CN104064301A - NdFeB magnet and preparation method thereof - Google Patents
NdFeB magnet and preparation method thereof Download PDFInfo
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- CN104064301A CN104064301A CN201410326924.0A CN201410326924A CN104064301A CN 104064301 A CN104064301 A CN 104064301A CN 201410326924 A CN201410326924 A CN 201410326924A CN 104064301 A CN104064301 A CN 104064301A
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Abstract
The invention provides an NdFeB magnet which comprises, by mass, 29% to 33% of Pr-Nd, 0.97% to 1.5% of B, 0.4% to 0.6% of Dy, 0.2% to 0.8% of Al, 0.6% to 0.8% of Co, 0.01% to 0.5% of Cu, 0.01% to 0.2% of Zr and the balance Fe. The invention further discloses a preparation method of the NdFeB magnet. The method includes the steps that firstly, Pr-Nd alloy, Zr-Fe alloy, B-Fe alloy, Dy-Fe alloy, aluminum, cobalt, copper and iron are molten to prepare an NdFeB cast ingot; secondly, the obtained NdFeB cast ingot is milled into NdFeB powder; finally, the NdFeB powder is sintered into the NdFeB magnet. The NdFeB magnet prepared through the method has a more refined magnet grain size and higher magnet stability.
Description
Technical field
The invention belongs to magnet preparing technical field, relate in particular to a kind of neodymium iron boron magnetic body and preparation method thereof.
Background technology
Magnet is the material that can produce magnetic field, has the ferromagnetic substance of attraction as the characteristic of the metals such as iron, nickel, cobalt.Magnet is generally divided into permanent magnet and soft magnetic bodies, is mostly soft magnetic bodies as the material of magnetic conductor and electromagnet, and its polarity is to change with added polarity of the magnetic field; And permanent magnet is hard magnetic body, can keep for a long time the magnet of its magnetic, be difficult for loss of excitation, be also difficult for being magnetized.Thereby, be no matter in industrial production or in daily life, one of powerful material that hard magnetic body is the most frequently used.
Hard magnetic body can be divided into natural magnet and artificial magnet, and artificial magnet refers to by the alloy of synthetic different materials can reach the effect identical with natural magnet (magnet), but also can improve magnetic force.Just occurred artificial magnet as far back as 18th century, but it is very slow to manufacture the process of strong magnetic material more, until produce alnico magnet (AlNiCo) thirties in 20th century, just makes the large-scale application of magnet become possibility.Subsequently, produced ferrite (Ferrite) the 1950's, the sixties, the appearance of rare earth permanent magnet, for the application of magnet has been opened up a New Times, first generation samarium cobalt permanent magnet SmCo
5, second generation precipitation hardenable samarium cobalt permanent magnet Sm
2co
17, up to now, develop into third generation Nd-Fe-Bo permanent magnet material (NdFeB).Although ferrimagnet remains the permanent magnetic material of consumption maximum at present, the output value of neodymium iron boron magnetic body has substantially exceeded ferrite permanent-magnet materials, has developed into a large industry.
Neodymium iron boron magnetic body is also referred to as neodymium magnet (Neodymium magnet), and its chemical formula is Nd
2fe
14b, is a kind of artificial permanent magnet, is also to have so far the permanent magnet of strong magnetic force.The advantage of neodymium iron boron magnetic body is that cost performance is high, the features such as the mechanical property that volume is little, lightweight, good and magnetic are strong, so the advantage of high-energy-density obtains a wide range of applications Nd-Fe-Bo permanent magnet material in modern industry and electronic technology, is described as magnetic king in magnetics circle.Thereby the preparation of neodymium iron boron magnetic body and expansion are the focuses giving more sustained attention in the industry always.
At present, industry often adopts sintering process to make neodymium iron boron magnetic body, wherein most sintering furnaces of preparing Sintered NdFeB magnet heat in thermal-radiating mode, but because sintering process is limit, be easy to cause the excessive sintering of magnet, produce abnormal grain growth, reduce magnet coercive force, or the phenomenon of the magnet sintering deficiency at center occurs.In prior art, patent CN10104187A discloses preparation technology of a kind of zirconium hydrogen crystal grain accretion inhibitor and uses thereof, and first it be ZrH by zirconium hydrogenation in hydrogen broken furnace
x, then use after becoming granularity to be less than the superfine powder of 2 μ m zirconium hydrogen crystal grain accretion inhibitor airflow milling, can suppress abnormal grain growth, but zirconium hydrogen superfine powder unstable properties, activity is higher, not easy to store, and integrated artistic complexity, is unfavorable for industrial production.
Therefore, how to find a kind of character to neodymium iron boron magnetic body self to improve, widen the sintering range of neodymium iron boron magnetic body, improve magnet performance stability, avoid the phenomenon of abnormal grain growth, technique is simply easy to the method for producing simultaneously, and for magnet generation, producer is of great practical significance.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of neodymium iron boron magnetic body and preparation method thereof, the neodymium iron boron magnetic body that adopts method provided by the invention to prepare, there is the magnet crystallite dimension of refinement more and the magnet stability of Geng Gao, and technique is simply easy to produce.
The invention provides a kind of neodymium iron boron magnetic body, it is characterized in that, composition comprises by mass percentage:
Pr-Nd：29％～33％；
B：0.97％～1.5％；
Dy：0.4％～0.6％；
Al：0.2％～0.8％；
Co：0.6％～0.8％；
Cu：0.01％～0.5％；
Zr：0.01％～0.2％；
Surplus is Fe.
Preferably, comprise 0.01%～0.099% Zr.
The preparation method who the invention provides a kind of neodymium iron boron magnetic body, comprises the following steps:
A), under vacuum condition, Pr-Nd alloy, Zr-Fe alloy, B-Fe alloy, Dy-Fe alloy, aluminium, cobalt, copper and iron melting are prepared to neodymium iron boron ingot casting;
B) by steps A) the neodymium iron boron ingot casting that obtains after powder process, obtain neodymium iron boron powder;
C) by after above-mentioned neodymium iron boron powder sintering, obtain neodymium iron boron magnetic body.
Preferably, the mass percentage content of the Pr in described Pr-Nd alloy is 23.0%～27.0%; In described Zr-Fe alloy, the mass percentage content of Zr is 77.0%～82.0%; In described B-Fe alloy, the mass percentage content of B is 17.0%～20.0%; In described Dy-Fe alloy, the mass percentage content of Dy is 77.0%～82.0%.
