CN103390477B - Sm-Co base and Nd-Fe-B base built-up magnet and preparation method thereof - Google Patents
Sm-Co base and Nd-Fe-B base built-up magnet and preparation method thereof Download PDFInfo
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- CN103390477B CN103390477B CN201310342358.8A CN201310342358A CN103390477B CN 103390477 B CN103390477 B CN 103390477B CN 201310342358 A CN201310342358 A CN 201310342358A CN 103390477 B CN103390477 B CN 103390477B
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Abstract
The invention discloses a kind of Sm-Co base and Nd-Fe-B base built-up magnet and preparation method thereof, belong to magnetic material and preparation field thereof.Described built-up magnet is composited by Hard Magnetic phase Sm-Co and Hard Magnetic phase Nd-Fe-B, and Nd-Fe-B base micron grain hard magnet parent phase and disperse Sm-Co base nanometer crystal grain Hard Magnetic wherein mutually exchange coupling occurs.Two kinds of Hard Magnetics are well combined with each other mutually, and this built-up magnet has higher magnetic energy product than Sm-Co base permanent magnet; Than Nd-Fe-B base magnet, there is better temperature stability, thus can better be applied in every field.
Description
Technical field
The present invention relates to a kind of Sm-Co base and Nd-Fe-B base built-up magnet and preparation method thereof, be specifically combined to the method for built-up magnet by a kind of Hard Magnetic phase and another kind of Hard Magnetic, belong to technical field of magnetic materials.
Background technology
Although third generation rare-earth permanent magnet almost reaches the maximum magnetic energy product of its theory at present, it can not be applicable to all application.Therefore wish very much can prepare a kind of desirable permanent magnet (there is high magnetic intensity, high-coercive force and high-curie temperature) and its cost is lower.
Although having done to make great efforts greatly after having found NdFeB is devoted to find new permanent magnet, a kind of single compound or alloy is not had to be found to have the high-performance of institute's palpus.
The magnet of Sm-Co base has good temperature stability, but its magnetization and magnetic energy product lower, and the magnet of Nd-Fe base has the high magnetization and magnetic energy product, but temperature stability is poor.Because the magnet Curie temperature of Nd-Fe base only has about 580K, it can not well be applied in high temperature environments, and NdFeB magnet crystallite dimension is when reaching nanoscale, magnet orientation is difficult to solve, and therefore NdFeB can obtain good magnetic property when grain size is micron, sub-micron.
In the past twenty years, people are finding a kind of " hybrid magnet " always, and it can have dissimilar magnet advantage separately simultaneously.But, but there is no several successful story up to now.Because dissimilar single-phase magnet differs widely due to its shaping thermodynamics and kinetics condition thus has significantly different machining process routes, the diffusion between two Hard Magnetic phase elements during high temperature sintering, can be caused.Therefore, be difficult to obtain this built-up magnet by traditional processing technology.
If a kind of method can be sought, Sm-Co base magnet and Nd-Fe base magnet two kinds of Hard Magnetics are combined with each other mutually well, there is exchange coupling, just can have a kind of new magnet simultaneously possessing the high magnetization and magnetic energy product and good temperature stability, thus can better be applied in every field.
Summary of the invention
The technical issues that need to address of the present invention are just the defect overcoming prior art, a kind of Sm-Co base and Nd-Fe-B base built-up magnet and preparation method thereof are provided, it synthesizes built-up magnet by a kind of Hard Magnetic phase and the exchange coupling of another kind of Hard Magnetic phase, obtain more high-coercive force and magnetic energy product and combination property better new magnet, possess the high magnetization and magnetic energy product and good temperature stability simultaneously, thus can better be applied in every field.
