CN102592770B - A kind of sintered NdFeB magnet and manufacture method thereof - Google Patents

A kind of sintered NdFeB magnet and manufacture method thereof Download PDF

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CN102592770B
CN102592770B CN201110008706.9A CN201110008706A CN102592770B CN 102592770 B CN102592770 B CN 102592770B CN 201110008706 A CN201110008706 A CN 201110008706A CN 102592770 B CN102592770 B CN 102592770B
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magnet
sintered
micropowder
manufacture method
sintered ndfeb
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CN102592770A (en
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赵玉刚
张瑾
胡伯平
饶晓雷
杨雁
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SANVAC (BEIJING) MAGNETICS CO Ltd
Beijing Zhong Ke San Huan High Tech Co Ltd
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SANVAC (BEIJING) MAGNETICS CO Ltd
Beijing Zhong Ke San Huan High Tech Co Ltd
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Abstract

A kind of sintered NdFeB magnet and manufacture method thereof, consisting of of its composition: Nd and Pr:27.3~27.8wt%, Tb:1.0~1.8wt%, Al:0.1~0.4wt%, Cu:0.08~0.14wt%, Co:0~2wt%, Ga:0~0.14wt%, B:0.93~1.0wt%, remaining is Fe;And (BH) max > 47MGOe, Hcj > 16kOe of described magnet.The manufacture method of this sintered NdFeB magnet comprises the steps: dispensing;Vacuum induction rapid hardening furnace melting, obtains getting rid of band alloy sheet;The hydrogenation of band alloy sheet will be got rid of broken, in airflow milling, then make micropowder;The micropowder obtained is carried out mixed powder;Mixed micropowder die mould is become blank;Put into vacuum sintering furnace after isostatic pressed to be sintered;Carry out secondary ageing after having sintered, obtain described magnet.The present invention passes through formula and the technological parameter of careful design sintered NdFeB magnet, can produce the magnet with high-coercive force and high energy product, and (BH) max > 47MGOe, Hcj > 16kOe in batches.