Preferably, the thickness of described neodymium iron boron ingot casting is less than or equal to 27mm.
Preferably, the granularity of described neodymium iron boron powder is 2～15 μ m.
Preferably, described steps A) also comprise, under vacuum condition, the neodymium iron boron ingot casting that melting is prepared heats up, constant temperature and cooling processing.
Preferably, the temperature after described intensification is 1000～1100 DEG C, and described cooled temperature is 20～80 DEG C.
Preferably, the time of described intensification is 2～4 hours, and the time of described constant temperature is 3～5 hours.
Preferably, described step C) be specially:
C1) above-mentioned neodymium iron boron powder is fired 5～7 hours at the first temperature, then at the second temperature, carried out tempering 3～5 hours, obtain green compact after cooling;
C2) green compact that above-mentioned steps obtained tempering 2～6 hours at the 3rd temperature, obtains neodymium iron boron magnetic body;
Described the first temperature is 1020～1050 DEG C, and described cooled temperature is 20～80 DEG C;
Described the second temperature is 850～950 DEG C, and described the 3rd temperature is 400～650 DEG C.
The invention discloses a kind of neodymium iron boron magnetic body, it is characterized in that, composition comprises by mass percentage: Pr-Nd:29%～33%, B:0.97%～1.5%, Dy:0.4%～0.6%, Al:0.2%～0.8%, Co:0.6%～0.8%, Cu:0.01%～0.5%, Zr:0.01%～0.2%, surplus is Fe.Compared with prior art, the present invention adopts the method for multielement alloys such as adding Pr-Nd alloy, Zr-Fe alloy, B-Fe alloy and Dy-Fe alloy, under the effect of multielement alloy, by refining effect and the distinctive rare earth element blend proportion of Zr, thereby refinement the crystallite dimension of neodymium iron boron magnetic body, suppress abnormal grain growth, and then widened magnet sintering temperature and improved magnet Magnetic stability, and improved coercive force and the squareness of magnet.And Zr-Fe alloy adds the rear Fe that there is no soft magnetic characteristic that forms in neodymium iron boron magnetic body
2zr phase, prevents the movement of neticdomain wall, thereby has improved the HCJ of material.Meanwhile, multielement alloy melting point lower-performance is stable, and aborning, technique is simply easy to control, and can also save production cost.Experimental result shows, the average grain size of neodymium iron boron magnetic body provided by the invention is 5.77～5.92 μ m, Hcb, Hcj, Hk and the Hk/Hcj of neodymium iron boron magnetic body increase respectively, and the standard variance of the item magnetic properties such as Br, Hcb, Hcj, (BH) m, Hk and Hk/Hcj has significantly reduction.
Brief description of the drawings
Fig. 1 is the metallurgical microstructrue figure of the neodymium iron boron magnetic body prepared of comparative example 1 of the present invention;
Fig. 2 is the metallurgical microstructrue figure of the neodymium iron boron magnetic body prepared of comparative example 2 of the present invention;
Fig. 3 is the metallurgical microstructrue figure of the neodymium iron boron magnetic body prepared of the embodiment of the present invention 1;
Fig. 4 is the metallurgical microstructrue figure of the neodymium iron boron magnetic body prepared of the embodiment of the present invention 2;
Fig. 5 is the metallurgical microstructrue figure of the neodymium iron boron magnetic body prepared of the embodiment of the present invention 3.
Embodiment
In order further to understand the present invention, below in conjunction with embodiment, the preferred embodiments of the invention are described, but should be appreciated that these are described is the restriction for further illustrating the features and advantages of the present invention instead of patent of the present invention being required.
The invention provides a kind of neodymium iron boron magnetic body, it is characterized in that, composition comprises by mass percentage:
Pr-Nd：29％～33％；
B：0.97％～1.5％；
Dy：0.4％～0.6％；
Al：0.2％～0.8％；
Co：0.6％～0.8％；
Cu：0.01％～0.5％；
Zr：0.01％～0.2％；
Surplus is Fe.
Neodymium iron boron magnetic body provided by the invention, by adding the method for the multielement alloys such as Pr-Nd alloy, Zr-Fe alloy, B-Fe alloy and Dy-Fe alloy, under the effect of multielement alloy, by refining effect and the distinctive rare earth element blend proportion of Zr, thereby refinement the crystallite dimension of neodymium iron boron magnetic body, suppress abnormal grain growth, and then widened magnet sintering temperature and improved magnet Magnetic stability, and improved coercive force and the squareness of magnet.
The present invention is raw materials used, and its source is not particularly limited, and on market, buys; The all raw materials of the present invention, are not particularly limited its purity, and the present invention preferably adopts analysis pure.
The present invention is not particularly limited the definition of room temperature, with room temperature definition well known to those skilled in the art, is preferably 20～30 DEG C.
In the present invention, composition by mass percentage, the mass percentage content of described Pr-Nd is preferably 29%～33%, and more preferably 29.5%～31.5%, most preferably be 30%～31.2%; The present invention is not particularly limited the source of Pr-Nd, with rare earth alloy well known to those skilled in the art source or commercially available rare earth alloy; The present invention is not particularly limited the purity of Pr-Nd, with the rare earth alloy purity for the preparation of neodymium iron boron magnetic body well known to those skilled in the art, is preferably analysis pure.
In the present invention, composition by mass percentage, the mass percentage content of described B is preferably 0.97%～1.5%, and more preferably 0.98%～1.4%, more preferably 0.99%～1.2%, most preferably be 1.0%; The present invention is not particularly limited the source of B, with source well known to those skilled in the art or commercially available; The present invention is not particularly limited the purity of B, with the purity for the preparation of neodymium iron boron magnetic body well known to those skilled in the art, is preferably analysis pure.
In the present invention, composition by mass percentage, the mass percentage content of described Dy is preferably 0.4%～0.6%, and more preferably 0.45%～0.55%, most preferably be 0.48%～0.52%; The present invention is not particularly limited the source of Dy, with rare earth element well known to those skilled in the art source or commercially available rare earth element; The present invention is not particularly limited the purity of Dy, with the rare earth element purity for the preparation of neodymium iron boron magnetic body well known to those skilled in the art, is preferably analysis pure.
The present invention joins in neodymium iron boron magnetic body Dy as rare earth element, by the refining effect of Dy element, in neodymium iron boron magnetic body, can form high temperature resistant metallographic structure tiny and that disperse distributes, therefore, can, under room temperature and hot conditions, there is better mechanical property.
