CN113903587A - Preparation method of high-temperature 2:17 type sintered samarium-cobalt magnet - Google Patents
Preparation method of high-temperature 2:17 type sintered samarium-cobalt magnet Download PDFInfo
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Abstract
The invention relates to a preparation method of a high-temperature 2:17 type sintered samarium cobalt magnet, belongs to the technical field of magnetic material preparation, solves the technical problem of high-temperature magnetic performance of the 2:17 type sintered samarium cobalt magnet, and comprises the following steps: preparing alloy ingot casting → milling powder by air flow → magnetic field orientation forming, cold isostatic pressing → sintering, solution treatment → aging treatment to prepare samarium cobalt magnet. The aging treatment of the invention adopts a microwave aging heat treatment method: firstly, preserving heat at 900-920 ℃ to form a Cu element net enrichment area; then, the magnet is subjected to heat preservation at 850-870 ℃ to obtain large cell size and wide cell wall phase; and then, preserving the heat at 800-830 ℃ to obtain a more complete cellular tissue structure. The invention can make the magnet obtain uniform and complete cellular organization structure, and the cell and cell wall phase have higher domain wall performance at 500 ℃, thus greatly improving the high-temperature magnetic performance of the magnet.
Description
Technical Field
The invention belongs to the technical field of magnetic material preparation, and particularly relates to a preparation method of a high-temperature 2:17 type sintered samarium-cobalt magnet.
Background
Since the 20 th century and the 60 th era, rare earth permanent magnetic materials are favored due to excellent magnetic properties, and are rapidly developed in scientific research, production and application. The 2:17 type samarium cobalt permanent magnet material serving as a second-generation rare earth permanent magnet material has the characteristics of high Curie temperature, excellent magnetic property, good temperature stability, excellent oxidation resistance and corrosion resistance and the like, and is widely applied to various fields such as national defense and military industry, aerospace, high-precision instruments, medical instruments, microwave devices, sensors, various magnetic transmission devices, high-end motors and the like.
In recent years, with the rapid development of science and technology, higher requirements are put forward on the development and application of permanent magnetic materials, and particularly in the field of aerospace, a magnet capable of still keeping higher magnetic performance at high temperature, namely a magnet with the service temperature of more than 500 ℃, namely Sm (samarium cobalt) is urgently needed2Co17Permanent magnets of the type are the best choice. High service temperature Sm2Co17The type sintered permanent magnet can still keep high magnetic performance at the temperature of more than 500 ℃, and further improves the magnetic performance at high temperature, thereby being beneficial to the miniaturization and the precision of a device used at high temperature. High service temperature Sm2Co17The magnetic properties of the permanent magnet are closely related to its microstructure. Usually, Sm is prepared by a suitable aging process2Co17The permanent magnet can obtain typical cell structure, and Cu element is enriched in cell wall phase. Because the coercive force of the magnet is made into a pinning mechanism, the coercive force is derived from the domain wall performance difference of the 1:5 cell wall and the 2:17 cell phase, and the domain wall performance is determined by the magnetocrystalline anisotropy field and the exchange integral constant of the 1:5 cell wall and the 2:17 cell phase, the different cell structures and the Cu element distribution result in that the 1:5 cell wall and the 2:17 cell phase of the magnet have different magnetocrystalline anisotropy fields and exchange integral constants, so that the magnet obtains different magnetic properties.
Sm is optimized by adjusting aging process2Co17The microstructure of the high-temperature permanent magnet can make the magnet obtain ideal magnetic performance. At present, Chinese patent discloses "a high HkA preparation method of samarium cobalt sintered permanent magnet material (publication number: CN 110473703A) comprises the steps of performing ultrahigh pressure pre-tempering (720-740 ℃), and then performing graded tempering or slow cooling tempering treatment, thereby improving the coercive force H of the knee point of the magnetkBut it is a high-performance Sm for preparing materials used below 350 DEG C2Co17Method for forming permanent magnets by low temperature pre-temperingThe size of the cellular microstructure is reduced, thereby increasing the volume fraction of the Cu-rich 1:5H cell wall pinning phase, and aiming at improving the high-performance Sm2Co17H of permanent magnetkThe value is obtained. Chinese patent discloses a microwave aging treatment method of samarium cobalt based rare earth permanent magnet material (publication number: CN 104233138A), which adopts microwave heating and heat preservation and then carries out secondary artificial aging or multi-stage artificial aging, aiming at refining cellular structure and improving saturation magnetization and mechanical property of the magnet, but does not improve the high-temperature magnetic property of the magnet.
