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CN115383122B - Hydrogen crushing preparation method of 2:17 sintered samarium cobalt permanent magnet - Google Patents

Hydrogen crushing preparation method of 2:17 sintered samarium cobalt permanent magnet Download PDF

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CN115383122B
CN115383122B CN202211023204.8A CN202211023204A CN115383122B CN 115383122 B CN115383122 B CN 115383122B CN 202211023204 A CN202211023204 A CN 202211023204A CN 115383122 B CN115383122 B CN 115383122B
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hydrogen
alloy
samarium cobalt
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permanent magnet
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CN115383122A (en
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王帅
雍辉
胡季帆
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Taiyuan University of Science and Technology
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Abstract

The invention relates to a hydrogen crushing preparation method of a 2:17 sintered samarium cobalt permanent magnet, belongs to the technical field of magnetic material preparation, and solves the technical problems of difficult hydrogen absorption and dehydrogenation of samarium cobalt alloy and poor magnet orientationThe title comprises the following steps: s1, weighing samarium cobalt permanent magnet alloy raw materials, preparing alloy cast ingots or quick-setting thin strip alloy sheets, and mechanically crushing to obtain alloy particles; s2, alloy particles and a catalyst CuF 2 Mixing the powder, and carrying out hydrogen crushing treatment to obtain hydrogen crushed powder; s3, grinding the hydrogen crushed powder by using an air flow to prepare samarium cobalt alloy powder; s4, performing magnetic field orientation molding and cold isostatic pressing molding on samarium cobalt alloy powder to obtain a green body; s5, sintering, solutionizing and aging the green body to obtain the 2:17 sintered samarium cobalt permanent magnet. The preparation method provided by the invention effectively reduces the hydrogen absorption and desorption pressure and temperature of the samarium cobalt alloy, is easy to operate, control and industrialize, reduces the energy consumption, and the prepared sintered samarium cobalt magnet has excellent magnetic performance.

Description

Hydrogen crushing preparation method of 2:17 sintered samarium cobalt permanent magnet
Technical Field
The invention belongs to the technical field of magnetic material preparation, and particularly relates to a hydrogen crushing preparation method of a 2:17 sintered samarium cobalt permanent magnet.
Background
Rare earth permanent magnet materials are favored for their excellent magnetic properties since the 60 s of the 20 th century, and have been rapidly developed in scientific research, production and application. The 2:17 samarium cobalt permanent magnet material serving as the second-generation rare earth permanent magnet material is widely applied to various fields such as national defense war industry, aerospace, high-precision instruments, medical instruments, microwave devices, sensors, various magnetic transmission devices, high-end motors and the like due to the characteristics of excellent magnetic performance, high Curie temperature, good temperature stability, excellent oxidation resistance, corrosion resistance and the like.
The high-efficiency powder preparation method of the rare earth permanent magnet material by hydrogen crushing is widely applied to the preparation of sintered Nd-Fe-B permanent magnet material, the quick-setting thin strip of the neodymium-iron-boron alloy reacts with hydrogen to generate hydride through hydrogen crushing treatment, and the generated huge stress causes a plurality of microcracks to be generated in NdFeB crystals due to lattice expansion during the generation of the hydride, so that the material becomes loose and even becomes coarse powder, single crystal particles can be formed through further airflow grinding to prepare powder, the final-state magnet orientation is effectively improved, and the comprehensive magnetic performance of the magnet is improved. The 2:17 sintered samarium cobalt alloy cast ingot has the problems of difficult hydrogen absorption and desorption and the like, so that the alloy powder is generally prepared by adopting a method of mechanical crushing and ball milling/air flow milling in production. Because the crushing effect of mechanical crushing and ball milling/air flow milling is poor, a plurality of samarium cobalt alloy powder particles cannot be crushed into single crystals, so that the orientation degree of the samarium cobalt magnet is poor and the magnetic property is reduced.
In the prior art, the patent 'a preparation method of samarium cobalt sintered material' (issued publication number: CN 102651263B) is to prepare magnetic powder by performing hydrogenation disproportionation reaction on an alloy casting belt and then grinding the alloy casting belt into powder by air flow grinding, so as to ensure the integrity of crystal grains and reduce the oxidation of the powder, thereby ensuring the magnetic property of the magnet. The patent 'a sintered samarium cobalt permanent magnet material and a preparation method thereof' (authorized bulletin number: CN 104637642B) is characterized in that the ingot is subjected to hydrogen absorption in a smelting furnace and then is subjected to air flow grinding to prepare powder, so that the production steps are saved, and the energy consumption is reduced. In addition, the patent 'a preparation method of samarium cobalt permanent magnet material' (issued publication number: CN 105304249B) is to absorb hydrogen and dehydrogenate two component alloy ingots respectively, respectively perform air flow grinding to powder, and then perform powder mixing to prepare the samarium cobalt permanent magnet.
