CN113205936A - NdFeB/YCo5 type high-performance magnet and preparation process thereof - Google Patents

NdFeB/YCo5 type high-performance magnet and preparation process thereof Download PDF

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CN113205936A
CN113205936A CN202110439362.0A CN202110439362A CN113205936A CN 113205936 A CN113205936 A CN 113205936A CN 202110439362 A CN202110439362 A CN 202110439362A CN 113205936 A CN113205936 A CN 113205936A
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yco5
magnetic field
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CN113205936B (en
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熊吉磊
陈敏
成丽春
刘星
周宏亮
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Anhui Jihua New Material Co ltd
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    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
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    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
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    • H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
    • H01F1/047—Alloys characterised by their composition
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    • H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
    • H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
    • H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
    • H01F1/0577—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together sintered
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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 Y16.67Co83.33‑x‑y‑z‑m‑nFexCuyAgzGamZrnThe type powder and the N38 neodymium iron boron 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 for preparing a high-coercivity neodymium iron boron permanent magnet, so that the prepared neodymium iron boron permanent magnet has high coercivity with relatively good cost performance.

Description

NdFeB/YCo5 type high-performance magnet and preparation process thereof
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.
The coercivity of sintered Nd-Fe-B magnet is 1/5-1/3 which is the theoretical value of the most representative rare earth permanent magnet material at present, and various efforts have been made to obtain a magnet with high coercivity and high stability, and the most effective method is to add heavy rare earth elements such as Dy and Tb, but the heavy rare earth elements have limited resources and are expensive.
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 150Koe) of Dy2Fe14B is about 2 times higher than the magnetocrystalline anisotropy field Ha (Ha is about 70Koe) of Nd2Fe14B, and YCo5 also has higher magnetocrystalline anisotropy field Ha (Ha is about 129Koe), so that the coercive force of the neodymium iron boron magnet can be also improved greatly theoretically by adding 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 has important application value in improving the coercive force of the magnet, so that the neodymium iron boron magnet has higher anisotropy by adding YCo5 single-phase micro powder into the Nd-Fe-B material, and the low-cost high-coercive force neodymium iron boron magnet 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 above 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: YCo5 type powder 5-20%, N38 neodymium iron boron magnet 80-95%; the YCo5 type powder is prepared according to the following atomic ratio: y is16.67Co83.33-x-y-z-m-nFexCuyAgzGamZrnWherein x is 5-15, y is 3-10, z is 0.6-6, m is 0.3-2, and n is 0.15-0.6.
A process for preparing NdFeB/YCo5 type high-performance magnet comprises the following steps:
(1) preparing materials: blending YCo5 type powder according to the atomic ratio in claim 1;
(2) quick-setting casting piece: adding the raw materials in the step (1) into a vacuum strip casting furnace, vacuumizing the vacuum strip casting furnace until the vacuum degree is less than 3Pa, drying the materials, adjusting the vacuum degree to be less than 5Pa, smelting, continuously refining after the metals are completely molten until the temperature is increased to 1465 plus materials, 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 the 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 strength is 2.0T, so as to obtain a formed compact for later use;
(6) microwave sintering: placing the formed green compact 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 polishing and shape 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 the N38 neodymium iron boron magnet by 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 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, air-cooling to below 30 ℃ under the protection of argon to discharge, 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 0.15-0.25 mm.
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, and D [3, 2] ═ 0.98-1.3 μm.
Preferably, the green compact formed in the step (5) has a density of 4.4 +/-0.5 g/cm3。
Preferably, the specific process of the microwave sintering in the step (6) is that the green body is put into a sintering furnace, the temperature is raised to 500-class sand 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-class sand 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, the microwave sintering temperature in the step (8) is 860-910 ℃, the temperature is kept for 30-60min, the microwave frequency is 2.0-2.5kW, and the magnetic field intensity applied 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, and compared with the prior art, the NdFeB/YCo5 type high-performance magnet has the advantages that:
the invention prepares YCo5 type powder Y16.67Co83.33-x-y-z-m-nFexCuyAgzGamZrnAnd 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.
Description of the 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: is a data analysis chart of example 1 of the invention;
FIG. 4: is 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 analysis chart of the present invention.
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 derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
