CN104157386A - N52 and 48M sintered neodyminum iron boron permanent magnet and production method thereof - Google Patents
N52 and 48M sintered neodyminum iron boron permanent magnet and production method thereof Download PDFInfo
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Abstract
The invention relates to the field of rare-earth permanent magnetic materials, in particular to a sintered neodyminum iron boron permanent magnet and a production method thereof. The N53 and 48M sintered neodyminum iron boron permanent magnet which is low in cost and high in energy production is produced by components including, by weight, 29.5-30.5wt% of PrNd, 0.1-0.5wt% of AL, 0.05-0.25wt% of Cmu, 0.1-0.3wt% of Nb, 0.05-0.1wt% of Zr, 0.1-0.2wt% of Ga, 0.5-1.5wt% of Co, 0.96-1.02wt% of B and the balance of Fe. The components and process parameters are optimized, so that the components for stable production of N52 and 48M dysprosium free magnet are produced. The N52 and 48M sintered neodyminum iron boron permanent magnet and production method thereof have the advantages that power size in moderate with no need of adding gasoline or solvent for powder protection, sintering time is short, and production cost is low; the magnet is free of heavy rare earth such as dysprosium and terbium, ingredient cost of the magnet is low; a blank is moderate in grain size, post processing efficiency of the blank is high, finished-product acceptability is high, and mass production is allowed; the production process is simple, and production cycle is short.
Description
Technical field
The invention belongs to rare earth permanent-magnetic material field, relate generally to low-cost N52 and 48M sintered Nd-Fe-B permanent magnet and preparation method thereof.
Background technology
High Energy Product magnet can device miniaturization, lightweight, is widely used in the fields such as computer, communication.Heavy rare earth dysprosium can effectively improve the coercive force of Sintered NdFeB magnet, reduce the working point of magnet, the miniaturization of device is achieved, yet heavy rare earth dysprosium is expensive, how to develop a kind ofly becomes without dysprosium and the coercitive sintered Nd-Fe-B permanent magnet that can improve Sintered NdFeB magnet the focus that everybody pays close attention to.
In order to improve the coercive force of Sintered NdFeB magnet, conventionally to reduce the granularity of powder, thereby reduce sintering blank crystallite dimension, reach and improve coercitive object.The patent that application Ren Wei Hitachi Metal Co., Ltd., publication number are CN101981634A is less than 3 microns of powder D50 and is placed in isoparaffin equal solvent, forms slurry, and then moulding, then vacuum-sintering, produce 4 microns of sintered magnets of crystallite dimension.Due to the long-time vacuum degreasing of needs, so complex process, production cycle longly, difficult are controlled, difficult batch production.And blank crystallite dimension is less, the difficulty of processing thereafter punching, trepanning, section is larger, has reduced the production efficiency of following process.Therefore how can high efficiency, technique batch production sintered Nd-Fe-B permanent magnet simple, with short production cycle becomes research purpose.
Summary of the invention
For the weak point existing in the problems referred to above, the invention provides a kind of production technology simple, with short production cycle, can realize low-cost N52 and the 48M sintered Nd-Fe-B permanent magnet of batch production.
For achieving the above object, the invention provides a kind of low-cost N52 and 48M sintered Nd-Fe-B permanent magnet, consist of the following composition: consist of the following composition: PrNd:29.5-30.5wt%, Al:0.1-0.5wt%, Cu:0.05-0.25wt%, Nb:0.1-0.3wt%, Zr:0.05-0.1wt%, Ga:0.1-0.2wt%, Co:0.5-1.5wt%, P:0.96-1.02%, Fe surplus.
Preferably, described praseodymium didymium content 25%, purity is more than 99.5%.
Preferably, described pure iron is the Armco iron below carbon content 50ppm.
Preferably, described ferro-boron is the more than 20% aluminothermic process ferro-boron of boron content.
Preferably, described N52 and 48M sintered Nd-Fe-B permanent magnet oxygen content are less than 1200ppm.