Disclosure of Invention
In order to overcome the defects of the prior art and solve the technical problems of difficult hydrogen absorption and dehydrogenation and poor magnet orientation of samarium cobalt alloy, the invention provides a method for preparing a 2:17 sintered samarium cobalt magnet by utilizing a catalyst to promote hydrogen crushing powder preparation, thereby reducing energy consumption, improving hydrogen crushing efficiency, improving magnet orientation degree and effectively improving the comprehensive magnetic performance of the 2:17 samarium cobalt magnet.
In order to achieve the above object, the present invention is achieved by the following technical means.
A hydrogen crushing preparation method of a 2:17 sintered samarium cobalt permanent magnet comprises the following steps:
s1, firstly, weighing samarium cobalt permanent magnet alloy raw materials according to the following components in percentage by weight: (Sm) 1-x Re x ) 25% -26.5%, 6.5% -22.5% of Fe, 2.0% -3.5% of Zr, 3.5% -5.5% of Cu and the balance of Co; wherein x is more than or equal to 0 and less than or equal to 0.4, and Re is one or more than or equal to Pr, nd, gd, dy, tb, er, Y, ho;
then smelting the weighed samarium cobalt permanent magnet alloy raw material in a medium-frequency induction smelting furnace to prepare an alloy cast ingot; or smelting the weighed samarium cobalt permanent magnet alloy raw materials in a vacuum rapid hardening thin strip furnace to prepare a rapid hardening thin strip alloy sheet;
finally, mechanically crushing the alloy cast ingot or the rapid hardening thin strip alloy sheet into alloy particles with the particle size of 0.5 mm-3 mm;
s2, preparing hydrogen powder with an average particle size of 10-500 mu m from the alloy particles prepared in the step S1 by adopting a catalytic hydrogen crushing method, wherein the catalytic hydrogen crushing method comprises the following steps of:
s2-1, alloy particles prepared in the step S1 and a catalyst CuF 2 Fully mixing the powder for 0.5-1 h; wherein the alloy particles and the catalyst CuF 2 The mass percentage of the powder is as follows: 90% -99% of alloy particles, and the balance of catalyst CuF 2 A powder;
s2-2, sequentially performing activation treatment and cyclic hydrogen absorption and desorption treatment on the mixed powder prepared in the step S2-1 in a hydrogen crushing furnace to prepare hydrogen crushed powder;
s3, preparing the hydrogen crushed powder prepared in the step S2 into samarium cobalt alloy powder with the average particle size of 2.5-5 mu m by adopting an air flow grinding method;
s4, weighing the samarium cobalt alloy powder prepared in the step S3 in an air atmosphere, performing orientation molding in a magnetic field of more than 1.5T, and performing cold isostatic pressing molding under the pressure of 230MPa to prepare a green body;
s5, firstly, sintering the green body prepared in the step S4 for 0.5-2 hours at the temperature of 1205-1220 ℃; then cooling the sintered blank to 1140-1190 ℃ along with a furnace for solution treatment, wherein the heat preservation time is 2-10 hours, and rapidly cooling to room temperature after the solution treatment; and finally, heating the blank to 800-850 ℃ again, preserving heat for 8-20 hours, controlling the temperature, cooling to 400 ℃, preserving heat for 1 hour, and cooling to room temperature to obtain the 2:17 sintered samarium cobalt permanent magnet.
Further, in the step S1, the thickness of the prepared alloy cast ingot is 8 mm-12 mm, and the thickness of the prepared rapid hardening ribbon alloy sheet is 0.5 mm-1 mm.
Further, in the step S2-1, the powder mixing process is performed under the protection of high-purity nitrogen atmosphere.
Further, in the step S2-2, the cyclic hydrogen absorption temperature is 20-80 ℃, the hydrogen absorption pressure is 0.2-1 MPa, and the hydrogen absorption time is 1-2 h; the cyclic hydrogen release temperature is 20-80 ℃; the cycle times of hydrogen absorption and desorption are 1 to 3 times.
Further, in the step S2-2, the hydrogen content of the alloy powder after dehydrogenation is 500ppm to 2000ppm.
Further, in the step S5, heat is preserved for 0.5 to 1 hour at 400 ℃ in the sintering temperature rising process, and residual hydrogen in the magnet is further removed.
Further, in the step S5, the temperature control and cooling speed is 0.5 ℃/min to 1 ℃/min.
Compared with the prior art, the invention has the beneficial effects that:
1. the method adopts a catalytic hydrogen crushing method to make samarium cobalt alloy particles and a catalyst CuF 2 The powder was mixed and hydrogen pulverized. CuF (Curie point) 2 The powder is added to accelerate dissociation of hydrogen molecules into hydrogen atoms on the surfaces of alloy particles so as to promote the hydrogen absorption of the alloy particles, and can also generate a rare earth fluoride through oxidation-reduction reaction with the samarium cobalt alloy so as to promote the hydrogen crushing process, so that the hydrogen absorption and release temperature and the hydrogen absorption pressure of the samarium cobalt alloy are effectively reduced, the energy consumption is reduced, and the hydrogen absorption efficiency is improved;
2. the invention utilizes the catalytic hydrogen crushing method to enable the alloy to form Sm 2 Co 17 H x And SmCo 5 H y The gap compound causes the expansion and the fragmentation of crystal lattices to form monocrystalline particles, which is favorable for orientation in the magnet forming process and improves the residual magnetism and magnetic energy product of the magnet;
3. the invention adds the catalyst CuF 2 The powder is subjected to oxidation-reduction reaction with samarium cobalt alloy in the hydrogen crushing process to generate a Cu simple substance, the Cu simple substance is uniformly distributed, and the cellular tissue structure at the grain boundary and the Cu element distribution at the cell wall can be improved in the subsequent heat treatment process, so that the knee point magnetic field and the intrinsic coercivity of the samarium cobalt magnet can be improved.
