CN115383122A - Hydrogen crushing preparation method of 2 - Google Patents

Hydrogen crushing preparation method of 2 Download PDF

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CN115383122A
CN115383122A CN202211023204.8A CN202211023204A CN115383122A CN 115383122 A CN115383122 A CN 115383122A CN 202211023204 A CN202211023204 A CN 202211023204A CN 115383122 A CN115383122 A CN 115383122A
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hydrogen
alloy
powder
temperature
samarium
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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 2The technical problems of difficult hydrogen absorption and dehydrogenation and poor magnet orientation comprise the following steps: s1, weighing samarium-cobalt permanent magnet alloy raw materials, preparing alloy ingots or rapid-hardening thin strip alloy sheets, and mechanically crushing to obtain alloy particles; s2, mixing the alloy particles with a catalyst CuF 2 Mixing the powders, and performing hydrogen crushing treatment to obtain hydrogen crushed powder; s3, preparing samarium cobalt alloy powder from the hydrogen crushed powder through airflow milling; s4, performing magnetic field orientation forming and cold isostatic pressing forming on samarium cobalt alloy powder to obtain a green body; and S5, sintering, solid dissolving and aging the green body to obtain the 2. 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 property.

Description

Hydrogen crushing preparation method of 2
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.
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-type samarium cobalt permanent magnet material serving as the second-generation rare earth permanent magnet material has the characteristics of excellent magnetic property, high Curie temperature, good temperature stability, excellent oxidation resistance, excellent 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.
The hydrogen crushing is used as the high-efficiency powder preparation method of the rare earth permanent magnet material, and is widely applied to the preparation of the sintered Nd-Fe-B permanent magnet material. And because the 2. Because the crushing effect of mechanical crushing and ball milling/jet milling powder is poor, a plurality of samarium cobalt alloy powder particles can not be crushed into single crystals, the orientation degree of the samarium cobalt magnet is poor, and the magnetic property is reduced.
In the prior art, the patent of 'a preparation method of samarium cobalt sintered material' (No. CN 102651263B) adopts an alloy casting belt to carry out hydrogenation disproportionation reaction, and then powder is prepared by air flow milling to prepare magnetic powder, aiming at ensuring the integrity of crystal grains and reducing the oxidation of the powder, thereby ensuring the magnetic performance of a magnet. The patent 'a sintered samarium cobalt permanent magnet material and a preparation method thereof' (No. CN 104637642B) is that hydrogen is absorbed by an ingot in a smelting furnace, and then powder is milled by airflow, thereby saving production steps and reducing energy consumption. In addition, the patent "a method for preparing samarium cobalt permanent magnet material" (No. CN 105304249B) is to prepare samarium cobalt permanent magnet by respectively absorbing hydrogen and dehydrogenating alloy cast ingots with two components, respectively grinding into powder by air flow, and then mixing the powder.
Disclosure of Invention
In order to overcome the defects of the prior art and solve the technical problems of difficult hydrogen absorption and dehydrogenation of the samarium-cobalt alloy and poor magnet orientation, the invention provides a method for preparing a 2.