A preparation method for N52 as above and 48M sintered Nd-Fe-B permanent magnet, comprises the steps:
1. prepare burden: raw material are weighed to scale;
2. alloy preparation: raw material pack successively crucible into by fusing point height and put into rapid hardening furnace, rapid hardening furnace is evacuated to vacuum degree to be less than after 5Pa, at 500-600 ℃ of bake out 10-15min, refining after filling with inert gas is heated to 1450-1550 ℃ under the maximum power of rapid hardening furnace, after making the molten clear molten steel of raw material evenly, cast, obtain slab;
3. meal preparation: slab in hydrogenation furnace, inhale hydrogen saturated after, 500-600 ℃ of dehydrogenation, to 30Pa, obtains meal;
4. fine powder preparation: add 0.1% following lubricant in meal, wear into the powder that D50 is 5.0-5.5 micron in airflow milling;
5. moulding: under inert gas shielding, the die for molding that powder is greater than 1.8 teslas in magnetic field of press intensity obtains blank, compact density is 3.8-4.2g/cm
3;
6. improve density: Vacuum Package blank further improves density with static pressure such as grade to blank under 180-200MPa pressure;
7. sintering and tempering: the blank improving after density is removed inner membrance in inert gas shielding case, moves into vacuum sintering furnace and carries out degasification, is then raised to 1040-1065 ℃ of insulation and within 4-6 hour, carries out densification sintering; Sintering finishes rear filling with inert gas and is cooled to below 100 ℃, be warmed up to 880-920 ℃ of insulation and within 2-3 hour, carry out first order tempering, insulation finishes rear filling with inert gas and is cooled to 100 ℃, be warming up to 470-500 ℃ of insulation and within 4-5 hour, carry out second level tempering, insulation finishes rear filling with inert gas and is cooled to 100 ℃ and comes out of the stove below.
Preferably, in step, also comprise before 1. corresponding raw material is eliminated rust, cuts off processing.
Preferably, step 2. in slab thickness 0.1-0.4mm.
Preferably, step 5. in compact density 4.0g/cm
3.
Preferably, described inert gas is argon gas.
Beneficial effect of the present invention is:
1, particle size is moderate, without adding gasoline or solvent, carries out powder protection, and the sintering desaeration time is short, and manufacturing expense is low.
2, in magnet, do not contain the heavy rare earth such as dysprosium terbium, magnet batching cost is low.
3, blank crystallite dimension is moderate, and after blank, working (machining) efficiency is high, and product qualified rate is high, is applicable to producing in enormous quantities.
4, production technology is simple, with short production cycle.
Accompanying drawing explanation
Fig. 1 is preparation method's process chart.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is further explained.
Embodiment 1:
Step 101: batching: raw material are weighed to scale, PrNd:29.6wt% specific as follows, Al:0.2wt%, Ga:0.1wt%, Cu:0.1wt%, Co:0.5wt%, B:1.0wt%, Nb:0.15wt%, Zr:0.05wt%, Fe surplus;
Step 102: alloy preparation: raw material pack successively crucible into by fusing point height and put into rapid hardening furnace, rapid hardening furnace is evacuated to after vacuum degree 3.2Pa, at 550 ℃ of bake out 15min, filling with inert gas is 1500 ℃ of refinings under the maximum power of rapid hardening furnace, the evenly rear casting of the molten clear molten steel of raw material, obtain slab, described slab thickness 0.3mm;
Step 103: meal preparation: slab in hydrogenation furnace, inhale hydrogen saturated after, 550 ℃ of dehydrogenations, to 20Pa, obtain meal;
Step 104: fine powder preparation: add 0.1% lubricant in meal, wear into D50 and be the powder of 5.2 microns in airflow milling;
Step 105: moulding: under inert gas shielding, powder obtains blank in the die for molding of magnetic field of press intensity 2 teslas;
Step 106: improve density: Vacuum Package blank is with waiting static pressure further to improve density to blank under 200MPa pressure, and after improving, density is 4.5g/cm
3;
Step 1071: sintering and tempering: the blank improving after density is removed inner membrance in inert gas shielding case, moves into vacuum sintering furnace and carries out degasification, is then raised to 1060 ℃ of insulations and within 6 hours, carries out densification sintering;
Step 1072: sintering finishes rear filling with inert gas and is cooled to 80 ℃, is warmed up to 900 ℃ of insulations and within 2.5 hours, carries out first order tempering;
Step 1073: insulation finishes rear filling with inert gas and is cooled to 100 ℃, is warming up to 480 ℃ of insulations and within 4 hours, carries out second level tempering, and insulation finishes rear filling with inert gas and is cooled to 80 ℃ and comes out of the stove below.
Comparative example 1:
Raw material are weighed according to following provisions ratio: PrNd:29.3wt%, Dy:0.5wt%, Al:0.1wt%, Ga:0.1wt%, Cu:0.1wt%, Co:1.0wt%, B:1wt%, Nb:0.1wt%, Fe surplus, step 102-106 is with embodiment 1;
Step 1071: sintering and tempering: the blank improving after density is removed inner membrance in inert gas shielding case, moves into vacuum sintering furnace and carries out degasification, is then raised to 1058 ℃ of insulations and within 5 hours, carries out densification sintering;
Step 1072-1073 is with embodiment 1.
