CN108517455A - A kind of nanocrystalline rare-earth permanent magnetic material and preparation method thereof with double main phase structures - Google Patents

A kind of nanocrystalline rare-earth permanent magnetic material and preparation method thereof with double main phase structures Download PDF

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CN108517455A
CN108517455A CN201810478421.3A CN201810478421A CN108517455A CN 108517455 A CN108517455 A CN 108517455A CN 201810478421 A CN201810478421 A CN 201810478421A CN 108517455 A CN108517455 A CN 108517455A
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powder
phase structures
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earth permanent
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江庆政
钟震晨
雷伟凯
曾庆文
何伦可
S.U.雷曼
刘仁辉
钟明龙
马胜灿
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Jiangxi University of Science and Technology
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    • H01F1/0555—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 pressed, sintered or bonded together
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    • 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
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    • 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
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    • H01F1/086—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 in the form of particles, e.g. powder pressed, sintered, or bound together sintered
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Abstract

The invention discloses a kind of nanocrystalline rare-earth permanent magnetic materials and preparation method thereof with double main phase structures, it is characterised in that：By the Ce with hard magnetic propertyxFe101‑x‑y‑zByMzMagnetic powder and non-magnetic Nd70Cu30Powder uniformly mixes by a certain percentage, and the nanocrystalline rare-earth permanent magnetic material with double main phase structures is prepared by discharge plasma sintering technique.The present invention utilizes melt spun alloy powder and non-magnetic rare earth alloy powder with hard magnetic property, obtain the nanocrystalline rare-earth permanent magnetic material with double main phase structures, microstructure, magnetic property and the corrosion resistance of permanent magnet are improved, and takes full advantage of high abundance rare earth element ce.In addition, the present invention also has sintering time short, the simple feature of technological process, the efficient balance for having effectively facilitated rare earth resources utilizes.