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:
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 to 26.5 percent of Fe, 6.5 to 22.5 percent of Fe, 2.0 to 3.5 percent of Zr, 3.5 to 5.5 percent 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 one or more of Pr, nd, gd, dy, tb, er, Y and Ho;
then, smelting the weighed samarium-cobalt permanent magnet alloy raw material in a medium-frequency induction smelting furnace to prepare an alloy ingot; or smelting the weighed samarium-cobalt permanent magnet alloy raw material 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 0.5mm to 3mm;
s2, preparing the alloy particles prepared in the step S1 into hydrogen crushed powder with the average particle size of 10-500 microns by a catalytic hydrogen crushing method, wherein the catalytic hydrogen crushing method comprises the following steps:
s2-1, mixing the alloy particles prepared in the step S1 with a catalyst CuF 2 Fully mixing the powder for 0.5h to 1h; wherein the alloy particles are mixed with a catalyst CuF 2 The powder comprises the following components in percentage by mass: 90-99% of alloy particles, and the balance of catalyst CuF 2 Powder;
s2-2, sequentially carrying out activation treatment and circular 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 microns by adopting an air jet mill method;
s4, weighing the samarium cobalt alloy powder prepared in the step S3 in an air atmosphere, then carrying out orientation forming under a magnetic field of more than 1.5T, and finally carrying out cold isostatic pressing forming under 230MPa pressure to obtain a green body;
s5, firstly, sintering the green body prepared in the step S4 at a temperature of 1205-1220 ℃ for 0.5-2h; then, cooling the sintered blank to 1140-1190 ℃ along with a furnace, carrying out solution treatment for 2-10h, and quickly cooling to room temperature after solution treatment; and finally, heating the blank again to 800-850 ℃, keeping the temperature for 8-20h, then controlling the temperature to be cooled to 400 ℃, keeping the temperature for 1h, and then cooling to room temperature by air to obtain the 2.
Further, in the step S1, the thickness of the prepared alloy ingot ranges from 8mm to 12mm, and the thickness of the prepared quick-setting thin strip alloy sheet ranges from 0.5mm to 1mm.
Further, in the step S2-1, the powder mixing process is performed under the protection of a high-purity nitrogen atmosphere.
Further, in the step S2-2, the circulating hydrogen absorption temperature is 20-80 ℃, the hydrogen absorption pressure is 0.2MPa-1MPa, and the hydrogen absorption time is 1h-2h; the temperature of the circular hydrogen release is 20-80 ℃; the number of hydrogen absorption and desorption cycles is 1 to 3.
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 preservation is carried out for 0.5 to 1h at 400 ℃ in the sintering temperature rise process, and residual hydrogen in the magnet is further removed.
Further, in the step S5, the temperature control cooling speed is 0.5-1 ℃/min.
Compared with the prior art, the invention has the beneficial effects that:
1. the method adopts a catalytic hydrogen crushing method to mix samarium-cobalt alloy particles and a catalyst CuF 2 And mixing the powders, and performing hydrogen crushing. CuF 2 The addition of the powder can accelerate hydrogen molecules to dissociate into hydrogen atoms on the surface of alloy particles so as to promote the hydrogen absorption of the alloy particles, and can also generate rare earth fluoride through an oxidation-reduction reaction with the samarium-cobalt alloy so as to promote the hydrogen crushing process, so that the hydrogen absorption and desorption 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 fragmentation method to ensure that the alloy can form Sm 2 Co 17 H x And SmCo 5 H y The interstitial compound causes lattice expansion and crushing to form single crystal particles, which is beneficial to orientation in the magnet forming process and improves the residual magnetism and magnetic energy product of the magnet;
3. the invention adds catalyst CuF 2 The powder is subjected to oxidation-reduction reaction with the samarium cobalt alloy in the hydrogen crushing process to generate a Cu simple substance, the Cu simple substance is uniformly distributed, and the cellular 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 magnetic field and the intrinsic coercive force of the samarium cobalt magnet can be improved.
In a word, the preparation method provided by the invention is easy to operate and control and is industrialized, and the prepared sintered samarium-cobalt magnet has excellent performance.
Drawings
FIG. 1 is a process flow diagram for preparing samarium cobalt magnets using catalytic hydrogen fragmentation in accordance with the present invention.
