CN108022708A - A kind of rich cerium yttrium Nd-Fe-B permanent magnet for sintering argentiferous and preparation method thereof - Google Patents
A kind of rich cerium yttrium Nd-Fe-B permanent magnet for sintering argentiferous and preparation method thereof Download PDFInfo
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- H—ELECTRICITY
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- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
- H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
- H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
- H01F1/0577—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together sintered
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- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
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- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
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Abstract
The present invention relates to a kind of rich cerium yttrium Nd-Fe-B permanent magnet for sintering argentiferous and preparation method thereof.The chemical formula general formula of the permanent magnet is by mass percentage：(CeaYbNd100‑a‑b)x(Fe100‑ cMc)100‑x‑yBy, wherein：5≤a≤30,0.3≤b≤2,0.5≤c≤5,28.8≤x≤32.5,0.9≤y≤1.1, M are one or more of metallic elements in Ga, Si, Ti, Mn, Ni, Sn, Co, Cu, Al, Nb, Zr and Ag.The preparation method of the rich cerium yttrium Nd-Fe-B permanent magnet of the sintering argentiferous includes：Raw material preparation, rapid hardening slab, hydrogen are broken, airflow milling, oriented moulding, isostatic pressed, sintering and heat treatment step.The present invention is by adjusting formula, add Ce, Y rare earth element of high abundance, adding the Ag of certain content at the same time improves the thermal conductivity of the slab of magnet containing Ce, and it is heat-treated in sintering stage using strong magnetic two level, so as to obtain the rich cerium yttrium Nd-Fe-B permanent magnet for sintering argentiferous that comprehensive magnetic can be higher, enterprise's production cost is reduced, is comprehensively utilized rare earth resources.
Description
Technical field
The present invention relates to rare-earth permanent magnet material technical field, more particularly to a kind of low cost, heat conductivility well simultaneously
And comprehensive magnetic can be higher sintering argentiferous rich cerium yttrium Nd-Fe-B permanent magnet with and preparation method thereof.
Background technology
Sintered Nd-Fe-B magnet is widely used in nuclear-magnetism with its price compared with high comprehensive magnetic properties and relative moderate
The field such as resonance, high-performance small and special electric machine, electric automobile, aerospace navigation device, wind-power electricity generation, office automation, household electrical appliances.With
Growing and preparation process the quick renewal of the market demand, causes to prepare the PrNd needed for magnet and largely consumes, and is stored up
It is relatively low to measure Ce, La, Y utilization rate of relative abundance, causes each rare earth element application uneven, plus rare earths materials such as recent PrNd
Price fluctuation is larger so that manufacturing enterprise's cost of raw material faces very big restriction.
Under the multiple pressure of environment, resource and cost, the light rare earth elements such as exploitation high abundance, inexpensive Ce, La, Y
It is always industry research hot spot to prepare Ce-Nd-Fe-B permanent magnets.Part PrNd is substituted to prepare work to study it by adding Ce
Skill, comprehensive magnetic energy and microcosmic mechanism, prepare the permanent magnet of low cost, meet the application field of industrial low side magnet, and will
Inexpensive Ce-Nd-Fe-B Magnet Industries application, can not only be greatly reduced cost, it is often more important that can make rare earth resources
Balanced use rate is improved.
At present, yttrium is added in sintered nd-fe-b magnet both at home and abroad also has certain research, but mass production
There is not been reported, and the relatively low (Hcj of neodymium iron boron magnetic body coercivity of the addition Y element of document report<12kGs), comprehensive magnetic energy
It is poor, meet that the possibility of the market demand is smaller.Saturated pole the intensity Js=14.1kGs, anisotropy field HA of yttrium
It is suitable with Ce, with Nd there is identical hexagonal closest packing to accumulate structure, reasonably add Y element, magnet can obtain preferable Js and
Intrinsic coercivity Hcj, and effectively improve the corrosion resistance of Nd-Fe-B permanent magnet.Such as China applies for a patent 201310314166.6
In disclose a kind of dysprosium cerium dopping neodymium iron boron magnetic body, but its corrosion resistance permanent magnet relatively produced by the present invention is poor.In another example
China discloses a kind of low-cost rare earth iron boron permanent magnet in applying for a patent 201610407554.2, pay close attention to its slab thermal conductivity
Can, it is found that its thermal conductivity is poorer than permanent magnet produced by the present invention.And the present invention is compared to above-mentioned two patent, in its system
In standby step, strong magnetic two level heat treatment is employed in sintering stage so that the comprehensive magnetic of permanent magnet can obtain very big carry
It is high.
The content of the invention
The purpose of the present invention is and addition high abundance rare earth member serious uneven for the application of rare earth element currently on the market
The problem of performance reduces after element, by adding cerium, yttrium cost declining, adding silver improves slab heat conductivility, and in sintering rank
Section takes strong magnetic heat treatment, improves the Grain-Boundary Phase of magnet microstructure, prepares the rich cerium yttrium neodymium iron of high performance sintering argentiferous
Boron permanent magnet.It is another object of the present invention to provide a kind of rich cerium yttrium Nd-Fe-B permanent magnet of inexpensive sintering argentiferous
Preparation method.
