is Fe, and wherein M element is one or more in titanium, tin, zirconium, copper, cobalt, niobium, aluminium, manganese, gallium, chromium, nickel, zinc, magnesium, and when copper, cobalt, niobium, aluminium exist, Co 0-3%; Al 0.2-1.5%; Nb 0-0.5%; Cu 0-0.2%.
Preferred as one, M element is for add by nano-powder, and described nano-powder is in one or both electrode assemblies protected in nitrogen or argon gas, the powder of size 10 ~ 100 nanometer adopting arc process to prepare.
Preferred as one, rare earth permanent-magnetic material is average grain size is 2.5 ~ 3.5 μm, and smallest particles >=1 μm, the largest particles≤20 μm, preferred the largest particles≤10 μm.
Preferred as one, rare earth permanent-magnetic material rare earth elements Pr, Nd, Dy, Tb total amount proportion is 29-35%.
The preparation method of rare earth permanent-magnetic material disclosed by the invention, a, is configured at high melt in vacuum rapid hardening furnace according to the aforementioned various raw material by rare earth permanent-magnetic material, b, the alloy liquid that step a melting obtains obtains chilling slab by 0 ~ 35 DEG C of water-cooled copper roller quick-cooling and (thus impels chilling slab to generate the column crystal evenly penetrating in a large number the scope of freedom from copper roller contact-making surface, paste the column crystal forming core point distance 2 ~ 100 μm of roll surface), chilling slab is stirred well to Homogeneous cooling and obtains alloy casting piece (column crystal of alloy casting piece is evenly distributed in aqueous cold plate, forming core point is intensive, alloy casting piece gauge is 0.05-0.5mm thus makes alloy casting piece institutional framework without α Fe with without amorphous state, rich neodymium Entropy density deviation is even, there is good crystalline structure), the alloy casting piece that c, step b obtain is through hydrogen fragmentation, airflow milling, compression molding, magnetization, demagnetization, vacuum packaging, isostatic pressed compacting, vacuum-sintering and reprocessing thus obtain finished product.
Preferred as one, in step c, vacuum-sintering also comprises dehydrogenating technology, and described dehydrogenating technology comprises step I, the magnet after isostatic pressed compacting is carried out preliminary dehydrogenation and removal of impurities in 1 ~ 3 hour 250 ~ 350 DEG C of insulations; The magnet of step II, tentatively dehydrogenation and removal of impurities removes rich neodymium phase hydrogen for 1 ~ 5 hour 450 ~ 600 DEG C of insulations.The anti-oxidation of performance in process of production in order to improve magnet, magnet itself is also containing a large amount of hydrogen.Now part hydrogen can be free in magnet space, can cause that magnet cracks, fragility increases, processability is poor, here free hydrogen, impurity and the rich neodymium phase hydrogen in magnet effectively can be removed by twice dehydrogenating technology, thus quality stability and the processability of magnet can be improved to a great extent, effectively improve rate of finished products.
Preferred as one, in step c, post-processing step is after high temperature 1000 ~ 1080 DEG C sinters 1 ~ 10 hour, cooling and sequentially through the tempering of 1 ~ 3 hour when 850 ~ 950 DEG C, is cooled to less than 80 DEG C after the double tempering of 2 ~ 5 hours when 450 ~ 550 DEG C and comes out of the stove.
Preferred as one, in step b, chilling slab is for being congeal into after rejection tablet in 0 ~ 35 DEG C of water-cooled copper roller rapidly in temperature, is incubated 600 ~ 900 DEG C and obtains for 1 ~ 30 minute.
Preferred as one, in step c, magnetized field strength is greater than 1.5T, and forming temperature is between 0 ~ 37 DEG C.
Preferred as one, in step c, after vacuum-sintering, the oxygen content of magnet is at 200 ~ 1200ppm, and hydrogen content is at 1 ~ 100ppm, and wherein the difference of the inside and outside oxygen content of single magnet is less than 500ppm.
Following table one is the proportioning table (all by weight percentage) of other component in the embodiment 1-14 of technical solution of the present invention except Fe:
Embodiment one:
1, prepare burden: according to the composition batching shown in upper table one.
2, melting: after loading vacuum rapid hardening furnace after directly being mixed by formulation weight (see table one) requirement by various main body raw material (major phase material except M), when being evacuated down to below 0.4Pa, start melting of heating, when in stove, material is rubescent, be filled with argon gas, and raise temperature, smelting temperature 1450 DEG C, until material melts completely in stove, refining was congealed into after rejection tablet by 0 DEG C of water-cooled copper roller quick-cooling after 10 minutes again, and be incubated 640 DEG C and obtain chilling slab in 20 minutes, chilling slab is stirred well to Homogeneous cooling in 0 DEG C of aqueous cold plate, thus obtains alloy casting piece.
3, hydrogen is broken: be positioned over by alloy casting piece in hydrogen crushing furnace, pass into hydrogen, and inhale completely until product and be warming up to 500 ~ 550 DEG C, 2 hours after hydrogen and carry out fragmentation, hydrogen flour material does not carry out dehydrogenation.
4, hydrogen flour material being put into oxygen content is that the high pure nitrogen shielding gas flow mill being less than 10ppm carries out powder process, controls powder particle mean size (laser particle analyzer) between 2 ~ 4 μm.
5, shaping: in aforementioned obtained powder, to add M element nano powder (composition is in table one) mix and blend 2 hours; the powder be stirred is weighed by predetermined weight; put into nitrogen protection and close press; control oxygen content 0 ~ 500ppm, forming temperature 0 DEG C, orientation in 40mm air gap 2T magnetic field; and then suppress; the encapsulation of demagnetization final vacuum, then the green compact of Vacuum Package are carried out isostatic pressed 150Mpa, pressurize was taken out after 3 minutes.
Corresponding alloy (see table one) arc process in the electrode assembly of nitrogen protection is obtained nano-powder by being prepared as of M element nano powder, and nano-powder is of a size of 10nm.
6, sinter: green compact are first carried out preliminary dehydrogenation and removal of impurities in 3 hours 250 DEG C of insulations, then within 1 ~ 5 hour, removes rich neodymium phase hydrogen 500 DEG C of insulations; Again in nitrogen protection; load in sintering basin after oxygen content 0 ~ 500ppm glove box stripping oil, put into sintering furnace sintering, under the sintering temperature of 1045 DEG C, sinter 1 hour; on 900 DEG C, once double tempering took out after 3 hours at tempering 2h and 500 DEG C, and Sintered NdFeB magnet operation completes.
By the Sintered NdFeB magnet that above operation is produced, after surface grinding, detect according to GB/T3217 permanent magnetism (Hard Magnetic) magnetism of material test method regulation, magnetic property is:
Remanent magnetism Br:13.913KGs
HCJ Hcj:14.91KOe
Coercivity H b:13.12KOe
Magnetic energy product BH (max): 46.63MGOe
HK/Hcj：0.98
Embodiment two:
1, prepare burden: according to the composition batching shown in upper table one.
