CN102592775A - High-performance neodymium iron boron sintered magnet and manufacturing method thereof - Google Patents
High-performance neodymium iron boron sintered magnet and manufacturing method thereof Download PDFInfo
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- CN102592775A CN102592775A CN2011100087393A CN201110008739A CN102592775A CN 102592775 A CN102592775 A CN 102592775A CN 2011100087393 A CN2011100087393 A CN 2011100087393A CN 201110008739 A CN201110008739 A CN 201110008739A CN 102592775 A CN102592775 A CN 102592775A
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Abstract
The invention provides a manufacturing method, which is capable of accurately controlling production of a high-remanence high-coercivity rare-earth sintered magnet. The remanence Br of the manufactured magnet ranges from 12.8kGs to 13.1kGs, the intrinsic coercivity Hcj ranges from 25kOe to 26kOe, and the maximum magnetic energy ranges from 39MGOe to 42MGOe. The formula of the rare-earth sintered magnet is (NdPr)X(DyTb)yFe(97.74-x-y-z)Co1Cu0.08A10.1Nb2Ga0.1B0.98. The oxygen content of the magnet is controlled within a range of 500ppm to 1000ppm. The manufacturing process includes: utilizing the vacuum rapid-hardening process in a smelting procedure, preparing micro powder by a jet mill after a hydrogen decrepitation process, then pressing, sintering and heat treatment by tempering, wherein the thickness of a manufactured thin alloy sheet ranges from 0.2mm to 0.5mm, and the average particle size of the micro powder ranges from 3.8 mu m to 3.9 mu m. In the manufacturing method, process parameters and formula components are optimized and high-service temperature high-remanence high-coercivity magnets can be produced stable in batch.
Description
Technical field
The present invention relates to a kind of high-performance Ne-Fe-B sintered magnet and manufacturing approach thereof, especially relate to NbFeB sintered magnet of a kind of high-residual magnetism high-coercive force and manufacturing approach thereof.
Background technology
NbFeB sintered magnet has become irreplaceable material in the modern industry with its excellent magnetism ability and high performance-price ratio.Because the NdFeB material temperature characterisitic is a negative temperature coefficient, therefore improve the research direction that its heat resistance is a neodymium iron boron magnetic body always.In recent years, the range of application of neodymium iron boron magnetic body is constantly expanded, and enters into like high-tech environmental protection fields such as frequency converting air-conditioner compressor and field of hybrid electric vehicles.In this type field, magnet not only requires higher magnetic flux usually, and the magnet serviceability temperature is had relatively high expectations, and high temperature magnetic flux demagnetizing factor is low, only produces the magnet that has high remanent magnetism and high-coercive force simultaneously and just can satisfy the demands.
Prepare at present the method for high-coercive force sintered Nd-Fe-B permanent magnetic material, a kind of method is mainly to adopt heavy rare earth element dysprosium (Dy), and terbium (Tb) part substitutes neodymium (Nd); Alloying elements cobalt (Co) is added, copper (Cu) in the enhanced anisotropy field; Niobium (Nb), gallium (Ga), aluminium (Al) waits crystal grain thinning; Increasing coercive force and improve serviceability temperature, is " a kind of ultra-high coercive force sintered Nd-Fe-B magnetic material and preparation method thereof " patent of ZL 200510049811.1 like the patent No..Also be CN 101707107A " a kind of manufacturing approach of high-residual magnetism high-coercive force rare earth permanent magnetic material " just like publication number; It mixes through compound powder and the surface treated sintered magnet with heavy rare earth; Diffusion reaction takes place in the long-time insulation of middle temperature; Make heavy rare earth diffuse into sintered magnet intergranular phase mutually, thereby do not reducing on the remanent magnetism basis, improve the magnet coercive force.For first method, described formula components scope is very big, and the technological parameter broad is not optimized, and just can not be used for accurately producing Br=12.8~13.1kGs, the magnet of Hcj=25~26kOe.Heavy rare earth Dy in addition, the Tb resource distribution is few, and price is higher, too much adds heavy rare earth element and increases substantially Hcj and be unfavorable for the resources effective utilization.Though produce the coercivity H j of magnet this moment can be greater than 35kOe, remanent magnetism Br is lower, and the scope of application is restricted.For second method; Can be owing to the degree of depth of the relative magnet surface deep diffusion of heavy rare earth in the diffusion reaction is irregular; Particularly for the laminar magnet of frequency converting air-conditioner compressor class; Diffusion depth is bigger to magnet Hcj influence, can not guarantee the magnet high conformity produced in enormous quantities, and it is difficult to cause the client to use.