Description

A kind of nanocrystalline rare-earth permanent magnetic material and preparation method thereof with double main phase structures
Technical field
The invention belongs to field of rare-earth permanent magnetic, especially provide a kind of nanocrystalline rare-earth permanent magnetism with double main phase structures Material and preparation method thereof.
Background technology
Nd2Fe14B classes rare earth permanent-magnetic material is widely used in wind-power electricity generation, consumer due to its excellent magnetic property The fields such as electronics, medical instrument, new-energy automobile, aerospace, rail traffic.Neodymium iron boron (Nd-Fe-B) magnet is answered extensively Surged with the demand of the low abundance rear earth element nd of global centering, praseodymium, dysprosium, terbium is promoted.However, the high abundance based on cerium (Ce) is dilute Earth elements are not widely applied yet in rare earth permanent magnet, cause the serious uneven utilization of rare earth resources.From the cost of raw material Consider with national strategy security standpoint, the research and development of the high abundance rare earth permanent magnet of high performance-price ratio are imperative.Although Ce2Fe14The intrinsic magnetic characteristic of B compounds is inferior to Nd2Fe14B compounds, but recent studies suggest that it, which still has, prepares hard magnetic The foreground of energy permanent-magnet material.
Microstructure feature specific to nanocrystalline magnet and stronger intergranular exchange-coupling interaction so that its temperature is stablized Property and fracture toughness are better than conventional sintering magnet and bonded permanent magnet.Therefore, Nano crystal neodymium, boron class magnet is current research Hot spot, and following developing direction.In general, double main phase structure magnets have magnetic more superior than single main phase structure magnet Performance.Therefore, there is the exploitation of the nanocrystalline Ce-Fe-B bases magnet of double main phase structures can make full use of high abundance Rare-Earth Ce, drop Low magnet cost improves permanent magnet cost performance, realizes that the efficient balance of rare earth resources utilizes.
Invention content
It is an object of the invention to make full use of high abundance Rare-Earth Ce, and by the addition of low melting point rare earth alloy, realize Double main phase structures of nanocrystalline Ce-Fe-B bases magnet, to further increase magnet magnetic property.
Technical solution of the present invention is as follows：
A kind of nanocrystalline rare-earth permanent magnetic material with double main phase structures, it is characterised in that：It will be with hard magnetic property CexFe101-x-y-zByMzMagnetic powder and non-magnetic Nd70Cu30Powder is 70-95 in mass ratio：5-30 is uniformly mixed, and passes through electric discharge The nanocrystalline rare-earth permanent magnetic material with double main phase structures is prepared in plasma sintering technique；CexFe101-x-y-zByMzMagnetic powder In, one or more, 11≤x≤20 in M Cu, Al, Ga, Nb, Zr, Hf element, 3≤y≤10,0≤z≤3.
Wherein：The CexFe101-x-y-zByMzIn magnetic powder, part Fe elements can be substituted by Co；Nd70Cu30In powdered ingredients Part Nd elements can be by one in Al, Ga, Zn by one or more replacements in Pr, Dy, Tb, Ho, Gd, part Cu elements Kind or a variety of replacements.
The present invention also provides the preparation method of the nanocrystalline rare-earth permanent magnetic material of double main phase structures, feature exists In：The nanocrystalline rare-earth permanent magnetic material for having double main phase structures is prepared using discharge plasma sintering technique, electric discharge etc. from Before son sintering and entire sintering process vacuum degree is less than 10Pa, and sintering temperature is 600~800 DEG C, and sintering pressure is 20~ 100MPa, sintering time are 0~20min.
There are two Curie temperature transition points in magnet obtained by preparing, i.e., there are double main phases in magnet, pass through change Nd70Cu30The purpose of regulation and control magnet Curie temperature may be implemented in the ingredient and additive amount of powder.Meanwhile main phase in gained magnet Crystallite dimension is in Nano grade, and grain boundaries Dispersed precipitate the nano particle that size is 10-15nm.
The preparation method of the nanocrystalline rare-earth permanent magnetic material of double main phase structures of the present invention, which is characterized in that specific step It is rapid as follows：