Disclosure of Invention
In order to overcome the defects of the prior art and solve the technical problem of high-temperature magnetic performance of a 2:17 type sintered samarium cobalt magnet, the invention provides a preparation method of the high-temperature 2:17 type sintered samarium cobalt magnet, the high-temperature 2:17 type sintered samarium cobalt magnet prepared by adopting a microwave aging heat treatment process can obtain a large-size cellular structure and a thick cell wall, and the magnet cell and the cell wall have large domain wall performance difference at the high temperature of 500 ℃, so that good high-temperature magnetic performance can be obtained.
The invention is realized by the following technical scheme.
A preparation method of a high-temperature 2:17 type sintered samarium-cobalt magnet comprises the following steps:
s1, preparing an alloy ingot:
firstly, weighing samarium cobalt alloy raw materials according to the following weight percentage: (Sm)1-xRex) 25 to 27%, 5 to 10% Fe, 2.5 to 3.5% Zr, 6 to 8% Cu, and the balance Co; wherein x is more than or equal to 0 and less than or equal to 0.4, and Re is one or more of Gd, Dy, Tb and Er;
then, smelting the weighed samarium cobalt alloy raw material in a medium-frequency induction smelting furnace, and casting in a single-side water-cooling disc copper mold to obtain an alloy ingot;
s2, airflow milling powder:
mechanically crushing the alloy ingot prepared in the step S1 into alloy particles with the particle size of 0.4-2 mm;
then, fully mixing the alloy particles with an antioxidant to prepare a mixture, and preparing the mixture into alloy powder with the average particle size of 2.5-5 microns by adopting an airflow milling powder method;
s3, magnetic field orientation forming and cold isostatic pressing:
carrying out orientation forming on the alloy powder prepared in the step S2 in a magnetic field orientation forming press, and then carrying out cold isostatic pressing to prepare a green body;
s4, sintering and solution treatment:
firstly, heating a green body prepared by cold isostatic pressing in the step S3 under a vacuum condition, and respectively carrying out heat preservation treatment at 300 ℃, 600 ℃ and 900 ℃ for 1 h; secondly, heating to 1200-1230 ℃ and sintering for 0.5-2 h; thirdly, carrying out solution treatment: cooling to 1160-1190 ℃ along with the furnace, and keeping the temperature for 2-4 h; finally, quickly cooling the mixture to room temperature;
s5, aging treatment:
adopting a microwave aging heat treatment method, firstly, heating the magnet prepared after the solution treatment in the step S4 to 900-920 ℃, and preserving the heat for 15-30min to form a Cu element net enrichment area inside the magnet; secondly, cooling to 850-; thirdly, cooling to 800-830 ℃, and preserving heat for 2-6 hours; and finally, controlling the temperature to be cooled to 400 ℃, and quickly cooling the mixture to room temperature by air to obtain the high-temperature 2:17 type sintered samarium-cobalt magnet.
Further, in the step S1, the samarium cobalt alloy raw material is weighed according to the following weight percentage: (Sm)1-xRex) 25.5 to 26.5%, 5.5 to 9.5% Fe, 2.6 to 3.4% Zr, 6 to 7.8% Cu, and the balance Co.
Further, in step S5, the temperature raising process of the magnet is performed in vacuum, and when the temperature raising is finished, argon gas of 0.2MPa is filled for subsequent heat preservation and cooling treatment.
Further, in the step S5, the average spacing of the Cu element enrichment areas is 50-100 nm, and the average mass percentage concentration of the Cu element peak values in the enrichment areas is 6-12%.
Further, in the step S5, the average size of the cell structure is 150 to 200nm, and the average thickness of the cell wall is 15 to 30 nm.
Further, in step S5, the temperature-controlled cooling sequentially includes the following stages:
the first stage is as follows: cooling to 700 ℃ at the speed of 1.5 ℃/min and preserving heat for 1 h;
and a second stage: cooling to 600 ℃ at the speed of 1.5 ℃/min and preserving heat for 1.5 h;
and a third stage: cooling to 500 ℃ at the speed of 1.5 ℃/min and preserving heat for 2 h;
a fourth stage: cooling to 400 ℃ at the speed of 1 ℃/min.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention can heat the magnet integrally by a microwave aging heat treatment method, so that the material is heated uniformly and has small temperature gradient, the magnet prepared by aging has more uniform cellular structure and element distribution at the cell wall, and the cell wall of the magnet can form uniform pinning effect, therefore, the magnet can obtain a high knee point magnetic field HkTo improve the magnetic properties of the magnet;
2. according to the invention, the aging heat treatment is carried out at a higher temperature for a short time (900-. Thus, when the magnet is further cooled to 850-. When the magnet is then insulated at 800-830 ℃ for 2-6 h, a more complete cellular structure can be obtained. Sm2Co17The coercive force of the permanent magnet at room temperature is attractive pinning, and the attractive pinning is changed to repulsive pinning along with the temperature rise. The coercivity is repulsion type pinning when the magnet is at high temperature of 500 ℃. Because the invention obtains a large cell structure and a wide cell wall phase, under the condition of a certain Cu content, the wider the cell wall, the lower the concentration and concentration gradient of Cu element at the cell wall of the magnet, so that the 1:5H phase of the cell wall of the magnet has higher domain wall energy, and the domain wall energy difference of the 1:5H cell wall and the 2:17R cell phase is larger, therefore, the magnet can obtain higher coercive force at high temperature.