In the present invention, composition by mass percentage, the mass percentage content of described Al is preferably 0.2%～0.8%, and more preferably 0.4%～0.5%, most preferably be 0.42%～0.48%; The present invention is not particularly limited the source of Al, with source well known to those skilled in the art or commercially available; The present invention is not particularly limited the purity of Al, with the purity for the preparation of neodymium iron boron magnetic body well known to those skilled in the art, is preferably analysis pure.
In the present invention, composition by mass percentage, the mass percentage content of described Co is preferably 0.6%～0.8%, and more preferably 0.65%～0.75%, most preferably be 0.68%～0.72%; The present invention is not particularly limited the source of Co, with source well known to those skilled in the art or commercially available; The present invention is not particularly limited the purity of Co, with the purity for the preparation of neodymium iron boron magnetic body well known to those skilled in the art, is preferably analysis pure.
In the present invention, composition by mass percentage, the mass percentage content of described Cu is preferably 0.01%～0.5%, and more preferably 0.05%～0.35%, most preferably be 0.08%～0.22%; The present invention is not particularly limited the source of Cu, with source well known to those skilled in the art or commercially available; The present invention is not particularly limited the purity of Cu, with the purity for the preparation of neodymium iron boron magnetic body well known to those skilled in the art, is preferably analysis pure.
In the present invention, composition by mass percentage, the mass percentage content of described Zr is preferably 0.01%～0.2%, and more preferably 0.02%～0.15%, more preferably 0.04%～0.07%, most preferably be 0.055%～0.065%.The present invention is not particularly limited the source of Zr, with method well known to those skilled in the art preparation or commercially available; The present invention is not particularly limited the purity of Zr, with the purity for the preparation of neodymium iron boron magnetic body well known to those skilled in the art, is preferably analysis pure.The present invention joins Zr in neodymium iron boron magnetic body in the mode of Zr-Fe alloy, crystal grain thinning significantly, thus widen the sintering temperature of magnet and improve magnet Magnetic stability.
In described neodymium iron boron magnetic body, form by mass percentage in the present invention, all the other are Fe; The present invention is not particularly limited the source of Fe, with method well known to those skilled in the art preparation or commercially available; The present invention does not have other to limit especially to the purity of Fe, with the purity for the preparation of neodymium iron boron magnetic body well known to those skilled in the art, is preferably analysis pure.In neodymium iron boron magnetic body of the present invention, also comprise the impurity of being introduced by raw material, the present invention is not particularly limited the content of described impurity, requires with impurity content control well known to those skilled in the art.
In the present invention, in described neodymium iron boron magnetic body by mass percentage, more preferably Pr-Nd:32.3%; B:1%; Dy:0.5%; Al:0.45%; Cu:0.1%; Co:0.7%; The Fe of Zr:0.06% and surplus, more preferably Pr-Nd:32.0%; B:1%; Dy:0.5%; Al:0.45%; Cu:0.1%; Co:0.7%; The Fe of Zr:0.04% and content.
The present invention is directed to neodymium iron boron magnetic body because sintering process is limit, easily cause the excessive sintering of magnet, produce abnormal grain growth, reduce magnet coercive force, or the phenomenon of the magnet sintering deficiency at center, adopt the method for adding multiple metallic element alloy, at rare earth element, under the effect of rare earth alloy and Zr-Fe alloy, by micro-refining effect and distinctive rare earth element blend proportion, thereby refinement the crystallite dimension of neodymium iron boron magnetic body, suppress abnormal grain growth, and then widen magnet sintering temperature and improved magnet Magnetic stability, and coercive force and the squareness of magnet are improved.
The preparation method who the invention also discloses a kind of neodymium iron boron magnetic body, comprises the following steps:
A), under vacuum condition, Pr-Nd alloy, Zr-Fe alloy, B-Fe alloy, Dy-Fe alloy, aluminium, cobalt, copper and iron melting are prepared to neodymium iron boron ingot casting;
B) by steps A) the neodymium iron boron ingot casting that obtains after powder process, obtain neodymium iron boron powder;
C) by after above-mentioned neodymium iron boron powder sintering, obtain neodymium iron boron magnetic body.
First the present invention under vacuum condition, prepares neodymium iron boron ingot casting by Pr-Nd alloy, Zr-Fe alloy, B-Fe alloy, Dy-Fe alloy, aluminium, cobalt, copper and iron melting; The present invention is not particularly limited the absolute pressure of described vacuum, and with the required pressure of neodymium iron boron ingot casting of preparing well known to those skilled in the art, the present invention is preferably 2.0～1000Pa, and more preferably 2.0～500Pa, most preferably is 2.0～200Pa.The present invention is not particularly limited the size of described neodymium iron boron ingot casting, with the size of neodymium iron boron ingot casting well known to those skilled in the art, the present invention is the performance that ensures prepared neodymium iron boron magnetic body, the thickness of described neodymium iron boron ingot casting is preferably and is less than or equal to 27mm, more preferably be less than or equal to 23mm, most preferably be and be less than or equal to 20mm.The present invention is not particularly limited the process of described melting, prepares the process of neodymium iron boron ingot casting with fusion method well known to those skilled in the art; The present invention is not particularly limited the equipment of described melting, prepares the equipment of neodymium iron boron ingot casting with fusion method well known to those skilled in the art, and the present invention is preferably vacuum melting furnace.
The present invention adds element Pr in raw materials with the form of described Pr-Nd alloy, and the mass percentage content of described element Pr in Pr-Nd alloy is preferably 23.0%～27.0%, and more preferably 23.5%～25.5%, most preferably be 24.0%～25.0%; The present invention is not particularly limited the source of described Pr-Nd alloy, with source well known to those skilled in the art or commercially available; The present invention is not particularly limited the purity of described Pr-Nd alloy, with the purity for the preparation of neodymium iron boron magnetic body well known to those skilled in the art.The present invention adds element Zr in raw materials with the form of described Zr-Fe alloy, and the mass percentage content of described element Zr in Zr-Fe alloy is preferably 77.0%～82.0%, and more preferably 78.0%～81.0%, most preferably be 79.0%～80.0%; The present invention is not particularly limited the source of described Zr-Fe alloy, with source well known to those skilled in the art or commercially available; The present invention is not particularly limited the purity of described Zr-Fe alloy, with the purity for the preparation of neodymium iron boron magnetic body well known to those skilled in the art.The present invention adds element B in raw materials with the form of described B-Fe alloy, and the mass percentage content of described element B in B-Fe alloy is preferably 17.0%～20.0%, and more preferably 17.5%～19.5%, most preferably be 17.8%～18.2%; The present invention is not particularly limited the source of described B-Fe alloy, with source well known to those skilled in the art or commercially available; The present invention is not particularly limited the purity of described B-Fe alloy, with the purity for the preparation of neodymium iron boron magnetic body well known to those skilled in the art.The present invention adds element Dy in raw materials with the form of described Dy-Fe alloy, and the mass percentage content of described element Dy in Dy-Fe alloy is preferably 77.0%～82.0%, and more preferably 77.5%～80.0%, most preferably be 78.0%～79.0%; The present invention is not particularly limited the source of described Dy-Fe alloy, with rare earth alloy well known to those skilled in the art source or commercially available rare earth alloy; The present invention is not particularly limited the purity of described Dy-Fe alloy, with the rare earth alloy purity for the preparation of neodymium iron boron magnetic body well known to those skilled in the art.