In a word, the preparation method provided by the invention is easy to operate, control and industrialize, and the prepared sintered samarium cobalt magnet has excellent performance.
Drawings
FIG. 1 is a process flow diagram of the present invention for preparing samarium cobalt magnets using catalytic hydrogen fragmentation.
Detailed Description
The invention provides a hydrogen crushing preparation method of a 2:17 sintered samarium cobalt permanent magnet, which comprises the following steps:
s1, firstly, weighing samarium cobalt permanent magnet alloy raw materials according to the following components in percentage by weight: (Sm) 1-x Re x ) 25% -26.5%, 6.5% -22.5% of Fe, 2.0% -3.5% of Zr, 3.5% -5.5% of Cu and the balance of Co; wherein x is more than or equal to 0 and less than or equal to 0.4, and Re is one or more than or equal to Pr, nd, gd, dy, tb, er, Y, ho;
then smelting the weighed samarium cobalt permanent magnet alloy raw material in a medium-frequency induction smelting furnace to prepare an alloy cast ingot; or smelting the weighed samarium cobalt permanent magnet alloy raw materials in a vacuum rapid hardening thin strip furnace to prepare a rapid hardening thin strip alloy sheet;
finally, mechanically crushing the alloy cast ingot or the rapid hardening thin strip alloy sheet into alloy particles with the particle size of 0.5 mm-3 mm;
the alloy cast ingot or the rapid hardening thin strip alloy sheet prepared by smelting comprises a 2:17H phase and a 1:5H phase, wherein the 2:17H phase has relatively high Fe and Co contents, the 1:5H phase has relatively high rare earth contents, and can absorb certain H atoms in the subsequent hydrogen absorption process to generate interstitial hydrides, and the lattice expansion occurs, so that the alloy is easy to crush, and therefore, the alloy cast ingot or the rapid hardening thin strip alloy sheet can be used as a hydrogen-crushing base alloy. The alloy cast ingot or the rapid hardening thin strip alloy sheet is mechanically crushed into alloy particles with the particle size of 0.5-3 mm, which is more beneficial to the alloy hydrogen absorption and desorption crushing.
S2, preparing hydrogen powder with an average particle size of 10-500 mu m from the alloy particles prepared in the step S1 by adopting a catalytic hydrogen crushing method, wherein the catalytic hydrogen crushing method comprises the following steps of:
s2-1, alloy particles prepared in the step S1 and a catalyst CuF 2 Fully mixing the powder for 0.5-1 h; wherein the alloy particles and the catalyst CuF 2 The mass percentage of the powder is as follows: 90% -99% of alloy particles, and the balance of catalyst CuF 2 A powder;
CuF 2 the powder can not only accelerate the hydrogen molecules on the surface of the alloy particlesDissociation into hydrogen atoms to promote the absorption of hydrogen by alloy particles, and oxidation-reduction reaction with samarium cobalt alloy to generate rare earth fluoride to promote the hydrogen crushing process; in addition, cuF 2 The powder can also undergo oxidation-reduction reaction with samarium cobalt alloy to generate elemental Cu. The elementary Cu can improve the cellular tissue structure at the grain boundary and Cu element distribution at the cell wall in the heat treatment process, so that the magnetic field and intrinsic coercivity of the knee point of the magnet are improved;
s2-2, sequentially performing activation treatment and cyclic hydrogen absorption and desorption treatment on the mixed powder prepared in the step S2-1 in a hydrogen crushing furnace to prepare hydrogen crushed powder;
the purpose of the activation treatment is to make the alloy particles capable of absorbing and releasing hydrogen in a circulating way to the maximum extent. When a certain amount of hydrogen is filled, H-H bonds are dissociated under the action of metal atoms, and atomic hydrogen enters into lattice gaps inside the alloy to generate hydride Sm 2 Co 17 H x And SmCo 5 H y The crystal lattice is expanded and crushed, and then the powder is ground by air flow grinding after the combination, so that alloy powder similar to single crystal particles can be prepared.
S3, preparing the hydrogen crushed powder prepared in the step S2 into samarium cobalt alloy powder with the average particle size of 2.5-5 mu m by adopting an air flow grinding method.