Description

A kind of sintered NdFeB magnet and manufacture method thereof
Technical field
The present invention relates to a kind of sintered NdFeB magnet and manufacture method, the most high performance sintered NdFeB magnetic Body and manufacture method thereof, the sintered NdFeB magnet of especially (BH) max > 47MGOe, Hcj > 16kOe and Manufacture method.
Background technology
Permanent magnet material is developed as the critical material supporting electronic device, and developing direction is towards high magnetic energy Long-pending and high-coercive force direction is carried out.Rare-earth magnet is widely used in many fields at present, as recent There is the walking robot of mechanical brains, the motor special of the integrated technology of rare earth Nd FeB magnet support, vapour Car automatic system etc. has all become new application.How to improve Br with Hcj and become NdFeB magnet Developing Tendency Gesture.
Due to NdFeB properties of materials, in conventional technology, if coercivity H j of magnet to be improved, The remanent magnetism Br of magnet will be affected;If the remanent magnetism Br of magnet to be improved, coercivity H j of magnet is just It is affected, thus causes magnet to have higher Hcj and but can not have higher magnetic energy product simultaneously (BH) max, makes the range of magnet be under some influence.Such as the Chinese patent of ZL93115008.6, its The magnetic property data of embodiment 4 are: (BH) max=47.5MGOe, Br=14.0kG, Hc=12.5kOe.
The and for example Chinese patent of ZL94101181.X, by the various trace element of interpolation to improving coercivity, But inevitably impacting remanent magnetism Br, wherein the performance of magnet is (BH) max > 42MGOe simultaneously, IHc > 12.5kOe.
Nd2Fe14B intermetallic compound theoretical maximum magnetic energy product is 64MGOe, in order to reach higher magnetic energy product, Just alloy composition should be controlled to as close possible to Nd2Fe14The composition of B, and realize height by liquid-phase sintering Density and high-coercive force.
Summary of the invention
The purpose of the present invention is through the alloy formula of accurate NdFeB magnet so that it is close to The component ratio of NdFeB magnet 2: 14: 1, refines the production technology of magnet simultaneously so that it is the magnet performance of manufacture Significantly improve, improving coercitive while, also keep higher remanent magnetism level, make magnetic energy product (BH) max > 47MGOe, coercivity H j > 16kOe.
A kind of sintered NdFeB magnet of the present invention, it is characterised in that: consisting of of described magnet composition: Nd and Pr:27.3~27.8wt%, Tb:1.0~1.8wt%, Al:0.1~0.4wt%, Cu:0.08~ 0.14wt%, Co:0~2wt%, Ga:0~0.14wt%, B:0.93~1.0wt%, remaining is Fe; And (BH) max > 47MGOe, Hcj > 16kOe of described magnet.
The manufacture method of sintered NdFeB magnet of the present invention, it comprises the steps: the most in proportion Carry out dispensing;Subsequently the material prepared is put into and vacuum induction rapid hardening furnace carries out melting, obtain getting rid of band alloy thin Sheet;Band alloy sheet will be got rid of first carry out hydrogenating in hydrogenation furnace crushing, in airflow milling, then make micropowder; The micropowder obtained is carried out under inert gas shielding mixed powder;By mixed micropowder under the protection of noble gas Die mould becomes blank;Packaged blank is put in isostatic pressing machine and suppresses;By the blank that suppresses lazy The protection down of property gas enters vacuum sintering furnace and is sintered;Carry out secondary ageing after having sintered, obtain institute State magnet;It is characterized in that: the thickness of described alloy sheet is 0.1~0.5mm.
Preferably, the particle mean size of described micropowder is 2.8~4.0 μm.
Preferably, described pressing pressure > 170MPa in isostatic pressing machine.
Preferably, described sintering temperature is 1045 DEG C~1080 DEG C, temperature retention time 3~5 hours.
Preferably, described secondary ageing makes vacuum sintering furnace be cooled to 100 DEG C for being filled with Ar gas after sintering completes Hereinafter proceeding by first order Ageing Treatment, first order aging temp 900 DEG C~950 DEG C after, insulation 3~5 is little Time;Being subsequently charged with Ar gas makes vacuum sintering furnace start second level Ageing Treatment after being again cooled to less than 100 DEG C, Second level aging temp 450 DEG C~620 DEG C, is incubated 3~5 hours;Then it is filled with Ar gas to vacuum sintering furnace, Sintering furnace is made to come out of the stove after being cooled to less than 80 DEG C.
The present invention passes through formula and the technological parameter of careful design sintered NdFeB magnet, can produce in batches simultaneously There is the magnet of high-coercive force and high energy product, and (BH) max > 47MGOe, Hcj > 16kOe.
Detailed description of the invention
The manufacture method producing sintered NdFeB magnet of the present invention is carried out in accordance with the following steps:
Mixing by the raw material of following weight ratio and carry out dispensing, the compositional ranges of dispensing is: (Nd, Pr): 27.3~27.8, Tb:1.0~1.8, Al:0.1~0.4, Cu:0.08~0.14, Co:0~2, Ga: 0~0.14, B:0.93~1.0, more than Fe;
The material of cooperation being put into vacuum induction rapid hardening furnace and enters melting, the thickness of its band is between 0.1~0.5mm;
In hydrogenation furnace, carry out oxidation broken, and to make particle mean size in airflow milling be 2.8~4.0 μm Micropowder, gained micropowder also carries out mixed powder under the protection of noble gas, and the purpose of mixed powder is equal for granularity Even property;
Micropowder is carried out under the protection having noble gas die mould;
The condition at pressure > 170MPa of being put into by packaged blank in isostatic pressing machine is suppressed;
At the protection down of noble gas, the blank suppressed is entered vacuum sintering furnace be sintered, sintering temperature It is 1045 DEG C~1080 DEG C, temperature retention time 3~be filled with Ar air cooling after 5 hours and then exist to less than 100 DEG C Carry out Ageing Treatment in vacuum drying oven, in vacuum drying oven, carry out timeliness, first order aging temp 900 DEG C~950 DEG C, It is filled with Ar air cooling to less than 100 DEG C after being incubated 3~5 hours.Second level aging temp 450 DEG C~620 DEG C, After being filled with Ar gas after being incubated 3~5 hours, it is cooled to less than 80 DEG C and comes out of the stove;Obtain (BH) max > 47MGOe, The magnet of Hcj > 16kOe.
The specific embodiment of the present invention is presented herein below.
Embodiment 1
First dispensing is carried out by such as following table.
Raw material Nd Pr Tb Al Cu Co Ga B Fe
Wt% 18 9.3 1.0 0.1 0.08 0.00 0.00 0.93 70.59
Raw material is put into vacuum rapid hardening furnace carries out melting, carry out cast after melting and get rid of band, gained silver Thickness range is 0.1~0.5mm, is put into by above-mentioned alloy in hydrogenation furnace and carries out hydrogen break process, after hydrogen processes Silver in airflow milling, carry out micropowder prepare, the particle mean size of gained micropowder controls in 2.8 μm, is being full of Suppress, by packaged blank in the press close inflated with nitrogen again after the container of nitrogen carries out mixed powder Put in isostatic pressing machine and suppress under 170MPa pressure;Institute's dabbing base enters true under nitrogen atmosphere is protected Empty sintering furnace is sintered, sintering temperature 1045 DEG C, sintering time 5 hours, is then charged with Ar gas pair Sintering furnace carries out being cooled to less than 100 DEG C (about 80 DEG C), after being again warmed up to 900 DEG C and being incubated 3 hours Fill Ar gas and sintering furnace is cooled to less than 100 DEG C (about 80 DEG C), then proceed to be warmed up to 620 DEG C And fill Ar gas after being incubated 3 hours and make sintering furnace come out of the stove after being cool below 80 DEG C.Blank line after coming out of the stove Cutting machine sample, sample chi be D10 ×10mm(10Represent magnet differently-oriented directivity), magnetic measured by gained sample Can be as follows: Br=14.25KGs, Hcj=16.3Koe, (BH) max=48.5MGoe.
Embodiment 2
Dispensing is carried out by such as following table.
Raw material Nd Pr Tb Al Cu Co Ga B Fe
Wt% 18.5 9.3 1.8 0.2 0.12 0..5 0.1 0.97 68.51
Raw material is put into vacuum rapid hardening furnace carries out melting, carry out cast after melting and get rid of band, gained silver Thickness is 0.1~0.5mm, is put into by above-mentioned alloy in hydrogenation furnace and carries out hydrogen break process, the bar after hydrogen process Sheet carries out micropowder in airflow milling to be prepared, and the particle mean size of gained micropowder controls in 3.0 μm, at full nitrogen Container in carry out mixed powder after suppress in the press close inflated with nitrogen again, packaged blank is put into Isostatic pressing machine is suppressed under 180MPa pressure;Institute's dabbing base enters vacuum under nitrogen atmosphere is protected and burns Freezing of a furnace is sintered, sintering temperature 1055 DEG C, sintering time 4 hours, is then charged with Ar gas to sintering Stove carries out being cooled to less than 100 DEG C (about 80 DEG C), fills after being again warmed up to 915 DEG C and being incubated 4 hours Sintering furnace is cooled to less than 100 DEG C (about 80 DEG C) by Ar gas, and follow-up continuing is warmed up to 470 DEG C and is incubated Filling Ar gas after 3 hours makes sintering furnace come out of the stove after being cool below 80 DEG C.Blank wire cutting machine after coming out of the stove takes Sample, sample chi be D10 ×10mm(10Represent magnet differently-oriented directivity), it is as follows that magnetic property measured by gained sample: Br=13.95KGs, Hcj=18.9Koe, (BH) max=47.3MGoe.
Embodiment 3
Dispensing is carried out by such as following table.
Raw material Nd Pr Tb Al Cu Co Ga B Fe
Wt% 18.9 8.5 1.5 0.4 0.14 1.0 0.14 1.0 68.42