Detailed Description
The invention provides a hydrogen crushing preparation method of a 2 type 17 sintered samarium cobalt permanent magnet, which comprises the following steps:
s1, firstly, weighing the following components in percentage by weightSamarium cobalt permanent magnet alloy raw materials: (Sm) 1-x Re x ) 25 to 26.5 percent of Fe, 6.5 to 22.5 percent of Fe, 2.0 to 3.5 percent of Zr, 3.5 to 5.5 percent 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 one or more of Pr, nd, gd, dy, tb, er, Y and Ho;
then, smelting the weighed samarium-cobalt permanent magnet alloy raw material in a medium-frequency induction smelting furnace to prepare an alloy ingot; or smelting the weighed samarium-cobalt permanent magnet alloy raw material 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 0.5mm to 3mm;
the alloy ingot or the rapid-hardening thin strip alloy sheet prepared by smelting comprises a 2. Mechanically crushing the alloy ingot or the rapid-hardening thin strip alloy sheet into alloy particles with the particle size of 0.5-3mm, which is more favorable for hydrogen absorption and desorption crushing of the alloy.
S2, preparing the alloy particles prepared in the step S1 into hydrogen crushed powder with the average particle size of 10-500 microns by a catalytic hydrogen crushing method, wherein the catalytic hydrogen crushing method comprises the following steps:
s2-1, mixing the alloy particles prepared in the step S1 with a catalyst CuF 2 Fully mixing the powder for 0.5h to 1h; wherein the alloy particles are mixed with a catalyst CuF 2 The powder comprises the following components in percentage by mass: 90-99% of alloy particles, and the balance of catalyst CuF 2 Powder;
CuF 2 the powder can not only accelerate hydrogen molecules to be dissociated into hydrogen atoms on the surfaces of alloy particles to promote the hydrogen absorption of the alloy particles, but also can generate a rare earth fluoride to promote the hydrogen crushing process by carrying out an oxidation-reduction reaction with samarium-cobalt alloy; further, cuF 2 The powder can also undergo redox reaction with samarium cobalt alloy to produce elemental Cu. The elementary substance Cu can improve the cellular structure and cells at the grain boundary in the heat treatment processCu element is distributed on the wall, so that the magnetic field and intrinsic coercive force of the knee point of the magnet are improved;
s2-2, sequentially carrying out activation treatment and circular hydrogen absorption and desorption treatment on the mixed powder prepared in the step S2-1 in a hydrogen crushing furnace to obtain hydrogen crushed powder;
the purpose of the activation treatment is to allow the alloy particles to absorb and release hydrogen in a maximum cycle. When a certain amount of hydrogen is filled, H-H bonds are dissociated under the action of metal atoms, and the atomic hydrogen enters into the internal crystal lattice gaps of the alloy to generate hydride Sm 2 Co 17 H x And SmCo 5 H y The alloy powder close to single crystal particles can be prepared by causing the crystal lattice to expand and break and then matching with the airflow milling powder.
And 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 microns by adopting an air flow mill method.
S4, weighing the samarium cobalt alloy powder prepared in the step S3 in an air atmosphere, then carrying out orientation forming in a magnetic field of more than 1.5T, and finally carrying out cold isostatic pressing forming under 230MPa to obtain a green body; because the catalytic hydrogen crushing method is added, the single crystal alloy powder is easier to form, the powder magnetic field orientation forming is facilitated, and the magnet orientation degree is improved.
S5, firstly, sintering the green body prepared in the step S4 at a temperature of 1205-1220 ℃ for 0.5-2h; then, cooling the sintered blank to 1140-1190 ℃ along with a furnace, carrying out solution treatment for 2-10h, and quickly cooling to room temperature after solution treatment; and finally, heating the blank again to 800-850 ℃, keeping the temperature for 8-20h, then controlling the temperature and cooling to 400 ℃, keeping the temperature for 1h, and then cooling to the room temperature by air to obtain the 2.
Furthermore, in the step S1, the thickness of the prepared alloy ingot is from 8mm to 12mm, and the thickness of the prepared quick-setting thin strip alloy sheet is from 0.5mm to 1mm, so that the alloy can obtain an ideal microstructure and phase composition, and the alloy can be better subjected to hydrogen crushing in the subsequent process.
Further, in the step S2-1, the powder mixing process is performed under the protection of a high-purity nitrogen atmosphere, so as to prevent the oxidation of the alloy particles.
