CN113205936B - NdFeB/YCo5 type high-performance magnet and preparation process thereof - Google Patents
NdFeB/YCo5 type high-performance magnet and preparation process thereof Download PDFInfo
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Abstract
The invention provides an NdFeB/YCo5 type high-performance magnet and a preparation process thereof, relating to the technical field of rare earth magnetic functional materials. The NdFeB/YCo5 type high-performance magnet is Y 16.67 Co 83.33‑x‑y‑z‑m‑n Fe x Cu y Ag z Ga m Zr n The magnetic powder consists of type powder and an N38 NdFeB magnet, and the preparation process mainly comprises the following steps: the method comprises the steps of material preparation, rapid hardening and casting, hydrogen crushing treatment, airflow milling treatment, magnetic field forming, microwave sintering, mixed neodymium iron boron magnet preparation, magnetic field microwave sintering, magnetic field heat treatment and the like. The invention overcomes the defects of the prior art, and provides a new low-cost neodymium iron boron permanent magnet with high coercivity, so that the prepared neodymium iron boron permanent magnet has high coercivity with relatively good cost performance.
Description
Technical Field
The invention relates to the technical field of rare earth magnetic functional materials, in particular to an NdFeB/YCo5 type high-performance magnet and a preparation process thereof.
Background
Magnetic materials, especially rare earth NdFeB series permanent magnetic materials, are the best permanent magnetic materials in comprehensive performance at present, and become indispensable important material basis in modern industry and scientific technology. The sintered Nd-Fe-B permanent magnet material is rapidly industrialized due to excellent cost performance, and is widely applied to various high and new technical fields of computer hard disk drives, hard disk voice coil motors, generators, nuclear magnetic resonance instruments, sound equipment, communication equipment and the like.
As the most representative rare earth permanent magnet material at present, the coercive force of a sintered neodymium iron boron magnet is only 1/5-1/3 of the theoretical value, various efforts are tried to obtain a magnet with high coercive force and high stability, and the most effective method is to add heavy rare earth elements such as Dy and Tb, however, the heavy rare earth resources are limited and the price is high.
Therefore, how to reduce the usage amount of expensive rare earth such as Dy, tb and the like on the premise of ensuring the coercive force and improve the cost performance of products becomes one of the key development directions of enterprises in the future. The reason why the coercive force of the magnet can be remarkably improved by replacing Nd by the heavy rare earth such as Dy is that the magnetocrystalline anisotropy field Ha (Ha is about 150 Koe) of Dy2Fe14B is about 2 times higher than the magnetocrystalline anisotropy field Ha (Ha is about 70 Koe) of Nd2Fe14B, and YCo5 also has higher magnetocrystalline anisotropy field Ha (Ha is about 129 Koe), so that the coercive force of the neodymium iron boron magnet can be theoretically and greatly improved by adding the YCo5 type magnetic powder into the neodymium iron boron magnetic powder by adopting a proper process technology. And Y is rich in raw materials and low in price, and YCo5 is used for improving the coercive force of the magnet, so that the method has an important application value, and the Nd-Fe-B material is added with single-phase micro powder of YCo5, so that the Nd-Fe-B magnet has higher anisotropy, and the Nd-Fe-B magnet with high coercive force and low cost is obtained.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides an NdFeB/YCo5 type high-performance magnet and a preparation process thereof, and provides a new low-cost NdFeB permanent magnet for preparing a high-coercivity NdFeB permanent magnet, so that the prepared NdFeB magnet has high coercivity with relatively good cost performance.
In order to achieve the purpose, the technical scheme of the invention is realized by the following technical scheme:
an NdFeB/YCo5 type high-performance magnet is prepared from the following raw materials in percentage by mass: 5% -20% of YCo5 type powder and 80% -95% of N38 neodymium iron boron magnet; the YCo5 type powder is prepared from the following components in atomic ratio: y is 16.67 Co 83.33-x-y-z-m-n Fe x Cu y Ag z Ga m Zr n Wherein x =5-15, y =3-10, z =0.6-6, m =0.3-2, n =0.15-0.6.