1., by Elements C e, Fe, B, M according to CexFe101-x-y-zByMzIt matches, part Fe elements also can be by Co elements in ingredient Substitution；The raw material prepared are put into electric arc furnaces, melting is carried out under an argon atmosphere and obtains mother alloy ingot, and pass through melt Melt spun alloy band is prepared in the mode of fast quenching, and alloy strip is broken into powder under atmosphere protection；
2., by element Nd, Cu according to Nd70Cu30It matches, part Nd elements can be replaced by Pr, Dy, Tb, Ho, Gd etc. in ingredient Generation, part Cu elements can be by replacements such as Al, Ga, Zn；The raw material prepared are put into electric arc furnaces, are melted under an argon atmosphere Refining obtains mother alloy ingot, and melt spun alloy band is prepared by way of fast melt-quenching, by alloy under atmosphere protection Band is broken into powder；
3., by CexFe101-x-y-zByMzPowder and Nd70Cu30Powder uniformly mixes by a certain percentage, pours into graphite jig In, the nanocrystalline magnet with double main phase structures is made by discharging plasma sintering equipment.Sintering temperature is 600~800 DEG C, Sintering pressure is 20~100MPa, and sintering time is 0~20min；
In general, double main phase structure magnets are obtained using two kinds of powders with hard magnetic property, the present invention passes through one Powder of the kind with hard magnetic property is mixed with a kind of nonmagnetic rare earth alloy, is prepared using plasma discharging Fast Sintering technology The double main phase permanent magnets of nano are obtained.The RE of two heterogeneities is existed simultaneously in magnet2Fe14B main phases are low by controlling The addition type and additive amount of fusing point rare earth alloy realize the controllable adjustment of second Curie transition point of magnet.The present invention improves The microstructure of permanent magnet, magnet consistency is high, and corrosion resistance is strong, and take full advantage of high abundance rare earth element ce.This Outside, the present invention also has sintering time short, the simple feature of technological process, has effectively facilitated the efficient balance profit of rare earth resources With.
Description of the drawings
Fig. 1 is to be not added with rare earth alloy Ce-Fe-B base discharge plasma sintering magnet M-T curves.
Fig. 2 is that 20wt.%NdCu adds Ce-Fe-B base discharge plasma sintering magnet M-T curves.
Fig. 3 is discharge plasma sintering magnet transmission electron microscope shape appearance figure.
Specific implementation mode
Below in conjunction with attached drawing embodiment, present invention is further described in detail, but the present invention is not limited to these Examples, Following embodiment only for the purpose of illustration, should not be taken to limit the present invention and the scope of the claims.
Embodiment 1
By Elements C e, Fe, B, Nb, Cu, Ga, Co according to Ce17Fe74.5Co2B6Nb0.5Cu0.5Ga0.5Proportioning, the original that will be prepared Material is put into arc-melting furnace, is carried out melting under an argon atmosphere and is obtained mother alloy ingot, is prepared soon by getting rid of band machine Quenched alloy band, central roll speed are 19m/s, and alloy strip is broken into powder under protection of argon gas；By element Nd, Cu according to Nd70Cu30Proportioning, the raw material prepared are put into electric arc furnaces, are carried out melting under an argon atmosphere and are obtained alloy cast ingot, and lead to Melt spun alloy band is prepared in the mode for crossing fast melt-quenching, wherein it is 30m/s to get rid of band machine roller speed, by alloy strip in glove box It is broken into powder；Under protection of argon gas by Ce17Fe74.5Co2B6Nb0.5Cu0.5Ga0.5Powder and Nd70Cu30Powder in mass ratio 95： 5 uniformly mixing.Mixed-powder is poured into graphite jig, magnet is made by discharging plasma sintering equipment Fast Sintering.It burns Before knot and entire sintering process vacuum degree is less than 10Pa, and sintering temperature is 650 DEG C, sintering pressure 50MPa, and sintering time is 2min。
There are two Curie transition points, respectively T in magnetc1=438K, Tc2=457K shows that there are two in magnet Hard Magnetic main phase has double main phase structures.
Comparative example
By Elements C e, Fe, B, Nb, Cu, Ga, Co according to Ce17Fe74.5Co2B6Nb0.5Cu0.5Ga0.5Proportioning, the original that will be prepared Material is put into arc-melting furnace, is carried out melting under an argon atmosphere and is obtained mother alloy ingot, is prepared soon by getting rid of band machine Quenched alloy band, central roll speed are 19m/s, and alloy strip is broken into powder under protection of argon gas；It will Ce17Fe74.5Co2B6Nb0.5Cu0.5Ga0.5Powder pours into graphite jig, is made by discharging plasma sintering equipment Fast Sintering Magnet.Before sintering and entire sintering process vacuum degree is less than 10Pa, and sintering temperature is 650 DEG C, sintering pressure 50MPa, sintering Time is 2min.