Further, in the step S2-2, the circulating hydrogen absorption temperature is 20-80 ℃, the hydrogen absorption pressure is 0.2MPa-1MPa, and the hydrogen absorption time is 1h-2h; the temperature of the circular hydrogen release is 20-80 ℃; the number of hydrogen absorption and desorption cycles is 1 to 3. CuF due to the addition of catalyst 2 The powder, samarium cobalt alloy particles, can absorb hydrogen at lower temperatures and pressures and the hydrogen release temperature is also lower. Through circulating hydrogen absorption and desorption, alloy particles can be more sufficiently and effectively crushed.
Further, in the step S2-2, the hydrogen content of the alloy powder after dehydrogenation is 500ppm to 2000ppm, so that the samarium cobalt alloy powder can be prevented from being oxidized in the subsequent processes of material weighing, magnetic field orientation forming and cold isostatic pressing, and the magnetic performance of the magnet is prevented from being deteriorated due to overhigh oxygen content. In addition, the lower hydrogen content of 500-2000 ppm can be completely eliminated in the sintering heat preservation at 400 ℃, so that the performance of the final magnet is not influenced.
Further, in the step S5, heat preservation is carried out for 0.5 to 1h at 400 ℃ in the sintering temperature rise process, and residual hydrogen in the magnet is further removed.
Further, in the step S5, the temperature control cooling speed is 0.5-1 ℃/min. The temperature control cooling speed is kept at 0.5 to 1 ℃/min for slow cooling, so that the Cu element can be enriched to the cell wall, the pinning force of the cell wall to a domain wall is improved, and the magnet is favorable for obtaining high coercivity.
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.
Example 1
A hydrogen crushing preparation method of a 2:
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 ingot with the thickness of about 10 mm; finally, mechanically crushing the alloy cast ingot into alloy particles with the particle size of 0.5mm to 3mm;
s2, preparing the alloy particles prepared in the step S1 into hydrogen crushed powder with the average particle size of 10-500 microns by adopting a catalytic hydrogen crushing method, wherein the catalytic hydrogen crushing method comprises the following steps:
s2-1, mixing the alloy particles prepared in the step S1 with a catalyst CuF 2 Fully mixing the powder for 1h; wherein the alloy particles are mixed with a catalyst CuF 2 The powder comprises the following components in percentage by mass: 95% of alloy particles and 5% of catalyst CuF 2 Powder;
s2-2, sequentially carrying out activation treatment and circular hydrogen absorption and desorption treatment on the mixed powder prepared in the step S2-1 in a hydrogen crushing furnace, wherein the circular hydrogen absorption temperature is 60 ℃, the hydrogen absorption pressure is 0.2MPa, and the hydrogen absorption time is 1.5h; the temperature of the circular hydrogen release is 80 ℃; absorbing and releasing hydrogen for 2 times to obtain 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 3.8 microns by adopting a jet mill method;
s4, weighing the samarium cobalt alloy powder prepared in the step S3 in an air atmosphere, then carrying out orientation forming in a magnetic field of more than 1.5T, and finally carrying out cold isostatic pressing forming under 230MPa to obtain a green body;
s5, firstly, sintering the green body prepared in the step S4 at the temperature of 1210 ℃ for 1h; then, cooling the sintered blank to 1170 ℃ along with a furnace for solution treatment, keeping the temperature for 4h, and quickly cooling the blank to room temperature after the solution treatment; and finally, heating the blank again to 820 ℃, keeping the temperature for 15h, cooling to 400 ℃ at the speed of 0.5 ℃/min, keeping the temperature for 1h, and then air-cooling to room temperature to obtain the 2.