In a word, the preparation method provided by the invention is easy to operate, control and industrialize, the prepared high-temperature sintered samarium-cobalt magnet is excellent in performance, and the problems of low coercive force and poor magnetic performance of the traditional samarium-cobalt magnet at high temperature are solved.
Drawings
FIG. 1 is a TEM image of the cell structure of a magnet according to an embodiment.
FIG. 2 is a TEM image of the cell structure of the comparative example magnet.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention. Unless otherwise specified, the examples follow conventional experimental conditions.
The invention provides a preparation method of a high-temperature 2:17 type sintered samarium-cobalt magnet, which comprises the following steps:
s1, preparing an alloy ingot:
firstly, weighing samarium cobalt alloy raw materials according to the following weight percentage: (Sm)1-xRex) 25 to 27%, 5 to 10% Fe, 2.5 to 3.5% Zr, 6 to 8% Cu, and the balance Co; wherein x is more than or equal to 0 and less than or equal to 0.4, and Re is one or more of Gd, Dy, Tb and Er; because the 1:5H cell wall phase has higher rare earth content than the 2:17R cell phase, the rare earth content with the mass percentage of 25-27% can ensure that the magnet can obtain a wider cell wall phase in the subsequent aging treatment process;
then, smelting the weighed samarium cobalt alloy raw material in a medium-frequency induction smelting furnace, and casting in a single-side water-cooling disc copper mold to obtain an alloy ingot;
s2, airflow milling powder:
mechanically crushing the alloy ingot prepared in the step S1 into alloy particles with the particle size of 0.4-2 mm;
then, fully mixing the alloy particles with an antioxidant to prepare a mixture, and preparing the mixture into alloy powder with the average particle size of 2.5-5 microns by adopting an airflow milling powder method;
s3, magnetic field orientation forming and cold isostatic pressing:
carrying out orientation forming on the alloy powder prepared in the step S2 in a magnetic field orientation forming press, and then carrying out cold isostatic pressing to prepare a green body;
s4, sintering and solution treatment:
firstly, heating a green body prepared by cold isostatic pressing in the step S3 under a vacuum condition, and respectively carrying out heat preservation treatment at 300 ℃, 600 ℃ and 900 ℃ for 1 h; secondly, heating to 1200-1230 ℃ and sintering for 0.5-2 h; thirdly, carrying out solution treatment: cooling to 1160-1190 ℃ along with the furnace, and keeping the temperature for 2-4 h; finally, quickly cooling the mixture to room temperature;
s5, aging treatment:
adopting a microwave aging heat treatment method, firstly, heating the magnet prepared after the solution treatment in the step S4 to 900-920 ℃, and preserving the heat for 15-30min to form a Cu element net enrichment area inside the magnet; secondly, cooling to 850-; a large-size cellular structure can be formed inside the magnet due to the formation of Cu element enrichment areas with wider intervals when the magnet is subjected to heat preservation at the temperature of 900-920 ℃ for 15-30 min; thirdly, cooling to 800-830 ℃, and preserving heat for 2-6 hours; further preserving the temperature at 800-830 ℃, so that the magnet can form a more complete cell structure, uniform pinning of a cell wall relative to a domain wall is facilitated, and the magnetic performance of the magnet is improved; and finally, controlling the temperature to be cooled to 400 ℃, and quickly cooling the mixture to room temperature by air to obtain the high-temperature 2:17 type sintered samarium-cobalt magnet.
The microwave aging heat treatment method can heat the whole magnet, so that the material is heated uniformly and has small temperature gradient. Because the formation of the cellular structure of the magnet is closely related to the temperature, the magnet prepared by aging has more uniform cellular structure and element distribution at the cell wall, and the uniform pinning effect can be formed at the cell wall of the magnet, so that the magnet can obtain a high knee point magnetic field HkThereby improving the magnetic properties of the magnet.
Sm2Co17The coercive force of the permanent magnet at room temperature is attractive pinning, and the attractive pinning is changed to repulsive pinning along with the temperature rise. The coercivity is repulsion type pinning when the magnet is at high temperature of 500 ℃. Because the invention obtains large cell structure and wide cell wall phase, the wider the cell wall, the lower the concentration and concentration gradient of Cu element at the cell wall of the magnet under the condition of certain Cu content, which leads to higher domain wall energy of the 1:5H phase of the magnet cell wall, and the larger the domain wall energy difference of the 1:5H cell wall and the 2:17R cell phase, therefore, the magnet can be used at high temperatureTo obtain a higher coercivity.