Simultaneously aborning; Tend to occur since the variable effect of weather the temperature and humidity of environment; Powder oxygen uptake and adsorbed gas state can change thereupon in the die mould process; Make that its magnetic property coercive force index of same formulation product is unstable, the high 1~2kOe of magnet coercive force that the magnet of producing winter was usually produced than summer.
Summary of the invention
The objective of the invention is to through optimizing technological parameter and component prescription; It is Br=12.8~13.1kGs that a kind of magnetic property index of can accurately producing is provided; Hcj=25~26kOe, (BH) composition of the NbFeB sintered magnet of max=39~42MGOe and method, this magnet has higher remanent magnetism and coercive force simultaneously; Can satisfy most of motor requirement of client, receive climatic effect less simultaneously.
High-performance Ne-Fe-B sintered magnet of the present invention is characterized in that, described neodymium iron boron magnetic body percentage by weight formula components is: (NdPr)
x(DyTb)
yFe
(97.74-x-y-z)Co
1Cu
0.08Al
0.1Nb
zGa
0.1B
0.98, x=24~25wt% wherein, y=5.5~5.8wt%, z=0.1~0.3wt%, the magnetic property of said magnet is Br=12.8~13.1kGs simultaneously, Hcj=25~26kOe, (BH) max=39~42MGOe.
Preferably, among the described mishmetal NdPr, its weight ratio is: Pr: Nd is 1: 4~1: 3.
Preferably, among the described mishmetal DyTb, Tb >=1.3wt%.
Preferably, among described mishmetal NdPr and the DyTb, rare earth total content x+y=29.5~30.5wt%.
Preferably, oxygen content is 500~1000ppm in the said magnet.
The method of high-performance Ne-Fe-B sintered magnet of the present invention is characterized in that, said method comprising the steps of:
Batching: will pass through the surface clean raw material of removing and prepare burden by the alloying component proportioning; Adopt rapid hardening thin slice prepared alloy rapid hardening thin slice, sheet thickness is 0.2~0.5mm;
Grind: adopt quick-fried PROCESS FOR TREATMENT of hydrogen and disintegrating machine that the rapid hardening thin slice is processed meal, be prepared into the micro mist that particle mean size is 3.8~3.9 μ m through airflow milling;
Die mould: made micro mist is put into the mould medium-pressure type that has the protection of anaerobic protective atmosphere, and alignment magnetic field is >=2.0T; Pressure with 200~220MPa waits static pressure then, waits 5~20 minutes static pressure dwell times;
Sintering and tempering heat treatment: wait and blank is put into sintering furnace behind the static pressure and carry out vacuum-sintering, sintering temperature is 1050~1075 ℃, is incubated 3~5 hours; Carry out 2 grades of tempering heat treatment after being cooled fast to below 100 ℃, first order tempering heat treatment temperature is 900~930 ℃, is preferably 920 ℃; 2~3 hours time; Carry out second level heat treatment after being cooled fast to below 100 ℃, 480~500 ℃ of temperature are preferably 480 ℃; 4~5 hours time, be quickly cooled to below 80 ℃ and come out of the stove.
Preferably, the gas of said protective atmosphere use comprises nitrogen (N
2) or argon gas (Ar).
The present invention can accurately control under hypoxia condition and produce magnetic property is Br=12.8~13.1kGs, Hcj=25~26kOe, (BH) the NbFeB sintered magnet of max=39~42MGOe.