The magnetic properties of the 2: remanence B r =10.77kGs, magnetic energy product (BH) m =27.63MGOe, intrinsic coercive force H cj =38.17kOe。
Example 2
A hydrogen crushing preparation method of a 2:
s1, firstly, weighing samarium-cobalt permanent magnet alloy raw materials according to the following components in percentage by weight: 26.5 percent of Sm, 6.5 percent of Fe, 3.5 percent of Zr, 3.5 percent of Cu and 60 percent of Co; then, smelting the weighed samarium-cobalt permanent magnet alloy raw material in a medium-frequency induction smelting furnace to prepare an alloy ingot with the thickness of about 10 mm; finally, mechanically crushing the alloy cast ingot into alloy particles with the particle size of 0.5mm to 3mm;
s2, preparing the alloy particles prepared in the step S1 into hydrogen crushed powder with the average particle size of 10-500 microns by adopting a catalytic hydrogen crushing method, wherein the catalytic hydrogen crushing method comprises the following steps:
s2-1, mixing the alloy particles prepared in the step S1 with a catalyst CuF 2 Fully mixing the powder for 1h; wherein the alloy particles are mixed with a catalyst CuF 2 The powder comprises the following components in percentage by mass: 90% of alloy particles and 10% of catalyst CuF 2 Powder;
s2-2, sequentially carrying out activation treatment and circular hydrogen absorption and desorption treatment on the mixed powder prepared in the step S2-1 in a hydrogen crushing furnace, wherein the circular hydrogen absorption temperature is 50 ℃, the hydrogen absorption pressure is 0.7MPa, and the hydrogen absorption time is 1h; the temperature of the circular hydrogen release is 70 ℃; hydrogen absorption and desorption cycle times 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 microns by adopting an airflow mill method;
s4, weighing the samarium cobalt alloy powder prepared in the step S3 in an air atmosphere, then carrying out orientation forming in a magnetic field of more than 1.5T, and finally carrying out cold isostatic pressing forming under 230MPa to obtain a green body;
s5, firstly, sintering the green body prepared in the step S4 at the temperature of 1220 ℃ for 1h; then, cooling the sintered blank to 1180 ℃ along with a furnace for solution treatment, keeping the temperature for 4 hours, and quickly cooling the blank to room temperature after the solution treatment; and finally, heating the blank again to 830 ℃, keeping the temperature for 10 hours, cooling to 400 ℃ at the speed of 0.5 ℃/min, keeping the temperature for 1 hour, and then air-cooling to room temperature to obtain the 2.
The magnetic properties of the 2: remanence B r =9.38kGs, magnetic energy product (BH) m =20.1MGOe, intrinsic coercive force H cj =36.83kOe。
Example 3
A hydrogen crushing preparation method of a 2:
s1, firstly, weighing samarium-cobalt permanent magnet alloy raw materials according to the following components in percentage by weight: 25.5 percent of Sm, 20 percent of Fe, 2.5 percent of Zr, 4 percent of Cu and 48 percent of Co; then smelting the weighed samarium-cobalt permanent magnet alloy raw materials in a vacuum rapid hardening thin strip furnace to obtain a rapid hardening thin strip alloy sheet with the thickness of about 0.6 mm; finally, mechanically crushing the quick-setting thin strip alloy sheet into alloy particles with the particle size of 0.5mm to 3mm;
s2, preparing the alloy particles prepared in the step S1 into hydrogen crushed powder with the average particle size of 10-500 microns by adopting a catalytic hydrogen crushing method, wherein the catalytic hydrogen crushing method comprises the following steps:
s2-1, mixing the alloy particles prepared in the step S1 with a catalyst CuF 2 Fully mixing the powder for 0.5h; wherein the alloy particles are mixed with a catalyst CuF 2 The powder comprises the following components in percentage by mass: 99% of alloy particles, 1% of catalyst CuF 2 Powder;
s2-2, sequentially carrying out activation treatment and circular hydrogen absorption and desorption treatment on the mixed powder prepared in the step S2-1 in a hydrogen crushing furnace, wherein the circular hydrogen absorption temperature is 80 ℃, the hydrogen absorption pressure is 1MPa, and the hydrogen absorption time is 2h; the temperature of the circular hydrogen release is 80 ℃; hydrogen absorption and desorption circulation times 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 microns by adopting an airflow mill method;
s4, weighing the samarium cobalt alloy powder prepared in the step S3 in an air atmosphere, then carrying out orientation forming in a magnetic field of more than 1.5T, and finally carrying out cold isostatic pressing forming under 230MPa to obtain a green body;
s5, firstly, sintering the green body prepared in the step S4 at a temperature of 1205 ℃ for 1h; then, cooling the sintered blank to 1150 ℃ along with a furnace for solution treatment, keeping the temperature for 10 hours, and quickly cooling the blank to room temperature after the solution treatment; and finally, heating the blank again to 830 ℃, keeping the temperature for 12 hours, cooling to 400 ℃ at the speed of 1 ℃/min, keeping the temperature for 1 hour, and then cooling to room temperature to obtain the 2.
