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CN108517455B - Nanocrystalline rare earth permanent magnetic material with double-main-phase structure and preparation method thereof - Google Patents

Nanocrystalline rare earth permanent magnetic material with double-main-phase structure and preparation method thereof Download PDF

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CN108517455B
CN108517455B CN201810478421.3A CN201810478421A CN108517455B CN 108517455 B CN108517455 B CN 108517455B CN 201810478421 A CN201810478421 A CN 201810478421A CN 108517455 B CN108517455 B CN 108517455B
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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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Buddhist Tzu Chi General Hospital
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Abstract

The invention discloses a nanocrystalline rare earth permanent magnetic material with a double-main-phase structure and a preparation method thereof, and is characterized in that: ce to have hard magnetic propertiesxFe101‑x‑y‑zByMzMagnetic powder and non-magnetic Nd70Cu30The powder is evenly mixed according to a certain proportion, and the nanocrystalline rare earth permanent magnet material with a double-main-phase structure is prepared by a discharge plasma sintering technology. The invention utilizes the rapid quenching alloy powder with hard magnetic property and the non-magnetic rare earth alloy powder to obtain the nanocrystalline rare earth permanent magnet material with a double-main-phase structure, improves the microstructure, the magnetic property and the corrosion resistance of the permanent magnet, and fully utilizes the high-abundance rare earth element Ce. In addition, the method has the characteristics of short sintering time and simple process flow, and effectively promotes the efficient and balanced utilization of rare earth resources.