2, melting: after loading vacuum rapid hardening furnace after directly being mixed by formulation weight (see table one) requirement by various main body raw material (major phase material except M), when vacuum spun furnace is evacuated down to below 0.4Pa, start melting of heating, when in stove, material is rubescent, be filled with argon gas, and raise temperature, smelting temperature 1460 DEG C, until raw material melt completely, refining was congealed into after rejection tablet by 20 DEG C of water-cooled copper roller quick-coolings after 10 minutes, and be incubated 720 DEG C and obtain chilling slab in 30 minutes, chilling slab is stirred well to Homogeneous cooling in 20 DEG C of aqueous cold plates, thus obtain alloy casting piece.
3, hydrogen is broken: be positioned in hydrogen crushing furnace by master alloying rejection tablet, pass into hydrogen, inhales completely be warming up to 550 ~ 600 DEG C, 2 hours after hydrogen and carry out fragmentation, hydrogen flour material powder intensification dehydrogenation 10 hours until product.
4, the hydrogen flour material after dehydrogenation being put into oxygen content is that the high pure nitrogen shielding gas flow mill being less than 10ppm carries out powder process, controls powder particle mean size (laser particle analyzer) between 3 ~ 3.5 μm.
5, shaping: in aforementioned obtained powder, to add M element nano powder (composition is in table one) mix and blend 3 hours; the powder be stirred is weighed by predetermined weight; put into nitrogen protection and close press; control oxygen content 500 ~ 1000ppm; forming temperature 21 DEG C, orientation, compacting in 40mm air gap 1.8T magnetic field, the encapsulation of demagnetization final vacuum; again the green compact of Vacuum Package are carried out isostatic pressed 200Mpa, pressurize was taken out after 1 minute.
Corresponding alloy (see table one) arc process in the electrode assembly of argon shield is obtained nano-powder by being prepared as of M element nano powder, and nano-powder is of a size of 20nm.
6, sinter: green compact are first carried out preliminary dehydrogenation and removal of impurities in 1 hour 300 DEG C of insulations, then within 1 ~ 5 hour, removes rich neodymium phase hydrogen 450 DEG C of insulations; Again in nitrogen protection; load after oxygen content 0 ~ 500ppm glove box stripping oil in sintering basin; put into sintering furnace sintering; 4.5 hours are sintered under the sintering temperature of 1000 DEG C; on 950 DEG C, once double tempering is cooled to 80 DEG C of taking-ups after 5 hours at tempering 1h and 550 DEG C, and Sintered NdFeB magnet operation completes.
By the Sintered NdFeB magnet that above operation is produced, after surface grinding, detect according to GB/T3217 permanent magnetism (Hard Magnetic) magnetism of material test method regulation, magnetic property is:
Remanent magnetism Br:13.46KGs
HCJ Hcj:17.93KOe
Coercivity H b:12.82KOe
Magnetic energy product BH (max): 43.35MGOe
HK/Hcj：0.97
Embodiment three:
1, prepare burden: according to the composition batching shown in upper table one.
2, melting: after loading vacuum rapid hardening furnace after directly being mixed by formulation weight requirement by formulation weight (see table one) by various main body raw material (major phase material except M), when vacuum spun furnace is evacuated down to below 0.4Pa, start melting of heating, when in stove, material is rubescent, be filled with argon gas, and raise temperature, smelting temperature 1470 DEG C, until raw material melt completely, refining was congealed into after rejection tablet by 15 DEG C of water-cooled copper roller quick-coolings after 10 minutes, and be incubated 820 DEG C and obtain chilling slab in 20 minutes, chilling slab is stirred well to Homogeneous cooling in 15 DEG C of aqueous cold plates, thus obtain alloy casting piece.
3, hydrogen is broken: be positioned in hydrogen crushing furnace by master alloying rejection tablet, pass into hydrogen, inhales completely be warming up to 550 ~ 600 DEG C, 2 hours after hydrogen and carry out fragmentation, hydrogen flour material powder intensification dehydrogenation 1 hour until product.
4, the hydrogen flour material after dehydrogenation being put into oxygen content is that the high pure nitrogen shielding gas flow mill being less than 10ppm carries out powder process, controls powder particle mean size (laser particle analyzer) between 2.5 ~ 3 μm.
5, shaping: in aforementioned obtained powder, to add M element nano powder (composition is in table one) stir 4 hours; the powder be stirred is weighed by predetermined weight; put into nitrogen protection and close press; control oxygen content 0 ~ 500ppm, forming temperature 16 DEG C, orientation in 40mm air gap 2T magnetic field; and then suppress; the encapsulation of demagnetization final vacuum, then the green compact of Vacuum Package are carried out isostatic pressed 200Mpa, pressurize was taken out after 2 minutes.
Corresponding alloy (see table one) arc process in nitrogen and helium mix protection (mixing mol ratio is 8:2 (nitrogen: the helium)) electrode assembly protected is obtained nano-powder by being prepared as of M element nano powder, and nano-powder is of a size of 30nm.
6, sinter: green compact are first carried out preliminary dehydrogenation and removal of impurities in 2 hours 260 DEG C of insulations, then within 1 ~ 5 hour, removes rich neodymium phase hydrogen 480 DEG C of insulations; Again in nitrogen protection; load in sintering basin after oxygen content 300ppm glove box stripping oil, put into sintering furnace sintering, under the sintering temperature of 1080 DEG C, sinter 4 hours; take out after 2 hours 850 DEG C of tempering 3h and 450 DEG C tempering, Sintered NdFeB magnet operation completes.
By the Sintered NdFeB magnet that above operation is produced, after surface grinding, detect according to GB/T3217 permanent magnetism (Hard Magnetic) magnetism of material test method regulation, magnetic property is:
Remanent magnetism Br:12.34KGs
HCJ Hcj:26.78KOe
Coercivity H b:12.05KOe
Magnetic energy product BH (max): 37.16MGOe
HK/Hcj：0.94
Embodiment four:
1, prepare burden: according to the composition batching shown in upper table one.
2, melting: after loading vacuum rapid hardening furnace after directly being mixed by formulation weight (see table one) requirement by various main body raw material (major phase material except M), when being evacuated down to below 0.4Pa, start melting of heating, when in stove, material is rubescent, be filled with argon gas, and raise temperature, smelting temperature 1450 DEG C, until material melts completely in stove, refining was congealed into after rejection tablet by 23 DEG C of water-cooled copper roller quick-coolings after 10 minutes again, and be incubated 720 DEG C and obtain chilling slab in 17 minutes, chilling slab is stirred well to Homogeneous cooling in 23 DEG C of aqueous cold plates, thus obtains alloy casting piece.
3, hydrogen is broken: be positioned over by alloy casting piece in hydrogen crushing furnace, pass into hydrogen, inhales completely be warming up to 500 ~ 550 DEG C, 2 hours after hydrogen and carry out fragmentation, hydrogen flour material powder intensification dehydrogenase 35 hour until product.
4, the hydrogen flour material after dehydrogenation being put into oxygen content is that the high pure nitrogen shielding gas flow mill being less than 10ppm carries out powder process, controls powder particle mean size (laser particle analyzer) between 2 ~ 4 μm.
5, shaping: in aforementioned obtained powder, to add M element nano powder (composition is in table one) mix and blend 2 hours; the powder be stirred is weighed by predetermined weight; put into nitrogen protection and close press; control oxygen content 0 ~ 500ppm, forming temperature 24 DEG C, orientation in 40mm air gap 2T magnetic field; and then suppress; the encapsulation of demagnetization final vacuum, then the green compact of Vacuum Package are carried out isostatic pressed 150Mpa, pressurize was taken out after 3 minutes.