To achieve these goals, the present invention provides following technical solution：
A kind of rich cerium yttrium Nd-Fe-B permanent magnet for sintering argentiferous, it is characterised in that：The rich cerium yttrium Nd-Fe-B permanent magnet
Chemical formula general formula be by mass percentage：(CeaYbNd100-a-b)x(Fe100-cMc)100-x-yBy, wherein：5≤a≤30,0.3≤b
≤ 2,0.5≤c≤5,28.8≤x≤32.5,0.9≤y≤1.1, M be selected from Ga, Si, Ti, Mn, Ni, Sn, Co, Cu, Al, Nb,
One or more of metallic elements in Zr and Ag.
Further, the chemical formula general formula of the permanent magnet is by mass percentage：(CeaYbNd100-a-b)x(Fe100- cMc)100-x-yBy, wherein：15≤a≤25,0.5≤b≤1.5,1≤c≤3,30.5≤x≤32,0.95≤y≤1.02, M are choosing
From one or more of metallic elements in Co, Cu, Al, Nb, Zr and Ag, Ag is wherein essential element, and Ag accounts for Mc and contains
The 10%~15% of amount.
The richness cerium yttrium Nd-Fe-B permanent magnet is made by the steps：Raw material preparation, rapid hardening slab, hydrogen are broken, airflow milling, take
To shaping, sintering and heat treatment.
A kind of preparation method of above-mentioned rich cerium yttrium Nd-Fe-B permanent magnet, includes the following steps：
(1) raw material prepares：According to the rich cerium yttrium Nd-Fe-B permanent magnet mass percent chemical formula of the sintering argentiferous
(CeaYbNd100-a-b)x(Fe100-cMc)100-x-yByPreparation raw material, wherein：5≤a≤30,0.3≤b≤2,0.5≤c≤5,28.8
≤ x≤32.5,0.9≤y≤1.1, M are one kind or several in Ga, Si, Ti, Mn, Ni, Sn, Co, Cu, Al, Nb, Zr and Ag
Kind metallic element；
(2) rapid hardening slab：In argon filling pressure≤3 × 104Slab, cast temperature 1300 are carried out in the rapid hardening slab stove of Pa
~1550 DEG C, rapid hardening copper roller rotating speed 41r/min, obtain the slab that thickness is 0.15-0.3mm；
(3) hydrogen is broken and airflow milling：Obtained slab in step (2) is made averagely with airflow milling anaerobic technique using hydrogen is broken
Granularity about 2.8um, the fine powder that size distribution is d [9,0]/d [1,0] ＜ 3.8；
(4) oriented moulding：By the fine powder obtained by step (3) in the Magnetic field press of 2T oriented moulding, then carry out cold etc. quiet
Green compact are pressed into, its density is 4.2g/cm3；
(5) sinter：Green compact obtained by step (4) are placed in vacuum≤3 × 10-2Acquisition is sintered in the sintering furnace of Pa
Sintered magnet, sintering temperature are 900~1180 DEG C, 2~5h of soaking time；
(6) it is heat-treated：Sintered magnet obtained by step (5) is carried out at strong magnetic level-one tempering and strong magnetic second annealing heat
Reason, finally obtains the rich cerium yttrium Nd-Fe-B permanent magnet of sintering argentiferous；Wherein, magnet shaping differently- oriented directivity is parallel to magnetic direction,
Magnetic field intensity is 1~13T, vacuum≤5Pa of the tempering of strong magnetic level-one and strong magnetic second annealing, level-one temperature for 800~
950 DEG C, level-one tempering time is 1~3h；Second annealing temperature is 400~530 DEG C, and the second annealing time is 2~4h.
Cast temperature in the step (2) is preferably 1380~1440 DEG C.
Sintering temperature in the step (5) is preferably 1000~1045 DEG C.
When being heat-treated in the step (6) using strong magnetic level-one and strong magnetic second annealing, magnet shaping differently- oriented directivity is put down
For row in magnetic direction, magnetic field intensity is preferably 3~10T.
The advantages and positive effects of the present invention are：Using the more high abundance cerium yttrium element element of storage capacity, balance
Weight rare earth is developed.Other metallic elements are coordinated by essential Ag, formula components and slab technique is rationally adjusted, improves
The microstructure of slab, is refined crystal grain.Airflow milling technological parameter is adjusted, obtains relatively narrow particle size distribution.It is high
After temperature sintering, strong magnetic two level tempering heat treatment technique is taken, high-intensity magnetic field had both changed magnetic domain arrangement inside magnet, and obtained thin and equal
Even magnet microstructure, and make magnet finer and close, the comprehensive magnetic for improving magnet can (Hcj>12kOe), market is met
Demand.
Specific embodiment
The present invention can be further well understood by specific examples presented below.But they are not to the present invention
Restriction.
A kind of rich cerium yttrium Nd-Fe-B permanent magnet for sintering argentiferous of embodiment 1, its mass percent chemical formula general formula are：
(Ce20Y1Nd79)30.8[Fe98(Co0.2Ag0.1Cu0.1Al0.5Nb0.1)2]68.2B1, and Ag accounts for the 10% of Mc contents.
The preparation method of the rich cerium yttrium Nd-Fe-B permanent magnet of above-mentioned sintering argentiferous carries out as follows：
(1) raw material prepares：By being designed to assignment system raw material.
(2) rapid hardening slab：In argon filling pressure≤3 × 104Slab, cast temperature 1420 are carried out in the rapid hardening slab stove of Pa
DEG C, rapid hardening copper roller rotating speed 41r/min, obtains the slab that thickness is 0.15-0.3mm.