Description

Nanocrystalline rare earth permanent magnetic material with double-main-phase structure and preparation method thereof
Technical Field
The invention belongs to the field of rare earth permanent magnet materials, and particularly provides a nanocrystalline rare earth permanent magnet material with a double-main-phase structure and a preparation method thereof.
Background
Nd2Fe14Due to the excellent magnetic property, the B-type rare earth permanent magnet material is widely applied to the fields of wind power generation, consumer electronics, medical appliances, new energy automobiles, aerospace, rail transit and the like. The wide application of neodymium iron boron (Nd-Fe-B) magnets has prompted a strong global demand for medium and low abundance rare earth elements, namely neodymium, praseodymium, dysprosium and terbium. However, the abundant rare earth elements mainly containing cerium (Ce) are not used in rare earth permanent magnets in large quantities, which results in serious unbalanced utilization of rare earth resources. From the perspective of raw material cost and national strategic safety, research and development of high-abundance rare earth permanent magnets with high cost performance are imperative. Although Ce is2Fe14The intrinsic magnetic properties of the B compound are inferior to those of Nd2Fe14The B compound has the prospect of preparing a hard magnetic performance permanent magnetic material.
The special microstructure characteristics of the nanocrystalline magnet and the strong intercrystalline exchange coupling effect ensure that the temperature stability and the fracture toughness of the nanocrystalline magnet are better than those of the traditional sintered magnet and the bonded magnet. Therefore, nanocrystalline neodymium iron boron magnets are the current research focus and are the development direction in the future. In general, the dual main phase structure magnet has more excellent magnetic properties than the single main phase structure magnet. Therefore, the development of the nanocrystalline Ce-Fe-B-based magnet with a double-main-phase structure can fully utilize the high-abundance rare earth Ce, reduce the cost of the magnet, improve the cost performance of the permanent magnet and realize the efficient balanced utilization of rare earth resources.
Disclosure of Invention
The invention aims to fully utilize high-abundance rare earth Ce and realize the double-main-phase structure of the nanocrystalline Ce-Fe-B-based magnet by adding the low-melting-point rare earth alloy, thereby further improving the magnetic property of the magnet.
The technical scheme of the invention is as follows:
nanocrystalline rare earth permanent magnet with double-main-phase structureA material characterized by: ce to have hard magnetic propertiesxFe101-x-y-zByMzMagnetic powder and non-magnetic Nd70Cu30The powder is 70-95 mass percent: 5-30, and preparing the nanocrystalline rare earth permanent magnet material with a double-main-phase structure by a spark plasma sintering technology; cexFe101-x-y-zByMzIn the magnetic powder, M is one or more of Cu, Al, Ga, Nb, Zr and Hf, x is more than or equal to 11 and less than or equal to 20, y is more than or equal to 3 and less than or equal to 10, and z is more than or equal to 0 and less than or equal to 3.
Wherein: the CexFe101-x-y-zByMzIn the magnetic powder, part of Fe element can be replaced by Co; nd (neodymium)70Cu30Part of Nd element in the powder component can be replaced by one or more of Pr, Dy, Tb, Ho and Gd, and part of Cu element can be replaced by one or more of Al, Ga and Zn.
The invention also provides a preparation method of the nanocrystalline rare earth permanent magnetic material with the double-main-phase structure, which is characterized by comprising the following steps: the nanocrystalline rare earth permanent magnet material with the double-main-phase structure is prepared by adopting a spark plasma sintering technology, the vacuum degree before spark plasma sintering and in the whole sintering process is less than 10Pa, the sintering temperature is 600-800 ℃, the sintering pressure is 20-100 MPa, and the sintering time is 0-20 min.
Two Curie temperature transition points exist in the prepared magnet, namely, double main phases exist in the magnet, and Nd is changed70Cu30The aim of regulating and controlling the Curie temperature of the magnet can be achieved by the components and the addition amount of the powder. Meanwhile, the size of the main phase crystal grain in the obtained magnet is in the nanometer level, and nanoparticles with the size of 10-15nm are dispersed and distributed at the grain boundary.
The preparation method of the nanocrystalline rare earth permanent magnetic material with the double-main-phase structure is characterized by comprising the following specific steps of:
①, the elements Ce, Fe, B and M are according to CexFe101-x-y-zByMzProportioning, wherein part of Fe element in the components can be replaced by Co element; the prepared raw materials are put into an electric arc furnace, are smelted under the argon atmosphere to obtain a master alloy ingot, and are rapidly quenched through a meltPreparing a rapid quenching alloy strip, and crushing the alloy strip into powder under the protection of atmosphere;
② elements Nd and Cu are Nd70Cu30Proportioning, wherein part of Nd elements in the components can be replaced by Pr, Dy, Tb, Ho, Gd and the like, and part of Cu elements can be replaced by Al, Ga, Zn and the like; putting the prepared raw materials into an electric arc furnace, smelting in argon atmosphere to obtain a mother alloy ingot, preparing a rapidly quenched alloy strip in a melt rapid quenching mode, and crushing the alloy strip into powder under the protection of atmosphere;
③, mixing CexFe101-x-y-zByMzPowder and Nd70Cu30The powder is evenly mixed according to a certain proportion, poured into a graphite mould and prepared into the nanocrystalline magnet with a double-main-phase structure through discharge plasma sintering equipment. The sintering temperature is 600-800 ℃, the sintering pressure is 20-100 MPa, and the sintering time is 0-20 min;
generally speaking, the double-main-phase structure magnet is obtained by utilizing two kinds of powder with hard magnetic property, and the invention prepares the nano crystal form double-main-phase permanent magnet by mixing the powder with hard magnetic property with a non-magnetic rare earth alloy and adopting a discharge plasma rapid sintering technology. Two RE's of different composition are present in a magnet at the same time2Fe14The B main phase realizes the controllable adjustment of the second Curie point of the magnet by controlling the addition type and the addition amount of the low-melting-point rare earth alloy. The invention improves the microstructure of the permanent magnet, has high density and strong corrosion resistance, and fully utilizes the high-abundance rare earth element Ce. In addition, the method has the characteristics of short sintering time and simple process flow, and effectively promotes the efficient and balanced utilization of rare earth resources.
Drawings
FIG. 1 is a M-T curve of a Ce-Fe-B base discharge plasma sintered magnet without rare earth alloy.
FIG. 2 is a M-T plot of a 20 wt.% NdCu additive Ce-Fe-B based spark plasma sintered magnet.
FIG. 3 is a transmission electron microscope morphology of spark plasma sintered magnet.
Detailed Description
The present invention will be described in further detail with reference to the following embodiments, but the present invention is not limited to these embodiments, and the following embodiments are only for illustrative purposes and should not be used to limit the scope of the present invention and claims.
