CN100514512C - Re-Fe-B base high performance nano composite permanent magnetic material containing titanium and carbon - Google Patents

Re-Fe-B base high performance nano composite permanent magnetic material containing titanium and carbon Download PDF

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Publication number
CN100514512C
CN100514512C CNB2006100316531A CN200610031653A CN100514512C CN 100514512 C CN100514512 C CN 100514512C CN B2006100316531 A CNB2006100316531 A CN B2006100316531A CN 200610031653 A CN200610031653 A CN 200610031653A CN 100514512 C CN100514512 C CN 100514512C
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nano composite
magnetic material
permanent magnetic
carbon
titaniferous
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CNB2006100316531A
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CN1858861A (en
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白书欣
张虹
陈柯
李顺
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National University of Defense Technology
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National University of Defense Technology
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Abstract

This invention relates to a Re-Fe-B base high performance nm compound permanent magent material of high magnet performance, low B content and high coercive force and obviously fined grains expressed by a general formula: RxFe100-x-y-z-wByTizCw, in which, R is a kind of rare earth element without La and Ce, the mol fraction x, y, z and w meet the inequalities: 4<=x<=11, 7<=y<= 9.95, 0.5<= z<= 10, 0.05<w<=3 and y+w<=10.

Description

The Re-Fe-B base high performance nano composite permanent magnetic material of titaniferous, carbon
Technical field
The present invention relates to a kind of permanent magnet that is applicable to all kinds motor and driver, relate in particular to a kind of Re-Fe-B base high performance nano composite permanent magnetic material.
Background technology
Permanent magnetic material has become the important material bases in field such as modern science and technology such as computer technology, information technology, aeronautical and space technology, the communication technology, has important effect in the national economic development.Recently more and more need further to reduce the performance of electronic equipment, business automation equipment and various other types electronic equipments and further reduce its size and weight.For this reason, when using permanent magnetic material, need its performance and weight ratio to reach best as the magnetic circuit component of these equipment.
Permanent magnetic material commonly used at present mainly contains ferrite permanent-magnet materials, Sm-Co series permanent magnetic material and NdFeB series permanent magnetic material.The main feature of ferrite permanent-magnet materials is that raw material resources is abundant, and price is low, but magnetic property is not high, when using ferrite as the magnetic circuit of the said equipment, can not make its performance and weight ratio reach best.Sm-Co series permanent magnetic material magnetic property is good, the Curie temperature height, and temperature stability is good, can satisfy the requirement of above-mentioned magnetic circuit to magnetic property, but contain strategic Elements C o, thereby cost an arm and a leg.The Nd-Fe-B series permanent magnetic material is made up of the Fe of relative low price, the performance height, and price is cheaply more a lot of than the basic magnet of Sm-Co, has therefore obtained using widely.The Nd-Fe-B series permanent magnetic material mainly contains sintered nd-fe-b magnet and mixes the bonded permanent magnet two big classes that form by magnetic and resinoid bond.The used magnetic of bonded permanent magnet is generally used the fast melt-quenching explained hereafter.
According to the difference of phase structure, the Nd-Fe-B of fast melt-quenching base magnetic is Nd for dividing content of rare earth 2Fe 14The single-phase magnetic and the content of rare earth of the normal composition of B are lower than Re 2Fe 14The nano combined magnetic normal composition of B, that contain the soft magnetism phase.
In order to improve the magnetic property that Nd-Fe-B is the fast melt-quenching magnetic, can in raw alloy, mix the element and at least a element that is selected from Ti, V and Cr that add at least a Zr of being selected from, Nb, Mo, Hf, Ta and W, when these elements add in the raw alloy, improved the coercive force of magnet.