It is not added with rare earth alloy magnet M-T curves and sees Fig. 1.There are 1 Curie transition points in Fig. 1, are Tc=443K, shows There is only a main phases in magnet.It is found that after the addition of non magnetic rare earth alloy compared with embodiment 1, Nd elements diffusions enter Inside main phase grain, lead to the formation of double main phase structures.
Embodiment 2
Difference from example 1 is that：By Ce17Fe74.5Co2B6Nb0.5Cu0.5Ga0.5Powder and Nd70Cu30Powder is pressed Mass ratio 90：10 uniformly mixing.Mixed-powder is poured into graphite jig, discharging plasma sintering equipment Fast Sintering system is passed through Obtain magnet.Before discharge plasma sintering and entire sintering process vacuum degree is less than 10Pa, and sintering temperature is 750 DEG C, sintering pressure For 30MPa, sintering time 3min.
There are two Curie transition points, respectively T in magnetc1=439K, Tc2=493K shows that there are two in magnet Hard Magnetic main phase has double main phase structures.
Embodiment 3
Difference from example 1 is that：By Ce17Fe74.5Co2B6Nb0.5Cu0.5Ga0.5Powder and Nd70Cu30Powder is pressed Mass ratio 80：20 uniformly mixing.Mixed-powder is poured into graphite jig, discharging plasma sintering equipment Fast Sintering system is passed through Obtain magnet.Before discharge plasma sintering and entire sintering process vacuum degree is less than 10Pa, and sintering temperature is 800 DEG C, sintering pressure For 50MPa, sintering time 1min.
Magnet M-T curves are shown in Fig. 2.There are two Curie transition points, respectively T in magnetc1=440K, Tc2=508K, table Two Hard Magnetic main phases are existed simultaneously in bright magnet, and there are double main phase structures.Fig. 3 is magnet transmission electron microscope shape appearance figure, can from figure To find out, all crystal grains size is Nano grade in magnet, and it is 10- that the crystal boundary Dispersed precipitate between main phase grain, which size, The nano particle of 15nm.
Embodiment 4
Difference from example 1 is that：By Ce17Fe74.5Co2B6Nb0.5Cu0.5Ga0.5Powder and Nd70Cu30Powder is pressed Mass ratio 70：30 uniformly mixing.Mixed-powder is poured into graphite jig, discharging plasma sintering equipment Fast Sintering system is passed through Obtain magnet.Before discharge plasma sintering and entire sintering process vacuum degree is less than 10Pa, and sintering temperature is 650 DEG C, sintering pressure For 50MPa, sintering time 2min.
There are two Curie transition points, respectively T in magnetc1=439K, Tc2=504K shows that there are two in magnet Hard Magnetic main phase has double main phase structures.
Embodiment 5
Difference from example 1 is that：By Ce20Fe71B8Nb0.5Cu0.5Ga1.0Powder and Nd70Cu30Powder presses quality Than 80：20 uniformly mixing.Mixed-powder is poured into graphite jig, magnetic is made by discharging plasma sintering equipment Fast Sintering Body.Before discharge plasma sintering and entire sintering process vacuum degree is less than 10Pa, and sintering temperature is 650 DEG C, and sintering pressure is 50MPa, sintering time 2min.
There are two Curie transition points in magnet, show that there are two Hard Magnetic main phases in magnet, have double main phase structures.
Embodiment 6
Difference from example 1 is that：By Ce18Fe73B8Zr0.5Al0.5Ga1.0Powder and Dy70Cu30Powder presses quality Than 85：15 uniformly mixing.Mixed-powder is poured into graphite jig, magnetic is made by discharging plasma sintering equipment Fast Sintering Body.Before discharge plasma sintering and entire sintering process vacuum degree is less than 10Pa, and sintering temperature is 650 DEG C, and sintering pressure is 40MPa, sintering time 5min.
There are two Curie transition points in magnet, show that there are two Hard Magnetic main phases in magnet, have double main phase structures.
Embodiment 7
Difference from example 1 is that：By Ce20Fe71B8Zr0.5Cu0.5Al1.0Powder and Pr70Cu30Powder presses quality Than 90：10 uniformly mixing.Mixed-powder is poured into graphite jig, magnetic is made by discharging plasma sintering equipment Fast Sintering Body.Before discharge plasma sintering and entire sintering process vacuum degree is less than 10Pa, and sintering temperature is 600 DEG C, and sintering pressure is 100MPa, sintering time 3min.
There are two Curie transition points in magnet, show that there are two Hard Magnetic main phases in magnet, have double main phase structures.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art Scholar cans understand the content of the present invention and implement it accordingly, and it is not intended to limit the scope of the present invention.It is all according to the present invention Equivalent change or modification made by Spirit Essence, should be covered by the protection scope of the present invention.