Example 1
Elements Ce, Fe, B, Nb, Cu, Ga, Co are according to Ce17Fe74.5Co2B6Nb0.5Cu0.5Ga0.5Proportioning, namely putting the proportioned raw materials into an electric arc melting furnace, melting in an argon atmosphere to obtain a mother alloy ingot, preparing a quick-quenching alloy strip by using a strip throwing machine, wherein the roll speed is 19m/s, and crushing the alloy strip into powder under the protection of argon; elements Nd and Cu are in accordance with Nd70Cu30Proportioning, namely putting the proportioned raw materials into an electric arc furnace, smelting in an argon atmosphere to obtain an alloy ingot, preparing a rapidly quenched alloy strip in a melt rapid quenching mode, wherein the roller speed of a belt throwing machine is 30m/s, and crushing the alloy strip into powder in a glove box; under the protection of argon, Ce is added17Fe74.5Co2B6Nb0.5Cu0.5Ga0.5Powder and Nd70Cu30The powder comprises the following components in percentage by mass 95: 5, uniformly mixing. And pouring the mixed powder into a graphite mold, and quickly sintering by using discharge plasma sintering equipment to obtain the magnet. Before sintering and in the whole sintering process, the vacuum degree is less than 10Pa, the sintering temperature is 650 ℃, the sintering pressure is 50MPa, and the sintering time is 2 min.
There are two Curie transition points in the magnet, T respectivelyc1＝438K，Tc2457K, indicates the presence of two hard magnetic main phases in the magnet, with a dual main phase structure.
Comparative example
Elements Ce, Fe, B, Nb, Cu, Ga, Co are according to Ce17Fe74.5Co2B6Nb0.5Cu0.5Ga0.5Proportioning, putting the proportioned raw materials into an electric arc melting furnace, melting in argon atmosphere to obtain mother alloy cast ingots, and preparing a quick-quenching alloy strip by a melt spinning machine, wherein the roll speed is 19m/s, and the quick-quenching alloy strip is prepared in argon atmosphereCrushing the alloy strip into powder under the protection of gas; adding Ce17Fe74.5Co2B6Nb0.5Cu0.5Ga0.5And pouring the powder into a graphite mold, and quickly sintering by using discharge plasma sintering equipment to obtain the magnet. Before sintering and in the whole sintering process, the vacuum degree is less than 10Pa, the sintering temperature is 650 ℃, the sintering pressure is 50MPa, and the sintering time is 2 min.
The M-T curve of the magnet without the rare earth alloy is shown in figure 1. In FIG. 1, there are 1 Curie transition point, Tc443K, indicating that only one main phase is present in the magnet. As is clear from comparison with example 1, when the nonmagnetic rare earth alloy is added, the Nd element diffuses into the main phase grains, resulting in formation of a two-main-phase structure.
Example 2
The difference from example 1 is that: adding Ce17Fe74.5Co2B6Nb0.5Cu0.5Ga0.5Powder and Nd70Cu30The powder comprises the following components in percentage by mass 90: 10 are mixed uniformly. And pouring the mixed powder into a graphite mold, and quickly sintering by using discharge plasma sintering equipment to obtain the magnet. The vacuum degree before the spark plasma sintering and in the whole sintering process is less than 10Pa, the sintering temperature is 750 ℃, the sintering pressure is 30MPa, and the sintering time is 3 min.
There are two Curie transition points in the magnet, T respectivelyc1＝439K，Tc2493K, indicating the presence of two hard magnetic major phases in the magnet, having a dual major phase structure.
Example 3
The difference from example 1 is that: adding Ce17Fe74.5Co2B6Nb0.5Cu0.5Ga0.5Powder and Nd70Cu30The powder comprises the following components in percentage by mass 80: 20 and uniformly mixing. And pouring the mixed powder into a graphite mold, and quickly sintering by using discharge plasma sintering equipment to obtain the magnet. Before the spark plasma sintering and in the whole sintering process, the vacuum degree is less than 10Pa, the sintering temperature is 800 ℃, the sintering pressure is 50MPa, and the sintering time is 1 min.
The M-T curve of the magnet is shown in FIG. 2. Two in the magnetEach Curie transition point is Tc1＝440K，Tc2508K, indicating that there are two hard magnetic main phases in the magnet at the same time, with a dual main phase structure. FIG. 3 is a transmission electron microscope image of a magnet, from which it can be seen that all the crystal grains in the magnet are in nanometer level, and nanoparticles with a size of 10-15nm are dispersed and distributed in the grain boundaries between the main phase crystal grains.
Example 4
The difference from example 1 is that: adding Ce17Fe74.5Co2B6Nb0.5Cu0.5Ga0.5Powder and Nd70Cu30Powder is prepared from the following components in percentage by mass of 70: 30, and uniformly mixing. And pouring the mixed powder into a graphite mold, and quickly sintering by using discharge plasma sintering equipment to obtain the magnet. Before the spark plasma sintering and in the whole sintering process, the vacuum degree is less than 10Pa, the sintering temperature is 650 ℃, the sintering pressure is 50MPa, and the sintering time is 2 min.
There are two Curie transition points in the magnet, T respectivelyc1＝439K，Tc2504K, indicating that there are two hard magnetic main phases in the magnet, with a dual main phase structure.
Example 5
The difference from example 1 is that: adding Ce20Fe71B8Nb0.5Cu0.5Ga1.0Powder and Nd70Cu30The powder comprises the following components in percentage by mass 80: 20 and uniformly mixing. And pouring the mixed powder into a graphite mold, and quickly sintering by using discharge plasma sintering equipment to obtain the magnet. Before the spark plasma sintering and in the whole sintering process, the vacuum degree is less than 10Pa, the sintering temperature is 650 ℃, the sintering pressure is 50MPa, and the sintering time is 2 min.
The presence of two curie transition points in the magnet indicates the presence of two hard magnetic main phases in the magnet, having a dual main phase structure.
Example 6
The difference from example 1 is that: adding Ce18Fe73B8Zr0.5Al0.5Ga1.0Powder and Dy70Cu30Powder is prepared from the following components in percentage by mass 85: 15 are mixed homogeneously. Mixing the powdersPouring the powder into a graphite mold, and rapidly sintering by using discharge plasma sintering equipment to obtain the magnet. Before the spark plasma sintering and in the whole sintering process, the vacuum degree is less than 10Pa, the sintering temperature is 650 ℃, the sintering pressure is 40MPa, and the sintering time is 5 min.
The presence of two curie transition points in the magnet indicates the presence of two hard magnetic main phases in the magnet, having a dual main phase structure.
Example 7
The difference from example 1 is that: adding Ce20Fe71B8Zr0.5Cu0.5Al1.0Powder and Pr70Cu30The powder comprises the following components in percentage by mass 90: 10 are mixed uniformly. And pouring the mixed powder into a graphite mold, and quickly sintering by using discharge plasma sintering equipment to obtain the magnet. Before the spark plasma sintering and in the whole sintering process, the vacuum degree is less than 10Pa, the sintering temperature is 600 ℃, the sintering pressure is 100MPa, and the sintering time is 3 min.
The presence of two curie transition points in the magnet indicates the presence of two hard magnetic main phases in the magnet, having a dual main phase structure.
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.