The magnetic property of the 2: remanence B r =11.75kGs, magnetic energy product (BH) m ＝32.84MGOe, intrinsic coercivity H cj =29.5kOe。
Example 4
A hydrogen crushing preparation method of a 2:
s1, firstly, weighing 20% of Sm, 5.3% of Gd, 15.5% of Fe, 2.8% of Zr, 5% of Cu and 51.4% of Co according to the following components in percentage by weight; then smelting the weighed samarium-cobalt permanent magnet alloy raw material 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 quick-setting thin strip alloy sheet into alloy particles with the particle size of 0.5mm to 3mm;
s2, preparing the alloy particles prepared in the step S1 into hydrogen crushed powder with the average particle size of 10-500 microns by adopting a catalytic hydrogen crushing method, wherein the catalytic hydrogen crushing method comprises the following steps:
s2-1, mixing the alloy particles prepared in the step S1 with a catalyst CuF 2 Fully mixing the powder for 0.5h; wherein the alloy particles are mixed with a catalyst CuF 2 The powder comprises the following components in percentage by mass: 97% of alloy particles and 3% of catalyst CuF 2 Powder;
s2-2, sequentially carrying out activation treatment and circular hydrogen absorption and desorption treatment on the mixed powder prepared in the step S2-1 in a hydrogen crushing furnace, wherein the circular hydrogen absorption temperature is 70 ℃, the hydrogen absorption pressure is 0.7MPa, and the hydrogen absorption time is 1.5h; the temperature of the circular hydrogen release is 70 ℃; absorbing and releasing hydrogen for 2 times to obtain 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 3.6 microns by adopting a jet mill method;
s4, weighing the samarium cobalt alloy powder prepared in the step S3 in an air atmosphere, then carrying out orientation forming in a magnetic field of more than 1.5T, and finally carrying out cold isostatic pressing forming under 230MPa to obtain a green body;
s5, firstly, sintering the green body prepared in the step S4 for 1 hour at the temperature of 1210 ℃; then, cooling the sintered blank to 1180 ℃ along with a furnace for solution treatment, keeping the temperature for 4 hours, and quickly cooling the blank to room temperature after the solution treatment; and finally, heating the blank again to 830 ℃, keeping the temperature for 10 hours, cooling to 400 ℃ at the speed of 0.5 ℃/min, keeping the temperature for 1 hour, and then air-cooling to room temperature to obtain the 2.