The prepared N52 sintered Nd-Fe-B permanent magnet performance of N52 sintered Nd-Fe-B permanent magnet prepared by method described in embodiment 1 and comparative example 1 is measured with magnetic property measuring instrument, and its performance is as follows:
| Classification | Br(kGs) | Hcj(kOe) | (BH)max(MGOe) | Hk(kOe) |
| Embodiment 1 | 14.41 | 12.3 | 50.2 | 11.9 |
| Comparative example 1 | 14.4 | 12.5 | 50.1 | 11.8 |
As can be seen from the table above, the N52 magnet performance of its magnetic property of N52 magnet of preparing by the present embodiment 1 method and comparative example 1 preparation is suitable, can meet N52 performance index, but embodiment 1 formula does not have heavy metal Dy, formulation cost is low, illustrates by optimizing component and can remove Dy element.
Embodiment 2:
Step 101: batching: raw material are weighed to scale, specific as follows: PrNd:30.5wt%, Al:0.4wt%, Ga:0.2wt%, Cu:0.2wt%, Co:0.5wt%, B:1.0wt%, Nb:0.2wt%, Zr:0.05wt%, Fe surplus;
Step 102: alloy preparation: raw material pack successively crucible into by fusing point height and put into rapid hardening furnace, rapid hardening furnace is evacuated to after vacuum degree 2Pa, at 600 ℃ of bake out 15min, filling with inert gas heats under the maximum power of rapid hardening furnace, 1550 ℃ of refinings, the evenly rear casting of the molten clear molten steel of raw material, obtains slab, described slab thickness 0.32mm;
Step 103: meal preparation: slab in hydrogenation furnace, inhale hydrogen saturated after, 550 ℃ of dehydrogenations, to 20Pa, obtain meal;
Step 104: fine powder preparation: add 0.08% lubricant in meal, wear into particle mean size and be the powder of 5.4 microns in airflow milling;
Step 105: moulding: under inert gas shielding, powder obtains blank in the die for molding of magnetic field of press intensity 1.9 teslas;
Step 106: improve density: Vacuum Package blank is with waiting static pressure further to improve density to blank under 200MPa pressure, and after improving, density is 4.5g/cm
3;
Step 1071: sintering and tempering: the blank improving after density is removed inner membrance in inert gas shielding case, moves into vacuum sintering furnace and carries out degasification, is then raised to 1065 ℃ of insulations and within 6 hours, carries out densification sintering;
Step 1072: sintering finishes rear filling with inert gas and is cooled to 80 ℃, is warmed up to 900 ℃ of insulations and within 2.5 hours, carries out first order tempering;
Step 1073: insulation finishes rear filling with inert gas and is cooled to 100 ℃, is warming up to 480 ℃ of insulations and within 4 hours, carries out second level tempering, and insulation finishes rear filling with inert gas and is cooled to normal temperature and comes out of the stove.
Comparative example 2:
Raw material are weighed according to following provisions ratio: PrNd:29.7wt%, Dy:0.8wt%, Al:0.2wt%, Ga:0.1wt%, Cu:0.1wt%, Co:1.0wt%, B:1wt%, Nb:0.2wt%, Fe surplus, step 102-106 is identical with embodiment 2;
Step 1071: sintering and tempering: the blank improving after density is removed inner membrance in inert gas shielding case, moves into vacuum sintering furnace and carries out degasification, is then raised to 1057 ℃ of insulations and within 5 hours, carries out densification sintering;
Step 1072: sintering finishes rear filling with inert gas and is cooled to 80 ℃, is warmed up to 900 ℃ of insulations and within 2.5 hours, carries out first order tempering;
Step 1073: insulation finishes rear filling with inert gas and is cooled to 100 ℃, is warming up to 500 ℃ of insulations and within 4 hours, carries out second level tempering, and insulation finishes rear filling with inert gas and is cooled to normal temperature and comes out of the stove.
The prepared 48M sintered Nd-Fe-B permanent magnet performance of 48M sintered Nd-Fe-B permanent magnet prepared by method described in embodiment 2 and comparative example 1 is measured with magnetic property measuring instrument, and its performance is as follows:
| Classification | Br(kGs) | Hcj(kOe) | (BH)max(MGOe) | Hk(kOe) |
| Embodiment 2 | 13.95 | 14.6 | 47.5 | 14.3 |
| Comparative example 2 | 13.9 | 15 | 47.2 | 14.5 |
As can be seen from the table above, its performance of 48M sintered Nd-Fe-B permanent magnet of preparing by the present embodiment 2 methods is equally matched with comparative example 2 performances, can meet 48M performance index, but embodiment 2 uses 0.8wt%Dy less compared with embodiment 1, formulation cost is low, has improved the market competitiveness; Because particle size is controlled at normal range (NR), there is no the production efficiency of processing punching, trepanning, section after reducing simultaneously.
Only as described above, be only preferred embodiment of the present invention, such as professional who are familiar with this art.After understanding technological means of the present invention, natural energy, according to actual needs, is changed under instruction of the present invention.Therefore all equal variation and modifications of doing according to the present patent application the scope of the claims, all should still remain within the scope of the patent.