Contain the nano combined magnetic of soft magnetism phase owing to be difficult to obtain desirable nano composite structure, performance can not reach the magnetic property of single-phase magnetic always.With the rare-earth-iron-boron is that basic nano composite rare earth permanent magnet mainly contains Re by the system branch 2Fe 14B/ α-Fe system and Re 2Fe 14B/Fe 3B system etc., preparation technology obtains amorphous thin ribbon by fast quenching, and annealing obtains the strip and the magnetic of nanocrystalline structure then, is used to prepare bonded permanent magnet.Re 2Fe 14B/ α-Fe is the saturation magnetization height of nano composite permanent magnetic permanent magnetism powder, has higher magnetic property in theory, also industrialization of magnetic at present, use also more and more widely, but actual poor-performing mainly is because α-Fe wherein is easy to nucleation and grows up unusually at the annealing process generation crystal grain of postorder easily in the fast solidification technology process, has exceeded the scope of nanoscale, be unfavorable for the generation of the exchange-coupling interaction that soft or hard magnetic is alternate, cause coercive force on the low side.Re 2Fe 14B/Fe 3B is that magnetic does not also have industrialization at present, mainly is that hard magnetic property is very poor because Re content is when low, and Re content (surpassing 5%) forms soft magnetism Re when higher easily 2Fe 23B 3Phase reduces the Hard Magnetic phase content, and hard magnetic property is also poor, thereby is difficult to improve coercive force and comprehensive magnetic property by the content that improves Re.But Re 2Fe 14B/Fe 3B is that advantage is that the B constituent content is higher, and the amorphous formation ability of system is strong, can obtain tiny and uniform nanocrystalline structure after the annealing.
For this reason, improve nano composite permanent magnetic material amorphous formation ability, suppress α-Fe in process of setting separate out and too growing up during crystallization process is the key of the good magnetic property of acquisition.Based on this, publication number is that the Chinese patent of CN1461486A has proposed that a kind of to have general formula be (Fe 1-mT m) 100-x-y-zQ xR yTi zThe Nanocomposite magnet of represented composition, wherein T is Co and/or Ni, Q is B and/or C, and R is not for comprising the rare earth element of La or Ce basically.Publication number is that the Chinese patent of CN1484837A has proposed that a kind of to have general formula be (Fe 1-mT m) 100-x-y-z-nQ xR yTi zM nThe Nanocomposite magnet of represented composition, wherein T is at least a element that is selected from Co and Ni, Q is at least a element that is selected from B and C, R is at least a rare earth element that generally includes a kind of of Nd and Pr at least and optionally comprise Dy and/or Tb, and M is at least a element that is selected from Al, Si, V, Cr, Mn, Cu, Zn, Ga, Zr, Nb, Mo, Ag, Hf, Ta, W, Pt, Au and Pb.This two China's patent is pointed out, the raising of B constituent content has increased the amorphous formation ability of system, the interpolation of Ti or other metallic elements has suppressed alloy the growing up unusually of α-Fe phase crystallite dimension in rapid solidification and follow-up heat treatment process, optimized the microstructure of magnet, thereby obtained industrially can be applied to actual high-coercive force (coercive force 〉=480kA/m).And point out that the gained Nanocomposite magnet is by Hard Magnetic phase R 2Fe 14Q and be present in R 2Fe 14Soft magnetism phase iron-based boride on the interface between the Q type compound crystal grain and a spot of soft magnetism α-Fe phase crystal grain is formed.But this two China's patent is pointed out emphatically simultaneously, in the Nanocomposite magnet of given composition the content of B element can not be lower than 10at%, otherwise magnet can not obtain sufficiently highly can be applied to actual magnetic property.
Summary of the invention
The technical problem to be solved in the present invention is the shortcoming that overcomes prior art, provides a kind of boron content low and coercive force height, the obvious refinement of crystal grain, the Re-Fe-B base high performance nano composite permanent magnetic material of the titaniferous that magnetic property is high, carbon.
Technical scheme of the present invention is: the Re-Fe-B base high performance nano composite permanent magnetic material of a kind of titaniferous, carbon has general formula R e xFe 100-x-y-z-wB yTi zC wRepresented composition, wherein Re is at least a rare earth element that does not comprise La, Ce, molar fraction x, y, z and w satisfy inequality respectively:
4≤x≤11；
7≤y≤9.95；
0.5≤z≤10; With
0.05<w≤3；
y+w≤10。
Described microscopic structure comprises two or more ferromagnetic crystalline phases at least, and a kind of ferromagnetic crystalline phase wherein is at least the Hard Magnetic phase, another kind is at least the soft magnetism phase, and the average grain size of Hard Magnetic phase is 5nm to 50nm, and the average grain size of soft magnetism phase is 1nm to 50nm.
Described Hard Magnetic comprises Re mutually at least 2Fe 14The B phase.
The powder of described nano composite permanent magnetic material demonstrates remanent magnetism 0.7T at least, and coercivity H i is the hard magnetic property of 500kA/m at least.