The magnetic properties of the 2: remanence B r =10.3kGs, magnetic energy product (BH) m =24.56MGOe, intrinsic coercive force H cj =37.13kOe。
Example 5
A hydrogen crushing preparation method of a 2:
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 percent, 17 percent of Fe, 2.5 percent of Zr, 5.5 percent of Cu and 49.6 percent of Co; then smelting the weighed samarium-cobalt permanent magnet alloy raw materials in a vacuum rapid hardening thin strip furnace to obtain a rapid hardening thin strip alloy sheet with the thickness of about 0.8 mm; finally, mechanically crushing the quick-setting thin strip alloy sheet into alloy particles with the particle size of 0.5mm to 3mm;
s2, preparing the alloy particles prepared in the step S1 into hydrogen crushed powder with the average particle size of 10-500 microns by adopting a catalytic hydrogen crushing method, wherein the catalytic hydrogen crushing method comprises the following steps:
s2-1, mixing the alloy particles prepared in the step S1 with a catalyst CuF 2 Fully mixing the powder for 0.5h; wherein the alloy particles are mixed with a catalyst CuF 2 The powder comprises the following components in percentage by mass: 99% of alloy particles, 1% of catalyst CuF 2 Powder;
s2-2, sequentially carrying out activation treatment and circular hydrogen absorption and desorption treatment on the mixed powder prepared in the step S2-1 in a hydrogen crushing furnace, wherein the circular hydrogen absorption temperature is 80 ℃, the hydrogen absorption pressure is 0.8MPa, and the hydrogen absorption time is 2h; the temperature of the circular hydrogen release is 80 ℃; hydrogen absorption and desorption cycle times 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 microns by adopting an airflow mill method;
s4, weighing the samarium cobalt alloy powder prepared in the step S3 in an air atmosphere, then carrying out orientation forming in a magnetic field of more than 1.5T, and finally carrying out cold isostatic pressing forming under 230MPa to obtain a green body;
s5, firstly, sintering the green body prepared in the step S4 for 1h at 1215 ℃; then, cooling the sintered blank along with a furnace to 1180 ℃ for solution treatment, keeping the temperature for 8 hours, and quickly cooling the sintered blank to room temperature by air after the solution treatment; and finally, heating the blank again to 830 ℃, keeping the temperature for 15h, cooling to 400 ℃ at the speed of 0.5 ℃/min, keeping the temperature for 1h, and then air-cooling to room temperature to obtain the 2.
The magnetic properties of the 2: remanence B r =11.03kGs, magnetic energy product (BH) m =28.79MGOe, intrinsic coercive force H cj =21.58kOe。
Example 6
A hydrogen crushing preparation method of a 2:
s1, firstly, weighing samarium-cobalt permanent magnet alloy raw materials according to the following components in percentage by weight: 25.5 percent of Sm, 18 percent of Fe, 2.5 percent of Zr, 4.5 percent of Cu and 49.5 percent of Co; then smelting the weighed samarium-cobalt permanent magnet alloy raw materials in a vacuum rapid hardening thin strip furnace to obtain a rapid hardening thin strip alloy sheet with the thickness of about 0.5 mm; finally, mechanically crushing the quick-setting thin strip alloy sheet into alloy particles with the particle size of 0.5mm to 3mm;
s2, preparing the alloy particles prepared in the step S1 into hydrogen crushed powder with the average particle size of 10-500 microns by adopting a catalytic hydrogen crushing method, wherein the catalytic hydrogen crushing method comprises the following steps:
s2-1, mixing the alloy particles prepared in the step S1 with a catalyst CuF 2 Fully mixing the powder for 0.5h; wherein the alloy particles are mixed with a catalyst CuF 2 The powder comprises the following components in percentage by mass: 98% of alloy particles and 2% of catalyst CuF 2 Powder;
s2-2, sequentially carrying out activation treatment and circular hydrogen absorption and desorption treatment on the mixed powder prepared in the step S2-1 in a hydrogen crushing furnace, wherein the circular hydrogen absorption temperature is 60 ℃, the hydrogen absorption pressure is 0.8MPa, and the hydrogen absorption time is 2h; the temperature of the circular hydrogen discharge is 70 ℃; hydrogen absorption and desorption circulation times 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 microns by adopting an airflow mill method;
s4, weighing the samarium cobalt alloy powder prepared in the step S3 in an air atmosphere, then carrying out orientation forming under a magnetic field of more than 1.5T, and finally carrying out cold isostatic pressing forming under 230MPa pressure to obtain a green body;
s5, firstly, sintering the green body prepared in the step S4 at the temperature of 1210 ℃ for 1h; then, cooling the sintered blank to 1150 ℃ along with a furnace for solution treatment, keeping the temperature for 10 hours, and quickly cooling the blank to room temperature after the solution treatment; and finally, heating the blank again to 830 ℃, keeping the temperature for 12h, cooling to 400 ℃ at the speed of 1 ℃/min, keeping the temperature for 1h, and then air-cooling to room temperature to obtain the 2.