Further, in the step S1, the samarium cobalt alloy raw material is weighed according to the following weight percentage: (Sm)1-xRex) 25.5 to 26.5%, 5.5 to 9.5% Fe, 2.6 to 3.4% Zr, 6 to 7.8% Cu, and the balance Co.
Further, in the step S5, the temperature rising process of the magnet is performed in vacuum, and when the temperature rising is finished, 0.2MPa argon gas is filled for subsequent heat preservation and cooling treatment, so as to prevent oxidation of the magnet during long-time heat treatment.
Further, in the step S5, the average spacing of the Cu element enrichment areas is 50-100 nm, and the average mass percentage concentration of the Cu element peak in the enrichment areas is 6-12%, so that a basis is provided for Cu element enrichment at the cell wall of the final magnet.
Further, in the step S5, the average size of the cell structure is 150 to 200nm, and the average thickness of the cell wall is 15 to 30 nm.
Further, in step S5, the temperature-controlled cooling sequentially includes the following stages:
the first stage is as follows: cooling to 700 ℃ at the speed of 1.5 ℃/min and preserving heat for 1 h;
and a second stage: cooling to 600 ℃ at the speed of 1.5 ℃/min and preserving heat for 1.5 h;
and a third stage: cooling to 500 ℃ at the speed of 1.5 ℃/min and preserving heat for 2 h;
a fourth stage: cooling to 400 ℃ at the speed of 1 ℃/min.
In the aging temperature-control cooling process of the magnet, Cu element is enriched to the cell wall, and the long-time heat treatment is carried out in the interval, so that the cell wall can obtain high Cu concentration, the pinning force of the cell wall to a domain wall is improved, and the magnet can obtain high coercive force and knee point magnetic field.
Hereinafter, the present invention will be further described with reference to specific examples and drawings.
Example one
A preparation method of a high-temperature 2:17 type sintered samarium-cobalt magnet comprises the following steps:
s1, preparing an alloy ingot:
firstly, weighing samarium cobalt alloy raw materials according to the following weight percentage: 26 percent of Sm, 5.5 percent of Fe, 3.1 percent of Zr, 7.2 percent of Cu and 58.2 percent of Co;
then, smelting the weighed samarium cobalt alloy raw material in a medium-frequency induction smelting furnace, and casting in a single-side water-cooling disc copper mold to obtain an alloy ingot;
s2, airflow milling powder:
mechanically crushing the alloy ingot prepared in the step S1 into alloy particles with the particle size of 0.4-2 mm;
then, fully mixing the alloy particles with an antioxidant to prepare a mixture, and preparing the mixture into alloy powder with the average particle size range of 4.5 microns by adopting a jet milling powder method;
s3, magnetic field orientation forming and cold isostatic pressing:
carrying out orientation forming on the samarium cobalt alloy powder prepared in the step S2 in a magnetic field orientation forming press, and then carrying out cold isostatic pressing to prepare a green body;
s4, sintering and solution treatment:
firstly, heating a green body prepared by cold isostatic pressing in the step S3 under a vacuum condition, and respectively carrying out heat preservation treatment at 300 ℃, 600 ℃ and 900 ℃ for 1 h; secondly, heating to 1228 ℃ and sintering for 1 h; thirdly, carrying out solution treatment: cooling to 1180 ℃ along with the furnace, and keeping the temperature for 4 hours; finally, quickly cooling the mixture to room temperature;
s5, aging treatment:
adopting a microwave aging heat treatment method, firstly, heating the magnet prepared after the solid solution in the step S4 to 920 ℃, and preserving the temperature for 17min to form a Cu element net enrichment area in the magnet, wherein the average distance between the Cu element enrichment areas is 95nm, and the average mass percentage concentration of Cu elements in the enrichment areas is 8%; secondly, cooling to 870 ℃, and preserving heat for 4h to form a large-size cellular structure inside the magnet, wherein the average size of the cellular structure is 198nm, and the average thickness of the cell wall is 28 nm; then, cooling to 830 ℃, and preserving heat for 2 h; and finally, controlling temperature and cooling: cooling to 700 ℃ at the speed of 1.5 ℃/min for 1h → cooling to 600 ℃ at the speed of 1.5 ℃/min for 1.5h → cooling to 500 ℃ at the speed of 1.5 ℃/min for 2h → cooling to 400 ℃ at the speed of 1 ℃/min, and rapidly cooling to room temperature by air to prepare the high-temperature 2:17 type sintered samarium-cobalt magnet.
