CN108022708B - A kind of rich cerium yttrium Nd-Fe-B permanent magnet and preparation method thereof being sintered argentiferous - Google Patents
A kind of rich cerium yttrium Nd-Fe-B permanent magnet and preparation method thereof being sintered argentiferous Download PDFInfo
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- CN108022708B CN108022708B CN201711381033.5A CN201711381033A CN108022708B CN 108022708 B CN108022708 B CN 108022708B CN 201711381033 A CN201711381033 A CN 201711381033A CN 108022708 B CN108022708 B CN 108022708B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- 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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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/04—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering with simultaneous application of supersonic waves, magnetic or electric fields
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/02—Making ferrous alloys by powder metallurgy
- C22C33/0257—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements
- C22C33/0278—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5%
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—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
- 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
- H01F41/0206—Manufacturing of magnetic cores by mechanical means
- H01F41/0246—Manufacturing of magnetic circuits by moulding or by pressing powder
Abstract
The present invention relates to a kind of rich cerium yttrium Nd-Fe-B permanent magnets and preparation method thereof for being sintered argentiferous.The chemical formula general formula of the permanent magnet is by mass percentage are as follows: (CeaYbNd100‑a‑b)x(Fe100‑ cMc)100‑x‑yBy, in which: 5≤a≤30,0.3≤b≤2,0.5≤c≤5,28.8≤x≤32.5,0.9≤y≤1.1, M are selected from one or more of Ga, Si, Ti, Mn, Ni, Sn, Co, Cu, Al, Nb, Zr and Ag metallic element.The preparation method of the rich cerium yttrium Nd-Fe-B permanent magnet of the sintering argentiferous include: broken raw material preparation, rapid hardening slab, hydrogen, airflow milling, oriented moulding, etc. static pressure, sintering and heat treatment procedure.The present invention is by adjusting formula, add Ce, Y rare earth element of high abundance, the Ag for adding certain content simultaneously improves the thermal conductivity of the slab of magnet containing Ce, and it is heat-treated in sintering stage using strong magnetic second level, to obtain the rich cerium yttrium Nd-Fe-B permanent magnet of the higher sintering argentiferous of comprehensive magnetic energy, enterprise's production cost is reduced, rare earth resources are comprehensively utilized.
Description
Technical field
The present invention relates to rare-earth permanent magnet material technical field, well simultaneously more particularly to a kind of low cost, heating conduction
And comprehensive magnetic can it is higher sintering argentiferous rich cerium yttrium Nd-Fe-B permanent magnet with and preparation method thereof.
Background technique
Sintered Nd-Fe-B magnet is widely used in nuclear-magnetism with its price compared with high comprehensive magnetic properties and relative moderate
The fields such as resonance, high-performance small and special electric machine, electric car, aerospace navigation device, wind-power electricity generation, office automation, household electrical appliances.With
Growing and preparation process the quick update of the market demand, cause PrNd needed for preparing magnet largely to consume, and store up
Ce, La, Y utilization rate for measuring relative abundance are lower, cause each rare earth element application uneven, in addition the 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
Preparing Ce-Nd-Fe-B permanent magnet is always industry research hot spot.Part PrNd is replaced to prepare work to study it by addition 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 Industry application, can not only be greatly reduced cost, it is often more important that can make rare earth resources
Balanced use rate is improved.
Currently, yttrium is added in sintered nd-fe-b magnet both at home and abroad also certain research, but mass production
There is not been reported, and the neodymium iron boron magnetic body coercivity of addition Y element reported in the literature is relatively low (Hcj < 12kGs), comprehensive magnetic energy
Poor, a possibility that meeting the market demand, is smaller.The saturation magnetic polarization Js=14.1kGs of yttrium, anisotropy field HA
Suitable with Ce, and Nd hexagonal closest packing having the same product structure reasonably adds Y element, magnet can be obtained 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, which applies for a patent, discloses a kind of low-cost rare earth iron boron permanent magnet in 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, it is heat-treated in sintering stage using strong magnetic second level, the comprehensive magnetic of permanent magnet is enabled to obtain very big mention
It is high.