(3) hydrogen is broken and airflow milling：Obtained slab in step (2) is made averagely with airflow milling anaerobic technique using hydrogen is broken
Granularity about 2.8um, the fine powder that size distribution is d [9,0]/d [1,0]=3.5.
(4) oriented moulding：By the fine powder obtained by step (3) in the Magnetic field press of 2T oriented moulding, then carry out cold etc. quiet
Green compact are pressed into, its density is 4.2g/cm3。
(5) sinter：Green compact obtained by step (4) are placed in vacuum≤3 × 10-2Acquisition is sintered in the sintering furnace of Pa
Sintered magnet, sintering temperature are 1020 DEG C, soaking time 4.5h.
(6) it is heat-treated：Sintered magnet obtained by step (5) is carried out at strong magnetic level-one tempering and strong magnetic second annealing heat
Reason, finally obtains the rich cerium yttrium Nd-Fe-B permanent magnet of sintering argentiferous.Wherein, magnet shaping differently- oriented directivity is parallel to magnetic direction,
Magnetic field intensity is 8T, and vacuum≤5Pa of strong magnetic level-one tempering and strong magnetic second annealing, level-one temperature is 850 DEG C, level-one
Tempering time is 1.5h；Second annealing temperature is 450 DEG C, and the second annealing time is 3h.Argon filling is cooled to less than 60 DEG C, takes out and burns
Magnet is tied, obtains the N38 high-performance magnet containing Ce of intrinsic coercivity ＞ 13kOe.
By the rich cerium yttrium Nd-Fe-B permanent magnet of above-mentioned gained in 20 DEG C of progressCylinder is tested, and measures remanent magnetism
(Br), J=0.9J on the J demagnetizing curves of coercivity (Hcb), intrinsic coercivity (Hcj), magnetic energy product ((BH) max), magnetrWhen
Opposing magnetic field (Hk), squareness (Hk/Hcj), obtain data as shown in the table：
A kind of rich cerium yttrium Nd-Fe-B permanent magnet for sintering argentiferous of embodiment 2, its mass percent chemical formula general formula are：
(Ce30Y0.5Nd69.5)30.8[Fe98(Co0.2Ag0.1Cu0.1Al0.5Nb0.1)2]68.2B1, and Ag accounts for the 10% of Mc contents.
The preparation method of the rich cerium yttrium Nd-Fe-B permanent magnet of above-mentioned sintering argentiferous is identical with embodiment 1.Obtain permanent magnetism
Body, in 20 DEG C of progressCylinder is tested, measurement remanent magnetism (Br), coercivity (Hcb), intrinsic coercivity (Hcj), magnetic energy product
J=0.9J on the J demagnetizing curves of ((BH) max), magnetrWhen opposing magnetic field (Hk), squareness (Hk/Hcj), obtain such as following table
Shown data：
A kind of rich cerium yttrium Nd-Fe-B permanent magnet for sintering argentiferous of embodiment 3, its mass percent chemical formula general formula are：
(Ce20Nd80)30.8[Fe98(Co0.2Ag0.1Cu0.1Al0.5Nb0.1)2]68.2B1, and Ag accounts for the 10% of Mc contents.
The preparation method of the rich cerium yttrium Nd-Fe-B permanent magnet of above-mentioned sintering argentiferous is identical with embodiment 1.Obtain permanent magnetism
Body, in 20 DEG C of progressCylinder is tested, measurement remanent magnetism (Br), coercivity (Hcb), intrinsic coercivity (Hcj), magnetic energy product
J=0.9J on the J demagnetizing curves of ((BH) max), magnetrWhen opposing magnetic field (Hk), squareness (Hk/Hcj), obtain such as following table
Shown data：
A kind of rich cerium yttrium Nd-Fe-B permanent magnet for sintering argentiferous of embodiment 4, its mass percent chemical formula general formula are：
(Ce20Y1Nd79)30.8[Fe98(Co0.2Ag0.1Cu0.1Al0.2Zr0.3Nb0.1)2]68.2B1, and Ag accounts for the 10% of Mc contents.
The preparation method of the rich cerium yttrium Nd-Fe-B permanent magnet of above-mentioned sintering argentiferous is identical with embodiment 1.Obtain permanent magnetism
Body, in 20 DEG C of progressCylinder is tested, measurement remanent magnetism (Br), coercivity (Hcb), intrinsic coercivity (Hcj), magnetic energy product
J=0.9J on the J demagnetizing curves of ((BH) max), magnetrWhen opposing magnetic field (Hk), squareness (Hk/Hcj), obtain such as following table
Shown data：
A kind of rich cerium yttrium Nd-Fe-B permanent magnet for sintering argentiferous of embodiment 5, its mass percent chemical formula general formula are：
(Ce20Y1Nd79)30.8[Fe98(Co0.2Ag0.1Cu0.1Al0.1Si0.1Zr0.2Ti0.1Nb0.1)2]68.2B1, and Ag accounts for the 10% of Mc contents.
The preparation method of the rich cerium yttrium Nd-Fe-B permanent magnet of above-mentioned sintering argentiferous is identical with embodiment 1.Obtain permanent magnetism
Body, in 20 DEG C of progressCylinder is tested, measurement remanent magnetism (Br), coercivity (Hcb), intrinsic coercivity (Hcj), magnetic energy product
J=0.9J on the J demagnetizing curves of ((BH) max), magnetrWhen opposing magnetic field (Hk), squareness (Hk/Hcj), obtain such as following table
Shown data：
A kind of rich cerium yttrium Nd-Fe-B permanent magnet for sintering argentiferous of embodiment 6, its mass percent chemical formula general formula are：
(Ce20Y1Nd79)30.8[Fe98(Co0.3Ag0.1Al0.6)2]68.2B1, and Ag accounts for the 10% of Mc contents.