Raw material is put into vacuum rapid hardening furnace carries out melting, carry out cast after melting and get rid of band, gained silver Thickness is 0.1~0.5mm, is put into by above-mentioned alloy in hydrogenation furnace and carries out hydrogen break process, the bar after hydrogen process Sheet carries out micropowder in airflow milling to be prepared, and the particle mean size of gained micropowder controls between 3.2 μm, is being full of Suppress, by packaged blank in the press close inflated with nitrogen again after the container of nitrogen carries out mixed powder Put in isostatic pressing machine and suppress under 190MPa pressure;Institute's dabbing base enters true under nitrogen atmosphere is protected Being sintered in empty sintering furnace, sintering condition is 1067 DEG C × 4.5h, is then charged with Ar gas and carries out sintering furnace It is cooled to less than 100 DEG C (about 80 DEG C), after being again warmed up to 920 DEG C and being incubated 4.5 hours, fills Ar gas pair Sintering furnace carries out being cooled to less than 100 DEG C (about 80 DEG C), after be again warmed up to 480 DEG C and to be incubated 4.5 little Filling Ar gas time after makes sintering furnace come out of the stove after being cool below 80 DEG C.Blank wire cutting machine sampling after coming out of the stove, Sample chi be D10 ×10mm(10Represent magnet differently-oriented directivity), it is as follows that magnetic property measured by gained sample: Br=13.98KGs, Hcj=17.5Koe, (BH) max=47.1MGoe.
Embodiment 4
Dispensing is carried out by such as following table.
Raw material Nd Pr Tb Al Cu Co Ga B Fe
Wt% 20 7.6 1.2 0.2 0.14 2.0 0.14 0.96 67.76
Raw material is put into vacuum rapid hardening furnace carries out melting, carry out cast after melting and get rid of band, gained silver Thickness is 0.1~0.5mm, is put into by above-mentioned alloy in hydrogenation furnace and carries out hydrogen break process, the bar after hydrogen process Sheet carries out micropowder in airflow milling to be prepared, and the particle mean size of gained micropowder controls in 3.4 μm, at full nitrogen Container in carry out mixed powder after suppress in the press close inflated with nitrogen again, packaged blank is put into Isostatic pressing machine is suppressed under 200MPa pressure;Institute's dabbing base enters vacuum under nitrogen atmosphere is protected and burns Being sintered in freezing of a furnace, sintering condition is 1075 DEG C × 4 hours, is then charged with Ar gas and carries out cold to sintering furnace But to less than 100 DEG C (about 80 DEG C), Ar gas is filled after being again warmed up to 930 DEG C and being incubated 3 hours to burning Freezing of a furnace carries out being cooled to less than 100 DEG C (about 80 DEG C), follow-up continuous be warmed up to 490 DEG C and be incubated 3 hours and fill Ar gas makes sintering furnace come out of the stove after being cool below 80 DEG C.Blank wire cutting machine sampling after coming out of the stove, sample chi For D10 ×10mm(10Represent magnet differently-oriented directivity), it is as follows that magnetic property measured by gained sample: Br=14.32KGs, Hcj=16.2Koe, (BH) max=49.7MGoe.
Embodiment 5-8 is identical with the process route of embodiment 1-4, and technological parameter is different.The work of all embodiments Skill parameter and magnetic property testing result see table 1.
Table 1
Element wt when technique Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4 Embodiment 5 Embodiment 6 Embodiment 7 Embodiment 8
Nd (wt%) 18 18.5 18.9 20 18.5 18.8 19.9 19.9
Pr (wt%) 9.3 9.3 8.5 7.6 9.4 8.5 7.6 7.6
Tb (wt%) 1 1.8 1.5 1.2 1.7 1.6 1.3 1.3
Al (wt%) 0.1 0.2 0.4 0.2 0.2 0.4 0.2 0.2
Cu (wt%) 0.08 0.12 0.14 0.14 0.12 0.14 0.14 0.14
Co (wt%) 0 0.5 1 2 0.5 1 2 0
Ga (wt%) 0 0.1 0.14 0.14 0.12 0.14 0.14 0.13
B (wt%) 0.93 0.97 1 0.96 0.97 1 0.95 0.98
Fe (wt%) 70.59 68.51 68.42 67.76 68.49 68.42 67.77 69.75
Beam thickness scope (mm) 0.10.5 0.10.5 0.10.5 0.10.5 0.10.5 0.10.5 0.10.5 0.10.5
The particle mean size (μ) of micropowder 2.8 3 3.2 3.4 3.5 3.8 4 3.2
The pressure (Mpa) of isostatic pressed 170 180 190 200 180 210 220 190
Sintering temperature DEG C * hour 1045*5 1055*4 1067*4.5 1075*4 1080*5 1070*4 1080*3 1075*4.5
One-level temperature DEG C * hour 900*3 915*4 920*4.5 930*3 940*5 950*3.5 925*4 935*3
Second annealing temperature DEG C * hour 620*5 470*4 480*4.5 490*3 620*4 485*5 450*5 620*4
(B.H)max(MG0e) 48.5 47.3 47.1 49.7 48.6 47 49.6 49.2
Hcj(kOe) 16.3 18.9 17.5 16.2 16.4 16.5 16.5 16.8
Advantage of the invention is that the concrete work of the magnet designing (BH) max > 47MGOe, Hcj > 16kOe Skill formula and process route, and production high energy product can be prepared under conditions of hypoxia in batches and there is height simultaneously Coercitive magnet.
It is to be understood that, foregoing invention content and detailed description of the invention are intended to prove technology provided by the present invention The actual application of scheme, should not be construed as limiting the scope of the present invention.Those skilled in the art are at this In the spirit of invention and principle, when can various modifications may be made, equivalent or improvement.Protection scope of the present invention It is as the criterion with appended claims.