Corresponding alloy (see table one) arc process in the electrode assembly of nitrogen protection is obtained nano-powder by being prepared as of M element nano powder, and nano-powder is of a size of 40nm.
6, sinter: green compact are first carried out preliminary dehydrogenation and removal of impurities in 3 hours 350 DEG C of insulations, then within 1 ~ 5 hour, removes rich neodymium phase hydrogen 590 DEG C of insulations; Again in nitrogen protection; load in sintering basin after oxygen content 0 ~ 500ppm glove box stripping oil, put into sintering furnace sintering, under the sintering temperature of 1045 DEG C, sinter 3 hours; on 900 DEG C, once double tempering took out after 3 hours at tempering 2h and 500 DEG C, and Sintered NdFeB magnet operation completes.
By the Sintered NdFeB magnet that above operation is produced, after surface grinding, detect according to GB/T3217 permanent magnetism (Hard Magnetic) magnetism of material test method regulation, magnetic property is:
Remanent magnetism Br:13.913KGs
HCJ Hcj:14.91KOe
Coercivity H b:13.12KOe
Magnetic energy product BH (max): 46.63MGOe
HK/Hcj：0.98
| Heavy rare earth dysprosium content | Compression strength Mp | Corner oxygen content ppm | Inner oxygen content ppm | Hydrogen content ppm | |
| Traditional handicraft | 0.7~1% | 286 | 700~1000 | 600~800 | 30~50 |
| Present invention process | 0.5% | 326 | 650~6900 | 620~640 | 1~20 |
Embodiment five:
1, prepare burden: according to the composition batching shown in upper table one.
2, melting: after loading vacuum rapid hardening furnace after directly being mixed by formulation weight (see table one) requirement by various main body raw material (major phase material except M), when vacuum spun furnace is evacuated down to below 0.4Pa,
Start melting of heating, when in stove, material is rubescent, be filled with argon gas, and raising temperature, smelting temperature 1460 DEG C, until raw material melt completely, refining obtained congealing into after rejection tablet by 35 DEG C of water-cooled copper roller quick-coolings after 10 minutes, and being incubated 630 DEG C of 17 minutes chilling slabs, chilling slab is stirred well to Homogeneous cooling in 35 DEG C of aqueous cold plates, thus obtains alloy casting piece.
3, hydrogen is broken: be positioned in hydrogen crushing furnace by master alloying rejection tablet, pass into hydrogen, inhales completely be warming up to 550 ~ 600 DEG C, 2 hours after hydrogen and carry out fragmentation, hydrogen flour material powder intensification dehydrogenation 8 hours until product.
4, the hydrogen flour material after dehydrogenation being put into oxygen content is that the high pure nitrogen shielding gas flow mill being less than 10ppm carries out powder process, controls powder particle mean size (laser particle analyzer) between 3 ~ 3.5 μm.
5, shaping: in aforementioned obtained powder, to add M element nano powder (composition is in table one) mix and blend 3 hours; the powder be stirred is weighed by predetermined weight; put into nitrogen protection and close press; control oxygen content 500 ~ 1000ppm; forming temperature 37 DEG C, orientation, compacting in 40mm air gap 1.8T magnetic field, the encapsulation of demagnetization final vacuum; again the green compact of Vacuum Package are carried out isostatic pressed 200Mpa, pressurize was taken out after 1 minute.
Corresponding alloy (see table one) arc process in the electrode assembly of argon shield is obtained nano-powder by being prepared as of M element nano powder, and nano-powder is of a size of 50nm.
6, sinter: green compact are first carried out preliminary dehydrogenation and removal of impurities in 1 hour 270 DEG C of insulations, then within 1 ~ 5 hour, removes rich neodymium phase hydrogen 460 DEG C of insulations; Again in nitrogen protection; load after oxygen content 0 ~ 500ppm glove box stripping oil in sintering basin; put into sintering furnace sintering; 10 hours are sintered under the sintering temperature of 1000 DEG C; on 950 DEG C, once double tempering is cooled to 80 DEG C of taking-ups after 5 hours at tempering 1h and 550 DEG C, and Sintered NdFeB magnet operation completes.
By the Sintered NdFeB magnet that above operation is produced, after surface grinding, detect according to GB/T3217 permanent magnetism (Hard Magnetic) magnetism of material test method regulation, magnetic property is:
Remanent magnetism Br:13.46KGs
HCJ Hcj:17.93KOe
Coercivity H b:12.82KOe
Magnetic energy product BH (max): 43.35MGOe
HK/Hcj：0.97
Embodiment six:
1, prepare burden: according to the composition batching shown in upper table one.
2, melting: after loading vacuum rapid hardening furnace after directly being mixed by formulation weight requirement by formulation weight (see table one) by various main body raw material (major phase material except M), when vacuum spun furnace is evacuated down to below 0.4Pa, start melting of heating, when in stove, material is rubescent, be filled with argon gas, and raise temperature, smelting temperature 1470 DEG C, until raw material melt completely, refining was congealed into after rejection tablet by 7 DEG C of water-cooled copper roller quick-coolings after 10 minutes, and be incubated 650 DEG C and obtain chilling slab in 23 minutes, chilling slab is stirred well to Homogeneous cooling in 7 DEG C of aqueous cold plates, thus obtain alloy casting piece.
3, hydrogen is broken: be positioned in hydrogen crushing furnace by master alloying rejection tablet, pass into hydrogen, and inhale completely until product and be warming up to 550 ~ 600 DEG C, 2 hours after hydrogen and carry out fragmentation, hydrogen flour material does not carry out dehydrogenation.
4, powder being put into oxygen content is that the high pure nitrogen shielding gas flow mill being less than 10ppm carries out powder process, controls powder particle mean size (laser particle analyzer) between 2.5 ~ 3 μm.
5, shaping: in aforementioned obtained powder, to add M element nano powder (composition is in table one) stir 4 hours; the powder be stirred is weighed by predetermined weight; put into nitrogen protection and close press; control oxygen content 0 ~ 500ppm, forming temperature 6 DEG C, orientation in 40mm air gap 2T magnetic field; and then suppress; the encapsulation of demagnetization final vacuum, then the green compact of Vacuum Package are carried out isostatic pressed 200Mpa, pressurize was taken out after 2 minutes.
Corresponding alloy (see table one) arc process in nitrogen and helium mix protection (mixing mol ratio is 8:2 (nitrogen: the helium)) electrode assembly protected is obtained nano-powder by being prepared as of M element nano powder, and nano-powder is of a size of 60nm.
6, sinter: green compact are first carried out preliminary dehydrogenation and removal of impurities in 2 hours 310 DEG C of insulations, then within 1 ~ 5 hour, removes rich neodymium phase hydrogen 600 DEG C of insulations; Again in nitrogen protection; load in sintering basin after oxygen content 300ppm glove box stripping oil, put into sintering furnace sintering, under the sintering temperature of 1080 DEG C, sinter 9 hours; take out after 2 hours 850 DEG C of tempering 3h and 450 DEG C tempering, Sintered NdFeB magnet operation completes.