Described material can be heat-treated the alloy with nanometer soft or hard magnetic phase composite construction that generation obtains for rapidly solidified alloy with nanometer soft or hard magnetic phase composite construction or to the amorphous rapidly solidified alloy after amorphous rapidly solidified alloy or the fragmentation.
Described material can be thickness 10 μ m to 200 μ m, and width is the thin band shape of 3mm to 10mm.
Described material also can be fractured into the powder that average grain diameter is 10 μ m to 350 μ m.
Described material can also be bonded permanent magnet that above-mentioned powder is obtained by mold pressing or injection or extrusion molding or the compactness magnet that above-mentioned powder is formed through hot pressing, thermal deformation.
The inventor found through experiments by a certain amount of Ti element and C element unite interpolation after, obviously refinement crystallite dimension, be lower than at the content of B element under the situation of 10at% and also can obtain desirable composite construction, the coercive force raising of material (coercive force 〉=500kA/m), its remanent magnetism has the desired magnetic property of commercial Application greater than 0.7T simultaneously.
Its preparation method is: (1) adopts vacuum induction melting composition (atomic percentage) is Re xFe 100-x-y-z-wB yTi zC wAlloy, Re is at least a rare earth element that does not comprise La, Ce, molar fraction x, y, z and w satisfy 4≤x≤10,7≤y＜10,0.5≤z≤10,0.05＜w≤8, y+w≤10 respectively; (2) prepared alloy is put into crucible, place the single roller melt of vacuum to get rid of radio-frequency induction coil in the band machine chamber, the distance of crucible bottom from copper roller surface is 3～10mm; (3) feeding argon gas makes the pressure that gets rid of in the band machine cavity in the scope of 10kPa to 90kPa, regulate in the crucible and melt gets rid of pressure differential in the band machine chamber, with radio-frequency induction coil heating and fusing sample, under 60～100kPa argon pressure difference, be on 20～30m/s copper roller rotating to linear velocity with melt jet, obtain the about 10 μ m of thickness to about 200 μ m, the alloy thin band of the about 3mm to 10mm of width; (4) with this alloy thin band at 650 ℃～800 ℃ following heat treatment 1～20min, prepare the nano composite permanent magnetic material strip; (5) the broken strip of method that adopts gas or machinery obtains the nano composite permanent magnetic material magnetic to the about 10 μ m of particle diameter～350 μ m; (6) Magnaglo mixes the bonded permanent magnet that obtains by mold pressing or injection or extrusion molding with binding agent.(7) magnetic forms compactness magnet through hot pressing, thermal deformation mode.
Contain Ti and C simultaneously in its composition of nano composite permanent magnetic material of the present invention, the raw alloy of this composition is easy to decrystallized under the rapid solidification mode, when raw alloy contains crystalline phase hardly with the cooling of 20～30m/s speed with after solidifying, can make the amorphous phase crystallization by Technology for Heating Processing subsequently.
The inventor found through experiments and confirms, when adding Ti, and the crystal growth minimum of α-Fe in the melt cools, and to the contributive Re of obtaining magnet hard magnetic property 2Fe 14B phase crystal grain can be preferentially nucleating growth equably; The interpolation of C can remedy Ti and add back TiB 2Phase be formed on the hard magnetic phase Re that causes to a certain extent 2Fe 14The reduction of B volumn concentration, and can crystal grain thinning, optimize the microstructure of magnet.
Description of drawings
Fig. 1 is the used fast melt-quenching device of an embodiment schematic diagram;
Fig. 2 is the TEM photo of high performance nano composite permanent magnetic body.
Embodiment
Embodiment 1
(1) according to alloying component Nd 9Fe 79B 8Ti 3C 1Preparing raw material, is the 500g raw material by B, the 3at%Ti of Fe, the 8at% of Nd, the 79at% of 9at%, the C preparation total amount of 1at% promptly, and they are put into crucible, adopts vaccum sensitive stove to be smelted into Nd under the high-purity Ar protective atmosphere 9Fe 79B 8Ti 3C 1Alloy, and cast in and obtain alloy cast ingot on the water cooled copper mould; (2) as shown in Figure 1, (1) prepared alloy is put into quartz ampoule 1, place the single roller melt of vacuum to get rid of the interior radio-frequency induction coil 2 of band machine cavity, the quartz ampoule bottom is 5mm from the distance of copper roller; (3) be evacuated to 5 * 10 -2Close the vacuum unit behind the pa, feed argon gas, making the pressure that gets rid of the argon gas in the band machine cavity is 50kPa, behind the alloy in radio-frequency induction coil heating and the fused quartz pipe, being on the 25m/s copper roller rotating 3 with melt jet to linear velocity under the 200kPa pressure differential, obtain alloy thin band 4; (4) alloy thin band that (3) are made can obtain the hard magnetic phase Nd by nanoscale at 740 ℃ of following heat treatment 6min 2Fe 14The soft magnetism of B and nanoscale is the permanent magnetic material strip of α-Fe composite construction (see figure 2) mutually; (5) it is 0.936T that the nano composite permanent magnetic strip of preparing is broken into its remanent magnetism of powder, coercive force H CiBe 1050.4kA/m, magnetic energy product reaches 148.77kJ/m 3