S4, weighing the samarium cobalt alloy powder prepared in the step S3 in an air atmosphere, performing orientation molding in a magnetic field of more than 1.5T, and performing cold isostatic pressing molding under the pressure of 230MPa to prepare a green body; because the catalytic hydrogen crushing method is added, single crystal alloy powder is easier to form, the powder magnetic field orientation molding is facilitated, and the magnet orientation degree is improved.
S5, firstly, sintering the green body prepared in the step S4 for 0.5-2 hours at the temperature of 1205-1220 ℃; then cooling the sintered blank to 1140-1190 ℃ along with a furnace for solution treatment, wherein the heat preservation time is 2-10 hours, and rapidly cooling to room temperature after the solution treatment; and finally, heating the blank to 800-850 ℃ again, preserving heat for 8-20 hours, controlling the temperature, cooling to 400 ℃, preserving heat for 1 hour, and cooling to room temperature to obtain the 2:17 sintered samarium cobalt permanent magnet.
Further, in the step S1, the thickness of the prepared alloy cast ingot is 8-12 mm, and the thickness of the prepared rapid hardening ribbon alloy sheet is 0.5-1 mm, so that the alloy can obtain an ideal microstructure structure and phase composition, and hydrogen crushing can be better carried out in the subsequent process.
Further, in the step S2-1, the powder mixing process is performed under the protection of high-purity nitrogen atmosphere to prevent the oxidation of alloy particles.
Further, in the step S2-2, the cyclic hydrogen absorption temperature is 20-80 ℃, the hydrogen absorption pressure is 0.2-1 MPa, and the hydrogen absorption time is 1-2 h; the cyclic hydrogen release temperature is 20-80 ℃; the cycle times of hydrogen absorption and desorption are 1 to 3 times. Due to addition of catalyst CuF 2 The powder and samarium cobalt alloy particles can absorb hydrogen at lower temperature and pressure, and the hydrogen release temperature is also lower. Through the cyclic absorption and desorption of hydrogen, alloy particles can be crushed more fully and effectively.
Further, in the step S2-2, the hydrogen content of the alloy powder after dehydrogenation is 500-2000 ppm, and the samarium cobalt alloy powder can be prevented from being oxidized in the processes of subsequent material weighing, magnetic field orientation molding and cold isostatic pressing, so that the magnetic property of the magnet is prevented from being deteriorated due to the fact that the oxygen content is too high. In addition, the lower hydrogen content of 500ppm to 2000ppm can be completely removed in the sintering heat preservation at 400 ℃, so that the performance of the final magnet is not affected.
Further, in the step S5, heat is preserved for 0.5 to 1 hour at 400 ℃ in the sintering temperature rising process, and residual hydrogen in the magnet is further removed.
Further, in the step S5, the temperature control and cooling speed is 0.5 ℃/min to 1 ℃/min. The temperature control cooling speed is kept 0.5-1 ℃/min for slow cooling, and Cu element can be enriched towards the cell wall, so that the pinning force of the cell wall to the domain wall is improved, and the magnet is facilitated to obtain high coercivity.
The following examples are illustrative of the invention and are not intended to limit the scope of the invention. Unless otherwise indicated, the examples were all under conventional experimental conditions.
Example 1
A hydrogen crushing preparation method of a 2:17 sintered samarium cobalt permanent magnet comprises the following steps:
s1, firstly, weighing samarium cobalt permanent magnet alloy raw materials according to the following components in percentage by weight: 25% of Sm, 15% of Fe, 3% of Zr, 3.5% of Cu and 53.5% of Co; then smelting the weighed samarium cobalt permanent magnet alloy raw material in a medium-frequency induction smelting furnace to prepare an alloy cast ingot with the thickness of about 10 mm; finally, mechanically crushing the alloy ingot into alloy particles with the particle size of 0.5 mm-3 mm;
s2, preparing hydrogen powder with the average particle diameter of 10-500 mu m from the alloy particles prepared in the step S1 by adopting a catalytic hydrogen crushing method, wherein the catalytic hydrogen crushing method comprises the following steps of:
s2-1, alloy particles prepared in the step S1 and a catalyst CuF 2 Fully mixing the powder for 1h; wherein the alloy particles and the catalyst CuF 2 The mass percentage of the powder is as follows: 95% alloy particles, 5% catalyst CuF 2 A powder;
s2-2, sequentially carrying out activation treatment and cyclic hydrogen absorption and desorption treatment on the mixed powder prepared in the step S2-1 in a hydrogen crushing furnace, wherein the cyclic hydrogen absorption temperature is 60 ℃, the hydrogen absorption pressure is 0.2MPa, and the hydrogen absorption time is 1.5h; the temperature of the cyclic hydrogen release is 80 ℃; the cycle times of hydrogen absorption and desorption are 2 times, and hydrogen crushed powder is prepared;
s3, preparing the hydrogen crushed powder prepared in the step S2 into samarium cobalt alloy powder with the average particle size of 3.8 mu m by adopting an air flow grinding method;
s4, weighing the samarium cobalt alloy powder prepared in the step S3 in an air atmosphere, performing orientation molding in a magnetic field of more than 1.5T, and performing cold isostatic pressing molding under the pressure of 230MPa to prepare a green body;
s5, firstly, sintering the green body prepared in the step S4 for 1h at the temperature of 1210 ℃; then, cooling the sintered blank to 1170 ℃ along with a furnace for solution treatment, wherein the heat preservation time is 4 hours, and rapidly cooling to room temperature after the solution treatment; and finally, heating the blank to 820 ℃ again, preserving heat for 15 hours, cooling to 400 ℃ at a speed of 0.5 ℃/min, preserving heat for 1 hour, and cooling to room temperature by air cooling to obtain the 2:17 sintered samarium cobalt permanent magnet.