A process for preparing NdFeB/YCo5 type high-performance magnets comprises the following steps:
(1) Preparing materials: compounding YCo5 type powder according to the atomic ratio;
(2) Rapid hardening of the cast sheet: adding the raw materials in the step (1) into a vacuum melt-spun furnace, vacuumizing the vacuum melt-spun furnace until the vacuum degree is less than 3Pa, drying the materials, then adjusting the vacuum degree to be less than 5Pa, smelting, continuing refining after the metals are completely molten until the temperature is increased to 1465-1485 ℃, adjusting the rotating speed of a water-cooling copper roller to 50rpm, and controlling the water inlet temperature to 10-15 ℃ to start casting to obtain a sheet alloy for later use;
(3) Hydrogen crushing treatment: placing the sheet alloy in a reaction kettle of a rotary hydrogen explosion furnace for treatment, then discharging under the protection of argon gas and placing in a mixing tank to obtain HD powder;
(4) Airflow grinding treatment: putting the HD powder in the step (3) into a pneumatic pulverizer, pulverizing under the protection of nitrogen, controlling the oxygen content to be below 5PPm, controlling the grinding pressure to be between 0.60 and 0.62Mpa, controlling the inlet temperature of nitrogen to be between 5 and 10 ℃, and controlling the temperature of cooling circulating water outside a grinding chamber to be between 5 and 0 ℃ to obtain YCo5 fine powder for later use;
(5) Magnetic field forming: placing the YCo5 fine powder in the step (4) into a fully-sealed magnetic field forming press with the oxygen content less than 10ppm, and carrying out orientation forming, wherein the magnetic field orientation preferably adopts a positive and negative pulse magnetic field for multiple orientations, and the magnetic field intensity is 2.0T, so as to obtain a formed compact for later use;
(6) Microwave sintering: placing the formed pressed blank in the step (5) into a microwave vacuum sintering furnace under the protection of argon gas for high-temperature sintering to obtain a target blank, and performing surface grinding and polishing and appearance processing on the formed target blank to obtain YCo5 type alloy for later use;
(7) Preparing a mixed neodymium iron boron magnet: plating YCo5 type alloy on an N38 neodymium iron boron magnet by adopting magnetron sputtering to obtain a sputtered mixed neodymium iron boron magnet;
(8) Magnetic field microwave sintering: performing high-intensity magnetic field microwave sintering treatment on the mixed neodymium iron boron magnet obtained in the step (7) to obtain a treated magnet for later use;
(9) Magnetic field heat treatment: and (3) putting the treated magnet in the step (8) into a vacuum magnetic field heat treatment furnace with the vacuum degree of less than 7.0E-1Pa for magnetic field heat treatment, and after the treatment is finished, carrying out air cooling to below 30 ℃ under the protection of argon gas to discharge the magnet out of the furnace, thus obtaining the NdFeB/YCo5 type high-performance magnet.
Preferably, in the step (2), the material drying power is 200KW, the material drying time is 30min, the smelting power is 500KW, the refining power is 540KW, the refining time is 5min, and the thickness of the prepared sheet alloy is controlled to be 0.15-0.25mm.
Preferably, the specific process of hydrogen crushing in the step (3) is that the sheet alloy is placed in a reaction kettle of a rotary hydrogen explosion furnace and then is vacuumized, argon is filled to normal pressure when the vacuum degree reaches below 0.5Pa, then high-purity industrial hydrogen with the purity of 99.99% is filled in the reaction kettle, hydrogen absorption is saturated, hydrogen absorption is finished when the pressure loss of the hydrogen absorption is less than or equal to 0.02Mpa/5min, the temperature is controlled below 100 ℃ in the hydrogen absorption process, after the hydrogen absorption is finished, the furnace is closed and heated to 600 ℃ to perform dehydrogenation until the vacuum degree reaches below 40Pa, the dehydrogenation is finished, then water cooling is performed, the temperature is reduced to below 30 ℃, and the sheet alloy is discharged into a mixing tank protected by argon gas.
Preferably, the particle size distribution range of the YCo5 fine powder in the step (4) is as follows: x10=0.40-0.52 μm, X50=1.02-1.22 μm, X90= 2.22-2.98 μm, D [3,2] =0.98-1.3 μm.
Preferably, the density of the green compact formed in the step (5) is 4.4 +/-0.5 g/cm 3 。
Preferably, the specific process of microwave sintering in the step (6) is that the green body is put into a sintering furnace, the temperature is raised to 500-600 ℃ when the vacuum pumping is carried out to 7.0E-1Pa, the temperature is kept for 10-30min, the microwave power is 1.0-2.0kW, the temperature is raised to 900-950 ℃ after the heat preservation is finished, the temperature is kept for 15-25min, the microwave power is 4.5-5.6kW, and the green body is air-cooled to below 30 ℃ under the protection of argon after the heat preservation is finished and then taken out of the furnace.
Preferably, in the step (8), the microwave sintering temperature is 860-910 ℃, the temperature is kept for 30-60min, the microwave frequency is 2.0-2.5kW, and the magnetic field intensity added in the process is 1.0-2.5T.