Summary of the invention
The purpose of the present invention is and addition high abundance rare earth members serious uneven for the application of rare earth element currently on the market
After element the problem of reduced performance, by adding cerium, yttrium cost declining, adding silver improves slab heating conduction, 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 magnets of the sintering argentiferous of low cost
Preparation method.
To achieve the goals above, the present invention provides the following technical scheme that
A kind of rich cerium yttrium Nd-Fe-B permanent magnet being sintered argentiferous, it is characterised in that: the rich cerium yttrium Nd-Fe-B permanent magnet
Chemical formula general formula by mass percentage are as follows: (CeaYbNd100-a-b)x(Fe100-cMc)100-x-yBy, in which: 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 Zr and Ag metallic element, Ag are essential elements in formula.
Further, the chemical formula general formula of the permanent magnet is by mass percentage are as follows: (CeaYbNd100-a-b)x(Fe100- cMc)100-x-yBy, in which: 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 Co, Cu, Al, Nb, Zr and Ag metallic element, 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 molding, 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 preparation: 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, in which: 5≤a≤30,0.3≤b≤2,0.5≤c≤5,28.8
≤ x≤32.5,0.9≤y≤1.1, M are selected from one of Ga, Si, Ti, Mn, Ni, Sn, Co, Cu, Al, Nb, Zr and Ag or several
Kind metallic element, Ag are essential elements in formula；
(2) rapid hardening slab: in argon filling pressure≤3 × 104Slab, cast temperature 1300 are carried out in the rapid hardening slab furnace of Pa
~1550 DEG C, rapid hardening copper roller revolving speed 41r/min, obtain the slab with a thickness of 0.15-0.3mm；
(3) hydrogen is broken and airflow milling: using hydrogen is broken and airflow milling anaerobic technique slab obtained in step (2) is made it is average
Granularity is 2.8 μm, size distribution x90/x10The fine powder of < 3.8；
(4) it oriented moulding: by step (3) resulting fine powder oriented moulding in the Magnetic field press of 2T, then carries out cold etc. quiet
It is pressed into green compact, density 4.2g/cm3；
(5) it is sintered: step (4) resulting green compact is placed in vacuum degree≤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: the resulting sintered magnet of 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 molding differently- oriented directivity is parallel to magnetic direction,
Magnetic field strength is 1~13T, vacuum degree≤5Pa of strong magnetic level-one tempering and strong magnetic second annealing, level-one tempering temperature is 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 in the step (6) using strong magnetic level-one and strong magnetic secondary tempering heat treatment, it is flat that magnet forms differently- oriented directivity
For row in magnetic direction, magnetic field strength 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, balancing
The exploitation of weight rare earth.Cooperate other metallic elements by essential Ag, reasonably adjust formula components and slab technique, improves
The microstructure of slab, refines crystal grain.Jet milling process parameter is adjusted, relatively narrow particle size distribution is obtained.It is high
After temperature sintering, strong magnetic second 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 keep magnet finer and close, the comprehensive magnetic energy (Hcj > 12kOe) of magnet is improved, market is met
Demand.
Specific embodiment
The present invention can further be 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 being sintered argentiferous of embodiment 1, mass percent chemical formula general formula are as follows:
(Ce20Y1Nd79)30.8[Fe98(Co0.2Ag0.1Cu0.1Al0.5Nb0.1)2]68.2B1, and Ag accounts for the 10% of Mc content.
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 preparation: 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 furnace of Pa
DEG C, rapid hardening copper roller revolving speed 41r/min obtains the slab with a thickness of 0.15-0.3mm.
(3) hydrogen is broken and airflow milling: using hydrogen is broken and airflow milling anaerobic technique slab obtained in step (2) is made it is average
Granularity is 2.8 μm, size distribution x90/x10=3.5 fine powder.
