CN104124052A - Preparation method for high-performance rare earth-iron-boron sintered permanent magnet - Google Patents
Preparation method for high-performance rare earth-iron-boron sintered permanent magnet Download PDFInfo
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- CN104124052A CN104124052A CN201410356472.0A CN201410356472A CN104124052A CN 104124052 A CN104124052 A CN 104124052A CN 201410356472 A CN201410356472 A CN 201410356472A CN 104124052 A CN104124052 A CN 104124052A
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Abstract
The invention discloses a preparation method for a high-performance rare earth-iron-boron sintered permanent magnet. The method includes the steps that (1) hydrogen absorption is carried out on neodymium iron boron alloy for breaking, and powder is prepared in a jet milling mode; (2) light rare earth elements are sputtered to the magnetic powder in a magnetron sputtering mode; (3) orientation forming is conducted to obtain a compact, and isostatic cool pressing processing is carried out on the compact; (4) vacuum sintering two-stage tempering treatment is conducted on the processed compact. On the basis that Nd-Fe-B alloy powder is prepared, the magnetron sputtering method is used for sputtering the light rare earth elements to the surface of the jet milling micro powder, the light rare earth elements serve as intergranular liquid phases to repair damaged grain boundary edges, grain boundaries are smoother, and the magnet has better magnetic performance because of optimization of the structure of the grain boundaries. The grain boundary light rare earth element liquid phases are evenly distributed and wrap a principal phase and play a role in exchange coupling removal, the influences of uneven distribution of dual-alloyage RE-rich phases in the grain boundary are overcome, and coercivity is improved.
Description
Technical field
The preparation method who the invention provides a kind of rare-earth-iron-boron series high-performance sintered permanent magnet, belongs to field of magnetic material.
Background technology
Sintering rare-earth-iron-boron (Re-Fe-B) is that sintered permanent magnet (neodymium iron boron Nd-Fe-B is its Typical Representative) is the best permanent magnetic material of current magnetic property, there is high remanent magnetism (Br), high-coercive force (Hcj), high energy product (BH) max feature, be the Core Feature device of the high-technology fields such as computer, information industry, traffic, become the important substance basis of new and high technology, new industry.Manufacturing high-performance magnet, is first the rare-earth-iron-boron principal phase in composition with high-volume fractional, is secondly that the rich rare-earth phase between crystal boundary evenly fully distributes, and has good intergranular structure.At present, the basic skills of research and development high-performance magnet is: melting high-volume fractional Nd Fe B alloys composition, and during powder process, add rich rare-earth phase and enter crystal boundary, improve grain boundary structure.Two alloyages are to prepare at present the common method of high-performance magnet: (master alloying composition has high-volume fractional to the major-minor alloy of melting respectively, auxiliary alloying component is rich rare-earth phase substantially), master alloying is pulverized rear and auxiliary alloy liquid phase (liquid phase has micron order and nano-grade size) batch mixing sintering, change by major-minor alloying component, proportioning realizes the modification to main-phase alloy particle crystal boundary, as " the increasing sintering Nd-Fe-B coercive force by adding nano-oxide in crystal boundary phase method " of Chinese patent 200510049962.7 propositions.Auxiliary mutually rich rare-earth phase, particularly nano level rich rare earth liquid phase that two alloyages are added, by rotating or the mechanical system such as rolling is mixed with main-phase alloy composition, there is reunion quadrant in rich rare-earth phase, and what in micro mist, distribute is inhomogeneous.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of performance Nd Fe B sintered magnet.
In order to realize foregoing invention object, adopt following technical proposals:
High-performance rare-earth-iron-boron is a preparation method for sintered permanent magnet, comprises the steps:
1., get Nd Fe B alloys, in hydrogen crushing furnace, inhale hydrogen fragmentation, high-temperature dehydrogenation and process, in hydrogen flour, add sintered Nd-Fe-B permanent magnet to prepare conventional auxiliary agent, at nitrogen or argon gas atmosphere lower seal, mix, then make magnetic through airflow milling powder;
2., the mixed magnetic of airflow milling is placed on the rolling sample stage of magnetron sputtering, with one or more the alloy in light rare earth element, do target, in argon gas atmosphere, light rare earth element in target is splashed on sample stage on the magnetic with gravity fall, obtains the neodymium iron boron powder that surface sputtering has light rare earth element;
3., above-mentioned neodymium iron boron powder oriented moulding in alignment magnetic field is obtained to pressed compact, pressed compact is processed through isostatic cool pressing again;
4., the pressed compact of isostatic cool pressing after processing be through vacuum-sintering, two-stage temper, makes magnet.