Preferably, the conditions of the magnetic field heat treatment in the step (9) are that the temperature is increased to 500-540 ℃, the temperature is kept for 2.5-3h, and the magnetic field intensity is 2.5-3T.
The invention provides an NdFeB/YCo5 type high-performance magnet and a preparation process thereof, compared with the prior art, the invention has the advantages that:
the invention prepares YCo5 type powder Y 16.67 Co 83.33-x-y-z-m-n Fe x Cu y Ag z Ga m Zr n And NdFeB is added and mixed to prepare the high-performance magnet material, so that the coercive force of the material is effectively improved, the use of heavy rare earth is reduced, and the economic benefit of the material is improved.
Drawings
FIG. 1: is an XRD pattern of the powder in example 2 of the invention;
FIG. 2: is the particle size distribution diagram of the powder in the embodiment 2 of the invention;
FIG. 3: a data analysis chart of example 1 of the present invention;
FIG. 4: a data analysis chart of the embodiment 2 of the invention;
FIG. 5: is a data analysis chart of the embodiment 3 of the invention;
FIG. 6: the comparative example data of the present invention is analyzed.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention are clearly and completely described below in conjunction with the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without inventive step based on the embodiments of the present invention, are within the scope of protection of the present invention.
Example 1
A process for preparing NdFeB/YCo5 type high-performance magnets comprises the following steps:
(1) Compounding material, the YCo5 type powder is compounded according to the following atomic ratio, Y 16.67 Co 83.33-x-y-z-m- n Fe x Cu y Ag z Ga m Zr n ，x=5，y=3，z=0.6，m=0.3，n=0.15；
(2) Adopting a ZDL-600 vacuum melt-spun furnace produced by Aifa vacuum equipment Limited, starting to bake materials when a smelting melt-spun furnace is pumped into an environment with the vacuum degree of less than 3Pa, setting the baking power to be 200KW, baking the materials for 30 minutes, charging argon gas and increasing the power to 500KW for smelting when the vacuum degree is less than 5Pa, adjusting the power to 540KW for refining for 5 minutes after the metal is completely melted, adjusting the rotating speed of a water-cooling copper roller to 50rpm when the temperature reaches 1465-1485 ℃, controlling the water inlet temperature to 10-15 ℃ and starting to cast to obtain a sheet alloy, wherein the thickness of the prepared sheet alloy is controlled to be 0.15-0.25mm;
(3) Loading the melt-spun piece into a reaction kettle of a rotary hydrogen explosion furnace for vacuumizing treatment, filling argon to normal pressure when the vacuum degree reaches below 0.5Pa, vacuumizing and filling high-purity industrial hydrogen (the purity is 99.99%), absorbing hydrogen in saturation, finishing hydrogen absorption when the pressure loss of the hydrogen absorption is less than or equal to 0.02Mpa/5min, using water cooling and using an infrared thermometer to measure the temperature in the hydrogen absorption process to ensure that the temperature in the hydrogen absorption process is controlled below 100 ℃, closing the furnace after the hydrogen absorption is finished, heating to 600 ℃, performing dehydrogenation until the vacuum degree reaches below 40Pa, finishing dehydrogenation, finally performing water cooling treatment, reducing the temperature to below 30 ℃, discharging the product into a mixing tank protected by argon gas, and obtaining HD powder;
(4) Adopting QLMR-400G type airflow milling equipment, putting the HD powder mixed in the step (3) into an airflow milling machine, controlling the oxygen content in the milling process to be below 5PPm, operating the whole airflow milling machine under the protection of nitrogen, controlling the milling pressure to be between 0.60 and 0.62Mpa, controlling the inlet temperature of nitrogen to be between 5 and 10 ℃, and controlling the temperature of cooling circulating water outside a milling chamber to be between 5 and 10 ℃; obtaining a fine powder having a particle size distribution in the range of X10=0.45 μm, X50=1.12 μm, X90= 2.72 μm, D [3,2] =1.15 μm;
(5) Magnetic field forming: placing the fine powder obtained in the step (4) into a fully-sealed magnetic field forming press with oxygen content less than 10ppm, and performing orientation forming, wherein the magnetic field orientation preferably adopts a positive and negative pulse magnetic field for multiple orientations, the magnetic field intensity is 2.0T, and the density of the formed pressed compact is 4.4 +/-0.5 g/cm 3 ；