Embodiment 2
(1) according to alloying component Nd 8Fe 80B 8Ti 2C 2Preparing raw material, is the 500g raw material by B, the 2at%Ti of Fe, the 8at% of Nd, the 80at% of 8at%, the C preparation total amount of 2at% promptly, and they are put into crucible, adopts vaccum sensitive stove to be smelted into Nd under the high-purity Ar protective atmosphere 8Fe 80B 8Ti 2C 2Alloy, and cast in and obtain alloy cast ingot on the water cooled copper mould; (2) (1) prepared alloy is put into quartz ampoule, place the single roller melt of vacuum to get rid of the interior radio-frequency induction coil of band machine cavity, the quartz ampoule bottom is 5mm from the distance of copper roller; (3) be evacuated to 5 * 10 -2Close the vacuum unit behind the pa, feed argon gas, making the pressure that gets rid of the argon gas in the band machine cavity is 50kPa, behind the alloy in radio-frequency induction coil heating and the fused quartz pipe, being on the 25m/s copper roller rotating with melt jet to linear velocity under the 200kPa pressure differential, obtain alloy thin band; (4) alloy thin band that (3) are made can obtain the permanent magnetic material strip by nano composite structure at 730 ℃ of following heat treatment 10min; (5) it is 1.1T that the nano composite permanent magnetic strip of preparing is broken into its remanent magnetism of powder that particle diameter is about 200 μ m, coercive force H CiBe 640KA/m, magnetic energy product reaches 168kJ/m 3
Embodiment 3
(1) according to alloying component Pr 9Fe 78B 8Ti 3C 2Preparing raw material, is the 500g raw material by B, the 3at%Ti of Fe, the 8at% of Pr, the 78at% of 9at%, the C preparation total amount of 2at% promptly, and they are put into the crucible of vacuum induction melting furnace, is evacuated to 5 * 10 earlier -2Pa feeds high-purity argon gas, to induction coil energising melt raw material, is smelted into Pr then 9Fe 78B 8Ti 3C 2Alloy, and cast in and obtain alloy cast ingot on the water cooled copper mould; (2) (1) prepared alloy cast ingot is put into quartz ampoule, place the single roller melt of vacuum to get rid of the interior radio-frequency induction coil of band machine cavity, the quartz ampoule bottom is 5mm from the distance of copper roller; (3) be evacuated to 5 * 10 -2Close the vacuum unit behind the pa, feed argon gas, making the pressure that gets rid of the argon gas in the band machine cavity is 50kPa, behind the alloy in radio-frequency induction coil heating and the fused quartz pipe, being on the 20m/s copper roller rotating with melt jet to linear velocity under the 200kPa pressure differential, obtain alloy thin band; (4) alloy thin band that (3) are made can obtain the hard magnetic phase Pr by nanoscale at 720 ℃ of following heat treatment 6min 2Fe 14The soft magnetism of B and nanoscale is the permanent magnetic material strip of α-Fe composite construction mutually; (5) it is 0.90T that the nano composite permanent magnetic strip of preparing is broken into its remanent magnetism of powder, coercive force H CiBe 720kA/m, magnetic energy product reaches 120kJ/m 3
Embodiment 4
(1) according to alloying component (Nd0.5Pr0.5) 11Fe 78B 7Ti 3C 1Prepare raw material, promptly preparing total amount by the C of B, the 3at%Ti of Fe, the 7at% of Nd, the 78at% of Pr, the 0.5 * 11at% of 0.5 * 11at%, 1at% is the 500g raw material, and they are put into the crucible of vacuum induction melting furnace, is evacuated to 5 * 10 earlier -2Pa feeds high-purity argon gas, to induction coil energising melt raw material, is smelted into (Nd0.5Pr0.5) then 11Fe 78B 7Ti 3C 1Alloy, and cast in and obtain alloy cast ingot on the water cooled copper mould; (2) (1) prepared alloy cast ingot is put into quartz ampoule, place the single roller melt of vacuum to get rid of the interior radio-frequency induction coil of band machine cavity, the quartz ampoule bottom is 5mm from the distance of copper roller; (3) be evacuated to 5 * 10 -2Close the vacuum unit behind the pa, feed argon gas, making the pressure that gets rid of the argon gas in the band machine cavity is 50kPa, behind the alloy in radio-frequency induction coil heating and the fused quartz pipe, being on the 20m/s copper roller rotating with melt jet to linear velocity under the 200kPa pressure differential, obtain alloy thin band; (4) alloy thin band that (3) are made can obtain the hard magnetic phase Pr by nanoscale at 740 ℃ of following heat treatment 6min 2Fe 14The soft magnetism of B and nanoscale is the permanent magnetic material strip of α-Fe composite construction mutually; (5) it is 0.92T that the nano composite permanent magnetic strip of preparing is broken into its remanent magnetism of powder, coercive force H Ci690kA/m, magnetic energy product reaches 120kJ/m 3