Described light rare earth element comprises praseodymium Pr, neodymium Nd, lanthanum La, cerium Ce.
Further, step 1. 520-580 ℃ of hydrogen crushing furnace high-temperature dehydrogenation treatment temperature be good.
As preferably, 1. step makes magnetic particle mean size is 2-7 μ m.
Further, step 2. light rare earth element sputtering layer thickness at 10-50nm, preferred 15-40 nm.
Further, 3. alignment magnetic field 1.0-2.0T of step.
As preferably, step 3. isostatic cool pressing processing pressure is 150-200MPa.
Further, step is vacuum-sintering 4-6 hour at 1030 ℃-1130 ℃ 4., and 2-4 hour, 450 ℃-600 ℃ of second annealings of 890 ℃ of-910 ℃ of one-level temper are processed 4-6 hour.
Step 2. described in described auxiliary agent comprise that neodymium iron boron produces with antioxidant, lubricant, its consumption is generally 0.1 of Nd Fe B alloys quality～2.0 ‰, described auxiliary agent also comprises the gasoline that accounts for Nd Fe B alloys quality 0.1～2.0%.
Described in the present invention, Nd Fe B alloys comprises: alloy of ingot or rapid hardening slab alloy, it can be purchased from manufacture the Nd Fe B alloys manufacturing enterprise of the specialties such as Co., Ltd as Anhui Dai Xiongxin New Material Co., Ltd, Anhui Baogang RE permanent magnetic alloy, or it also can obtain as melting in vacuum induction melting furnace by conventional neodymium iron boron rapid hardening slab alloy preparation technology.
It can be M that described alloying component weight percent forms
cq
xp
yr
z, 29≤c≤33 wherein, 63≤x≤66,0.98≤y≤1.1,0≤z≤1, M is one or more in Pr, Nd, Dy, Tb element, Q be Fe, Co element one or both, P is B element, R is one or more of Al, Nb, Cu, Ga element.
The present invention utilizes magnetically controlled sputter method that light rare earth element is splashed to airflow milling micro mist surface on the basis of preparing neodymium iron boron Nd-Fe-B alloy powder, light rare earth element is as intergranular liquid phase, repair impaired crystal boundary edge, make crystal boundary more smooth, the optimization of grain boundary structure, magnet has had better magnetic property.In the present invention, crystal boundary light rare earth element liquid phase is uniformly distributed and wraps up principal phase, rises and removes exchange-coupling interaction, has overcome the skewness impact on magnet performance in crystal boundary of the rich rare earth liquid phase of two alloyages, has improved coercive force.
Embodiment
Following embodiment is usingd as the explaination to the technology of the present invention content for further illustrating of content of the present invention; but flesh and blood of the present invention is not limited in described in following embodiment, those of ordinary skill in the art can and should know any simple change or replacement based on connotation of the present invention all should belong to protection range of the presently claimed invention.