(6) Microwave sintering: putting the green body obtained in the step (5) into a microwave vacuum sintering furnace under the protection of argon gas for high-temperature sintering, wherein the specific process comprises the steps of putting the green body into the sintering furnace, vacuumizing to 7.0E-1Pa, heating to 600 ℃, preserving heat for 20min, keeping the microwave power at 1.5kW, heating to 910 ℃ after heat preservation is finished, preserving heat for 20min, keeping the microwave power at 5.5kW, carrying out air cooling to below 30 ℃ under the protection of argon gas after heat preservation is finished, discharging to obtain a target blank, and carrying out surface grinding and polishing and appearance processing on the formed target blank to obtain a YCo5 type target;
(7) Plating YCo5 type alloy on the commercial N38 neodymium-iron-boron magnet by adopting magnetron sputtering, and controlling the content of the YCo5 alloy by controlling the sputtering time to make the weight of the YCo5 type alloy respectively account for 5%, 10%, 15% and 20% of the total weight to obtain a sputtered mixed neodymium-iron-boron magnet;
(8) Magnetic field microwave sintering: performing high-intensity magnetic field microwave sintering on the product obtained in the step (7), wherein the microwave sintering temperature is 910 ℃, the temperature is kept for 30min, the microwave frequency is 2.5kW, and the intensity of the magnetic field applied in the process is 2.0T;
(9) Magnetic field heat treatment: and (3) putting the product obtained in the step (8) into a vacuum magnetic field heat treatment furnace with the vacuum degree of less than 7.0E-1Pa for magnetic field heat treatment, heating to 520 ℃, keeping the temperature for 3 hours, keeping the magnetic field intensity at 3.0T, carrying out air cooling to below 30 ℃ under the protection of argon after the heat preservation is finished, discharging, and testing the product performance, wherein the specific results are shown in the following table 1:
TABLE 1
Example 2
A process for preparing NdFeB/YCo5 type high-performance magnets comprises the following steps:
(1) Compounding material, the YCo5 type powder is compounded according to the following atomic ratio, Y 16.67 Co 83.33-x-y-z-m- n Fe x Cu y Ag z Ga m Zr n ，x=10， y=6，z=3.5， m=0.5，n=0.3；
(2) Adopting a ZDL-600 vacuum melt-spun furnace produced by AIFACH vacuum equipment Limited company, starting to dry materials when a smelting melt-spun furnace is pumped into an environment with the vacuum degree of less than 3Pa, setting the power of the dried materials to be 200KW, drying the materials for 30 minutes, filling argon, increasing the power to 500KW for smelting when the vacuum degree is less than 5Pa, adjusting the power to 540KW for refining for 5 minutes after all metals are molten, adjusting the rotating speed of a water-cooling copper roller to be 50rpm when the temperature reaches 1465-1485 ℃, controlling the water inlet temperature to be 10-15 ℃ and starting to cast to obtain a sheet alloy, wherein the thickness of the prepared sheet alloy is controlled to be 0.15-0.25mm;
(3) Loading the melt-spun sheet into a reaction kettle of a rotary hydrogen explosion furnace for vacuumizing treatment, filling argon to normal pressure when the vacuum degree reaches below 0.5Pa, then vacuumizing and filling high-purity industrial hydrogen (purity 99.99%), saturated hydrogen absorption, finishing hydrogen absorption when the pressure loss of the hydrogen absorption is less than or equal to 0.02Mpa/5min, using water cooling and using an infrared thermometer to measure the temperature in the hydrogen absorption process to ensure that the temperature is controlled below 100 ℃, closing the furnace after the hydrogen absorption is finished, heating to 600 ℃, performing dehydrogenation until the vacuum degree reaches below 40Pa, finishing the dehydrogenation, finally performing water cooling treatment, reducing the temperature to below 30 ℃, discharging the mixture to a mixing tank protected by argon, and obtaining HD powder;
(4) Adopting QLMR-400G type airflow milling equipment, putting the HD powder mixed in the step (3) into an airflow milling machine, controlling the oxygen content in the milling process to be below 5PPm, operating the whole airflow milling machine under the protection of nitrogen, controlling the milling pressure to be between 0.60 and 0.62Mpa, controlling the inlet temperature of nitrogen to be between 5 and 10 ℃, and controlling the temperature of cooling circulating water outside a milling chamber to be between 5 and 10 ℃; obtaining a fine powder having a particle size distribution in the range of X10=0.40 μm, X50=1.02 μm, X90= 2.22 μm, D [3,2] =0.98 μm;
(5) Magnetic field forming: placing the fine powder obtained in the step (4) into a fully-sealed magnetic field forming press with oxygen content less than 10ppm, and performing orientation forming, wherein the magnetic field orientation preferably adopts a positive and negative pulse magnetic field for multiple orientations, the magnetic field intensity is 2.0T, and the density of the formed pressed compact is 4.4 +/-0.5 g/cm 3 ；