Example two
A preparation method of a high-temperature 2:17 type sintered samarium-cobalt magnet comprises the following steps:
s1, preparing an alloy ingot:
firstly, weighing samarium cobalt alloy raw materials according to the following weight percentage: 25.5 percent of Sm, 9.5 percent of Fe, 3 percent of Zr, 6.5 percent of Cu and 55.5 percent of Co;
then, smelting the weighed samarium cobalt alloy raw material in a medium-frequency induction smelting furnace, and casting in a single-side water-cooling disc copper mold to obtain an alloy ingot;
s2, airflow milling powder:
mechanically crushing the alloy ingot prepared in the step S1 into alloy particles with the particle size of 0.4-2 mm;
then, fully mixing the alloy particles with an antioxidant to prepare a mixture, and preparing the mixture into alloy powder with the average particle size range of 3 microns by adopting a jet mill powder preparation method;
s3, magnetic field orientation forming and cold isostatic pressing:
carrying out orientation forming on the samarium cobalt alloy powder prepared in the step S2 in a magnetic field orientation forming press, and then carrying out cold isostatic pressing to prepare a green body;
s4, sintering and solution treatment:
firstly, heating a green body prepared by cold isostatic pressing in the step S3 under a vacuum condition, and respectively carrying out heat preservation treatment at 300 ℃, 600 ℃ and 900 ℃ for 1 h; secondly, heating to 1215 ℃ and sintering for 1 h; thirdly, carrying out solution treatment: cooling to 1170 ℃ along with the furnace, and keeping the temperature for 4 h; finally, quickly cooling the mixture to room temperature;
s5, aging treatment:
adopting a microwave aging heat treatment method, firstly, heating the magnet prepared after the solid solution in the step S4 to 900 ℃, and preserving the temperature for 25min to form a Cu element net enrichment area in the magnet, wherein the average distance between the Cu element enrichment areas is 55nm, and the average mass percentage concentration of the Cu element in the enrichment areas is 7.5%; secondly, cooling to 850 ℃ and preserving the temperature for 4h to form a large-size cellular structure inside the magnet, wherein the average size of the cellular structure is 158nm, and the average thickness of the cell wall is 18 nm; then, cooling to 830 ℃, and preserving heat for 4 hours; and finally, controlling temperature and cooling: cooling to 700 ℃ at the speed of 1.5 ℃/min for 1h → cooling to 600 ℃ at the speed of 1.5 ℃/min for 1.5h → cooling to 500 ℃ at the speed of 1.5 ℃/min for 2h → cooling to 400 ℃ at the speed of 1 ℃/min, and rapidly cooling to room temperature by air to prepare the high-temperature 2:17 type sintered samarium-cobalt magnet.
EXAMPLE III
A preparation method of a high-temperature 2:17 type sintered samarium-cobalt magnet comprises the following steps:
s1, preparing an alloy ingot:
firstly, weighing samarium cobalt alloy raw materials according to the following weight percentage: 26.2 percent of Sm, 6 percent of Fe, 2.6 percent of Zr, 6 percent of Cu and 59.2 percent of Co;
then, smelting the weighed samarium cobalt alloy raw material in a medium-frequency induction smelting furnace, and casting in a single-side water-cooling disc copper mold to obtain an alloy ingot;
s2, airflow milling powder:
mechanically crushing the alloy ingot prepared in the step S1 into alloy particles with the particle size of 0.4-2 mm;
then, fully mixing the alloy particles with an antioxidant to prepare a mixture, and preparing the mixture into alloy powder with the average particle size range of 4.2 microns by adopting a jet milling powder method;
s3, magnetic field orientation forming and cold isostatic pressing:
carrying out orientation forming on the samarium cobalt alloy powder prepared in the step S2 in a magnetic field orientation forming press, and then carrying out cold isostatic pressing to prepare a green body;
s4, sintering and solution treatment:
firstly, heating a green body prepared by cold isostatic pressing in the step S3 under a vacuum condition, and respectively carrying out heat preservation treatment at 300 ℃, 600 ℃ and 900 ℃ for 1 h; secondly, heating to 1220 ℃ and sintering for 1.5 h; thirdly, carrying out solution treatment: cooling to 1175 ℃ along with the furnace, and keeping the temperature for 4 hours; finally, quickly cooling the mixture to room temperature;
s5, aging treatment:
adopting a microwave aging heat treatment method, firstly, heating the magnet prepared after the solid solution in the step S4 to 910 ℃, and preserving the temperature for 30min to form a Cu element net enrichment area in the magnet, wherein the average distance between the Cu element enrichment areas is 89nm, and the average mass percentage concentration of Cu elements in the enrichment areas is 6.2%; secondly, cooling to 860 ℃ and preserving the temperature for 4h to form a large-size cellular tissue structure inside the magnet, wherein the average size of the cellular tissue structure is 182nm, and the average thickness of the cell wall is 24 nm; then, cooling to 825 ℃, and preserving heat for 3 hours; and finally, controlling temperature and cooling: cooling to 700 ℃ at the speed of 1.5 ℃/min for 1h → cooling to 600 ℃ at the speed of 1.5 ℃/min for 1.5h → cooling to 500 ℃ at the speed of 1.5 ℃/min for 2h → cooling to 400 ℃ at the speed of 1 ℃/min, and rapidly cooling to room temperature by air to prepare the high-temperature 2:17 type sintered samarium-cobalt magnet.