By the Sintered NdFeB magnet that above operation is produced, after surface grinding, detect according to GB/T3217 permanent magnetism (Hard Magnetic) magnetism of material test method regulation, magnetic property is:
Remanent magnetism Br:12.34KGs
HCJ Hcj:26.78KOe
Coercivity H b:12.05KOe
Magnetic energy product BH (max): 37.16MGOe
HK/Hcj：0.94
Embodiment seven:
1, prepare burden: according to the composition batching shown in upper table one.
2, melting: after loading vacuum rapid hardening furnace after directly being mixed by formulation weight (see table one) requirement by various main body raw material (major phase material except M), when being evacuated down to below 0.4Pa, start melting of heating, when in stove, material is rubescent, be filled with argon gas, and raise temperature, smelting temperature 1450 DEG C, until material melts completely in stove, refining was congealed into after rejection tablet by 27 DEG C of water-cooled copper roller quick-coolings after 10 minutes again, and be incubated 700 DEG C and obtain chilling slab in 12 minutes, chilling slab is stirred well to Homogeneous cooling in 27 DEG C of aqueous cold plates, thus obtains alloy casting piece.
3, hydrogen is broken: be positioned over by alloy casting piece in hydrogen crushing furnace, pass into hydrogen, and inhale completely until product and be warming up to 500 ~ 550 DEG C, 2 hours after hydrogen and carry out fragmentation, hydrogen flour material does not carry out dehydrogenation.
4, hydrogen flour material being put into oxygen content is that the high pure nitrogen shielding gas flow mill being less than 10ppm carries out powder process, controls powder particle mean size (laser particle analyzer) between 2 ~ 4 μm.
5, shaping: in aforementioned obtained powder, to add M element nano powder (composition is in table one) mix and blend 2 hours; the powder be stirred is weighed by predetermined weight; put into nitrogen protection and close press; control oxygen content 0 ~ 500ppm, forming temperature 28 DEG C, orientation in 40mm air gap 2T magnetic field; and then suppress; the encapsulation of demagnetization final vacuum, then the green compact of Vacuum Package are carried out isostatic pressed 150Mpa, pressurize was taken out after 3 minutes.
Corresponding alloy (see table one) arc process in the electrode assembly of nitrogen protection is obtained nano-powder by being prepared as of M element nano powder, and nano-powder is of a size of 70nm.
6, sinter: green compact are first carried out preliminary dehydrogenation and removal of impurities in 3 hours 320 DEG C of insulations, then within 1 ~ 5 hour, removes rich neodymium phase hydrogen 520 DEG C of insulations; Again in nitrogen protection; load in sintering basin after oxygen content 0 ~ 500ppm glove box stripping oil, put into sintering furnace sintering, under the sintering temperature of 1045 DEG C, sinter 8 hours; on 900 DEG C, once double tempering took out after 3 hours at tempering 2h and 500 DEG C, and Sintered NdFeB magnet operation completes.
By the Sintered NdFeB magnet that above operation is produced, after surface grinding, detect according to GB/T3217 permanent magnetism (Hard Magnetic) magnetism of material test method regulation, magnetic property is:
Remanent magnetism Br:13.913KGs
HCJ Hcj:14.91KOe
Coercivity H b:13.12KOe
Magnetic energy product BH (max): 46.63MGOe
HK/Hcj：0.98
Embodiment eight:
1, prepare burden: according to the composition batching shown in upper table one.
2, melting: after loading vacuum rapid hardening furnace after directly being mixed by formulation weight (see table one) requirement by various main body raw material (major phase material except M), when vacuum spun furnace is evacuated down to below 0.4Pa, start melting of heating, when in stove, material is rubescent, be filled with argon gas, and raise temperature, smelting temperature 1460 DEG C, until raw material melt completely, refining was congealed into after rejection tablet by 13 DEG C of water-cooled copper roller quick-coolings after 10 minutes, and be incubated 800 DEG C and obtain chilling slab in 5 minutes, chilling slab is stirred well to Homogeneous cooling in 13 DEG C of aqueous cold plates, thus obtain alloy casting piece.
3, hydrogen is broken: be positioned in hydrogen crushing furnace by master alloying rejection tablet, pass into hydrogen, and inhale completely until product and be warming up to 550 ~ 600 DEG C, 2 hours after hydrogen and carry out fragmentation, hydrogen flour material does not carry out dehydrogenation.
4, hydrogen flour material being put into oxygen content is that the high pure nitrogen shielding gas flow mill being less than 10ppm carries out powder process, controls powder particle mean size (laser particle analyzer) between 3 ~ 3.5 μm.
5, shaping: in aforementioned obtained powder, to add M element nano powder (composition is in table one) mix and blend 3 hours; the powder be stirred is weighed by predetermined weight; put into nitrogen protection and close press; control oxygen content 500 ~ 1000ppm; forming temperature 12 DEG C, orientation, compacting in 40mm air gap 1.8T magnetic field, the encapsulation of demagnetization final vacuum; again the green compact of Vacuum Package are carried out isostatic pressed 200Mpa, pressurize was taken out after 1 minute.
Corresponding alloy (see table one) arc process in the electrode assembly of argon shield is obtained nano-powder by being prepared as of M element nano powder, and nano-powder is of a size of 80nm.
6, sinter: green compact are first carried out preliminary dehydrogenation and removal of impurities in 1 hour 290 DEG C of insulations, then within 1 ~ 5 hour, removes rich neodymium phase hydrogen 570 DEG C of insulations; Again in nitrogen protection; load after oxygen content 0 ~ 500ppm glove box stripping oil in sintering basin; put into sintering furnace sintering; 5 hours are sintered under the sintering temperature of 1000 DEG C; on 950 DEG C, once double tempering is cooled to 80 DEG C of taking-ups after 5 hours at tempering 1h and 550 DEG C, and Sintered NdFeB magnet operation completes.
By the Sintered NdFeB magnet that above operation is produced, after surface grinding, detect according to GB/T3217 permanent magnetism (Hard Magnetic) magnetism of material test method regulation, magnetic property is:
Remanent magnetism Br:13.46KGs
HCJ Hcj:17.93KOe
Coercivity H b:12.82KOe
Magnetic energy product BH (max): 43.35MGOe
HK/Hcj：0.97
Embodiment nine:
1, prepare burden: according to the composition batching shown in upper table one.
2, melting: after loading vacuum rapid hardening furnace after directly being mixed by formulation weight requirement by formulation weight (see table one) by various main body raw material (major phase material except M), when vacuum spun furnace is evacuated down to below 0.4Pa, start melting of heating, when in stove, material is rubescent, be filled with argon gas, and raise temperature, smelting temperature 1470 DEG C, until raw material melt completely, refining was congealed into after rejection tablet by 28 DEG C of water-cooled copper roller quick-coolings after 10 minutes, and be incubated 750 DEG C and obtain chilling slab in 20 minutes, chilling slab is stirred well to Homogeneous cooling in 28 DEG C of aqueous cold plates, thus obtain alloy casting piece.
3, hydrogen is broken: be positioned in hydrogen crushing furnace by master alloying rejection tablet, pass into hydrogen, and inhale completely until product and be warming up to 550 ~ 600 DEG C, 2 hours after hydrogen and carry out fragmentation, hydrogen flour material does not carry out dehydrogenation.