Claims (6)

1. a kind of nanocrystalline rare-earth permanent magnetic material with double main phase structures, it is characterised in that：It will be with hard magnetic property CexFe101-x-y-zByMzMagnetic powder and non-magnetic Nd70Cu30Powder is 70-95 in mass ratio：5-30 is uniformly mixed, and passes through electric discharge The nanocrystalline rare-earth permanent magnetic material with double main phase structures is prepared in plasma sintering technique；
Wherein CexFe101-x-y-zByMzMagnetic powder, one or more, 11≤x≤20 in M Cu, Al, Ga, Nb, Zr, Hf element, 3 ≤ y≤10,0≤z≤3.
2. according to the nanocrystalline rare-earth permanent magnetic material of double main phase structures described in claim 1, it is characterised in that：It is described CexFe101-x-y-zByMzIn magnetic powder, part Fe elements are substituted by Co.
3. according to the nanocrystalline rare-earth permanent magnetic material of double main phase structures described in claim 1, it is characterised in that：Nd70Cu30Powder at Part Nd elements in point are by one or more replacements in Pr, Dy, Tb, Ho, Gd, and part Cu elements are by one in Al, Ga, Zn Kind or a variety of replacements.
4. the preparation method of the nanocrystalline rare-earth permanent magnetic material of double main phase structures described in a kind of claim 1, it is characterised in that：It adopts The nanocrystalline rare-earth permanent magnetic material with double main phase structures, discharge plasma sintering are prepared with discharge plasma sintering technique Preceding and entire sintering process vacuum degree is less than 10Pa, and sintering temperature is 600~800 DEG C, and sintering pressure is 20~100MPa, sintering Time is 0~20min.
5. according to the preparation method of the nanocrystalline rare-earth permanent magnetic material of double main phase structures described in claim 4, it is characterised in that：Institute There are two Curie temperature transition points in magnet, pass through change Nd70Cu30The ingredient and additive amount of powder, may be implemented The purpose of magnet Curie temperature.
6. according to the preparation method of the nanocrystalline rare-earth permanent magnetic material of double main phase structures described in claim 4, it is characterised in that：Institute Main phase grain size is in Nano grade in magnet, and grain boundaries Dispersed precipitate the nano particle that size is 10-15nm.
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109243797A (en) * 2018-08-31 2019-01-18 江西理工大学 A kind of preparation method of the nanocrystalline rare-earth permanent magnetic material containing Ce
CN110246644A (en) * 2019-08-01 2019-09-17 泮敏翔 A kind of preparation method of the more main phase Ce base nanometer crystal magnets of high-performance
CN111063536A (en) * 2019-12-31 2020-04-24 浙江大学 Grain boundary diffusion method suitable for bulk rare earth permanent magnet material
CN111161949A (en) * 2019-12-31 2020-05-15 浙江大学 YCe co-doped nanocrystalline rare earth permanent magnet and preparation method thereof

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Publication number Priority date Publication date Assignee Title
CN109243797A (en) * 2018-08-31 2019-01-18 江西理工大学 A kind of preparation method of the nanocrystalline rare-earth permanent magnetic material containing Ce
CN110246644A (en) * 2019-08-01 2019-09-17 泮敏翔 A kind of preparation method of the more main phase Ce base nanometer crystal magnets of high-performance
CN110246644B (en) * 2019-08-01 2020-08-07 中国计量大学 Preparation method of high-performance multi-main-phase Ce-based nanocrystalline magnet
CN111063536A (en) * 2019-12-31 2020-04-24 浙江大学 Grain boundary diffusion method suitable for bulk rare earth permanent magnet material
CN111161949A (en) * 2019-12-31 2020-05-15 浙江大学 YCe co-doped nanocrystalline rare earth permanent magnet and preparation method thereof

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