Claims (5)

1. A nanocrystalline rare earth permanent magnetic material with a double-main-phase structure is characterized in that: ce to have hard magnetic propertiesxFe101-x-y-zByMzMagnetic powder and non-magnetic Nd70Cu30The powder is 70-95 mass percent: 5-30, and preparing the nanocrystalline rare earth permanent magnet material with a double-main-phase structure by a spark plasma sintering technology;
wherein CexFe101-x-y-zByMzMagnetic powder, wherein M is one or more of Cu, Al, Ga, Nb, Zr and Hf, x is more than or equal to 11 and less than or equal to 20, y is more than or equal to 3 and less than or equal to 10, and z is more than or equal to 0 and less than or equal to 103；
The vacuum degree before the spark plasma sintering and in the whole sintering process is less than 10Pa, the sintering temperature is 600-800 ℃, the sintering pressure is 20-100 MPa, and the sintering time is 0-20 min.
2. The nanocrystalline rare earth permanent magnetic material of a bi-main phase structure according to claim 1, characterized in that: the CexFe101-x-y-zByMzIn the magnetic powder, part of Fe element is replaced by Co.
3. The nanocrystalline rare earth permanent magnetic material of a bi-main phase structure according to claim 1, characterized in that: nd (neodymium)70Cu30Part of Nd element in the powder component is replaced by one or more of Pr, Dy, Tb, Ho and Gd, and part of Cu element is replaced by one or more of Al, Ga and Zn.
4. The nanocrystalline rare earth permanent magnetic material of a bi-main phase structure according to claim 1, characterized in that: two Curie temperature transition points exist in the obtained magnet by changing Nd70Cu30The aim of regulating and controlling the Curie temperature of the magnet can be achieved by the components and the addition amount of the powder.
5. The nanocrystalline rare earth permanent magnetic material of a bi-main phase structure according to claim 1, characterized in that: the size of the main phase crystal grain in the obtained magnet is in the nanometer level, and nanoparticles with the size of 10-15nm are dispersed and distributed at the crystal boundary.
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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
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CN111063536B (en) * 2019-12-31 2022-03-22 浙江大学 Grain boundary diffusion method suitable for bulk rare earth permanent magnet material
CN111161949B (en) * 2019-12-31 2022-02-11 浙江大学 YCe co-doped nanocrystalline rare earth permanent magnet and preparation method thereof

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