CN116855815A - A method to improve the phase stability of the rare earth permanent magnet material Pr2Fe14C that can reduce the harm of residual carbon - Google Patents
A method to improve the phase stability of the rare earth permanent magnet material Pr2Fe14C that can reduce the harm of residual carbon Download PDFInfo
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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
- C22C33/04—Making ferrous alloys by melting
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
- B22D11/001—Continuous casting of metals, i.e. casting in indefinite lengths of specific alloys
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
- B22D11/06—Continuous casting of metals, i.e. casting in indefinite lengths into moulds with travelling walls, e.g. with rolls, plates, belts, caterpillars
- B22D11/0611—Continuous casting of metals, i.e. casting in indefinite lengths into moulds with travelling walls, e.g. with rolls, plates, belts, caterpillars formed by a single casting wheel, e.g. for casting amorphous metal strips or wires
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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
- C21D1/18—Hardening; Quenching with or without subsequent tempering
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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
- C21D1/26—Methods of annealing
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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
- C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
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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
- C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
- C21D9/52—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for wires; for strips ; for rods of unlimited length
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
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Abstract
一种可降低残余碳危害的稀土永磁材料Pr2Fe14C的相稳定性提升方法，涉及永磁材料技术领域。由具有如下所示化学计量比的物质组成：(Pr,RE)2Fe14C；其中RE＝Sm、Gd；制备工艺包括配料、熔炼、熔体快淬、退火，其中，熔体快淬是采用铜辊转速20≤V≤40m/s的真空快淬炉在保护气氛下进行，退火是在保护气氛下500～1100℃的退火炉中进行。在本发明利用Sm2Fe14C和Gd2Fe14C相的高稳定性，用Sm、Gd原子置换Pr2Fe14C中的部分Pr原子，扩展了Pr2Fe14C相的稳定区间，制得了纯相的(Pr,RE)2Fe14C型稀土永磁材料。A method for improving the phase stability of the rare earth permanent magnet material Pr 2 Fe 14 C that can reduce the harm of residual carbon, and relates to the technical field of permanent magnet materials. It is composed of substances with the following stoichiometric ratio: (Pr, RE) 2 Fe 14 C; where RE = Sm, Gd; the preparation process includes batching, smelting, melt rapid quenching, and annealing, where the melt rapid quenching is A vacuum quick quenching furnace with a copper roller speed of 20 ≤ V ≤ 40 m/s is used under a protective atmosphere, and annealing is performed in an annealing furnace at 500 to 1100°C under a protective atmosphere. In the present invention, the high stability of the Sm 2 Fe 14 C and Gd 2 Fe 14 C phases is used to replace part of the Pr atoms in Pr 2 Fe 14 C with Sm and Gd atoms, thereby expanding the stability range of the Pr 2 Fe 14 C phase. A pure phase (Pr,RE) 2 Fe 14 C type rare earth permanent magnet material was prepared.
Description
Technical Field
The invention relates to the technical field of rare earth permanent magnet materials, in particular to a Pr capable of reducing residual carbon hazard in a 3D printing or metal powder injection molding process 2 Fe 14 And C, phase stability of the permanent magnetic material.
Background
In recent years, with the development of electronic terminal products, there is a higher demand for the shape and performance of electronic component products mainly made of permanent magnet materials. On one hand, the traditional preparation method is difficult to meet the requirements, and on the other hand, larger rare earth resource waste is brought. Therefore, how to efficiently produce small-sized and shaped magnets is a technical problem to be solved. In recent years, metal powder injection molding (MIM) and 3D printing technologies are rapidly developed, and the process characteristics are suitable for producing special-shaped devices and can greatly save resources. The MIM and 3D printing technology is introduced in the molding processing process of the rare earth permanent magnet material, so that the magnet preparation efficiency and the resource utilization efficiency can be greatly improved. The key process steps of MIM and 3D printing rare earth permanent magnet materials are that the binder is mixed with rare earth permanent magnet powder and molded at high temperature. However, most binders with better performance are organic materials, and carbon elements contained in the binders are difficult to thoroughly remove. Residual carbon can cause great harm to the performance of the permanent magnet material. Therefore, the rare earth permanent magnet material with the performance insensitive to residual carbon is developed, so that the applicability of MIM and 3D printing technology in the preparation of the permanent magnet material can be greatly improved, and the manufacturing capacity of the magnet with the complex shape is greatly improved.