The preparation method of the rich cerium yttrium Nd-Fe-B permanent magnet of above-mentioned sintering argentiferous is identical with embodiment 1.Obtain permanent magnetism
Body, in 20 DEG C of progressCylinder is tested, measurement remanent magnetism (Br), coercivity (Hcb), intrinsic coercivity (Hcj), magnetic energy product
J=0.9J on the J demagnetizing curves of ((BH) max), magnetrWhen opposing magnetic field (Hk), squareness (Hk/Hcj), obtain such as following table
Shown data：
A kind of rich cerium yttrium Nd-Fe-B permanent magnet for sintering argentiferous of embodiment 7, its mass percent chemical formula general formula are：
(Ce20Y1Nd79)30.8[Fe98(Co0.1Ag0.15Cu0.15Al0.5Nb0.1)2]68.2B1, and Ag accounts for the 15% of Mc contents.
The preparation method of the rich cerium yttrium Nd-Fe-B permanent magnet of above-mentioned sintering argentiferous is identical with embodiment 1.Obtain permanent magnetism
Body, in 20 DEG C of progressCylinder is tested, measurement remanent magnetism (Br), coercivity (Hcb), intrinsic coercivity (Hcj), magnetic energy product
J=0.9J on the J demagnetizing curves of ((BH) max), magnetrWhen opposing magnetic field (Hk), squareness (Hk/Hcj), obtain such as following table
Shown data：
A kind of rich cerium yttrium Nd-Fe-B permanent magnet for sintering argentiferous of embodiment 8, its mass percent chemical formula general formula are：
(Ce20Y1Nd79)30.8[Fe98(Co0.1Ag0.12Cu0.18Al0.5Nb0.1)2]68.2B1, and Ag accounts for the 12% of Mc contents.
The preparation method of the rich cerium yttrium Nd-Fe-B permanent magnet of above-mentioned sintering argentiferous is identical with embodiment 1.Obtain permanent magnetism
Body, in 20 DEG C of progressCylinder is tested, measurement remanent magnetism (Br), coercivity (Hcb), intrinsic coercivity (Hcj), magnetic energy product
J=0.9J on the J demagnetizing curves of ((BH) max), magnetrWhen opposing magnetic field (Hk), squareness (Hk/Hcj), obtain such as following table
Shown data：
A kind of rich cerium yttrium Nd-Fe-B permanent magnet for sintering argentiferous of embodiment 9, its mass percent chemical formula general formula are：
(Ce20Y1Nd79)30.8[Fe98(Co0.1Ag0.2Cu0.1Al0.5Nb0.1)2]68.2B1, and Ag accounts for the 20% of Mc contents.
The preparation method of the rich cerium yttrium Nd-Fe-B permanent magnet of above-mentioned sintering argentiferous is with embodiment 1 only difference is that step
(6) when strong magnetic level-one tempering and the heat treatment of strong magnetic second annealing are carried out in the sintered magnet obtained by step (5), wherein, magnetic field
Intensity is 3T.Permanent magnet is obtained, in 20 DEG C of progressCylinder is tested, measurement remanent magnetism (Br), coercivity (Hcb), intrinsic
Coercivity (Hcj), magnetic energy product ((BH) max), magnet J demagnetizing curves on J=0.9JrWhen opposing magnetic field (Hk), squareness
(Hk/Hcj), data as shown in the table are obtained：
A kind of rich cerium yttrium Nd-Fe-B permanent magnet for sintering argentiferous of embodiment 10, its mass percent chemical formula general formula are：
(Ce20Y1Nd79)30.8[Fe98(Co0.1Ag0.15Cu0.15Al0.5Nb0.1)2]68.2B1, and Ag accounts for the 15% of Mc contents.
The preparation method of the rich cerium yttrium Nd-Fe-B permanent magnet of above-mentioned sintering argentiferous is with embodiment 1 only difference is that step
(6) when strong magnetic level-one tempering and the heat treatment of strong magnetic second annealing are carried out in the sintered magnet obtained by step (5), wherein, magnetic field
Intensity is 10T.Permanent magnet is obtained, in 20 DEG C of progressCylinder is tested, measurement remanent magnetism (Br), coercivity (Hcb), intrinsic
Coercivity (Hcj), magnetic energy product ((BH) max), magnet J demagnetizing curves on J=0.9JrWhen opposing magnetic field (Hk), squareness
(Hk/Hcj), data as shown in the table are obtained：
A kind of rich cerium yttrium Nd-Fe-B permanent magnet for sintering argentiferous of embodiment 11, its mass percent chemical formula general formula are：
(Ce20Y1Nd79)30.8[Fe98(Co0.1Ag0.2Cu0.1Al0.5Nb0.1)2]68.2B1, and Ag accounts for the 20% of Mc contents.