Example four
A preparation method of a high-temperature 2:17 type sintered samarium-cobalt magnet comprises the following steps:
s1, preparing an alloy ingot:
firstly, weighing samarium cobalt alloy raw materials according to the following weight percentage: 26.5 percent of Sm, 5.6 percent of Fe, 3.4 percent of Zr, 7 percent of Cu and 57.5 percent of Co;
then, smelting the weighed samarium cobalt alloy raw material in a medium-frequency induction smelting furnace, and casting in a single-side water-cooling disc copper mold to obtain an alloy ingot;
s2, airflow milling powder:
mechanically crushing the alloy ingot prepared in the step S1 into alloy particles with the particle size of 0.4-2 mm;
then, fully mixing the alloy particles with an antioxidant to prepare a mixture, and preparing the mixture into alloy powder with the average particle size range of 4.4 microns by adopting a jet milling powder method;
s3, magnetic field orientation forming and cold isostatic pressing:
carrying out orientation forming on the samarium cobalt alloy powder prepared in the step S2 in a magnetic field orientation forming press, and then carrying out cold isostatic pressing to prepare a green body;
s4, sintering and solution treatment:
firstly, heating a green body prepared by cold isostatic pressing in the step S3 under a vacuum condition, and respectively carrying out heat preservation treatment at 300 ℃, 600 ℃ and 900 ℃ for 1 h; secondly, heating to 1225 ℃ and sintering for 1 h; thirdly, carrying out solution treatment: cooling to 1180 ℃ along with the furnace, and keeping the temperature for 4 hours; finally, quickly cooling the mixture to room temperature;
s5, aging treatment:
adopting a microwave aging heat treatment method, firstly, heating the magnet prepared after the solid solution in the step S4 to 920 ℃, and preserving the temperature for 15min to form a Cu element net enrichment area in the magnet, wherein the average distance between the Cu element enrichment areas is 93nm, and the average mass percentage concentration of Cu elements in the enrichment areas is 7.9%; secondly, cooling to 870 ℃, and preserving heat for 4h to form a large-size cellular structure inside the magnet, wherein the average size of the cellular structure is 192nm, and the average thickness of the cell wall is 26 nm; then, cooling to 830 ℃, and preserving heat for 2 h; and finally, controlling temperature and cooling: cooling to 700 ℃ at the speed of 1.5 ℃/min for 1h → cooling to 600 ℃ at the speed of 1.5 ℃/min for 1.5h → cooling to 500 ℃ at the speed of 1.5 ℃/min for 2h → cooling to 400 ℃ at the speed of 1 ℃/min, and rapidly cooling to room temperature by air to prepare the high-temperature 2:17 type sintered samarium-cobalt magnet.