The present invention is the performance that improves prepared neodymium iron boron magnetic body, and preferably under vacuum condition, the neodymium iron boron ingot casting that melting is prepared heats up again, constant temperature and cooling processing, i.e. steel ingot homogenizing; The present invention is not particularly limited the process of described steel ingot homogenizing, with the process of the steel ingot homogenizing of neodymium iron boron ingot casting well known to those skilled in the art, the present invention preferably carries out according to the following steps, first under vacuum condition, neodymium iron boron ingot casting is carried out to hyperthermic treatment, carry out again constant temperature method, then carry out coolingly, finally obtain the neodymium iron boron ingot casting of homogenizing processing; The time of described intensification is preferably 2～4 hours, more preferably 2.5～3.5 hours, most preferably is 2.7～3.3 hours; Temperature after described intensification is preferably 1000～1100 DEG C, more preferably 1030～1070 DEG C; The time of described constant temperature is preferably 3～5 hours, more preferably 3.5～4.5 hours; The pressure of described vacuum is preferably 4.0～1000Pa, more preferably 4.0～500Pa.The present invention is not particularly limited described cooling mode, and with the type of cooling of the steel ingot homogenizing of neodymium iron boron ingot casting well known to those skilled in the art, it is cooling that the present invention is preferably argon gas air blast.Cooled temperature of the present invention is not particularly limited, and with chilling temperature well known to those skilled in the art, the present invention is preferably 20～80 DEG C.
The present invention then by neodymium iron boron ingot casting ingot after treatment above-mentioned homogenizing after powder process, obtain neodymium iron boron powder; The granularity of described powder is preferably 2～15 μ m, and more preferably 3～10 μ m, most preferably are 3～5 μ m; The present invention is not particularly limited the process of powder process, with the pulverizing process of neodymium iron boron ingot casting well known to those skilled in the art, the present invention preferably carries out according to the following steps, first neodymium iron boron ingot casting ingot after treatment above-mentioned homogenizing is placed in to rotation hydrogen crushing furnace, in hydrogen crushing furnace, pass into pressurized with hydrogen, then the dehydrogenation that heats up, finally puts into airflow milling and grinds, and obtains neodymium iron boron powder.The pressure of described pressurization is preferably 0.1～0.2MPa, more preferably 0.13～0.17MPa; The temperature of described intensification dehydrogenation is preferably 400～700 DEG C, more preferably 550～650 DEG C, most preferably is 550～600 DEG C; The present invention is not particularly limited other conditions in above-mentioned pulverizing process, with the pulverizing process condition of neodymium iron boron ingot casting well known to those skilled in the art.The present invention is the performance that improves prepared neodymium iron boron magnetic body, and the neodymium iron boron powder preferably above-mentioned grinding being obtained mixes powder processing; The time of described mixed powder is preferably 45～75 minutes, more preferably 50～70 minutes, most preferably is 55～65 minutes.
The present invention is the effect that improves follow-up sintering process, preferably, before sintering, first the neodymium iron boron powder after above-mentioned mixed powder is carried out to die mould processing.The present invention is not particularly limited the process of described die mould processing, with the process of neodymium iron boron powder die mould well known to those skilled in the art processing, the present invention preferably carries out according to the following steps, first neodymium iron boron powder after treatment above-mentioned mixed powder being put into moulding press mould adds magnetic field and is orientated, compressing, also Vacuum Package of demagnetization again, then put into after isostatic pressing machine pressurization and pressurize, obtain neodymium iron boron base substrate.Described magnetic field intensity is preferably more than and equals 16000Gs, is more preferably more than or equal to 18000Gs; The pressure of described pressurization is 150～230MPa, more preferably 180～220MPa; The time of described pressurize is preferably 2～10 minutes, more preferably 4～8 minutes; The present invention is not particularly limited other conditions of above-mentioned neodymium iron boron powder die mould processing, selects with die mould processing procedure well known to those skilled in the art or according to practical condition is concrete.
The present invention carries out above-mentioned neodymium iron boron base substrate after sintering, finally to obtain neodymium iron boron magnetic body.The present invention is not particularly limited the process of described sintering, and with the process of Sintered NdFeB magnet well known to those skilled in the art, the present invention preferably specifically carries out according to the following steps,
First above-mentioned neodymium iron boron base substrate is fired at the first temperature, then at the second temperature, carried out tempering, obtain green compact after cooling; Then the green compact that above-mentioned steps obtained tempering 2～6 hours at the 3rd temperature, obtains neodymium iron boron magnetic body.
Described the first temperature is preferably 1020～1060 DEG C, more preferably 1030～1045 DEG C; At described the first temperature, fire and be preferably 5～7 hours, more preferably 5.5～6.5 hours; Described cooled temperature is preferably 20 DEG C～80 DEG C, more preferably 20 DEG C～70 DEG C; Described the second temperature is preferably 850～950 DEG C, more preferably 880～920 DEG C; The described time of carrying out tempering at the second temperature is preferably 3～5 hours, more preferably 3.5～4.5 hours; Described the 3rd temperature is preferably 400～650 DEG C, more preferably 450～600 DEG C; The described time of carrying out tempering at the 3rd temperature is preferably 2～6 hours, more preferably 3～5 hours.The present invention is not particularly limited other conditions of above-mentioned sintering process, with the condition of neodymium iron boron magnetic body sintering well known to those skilled in the art; The present invention is not particularly limited the equipment of above-mentioned sintering, and with neodymium iron boron magnetic body agglomerating plant well known to those skilled in the art, the present invention is preferably single chamber sintering furnace.