The magnetic properties of the 2:17 sintered samarium cobalt permanent magnet prepared in the embodiment 1 are as follows: remanence B r =10.77 kGs, magnetic energy product (BH) m =27.63 MGOe, intrinsic coercivity H cj =38.17kOe。
Example 2
A hydrogen crushing preparation method of a 2:17 sintered samarium cobalt permanent magnet comprises the following steps:
s1, firstly, weighing samarium cobalt permanent magnet alloy raw materials according to the following components in percentage by weight: 26.5% of Sm, 6.5% of Fe, 3.5% of Zr, 3.5% of Cu and 60% of Co; then smelting the weighed samarium cobalt permanent magnet alloy raw material in a medium-frequency induction smelting furnace to prepare an alloy cast ingot with the thickness of about 10 mm; finally, mechanically crushing the alloy ingot into alloy particles with the particle size of 0.5 mm-3 mm;
s2, preparing hydrogen powder with the average particle diameter of 10-500 mu m from the alloy particles prepared in the step S1 by adopting a catalytic hydrogen crushing method, wherein the catalytic hydrogen crushing method comprises the following steps of:
s2-1, alloy particles prepared in the step S1 and a catalyst CuF 2 Fully mixing the powder for 1h; wherein the alloy particles and the catalyst CuF 2 The mass percentage of the powder is as follows: 90% alloy particles, 10% catalyst CuF 2 A powder;
s2-2, sequentially performing activation treatment and cyclic hydrogen absorption and desorption treatment on the mixed powder prepared in the step S2-1 in a hydrogen crushing furnace, wherein the cyclic hydrogen absorption temperature is 50 ℃, the hydrogen absorption pressure is 0.7MPa, and the hydrogen absorption time is 1h; the cyclic hydrogen release temperature is 70 ℃; the cycle times of hydrogen absorption and desorption are 1 time, and hydrogen crushed powder is prepared;
s3, preparing the hydrogen crushed powder prepared in the step S2 into samarium cobalt alloy powder with the average particle size of 4.2 mu m by adopting an air flow grinding method;
s4, weighing the samarium cobalt alloy powder prepared in the step S3 in an air atmosphere, performing orientation molding in a magnetic field of more than 1.5T, and performing cold isostatic pressing molding under the pressure of 230MPa to prepare a green body;
s5, firstly, sintering the green body prepared in the step S4 for 1h at the temperature of 1220 ℃; then, cooling the sintered blank to 1180 ℃ along with a furnace for solution treatment, wherein the heat preservation time is 4 hours, and rapidly cooling the blank to room temperature after the solution treatment; and finally, heating the blank to 830 ℃, preserving heat for 10 hours, cooling to 400 ℃ at a speed of 0.5 ℃/min, preserving heat for 1 hour, and cooling to room temperature by air cooling to obtain the 2:17 sintered samarium cobalt permanent magnet.
The 2:17 sintered samarium cobalt permanent magnet prepared in this example 2 has the following magnetic properties: remanence B r =9.38 kGs, magnetic energy product (BH) m =20.1 MGOe, intrinsic coercivity H cj =36.83kOe。
Example 3
A hydrogen crushing preparation method of a 2:17 sintered samarium cobalt permanent magnet comprises the following steps:
s1, firstly, weighing samarium cobalt permanent magnet alloy raw materials according to the following components in percentage by weight: 25.5% of Sm, 20% of Fe, 2.5% of Zr, 4% of Cu and 48% of Co; then smelting the weighed samarium cobalt permanent magnet alloy raw materials in a vacuum rapid hardening thin strip furnace to prepare a rapid hardening thin strip alloy sheet with the thickness of about 0.6 mm; finally, mechanically crushing the rapid hardening thin strip alloy sheet into alloy particles with the particle size of 0.5 mm-3 mm;
s2, preparing hydrogen powder with the average particle diameter of 10-500 mu m from the alloy particles prepared in the step S1 by adopting a catalytic hydrogen crushing method, wherein the catalytic hydrogen crushing method comprises the following steps of:
s2-1, alloy particles prepared in the step S1 and a catalyst CuF 2 Fully mixing the powder for 0.5h; wherein the alloy particles and the catalyst CuF 2 The mass percentage of the powder is as follows: 99% alloy particles, 1% catalyst CuF 2 A powder;
s2-2, sequentially performing activation treatment and cyclic hydrogen absorption and desorption treatment on the mixed powder prepared in the step S2-1 in a hydrogen crushing furnace, wherein the cyclic hydrogen absorption temperature is 80 ℃, the hydrogen absorption pressure is 1MPa, and the hydrogen absorption time is 2 hours; the temperature of the cyclic hydrogen release is 80 ℃; the cycle times of hydrogen absorption and desorption are 3 times, and hydrogen crushed powder is prepared;
s3, preparing the hydrogen crushed powder prepared in the step S2 into samarium cobalt alloy powder with the average particle size of 3.5 mu m by adopting an air flow grinding method;
s4, weighing the samarium cobalt alloy powder prepared in the step S3 in an air atmosphere, performing orientation molding in a magnetic field of more than 1.5T, and performing cold isostatic pressing molding under the pressure of 230MPa to prepare a green body;
s5, firstly, sintering the green body prepared in the step S4 for 1h at the temperature of 1205 ℃; then, cooling the sintered blank to 1150 ℃ along with a furnace for solution treatment, wherein the heat preservation time is 10h, and rapidly cooling to room temperature after the solution treatment; and finally, heating the blank to 830 ℃, preserving heat for 12 hours, cooling to 400 ℃ at a speed of 1 ℃/min, preserving heat for 1 hour, and cooling to room temperature by air cooling to obtain the 2:17 sintered samarium cobalt permanent magnet.