4, powder being put into oxygen content is that the high pure nitrogen shielding gas flow mill being less than 10ppm carries out powder process, controls powder particle mean size (laser particle analyzer) between 2.5 ~ 3 μm.
5, shaping: in aforementioned obtained powder, to add M element nano powder (composition is in table one) stir 4 hours; the powder be stirred is weighed by predetermined weight; put into nitrogen protection and close press; control oxygen content 0 ~ 500ppm, forming temperature 27 DEG C, orientation in 40mm air gap 2T magnetic field; and then suppress; the encapsulation of demagnetization final vacuum, then the green compact of Vacuum Package are carried out isostatic pressed 200Mpa, pressurize was taken out after 2 minutes.
Corresponding alloy (see table one) arc process in nitrogen and helium mix protection (mixing mol ratio is 8:2 (nitrogen: the helium)) electrode assembly protected is obtained nano-powder by being prepared as of M element nano powder, and nano-powder is of a size of 90nm.
6, sinter: green compact are first carried out preliminary dehydrogenation and removal of impurities in 2 hours 330 DEG C of insulations, then within 1 ~ 5 hour, removes rich neodymium phase hydrogen 550 DEG C of insulations; Again in nitrogen protection; load in sintering basin after oxygen content 300ppm glove box stripping oil, put into sintering furnace sintering, under the sintering temperature of 1080 DEG C, sinter 6 hours; take out after 2 hours 850 DEG C of tempering 3h and 450 DEG C tempering, Sintered NdFeB magnet operation completes.
By the Sintered NdFeB magnet that above operation is produced, after surface grinding, detect according to GB/T3217 permanent magnetism (Hard Magnetic) magnetism of material test method regulation, magnetic property is:
Remanent magnetism Br:12.34KGs
HCJ Hcj:26.78KOe
Coercivity H b:12.05KOe
Magnetic energy product BH (max): 37.16MGOe
HK/Hcj：0.94
Embodiment ten:
1, prepare burden: according to the composition batching shown in upper table one.
2, melting: after loading vacuum rapid hardening furnace after directly being mixed by formulation weight (see table one) requirement by various main body raw material (major phase material except M), when being evacuated down to below 0.4Pa, start melting of heating, when in stove, material is rubescent, be filled with argon gas, and raise temperature, smelting temperature 1450 DEG C, until material melts completely in stove, refining was congealed into after rejection tablet by 19 DEG C of water-cooled copper roller quick-coolings after 10 minutes again, and be incubated 850 DEG C and obtain chilling slab in 15 minutes, chilling slab is stirred well to Homogeneous cooling in 19 DEG C of aqueous cold plates, thus obtains alloy casting piece.
3, hydrogen is broken: be positioned over by alloy casting piece in hydrogen crushing furnace, pass into hydrogen, and inhale completely until product and be warming up to 500 ~ 550 DEG C, 2 hours after hydrogen and carry out fragmentation, hydrogen flour material does not carry out dehydrogenation.
4, hydrogen flour material being put into oxygen content is that the high pure nitrogen shielding gas flow mill being less than 10ppm carries out powder process, controls powder particle mean size (laser particle analyzer) between 2 ~ 4 μm.
5, shaping: in aforementioned obtained powder, to add M element nano powder (composition is in table one) mix and blend 2 hours; the powder be stirred is weighed by predetermined weight; put into nitrogen protection and close press; control oxygen content 0 ~ 500ppm, forming temperature 18 DEG C, orientation in 40mm air gap 2T magnetic field; and then suppress; the encapsulation of demagnetization final vacuum, then the green compact of Vacuum Package are carried out isostatic pressed 150Mpa, pressurize was taken out after 3 minutes.
Corresponding alloy (see table one) arc process in the electrode assembly of nitrogen protection is obtained nano-powder by being prepared as of M element nano powder, and nano-powder is of a size of 100nm.
6, sinter: green compact are first carried out preliminary dehydrogenation and removal of impurities in 3 hours 280 DEG C of insulations, then within 1 ~ 5 hour, removes rich neodymium phase hydrogen 540 DEG C of insulations; Again in nitrogen protection; load in sintering basin after oxygen content 0 ~ 500ppm glove box stripping oil, put into sintering furnace sintering, under the sintering temperature of 1045 DEG C, sinter 5.6 hours; on 900 DEG C, once double tempering took out after 3 hours at tempering 2h and 500 DEG C, and Sintered NdFeB magnet operation completes.
By the Sintered NdFeB magnet that above operation is produced, after surface grinding, detect according to GB/T3217 permanent magnetism (Hard Magnetic) magnetism of material test method regulation, magnetic property is:
Remanent magnetism Br:13.913KGs
HCJ Hcj:14.91KOe
Coercivity H b:13.12KOe
Magnetic energy product BH (max): 46.63MGOe
HK/Hcj：0.98
Embodiment 11:
1, prepare burden: according to the composition batching shown in upper table one.
2, melting: after loading vacuum rapid hardening furnace after directly being mixed by formulation weight (see table one) requirement by various main body raw material (major phase material except M), when vacuum spun furnace is evacuated down to below 0.4Pa, start melting of heating, when in stove, material is rubescent, be filled with argon gas, and raise temperature, smelting temperature 1460 DEG C, until raw material melt completely, refining was congealed into after rejection tablet by 5 DEG C of water-cooled copper roller quick-coolings after 10 minutes, and be incubated 700 DEG C and obtain chilling slab in 20 minutes, chilling slab is stirred well to Homogeneous cooling in 5 DEG C of aqueous cold plates, thus obtain alloy casting piece.
3, hydrogen is broken: be positioned in hydrogen crushing furnace by master alloying rejection tablet, pass into hydrogen, and inhale completely until product and be warming up to 550 ~ 600 DEG C, 2 hours after hydrogen and carry out fragmentation, hydrogen flour material does not carry out dehydrogenation.
4, hydrogen flour material being put into oxygen content is that the high pure nitrogen shielding gas flow mill being less than 10ppm carries out powder process, controls powder particle mean size (laser particle analyzer) between 3 ~ 3.5 μm.
5, shaping: in aforementioned obtained powder, to add M element nano powder (composition is in table one) mix and blend 3 hours; the powder be stirred is weighed by predetermined weight; put into nitrogen protection and close press; control oxygen content 500 ~ 1000ppm; forming temperature 6 DEG C, orientation, compacting in 40mm air gap 1.8T magnetic field, the encapsulation of demagnetization final vacuum; again the green compact of Vacuum Package are carried out isostatic pressed 200Mpa, pressurize was taken out after 1 minute.
Corresponding alloy (see table one) arc process in the electrode assembly of argon shield is obtained nano-powder by being prepared as of M element nano powder, and nano-powder is of a size of 55nm.
6, sinter: green compact are first carried out preliminary dehydrogenation and removal of impurities in 1 hour 305 DEG C of insulations, then within 1 ~ 5 hour, removes rich neodymium phase hydrogen 470 DEG C of insulations; Again in nitrogen protection; load after oxygen content 0 ~ 500ppm glove box stripping oil in sintering basin; put into sintering furnace sintering; 8.7 hours are sintered under the sintering temperature of 1000 DEG C; on 950 DEG C, once double tempering is cooled to 80 DEG C of taking-ups after 5 hours at tempering 1h and 550 DEG C, and Sintered NdFeB magnet operation completes.