embodiment 1
1., melting prepared composition is 30.3Nd0.9Dy 66.5Fe 1.0B 0.2Nb 0.8Co 0.1Cu 0.2Ga(mass percent) neodymium iron boron rapid hardening slab alloy, it is broken that alloy sheet is inhaled hydrogen through hydrogen crushing furnace, after 540 ℃ of dehydrogenations are processed, in hydrogen flour, add antioxidant 0.5 ‰ (percentage by weight) (antioxidant is Taiyuan Jia Ci Co., Ltd commercially available prod), lubricant 0.3 ‰ (percentage by weight) (lubricant is Tianjin Yue Sheng new material research institute commercially available prod), gasoline 1.2%, in the hermetically sealed can under nitrogen protection, mix, through airflow milling powder, become micro mist again, micro mist particle mean size is 3.5um,
2., by the mixed micro mist of airflow milling (canned), be placed on the rolling sample stage of magnetron sputtering, neodymium metal Nd does target, after magnetic control sputtering system vacuumizes, in argon atmosphere, neodymium in target is splashed in sample stage on the magnetic with gravity fall, magnetic surface sputtering neodymium metal Nd thickness is at 15nm;
3., neodymium iron boron powder under sealing nitrogen protection mode moulding and room temperature condition, oriented moulding first pressing in the magnetic field of 1.2T, then be that 180MPa isostatic cool pressing is pressed into blank through pressure;
4., pressed compact is 1050 ℃ of vacuum-sinterings 5 hours, then processes 5 hours through 900 ℃ of one-level tempering 3 hours and 480 ℃ of second annealings, makes magnet;
The magnet magnetic property (20 ℃ ± 3 ℃ of temperature) of manufacturing through above-mentioned technique reach remanent magnetism Br 13.75KGs, in grasp coercivity H j 16.42KOe; And under identical component, after airflow milling, add magnet remanent magnetism Br 13.74KGs prepared by PrNd nano powder technique, in grasp coercivity H j 15.50KOe, new technology has improved the coercive force 0.92KOe of magnet, successful.
embodiment 2
1., melting prepared composition is 28.8Pr3.2Dy 65.4Fe 1.0B 0.3Nb 1.0Co 0.1Cu 0.2Al(mass percent) neodymium iron boron rapid hardening slab alloy, alloy sheet is after hydrogen crushing furnace is inhaled hydrogen fragmentation, 540 ℃ of dehydrogenations processing, in hydrogen flour, add antioxidant 0.8 ‰ (percentage by weight), gasoline 1.6%, in the hermetically sealed can under nitrogen protection, mix, through airflow milling powder, become micro mist again, micro mist particle mean size is 2.8um;
2., by the mixed micro mist of airflow milling (canned), be placed on the rolling sample stage of magnetron sputtering, metal praseodymium Pr does target, after magnetic control sputtering system vacuumizes, in argon atmosphere, metal praseodymium Pr in target is splashed in sample stage on the magnetic with gravity fall, magnetic surface sputtering praseodymium Pr thickness is at 25nm;
3., neodymium iron boron powder under sealing nitrogen protection mode moulding and room temperature condition, oriented moulding first pressing in the magnetic field of 1.2T, then be that 180MPa isostatic cool pressing is pressed into blank through pressure;
4., pressed compact is 1058 ℃ of vacuum-sinterings 5 hours, then processes 5 hours through 900 ℃ of one-level tempering 3 hours and 470 ℃ of second annealings, makes magnet;
The magnet magnetic property (20 ℃ ± 3 ℃ of temperature) of manufacturing through above-mentioned technique reach remanent magnetism Br 12.75KGs, in grasp coercivity H j 22.42KOe; And under identical component, after airflow milling, add magnet remanent magnetism Br 12.76KGs prepared by PrNd nano powder technique, in grasp coercivity H j 23.50KOe, new technology has improved the coercive force 1.08KOe of magnet, magnet more can adapt to the instructions for use of high temperature.
embodiment 3
1., melting prepared composition is 30.2(PrNd) 0.3Tb 67.15Fe 1.0B 0.15Nb 0.9Co 0.1Cu 0.2Ga(mass percent) neodymium iron boron rapid hardening slab alloy, alloy sheet is after hydrogen crushing furnace is inhaled hydrogen fragmentation, 540 ℃ of dehydrogenations processing, in hydrogen flour, add antioxidant 1.2 ‰ (percentage by weight), lubricant 0.5 ‰ (percentage by weight), gasoline 1.8%, in the hermetically sealed can under nitrogen protection, mix, through airflow milling powder, become micro mist again, micro mist particle mean size is 3.0um;
2., by the mixed micro mist of airflow milling (canned), be placed on the rolling sample stage of magnetron sputtering, praseodymium neodymium PrNd alloy (percentage by weight composition: 65Pr 35Nd) do target, after magnetic control sputtering system vacuumizes, in argon atmosphere, praseodymium neodymium in target is splashed in sample stage on the magnetic with gravity fall, magnetic surface sputtering praseodymium neodymium thickness is at 40nm;
3., neodymium iron boron powder under sealing nitrogen protection mode moulding and room temperature condition, oriented moulding first pressing in the magnetic field of 1.2T, then be that 180MPa isostatic cool pressing is pressed into blank through pressure;
4., pressed compact is 1045 ℃ of vacuum-sinterings 5 hours, then processes 5 hours through 900 ℃ of one-level tempering 3 hours and 490 ℃ of second annealings, makes magnet;
The magnet magnetic property (20 ℃ ± 3 ℃ of temperature) of manufacturing through above-mentioned technique reach remanent magnetism Br 14.15KGs, in grasp coercivity H j 14.20KOe; And under identical component, airflow milling add magnet remanent magnetism Br 14.14KGs prepared by PrNd nano powder technique, in grasp coercivity H j 13.42KOe, new technology has improved the coercive force 0.78KOe of magnet.