(4) it oriented moulding: by step (3) resulting fine powder oriented moulding in the Magnetic field press of 2T, then carries out cold etc. quiet
It is pressed into green compact, density 4.2g/cm3。
(5) it is sintered: step (4) resulting green compact is placed in vacuum degree≤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: the resulting sintered magnet of 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 molding differently- oriented directivity is parallel to magnetic direction,
Magnetic field strength is 8T, and vacuum degree≤5Pa of strong magnetic level-one tempering and strong magnetic second annealing, level-one tempering 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 60 DEG C and burns hereinafter, taking out
Magnet is tied, the N38 high-performance magnet containing Ce of intrinsic coercivity > 13kOe is obtained.
Above-mentioned resulting rich cerium yttrium Nd-Fe-B permanent magnet is carried out at 20 DEG CCylinder test, measures remanent magnetism
(Br), J=0.9J on the J demagnetizing curve 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 being sintered argentiferous of embodiment 2, mass percent chemical formula general formula are as follows:
(Ce30Y0.5Nd69.5)30.8[Fe98(Co0.2Ag0.1Cu0.1Al0.5Nb0.1)2]68.2B1, and Ag accounts for the 10% of Mc content.
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 is carried out at 20 DEG CCylinder test, measures remanent magnetism (Br), coercivity (Hcb), intrinsic coercivity (Hcj), magnetic energy product
J=0.9J on the J demagnetizing curve of ((BH) max), magnetrWhen opposing magnetic field (Hk), squareness (Hk/Hcj), obtain such as following table
Shown data:
| 2 | 12.19 | 11.54 | 12.49 | 35.24 | 12.49 | 0.984 |
| 3 | 12.10 | 11.53 | 12.44 | 34.70 | 12.35 | 0.977 |
| Average value | 12.13 | 11.54 | 12.45 | 34.90 | 12.41 | 0.978 |
A kind of rich cerium yttrium Nd-Fe-B permanent magnet for being sintered argentiferous of embodiment 3, mass percent chemical formula general formula are as follows:
(Ce20Nd80)30.8[Fe98(Co0.2Ag0.1Cu0.1Al0.5Nb0.1)2]68.2B1, and Ag accounts for the 10% of Mc content.
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 is carried out at 20 DEG CCylinder test, measures remanent magnetism (Br), coercivity (Hcb), intrinsic coercivity (Hcj), magnetic energy product
J=0.9J on the J demagnetizing curve 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 being sintered argentiferous of embodiment 4, mass percent chemical formula general formula are as follows:
(Ce20Y1Nd79)30.8[Fe98(Co0.2Ag0.1Cu0.1Al0.2Zr0.3Nb0.1)2]68.2B1, and Ag accounts for the 10% of Mc content.
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 is carried out at 20 DEG CCylinder test, measures remanent magnetism (Br), coercivity (Hcb), intrinsic coercivity (Hcj), magnetic energy product
J=0.9J on the J demagnetizing curve of ((BH) max), magnetrWhen opposing magnetic field (Hk), squareness (Hk/Hcj), obtain such as following table
Shown data:
| 1 | 12.23 | 11.62 | 13.36 | 35.48 | 12.85 | 0.962 |
| 2 | 12.21 | 11.58 | 13.33 | 35.36 | 12.84 | 0.964 |
| 3 | 12.21 | 11.65 | 13.37 | 35.32 | 12.80 | 0.957 |
| Average value | 12.22 | 11.62 | 13.36 | 35.38 | 12.83 | 0.961 |
A kind of rich cerium yttrium Nd-Fe-B permanent magnet for being sintered argentiferous of embodiment 5, mass percent chemical formula general formula are as follows:
(Ce20Y1Nd79)30.8[Fe98(Co0.2Ag0.1Cu0.1Al0.1Si0.1Zr0.2Ti0.1Nb0.1)2]68.2B1, and Ag accounts for the 10% of Mc content.
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 is carried out at 20 DEG CCylinder test, measures remanent magnetism (Br), coercivity (Hcb), intrinsic coercivity (Hcj), magnetic energy product
J=0.9J on the J demagnetizing curve 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 being sintered argentiferous of embodiment 6, mass percent chemical formula general formula are as follows:
(Ce20Y1Nd79)30.8[Fe98(Co0.3Ag0.1Al0.6)2]68.2B1, and Ag accounts for the 10% of Mc content.