Claims (6)

1. a sintered NdFeB magnet, it is characterised in that: consisting of of described magnet composition: Nd and Pr:27.3~ 27.8wt%, Tb:1.0~1.8wt%, Al:0.1~0.4wt%, Cu:0.08~0.14wt%, Co:0~2wt%, Ga:0~0.14wt%, B:0.93~1.0wt%, remaining is Fe;And (BH) max the > 47MGOe, Hcj > of described magnet 16kOe。
2. a manufacture method for sintered NdFeB magnet as claimed in claim 1, its comprise the steps: first by Ratio carries out dispensing;Subsequently the material prepared is put into and vacuum induction rapid hardening furnace carries out melting, obtain getting rid of band alloy sheet;Will Get rid of band alloy sheet first to carry out hydrogenating in hydrogenation furnace crushing, in airflow milling, then make micropowder;By the micropowder that obtains lazy Property gas shield under carry out mixed powder;Mixed micropowder is become blank at the protection down-pressing type of noble gas;By packaged blank Put in isostatic pressing machine and suppress;At the protection down of noble gas, the blank suppressed is entered vacuum sintering furnace burn Knot;Carry out secondary ageing after having sintered, obtain described magnet;It is characterized in that: the thickness of described alloy sheet be 0.1~ 0.5mm。
3. the manufacture method of sintered NdFeB magnet as claimed in claim 2, it is characterised in that: the average particle of described micropowder Degree is 2.8~4.0 μm.
4. the manufacture method of sintered NdFeB magnet as claimed in claim 2, it is characterised in that: described in isostatic pressing machine Pressing pressure > 170MPa.
5. the manufacture method of sintered NdFeB magnet as claimed in claim 2, it is characterised in that: described sintering temperature is 1045 DEG C~1080 DEG C, temperature retention time 3~5 hours.
6. the manufacture method of sintered NdFeB magnet as claimed in claim 2, it is characterised in that: described secondary ageing be Being filled with Ar gas after having sintered makes vacuum sintering furnace proceed by first order Ageing Treatment, the first order after being cooled to less than 100 DEG C Aging temp 900 DEG C~950 DEG C, is incubated 3~5 hours;Being subsequently charged with Ar gas makes vacuum sintering furnace be again cooled to 100 DEG C Hereinafter start second level Ageing Treatment, second level aging temp 450 DEG C~620 DEG C after, be incubated 3~5 hours;Then to vacuum Sintering furnace is filled with Ar gas, makes sintering furnace come out of the stove after being cooled to less than 80 DEG C.
CN201110008706.9A 2011-01-17 A kind of sintered NdFeB magnet and manufacture method thereof Active CN102592770B (en)

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CN102592770B true CN102592770B (en) 2016-12-14

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2000019456A1 (en) * 1998-09-28 2000-04-06 Rhodia Chimie Magnetic material based on iron, cobalt, rare earths and boron and magnet based on said material
CN101562067A (en) * 2008-04-18 2009-10-21 沈阳中北通磁科技有限公司 Manufacture method of corrosion-resistant R-Fe-B rare-earth permanent magnet
CN101853725A (en) * 2009-04-03 2010-10-06 中国科学院宁波材料技术与工程研究所 Preparation method of sintered Nd-Fe-B permanent magnetic material

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2000019456A1 (en) * 1998-09-28 2000-04-06 Rhodia Chimie Magnetic material based on iron, cobalt, rare earths and boron and magnet based on said material
CN101562067A (en) * 2008-04-18 2009-10-21 沈阳中北通磁科技有限公司 Manufacture method of corrosion-resistant R-Fe-B rare-earth permanent magnet
CN101853725A (en) * 2009-04-03 2010-10-06 中国科学院宁波材料技术与工程研究所 Preparation method of sintered Nd-Fe-B permanent magnetic material

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