Pr 2 Fe 14 The C permanent magnet material has Nd which is the main phase of Nd-Fe-B permanent magnet 2 Fe 14 B the same crystal structure, and Pr 2 Fe 14 C magnetic anisotropic field is larger, and magnetic hardening is easier to realize. This means that the material can be used for preparing high-coercivity permanent magnets which are completely free of heavy rare earth. More importantly, such materials are inherently carbides, which have a natural insensitivity to MIM and residual carbon during 3D printing. Therefore, this material is an ideal candidate for MIM and 3D printed rare earth permanent magnet materials. However, pr 2 Fe 14 The stability of phase C is low and must be achieved through slow solid phase transitions over a specific temperature range, which is very detrimental to large scale mass production. To overcome this difficulty, new ingredients and processes need to be designed to accelerate Pr 2 Fe 14 C, thereby obtaining stable single phase with high efficiency.
Disclosure of Invention
The invention aims to provide a method for rapidly and stably obtaining pure Pr 2 Fe 14 Phase C method, pr provided by the invention 2 Fe 14 C material or Pr prepared by adopting the preparation method of the invention 2 Fe 14 The C material has high phase stability.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a Pr-improving agent 2 Fe 14 Scheme of C phase stability, adopting medium and heavy rare earth elements to adjust Pr 2 Fe 14 The composition of the C alloy to improve phase stability is characterized by the following chemical composition:
(Pr,RE) 2 Fe 14 c (formula 1) and is a 2:14:1 pure phase structure;
RE in the formula 1 is middle and heavy rare earth elements Sm, gd and the like.
The invention provides the scheme (Pr, RE) 2 Fe 14 The preparation method of the phase C comprises the following steps:
(1) Smelting the mixture containing RE, pr, fe and C to obtain cast ingot, and mixing (Pr, RE) 2 Fe 14 Based on the theory of C, pr and RE are additionally increased by 1-5% to compensate the loss, preferably according to the following Pr 6 RE 9 Fe 79 C 6 Preparing nominal components;
(2) Carrying out melt rapid quenching on the cast ingot to obtain a rapid quenching belt;
(3) Annealing and quenching the rapid quenching belt under the protection of argon to obtain (Pr, RE) 2 Fe 14 C-type rare earth permanent magnetic material;
wherein the mass of Fe and C in the step (1) corresponds to the theoretical mass in the formula 1, and the mass of Pr and RE is respectively increased by 1-5% on the basis of the theoretical mass of Pr and RE calculated according to the formula 1.
The smelting in the step (2) is performed in a high-frequency induction smelting furnace.
In the step (2), the melt rapid quenching is carried out in a melt rapid quenching furnace, wherein in the rapid quenching process, the rotating speed of a copper roller is 20-40 m/s, the diameter of a quartz tube nozzle is 0.5-2 mm, and the distance from the bottom of the quartz tube to the copper roller is 2-4 mm.
The annealing temperature in the step (3) is 500-1100 ℃ and the annealing time is 0.01-1h.
The annealing in the step (3) is performed in a semi-open atmosphere filled with a protective gas.
Preferably, the annealing of step (3) includes: placing a quartz tube with one end closed and one end open into a heating furnace, introducing argon at the speed of 10L/min, heating the furnace to 500-1100 ℃, placing the rapid quenching belt obtained in the step (2) into a crucible or tantalum foil after 10-30min, placing the rapid quenching belt into a tube orifice of the quartz tube for preheating, and pushing a sample into the bottom end of the quartz tube for annealing after 5-10 min. The annealing time is 0.01-1h.