embodiment 4
1., melting prepared composition is 27.5La4.5Dy 65.2Fe 1.0B 0.1Nb 1.5Co 0.2Cu (mass percent) neodymium iron boron ingot casting, after hydrogen crushing furnace is inhaled hydrogen fragmentation, 540 ℃ of dehydrogenations processing, in hydrogen flour, add antioxidant 0.9 ‰ (percentage by weight), gasoline 1.8%, in the hermetically sealed can under nitrogen protection, mix, through airflow milling powder, become micro mist again, micro mist particle mean size is 4.0um;
2., by the mixed micro mist of airflow milling (canned), be placed on the rolling sample stage of magnetron sputtering, rare earth lanthanum La does target, after magnetic control sputtering system vacuumizes, in argon atmosphere, lanthanum La in target is splashed in sample stage on the magnetic with gravity fall, magnetic surface sputtering lanthanum thickness is at 40nm;
3., neodymium iron boron powder under sealing nitrogen protection mode moulding and room temperature condition, oriented moulding first pressing in the magnetic field of 1.2T, then be that 180MPa isostatic cool pressing is pressed into blank through pressure;
4., pressed compact is 1125 ℃ of vacuum-sinterings 5 hours, then processes 5 hours through 900 ℃ of one-level tempering 3 hours and 460 ℃ of second annealings, makes magnet;
The magnet magnetic property (20 ℃ ± 3 ℃ of temperature) of manufacturing through above-mentioned technique reach remanent magnetism Br 12.35KGs, in grasp coercivity H j 25.30KOe; And under identical component, airflow milling add magnet remanent magnetism Br 12.34KGs prepared by PrNd nano powder technique, in grasp coercivity H j 26.62KOe, new technology has improved the coercive force 1.32KOe of magnet.
Length is limited, and only light rare earth element adding proportion and part technique single to part magnetron sputtering or alloy illustrate above-mentioned example.Above embodiment shows, in magnet, by magnetron sputtering, adding light rare earth liquid phase (alloy) powder compares with the magnet magnetic property that adds light rare earth liquid phase nano powder after airflow milling powder, remanent magnetism Br is substantially constant, coercivity H j improves obviously, has illustrated that the light rare earth element of magnetron sputtering enters after magnet crystal boundary, and evenly continuous distribution is at neodymium iron boron principal phase periphery, repaired principal phase border, make crystal boundary Paint Gloss, optimize and improved Grain-Boundary Phase structure, thereby improved the coercive force of magnet.
Claims (7)
1. high-performance rare-earth-iron-boron is a preparation method for sintered permanent magnet, comprises the steps:
1., get Nd Fe B alloys, in hydrogen crushing furnace, inhale hydrogen fragmentation, high-temperature dehydrogenation and process, in hydrogen flour, add sintered Nd-Fe-B permanent magnet to prepare conventional auxiliary agent, at nitrogen or argon gas atmosphere lower seal, mix, then make magnetic through airflow milling powder;
2., the mixed magnetic of airflow milling is placed on the rolling sample stage of magnetron sputtering, with one or more the alloy in light rare earth element, do target, in argon gas atmosphere, light rare earth element in target is splashed on sample stage on the magnetic with gravity fall, obtains the neodymium iron boron powder that surface sputtering has light rare earth element;
3., above-mentioned neodymium iron boron powder oriented moulding in alignment magnetic field is obtained to pressed compact, pressed compact is processed through isostatic cool pressing again;
4., the pressed compact of isostatic cool pressing after processing be through vacuum-sintering, two-stage temper, makes magnet.