The magnetic properties of the 2:17 sintered samarium cobalt permanent magnet prepared in this example 3 were: remanence B r =11.75 kGs, magnetic energy product (BH) m =32.84 MGOe, intrinsic coercivity H cj =29.5kOe。
Example 4
A hydrogen crushing preparation method of a 2:17 sintered samarium cobalt permanent magnet comprises the following steps:
s1, firstly, weighing the following components in percentage by weight; then smelting the weighed samarium cobalt permanent magnet alloy raw materials in a vacuum rapid hardening thin strip furnace to prepare a rapid hardening thin strip alloy sheet with the thickness of about 1 mm; finally, mechanically crushing the rapid hardening thin strip alloy sheet into alloy particles with the particle size of 0.5 mm-3 mm;
s2, preparing hydrogen powder with the average particle diameter of 10-500 mu m from the alloy particles prepared in the step S1 by adopting a catalytic hydrogen crushing method, wherein the catalytic hydrogen crushing method comprises the following steps of:
s2-1, alloy particles prepared in the step S1 and a catalyst CuF 2 Fully mixing the powder for 0.5h; wherein the alloy particles and the catalyst CuF 2 The mass percentage of the powder is as follows: 97% alloy particles, 3% catalyst CuF 2 A powder;
s2-2, sequentially carrying out activation treatment and cyclic hydrogen absorption and desorption treatment on the mixed powder prepared in the step S2-1 in a hydrogen crushing furnace, wherein the cyclic hydrogen absorption temperature is 70 ℃, the hydrogen absorption pressure is 0.7MPa, and the hydrogen absorption time is 1.5h; the cyclic hydrogen release temperature is 70 ℃; the cycle times of hydrogen absorption and desorption are 2 times, and hydrogen crushed powder is prepared;
s3, preparing the hydrogen crushed powder prepared in the step S2 into samarium cobalt alloy powder with the average particle size of 3.6 mu m by adopting an air flow grinding method;
s4, weighing the samarium cobalt alloy powder prepared in the step S3 in an air atmosphere, performing orientation molding in a magnetic field of more than 1.5T, and performing cold isostatic pressing molding under the pressure of 230MPa to prepare a green body;
s5, firstly, sintering the green body prepared in the step S4 for 1h at the temperature of 1210 ℃; then, cooling the sintered blank to 1180 ℃ along with a furnace for solution treatment, wherein the heat preservation time is 4 hours, and rapidly cooling the blank to room temperature after the solution treatment; and finally, heating the blank to 830 ℃, preserving heat for 10 hours, cooling to 400 ℃ at a speed of 0.5 ℃/min, preserving heat for 1 hour, and cooling to room temperature by air cooling to obtain the 2:17 sintered samarium cobalt permanent magnet.