The preparation method of the rich cerium yttrium Nd-Fe-B permanent magnet of above-mentioned sintering argentiferous is with embodiment 1 only difference is that step
(6) when strong magnetic level-one tempering and the heat treatment of strong magnetic second annealing are carried out in the sintered magnet obtained by step (5), wherein, magnetic field
Intensity is 1T.Permanent magnet is obtained, in 20 DEG C of progressCylinder is tested, measurement remanent magnetism (Br), coercivity (Hcb), intrinsic
Coercivity (Hcj), magnetic energy product ((BH) max), magnet J demagnetizing curves on J=0.9JrWhen opposing magnetic field (Hk), squareness
(Hk/Hcj), data as shown in the table are obtained：
A kind of rich cerium yttrium Nd-Fe-B permanent magnet for sintering argentiferous of embodiment 12, its mass percent chemical formula general formula are：
(Ce20Y1Nd79)30.8[Fe98(Co0.1Ag0.15Cu0.15Al0.5Nb0.1)2]68.2B1, and Ag accounts for the 15% of Mc contents.
The preparation method of the rich cerium yttrium Nd-Fe-B permanent magnet of above-mentioned sintering argentiferous is with embodiment 1 only difference is that step
(6) when strong magnetic level-one tempering and the heat treatment of strong magnetic second annealing are carried out in the sintered magnet obtained by step (5), wherein, magnetic field
Intensity is 13T.Permanent magnet is obtained, in 20 DEG C of progressCylinder is tested, measurement remanent magnetism (Br), coercivity (Hcb), intrinsic
Coercivity (Hcj), magnetic energy product ((BH) max), magnet J demagnetizing curves on J=0.9JrWhen opposing magnetic field (Hk), squareness
(Hk/Hcj), data as shown in the table are obtained：
A kind of rich cerium yttrium Nd-Fe-B permanent magnet for sintering argentiferous of comparative example 1, its mass percent chemical formula general formula are：
(Ce20Y1Nd79)30.8[Fe98(Co0.3Cu0.1Al0.5Nb0.1)2]68.2B1, Ag is not contained in component.
The preparation method of the rich cerium yttrium Nd-Fe-B permanent magnet of above-mentioned sintering argentiferous is identical with embodiment 1.Obtain permanent magnetism
Body, in 20 DEG C of progressCylinder is tested, measurement remanent magnetism (Br), coercivity (Hcb), intrinsic coercivity (Hcj), magnetic energy product
J=0.9J on the J demagnetizing curves of ((BH) max), magnetrWhen opposing magnetic field (Hk), squareness (Hk/Hcj), obtain such as following table
Shown data：
A kind of rich cerium yttrium Nd-Fe-B permanent magnet for sintering argentiferous of comparative example 2, its mass percent chemical formula general formula are：
(Ce20Y1Nd79)30.8[Fe98(Co0.12Ag0.08Cu0.2Al0.5Nb0.1)2]68.2B1, and Ag accounts for the 8% of Mc contents.
The preparation method of the rich cerium yttrium Nd-Fe-B permanent magnet of above-mentioned sintering argentiferous is identical with embodiment 1.Obtain permanent magnetism
Body, in 20 DEG C of progressCylinder is tested, measurement remanent magnetism (Br), coercivity (Hcb), intrinsic coercivity (Hcj), magnetic energy product
J=0.9J on the J demagnetizing curves of ((BH) max), magnetrWhen opposing magnetic field (Hk), squareness (Hk/Hcj), obtain such as following table
Shown data：
A kind of rich cerium yttrium Nd-Fe-B permanent magnet for sintering argentiferous of comparative example 3, its mass percent chemical formula general formula are：
(Ce20Y1Nd79)30.8[Fe98(Co0.03Ag0.17Cu0.2Al0.5Nb0.1)2]68.2B1, and Ag accounts for the 17% of Mc contents.
The preparation method of the rich cerium yttrium Nd-Fe-B permanent magnet of above-mentioned sintering argentiferous is identical with embodiment 1.Obtain permanent magnetism
Body, in 20 DEG C of progressCylinder is tested, measurement remanent magnetism (Br), coercivity (Hcb), intrinsic coercivity (Hcj), magnetic energy product
J=0.9J on the J demagnetizing curves of ((BH) max), magnetrWhen opposing magnetic field (Hk), squareness (Hk/Hcj), obtain such as following table
Shown data：
A kind of rich cerium yttrium Nd-Fe-B permanent magnet for sintering argentiferous of comparative example 4, its mass percent chemical formula general formula are：
(Ce20Y1Nd79)30.8[Fe98(Co0.1Ag0.2Cu0.1Al0.5Nb0.1)2]68.2B1, and Ag accounts for the 20% of Mc contents.
The preparation method of the rich cerium yttrium Nd-Fe-B permanent magnet of above-mentioned sintering argentiferous is with embodiment 1 only difference is that step
(6) when strong magnetic level-one tempering and the heat treatment of strong magnetic second annealing are carried out in the sintered magnet obtained by step (5), wherein, magnetic field
Intensity is 15T.Permanent magnet is obtained, in 20 DEG C of progressCylinder is tested, measurement remanent magnetism (Br), coercivity (Hcb), intrinsic
Coercivity (Hcj), magnetic energy product ((BH) max), magnet J demagnetizing curves on J=0.9JrWhen opposing magnetic field (Hk), squareness
(Hk/Hcj), data as shown in the table are obtained：
A kind of rich cerium yttrium Nd-Fe-B permanent magnet for sintering argentiferous of comparative example 5, its mass percent chemical formula general formula are：
(Ce20Y1Nd79)30.8[Fe98(Co0.1Ag0.2Cu0.1Al0.5Nb0.1)2]68.2B1, and Ag accounts for the 20% of Mc contents.