Preferably, the quenching mode in the step (3) is ice water quenching.
The invention provides a (Pr, RE) 2 Fe 14 The C-type rare earth permanent magnet material is formed by substances with chemical compositions shown in a formula 1: (Pr, RE) 2 Fe 14 C (formula 1); RE in the formula 1 is middle and heavy rare earth elements Sm and Gd. The invention utilizes the RE formed by Sm, gd and the like of medium and heavy rare earth 2 Fe 14 The high stability of C phase is improved by using Sm, gd and the like to replace Pr element 2 Fe 14 Phase stability of C.
The invention provides (Pr, RE) 2 Fe 14 The preparation method of the C-type rare earth permanent magnet material comprises the following steps: smelting a mixture comprising RE, pr, fe and C,obtaining an ingot; carrying out melt rapid quenching on the cast ingot to obtain a rapid quenching belt; annealing and quenching the rapid quenching belt under the protection of argon to obtain (Pr, RE) 2 Fe 14 C-type rare earth permanent magnetic material; the mass of Fe and C corresponds to the theoretical mass in the formula 1, and the mass of Pr and RE is respectively increased by 1-5% on the basis of the theoretical mass of Pr and RE calculated according to the formula 1. The invention can improve (Pr, RE) by replacing Pr with Sm, gd and the like of medium and heavy rare earth 2 Fe 14 Phase C stability, lowering its energy barrier formed and inhibiting its decomposition; the structure with more uniform components and finer grains is obtained by melt rapid quenching, which can reduce the energy barrier of atomic diffusion in the annealing process and accelerate the annealing process (Pr, RE) 2 Fe 14 Phase C is formed; can be obtained by annealing (Pr, RE) 2 Fe 14 C pure phase; then quenching is carried out to ensure (Pr, RE) 2 Fe 14 The pure phase C does not decompose during cooling.
The invention has the main advantages compared with other prior art that: the mixed use of rare earth elements is beneficial to the balance utilization of rare earth resources; medium and heavy rare earth substitution to improve Pr 2 Fe 14 Curie temperature of C; medium and heavy rare earth substitution for expanding Pr 2 Fe 14 A stable interval of phase C; medium and heavy rare earth substitution for improving Pr 2 Fe 14 And C, temperature stability of the permanent magnetic material.
Drawings
FIG. 1 is an XRD pattern of the sample of example 1;
FIG. 2 is an XRD pattern of the sample of example 2;
fig. 3 is an XRD pattern of the sample of comparative example 1.
The upper left corner in the drawing is a nominal component, and the upper right corner is a corresponding pure phase structure.
Detailed Description
The present invention will be further illustrated with reference to the following examples, but the present invention is not limited to the following examples.
Example 1
(1) The Sm, pr and Fe simple substance with the purity of 99.9 percent and the Fe-C alloy raw material with the mass percent of 5 percent are mixed according to the stoichiometric ratio Pr 6 Sm 9 Fe 79 C 6 Proportioning.
(2) And (3) putting the prepared raw materials into a vacuum arc melting furnace, and melting under an argon atmosphere to obtain an alloy ingot. Repeatedly smelting for 4 times, and taking out from the furnace for standby after the sample is completely cooled.
(3) Crushing the smelted cast ingot, and putting the crushed cast ingot into a quartz tube with the bottom nozzle diameter of 0.5-2 mm; filling the quartz tube into a melt rapid quenching furnace, so that the distance between the bottom of the quartz tube and a copper roller is 2-4 mm; and when the cast ingot is remelted in the quartz tube, opening and adjusting the rotating speed of the copper roller to 40m/s, and vertically spraying the remelted liquid onto the copper roller to obtain the rapid quenching belt.