For solving the problem, the present invention adopts following technical scheme:
The invention provides a kind of Sm-Co base and Nd-Fe-B base built-up magnet, described built-up magnet is composited by Hard Magnetic phase Sm-Co and Hard Magnetic phase Nd-Fe-B, the grain size of Nd-Fe-B base Hard Magnetic phase is 1.5-10 micron, and the grain size of Sm-Co base Hard Magnetic phase is 10-100 nanometer; Wherein Sm-Co base nanometer Hard Magnetic phase content is 5wt%-70wt%, and all the other are Nd-Fe-B base micron Hard Magnetic phase; There is exchange coupling mutually in Nd-Fe-B base micron grain hard magnet parent phase and disperse Sm-Co base nanometer crystal grain Hard Magnetic wherein.
In compound magnetic of the present invention, the grain size of Nd-Fe-B base Hard Magnetic phase is 1.5-10 micron, and the grain size of Sm-Co base Hard Magnetic phase is 10-100 nanometer.
Hard Magnetic phase Sm-Co of the present invention comprises the magnet of all Sm-Co bases.
Hard Magnetic phase Nd-Fe-B of the present invention comprises the magnet of all Nd-Fe-B bases.
Invention also provides the preparation method of a kind of described Sm-Co base and Nd-Fe-B base built-up magnet:
Smelt with vacuum rapid hardening smelting furnace and obtain Nd-Fe-B Hard Magnetic phase rapid hardening alloy, ingot casting is carried out homogenizing heat treatment 1-3 hour at 600 ~ 650 DEG C; Then be placed in hydrogen blasting furnace hydrogen quick-fried, then through airflow milling abrasive dust, obtain the Hard Magnetic phase powder that granularity is 1.5-10 micron; Alloy smelted into by another Hard Magnetic phase Sm-Co vacuum intermediate-frequency smelting furnace, with Ar hermetic seal in ball grinder, with surfactant auxiliary high-energy ball-milling method ball milling 3 ~ 6h, obtains the Hard Magnetic phase powder that granularity is 10-100 nanometer; By two kinds of Hard Magnetic phase powder Homogeneous phase mixing to form composite granule; By compressing in magnetic field for the composite granule obtained, then carry out isostatic pressed; Temperature lower than 650 DEG C, pressure carries out hot pressing under being 0.5 ~ 4GPa, then obtained magnet carried out vacuum magnetic heat treatment: under temperature 360 ~ 830 DEG C, magnetic field are 0.5 ~ 10T magnetic field environment, be incubated 0.5 ~ 3 hour.
In preparation method of the present invention, built-up magnet of the present invention forms magnetic uniaxial anisotropy by magnetic-field heat treatment technique.
In preparation method of the present invention, Sm-Co base nanometer Hard Magnetic is enclosed in Nd-Fe-B base micron Hard Magnetic mutually around mutually.
In preparation method of the present invention, surfactant assists the surfactant that uses in ball-milling method for oily ammonia or oleic acid or oily ammonia oil acid blend.
Advantage of the present invention has:
(1) Sm-Co base hard magnetic body and Nd-Fe base hard magnetic body two kinds of Hard Magnetics are the invention enables well to be combined with each other mutually, there is exchange-coupling interaction, this built-up magnet has the higher magnetization and magnetic energy product and better temperature stability than single-phase permanent magnet, thus can better be applied in every field.
(2) grain size of Nd-Fe-B base Hard Magnetic phase is 1.5-10 micron, the degree of orientation that can keep, magnetic property; The grain size of Sm-Co base Hard Magnetic phase is 10-100 nanometer, has good diffusion effect, plays coercive force pinning effect, and this micro-enzyme electrode is conducive to improving magnetic property.
(3) adopt magnetic-field heat treatment technique in the preparation process of built-up magnet, strengthen orientation effect, promote crystal grain recrystallization, improve crystal grain integrality.
(4) adopt the heat pressing process of low temperature, high pressure in the preparation process of built-up magnet, effective inhibiting grain growth, prevent two Hard Magnetics mutually between Elements Diffusion.