The preparation method of the rich cerium yttrium Nd-Fe-B permanent magnet of above-mentioned sintering argentiferous is with embodiment 1 only difference is that step
(6) when directly having carried out level-one tempering and second annealing heat treatment in the sintered magnet obtained by step (5), not in magnetic field
It is middle to carry out strong magnetic treatment.Permanent magnet is obtained, in 20 DEG C of progressCylinder is tested, measurement remanent magnetism (Br), coercivity
(Hcb), intrinsic coercivity (Hcj), magnetic energy product ((BH) max), magnet J demagnetizing curves on J=0.9JrWhen opposing magnetic field
(Hk), squareness (Hk/Hcj), obtains data as shown in the table：
Comparative example 6
The embodiment 1 disclosed in 201310314166.6, a kind of neodymium iron boron magnetic body are applied for a patent for China.
Comparative example 7
The embodiment 6 disclosed in 201610407554.2, a kind of low-cost rare earth iron boron permanent magnet are applied for a patent for China.
Contrast test
(1) average value of embodiment 1, embodiment 2, the comprehensive magnetic energy data of embodiment 3 is contrasted, it is as follows：
Permanent magnet (Ce made from embodiment 1 and embodiment 2aYbNd100-a-b)x(Fe100-cMc)100-x-yByIn contain Ce, Y
Element, in embodiment 1：A=20, b=1；In embodiment 2：A=30, b=0.5；Y element is not contained in embodiment 3.By upper table
Data are understood, during a kind of rich cerium yttrium Nd-Fe-B permanent magnet for sintering argentiferous is prepared, reasonably add Ce, Y element, can
Cost is reduced, while magnet can obtain preferable intrinsic coercivity Hcj, and in the case of identical Ce contents, what embodiment 1 obtained
The corrosion resistance of Nd-Fe-B permanent magnet is better than
Embodiment 3.By the corrosion resistance of Nd-Fe-B permanent magnet made from embodiment 1, embodiment 2 and the Chinese Shen of comparative example 6
Embodiment 1 that please be disclosed in patent 201310314166.6 is contrasted, it is again seen that embodiment 1, embodiment 2 are made in the present invention
The corrosion resistance of the Nd-Fe-B permanent magnet obtained is more preferable, so reasonably addition Y element is effectively improved neodymium iron in the present invention
The corrosion resistance of boron permanent magnet.
(2) average value of the comprehensive magnetic energy data of embodiment 1, embodiment 4-6 and comparative example 1 is contrasted, such as
Under：
The chemical formula general formula of the permanent magnet is by mass percentage：
(CeaYbNd100-a-b)x(Fe100-cMc)100-x-yBy, the M in embodiment 1cInclude several members of Co, Ag, Cu, Al and Nb
Element；M in embodiment 4cInclude several elements of Co, Ag, Cu, Al, Zr and Nb；M in embodiment 5cComprising Co, Ag, Cu, Al,
Several elements of Si, Zr, Ti and Nb；M in embodiment 6cInclude tri- kinds of elements of Co, Ag and Al；M in comparative example 1cComprising Co,
Cu, Al and Nb, not comprising Ag；Ag is not included in comparative example 6 and comparative example 7 in obtained permanent magnet.It can be obtained by upper table data
Know, the comprehensive magnetic of embodiment 1 can be better than embodiment 4 to 6, comparative example 1McIn when not including Ag, its comprehensive magnetic can be opposite
It is obvious far short of what is expected in embodiment 1, the embodiment 4-6 for including Ag, illustrate in the formula that the present invention prepares Nd-Fe-B permanent magnet,
McPreferred elements be：Co, Ag, Cu, Al and Nb, and Ag is essential element in formula.
(3) average value of comprehensive magnetic energy data of embodiment 1, embodiment 7-8, comparative example 2-3 are contrasted, such as
Under：
The chemical formula general formula of the permanent magnet is by mass percentage：
(CeaYbNd100-a-b)x(Fe100-cMc)100-x-yBy.In embodiment 1 in obtained permanent magnet, Ag accounts for Mc contents
10%；In permanent magnet made from embodiment 7, Ag accounts for the 15% of Mc contents；In permanent magnet made from embodiment 8, Ag accounts for Mc contents
12%；In permanent magnet made from comparative example 2, Ag accounts for the 8% of Mc contents；In permanent magnet made from comparative example 3, Ag accounts for Mc contents
17%.When Ag accounts for the 10%-15% of the content of Mc, the value of remanent magnetism Br reaches more than 12.3kGs, magnetic energy product (BH) max
Value reach more than 35.90MGOe, the value of squareness Hk/Hcj reaches more than 0.970；Observe comparative example 2 and comparative example 3
The magnetic property of obtained permanent magnet, it is found that its magnetic property is substantially poorer than embodiment 1, embodiment 7 and embodiment 8, squareness Hk/
The value of Hcj is below 0.970.Ag is accounted in the preparation formula of the rich cerium yttrium Nd-Fe-B permanent magnet of heretofore described sintering argentiferous
The suitable proportion of Mc contents is 10%~15%, unsuitable too low or excessive.