2. high-performance rare-earth-iron-boron is the preparation method of sintered permanent magnet as claimed in claim 1, it is characterized in that, step is hydrogen crushing furnace high-temperature dehydrogenation treatment temperature 520-580 ℃ 1..
3. high-performance rare-earth-iron-boron is the preparation method of sintered permanent magnet as claimed in claim 1, it is characterized in that, 1. step makes magnetic particle mean size is 2-7 μ m.
4. high-performance rare-earth-iron-boron is the preparation method of sintered permanent magnet as claimed in claim 1, it is characterized in that, step 2. described light rare earth element sputtering layer thickness at 10-50nm.
5. high-performance rare-earth-iron-boron is the preparation method of sintered permanent magnet as claimed in claim 1, it is characterized in that, step is alignment magnetic field 1.0-2.0T 3..
6. high-performance rare-earth-iron-boron is the preparation method of sintered permanent magnet as claimed in claim 1, it is characterized in that, step 3. isostatic cool pressing processing pressure is 150-200MPa.
7. high-performance rare-earth-iron-boron is the preparation method of sintered permanent magnet as claimed in claim 1, it is characterized in that, step is vacuum-sintering 4-6 hour at 1030 ℃-1130 ℃ 4., and 2-4 hour, 450 ℃-600 ℃ of second annealings of 890 ℃ of-910 ℃ of one-level temper are processed 4-6 hour.
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| CN106783128A (en) * | 2016-12-21 | 2017-05-31 | 包头稀土研究院 | The method for preparing low heavy rare earth high-coercive force neodymium iron boron magnetic body |
| CN108735494A (en) * | 2018-05-24 | 2018-11-02 | 北京京磁电工科技有限公司 | The preparation method of high-coercive force neodymium iron boron magnetic body |
| CN110373642A (en) * | 2019-08-01 | 2019-10-25 | 包头金山磁材有限公司 | A kind of heavy rare earth metal target restorative procedure |
| CN112750586A (en) * | 2020-12-28 | 2021-05-04 | 包头稀土研究院 | Mixed rare earth sintered neodymium-iron-boron permanent magnet and preparation method thereof |
| CN113421761A (en) * | 2021-06-12 | 2021-09-21 | 山西汇镪磁性材料制作有限公司 | Preparation method of high-performance sintered neodymium iron boron capable of reducing adsorption energy of modified magnetic powder |
| EP3955268A1 (en) | 2020-08-08 | 2022-02-16 | Yantai Shougang Magnetic Materials Inc. | Ndfeb alloy powder for forming high-coercivity sintered ndfeb magnets and use thereof |
| EP3955267A1 (en) | 2020-08-08 | 2022-02-16 | Yantai Shougang Magnetic Materials Inc. | Ndfeb alloy powder for forming high-coercivity sintered ndfeb magnets and use thereof |
| CN114686746A (en) * | 2022-04-27 | 2022-07-01 | 江苏晨朗电子集团有限公司 | Recycling method of nickel-plated sintered neodymium iron boron waste material |
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| CN106783128A (en) * | 2016-12-21 | 2017-05-31 | 包头稀土研究院 | The method for preparing low heavy rare earth high-coercive force neodymium iron boron magnetic body |
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| CN112750586B (en) * | 2020-12-28 | 2024-03-29 | 包头稀土研究院 | Mixed rare earth sintered NdFeB permanent magnet and preparation method thereof |
| CN113421761A (en) * | 2021-06-12 | 2021-09-21 | 山西汇镪磁性材料制作有限公司 | Preparation method of high-performance sintered neodymium iron boron capable of reducing adsorption energy of modified magnetic powder |
| CN113421761B (en) * | 2021-06-12 | 2023-03-24 | 山西汇镪磁性材料制作有限公司 | Preparation method of high-performance sintered neodymium iron boron capable of reducing adsorption energy of modified magnetic powder |
| CN114686746A (en) * | 2022-04-27 | 2022-07-01 | 江苏晨朗电子集团有限公司 | Recycling method of nickel-plated sintered neodymium iron boron waste material |
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Application publication date: 20141029 |