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 is carried out at 20 DEG CCylinder test, measures remanent magnetism (Br), coercivity (Hcb), intrinsic coercivity (Hcj), magnetic energy product
J=0.9J on the J demagnetizing curve 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 being sintered argentiferous of embodiment 7, mass percent chemical formula general formula are as follows:
(Ce20Y1Nd79)30.8[Fe98(Co0.1Ag0.15Cu0.15Al0.5Nb0.1)2]68.2B1, and Ag accounts for the 15% of Mc content.
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 is carried out at 20 DEG CCylinder test, measures remanent magnetism (Br), coercivity (Hcb), intrinsic coercivity (Hcj), magnetic energy product
J=0.9J on the J demagnetizing curve 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 being sintered argentiferous of embodiment 8, mass percent chemical formula general formula are as follows:
(Ce20Y1Nd79)30.8[Fe98(Co0.1Ag0.12Cu0.18Al0.5Nb0.1)2]68.2B1, and Ag accounts for the 12% of Mc content.
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 is carried out at 20 DEG CCylinder test, measures remanent magnetism (Br), coercivity (Hcb), intrinsic coercivity (Hcj), magnetic energy product
J=0.9J on the J demagnetizing curve 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 being sintered argentiferous of embodiment 9, mass percent chemical formula general formula are as follows:
(Ce20Y1Nd79)30.8[Fe98(Co0.1Ag0.2Cu0.1Al0.5Nb0.1)2]68.2B1, and Ag accounts for the 20% of Mc content.
The preparation method and embodiment 1 of the rich cerium yttrium Nd-Fe-B permanent magnet of above-mentioned sintering argentiferous are only difference is that step
(6) when carrying out strong magnetic level-one tempering and strong magnetic secondary tempering heat treatment to the resulting sintered magnet of step (5) in, wherein magnetic field
Intensity is 3T.Permanent magnet is obtained, is carried out at 20 DEG CCylinder test, it is measurement remanent magnetism (Br), coercivity (Hcb), intrinsic
Coercivity (Hcj), magnetic energy product ((BH) max), magnet J demagnetizing curve 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 being sintered argentiferous of embodiment 10, mass percent chemical formula general formula are as follows:
(Ce20Y1Nd79)30.8[Fe98(Co0.1Ag0.15Cu0.15Al0.5Nb0.1)2]68.2B1, and Ag accounts for the 15% of Mc content.
The preparation method and embodiment 1 of the rich cerium yttrium Nd-Fe-B permanent magnet of above-mentioned sintering argentiferous are only difference is that step
(6) when carrying out strong magnetic level-one tempering and strong magnetic secondary tempering heat treatment to the resulting sintered magnet of step (5) in, wherein magnetic field
Intensity is 10T.Permanent magnet is obtained, is carried out at 20 DEG CCylinder test, it is measurement remanent magnetism (Br), coercivity (Hcb), intrinsic
Coercivity (Hcj), magnetic energy product ((BH) max), magnet J demagnetizing curve 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 being sintered argentiferous of embodiment 11, mass percent chemical formula general formula are as follows:
(Ce20Y1Nd79)30.8[Fe98(Co0.1Ag0.2Cu0.1Al0.5Nb0.1)2]68.2B1, and Ag accounts for the 20% of Mc content.
The preparation method and embodiment 1 of the rich cerium yttrium Nd-Fe-B permanent magnet of above-mentioned sintering argentiferous are only difference is that step
(6) when carrying out strong magnetic level-one tempering and strong magnetic secondary tempering heat treatment to the resulting sintered magnet of step (5) in, wherein magnetic field
Intensity is 1T.Permanent magnet is obtained, is carried out at 20 DEG CCylinder test, it is measurement remanent magnetism (Br), coercivity (Hcb), intrinsic
Coercivity (Hcj), magnetic energy product ((BH) max), magnet J demagnetizing curve on J=0.9JrWhen opposing magnetic field (Hk), squareness
(Hk/Hcj), data as shown in the table are obtained:
| Average value | 12.19 | 11.54 | 13.29 | 35.25 | 12.98 | 0.977 |
A kind of rich cerium yttrium Nd-Fe-B permanent magnet for being sintered argentiferous of embodiment 12, mass percent chemical formula general formula are as follows:
(Ce20Y1Nd79)30.8[Fe98(Co0.1Ag0.15Cu0.15Al0.5Nb0.1)2]68.2B1, and Ag accounts for the 15% of Mc content.