The present invention adopts the method for multielement alloys such as adding Pr-Nd alloy, Zr-Fe alloy, B-Fe alloy and Dy-Fe alloy, under the effect of multielement alloy, by refining effect and the distinctive rare earth element blend proportion of Zr, thereby refinement the crystallite dimension of neodymium iron boron magnetic body, suppress abnormal grain growth, and then widened magnet sintering temperature and improved magnet Magnetic stability, and coercive force and the squareness of magnet are improved.And Zr-Fe alloy adds the rear Fe that there is no soft magnetic characteristic that forms in neodymium iron boron magnetic body
2zr phase, prevents the movement of neticdomain wall, thereby has improved the HCJ of material.Meanwhile, multielement alloy melting point lower-performance is stable, and aborning, technique is simply easy to control, and can also save production cost.
The present invention is after above-mentioned steps obtains Sintered NdFeB magnet, it is carried out to Performance Detection, experimental result shows, the average grain size of neodymium iron boron magnetic body provided by the invention is 5.77～5.92 μ m, Hcb, Hcj, Hk and the Hk/Hcj of neodymium iron boron magnetic body increase respectively, and the standard variance of the item magnetic properties such as Br, Hcb, Hcj, (BH) max, Hk and Hk/Hcj has significantly reduction.
In order to further illustrate the present invention, below in conjunction with embodiment, neodymium iron boron magnetic body provided by the invention and preparation method thereof is described in detail.
Comparative example 1
First, according to mass percent composition Pr-Nd:32.3wt%, Dy:0.5wt%, Al:0.45wt%, B:1.0wt%, Cu:0.1wt%, Co:0.7wt% and Fe:64.95wt% take; The wherein content 24wt% of Pr in Pr-Nd alloy, B adds with the form of B-Fe alloy, and the content of B in B-Fe alloy is 18wt%; Dy adds with the form of Dy-Fe alloy, and the content of Dy in Dy-Fe alloy is 78wt%; Other raw materials are analytically pure metal.For ensureing that each alloying element content is stable in product, need estimate in advance the actual consume of raw material, the quality of the each element of reality weighing is, Pr-Nd alloy: 32.3kg, Dy-Fe alloy: 0.64kg, Al:0.45kg, B-Fe alloy: 5.56kg, Cu:0.1kg, Co:0.7kg, Fe:60.25kg.
Above-mentioned raw material are put into vacuum melting furnace, under the condition of 1300 DEG C of vacuum degree 2Pa and temperature, after fusing, pour into a mould completely, after cast, obtain the neodymium iron boron ingot casting that thickness is 20mm.Above-mentioned ingot casting is carried out to homogenizing processing, at the vacuum condition of 4Pa, temperature is risen to 1050 DEG C, the heating-up time is 2.5 hours, then constant temperature is after 4 hours, and applying argon gas air blast is cooled to 30 DEG C, obtains homogenizing neodymium iron boron ingot casting after treatment.
The neodymium iron boron ingot casting obtaining of above-mentioned steps is inserted in rotation hydrogen crushing furnace, in hydrogen crushing furnace, pass into hydrogen until furnace pressure reaches after 0.1Mpa, dehydrogenation after hydrogen crushing furnace is warming up to 580 DEG C, neodymium iron boron ingot casting after dehydrogenation is put into airflow milling powder process, controlling particle size is 3～5 μ m, average particle size is 3.6 μ m, then the powder after airflow milling is mixed to powder and processes 45min, obtains neodymium iron boron powder.
Neodymium iron boron powder is put into moulding press mould to be added magnetic field and is orientated, magnetic field intensity is 16000Gs, compressing after orientation, also Vacuum Package of demagnetization, put into isostatic pressing machine by the green compact of Vacuum Package and be forced into 220Mpa, pressurize after 2 minutes, obtains neodymium iron boron base substrate.
Neodymium iron boron base substrate after the moulding that above-mentioned steps is obtained, cut rear loose the piling up in material boat of material, put into sintering furnace sintering 5 hours at the temperature of 1035 DEG C, and at 900 DEG C tempering after 3 hours argon gas air-cooled, after neodymium iron boron base substrate after air-cooled is warming up to 520 DEG C again, tempering 2 hours, obtains neodymium iron boron magnetic body.
The neodymium iron boron magnetic body that above-mentioned steps is obtained is observed, result is referring to Fig. 1, Fig. 1 is the metallurgical microstructrue figure of the neodymium iron boron magnetic body prepared of comparative example 1 of the present invention, and the neodymium iron boron magnetic body crystal grain that comparative example 1 prepares is as can be seen from Figure 1 larger, and average grain size is 8.33 μ m.
Sintered NdFeB magnet prepared by said method is processed into the sample of D10*10, carry out Performance Detection, adopt NIM-10000 magnetic material measuring system test magnetic property, test result is referring to table 1, and table 1 is the performance data table of the Sintered NdFeB magnet of comparative example 1～2 and embodiment 1～3 preparation.
Referring to table 2, the standard variance table of the magnetic property of the Sintered NdFeB magnet that table 2 is prepared for comparative example 1 and embodiment 1.
Comparative example 2
First, according to mass percent composition Pr-Nd:32.3wt%, Dy:0.5wt%, Al:0.45wt%, B:1.0wt%, Cu:0.1wt%, Co:0.7wt%, Zr:0.06wt% and Fe:64.89wt% take; The wherein content 24wt% of Pr in Pr-Nd alloy, B adds with the form of B-Fe alloy, and the content of B in B-Fe alloy is 18wt%; Dy adds with the form of Dy-Fe alloy, and the content of Dy in Dy-Fe alloy is 78wt%, and other raw materials are analytically pure metal.For ensureing that in product, each alloying element content is stable, need estimate in advance the actual consume of raw material, the actual quality that weighs each element is, Pr-Nd alloy: 32.3kg, Dy-Fe alloy: 0.64kg, Al:0.45kg, B-Fe alloy: 5.56kg, Cu:0.1kg, Co:0.7kg, Zr:0.06kg, Fe:60.19kg.
Above-mentioned raw material are put into vacuum melting furnace, under the condition of 1300 DEG C of vacuum degree 2Pa and temperature, after fusing, pour into a mould completely, after cast, obtain the neodymium iron boron ingot casting that thickness is 20mm.Above-mentioned ingot casting is carried out to homogenizing processing, at the vacuum condition of 4Pa, temperature is risen to 1050 DEG C, the heating-up time is 2.5 hours, then constant temperature is after 4 hours, and applying argon gas air blast is cooled to 30 DEG C, obtains homogenizing neodymium iron boron ingot casting after treatment.