Embodiment
Below in conjunction with specific embodiment the present invention is further specified.
Embodiments of the invention are all operated according to following processing step.
(1) batching: at first will pass through the surface clean raw material of removing and prepare burden by the alloying component proportioning; Adopt rapid hardening thin slice prepared alloy rapid hardening thin slice then, sheet thickness is 0.2~0.5mm;
(2) grind: adopt quick-fried PROCESS FOR TREATMENT of hydrogen and disintegrating machine that the rapid hardening thin slice is processed meal earlier, be prepared into the micro mist that particle mean size is 3.8~3.9 μ m through airflow milling then;
(3) die mould: made micro mist is put into the mould medium-pressure type that has the protective atmosphere protection, and protective gas comprises nitrogen (N
2) or argon gas (Ar), alignment magnetic field is>=2.0T; Pressure with 200~220MPa waits static pressure then, and waiting the static pressure dwell time is 5~20 minutes;
(4) sintering and tempering heat treatment: wait and blank is put into sintering furnace behind the static pressure and carry out vacuum-sintering, sintering temperature is 1050~1075 ℃, is incubated 3~5 hours; Carry out 2 grades of tempering heat treatment after being quickly cooled to below 100 ℃, first order tempering heat treatment temperature is 900~930 ℃, is preferably 920 ℃; 2~3 hours time; Carry out second level heat treatment after being quickly cooled to below 100 ℃, 480~500 ℃ of temperature are preferably 480 ℃; 4~5 hours time, be quickly cooled to and come out of the stove after being lower than 80 ℃.
The back product of coming out of the stove carries out measurement of oxygen content.Be processed to the D10*7mm sample simultaneously, measure magnetic property and 150 ℃ of following high-temperature magnetic abilities under 20 ℃ of the normal temperature.
Embodiment 1-6 all carries out according to above-mentioned processing step, and concrete component prescription and technological parameter are seen table 1, and the oxygen content and the magnetic parameter of embodiment magnet that 1-6 obtains are also seen table 1 simultaneously.
Table 1
High-performance Ne-Fe-B sintered magnet provided by the invention and manufacturing approach thereof; Through meticulous proportioning of oxygen content scope while and optimization technological parameter in the control magnet; Make the large-scale production of high-residual magnetism high-coercive force neodymium iron boron magnetic body more stable; Can realize accurately making in batches Br=12.8~13.1kGs, Hcj=25~26kOe, (BH) the NbFeB sintered magnet of max=39~42MGOe.
What need statement is that foregoing invention content and embodiment are intended to prove the practical application of technical scheme provided by the present invention, should not be construed as the qualification to protection range of the present invention.Those skilled in the art are in spirit of the present invention and principle, when doing various modifications, being equal to replacement or improvement.Protection scope of the present invention is as the criterion with appended claims.
Claims (7)
1. a high-performance Ne-Fe-B sintered magnet is characterized in that, described neodymium iron boron magnetic body percentage by weight formula components is: (NdPr)
x(DyTb)
yFe
(97.74-x-y-z)Co
1Cu
0.08Al
0.1Nb
zGa
0.1B
0.98, x=24~25wt% wherein, y=5.5~5.8wt%, z=0.1~0.3wt%, the magnetic property of said magnet is Br=12.8~13.1kGs simultaneously, Hcj=25~26kOe, (BH) max=39~42MGOe.
2. high-performance Ne-Fe-B sintered magnet as claimed in claim 1 is characterized in that, among the described mishmetal NdPr, its weight ratio is: Pr: Nd is 1: 4~1: 3.
3. high-performance Ne-Fe-B sintered magnet as claimed in claim 1 is characterized in that, among the described mishmetal DyTb, and Tb >=1.3wt%.
4. high-performance Ne-Fe-B sintered magnet as claimed in claim 1 is characterized in that, among described mishmetal NdPr and the DyTb, and rare earth total content x+y=29.5~30.5wt%.