The preparation method and embodiment 1 of the rich cerium yttrium Nd-Fe-B permanent magnet of above-mentioned sintering argentiferous are only difference is that step
(6) when carrying out strong magnetic level-one tempering and strong magnetic secondary tempering heat treatment to the resulting sintered magnet of step (5) in, wherein magnetic field
Intensity is 13T.Permanent magnet is obtained, is carried out at 20 DEG CCylinder test, it is measurement remanent magnetism (Br), coercivity (Hcb), intrinsic
Coercivity (Hcj), magnetic energy product ((BH) max), magnet J demagnetizing curve 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 being sintered argentiferous of comparative example 1, mass percent chemical formula general formula are as follows:
(Ce20Y1Nd79)30.8[Fe98(Co0.3Cu0.1Al0.5Nb0.1)2]68.2B1, Ag is not contained in ingredient.
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 is carried out at 20 DEG CCylinder test, measures remanent magnetism (Br), coercivity (Hcb), intrinsic coercivity (Hcj), magnetic energy product
J=0.9J on the J demagnetizing curve of ((BH) max), magnetrWhen opposing magnetic field (Hk), squareness (Hk/Hcj), obtain such as following table
Shown data:
| 2 | 12.05 | 11.46 | 12.40 | 34.40 | 12.22 | 0.954 |
| 3 | 12.12 | 11.40 | 12.48 | 34.82 | 12.18 | 0.960 |
| Average value | 12.08 | 11.43 | 12.43 | 34.60 | 12.17 | 0.955 |
A kind of rich cerium yttrium Nd-Fe-B permanent magnet for being sintered argentiferous of comparative example 2, mass percent chemical formula general formula are as follows:
(Ce20Y1Nd79)30.8[Fe98(Co0.12Ag0.08Cu0.2Al0.5Nb0.1)2]68.2B1, and Ag accounts for the 8% of Mc content.
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 is carried out at 20 DEG CCylinder test, measures remanent magnetism (Br), coercivity (Hcb), intrinsic coercivity (Hcj), magnetic energy product
J=0.9J on the J demagnetizing curve 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 being sintered argentiferous of comparative example 3, mass percent chemical formula general formula are as follows:
(Ce20Y1Nd79)30.8[Fe98(Co0.03Ag0.17Cu0.2Al0.5Nb0.1)2]68.2B1, and Ag accounts for the 17% of Mc content.
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 is carried out at 20 DEG CCylinder test, measures remanent magnetism (Br), coercivity (Hcb), intrinsic coercivity (Hcj), magnetic energy product
J=0.9J on the J demagnetizing curve of ((BH) max), magnetrWhen opposing magnetic field (Hk), squareness (Hk/Hcj), obtain such as following table
Shown data:
| 1 | 12.32 | 11.50 | 13.23 | 36.00 | 12.69 | 0.960 |
| 2 | 12.28 | 11.54 | 13.28 | 35.78 | 12.67 | 0.954 |
| 3 | 12.25 | 11.60 | 13.25 | 35.62 | 12.68 | 0.956 |
| Average value | 12.28 | 11.55 | 13.22 | 35.65 | 12.68 | 0.957 |
A kind of rich cerium yttrium Nd-Fe-B permanent magnet for being sintered argentiferous of comparative example 4, mass percent chemical formula general formula are as follows:
(Ce20Y1Nd79)30.8[Fe98(Co0.1Ag0.2Cu0.1Al0.5Nb0.1)2]68.2B1, and Ag accounts for the 20% of Mc content.