(6) Microwave sintering: putting the green body obtained in the step (5) into a microwave vacuum sintering furnace under the protection of argon gas for high-temperature sintering, wherein the specific process comprises the steps of putting the green body into the sintering furnace, vacuumizing to 7.0E-1Pa, heating to 500 ℃, preserving heat for 10min, controlling the microwave power to be 2.0kW, heating to 950 ℃ after finishing preserving heat, preserving heat for 15min, controlling the microwave power to be 5.6kW, carrying out air cooling to below 30 ℃ under the protection of argon gas after finishing preserving heat, discharging to obtain a target blank, and carrying out surface grinding and polishing and appearance processing on the formed target blank to obtain a YCo5 type target;
(7) Plating YCo5 type alloy on the commercial N38 neodymium-iron-boron magnet by adopting a magnetron sputtering method, and controlling the content of the YCo5 alloy by controlling the sputtering time to make the weight of the YCo5 type alloy respectively account for 5%, 10%, 15% and 20% of the total weight to obtain a sputtered mixed neodymium-iron-boron magnet;
(8) Magnetic field microwave sintering: performing high-intensity magnetic field microwave sintering on the product obtained in the step (7), wherein the microwave sintering temperature is 890 ℃, the temperature is kept for 60min, the microwave frequency is 2.2kW, and the intensity of the magnetic field applied in the process is 2.5T;
(9) Magnetic field heat treatment: and (3) putting the product obtained in the step (8) into a vacuum magnetic field heat treatment furnace with the vacuum degree of less than 7.0E-1Pa for magnetic field heat treatment, heating to 500 ℃, preserving heat for 3 hours, keeping the magnetic field intensity for 3T, carrying out air cooling to below 30 ℃ under the protection of argon after heat preservation, discharging, and testing the product performance, wherein the specific results are shown in the following table 2:
TABLE 2
Example 3
A process for preparing NdFeB/YCo5 type high-performance magnets comprises the following steps:
(1) Compounding material, the YCo5 type powder is compounded according to the following atomic ratio, Y 16.67 Co 83.33-x-y-z-m- n Fe x Cu y Ag z Ga m Zr n ，x=15，y=10，z=6，m=2，n=0.6；
(2) Adopting a ZDL-600 vacuum melt-spun furnace produced by Aifa vacuum equipment Limited, starting to bake materials when a smelting melt-spun furnace is pumped into an environment with the vacuum degree of less than 3Pa, setting the baking power to be 200KW, baking the materials for 30 minutes, charging argon gas and increasing the power to 500KW for smelting when the vacuum degree is less than 5Pa, adjusting the power to 540KW for refining for 5 minutes after the metal is completely melted, adjusting the rotating speed of a water-cooling copper roller to 50rpm when the temperature reaches 1465-1485 ℃, controlling the water inlet temperature to 10-15 ℃ and starting to cast to obtain a sheet alloy, wherein the thickness of the prepared sheet alloy is controlled to be 0.15-0.25mm;
(3) Loading the melt-spun piece into a reaction kettle of a rotary hydrogen explosion furnace for vacuumizing treatment, filling argon to normal pressure when the vacuum degree reaches below 0.5Pa, vacuumizing and filling high-purity industrial hydrogen (the purity is 99.99%), absorbing hydrogen in saturation, finishing hydrogen absorption when the pressure loss of the hydrogen absorption is less than or equal to 0.02Mpa/5min, using water cooling and using an infrared thermometer to measure the temperature in the hydrogen absorption process to ensure that the temperature in the hydrogen absorption process is controlled below 100 ℃, closing the furnace after the hydrogen absorption is finished, heating to 600 ℃, performing dehydrogenation until the vacuum degree reaches below 40Pa, finishing dehydrogenation, finally performing water cooling treatment, reducing the temperature to below 30 ℃, discharging the product into a mixing tank protected by argon gas, and obtaining HD powder;
(4) Adopting QLMR-400G type airflow milling equipment, putting the HD powder mixed in the step (3) into an airflow milling machine, controlling the oxygen content in the milling process to be below 5PPm, operating the whole airflow milling machine under the protection of nitrogen, controlling the milling pressure to be between 0.60 and 0.62Mpa, controlling the inlet temperature of nitrogen to be between 5 and 10 ℃, and controlling the temperature of cooling circulating water outside a milling chamber to be between 5 and 10 ℃; obtaining a fine powder having a particle size distribution in the range of X10=0.52 μm, X50=1.18 μm, X90=2.98 μm, D [3,2] =1.3 μm;