Claims (8)
1. a N52 and 48M sintered Nd-Fe-B permanent magnet, it is characterized in that: consist of the following composition: PrNd:29.5-30.5wt%, Al:0.1-0.5wt%, Cu:0.05-0.25wt%, Nb:0.1-0.3wt%, Zr:0.05-0.1wt%, Ga:0.1-0.2wt%, Co:0.5-1.5wt%, B:0.96-1.02%, Fe surplus.
2. N52 as claimed in claim 1 and 48M sintered Nd-Fe-B permanent magnet, is characterized in that: described praseodymium neodymium metal is Pr25Nd75, and purity is more than 99.5%.
3. N52 as claimed in claim 1 and 48M sintered Nd-Fe-B permanent magnet, is characterized in that: described pure iron is the Armco iron below carbon content 50ppm.
4. N52 as claimed in claim 1 and 48M sintered Nd-Fe-B permanent magnet, is characterized in that: described boron element adds with ferro-boron state, and ferro-boron is the more than 20% aluminothermic process ferro-boron of boron content.
5. N52 as claimed in claim 1 and 48M sintered Nd-Fe-B permanent magnet, is characterized in that: described N52 and 48M sintered Nd-Fe-B permanent magnet oxygen content are less than 1200ppm.
6. the as above arbitrarily N52 described in claim and a preparation method for 48M sintered Nd-Fe-B permanent magnet, is characterized in that comprising the steps:
1. prepare burden: raw material are weighed to scale;
2. alloy preparation: raw material pack successively crucible into by fusing point height and put into rapid hardening furnace, rapid hardening furnace is evacuated to vacuum degree to be less than after 5Pa, at 500-600 ℃ of bake out 10-15min, refining after filling with inert gas is heated to 1450-1550 ℃ under the maximum power of rapid hardening furnace, after making the molten clear molten steel of raw material evenly, cast, obtain slab;
3. meal preparation: slab in hydrogenation furnace, inhale hydrogen saturated after, 500-600 ℃ of dehydrogenation, to 30Pa, obtains meal;
4. fine powder preparation: add 0.1% following lubricant in meal, wear into the powder that D50 is 5.0-5.5 micron in airflow milling;
5. moulding: under inert gas shielding, the die for molding that powder is greater than 1.8 teslas in magnetic field of press intensity obtains blank;
6. improve density: Vacuum Package blank further improves density with static pressure such as grade to blank under 180-200MPa pressure;
7. sintering and tempering: the blank improving after density is removed inner membrance in inert gas shielding case, moves into vacuum sintering furnace and carries out degasification, is then raised to 1040-1065 ℃ of insulation and within 4-6 hour, carries out densification sintering; Sintering finishes rear filling with inert gas and is cooled to below 100 ℃, be warmed up to 880-920 ℃ of insulation and within 2-3 hour, carry out first order tempering, insulation finishes rear filling with inert gas and is cooled to 100 ℃, be warming up to 470-500 ℃ of insulation and within 4-5 hour, carry out second level tempering, insulation finishes rear filling with inert gas and is cooled to 100 ℃ and comes out of the stove below.
7. the preparation method of low-cost N52 as claimed in claim 6 and 48M sintered Nd-Fe-B permanent magnet, is characterized in that: step is middle slab thickness 0.1-0.4mm 2..
8. the preparation method of low-cost N52 as claimed in claim 6 and 48M sintered Nd-Fe-B permanent magnet, is characterized in that: described inert gas is argon gas or nitrogen.
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| CN105741995B (en) * | 2016-04-27 | 2017-07-28 | 宁波耐力誉磁业科技有限公司 | A kind of high performance sintered neodymium-iron-boron permanent magnet and preparation method thereof |
| CN107240470A (en) * | 2017-07-12 | 2017-10-10 | 浙江中科磁业有限公司 | A kind of low weightless Sintered NdFeB magnet and preparation method |
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| CN113903590A (en) * | 2021-11-10 | 2022-01-07 | 赣州市钜磁科技有限公司 | Resource-saving 48H neodymium-iron-boron permanent magnet material preparation process |
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Address after: 226600, Donghai Avenue (middle) No. 18, Haian County, Nantong, Jiangsu Applicant after: Jiangsu Channelon Electronic Group Co., Ltd. Address before: The East Avenue East of the town of Haian County in Jiangsu city of Nantong province (226600 in 18) Applicant before: Jiangsu Channelon Electronic Group Co., Ltd. |
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Address after: The East Avenue East of the town of Haian County in Jiangsu city of Nantong province (226600 in 18) Applicant after: Jiangsu Channelon Electronic Group Co., Ltd. Address before: 226600, Donghai Avenue (middle) No. 18, Haian County, Nantong, Jiangsu Applicant before: Jiangsu Channelon Electronic Group Co., Ltd. |
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Application publication date: 20141119 |
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| RJ01 | Rejection of invention patent application after publication |