Claims (9)

1. the Re-Fe-B of a titaniferous, carbon base nano composite permanent magnetic material is characterized in that it has general formula R e xFe 100-x-y-z-wB yTi zC wRepresented composition, wherein Re is at least a rare earth element that does not comprise La, Ce, molar fraction x, y, z and w satisfy inequality respectively:
4≤x≤11；
7≤y≤9.95；
0.5≤z≤10; With
0.05<w≤3；
y+w≤10。
2. the Re-Fe-B base nano composite permanent magnetic material of titaniferous according to claim 1, carbon, it is characterized in that: the microscopic structure of the Re-Fe-B base nano composite permanent magnetic material of described titaniferous, carbon comprises plural ferromagnetic crystalline phase, in the described ferromagnetic crystalline phase, have at least one to be the Hard Magnetic phase, have at least one to be the soft magnetism phase, the average grain size of Hard Magnetic phase is 5nm to 50nm, and the average grain size of soft magnetism phase is 1nm to 50nm.
3. the Re-Fe-B base nano composite permanent magnetic material of titaniferous according to claim 2, carbon, it is characterized in that: described Hard Magnetic comprises Re mutually at least 2Fe 14The B phase.
4. according to the arbitrary described titaniferous of claim 1 to 3, the Re-Fe-B base nano composite permanent magnetic material of carbon, it is characterized in that: the powder of described nano composite permanent magnetic material demonstrates remanent magnetism 0.7T at least, and coercivity H i is the hard magnetic property of 500kA/m at least.
5. according to the Re-Fe-B base nano composite permanent magnetic material of the arbitrary described titaniferous of claim 1 to 3, carbon, it is characterized in that: described material is to have the rapidly solidified alloy of nanometer soft or hard magnetic phase composite construction or the amorphous rapidly solidified alloy after amorphous rapidly solidified alloy or the fragmentation heat-treated the alloy with nanometer soft or hard magnetic phase composite construction that is obtained.
6. according to the arbitrary described titaniferous of claim 1 to 3, the Re-Fe-B base nano composite permanent magnetic material of carbon, it is characterized in that: described material is thickness 10 μ m to 200 μ m, and width is the thin band shape of 3mm to 10mm.
7. the Re-Fe-B of a titaniferous, carbon base nano composite permanent magnetic material powder, it is characterized in that: this powder is to be formed by the thin band fragmentation of the basic nano composite permanent magnetic material of the Re-Fe-B of the described titaniferous of claim 6, carbon, and the average grain diameter of powder is 10 μ m to 350 μ m.
8. the Re-Fe-B of a titaniferous, carbon base nano composite permanent magnetic material bonded permanent magnet is characterized in that this bonded permanent magnet is that Re-Fe-B base nano composite permanent magnetic material powder by the described titaniferous of claim 7, carbon is through mold pressing or injection or extrusion molding and get.
9. the Re-Fe-B of a titaniferous, carbon base nano composite permanent magnetic material compactness magnet is characterized in that this compactness magnet is to be formed through hot pressing, thermal deformation by the Re-Fe-B base nano composite permanent magnetic material powder of the described titaniferous of claim 7, carbon.
CNB2006100316531A 2006-05-16 2006-05-16 Re-Fe-B base high performance nano composite permanent magnetic material containing titanium and carbon Expired - Fee Related CN100514512C (en)

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CN108701517B (en) * 2016-03-17 2020-07-24 日立金属株式会社 Method for producing R-T-B sintered magnet
CN108015268A (en) * 2016-10-28 2018-05-11 龙岩紫荆创新研究院 The bonded permanent magnet that a kind of R-B-Ti-Fe alloy powders and preparation method thereof are prepared with the alloy powder

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