The preparation method and embodiment 1 of the rich cerium yttrium Nd-Fe-B permanent magnet of above-mentioned sintering argentiferous are only difference is that step
(6) when carrying out strong magnetic level-one tempering and strong magnetic secondary tempering heat treatment to the resulting sintered magnet of step (5) in, wherein magnetic field
Intensity is 15T.Permanent magnet is obtained, is carried out at 20 DEG CCylinder test, it is measurement remanent magnetism (Br), coercivity (Hcb), intrinsic
Coercivity (Hcj), magnetic energy product ((BH) max), magnet J demagnetizing curve 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 being sintered argentiferous of comparative example 5, mass percent chemical formula general formula are as follows:
(Ce20Y1Nd79)30.8[Fe98(Co0.1Ag0.2Cu0.1Al0.5Nb0.1)2]68.2B1, and Ag accounts for the 20% of Mc content.
The preparation method and embodiment 1 of the rich cerium yttrium Nd-Fe-B permanent magnet of above-mentioned sintering argentiferous are only difference is that step
(6) when directly having carried out level-one tempering and secondary tempering heat treatment to step (5) resulting sintered magnet in, there is no in magnetic field
It is middle to carry out strong magnetic treatment.Permanent magnet is obtained, is carried out at 20 DEG C Cylinder test, measures remanent magnetism (Br), coercivity
(Hcb), intrinsic coercivity (Hcj), magnetic energy product ((BH) max), magnet J demagnetizing curve on J=0.9JrWhen opposing magnetic field
(Hk), squareness (Hk/Hcj) obtains data as shown in the table:
Comparative example 6
Embodiment 1 disclosed in 201310314166.6, a kind of neodymium iron boron magnetic body are applied for a patent for China.
Comparative example 7
Embodiment 6 disclosed in 201610407554.2, a kind of low-cost rare earth iron boron permanent magnet are applied for a patent for China.
Comparative test
(1) average value of embodiment 1, embodiment 2, the comprehensive magnetic energy data of embodiment 3 is compared, 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 reasonably add Ce, Y element it is found that during preparing a kind of rich cerium yttrium Nd-Fe-B permanent magnet for being sintered argentiferous, can
Cost is reduced, while preferable intrinsic coercivity Hcj can be obtained in magnet, and in the case of identical Ce content, 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
It embodiment 1 please compare disclosed in patent 201310314166.6, 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 adding Y element in the present invention effectively improves neodymium iron
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 compared, such as
Under:
The chemical formula general formula of the permanent magnet is by mass percentage are as follows:
(CeaYbNd100-a-b)x(Fe100-cMc)100-x-yBy, 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 do not include Ag；Ag is not included in comparative example 6 and comparative example 7 in permanent magnet obtained.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, comprehensive magnetic can be opposite
It wants obvious far short of what is expected in embodiment 1, the embodiment 4-6 for including Ag, illustrates that the present invention is prepared in the formula of Nd-Fe-B permanent magnet,
McPreferred elements are as follows: Co, Ag, Cu, Al and Nb, and Ag be formula in essential element.
(3) average value of embodiment 1, the comprehensive magnetic energy data of embodiment 7-8, comparative example 2-3 is compared, such as
Under:
The chemical formula general formula of the permanent magnet is by mass percentage are as follows:
(CeaYbNd100-a-b)x(Fe100-cMc)100-x-yBy.In embodiment 1 in permanent magnet obtained, Ag accounts for Mc content
10%；In permanent magnet made from embodiment 7, Ag accounts for the 15% of Mc content；In permanent magnet made from embodiment 8, Ag accounts for Mc content
12%；In permanent magnet made from comparative example 2, Ag accounts for the 8% of Mc content；In permanent magnet made from comparative example 3, Ag accounts for Mc content
17%.When Ag accounts for the 10%-15% of the content of Mc, the value of remanent magnetism Br reaches 12.3kGs or more, magnetic energy product (BH) max
Value reach 35.90MGOe or more, the value of squareness Hk/Hcj reaches 0.970 or more；Observe comparative example 2 and comparative example 3
The magnetic property of permanent magnet obtained finds that its magnetic property is obviously 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 content is 10%~15%, unsuitable too low or too high.