The neodymium iron boron ingot casting obtaining of above-mentioned steps is inserted in rotation hydrogen crushing furnace, in hydrogen crushing furnace, pass into hydrogen until furnace pressure reaches after 0.1Mpa, dehydrogenation after hydrogen crushing furnace is warming up to 580 DEG C, neodymium iron boron ingot casting after dehydrogenation is put into airflow milling powder process, controlling particle size is 3～5 μ m, average particle size is 3.6 μ m, then the powder after airflow milling is mixed to powder and processes 45min, obtains neodymium iron boron powder.
Neodymium iron boron powder is put into moulding press mould to be added magnetic field and is orientated, magnetic field intensity is 16000Gs, compressing after orientation, also Vacuum Package of demagnetization, put into isostatic pressing machine by the green compact of Vacuum Package and be forced into 220Mpa, pressurize after 2 minutes, obtains neodymium iron boron base substrate.
Neodymium iron boron base substrate after the moulding that above-mentioned steps is obtained, cut rear loose the piling up in material boat of material, put into sintering furnace sintering 5 hours at the temperature of 1035 DEG C, and at 900 DEG C tempering after 3 hours argon gas air-cooled, after neodymium iron boron base substrate after air-cooled is warming up to 520 DEG C again, tempering 2 hours, obtains neodymium iron boron magnetic body.
The neodymium iron boron magnetic body that above-mentioned steps is obtained is observed, result is referring to Fig. 2, Fig. 2 is the metallurgical microstructrue figure of the neodymium iron boron magnetic body prepared of comparative example 2 of the present invention, and the neodymium iron boron magnetic body crystal grain that comparative example 2 prepares is as can be seen from Figure 2 larger, and average grain size is 7.60 μ m.
Sintered NdFeB magnet prepared by said method is processed into the sample of D10*10, carry out Performance Detection, adopt NIM-10000 magnetic material measuring system test magnetic property, test result is referring to table 1, and table 1 is the performance data table of the Sintered NdFeB magnet of comparative example 1～2 and embodiment 1～3 preparation.
Embodiment 1
First, according to mass percent composition Pr-Nd:32.3wt%, Dy:0.5wt%, Al:0.45wt%, B:1.0wt%, Cu:0.1wt%, Co:0.7wt%, Zr:0.06wt% and Fe:64.89wt% take; The wherein content 24wt% of Pr in Pr-Nd alloy, B adds with the form of B-Fe alloy, and the content of B in B-Fe alloy is 18wt%; Dy adds with the form of Dy-Fe alloy, and the content of Dy in Dy-Fe alloy is 78wt%; Zr adds with the form of Zr-Fe alloy, and the content of Zr in Zr-Fe alloy is 80wt%, and other raw materials are analytically pure metal.For ensureing that in product, each alloying element content is stable, need estimate in advance the actual consume of raw material, the actual quality that weighs each element is, Pr-Nd alloy: 32.3kg, Dy-Fe alloy: 0.64kg, Al:0.45kg, B-Fe alloy: 5.56kg, Cu:0.1kg, Co:0.7kg, Zr-Fe alloy: 0.075kg, Fe:60.175kg.
Above-mentioned raw material are put into vacuum melting furnace, under the condition of 1300 DEG C of vacuum degree 2Pa and temperature, after fusing, pour into a mould completely, after cast, obtain the neodymium iron boron ingot casting that thickness is 20mm.Above-mentioned ingot casting is carried out to homogenizing processing, at the vacuum condition of 4Pa, temperature is risen to 1050 DEG C, the heating-up time is 2.5 hours, then constant temperature is after 4 hours, and applying argon gas air blast is cooled to 30 DEG C, obtains homogenizing neodymium iron boron ingot casting after treatment.
The neodymium iron boron ingot casting obtaining of above-mentioned steps is inserted in rotation hydrogen crushing furnace, in hydrogen crushing furnace, pass into hydrogen until furnace pressure reaches after 0.1Mpa, dehydrogenation after hydrogen crushing furnace is warming up to 580 DEG C, neodymium iron boron ingot casting after dehydrogenation is put into airflow milling powder process, controlling particle size is 3～5 μ m, average particle size is 3.6 μ m, then the powder after airflow milling is mixed to powder and processes 45min, obtains neodymium iron boron powder.
Neodymium iron boron powder is put into moulding press mould to be added magnetic field and is orientated, magnetic field intensity is 16000Gs, compressing after orientation, also Vacuum Package of demagnetization, put into isostatic pressing machine by the green compact of Vacuum Package and be forced into 220Mpa, pressurize after 2 minutes, obtains neodymium iron boron base substrate.
Neodymium iron boron base substrate after the moulding that above-mentioned steps is obtained, cut rear loose the piling up in material boat of material, put into sintering furnace sintering 5 hours at the temperature of 1035 DEG C, and at 900 DEG C tempering after 3 hours argon gas air-cooled, after neodymium iron boron base substrate after air-cooled is warming up to 520 DEG C again, tempering 2 hours, obtains neodymium iron boron magnetic body.
The neodymium iron boron magnetic body that above-mentioned steps is obtained is observed, result is referring to Fig. 3, Fig. 3 is the metallurgical microstructrue figure of the neodymium iron boron magnetic body prepared of the embodiment of the present invention 1, the neodymium iron boron magnetic body crystal grain densification that the present embodiment prepares as can be seen from Figure 3, and average grain size is 5.84 μ m.
Sintered NdFeB magnet prepared by said method is processed into the sample of D10*10, carry out Performance Detection, adopt NIM-10000 magnetic material measuring system test magnetic property, test result is referring to table 1, and table 1 is the performance data table of the Sintered NdFeB magnet of comparative example 1～2 and embodiment 1～3 preparation.
Referring to table 2, the standard variance table of the magnetic property of the Sintered NdFeB magnet that table 2 is prepared for comparative example 1 and embodiment 1.
Embodiment 2
First, according to mass percent composition Pr-Nd:32.0wt%, Dy:0.5wt%, Al:0.45wt%, B:1.0wt%, Cu:0.1wt%, Co:0.7wt%, Zr:0.04wt% and Fe:65.21wt% take; The wherein content 24wt% of Pr in Pr-Nd alloy, B adds with the form of B-Fe alloy, and the content of B in B-Fe alloy is 18wt%; Dy adds with the form of Dy-Fe alloy, and the content of Dy in Dy-Fe alloy is 78wt%; Zr adds with the form of Zr-Fe alloy, and the content of Zr in Zr-Fe alloy is 80wt%, and other raw materials are analytically pure metal.For ensureing that in product, each alloying element content is stable, need estimate in advance the actual consume of raw material, the actual quality that weighs each element is, Pr-Nd alloy: 32.0kg, Dy-Fe alloy: 0.64kg, Al:0.45kg, B-Fe alloy: 5.56kg, Cu:0.1kg, Co:0.7kg, Zr-Fe alloy: 0.05kg, Fe:60.5kg.