By the Sintered NdFeB magnet that above operation is produced, after surface grinding, detect according to GB/T3217 permanent magnetism (Hard Magnetic) magnetism of material test method regulation, magnetic property is:
Remanent magnetism Br:13.46KGs
HCJ Hcj:17.93KOe
Coercivity H b:12.82KOe
Magnetic energy product BH (max): 43.35MGOe
HK/Hcj：0.97
Embodiment 12:
1, prepare burden: according to the composition batching shown in upper table one.
2, melting: after loading vacuum rapid hardening furnace after directly being mixed by formulation weight requirement by formulation weight (see table one) by various main body raw material (major phase material except M), when vacuum spun furnace is evacuated down to below 0.4Pa, start melting of heating, when in stove, material is rubescent, be filled with argon gas, and raise temperature, smelting temperature 1470 DEG C, until raw material melt completely, refining was congealed into after rejection tablet by 33 DEG C of water-cooled copper roller quick-coolings after 10 minutes, and be incubated 650 DEG C and obtain chilling slab in 25 minutes, chilling slab is stirred well to Homogeneous cooling in 33 DEG C of aqueous cold plates, thus obtain alloy casting piece.
3, hydrogen is broken: be positioned in hydrogen crushing furnace by master alloying rejection tablet, pass into hydrogen, and inhale completely until product and be warming up to 550 ~ 600 DEG C, 2 hours after hydrogen and carry out fragmentation, hydrogen flour material does not carry out dehydrogenation.
4, powder being put into oxygen content is that the high pure nitrogen shielding gas flow mill being less than 10ppm carries out powder process, controls powder particle mean size (laser particle analyzer) between 2.5 ~ 3 μm.
5, shaping: in aforementioned obtained powder, to add M element nano powder (composition is in table one) stir 4 hours; the powder be stirred is weighed by predetermined weight; put into nitrogen protection and close press; control oxygen content 0 ~ 500ppm, forming temperature 34 DEG C, orientation in 40mm air gap 2T magnetic field; and then suppress; the encapsulation of demagnetization final vacuum, then the green compact of Vacuum Package are carried out isostatic pressed 200Mpa, pressurize was taken out after 2 minutes.
Corresponding alloy (see table one) arc process in nitrogen and helium mix protection (mixing mol ratio is 8:2 (nitrogen: the helium)) electrode assembly protected is obtained nano-powder by being prepared as of M element nano powder, and nano-powder is of a size of 35nm.
6, sinter: green compact are first carried out preliminary dehydrogenation and removal of impurities in 2 hours 275 DEG C of insulations, then within 1 ~ 5 hour, removes rich neodymium phase hydrogen 530 DEG C of insulations; Again in nitrogen protection; load in sintering basin after oxygen content 300ppm glove box stripping oil, put into sintering furnace sintering, under the sintering temperature of 1080 DEG C, sinter 9.3 hours; take out after 2 hours 850 DEG C of tempering 3h and 450 DEG C tempering, Sintered NdFeB magnet operation completes.
By the Sintered NdFeB magnet that above operation is produced, after surface grinding, detect according to GB/T3217 permanent magnetism (Hard Magnetic) magnetism of material test method regulation, magnetic property is:
Remanent magnetism Br:12.34KGs
HCJ Hcj:26.78KOe
Coercivity H b:12.05KOe
Magnetic energy product BH (max): 37.16MGOe
HK/Hcj：0.94
Embodiment 13:
1, prepare burden: according to the composition batching shown in upper table one.
2, melting: after loading vacuum rapid hardening furnace after directly being mixed by formulation weight requirement by formulation weight (see table one) by various main body raw material (major phase material except M), when vacuum spun furnace is evacuated down to below 0.4Pa, start melting of heating, when in stove, material is rubescent, be filled with argon gas, and raise temperature, smelting temperature 1470 DEG C, until raw material melt completely, refining was congealed into after rejection tablet by 17 DEG C of water-cooled copper roller quick-coolings after 10 minutes, and be incubated 900 DEG C and obtain chilling slab in 1 minute, chilling slab is stirred well to Homogeneous cooling in 17 DEG C of aqueous cold plates, thus obtain alloy casting piece.
3, hydrogen is broken: be positioned in hydrogen crushing furnace by master alloying rejection tablet, pass into hydrogen, and inhale completely until product and be warming up to 550 ~ 600 DEG C, 2 hours after hydrogen and carry out fragmentation, hydrogen flour material does not carry out dehydrogenation.
4, powder being put into oxygen content is that the high pure nitrogen shielding gas flow mill being less than 10ppm carries out powder process, controls powder particle mean size (laser particle analyzer) between 2.5 ~ 3 μm.
5, shaping: in aforementioned obtained powder, to add M element nano powder (composition is in table one) stir 4 hours; the powder be stirred is weighed by predetermined weight; put into nitrogen protection and close press; control oxygen content 0 ~ 500ppm, forming temperature 16 DEG C, orientation in 40mm air gap 2T magnetic field; and then suppress; the encapsulation of demagnetization final vacuum, then the green compact of Vacuum Package are carried out isostatic pressed 200Mpa, pressurize was taken out after 2 minutes.
Corresponding alloy (see table one) arc process in nitrogen and helium mix protection (mixing mol ratio is 8:2 (nitrogen: the helium)) electrode assembly protected is obtained nano-powder by being prepared as of M element nano powder, and nano-powder is of a size of 78nm.
6, sinter: green compact are first carried out preliminary dehydrogenation and removal of impurities in 2 hours 295 DEG C of insulations, then within 1 ~ 5 hour, removes rich neodymium phase hydrogen 525 DEG C of insulations; Again in nitrogen protection; load in sintering basin after oxygen content 300ppm glove box stripping oil, put into sintering furnace sintering, under the sintering temperature of 1080 DEG C, sinter 3.5 hours; take out after 2 hours 850 DEG C of tempering 3h and 450 DEG C tempering, Sintered NdFeB magnet operation completes.
By the Sintered NdFeB magnet that above operation is produced, after surface grinding, detect according to GB/T3217 permanent magnetism (Hard Magnetic) magnetism of material test method regulation, magnetic property is:
Remanent magnetism Br:12.34KGs
HCJ Hcj:26.78KOe
Coercivity H b:12.05KOe
Magnetic energy product BH (max): 37.16MGOe
HK/Hcj：0.94
Embodiment 14:
1, prepare burden: according to the composition batching shown in upper table one.
2, melting: after loading vacuum rapid hardening furnace after directly being mixed by formulation weight requirement by formulation weight (see table one) by various main body raw material (major phase material except M), when vacuum spun furnace is evacuated down to below 0.4Pa, start melting of heating, when in stove, material is rubescent, be filled with argon gas, and raise temperature, smelting temperature 1470 DEG C, until raw material melt completely, refining was congealed into after rejection tablet by 13 DEG C of water-cooled copper roller quick-coolings after 10 minutes, and be incubated 600 DEG C and obtain chilling slab in 30 minutes, chilling slab is stirred well to Homogeneous cooling in 20 DEG C of aqueous cold plates, thus obtain alloy casting piece.