EXAMPLE five
A preparation method of a high-temperature 2:17 type sintered samarium-cobalt magnet comprises the following steps:
s1, preparing an alloy ingot:
firstly, weighing samarium cobalt alloy raw materials according to the following weight percentage: 26.3 percent of Sm, 6.2 percent of Fe, 3.2 percent of Zr, 7.8 percent of Cu and 56.5 percent of Co;
then, smelting the weighed samarium cobalt alloy raw material in a medium-frequency induction smelting furnace, and casting in a single-side water-cooling disc copper mold to obtain an alloy ingot;
s2, airflow milling powder:
mechanically crushing the alloy ingot prepared in the step S1 into alloy particles with the particle size of 0.4-2 mm;
then, fully mixing the alloy particles with an antioxidant to prepare a mixture, and preparing the mixture into alloy powder with the average particle size range of 3.8 microns by adopting a jet milling powder method;
s3, magnetic field orientation forming and cold isostatic pressing:
carrying out orientation forming on the samarium cobalt alloy powder prepared in the step S2 in a magnetic field orientation forming press, and then carrying out cold isostatic pressing to prepare a green body;
s4, sintering and solution treatment:
firstly, heating a green body prepared by cold isostatic pressing in the step S3 under a vacuum condition, and respectively carrying out heat preservation treatment at 300 ℃, 600 ℃ and 900 ℃ for 1 h; secondly, heating to 1223 ℃ and sintering for 1 h; thirdly, carrying out solution treatment: cooling to 1178 ℃ along with the furnace, and keeping the temperature for 4 hours; finally, quickly cooling the mixture to room temperature;
s5, aging treatment:
adopting a microwave aging heat treatment method, firstly, heating the magnet prepared after the solid solution in the step S4 to 910 ℃, and preserving the temperature for 20min to form a Cu element net enrichment area in the magnet, wherein the average distance between the Cu element enrichment areas is 67nm, and the average mass percentage concentration of Cu elements in the enrichment areas is 10.3%; secondly, cooling to 865 ℃ and preserving heat for 3h to form a large-size cellular structure inside the magnet, wherein the average size of the cellular structure is 182nm, and the average thickness of the cell wall is 22 nm; then, cooling to 825 ℃, and preserving heat for 4 hours; and finally, controlling temperature and cooling: cooling to 700 ℃ at the speed of 1.5 ℃/min for 1h → cooling to 600 ℃ at the speed of 1.5 ℃/min for 1.5h → cooling to 500 ℃ at the speed of 1.5 ℃/min for 2h → cooling to 400 ℃ at the speed of 1 ℃/min, and rapidly cooling to room temperature by air to prepare the high-temperature 2:17 type sintered samarium-cobalt magnet.
EXAMPLE six
A preparation method of a high-temperature 2:17 type sintered samarium-cobalt magnet comprises the following steps:
s1, preparing an alloy ingot:
firstly, weighing samarium cobalt alloy raw materials according to the following weight percentage: 26.1 percent of Sm, 7 percent of Fe, 3.1 percent of Zr, 6.8 percent of Cu and 57 percent of Co;
then, smelting the weighed samarium cobalt alloy raw material in a medium-frequency induction smelting furnace, and casting in a single-side water-cooling disc copper mold to obtain an alloy ingot;
s2, airflow milling powder:
mechanically crushing the alloy ingot prepared in the step S1 into alloy particles with the particle size of 0.4-2 mm;
then, fully mixing the alloy particles with an antioxidant to prepare a mixture, and preparing the mixture into alloy powder with the average particle size range of 3.5 microns by adopting a jet milling powder method;
s3, magnetic field orientation forming and cold isostatic pressing:
carrying out orientation forming on the samarium cobalt alloy powder prepared in the step S2 in a magnetic field orientation forming press, and then carrying out cold isostatic pressing to prepare a green body;
s4, sintering and solution treatment:
firstly, heating a green body prepared by cold isostatic pressing in the step S3 under a vacuum condition, and respectively carrying out heat preservation treatment at 300 ℃, 600 ℃ and 900 ℃ for 1 h; secondly, heating to 1220 ℃ and sintering for 2 h; thirdly, carrying out solution treatment: cooling to 1170 ℃ along with the furnace, and keeping the temperature for 4 h; finally, quickly cooling the mixture to room temperature;
s5, aging treatment:
adopting a microwave aging heat treatment method, firstly, heating the magnet prepared after the solid solution in the step S4 to 905 ℃, and preserving the temperature for 30min to form a Cu element net enrichment area in the magnet, wherein the average distance between the Cu element enrichment areas is 73nm, and the average mass percentage concentration of Cu elements in the enrichment areas is 8.3%; secondly, cooling to 850 ℃ and preserving the temperature for 5h to form a large-size cellular structure inside the magnet, wherein the average size of the cellular structure is 167nm, and the average thickness of the cell wall is 20 nm; then, cooling to 800 ℃, and preserving heat for 6 h; and finally, controlling temperature and cooling: cooling to 700 ℃ at the speed of 1.5 ℃/min for 1h → cooling to 600 ℃ at the speed of 1.5 ℃/min for 1.5h → cooling to 500 ℃ at the speed of 1.5 ℃/min for 2h → cooling to 400 ℃ at the speed of 1 ℃/min, and rapidly cooling to room temperature by air to prepare the high-temperature 2:17 type sintered samarium-cobalt magnet.
Comparative example 1
A preparation method of a high-temperature 2:17 type sintered samarium-cobalt magnet comprises the steps of mixing and S1-S4.
In step S5, aging the magnet using a tube furnace: after solid solution, heating the magnet to 830 ℃, preserving heat for 10 hours, and then carrying out temperature control cooling: cooling to 700 ℃ at the speed of 1.5 ℃/min for 1h → cooling to 600 ℃ at the speed of 1.5 ℃/min for 1.5h → cooling to 500 ℃ at the speed of 1.5 ℃/min for 2h → cooling to 400 ℃ at the speed of 1 ℃/min, and rapidly cooling to room temperature to prepare the high-temperature samarium-cobalt magnet.