Above-mentioned raw material are put into vacuum melting furnace, under the condition of 1350 DEG C of vacuum degree 50Pa and temperature, after fusing, pour into a mould completely, after cast, obtain the neodymium iron boron ingot casting that thickness is 22mm.Above-mentioned ingot casting is carried out to homogenizing processing, at the vacuum condition of 200Pa, temperature is risen to 1050 DEG C, the heating-up time is 2.5 hours, then constant temperature is after 4 hours, and applying argon gas air blast is cooled to 30 DEG C, obtains homogenizing neodymium iron boron ingot casting after treatment.
The neodymium iron boron ingot casting obtaining of above-mentioned steps is inserted in rotation hydrogen crushing furnace, in hydrogen crushing furnace, pass into hydrogen until furnace pressure reaches after 0.1Mpa, dehydrogenation after hydrogen crushing furnace is warming up to 580 DEG C, neodymium iron boron ingot casting after dehydrogenation is put into airflow milling powder process, controlling particle size is 3～8 μ m, average particle size is 4.0 μ m, then the powder after airflow milling is mixed to powder and processes 45min, obtains neodymium iron boron powder.
Neodymium iron boron powder is put into moulding press mould to be added magnetic field and is orientated, magnetic field intensity is 16000Gs, compressing after orientation, also Vacuum Package of demagnetization, put into isostatic pressing machine by the green compact of Vacuum Package and be forced into 220Mpa, pressurize after 2 minutes, obtains neodymium iron boron base substrate.
Neodymium iron boron base substrate after the moulding that above-mentioned steps is obtained, cut rear loose the piling up in material boat of material, put into sintering furnace sintering 5 hours at the temperature of 1035 DEG C, and at 900 DEG C tempering after 3 hours argon gas air-cooled, after neodymium iron boron base substrate after air-cooled is warming up to 520 DEG C again, tempering 2 hours, obtains neodymium iron boron magnetic body.
The neodymium iron boron magnetic body that above-mentioned steps is obtained is observed, result is referring to Fig. 4, Fig. 4 is the metallurgical microstructrue figure of the neodymium iron boron magnetic body prepared of the embodiment of the present invention 2, the neodymium iron boron magnetic body crystal grain densification that the present embodiment prepares as can be seen from Figure 4, and average grain size is 5.92 μ m.
Sintered NdFeB magnet prepared by said method is processed into the sample of D10*10, carry out Performance Detection, adopt NIM-10000 magnetic material measuring system test magnetic property, test result is referring to table 1, and table 1 is the performance data table of the Sintered NdFeB magnet of comparative example 1～2 and embodiment 1～3 preparation.
Embodiment 3
First, according to mass percent composition Pr-Nd:32.0wt%, Dy:0.5wt%, Al:0.45wt%, B:1.0wt%, Cu:0.1wt%, Co:0.7wt%, Zr:0.06wt% and Fe:65.21wt% take; The wherein content 24wt% of Pr in Pr-Nd alloy, B adds with the form of B-Fe alloy, and the content of B in B-Fe alloy is 18wt%; Dy adds with the form of Dy-Fe alloy, and the content of Dy in Dy-Fe alloy is 78wt%; Zr adds with the form of Zr-Fe alloy, and the content of Zr in Zr-Fe alloy is 80wt%, and other raw materials are analytically pure metal.For ensureing that in product, each alloying element content is stable, need estimate in advance the actual consume of raw material, the actual quality that weighs each element is, Pr-Nd alloy: 32.0kg, Dy-Fe alloy: 0.64kg, Al:0.45kg, B-Fe alloy: 5.56kg, Cu:0.1kg, Co:0.7kg, Zr-Fe alloy: 0.075kg, Fe:60.475kg.
Above-mentioned raw material are put into vacuum melting furnace, under the condition of 1350 DEG C of vacuum degree 50Pa and temperature, after fusing, pour into a mould completely, after cast, obtain the neodymium iron boron ingot casting that thickness is 22mm.Above-mentioned ingot casting is carried out to homogenizing processing, at the vacuum condition of 200Pa, temperature is risen to 1050 DEG C, the heating-up time is 2.5 hours, then constant temperature is after 4 hours, and applying argon gas air blast is cooled to 30 DEG C, obtains homogenizing neodymium iron boron ingot casting after treatment.
The neodymium iron boron ingot casting obtaining of above-mentioned steps is inserted in rotation hydrogen crushing furnace, in hydrogen crushing furnace, pass into hydrogen until furnace pressure reaches after 0.1Mpa, dehydrogenation after hydrogen crushing furnace is warming up to 580 DEG C, neodymium iron boron ingot casting after dehydrogenation is put into airflow milling powder process, controlling particle size is 3～8 μ m, average particle size is 3.7 μ m, then the powder after airflow milling is mixed to powder and processes 60min, obtains neodymium iron boron powder.
Neodymium iron boron powder is put into moulding press mould to be added magnetic field and is orientated, magnetic field intensity is 16000Gs, compressing after orientation, also Vacuum Package of demagnetization, put into isostatic pressing machine by the green compact of Vacuum Package and be forced into 220Mpa, pressurize after 2 minutes, obtains neodymium iron boron base substrate.
Neodymium iron boron base substrate after the moulding that above-mentioned steps is obtained, cut rear loose the piling up in material boat of material, put into sintering furnace sintering 7 hours at the temperature of 1040 DEG C, and at 900 DEG C tempering after 3 hours argon gas air-cooled, after neodymium iron boron base substrate after air-cooled is warming up to 520 DEG C again, tempering 2 hours, obtains neodymium iron boron magnetic body.
The neodymium iron boron magnetic body that above-mentioned steps is obtained is observed, result is referring to Fig. 5, Fig. 5 is the metallurgical microstructrue figure of the neodymium iron boron magnetic body prepared of the embodiment of the present invention 3, the neodymium iron boron magnetic body crystal grain densification that the present embodiment prepares as can be seen from Figure 5, and average grain size is 5.77 μ m.