3, hydrogen is broken: be positioned in hydrogen crushing furnace by master alloying rejection tablet, pass into hydrogen, and inhale completely until product and be warming up to 550 ~ 600 DEG C, 2 hours after hydrogen and carry out fragmentation, hydrogen flour material does not carry out dehydrogenation.
4, powder being put into oxygen content is that the high pure nitrogen shielding gas flow mill being less than 10ppm carries out powder process, controls powder particle mean size (laser particle analyzer) between 2.5 ~ 3 μm.
5, shaping: in aforementioned obtained powder, to add M element nano powder (composition is in table one) stir 4 hours; the powder be stirred is weighed by predetermined weight; put into nitrogen protection and close press; control oxygen content 0 ~ 500ppm, forming temperature 31 DEG C, orientation in 40mm air gap 2T magnetic field; and then suppress; the encapsulation of demagnetization final vacuum, then the green compact of Vacuum Package are carried out isostatic pressed 200Mpa, pressurize was taken out after 2 minutes.
Corresponding alloy (see table one) arc process in nitrogen and helium mix protection (mixing mol ratio is 8:2 (nitrogen: the helium)) electrode assembly protected is obtained nano-powder by being prepared as of M element nano powder, and nano-powder is of a size of 65nm.
6, sinter: green compact are first carried out preliminary dehydrogenation and removal of impurities in 2 hours 295 DEG C of insulations, then within 1 ~ 5 hour, removes rich neodymium phase hydrogen 480 DEG C of insulations; Again in nitrogen protection; load in sintering basin after oxygen content 300ppm glove box stripping oil, put into sintering furnace sintering, under the sintering temperature of 1080 DEG C, sinter 6.7 hours; take out after 2 hours 850 DEG C of tempering 3h and 450 DEG C tempering, Sintered NdFeB magnet operation completes.
By the Sintered NdFeB magnet that above operation is produced, after surface grinding, detect according to GB/T3217 permanent magnetism (Hard Magnetic) magnetism of material test method regulation, magnetic property is:
Remanent magnetism Br:12.34KGs
HCJ Hcj:26.78KOe
Coercivity H b:12.05KOe
Magnetic energy product BH (max): 37.16MGOe
HK/Hcj：0.94
Rare earth magnet disclosed by the invention has lower oxygen content, has good crystal boundary structure and average crystal grain simultaneously.Magnet can obtain the HCJ of higher than common process about 10%, thus reduces the use amount of heavy rare earth dysprosium terbium etc., and protium is departed from substantially, oxygen content is balanced inside and outside magnet, and the machinability of magnet itself is good, and qualification rate is high.
In view of the present invention program's embodiment is numerous, each embodiment experimental data is huge numerous, be not suitable for particularize explanation herein, but the content of the required checking of each embodiment is all close with the final conclusion obtained, so do not illustrate one by one the checking content of each embodiment, only with embodiment 6, the excellent part of the present patent application is representatively described herein.
The non-limit part of technical scope midrange that this place embodiment is protected application claims, equally all in the scope of protection of present invention.
Technological means disclosed in the present invention program is not limited only to the technological means disclosed in above-mentioned technological means, also comprises the technical scheme be made up of above technical characteristic combination in any.The above is the specific embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications are also considered as protection scope of the present invention.
Claims (10)
1. a rare earth permanent-magnetic material, is characterized in that: mainly consisting of (by weight percentage, wt%) of described rare earth permanent-magnetic material, PrNd 28-35%; In Dy or Tb, one or both add up to 0-5%; B 1.0%; M 0.01-10%, surplus is Fe, and wherein M element is one or more in titanium, tin, zirconium, copper, cobalt, niobium, aluminium, manganese, gallium, chromium, nickel, zinc, magnesium, and when copper, cobalt, niobium, aluminium exist, Co 0-3%; Al 0.2-1.5%; Nb 0-0.5%; Cu 0-0.2%.
2. rare earth permanent-magnetic material according to claim 1; it is characterized in that: described M element is for add by nano-powder; described nano-powder is in one or both electrode assemblies protected in nitrogen or argon gas, the powder of size 10 ~ 100 nanometer adopting arc process to prepare.
3. rare earth permanent-magnetic material according to claim 1, is characterized in that: described rare earth permanent-magnetic material is average grain size is 2.5 ~ 3.5 μm, and smallest particles >=1 μm, the largest particles≤20 μm.
4. rare earth permanent-magnetic material according to claim 1, is characterized in that: described rare earth permanent-magnetic material rare earth elements Pr, Nd, Dy, Tb total amount proportion is 29-35%.
5. a preparation method for rare earth permanent-magnetic material as claimed in claim 1, is characterized in that: a, be configured at high melt in vacuum rapid hardening furnace according to the aforementioned various raw material by rare earth permanent-magnetic material; The alloy liquid that b, step a melting obtain obtains chilling slab by 0 ~ 35 DEG C of water-cooled copper roller quick-cooling, and chilling slab is stirred well to Homogeneous cooling and obtains alloy casting piece in aqueous cold plate; The alloy casting piece that c, step b obtain is through hydrogen fragmentation, airflow milling, compression molding, magnetization, demagnetization, vacuum packaging, isostatic pressed compacting, vacuum-sintering and reprocessing thus obtain finished product.
6. the preparation method of rare earth permanent-magnetic material according to claim 5, it is characterized in that: in described step c, vacuum-sintering also comprises dehydrogenating technology, described dehydrogenating technology comprises step I, the magnet after isostatic pressed compacting is carried out preliminary dehydrogenation and removal of impurities in 1 ~ 3 hour 250 ~ 350 DEG C of insulations; The magnet of step II, tentatively dehydrogenation and removal of impurities removes rich neodymium phase hydrogen for 1 ~ 5 hour 450 ~ 600 DEG C of insulations.
7. the preparation method of rare earth permanent-magnetic material according to claim 5, it is characterized in that: in described step c, post-processing step is after high temperature 1000 ~ 1080 DEG C sinters 1 ~ 10 hour, cooling and sequentially through the tempering of 1 ~ 3 hour when 850 ~ 950 DEG C, is cooled to less than 80 DEG C after the double tempering of 2 ~ 5 hours when 450 ~ 550 DEG C and comes out of the stove.
8. the preparation method of rare earth permanent-magnetic material according to claim 5, is characterized in that: in described step b, chilling slab is for being congeal into after rejection tablet in 0 ~ 35 DEG C of water-cooled copper roller rapidly in temperature, and is incubated 600 ~ 900 DEG C and obtains for 1 ~ 30 minute.
9. the preparation method of rare earth permanent-magnetic material according to claim 5, is characterized in that: in described step c, magnetized field strength is greater than 1.5T, and forming temperature is between 0 ~ 37 DEG C.
10. the preparation method of rare earth permanent-magnetic material according to claim 5, it is characterized in that: in described step c after vacuum-sintering the oxygen content of magnet at 200 ~ 1200ppm, hydrogen content is at 1 ~ 100ppm, and wherein the difference of the inside and outside oxygen content of single magnet is less than 500ppm.