(4) being averaged comprehensive magnetic energy data made from embodiment 1, embodiment 12-15, comparative example 1 and comparative example 3
Value is contrasted, as follows：
In the rich cerium of sintering argentiferous in embodiment 1, embodiment 9, embodiment 10, embodiment 11, embodiment 12, comparative example 4
The sintered magnet obtained by step (5) is carried out in the preparation process of yttrium Nd-Fe-B permanent magnet, in step (6) tempering of strong magnetic level-one and
During strong magnetic second annealing heat treatment, wherein, magnetic field intensity is respectively 8T, 3T, 10T, 1T, 13T, 15T；And comparative example 5 is carrying out
During tempering heat treatment, strong magnetic treatment is carried out not in magnetic field；Its comprehensive magnetic energy data is contrasted, it can be found that preparing
Carry out the comprehensive magnetic of permanent magnet made from strong magnetic treatment technique in journey and can be better than not carry out permanent magnetism made from strong magnetic treatment
Body.6 China of comparative example applies for a patent embodiment 1 disclosed in 201310314166.6 and 7 China of comparative example applies for a patent
Embodiment 6 disclosed in 201610407554.2, does not all exist when carrying out tempering heat treatment during preparing permanent magnet
Strong magnetic treatment is carried out in magnetic field, can be seen that its comprehensive magnetic from upper table data can will be significantly worse than and sintered in preparation process
Stage has carried out permanent magnet made from strong magnetic treatment technique；The value of the remanent magnetism Br of permanent magnet in comparative example 7 is only 9.83kGs,
The value of magnetic energy product (BH) max is only 21.8MGOe, and the value of intrinsic coercivity Hcj is only 8.42kOe, its comprehensive magnetic can want obvious
Less than the rich cerium yttrium Nd-Fe-B permanent magnet that argentiferous is sintered made from embodiment 1, embodiment 9-12, comparative example 4-5.In the present invention
During the rich cerium yttrium Nd-Fe-B permanent magnet for preparing sintering argentiferous, strong magnetic two level heat treatment, optimization are employed in sintering stage
Crystal morphology and the magnetic domain distribution of magnet, improve magnet microstructure, so as to obtain the burning that comprehensive magnetic can be higher
Tie the rich cerium yttrium Nd-Fe-B permanent magnet of argentiferous.
Thermal conductivity contrasts
The thermal conductivity factor of permanent magnet, obtains made from thermal conductivity measuring apparatus measure embodiment 1-12 and comparative example 1-7
Such as the data of following table：
| Embodiment | Thermal conductivity factor unit：W·(m2·K)-1 |
| Embodiment 1 | 0.239 |
| Embodiment 2 | 0.232 |
| Embodiment 3 | 0.229 |
| Embodiment 4 | 0.233 |
| Embodiment 5 | 0.235 |
| Embodiment 6 | 0.230 |
| Embodiment 7 | 0.237 |
| Embodiment 8 | 0.234 |
| Embodiment 9 | 0.224 |
| Embodiment 10 | 0.229 |
| Embodiment 11 | 0.201 |
| Embodiment 12 | 0.218 |
| Comparative example 1 | 0.167 |
| Comparative example 2 | 0.211 |
| Comparative example 3 | 0.214 |
| Comparative example 4 | 0.212 |
| Comparative example 5 | 0.171 |
| Comparative example 6 | 0.189 |
| Comparative example 7 | 0.191 |
The heat conduction of rich cerium yttrium neodymium iron permanent magnet made from comparative example 1, embodiment 7-8, comparative example 2-3 and comparative example 1
Coefficient, it is found that its thermal conductivity factor reaches 0.2W (m when containing Ag in preparing formula2·K)-1More than, and comparative example 1 is rich
Ag is not contained in the preparation formula of cerium yttrium neodymium iron permanent magnet, its thermal conductivity factor is only 0.167W (m2·K)-1；China's application is special
Embodiment 1 and China disclosed in profit 201310314166.6 are applied for a patent in the embodiment 6 disclosed in 201610407554.2
Rare-earth iron-boron permanent magnet preparation formula in do not contain Ag yet, its thermal conductivity factor is respectively 0.189W (m2·K)-1With
0.191W·(m2·K)-1, to be also less than the thermal conductivity factor for preparing and with the addition of permanent magnet made from Ag in formula, can learn this hair
The thermal conductivity of the slab of magnet containing Ce is improved by the addition of certain content Ag in bright.
Embodiment 1, embodiment 9-12, comparative example 4 are strong in different magnetic field respectively during sintering stage tempering heat treatment
Strong magnetic treatment has been carried out in the magnetic field of degree, and comparative example 5 finds to be made after strong magnetic treatment has been carried out without strong magnetic treatment is carried out
The thermal conductivity factor of rich cerium yttrium neodymium iron permanent magnet to be significantly greater than without the rich cerium yttrium neodymium iron permanent magnet for carrying out strong magnetic treatment.Contrast
Example 6 and comparative example 7 also carry out strong magnetic treatment when carrying out tempering heat treatment not in magnetic field, its thermal conductivity factor will also be less than this
The thermal conductivity factor of rich cerium yttrium neodymium iron permanent magnet made from strong magnetic two level heat treatment is employed in invention, it can be found that being sintered preparing
During the rich cerium yttrium Nd-Fe-B permanent magnet of argentiferous, it is heat-treated, can be improved containing rich cerium using strong magnetic two level in sintering stage
The thermal conductivity of yttrium Nd-Fe-B permanent magnet Ce.