(4) And annealing and quenching the rapid quenching belt under the protection of argon. The annealing steps are as follows: the quartz tube and the air tube with one end closed for a section of opening are put into a muffle furnace in advance, and argon is opened for purging for 10min. Wrapping the rapid quenching belt with a special tantalum sheet, placing the rapid quenching belt at the mouth of a quartz tube for preheating for 10min, and pushing a sample wrapped by the tantalum sheet into the bottom end of the quartz tube by a fine iron rod for isothermal annealing at 850 ℃ for 1h. Followed by quenching in ice water. The annealing and quenching process is always performed in an argon purged environment.
Example 2
(1) The pure Gd, pr and Fe simple substance with 99.9 percent and the mass fraction of 5 percent of Fe-C alloy raw material are mixed according to the stoichiometric ratio Pr 6 Gd 9 Fe 79 C 6 Proportioning.
(2) And (3) putting the prepared raw materials into a vacuum arc melting furnace, and melting under an argon atmosphere to obtain an alloy ingot. Repeatedly smelting for 4 times, and taking out from the furnace for standby after the sample is completely cooled.
(3) Crushing the smelted cast ingot, and putting the crushed cast ingot into a quartz tube with the bottom nozzle diameter of 0.5-2 mm; filling the quartz tube into a melt rapid quenching furnace, so that the distance between the bottom of the quartz tube and a copper roller is 2-4 mm; and when the cast ingot is remelted in the quartz tube, opening and adjusting the rotating speed of the copper roller to 40m/s, and vertically spraying the remelted liquid onto the copper roller to obtain the rapid quenching belt.
(4) And annealing and quenching the rapid quenching belt under the protection of argon. The annealing steps are as follows: the quartz tube and the air tube with one end closed for a section of opening are put into a muffle furnace in advance, and argon is opened for purging for 10min. Wrapping the rapid quenching belt with a special tantalum sheet, placing the rapid quenching belt at the mouth of a quartz tube for preheating for 10min, and pushing a sample wrapped by the tantalum sheet into the bottom end of the quartz tube by a fine iron rod for isothermal annealing at 850 ℃ for 1h. Followed by quenching in ice water. The annealing and quenching process is always performed in an argon purged environment.
Comparative example 1
(1) Pr with purity of 99.9% and Fe simple substance, and Fe-C alloy raw material with mass fraction of 5% are mixed according to stoichiometric ratio Pr 15 Fe 79 C 6 Proportioning.
(2) And (3) putting the prepared raw materials into a vacuum arc melting furnace, and melting under an argon atmosphere to obtain an alloy ingot. Repeatedly smelting for 4 times, and taking out from the furnace for standby after the sample is completely cooled.
(3) Crushing the smelted cast ingot, and putting the crushed cast ingot into a quartz tube with the bottom nozzle diameter of 0.5-2 mm; filling the quartz tube into a melt rapid quenching furnace, so that the distance between the bottom of the quartz tube and a copper roller is 2-4 mm; and when the cast ingot is remelted in the quartz tube, opening and adjusting the rotating speed of the copper roller to 40m/s, and vertically spraying the remelted liquid onto the copper roller to obtain the rapid quenching belt.
(4) And annealing and quenching the rapid quenching belt under the protection of argon. The annealing steps are as follows: the quartz tube and the air tube with one end closed for a section of opening are put into a muffle furnace in advance, and argon is opened for purging for 10min. Wrapping the rapid quenching belt with a special tantalum sheet, placing the rapid quenching belt at the mouth of a quartz tube for preheating for 10min, and pushing a sample wrapped by the tantalum sheet into the bottom end of the quartz tube by a fine iron rod for isothermal annealing at 600-850 ℃ for 1h. Followed by quenching in ice water. The annealing and quenching process is always performed in an argon purged environment.