Embodiment
embodiment 1
The composition of Hard Magnetic phase Nd-Fe-B by the percentage by weight of each element is:
Nd:Fe:B:Al=32.2:66.27:1.03:0.5；
The composition of Hard Magnetic phase Sm-Co by the percentage by weight of each element is:
Sm:Co：Cu：Fe：Zr=33:66：0.2：0.6：0.2
Hard Magnetic phase Nd-Fe-B alloy and Hard Magnetic phase Sm-Co alloy is smelted with vacuum intermediate-frequency smelting furnace, ingot casting is carried out homogenizing vacuum heat 2 hours respectively at 650 DEG C and 1100 DEG C, coarse crushing subsequently, be placed in hydrogen blasting furnace hydrogen quick-fried, Hard Magnetic phase Nd-Fe-B granularity is milled to 3.5 microns, and another Hard Magnetic phase Sm-Co is milled to 200 nanometers.
Smelt with vacuum intermediate-frequency rapid hardening smelting furnace and obtain Hard Magnetic phase Nd-Fe-B-Al rapid hardening alloy, then hydrogen blasting furnace hydrogen is placed in quick-fried, use airflow milling that Hard Magnetic phase Nd-Fe-B-Al granularity is milled to 3.5 microns, smelt with vacuum intermediate-frequency smelting furnace and obtain Hard Magnetic phase Sm-Co-Cu-Fe-Zr alloy, ingot casting is carried out homogenizing vacuum heat 2 hours at 600 DEG C, and uses high energy ball mill to be milled to 20 nanometers.
The Hard Magnetic phase Nd-Fe-B-Al powder of 3.5 microns is mixed and made into composite granule with the Hard Magnetic phase Sm-Co-Cu-Fe-Zr of 20 nanometers.
By compressing in magnetic field for the composite granule obtained, carry out isostatic pressed again, then at 650 DEG C, pressure is carry out hot pressing under 3GPa, then obtained sintered magnet is carried out vacuum magnetic heat treatment: under the magnetic field environment of temperature 750 DEG C of magnetic field 1T, be incubated 0.5 hour.
embodiment 2
The composition of Hard Magnetic phase Nd-Fe-B by the percentage by weight of each element is:
Nd:Fe:B:Al=32.2:66.27:1.03:0.5；
The composition of Hard Magnetic phase Sm-Co by the percentage by weight of each element is:
Sm:Co=33.75:66.25；
Hard Magnetic phase Nd-Fe-B alloy and Hard Magnetic phase Sm-Co alloy is smelted with vacuum intermediate-frequency smelting furnace, ingot casting is carried out homogenizing vacuum heat 2 hours respectively at 600 DEG C and 1100 DEG C, with being placed on, hydrogen in hydrogen blasting furnace is quick-fried, Hard Magnetic phase Nd-Fe-B granularity uses airflow milling to be milled to 3.5 microns, and another Hard Magnetic phase Sm-Co is milled to 20 nanometers.
By nanometer Hard Magnetic phase powder and micron Hard Magnetic phase powder Homogeneous phase mixing, in mixture, the content of nanometer Hard Magnetic phase powder is 50wt%.
By compressing in magnetic field for the composite granule obtained, then carry out isostatic pressed, then at 650 DEG C, pressure is carry out hot pressing under 3GPa, then obtained magnet is carried out vacuum magnetic heat treatment: under the magnetic field environment of temperature 750 DEG C of magnetic field 1T, be incubated 0.5 hour.
Last it is noted that obviously, above-described embodiment is only for example of the present invention is clearly described, and the restriction not to execution mode.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here exhaustive without the need to also giving all execution modes.And thus the apparent change of amplifying out or variation be still among protection scope of the present invention.
Claims (5)
1. a Sm-Co base and Nd-Fe-B base built-up magnet, it is characterized in that: described built-up magnet is composited by Hard Magnetic phase Sm-Co and Hard Magnetic phase Nd-Fe-B, the grain size of Nd-Fe-B base Hard Magnetic phase is 1.5-10 micron, and the grain size of Sm-Co base Hard Magnetic phase is 10-100 nanometer; Wherein Sm-Co base nanometer Hard Magnetic phase content is 5wt%-70wt%, and all the other are Nd-Fe-B base micron Hard Magnetic phase; There is exchange coupling mutually in Nd-Fe-B base micron grain hard magnet parent phase and disperse Sm-Co base nanometer crystal grain Hard Magnetic wherein.