Claims (8)
- A kind of 1. rich cerium yttrium Nd-Fe-B permanent magnet for sintering argentiferous, it is characterised in that：The chemical formula general formula of the permanent magnet presses matter Measuring percentage is：(CeaYbNd100-a-b)x(Fe100-cMc)100-x-yBy, wherein：5≤a≤30,0.3≤b≤2,0.5≤c≤5, 28.8≤x≤32.5,0.9≤y≤1.1, M are one kind in Ga, Si, Ti, Mn, Ni, Sn, Co, Cu, Al, Nb, Zr and Ag Or several metallic elements.
- 2. the rich cerium yttrium Nd-Fe-B permanent magnet of sintering argentiferous according to claim 1, it is characterised in that：The permanent magnet Chemical formula general formula is by mass percentage：(CeaYbNd100-a-b)x(Fe100-cMc)100-x-yBy, wherein：15≤a≤25,0.5≤b ≤ 1.5,1≤c≤3,30.5≤x≤32,0.95≤y≤1.02, M are one kind or several in Co, Cu, Al, Nb, Zr and Ag Kind metallic element, Ag is essential element in formula, and Ag accounts for the 10%~15% of Mc contents.
- 3. the rich cerium yttrium Nd-Fe-B permanent magnet of sintering argentiferous according to claim 1, it is characterised in that：The permanent magnet passes through It is prepared by following steps：Raw material preparation, rapid hardening slab, hydrogen are broken, airflow milling, oriented moulding, sintering and heat treatment.
- 4. the preparation method of the rich cerium yttrium Nd-Fe-B permanent magnet of sintering argentiferous according to claim 3, it is characterised in that：Heat Treatment process step includes：Any strong magnetic tempering process among strong magnetic level-one tempering and strong magnetic second annealing, or both.
- A kind of 5. preparation method of the rich cerium yttrium Nd-Fe-B permanent magnet of the sintering argentiferous described in claim 1, it is characterised in that：Bag Include following processing step：(1) raw material prepares：According to the rich cerium yttrium Nd-Fe-B permanent magnet mass percent chemical formula of the sintering argentiferous (CeaYbNd100-a-b)x(Fe100-cMc)100-x-yByPreparation raw material, wherein：5≤a≤30,0.3≤b≤2,0.5≤c≤5,28.8 ≤ x≤32.5,0.9≤y≤1.1, M are one kind or several in Ga, Si, Ti, Mn, Ni, Sn, Co, Cu, Al, Nb, Zr and Ag Kind metallic element；(2) rapid hardening slab：In argon filling pressure≤3 × 104Carry out slab in the rapid hardening slab stove of Pa, cast temperature for 1300~ 1550 DEG C, rapid hardening copper roller rotating speed 41r/min, obtain the slab that thickness is 0.15-0.3mm；(3) hydrogen is broken and airflow milling：Particle mean size is made in obtained slab in step (2) with airflow milling anaerobic technique using hydrogen is broken About 2.8um, the fine powder that size distribution is d [9,0]/d [1,0] ＜ 3.8；(4) oriented moulding：By the fine powder obtained by step (3) in the Magnetic field press of 2T oriented moulding, then carry out cold isostatic pressing Into green compact, its density is 4.2g/cm3；(5) sinter：Green compact obtained by step (4) are placed in vacuum≤3 × 10-2It is sintered and is sintered in the sintering furnace of Pa Magnet, sintering temperature are 900~1180 DEG C, 2~5h of soaking time.(6) it is heat-treated：Sintered magnet obtained by step (5) is subjected to strong magnetic level-one tempering and the heat treatment of strong magnetic second annealing, most The rich cerium yttrium Nd-Fe-B permanent magnet of sintering argentiferous is obtained eventually.Wherein, magnet shaping differently- oriented directivity is strong parallel to magnetic direction, magnetic field It is 800~950 DEG C to spend for vacuum≤5Pa of 1~13T, strong magnetic level-one tempering and strong magnetic second annealing, level-one temperature, Level-one tempering time is 1~3h；Second annealing temperature is 400~530 DEG C, and the second annealing time is 2~4h.
- 6. the preparation method of the rich cerium yttrium Nd-Fe-B permanent magnet of sintering argentiferous according to claim 5, it is characterised in that：Institute It is 1380~1440 DEG C to state the cast temperature in step (2).
- 7. the preparation method of the rich cerium yttrium Nd-Fe-B permanent magnet of sintering argentiferous according to claim 5, it is characterised in that：Institute It is 1000~1045 DEG C to state the sintering temperature in step (5).
- 8. the preparation method of the rich cerium yttrium Nd-Fe-B permanent magnet of sintering argentiferous according to claim 5, it is characterised in that：Institute When stating in step (6) using the heat treatment of strong magnetic firsts and seconds, magnet is molded differently- oriented directivity parallel to magnetic direction, magnetic field intensity For 3~10T.
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| CN112071544A (en) * | 2020-08-20 | 2020-12-11 | 钢铁研究总院 | Low-density Y-containing permanent magnet and preparation method thereof |
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| CN113764147A (en) * | 2021-09-18 | 2021-12-07 | 泮敏翔 | Method for improving coercive force of neodymium iron boron magnet through low-melting-point mixed diffusion |
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| WO2022123990A1 (en) * | 2020-12-09 | 2022-06-16 | Tdk株式会社 | R-t-b permanent magnet |
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