(5) Magnetic field forming: placing the fine powder obtained in the step (4) into a fully-sealed magnetic field forming press with the oxygen content of less than 10ppm for orientation forming, wherein the magnetic field orientation preferably adopts a positive and negative pulse magnetic field for multiple orientations, the magnetic field intensity is 2.0T, and the density of a formed pressed compact is 4.4 +/-0.5 g/cm 3 ；
(6) Microwave sintering: placing the green body obtained in the step (5) into a microwave vacuum sintering furnace under the protection of argon gas for high-temperature sintering, wherein the specific process comprises the steps of placing the green body into the sintering furnace, vacuumizing to 7.0E-1Pa, heating to 500 ℃, keeping the temperature for 10min, keeping the microwave power at 2.0kW, heating to 950 ℃ after the heat preservation is finished, keeping the temperature for 15min, keeping the microwave power at 5.6kW, carrying out air cooling to below 30 ℃ under the protection of argon gas after the heat preservation is finished, discharging to obtain a target blank, and carrying out surface grinding polishing and appearance processing on the formed target blank to obtain a YCo5 type target;
(7) Plating YCo5 type alloy on the commercial N38 neodymium iron boron magnet by adopting a magnetron sputtering method, controlling the content of the YCo5 alloy by controlling the sputtering time to ensure that the weight of the YCo5 type alloy accounts for 5 percent, 10 percent, 15 percent and 20 percent of the total weight respectively, and obtaining the sputtered mixed neodymium iron boron magnet;
(8) Magnetic field microwave sintering: performing high-intensity magnetic field microwave sintering on the product obtained in the step (7), wherein the microwave sintering temperature is 890 ℃, the temperature is kept for 60min, the microwave frequency is 2.2kW, and the intensity of the magnetic field applied in the process is 2.5T;
(9) Magnetic field heat treatment: and (3) putting the product obtained in the step (8) into a vacuum magnetic field heat treatment furnace with the vacuum degree of less than 7.0E-1Pa for magnetic field heat treatment, heating to 500 ℃, keeping the temperature for 3 hours, keeping the magnetic field intensity for 3T, carrying out air cooling under the protection of argon to below 30 ℃ after heat preservation, discharging, and testing the product performance, wherein the specific results are shown in the following table 3:
TABLE 3
Comparative example
The preparation process of the NdFeB/YCo5 type magnet comprises the following steps:
(1) Compounding material, the YCo5 type powder is compounded according to the following atomic ratio, Y 16.67 Co 83.33-x-y-z-m- n Fe x Cu y Ag z Ga m Zr n ，x=0，y=0，z=0，m=0，n=0；
(2) Adopting a ZDL-600 vacuum melt-spun furnace produced by Aifa vacuum equipment Limited, starting to dry materials when a smelting melt-spun furnace is pumped into an environment with the vacuum degree of less than 3Pa, setting the power of the dried materials to be 200KW, drying the materials for 30 minutes, charging argon gas and increasing the power to 500KW for smelting when the vacuum degree is less than 5Pa, adjusting the power to 540KW for refining for 5 minutes after the metal is completely molten, adjusting the rotating speed of a water-cooling copper roller to 50rpm when the temperature reaches 1465-1485 ℃, and controlling the water inlet temperature to 10-15 ℃ to start casting to obtain the sheet alloy; the thickness of the prepared sheet alloy is controlled to be 0.15-0.25mm;
(3) Loading the melt-spun piece into a reaction kettle of a rotary hydrogen explosion furnace for vacuumizing treatment, filling argon to normal pressure when the vacuum degree reaches below 0.5Pa, vacuumizing and filling high-purity industrial hydrogen (the purity is 99.99%), absorbing hydrogen in a saturated mode, finishing hydrogen absorption when the pressure loss of the absorbed hydrogen is less than or equal to 0.02Mpa/5min, using water cooling and using an infrared thermometer to measure the temperature in the hydrogen absorption process to ensure that the temperature in the hydrogen absorption process is controlled below 100 ℃, closing the furnace after the hydrogen absorption is finished, heating to 600 ℃, performing dehydrogenation until the vacuum degree reaches below 40Pa, finishing dehydrogenation, finally performing water cooling treatment, reducing the temperature to below 30 ℃, discharging the product into a argon-protected material mixing tank to obtain HD powder;