(4) being averaged comprehensive magnetic energy data made from embodiment 1, embodiment 12-15, comparative example 1 and comparative example 3
Value compares, as follows:
Embodiment 1, embodiment 9, embodiment 10, embodiment 11, embodiment 12, in comparative example 4 in the rich cerium of sintering argentiferous
In the preparation process of yttrium Nd-Fe-B permanent magnet, in step (6) to the resulting sintered magnet of step (5) carry out the tempering of strong magnetic level-one and
When strong magnetic secondary tempering heat treatment, wherein magnetic field strength is respectively 8T, 3T, 10T, 1T, 13T, 15T；And comparative example 5 is carrying out
When tempering heat treatment, there is no strong magnetic treatment is carried out in magnetic field；Its comprehensive magnetic energy data is compared, it can be found that preparing
The comprehensive magnetic that permanent magnet made from strong magnetic treatment technique has been carried out in journey, which can be better than, does 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 all do not exist during preparing permanent magnet when carrying out tempering heat treatment
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 be sintered during the 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, and comprehensive magnetic can want obvious
Lower than the rich cerium yttrium Nd-Fe-B permanent magnet for being sintered argentiferous 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 of preparation sintering argentiferous, it is heat-treated in sintering stage using strong magnetic second level, optimization
Crystal morphology and the magnetic domain distribution of magnet, improve magnet microstructure, so that obtaining comprehensive magnetic can higher burning
Tie the rich cerium yttrium Nd-Fe-B permanent magnet of argentiferous.
Thermal conductivity comparison
The thermal coefficient of the permanent magnet made from thermal conductivity measuring apparatus measurement embodiment 1-12 and comparative example 1-7, obtains
Such as the data of following table:
Richness cerium yttrium neodymium iron permanent magnet is thermally conductive made from comparative example 1, embodiment 7-8, comparative example 2-3 and comparative example 1
Coefficient, when discovery contains Ag in preparation formula, thermal coefficient reaches 0.2W (m2·K)-1More than, and comparative example 1 is rich
Ag is not contained in the preparation formula of cerium yttrium neodymium iron permanent magnet, thermal coefficient is only 0.167W (m2·K)-1；China's application is special
Embodiment 1 disclosed in benefit 201310314166.6 and China apply for a patent in embodiment 6 disclosed in 201610407554.2
Rare-earth iron-boron permanent magnet preparation formula in also do not contain Ag, thermal coefficient is respectively 0.189W (m2·K)-1With
0.191W·(m2·K)-1, also will be lower than the thermal coefficient for being added to permanent magnet made from Ag in preparation formula, it can be seen that this hair
The thermal conductivity of the slab of magnet containing Ce is improved in bright by the addition of certain content Ag.
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 does not carry out strong magnetic treatment, discovery is made after having carried out strong magnetic treatment
The thermal coefficient of rich cerium yttrium neodymium iron permanent magnet to be significantly greater than the rich cerium yttrium neodymium iron permanent magnet without carrying out strong magnetic treatment.Comparison
Example 6 and comparative example 7 also carry out strong magnetic treatment when carrying out tempering heat treatment not in magnetic field, and thermal coefficient also will be lower than this
The thermal coefficient of strong magnetic second level heat treatment rich cerium yttrium neodymium iron permanent magnet obtained is used in invention, it can be found that being sintered in preparation
It during the rich cerium yttrium Nd-Fe-B permanent magnet of argentiferous, is heat-treated, can be improved containing rich cerium using strong magnetic second level in sintering stage
The thermal conductivity of yttrium Nd-Fe-B permanent magnet Ce.
Claims (7)
1. a kind of rich cerium yttrium Nd-Fe-B permanent magnet for being sintered argentiferous, it is characterised in that: the chemical formula general formula of the permanent magnet presses matter
Measure percentage are as follows: (CeaYbNd100-a-b)x(Fe100-cMc)100-x-yBy, in which: 15≤a≤25,0.5≤b≤1.5,1≤c≤3,
30.5≤x≤32,0.95≤y≤1.02, M are selected from one or more of Co, Cu, Al, Nb, Zr and Ag metallic element, Ag
It is essential element in formula, and Ag accounts for the 10%~15% of M content.