a process for preparing NdFeB/YCo5 type high-performance magnet comprises the following steps:
(1) mixing materials, wherein the YCo5 type powder is mixed according to the following atomic ratio, Y16.67Co83.33-x-y-z-m- nFexCuyAgzGamZrn，x＝5，y＝3，z＝0.6，m＝0.3，n＝0.15；
(2) Adopting a ZDL-600 vacuum melt-spun furnace produced by Aikeke 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, 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 be 50rpm when the temperature reaches 1465 ℃ and 1485 ℃, controlling the water inlet temperature to be 10-15 ℃ and starting to cast to obtain a sheet alloy, and controlling the thickness of the prepared sheet alloy to be 0.15-0.25 mm;
(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 fine powder with particle size distribution X10 ═ 0.45 μm, X50 ═ 1.12 μm, X90 ═ 2.72 μm, and 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/cm3；
(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, 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 an YCo5 type target;
(7) plating YCo5 type alloy on the commercial N38 neodymium iron boron magnet by magnetron sputtering, and controlling the content of YCo5 alloy by controlling the sputtering time to make the weight of the alloy respectively account for 5%, 10%, 15% and 20% of the total weight to obtain 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 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
Figure BDA0003034422610000061
Example 2:
a process for preparing NdFeB/YCo5 type high-performance magnet comprises the following steps:
(1) mixing materials, wherein the YCo5 type powder is mixed according to the following atomic ratio, Y16.67Co83.33-x-y-z-m- nFexCuyAgzGamZrn，x＝10，y＝6，z＝3.5，m＝0.5，n＝0.3；
(2) Adopting a ZDL-600 vacuum melt-spun furnace produced by Aikeke 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, 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 be 50rpm when the temperature reaches 1465 ℃ and 1485 ℃, controlling the water inlet temperature to be 10-15 ℃ and starting to cast to obtain a sheet alloy, and controlling the thickness of the prepared sheet alloy to be 0.15-0.25 mm;
(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 fine powder with particle size distribution X10 ═ 0.40 μm, X50 ═ 1.02 μm, X90 ═ 2.22 μm, and 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 the oxygen content of less than 10ppm for orientation forming, wherein the magnetic field orientation isPreferably adopting positive and negative pulse magnetic field for multiple orientation, wherein the magnetic field intensity is 2.0T, and the density of the formed compact is 4.4 + -0.5 g/cm3；
(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 YCo 5-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 YCo5 alloy by controlling the sputtering time to enable the weight of the alloy to respectively account for 5%, 10%, 15% and 20% of the total weight, 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 ℃, 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
Figure BDA0003034422610000081
Example 3:
a process for preparing NdFeB/YCo5 type high-performance magnet comprises the following steps:
(1) mixing materials, wherein the YCo5 type powder is mixed according to the following atomic ratio, Y16.67Co83.33-x-y-z-m- nFexCuyAgzGamZrn，x＝15，y＝10，z＝6，m＝2，n＝0.6；
(2) Adopting a ZDL-600 vacuum melt-spun furnace produced by Aikeke 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, 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 be 50rpm when the temperature reaches 1465 ℃ and 1485 ℃, controlling the water inlet temperature to be 10-15 ℃ and starting to cast to obtain a sheet alloy, and controlling the thickness of the prepared sheet alloy to be 0.15-0.25 mm;
(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 fine powder with particle size distribution X10 ═ 0.52 μm, X50 ═ 1.18 μm, X90 ═ 2.98 μm, and 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 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/cm3；
(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 YCo 5-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 YCo5 alloy by controlling the sputtering time to enable the weight of the alloy to respectively account for 5%, 10%, 15% and 20% of the total weight, 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 ℃, 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 3:
TABLE 3
Figure BDA0003034422610000101
Comparative example:
a process for preparing an NdFeB/YCo5 type magnet, the process for preparing the NdFeB/YCo5 type magnet comprising the steps of:
(1) mixing materials, wherein the YCo5 type powder is mixed according to the following atomic ratio, Y16.67Co83.33-x-y-z-m- nFexCuyAgzGamZrn，x＝0，y＝0，z＝0，m＝0，n＝0；
(2) Adopting a ZDL-600 vacuum melt-spun furnace produced by Aikeke 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 drying power to be 200KW, drying the materials for 30 minutes, 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 ℃ and 1485 ℃, and starting to cast at 10-15 ℃ to obtain a sheet alloy; the thickness of the prepared sheet alloy is controlled to be 0.15-0.25 mm;
(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 fine powder with particle size distribution X10 ═ 0.50 μm, X50 ═ 1.22 μm, X90 ═ 2.82 μm, and 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/cm3；
(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 an YCo5 type target;
(7) plating YCo5 type alloy on the commercial N38 neodymium iron boron magnet by magnetron sputtering, and controlling the content of YCo5 alloy by controlling the sputtering time to make the weight of the alloy respectively account for 5%, 10%, 15% and 20% of the total weight to obtain 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 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
Figure BDA0003034422610000111
Figure BDA0003034422610000121
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 phrase "comprising an … …" does not exclude the presence of other identical 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, but 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 (9)