(4) Adopting QLMR-400G type airflow milling equipment, putting the HD powder mixed in the step (3) into an airflow milling machine, controlling the oxygen content in the milling process to be below 5PPm, operating the whole airflow milling machine under the protection of nitrogen, controlling the milling pressure to be between 0.60 and 0.62Mpa, controlling the inlet temperature of nitrogen to be between 5 and 10 ℃, and controlling the temperature of cooling circulating water outside a milling chamber to be between 5 and 10 ℃; obtaining a fine powder having a particle size distribution in the range of X10=0.50 μm, X50=1.22 μm, X90= 2.82 μm, D [3,2] =1.2 μm;
(5) Magnetic field forming: placing the fine powder obtained in the step (4) into a fully-sealed magnetic field forming press with oxygen content less than 10ppm, and performing orientation forming, wherein the magnetic field orientation preferably adopts a positive and negative pulse magnetic field for multiple orientations, the magnetic field intensity is 2.0T, and the density of the formed pressed compact is 4.4 +/-0.5 g/cm 3 ；
(6) Microwave sintering: putting the green body obtained in the step (5) into a microwave vacuum sintering furnace under the protection of argon gas for high-temperature sintering, wherein the specific process comprises the steps of putting the green body into the sintering furnace, vacuumizing to 7.0E-1Pa, heating to 500 ℃, keeping the temperature for 30min, keeping the microwave power at 1.0kW, heating to 900 ℃ after the heat preservation is finished, keeping the temperature for 25min, keeping the microwave power at 4.5kW, carrying out air cooling to below 30 ℃ under the protection of argon gas after the heat preservation is finished, discharging to obtain a target blank, and carrying out surface grinding and polishing and appearance processing on the formed target blank to obtain a YCo5 type target;
(7) Plating YCo5 type alloy on the commercial N38 neodymium-iron-boron magnet by adopting magnetron sputtering, and controlling the content of the YCo5 alloy by controlling the sputtering time to make the weight of the YCo5 type alloy respectively account for 5%, 10%, 15% and 20% of the total weight to obtain a sputtered mixed neodymium-iron-boron magnet;
(8) Magnetic field microwave sintering: performing high-intensity magnetic field microwave sintering on the product obtained in the step (7), wherein the microwave sintering temperature is 860 ℃, the temperature is kept for 30min, the microwave frequency is 2.0kW, and the intensity of the magnetic field applied in the process is 1.0T;
(9) Magnetic field heat treatment: and (3) putting the product obtained in the step (8) into a vacuum magnetic field heat treatment furnace with the vacuum degree of less than 7.0E-1Pa for magnetic field heat treatment, heating to 540 ℃, preserving heat for 2.5 hours, keeping the magnetic field intensity at 2.5T, carrying out air cooling to below 30 ℃ under the protection of argon after heat preservation, discharging, and testing the product performance, wherein the results are shown in the following table 4:
TABLE 4
In conclusion, the magnet materials prepared in examples 1 to 3 of the present invention have more excellent intrinsic coercive force.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrases "comprising one of 8230; \8230;" 8230; "does not exclude the presence of additional like elements in a process, method, article, or apparatus that comprises the element.
The above examples are only intended to illustrate the technical solution of the present invention, and not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (8)
1. An NdFeB/YCo5 type high-performance magnet is characterized by comprising the following raw materials in percentage by mass: 5-20% of YCo5 type powder and 80-95% of N38 NdFeB magnet; the YCo5 type powder is prepared from the following components in atomic ratio: y is 16.67 Co 83.33-x-y-z-m-n Fe x Cu y Ag z Ga m Zr n Wherein x =5-15, y =3-10, z =0.6-6, m =0.3-2, n =0.15-0.6;
the preparation process of the NdFeB/YCo5 type high-performance magnet comprises the following steps of:
(1) Preparing materials: mixing YCo5 type powder with above Y 16.67 Co 83.33-x-y-z-m-n Fe x Cu y Ag z Ga m Zr n The materials are mixed according to the atomic ratio;
(2) Quick-setting casting piece: adding the raw materials in the step (1) into a vacuum melt-spun furnace, vacuumizing the vacuum melt-spun furnace until the vacuum degree is less than 3Pa, drying the materials, then adjusting the vacuum degree to be less than 5Pa, smelting, continuing refining after the metals are completely molten until the temperature is increased to 1465-1485 ℃, adjusting the rotating speed of a water-cooling copper roller to 50rpm, and controlling the water inlet temperature to 10-15 ℃ to start casting to obtain a sheet alloy for later use;