The magnetic properties of the 2:17 sintered samarium cobalt permanent magnet prepared in this example 4 were: remanence B r =10.3 kGs, magnetic energy product (BH) m =24.56 MGOe, intrinsic coercivity H cj =37.13kOe。
Example 5
A hydrogen crushing preparation method of a 2:17 sintered samarium cobalt permanent magnet comprises the following steps:
s1, firstly, weighing samarium cobalt permanent magnet alloy raw materials according to the following components in percentage by weight: 22% of Sm, 3% of Pr and Dy:0.4%, fe 17%, zr 2.5%, cu 5.5%, co 49.6%; then smelting the weighed samarium cobalt permanent magnet alloy raw materials in a vacuum rapid hardening thin strip furnace to prepare a rapid hardening thin strip alloy sheet with the thickness of about 0.8 mm; finally, mechanically crushing the rapid hardening thin strip alloy sheet into alloy particles with the particle size of 0.5 mm-3 mm;
s2, preparing hydrogen powder with the average particle diameter of 10-500 mu m from the alloy particles prepared in the step S1 by adopting a catalytic hydrogen crushing method, wherein the catalytic hydrogen crushing method comprises the following steps of:
s2-1, alloy particles prepared in the step S1 and a catalyst CuF 2 Fully mixing the powder for 0.5h; wherein the alloy particles and the catalyst CuF 2 The mass percentage of the powder is as follows: 99% alloy particles, 1% catalyst CuF 2 A powder;
s2-2, sequentially performing activation treatment and cyclic hydrogen absorption and desorption treatment on the mixed powder prepared in the step S2-1 in a hydrogen crushing furnace, wherein the cyclic hydrogen absorption temperature is 80 ℃, the hydrogen absorption pressure is 0.8MPa, and the hydrogen absorption time is 2 hours; the temperature of the cyclic hydrogen release is 80 ℃; the cycle times of hydrogen absorption and desorption are 2 times, and hydrogen crushed powder is prepared;
s3, preparing the hydrogen crushed powder prepared in the step S2 into samarium cobalt alloy powder with the average particle size of 4.2 mu m by adopting an air flow grinding method;
s4, weighing the samarium cobalt alloy powder prepared in the step S3 in an air atmosphere, performing orientation molding in a magnetic field of more than 1.5T, and performing cold isostatic pressing molding under the pressure of 230MPa to prepare a green body;
s5, firstly, sintering the green body prepared in the step S4 for 1h at the temperature of 1215 ℃; then, cooling the sintered blank to 1180 ℃ along with a furnace for solution treatment, wherein the heat preservation time is 8 hours, and rapidly cooling to room temperature after the solution treatment; and finally, heating the blank to 830 ℃, preserving heat for 15 hours, cooling to 400 ℃ at a speed of 0.5 ℃/min, preserving heat for 1 hour, and cooling to room temperature by air cooling to obtain the 2:17 sintered samarium cobalt permanent magnet.
The magnetic properties of the 2:17 sintered samarium cobalt permanent magnet prepared in this example 5 were: remanence B r =11.03 kGs, magnetic energy product (BH) m =28.79 MGOe, intrinsic coercivity H cj =21.58kOe。
Example 6
A hydrogen crushing preparation method of a 2:17 sintered samarium cobalt permanent magnet comprises the following steps:
s1, firstly, weighing samarium cobalt permanent magnet alloy raw materials according to the following components in percentage by weight: 25.5% of Sm, 18% of Fe, 2.5% of Zr, 4.5% of Cu and 49.5% of Co; then smelting the weighed samarium cobalt permanent magnet alloy raw materials in a vacuum rapid hardening thin strip furnace to prepare a rapid hardening thin strip alloy sheet with the thickness of about 0.5 mm; finally, mechanically crushing the rapid hardening thin strip alloy sheet into alloy particles with the particle size of 0.5 mm-3 mm;
s2, preparing hydrogen powder with the average particle diameter of 10-500 mu m from the alloy particles prepared in the step S1 by adopting a catalytic hydrogen crushing method, wherein the catalytic hydrogen crushing method comprises the following steps of:
s2-1, alloy particles prepared in the step S1 and a catalyst CuF 2 Fully mixing the powder for 0.5h; wherein the alloy particles and the catalyst CuF 2 The mass percentage of the powder is as follows: 98% alloy particles, 2% catalyst CuF 2 A powder;
s2-2, sequentially performing activation treatment and cyclic hydrogen absorption and desorption treatment on the mixed powder prepared in the step S2-1 in a hydrogen crushing furnace, wherein the cyclic hydrogen absorption temperature is 60 ℃, the hydrogen absorption pressure is 0.8MPa, and the hydrogen absorption time is 2 hours; the cyclic hydrogen release temperature is 70 ℃; the cycle times of hydrogen absorption and desorption are 3 times, and hydrogen crushed powder is prepared;
s3, preparing the hydrogen crushed powder prepared in the step S2 into samarium cobalt alloy powder with the average particle size of 4.1 mu m by adopting an air flow grinding method;
s4, weighing the samarium cobalt alloy powder prepared in the step S3 in an air atmosphere, performing orientation molding in a magnetic field of more than 1.5T, and performing cold isostatic pressing molding under the pressure of 230MPa to prepare a green body;
s5, firstly, sintering the green body prepared in the step S4 for 1h at the temperature of 1210 ℃; then, cooling the sintered blank to 1150 ℃ along with a furnace for solution treatment, wherein the heat preservation time is 10h, and rapidly cooling to room temperature after the solution treatment; and finally, heating the blank to 830 ℃, preserving heat for 12 hours, cooling to 400 ℃ at a speed of 1 ℃/min, preserving heat for 1 hour, and cooling to room temperature by air cooling to obtain the 2:17 sintered samarium cobalt permanent magnet.