Sintered NdFeB magnet prepared by said method is processed into the sample of D10*10, carry out Performance Detection, adopt NIM-10000 magnetic material measuring system test magnetic property, test result is referring to table 1, and table 1 is the performance data table of the Sintered NdFeB magnet of comparative example 1～2 and embodiment 1～3 preparation.
The performance data table of the Sintered NdFeB magnet of table 1 comparative example 1～2 and embodiment 1～3 preparation
As can be seen from the above data, in embodiment 1, add Zr-Fe alloy and can significantly improve HCJ Hcj and Hk/Hcj, and add the effect that the effect of Zr-Fe alloy is better than adding Zr metal.
The embodiment 1 that adds Zr-Fe alloy is contrasted with the standard variance of magnetic property of the comparative example 1 that does not add Zr, in table 2, the standard variance table of the magnetic property of the Sintered NdFeB magnet that table 2 is prepared for comparative example 1 and embodiment 1.
The standard variance table of the magnetic property of Sintered NdFeB magnet prepared by table 2 comparative example 1 and embodiment 1
| σ/Br | σ/Hcb | σ/Hcj | σ/(BH)m | σ/Hk | σ/(Hk/Hcj) | |
| Comparative example 1 | 0.064 | 0.077 | 0.120 | 0.402 | 0.235 | 0.012 |
| Embodiment 1 | 0.025 | 0.046 | 0.091 | 0.234 | 0.147 | 0.006 |
As can be seen from the above data, in embodiment 1, the standard variance of the magnetic property of the neodymium iron boron magnetic body of Zr-Fe alloy is far smaller than the standard variance that does not add the neodymium iron boron magnetic body of Zr element in comparative example 1, and the standard variance of Br, Hcb, Hcj, (BH) m, Hk, Hk/Hcj has reduced respectively 60.93%, 40.25%, 24.17%, 41.79%, 34.45%, 50%.The significantly reduction of every magnetic property standard variance has shown that the interpolation of Zr element has improved the stability of magnet performance significantly.
Above a kind of neodymium iron boron magnetic body provided by the invention and preparation method thereof is described in detail; having applied specific case herein sets forth principle of the present invention and execution mode; the explanation of above embodiment is just for helping to understand method of the present invention and core concept thereof; should be understood that; for those skilled in the art; under the premise without departing from the principles of the invention; can also carry out some improvement and modification to the present invention, these improvement and modification also fall in the protection range of the claims in the present invention.
Claims (10)
1. a neodymium iron boron magnetic body, is characterized in that, composition comprises by mass percentage:
Pr-Nd：29％～33％；
B：0.97％～1.5％；
Dy：0.4％～0.6％；
Al：0.2％～0.8％；
Co：0.6％～0.8％；
Cu：0.01％～0.5％；
Zr：0.01％～0.2％；
Surplus is Fe.
2. neodymium iron boron magnetic body according to claim 1, is characterized in that, comprises 0.01%～0.099% Zr.
3. a preparation method for neodymium iron boron magnetic body, comprises the following steps:
A), under vacuum condition, Pr-Nd alloy, Zr-Fe alloy, B-Fe alloy, Dy-Fe alloy, aluminium, cobalt, copper and iron melting are prepared to neodymium iron boron ingot casting;
B) by steps A) the neodymium iron boron ingot casting that obtains after powder process, obtain neodymium iron boron powder;
C) by after above-mentioned neodymium iron boron powder sintering, obtain neodymium iron boron magnetic body.
4. preparation method according to claim 3, is characterized in that, the mass percentage content of the Pr in described Pr-Nd alloy is 23.0%～27.0%; In described Zr-Fe alloy, the mass percentage content of Zr is 77.0%～82.0%; In described B-Fe alloy, the mass percentage content of B is 17.0%～20.0%; In described Dy-Fe alloy, the mass percentage content of Dy is 77.0%～82.0%.
5. preparation method according to claim 3, is characterized in that, the thickness of described neodymium iron boron ingot casting is less than or equal to 27mm.
6. preparation method according to claim 3, is characterized in that, the granularity of described neodymium iron boron powder is 2～15 μ m.
7. preparation method according to claim 3, is characterized in that, described steps A) also comprise, under vacuum condition, the neodymium iron boron ingot casting that melting is prepared heats up, constant temperature and cooling processing.
8. preparation method according to claim 7, is characterized in that, the temperature after described intensification is 1000～1100 DEG C, and described cooled temperature is 20～80 DEG C.
9. preparation method according to claim 7, is characterized in that, the time of described intensification is 2～4 hours, and the time of described constant temperature is 3～5 hours.
10. preparation method according to claim 3, is characterized in that, described step C) be specially:
C1) above-mentioned neodymium iron boron powder is fired 5～7 hours at the first temperature, then at the second temperature, carried out tempering 3～5 hours, obtain green compact after cooling;
C2) green compact that above-mentioned steps obtained tempering 2～6 hours at the 3rd temperature, obtains neodymium iron boron magnetic body;
Described the first temperature is 1020～1050 DEG C, and described cooled temperature is 20～80 DEG C;
Described the second temperature is 850～950 DEG C, and described the 3rd temperature is 400～650 DEG C.
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| CN105679482A (en) * | 2016-04-18 | 2016-06-15 | 赣州诚博科技服务有限公司 | NdFeB permanent magnet material and preparation method thereof |
| CN106128671A (en) * | 2016-06-16 | 2016-11-16 | 宁波雄海稀土速凝技术有限公司 | High-performance Ne-Fe-B permanent-magnet material and preparation method thereof |
| CN106486281A (en) * | 2016-10-20 | 2017-03-08 | 重庆科技学院 | The preparation method of anisotropy Nanocrystalline NdFeB densification permanent magnet |
| CN106486281B (en) * | 2016-10-20 | 2017-12-15 | 重庆科技学院 | The preparation method of anisotropy Nanocrystalline NdFeB densification permanent magnet |
| CN107887091A (en) * | 2017-11-15 | 2018-04-06 | 宁德市星宇科技有限公司 | A kind of neodymium iron boron magnetic body containing dysprosium and its method for preparation |
| CN109686524A (en) * | 2019-01-14 | 2019-04-26 | 安徽包钢稀土永磁合金制造有限责任公司 | A kind of preparation method of Sintered NdFeB magnet slab |
| CN112582121A (en) * | 2019-09-27 | 2021-03-30 | 河北泛磁聚智电子元件制造有限公司 | Preparation method of ultrahigh-performance sintered samarium-cobalt magnet |
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