(3) Hydrogen crushing treatment: placing the sheet alloy in a reaction kettle of a rotary hydrogen explosion furnace for treatment, then discharging under the protection of argon gas and placing in a mixing tank to obtain HD powder;
(4) And (3) airflow grinding treatment: putting the HD powder in the step (3) into a pneumatic pulverizer, pulverizing under the protection of nitrogen, controlling the oxygen content to be below 5PPm, controlling the grinding pressure to be between 0.60 and 0.62Mpa, controlling the inlet temperature of nitrogen to be between 5 and 10 ℃, and controlling the temperature of cooling circulating water outside a grinding chamber to be between 5 and 0 ℃ to obtain YCo5 fine powder for later use;
(5) Magnetic field forming: placing the YCo5 fine powder in the step (4) into a fully-sealed magnetic field forming press with the oxygen content less than 10ppm, and carrying out orientation forming, wherein the magnetic field orientation adopts a positive and negative pulse magnetic field for multiple orientations, and the magnetic field intensity is 2.0T, so as to obtain a formed compact for later use;
(6) Microwave sintering: placing the formed pressed blank in the step (5) into a microwave vacuum sintering furnace under the protection of argon gas for high-temperature sintering to obtain a target blank, and performing surface grinding and polishing and appearance processing on the formed target blank to obtain YCo5 type alloy for later use;
(7) Preparing a mixed neodymium iron boron magnet: plating YCo5 type alloy on an N38 neodymium iron boron magnet by adopting magnetron sputtering to obtain a sputtered mixed neodymium iron boron magnet;
(8) Magnetic field microwave sintering: performing high-intensity magnetic field microwave sintering treatment on the mixed neodymium iron boron magnet obtained in the step (7) to obtain a treated magnet for later use;
(9) Magnetic field heat treatment: and (5) putting the processed magnet in the step (8) into a vacuum magnetic field heat treatment furnace with the vacuum degree of less than 7.0E-1Pa for magnetic field heat treatment, and after the treatment is finished, carrying out air cooling to below 30 ℃ under the protection of argon to discharge the magnet, thus obtaining the NdFeB/YCo5 type high-performance magnet.
2. An NdFeB/YCo5 type high performance magnet according to claim 1, wherein: in the step (2), the material drying power is 200KW, the material drying time is 30min, the smelting power is 500KW, the refining power is 540KW, the refining time is 5min, and the thickness of the prepared sheet alloy is controlled to be 0.15-0.25mm.
3. An NdFeB/YCo5 type high performance magnet according to claim 1, wherein: and (3) putting the sheet alloy in a reaction kettle of a rotary hydrogen explosion furnace, vacuumizing, filling argon to normal pressure when the vacuum degree reaches below 0.5Pa, vacuumizing, filling high-purity industrial hydrogen with the purity of 99.99 percent, absorbing hydrogen in saturation, finishing hydrogen absorption when the pressure loss of the absorbed hydrogen is less than or equal to 0.02Mpa/5min, controlling the temperature below 100 ℃ in the hydrogen absorption process, heating the furnace to 600 ℃ after the hydrogen absorption is finished, dehydrogenating until the vacuum degree reaches below 40Pa, finishing the dehydrogenation, cooling with water, and discharging the alloy to a mixing tank protected by argon when the temperature is reduced below 30 ℃.
4. An NdFeB/YCo5 type high performance magnet according to claim 1, wherein: the particle size distribution range of the YCo5 fine powder in the step (4) is as follows: x10=0.40-0.52 μm, X50=1.02-1.22 μm, X90= 2.22-2.98 μm, D [3,2] =0.98-1.3 μm.
5. An NdFeB/YCo5 type high performance magnet according to claim 1, wherein: the density of the green compact formed in the step (5) is 4.4 +/-0.5 g/cm 3 。
6. An NdFeB/YCo5 type high performance magnet according to claim 1, wherein: and (6) putting the green body into a sintering furnace, vacuumizing to 7.0E-1Pa, heating to 500-600 ℃, preserving heat for 10-30min, wherein the microwave power is 1.0-2.0kW, heating to 900-950 ℃, preserving heat for 15-25min, the microwave power is 4.5-5.6kW, and air cooling to below 30 ℃ under the protection of argon after heat preservation.
7. An NdFeB/YCo5 type high performance magnet according to claim 1, wherein: in the step (8), the microwave sintering temperature is 860-910 ℃, the temperature is kept for 30-60min, the microwave frequency is 2.0-2.5kW, and the magnetic field intensity added in the process is 1.0-2.5T.
8. An NdFeB/YCo5 type high performance magnet according to claim 1, wherein: the magnetic field heat treatment in the step (9) is carried out under the conditions of heating to 500-540 ℃, heat preservation for 2.5-3h and magnetic field intensity of 2.5-3T.
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