The magnetic properties of the 2:17 sintered samarium cobalt permanent magnet prepared in this example 6 were: remanence B r =11.34 kGs, magnetic energy product (BH) m =30.37 MGOe, intrinsic coercivity H cj =35.6kOe。
The foregoing is merely illustrative of the present invention, and the present invention is not limited thereto, and any changes or substitutions easily contemplated by those skilled in the art within the scope of the present invention should be 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 claims.

Claims (7)

1. The hydrogen crushing preparation method of the 2:17 sintered samarium cobalt permanent magnet is characterized by comprising the following steps of:
s1, firstly, weighing samarium cobalt permanent magnet alloy raw materials according to the following components in percentage by weight: (Sm) 1-x Re x ) 25% -26.5%, 6.5% -22.5% of Fe, 2.0% -3.5% of Zr, 3.5% -5.5% of Cu and the balance of Co; wherein x is more than or equal to 0 and less than or equal to 0.4, re is PrOne or more of Nd, gd, dy, tb, er, Y, ho;
then smelting the weighed samarium cobalt permanent magnet alloy raw material in a medium-frequency induction smelting furnace to prepare an alloy cast ingot; or smelting the weighed samarium cobalt permanent magnet alloy raw materials in a vacuum rapid hardening thin strip furnace to prepare a rapid hardening thin strip alloy sheet;
finally, mechanically crushing the alloy cast ingot or the rapid hardening thin strip alloy sheet into alloy particles with the particle size of 0.5 mm-3 mm;
s2, preparing hydrogen powder with an average particle size of 10-500 mu m from the alloy particles prepared in the step S1 by adopting a catalytic hydrogen crushing method, wherein the catalytic hydrogen crushing method comprises the following steps of:
s2-1, alloy particles prepared in the step S1 and a catalyst CuF 2 Fully mixing the powder for 0.5-1 h; wherein the alloy particles and the catalyst CuF 2 The mass percentage of the powder is as follows: 90% -99% of alloy particles, and the balance of catalyst CuF 2 A powder;
s2-2, sequentially performing activation treatment and cyclic hydrogen absorption and desorption treatment on the mixed powder prepared in the step S2-1 in a hydrogen crushing furnace to prepare hydrogen crushed powder;
s3, preparing the hydrogen crushed powder prepared in the step S2 into samarium cobalt alloy powder with the average particle size of 2.5-5 mu m by adopting an air flow grinding method;
s4, weighing the samarium cobalt alloy powder prepared in the step S3 in an air atmosphere, performing orientation molding in a magnetic field of more than 1.5T, and performing cold isostatic pressing molding under the pressure of 230MPa to prepare a green body;
s5, firstly, sintering the green body prepared in the step S4 for 0.5-2 hours at the temperature of 1205-1220 ℃; then cooling the sintered blank to 1140-1190 ℃ along with a furnace for solution treatment, wherein the heat preservation time is 2-10 hours, and rapidly cooling to room temperature after the solution treatment; and finally, heating the blank to 800-850 ℃ again, preserving heat for 8-20 hours, controlling the temperature, cooling to 400 ℃, preserving heat for 1 hour, and cooling to room temperature to obtain the 2:17 sintered samarium cobalt permanent magnet.
2. The hydrogen crushing preparation method of the 2:17 sintered samarium cobalt permanent magnet according to claim 1, which is characterized by comprising the following steps: in the step S1, the thickness of the prepared alloy cast ingot is 8-12 mm, and the thickness of the prepared rapid hardening thin strip alloy sheet is 0.5-1 mm.
3. The hydrogen crushing preparation method of the 2:17 sintered samarium cobalt permanent magnet according to claim 1, which is characterized by comprising the following steps: in the step S2-1, the powder mixing process is carried out under the protection of high-purity nitrogen atmosphere.
4. The hydrogen crushing preparation method of the 2:17 sintered samarium cobalt permanent magnet according to claim 1, which is characterized by comprising the following steps: in the step S2-2, the cyclic hydrogen absorption temperature is 20-80 ℃, the hydrogen absorption pressure is 0.2-1 MPa, and the hydrogen absorption time is 1-2 h; the cyclic hydrogen release temperature is 20-80 ℃; the cycle times of hydrogen absorption and desorption are 1 to 3 times.
5. The hydrogen crushing preparation method of the 2:17 sintered samarium cobalt permanent magnet according to claim 1, which is characterized by comprising the following steps: in the step S2-2, the hydrogen content of the alloy powder after dehydrogenation is 500 ppm-2000 ppm.
6. The hydrogen crushing preparation method of the 2:17 sintered samarium cobalt permanent magnet according to claim 1, which is characterized by comprising the following steps: in the step S5, heat is preserved for 0.5 to 1 hour at the temperature of 400 ℃ in the sintering temperature rising process.
7. The hydrogen crushing preparation method of the 2:17 sintered samarium cobalt permanent magnet according to claim 1, which is characterized by comprising the following steps: in the step S5, the temperature control and cooling speed is 0.5-1 ℃/min.
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