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 passes through
Following steps preparation: raw material preparation, rapid hardening slab, hydrogen is broken, airflow milling, oriented moulding, sintering and heat treatment.
3. the rich cerium yttrium Nd-Fe-B permanent magnet of sintering argentiferous according to claim 2, it is characterised in that: heat treatment procedure step
It suddenly include: any strong magnetic tempering process in strong magnetic level-one tempering and strong magnetic second annealing, or both.
4. a kind of preparation method of the rich cerium yttrium Nd-Fe-B permanent magnet of sintering argentiferous described in claim 1, it is characterised in that: packet
Include following processing step:
(1) raw material preparation: 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, in which: 5≤a≤30,0.3≤b≤2,0.5≤c≤5,28.8
≤ x≤32.5,0.9≤y≤1.1, M are selected from one of Ga, Si, Ti, Mn, Ni, Sn, Co, Cu, Al, Nb, Zr and Ag or several
Kind metallic element, Ag are essential elements in formula；
(2) rapid hardening slab: in argon filling pressure≤3 × 104Carrying out slab in the rapid hardening slab furnace of Pa, cast temperature is 1300~
1550 DEG C, rapid hardening copper roller revolving speed 41r/min, obtain the slab with a thickness of 0.15-0.3mm；
(3) hydrogen is broken and airflow milling: using hydrogen is broken and average particle size is made in slab obtained in step (2) by airflow milling anaerobic technique
For 2.8 μm, size distribution x90/x10The fine powder of < 3.8；
(4) oriented moulding: by step (3) resulting fine powder oriented moulding in the Magnetic field press of 2T, then cold isostatic pressing is carried out
At green compact, density 4.2g/cm3；
(5) it is sintered: step (4) resulting green compact is placed in vacuum degree≤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: the resulting sintered magnet of step (5) being subjected to strong magnetic level-one tempering and strong magnetic secondary tempering heat treatment, most
The rich cerium yttrium Nd-Fe-B permanent magnet of sintering argentiferous is obtained eventually；Wherein, magnet molding differently- oriented directivity is parallel to magnetic direction, and magnetic field is strong
Degree is 1~13T, and vacuum degree≤5Pa of strong magnetic level-one tempering and strong magnetic second annealing, level-one tempering temperature is 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.
5. the preparation method of the rich cerium yttrium Nd-Fe-B permanent magnet of sintering argentiferous according to claim 4, it is characterised in that: institute
Stating the cast temperature in step (2) is 1380~1440 DEG C.
6. the preparation method of the rich cerium yttrium Nd-Fe-B permanent magnet of sintering argentiferous according to claim 4, it is characterised in that: institute
Stating the sintering temperature in step (5) is 1000~1045 DEG C.
7. the preparation method of the rich cerium yttrium Nd-Fe-B permanent magnet of sintering argentiferous according to claim 4, it is characterised in that: institute
When stating in step (6) using the heat treatment of strong magnetic firsts and seconds, magnet molding differently- oriented directivity is parallel to magnetic direction, magnetic field strength
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 |
| CN112216500B (en) * | 2020-09-30 | 2022-03-11 | 惠州市德创磁业科技有限公司 | Method for processing neodymium magnet added with yttrium element |
| JP2022091614A (en) * | 2020-12-09 | 2022-06-21 | Tdk株式会社 | R-t-b based permanent magnet |
| JP2022091616A (en) * | 2020-12-09 | 2022-06-21 | Tdk株式会社 | R-t-b based permanent magnet |
| CN113223807B (en) * | 2021-05-31 | 2022-08-19 | 包头金山磁材有限公司 | Neodymium-iron-boron permanent magnet and preparation method and application thereof |
| CN117095892B (en) * | 2023-10-13 | 2024-02-09 | 包头天石稀土新材料有限责任公司 | Sintered NdFeB permanent magnet and preparation method thereof |
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