2. Sm-Co base according to claim 1 and Nd-Fe-B base built-up magnet, it is characterized in that: Hard Magnetic phase Nd-Fe-B comprises the magnet of all Nd-Fe-B bases, Hard Magnetic phase Sm-Co comprises the magnet of all Sm-Co bases.
3., according to arbitrary described Sm-Co base of claim 1-2 and the preparation method of Nd-Fe-B base built-up magnet, it is characterized in that:
Smelt with vacuum rapid hardening smelting furnace and obtain Nd-Fe-B Hard Magnetic phase rapid hardening alloy, ingot casting is carried out homogenizing heat treatment 1-3 hour at 600 ~ 650 DEG C; Then be placed in hydrogen blasting furnace hydrogen quick-fried, then through airflow milling abrasive dust, obtain the Hard Magnetic phase powder that granularity is 1.5-10 micron; Alloy smelted into by another Hard Magnetic phase Sm-Co vacuum intermediate-frequency smelting furnace, with Ar hermetic seal in ball grinder, with surfactant auxiliary high-energy ball-milling method ball milling 3 ~ 6h, obtains the Hard Magnetic phase powder that granularity is 10-100 nanometer; By two kinds of Hard Magnetic phase powder Homogeneous phase mixing to form composite granule; By compressing in magnetic field for the composite granule obtained, then carry out isostatic pressed; Temperature lower than 650 DEG C, pressure carries out hot pressing under being 0.5 ~ 4GPa, then obtained magnet carried out vacuum magnetic heat treatment: under temperature 360 ~ 830 DEG C, magnetic field are 0.5 ~ 10T magnetic field environment, be incubated 0.5 ~ 3 hour.
4. the preparation method of Sm-Co base according to claim 3 and Nd-Fe-B base built-up magnet, is characterized in that: Sm-Co base nanometer Hard Magnetic is enclosed in Nd-Fe-B base micron Hard Magnetic mutually around mutually.
5. the preparation method of Sm-Co base according to claim 4 and Nd-Fe-B base built-up magnet, is characterized in that: surfactant assists the surfactant that uses in ball-milling method for oily ammonia or oleic acid or oily ammonia oil acid blend.
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| CN104759628A (en) * | 2015-01-26 | 2015-07-08 | 横店集团东磁股份有限公司 | Method for preparing heat-resistance sintering NdFeB permanent magnet material |
| CN105374485B (en) * | 2015-11-26 | 2018-06-05 | 宁波科星材料科技有限公司 | A kind of MULTILAYER COMPOSITE magnet and preparation method thereof |
| CN105448513B (en) * | 2015-12-29 | 2017-09-05 | 江苏大学 | A kind of preparation method of multi-phase compound permanent-magnet body |
| CN110098026A (en) * | 2018-01-28 | 2019-08-06 | 蒋盼盼 | A kind of preparation method of rare-earth permanent magnet |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003124012A (en) * | 2001-10-12 | 2003-04-25 | Hitachi Ltd | Composite magnet, composite magnetic material, and motor |
| CN101299370A (en) * | 2008-03-05 | 2008-11-05 | 内蒙古科技大学 | Synthesis magnet of hard magnetic phase and soft magnetic phase as well as preparing method |
| CN102655050A (en) * | 2012-05-04 | 2012-09-05 | 江苏大学 | Method for preparing high-performance high-temperature-resisting nanometer composite permanent magnet |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003124012A (en) * | 2001-10-12 | 2003-04-25 | Hitachi Ltd | Composite magnet, composite magnetic material, and motor |
| CN101299370A (en) * | 2008-03-05 | 2008-11-05 | 内蒙古科技大学 | Synthesis magnet of hard magnetic phase and soft magnetic phase as well as preparing method |
| CN102655050A (en) * | 2012-05-04 | 2012-09-05 | 江苏大学 | Method for preparing high-performance high-temperature-resisting nanometer composite permanent magnet |
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