The high temperature samarium cobalt magnets prepared in the above examples and comparative examples were subjected to magnetic property tests at room temperature (25 ℃ C.) and at high temperature (500 ℃ C.) respectively. The performance results are shown in table 1 below.
As can be seen by comparing example one with comparative example one, samarium cobalt magnets prepared by the method of the present invention have higher magnetic properties at high temperatures (500 ℃ C.). And the magnet in the embodiment can obtain good magnetic performance at high temperature. Therefore, the method has certain value in the aspects of improving the microstructure of the magnet and improving the magnetic property of the magnet.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (6)
1. A preparation method of a high-temperature 2:17 type sintered samarium-cobalt magnet is characterized by comprising the following steps of:
s1, preparing an alloy ingot:
firstly, weighing samarium cobalt alloy raw materials according to the following weight percentage: (Sm)1-xRex) 25 to 27%, 5 to 10% Fe, 2.5 to 3.5% Zr, 6 to 8% Cu, and the balance Co; wherein x is more than or equal to 0 and less than or equal to 0.4, and Re is one or more of Gd, Dy, Tb and Er;
then, smelting the weighed samarium cobalt alloy raw material in a medium-frequency induction smelting furnace, and casting in a single-side water-cooling disc copper mold to obtain an alloy ingot;
s2, airflow milling powder:
mechanically crushing the alloy ingot prepared in the step S1 into alloy particles with the particle size of 0.4-2 mm;
then, fully mixing the alloy particles with an antioxidant to prepare a mixture, and preparing the mixture into alloy powder with the average particle size of 2.5-5 microns by adopting an airflow milling powder method;
s3, magnetic field orientation forming and cold isostatic pressing:
carrying out orientation forming on the alloy powder prepared in the step S2 in a magnetic field orientation forming press, and then carrying out cold isostatic pressing to prepare a green body;
s4, sintering and solution treatment:
firstly, heating a green body prepared by cold isostatic pressing in the step S3 under a vacuum condition, and respectively carrying out heat preservation treatment at 300 ℃, 600 ℃ and 900 ℃ for 1 h; secondly, heating to 1200-1230 ℃ and sintering for 0.5-2 h; thirdly, carrying out solution treatment: cooling to 1160-1190 ℃ along with the furnace, and keeping the temperature for 2-4 h; finally, quickly cooling the mixture to room temperature;
s5, aging treatment:
adopting a microwave aging heat treatment method, firstly, heating the magnet prepared after the solution treatment in the step S4 to 900-920 ℃, and preserving the heat for 15-30min to form a Cu element net enrichment area inside the magnet; secondly, cooling to 850-; thirdly, cooling to 800-830 ℃, and preserving heat for 2-6 hours; and finally, controlling the temperature to be cooled to 400 ℃, and quickly cooling the mixture to room temperature by air to obtain the high-temperature 2:17 type sintered samarium-cobalt magnet.
2. The method of making a high temperature 2:17 type sintered samarium cobalt magnet of claim 1, further comprising: in step S1, weighing samarium cobalt alloy raw materials in the following weight percentages: (Sm)1-xRex) 25.5 to 26.5%, 5.5 to 9.5% Fe, 2.6 to 3.4% Zr, 6 to 7.8% Cu, and the balance Co.
3. The method of making a high temperature 2:17 type sintered samarium cobalt magnet of claim 1, further comprising: in step S5, the temperature of the magnet is raised in vacuum, and after the temperature is raised, 0.2MPa argon gas is introduced for subsequent heat preservation and cooling.
4. The method of making a high temperature 2:17 type sintered samarium cobalt magnet of claim 1, further comprising: in the step S5, the average spacing of the Cu element enrichment areas is 50-100 nm, and the average mass percentage concentration of Cu element peaks in the enrichment areas is 6-12%.
5. The method of making a high temperature 2:17 type sintered samarium cobalt magnet of claim 1, further comprising: in step S5, the average size of the cell structure is 150-200 nm, and the average thickness of the cell wall is 15-30 nm.
6. The method of making a high temperature 2:17 type sintered samarium cobalt magnet of claim 1, further comprising: in step S5, the temperature-controlled cooling sequentially includes the following stages:
the first stage is as follows: cooling to 700 ℃ at the speed of 1.5 ℃/min and preserving heat for 1 h;
and a second stage: cooling to 600 ℃ at the speed of 1.5 ℃/min and preserving heat for 1.5 h;
and a third stage: cooling to 500 ℃ at the speed of 1.5 ℃/min and preserving heat for 2 h;
a fourth stage: cooling to 400 ℃ at the speed of 1 ℃/min.
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