The magnetic properties of the 2: remanence B r =11.34kGs, magnetic energy product (BH) m =30.37MGOe, intrinsic coercive force H cj =35.6kOe。
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 (7)

1. A hydrogen crushing preparation method of a 2:
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 to 26.5 percent of Fe, 6.5 to 22.5 percent of Zr, 2.0 to 3.5 percent of Cu, 3.5 to 5.5 percent 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 one or more of Pr, nd, gd, dy, tb, er, Y and Ho;
then, smelting the weighed samarium-cobalt permanent magnet alloy raw material in a medium-frequency induction smelting furnace to prepare an alloy ingot; or smelting the weighed samarium-cobalt permanent magnet alloy raw material 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 0.5mm to 3mm;
s2, preparing the alloy particles prepared in the step S1 into hydrogen crushed powder with the average particle size of 10-500 microns by a catalytic hydrogen crushing method, wherein the catalytic hydrogen crushing method comprises the following steps:
s2-1, mixing the alloy particles prepared in the step S1 with a catalyst CuF 2 Fully mixing the powder for 0.5h to 1h; wherein the alloy particles are mixed with a catalyst CuF 2 The powder comprises the following components in percentage by mass: 90-99% of alloy particles, and the balance of catalyst CuF 2 Powder;
s2-2, sequentially carrying out activation treatment and circular 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 microns by adopting an airflow mill method;
s4, weighing the samarium cobalt alloy powder prepared in the step S3 in an air atmosphere, then carrying out orientation forming in a magnetic field of more than 1.5T, and finally carrying out cold isostatic pressing forming under 230MPa to obtain a green body;
s5, firstly, sintering the green body prepared in the step S4 at a temperature of 1205-1220 ℃ for 0.5-2h; then, cooling the sintered blank to 1140-1190 ℃ along with a furnace, carrying out solution treatment for 2-10h, and quickly cooling to room temperature after solution treatment; and finally, heating the blank again to 800-850 ℃, keeping the temperature for 8-20h, then controlling the temperature to be cooled to 400 ℃, keeping the temperature for 1h, and then cooling to room temperature by air to obtain the 2.
2. The method for preparing a 2: in the step S1, the thickness of the prepared alloy ingot ranges from 8mm to 12mm, and the thickness of the prepared quick-setting thin strip alloy sheet ranges from 0.5mm to 1mm.
3. The method of hydriding a 2-type sintered samarium cobalt permanent magnet of claim 1, comprising: in the step S2-1, the powder mixing process is performed under the protection of a high-purity nitrogen atmosphere.
4. The method for preparing a 2: in the step S2-2, the circulating hydrogen absorption temperature is 20-80 ℃, the pressure of hydrogen absorption hydrogen is 0.2MPa-1MPa, and the hydrogen absorption time is 1h-2h; the temperature of the circular hydrogen release is 20-80 ℃; the number of hydrogen absorption and desorption cycles is 1 to 3.
5. The method of hydriding a 2-type sintered samarium cobalt permanent magnet of claim 1, comprising: in the step S2-2, the hydrogen content of the alloy powder after dehydrogenation ranges from 500ppm to 2000ppm.
6. The method for preparing a 2: in the step S5, the temperature is kept for 0.5 to 1h at 400 ℃ in the sintering temperature rise process.
7. The method of hydriding a 2-type sintered samarium cobalt permanent magnet of claim 1, comprising: in the step S5, the temperature control cooling speed is 0.5-1 ℃/min.
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