FIG. 1 shows that in example 1, pure (Pr, sm) is obtained 2 Fe 14 The C phase has no other impurity phase, and shows that the preparation method of the invention can obtain pure phase (Pr, sm) 2 Fe 14 C-type rare earth permanent magnet material, in contrast, was not obtained in comparative example 1 due to the absence of Sm element (Pr, sm) 2 Fe 14 And C phase.
FIG. 2 shows that pure (Pr, G) is obtained in example 2d) 2 Fe 14 The C phase has no other impurity phase, and shows that the preparation method of the invention can obtain pure phase (Pr, gd) 2 Fe 14 C-type rare earth permanent magnet material, in contrast, was not obtained (Pr, gd) due to the absence of Gd element in comparative example 1 2 Fe 14 And C phase.
FIG. 3 shows that in comparative example 1, sm and Gd elements were not added (Pr, RE) 2 Fe 14 And C phase.
While particular embodiments of the present invention have been described, it will be obvious to those skilled in the art that various other changes and modifications can be made without departing from the spirit and scope of the invention. It is therefore intended to cover in the appended claims all such changes and modifications that are within the scope of this invention.
Claims (8)
1. Rare earth permanent magnet material Pr capable of improving residual carbon harm reduction 2 Fe 14 A method for stabilizing C phase is characterized by that the medium-heavy rare-earth element is used to replace Pr 2 Fe 14 Part of the Pr atoms in C, a substance is produced with the stoichiometric ratio shown below: (Pr, RE) 2 Fe 14 C, wherein re=sm, gd; and is a 2:14:1 pure phase structure.
2. According to claim 1 (Pr, RE) 2 Fe 14 The C rare earth permanent magnet material is characterized by comprising the following steps:
smelting a mixture comprising RE, pr, fe and C to obtain an ingot;
carrying out melt rapid quenching on the cast ingot to obtain a rapid quenching belt;
annealing and quenching the rapid quenching belt under the protection of argon to obtain (Pr, RE) 2 Fe 14 C-type rare earth permanent magnetic material;
the mass of Fe and C corresponds to the theoretical mass in the formula 1, and the mass of Pr and RE is respectively increased by 1-5% on the basis of the theoretical mass of Pr and RE calculated according to the formula 1.
3. The method of manufacturing according to claim 2, characterized in that the smelting is performed in a high frequency induction smelting furnace.
4. The preparation method according to claim 2, wherein the melt rapid quenching is performed in a melt rapid quenching furnace, and the copper roller rotating speed is 20-40 m/s, the diameter of a quartz tube nozzle is 0.5-2 mm, and the distance from the bottom of the quartz tube to the copper roller is 2-4 mm in the rapid quenching process.
5. The method according to claim 2, wherein the annealing is performed at a temperature of 500 to 1100 ℃ for a time of 0.01 to 1 hour.
6. The method of claim 2, wherein the annealing is performed in a semi-open atmosphere filled with a shielding gas.
7. The method of manufacturing according to claim 2, wherein the annealing comprises: placing a quartz tube with one end closed and one end open into a heating furnace, introducing argon at the speed of 10L/min, heating the furnace to 500-1100 ℃, placing a rapid quenching belt into a crucible or tantalum foil after 10-30min, placing a tube orifice of the quartz tube for preheating, and pushing a sample into the bottom end of the quartz tube for annealing after 5-10 min. The annealing time is 0.01-1h.
8. The method according to claim 2, wherein the quenching is performed by ice water quenching.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310244834.6A CN116855815B (en) | 2023-03-14 | A method for improving the phase stability of rare-earth permanent magnet material Pr2Fe14C to reduce the harm of residual carbon. |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310244834.6A CN116855815B (en) | 2023-03-14 | A method for improving the phase stability of rare-earth permanent magnet material Pr2Fe14C to reduce the harm of residual carbon. |
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| Publication Number | Publication Date |
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| CN116855815A true CN116855815A (en) | 2023-10-10 |
| CN116855815B CN116855815B (en) | 2026-02-13 |
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