1. An NdFeB/YCo5 type high-performance magnet is characterized by comprising the following raw materials in percentage by mass: YCo5 type powder 5-20%, N38 neodymium iron boron magnet 80-95%; the YCo5 type powder is prepared according to the following atomic ratio: y is16.67Co83.33-x-y-z-m-nFexCuyAgzGamZrnWherein x is 5-15, y is 3-10, z is 0.6-6, m is 0.3-2, and n is 0.15-0.6.
2. A preparation process of NdFeB/YCo5 type high-performance magnet is characterized in that: the preparation process of the NdFeB/YCo5 type high-performance magnet comprises the following steps:
(1) preparing materials: blending YCo5 type powder according to the atomic ratio in claim 1;
(2) quick-setting casting piece: adding the raw materials in the step (1) into a vacuum strip casting furnace, vacuumizing the vacuum strip casting furnace until the vacuum degree is less than 3Pa, drying the materials, adjusting the vacuum degree to be less than 5Pa, smelting, continuously refining after the metals are completely molten until the temperature is increased to 1465 plus materials, 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 the 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 strength is 2.0T, so as to obtain a formed compact for later use;
(6) microwave sintering: placing the formed green compact 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 polishing and shape 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 the N38 neodymium iron boron magnet by 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 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, air-cooling to below 30 ℃ under the protection of argon to discharge, thus obtaining the NdFeB/YCo5 type high-performance magnet.
3. The process for preparing an NdFeB/YCo5 type high performance magnet according to claim 2, 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 0.15-0.25 mm.
4. The process for preparing an NdFeB/YCo5 type high performance magnet according to claim 2, 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 ℃.
5. The process for preparing an NdFeB/YCo5 type high performance magnet according to claim 2, 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, and D [3, 2] ═ 0.98-1.3 μm.
6. The process for preparing an NdFeB/YCo5 type high performance magnet according to claim 2, wherein: the density of the green compact formed in the step (5) is 4.4 +/-0.5 g/cm3。
7. The process for preparing an NdFeB/YCo5 type high performance magnet according to claim 2, wherein: the specific process of the microwave sintering in the step (6) is that the green body is put into a sintering furnace, the temperature is raised to 500-minus-one-year-temperature 600 ℃ when the vacuum pumping is carried out to 7.0E-1Pa, the temperature is preserved for 10-30min, the microwave power is 1.0-2.0kW, the temperature is raised to 900-minus-one-year-temperature 950 ℃ after the heat preservation is finished, the temperature is preserved 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.
8. The process for preparing an NdFeB/YCo5 type high performance magnet according to claim 2, 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.
9. The process for preparing an NdFeB/YCo5 type high performance magnet according to claim 2, wherein: the conditions of the magnetic field heat treatment in the step (9) are that the temperature is raised to 500-540 ℃, the temperature is kept for 2.5-3h, and the magnetic field intensity is 2.5-3T.
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