5. like the described high-performance Ne-Fe-B sintered magnet of claim 1-4, it is characterized in that oxygen content is 500~1000ppm in the said magnet.
6. a method of making the described high-performance Ne-Fe-B sintered magnet of claim 1 is characterized in that, said method comprising the steps of:
Batching: will pass through the surface clean raw material of removing and prepare burden by the alloying component proportioning; Adopt rapid hardening thin slice prepared alloy rapid hardening thin slice, sheet thickness is 0.2~0.5mm;
Grind: adopt quick-fried PROCESS FOR TREATMENT of hydrogen and disintegrating machine that the rapid hardening thin slice is processed meal, be prepared into the micro mist that particle mean size is 3.8~3.9 μ m through airflow milling;
Die mould: made micro mist is put into the mould medium-pressure type that has the protection of anaerobic protective atmosphere, and alignment magnetic field is >=2.0T; Pressure with 200~220MPa waits static pressure then, waits 5~20 minutes static pressure dwell times;
Sintering and tempering heat treatment: wait and blank is put into sintering furnace behind the static pressure and carry out vacuum-sintering, sintering temperature is 1050~1075 ℃, is incubated 3~5 hours; Carry out 2 grades of tempering heat treatment after being cooled fast to below 100 ℃, first order tempering heat treatment temperature is 900~930 ℃, is preferably 920 ℃; 2~3 hours time; Carry out second level heat treatment after being cooled fast to below 100 ℃, 480~500 ℃ of temperature are preferably 480 ℃; 4~5 hours time, be quickly cooled to below 80 ℃ and come out of the stove.
7. the method for high-performance Ne-Fe-B sintered magnet as claimed in claim 6 is characterized in that, the gas that said protective atmosphere uses comprises nitrogen (N
2) or argon gas (Ar).
Priority Applications (1)
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CN201110008739.3A CN102592775B (en) | 2011-01-17 | A kind of high-performance neodymium iron boron sintered magnet and manufacture method thereof |
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CN201110008739.3A CN102592775B (en) | 2011-01-17 | A kind of high-performance neodymium iron boron sintered magnet and manufacture method thereof |
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CN102592775A true CN102592775A (en) | 2012-07-18 |
CN102592775B CN102592775B (en) | 2016-12-14 |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN104036897A (en) * | 2013-03-07 | 2014-09-10 | 三环瓦克华(北京)磁性器件有限公司 | Permanent magnet material and manufacture method thereof |
CN104637664A (en) * | 2013-11-14 | 2015-05-20 | 天津三环乐喜新材料有限公司 | Method for manufacturing corrosion-resistant neodymium-iron-boron permanent magnet |
EP2937876A4 (en) * | 2012-12-24 | 2016-08-24 | Beijing Zhong Ke San Huan | Sintered neodymium-iron-boron magnet and manufacturing method therefor |
CN105957679A (en) * | 2016-07-18 | 2016-09-21 | 江苏东瑞磁材科技有限公司 | Ndfeb permanent magnet material with high magnetic energy product and high coercivity and manufacturing method thereof |
CN113871120A (en) * | 2017-12-26 | 2021-12-31 | 钢铁研究总院 | Mixed rare earth permanent magnetic material and preparation method thereof |
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Publication number | Priority date | Publication date | Assignee | Title |
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EP2937876A4 (en) * | 2012-12-24 | 2016-08-24 | Beijing Zhong Ke San Huan | Sintered neodymium-iron-boron magnet and manufacturing method therefor |
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CN104036897B (en) * | 2013-03-07 | 2017-11-21 | 三环瓦克华(北京)磁性器件有限公司 | A kind of permanent-magnet material and its manufacture method |
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CN105957679A (en) * | 2016-07-18 | 2016-09-21 | 江苏东瑞磁材科技有限公司 | Ndfeb permanent magnet material with high magnetic energy product and high coercivity and manufacturing method thereof |
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CN113871120A (en) * | 2017-12-26 | 2021-12-31 | 钢铁研究总院 | Mixed rare earth permanent magnetic material and preparation method thereof |
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