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN105161240A (en) * | 2015-10-13 | 2015-12-16 | 南通长江电器实业有限公司 | High-performance rare earth permanent magnet material |
| CN107134337A (en) * | 2017-04-05 | 2017-09-05 | 东莞市嘉达磁电制品有限公司 | A kind of plus Tb does N45H NdFeB material formula |
| CN107424822A (en) * | 2016-05-23 | 2017-12-01 | 现代自动车株式会社 | The method of rare earth permanent magnets of the manufacture with excellent magnetic property |
| EP3261101A1 (en) * | 2016-06-22 | 2017-12-27 | Yantai Shougang Magnetic Materials Inc. | A sintered nd-fe-b magnet and manufacturing method thereof |
| CN107610860A (en) * | 2017-09-20 | 2018-01-19 | 北京工业大学 | A kind of method that centreless mill processing neodymium iron boron greasy filth waste material prepares recycled sinter magnet |
| CN108352233A (en) * | 2015-09-28 | 2018-07-31 | 厦门钨业股份有限公司 | A kind of compound R-Fe-B systems rare-earth sintered magnet containing Pr and W |
| CN108389674A (en) * | 2017-02-02 | 2018-08-10 | 日立金属株式会社 | R-T-B systems sintered magnet |
| CN108538531A (en) * | 2017-11-16 | 2018-09-14 | 赣州富尔特电子股份有限公司 | A kind of permanent magnetic steel and preparation method thereof for magnetic latching relay |
| CN108831650A (en) * | 2018-06-21 | 2018-11-16 | 宁波可可磁业股份有限公司 | A kind of neodymium iron boron magnetic body and preparation method thereof |
| CN108907203A (en) * | 2018-05-21 | 2018-11-30 | 中国计量大学 | A kind of heat treatment method improving neodymium iron boron blank intrinsic coercivity consistency |
| CN108998674A (en) * | 2018-08-17 | 2018-12-14 | 杭州红山磁性材料有限公司 | A kind of method that alnico waste recovery recycles |
| CN110150806A (en) * | 2018-11-22 | 2019-08-23 | 毛爱波 | A kind of dilute crystal ear pendant and its processing technology |
| CN111968813A (en) * | 2020-07-10 | 2020-11-20 | 瑞声科技（南京）有限公司 | NdFeB system magnetic powder, NdFeB system sintered magnet and preparation method |
| CN112216499A (en) * | 2020-08-25 | 2021-01-12 | 宁波同创强磁材料有限公司 | Preparation method of antioxidant sintered neodymium-iron-boron magnet |
| CN112331468A (en) * | 2020-10-14 | 2021-02-05 | 宁波韵升股份有限公司 | Preparation method of high-remanence sintered neodymium-iron-boron magnet |
| CN115007857A (en) * | 2022-06-09 | 2022-09-06 | 宁波中杭磁材有限公司 | Magnetic steel for hybrid excitation synchronous motor and preparation method thereof |
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| CN104966606A (en) * | 2015-06-18 | 2015-10-07 | 安徽大地熊新材料股份有限公司 | Preparation for low-weightlessness rare earth-iron-boron magnetic body |
| CN108352233A (en) * | 2015-09-28 | 2018-07-31 | 厦门钨业股份有限公司 | A kind of compound R-Fe-B systems rare-earth sintered magnet containing Pr and W |
| CN108352233B (en) * | 2015-09-28 | 2020-09-18 | 厦门钨业股份有限公司 | R-Fe-B rare earth sintered magnet compositely containing Pr and W |
| CN105161240A (en) * | 2015-10-13 | 2015-12-16 | 南通长江电器实业有限公司 | High-performance rare earth permanent magnet material |
| CN107424822A (en) * | 2016-05-23 | 2017-12-01 | 现代自动车株式会社 | The method of rare earth permanent magnets of the manufacture with excellent magnetic property |
| US10978226B2 (en) | 2016-06-22 | 2021-04-13 | Yantai Shougang Magnetic Materials Inc. | Sintered Nd—Fe—B magnet composition and a production method for the sintered Nd—Fe—B magnet |
| EP3261101A1 (en) * | 2016-06-22 | 2017-12-27 | Yantai Shougang Magnetic Materials Inc. | A sintered nd-fe-b magnet and manufacturing method thereof |
| CN108389674A (en) * | 2017-02-02 | 2018-08-10 | 日立金属株式会社 | R-T-B systems sintered magnet |
| CN108389674B (en) * | 2017-02-02 | 2021-07-23 | 日立金属株式会社 | R-T-B sintered magnet |
| CN107134337A (en) * | 2017-04-05 | 2017-09-05 | 东莞市嘉达磁电制品有限公司 | A kind of plus Tb does N45H NdFeB material formula |
| CN107610860A (en) * | 2017-09-20 | 2018-01-19 | 北京工业大学 | A kind of method that centreless mill processing neodymium iron boron greasy filth waste material prepares recycled sinter magnet |
| CN108538531A (en) * | 2017-11-16 | 2018-09-14 | 赣州富尔特电子股份有限公司 | A kind of permanent magnetic steel and preparation method thereof for magnetic latching relay |
| CN108907203A (en) * | 2018-05-21 | 2018-11-30 | 中国计量大学 | A kind of heat treatment method improving neodymium iron boron blank intrinsic coercivity consistency |
| CN108831650B (en) * | 2018-06-21 | 2020-10-23 | 宁波可可磁业股份有限公司 | Neodymium-iron-boron magnet and preparation method thereof |
| CN108831650A (en) * | 2018-06-21 | 2018-11-16 | 宁波可可磁业股份有限公司 | A kind of neodymium iron boron magnetic body and preparation method thereof |
| CN108998674A (en) * | 2018-08-17 | 2018-12-14 | 杭州红山磁性材料有限公司 | A kind of method that alnico waste recovery recycles |
| CN110150806A (en) * | 2018-11-22 | 2019-08-23 | 毛爱波 | A kind of dilute crystal ear pendant and its processing technology |
| CN111968813A (en) * | 2020-07-10 | 2020-11-20 | 瑞声科技（南京）有限公司 | NdFeB system magnetic powder, NdFeB system sintered magnet and preparation method |
| WO2022006973A1 (en) * | 2020-07-10 | 2022-01-13 | 瑞声声学科技(深圳)有限公司 | Ndfeb magnetic powder, ndfeb sintered magnet and preparation method therefor |
| CN111968813B (en) * | 2020-07-10 | 2023-11-07 | 瑞声科技（南京）有限公司 | NdFeB-based magnetic powder, ndFeB-based sintered magnet, and method for producing same |
| CN112216499A (en) * | 2020-08-25 | 2021-01-12 | 宁波同创强磁材料有限公司 | Preparation method of antioxidant sintered neodymium-iron-boron magnet |
| CN112331468A (en) * | 2020-10-14 | 2021-02-05 | 宁波韵升股份有限公司 | Preparation method of high-remanence sintered neodymium-iron-boron magnet |
| CN115007857A (en) * | 2022-06-09 | 2022-09-06 | 宁波中杭磁材有限公司 | Magnetic steel for hybrid excitation synchronous motor and preparation method thereof |
| CN115007857B (en) * | 2022-06-09 | 2024-04-30 | 宁波中杭磁材有限公司 | Magnetic steel for hybrid excitation synchronous motor and preparation method thereof |
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