CN113205938B - Low-cost high-performance sintered neodymium-iron-boron permanent magnet material and preparation process thereof - Google Patents

Low-cost high-performance sintered neodymium-iron-boron permanent magnet material and preparation process thereof Download PDF

Info

Publication number
CN113205938B
CN113205938B CN202110439465.7A CN202110439465A CN113205938B CN 113205938 B CN113205938 B CN 113205938B CN 202110439465 A CN202110439465 A CN 202110439465A CN 113205938 B CN113205938 B CN 113205938B
Authority
CN
China
Prior art keywords
powder
permanent magnet
temperature
magnet material
low
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202110439465.7A
Other languages
Chinese (zh)
Other versions
CN113205938A (en
Inventor
熊吉磊
陈敏
成丽春
刘星
周宏亮
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Anhui Jihua New Material Co ltd
Original Assignee
Anhui Jihua New Material Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Anhui Jihua New Material Co ltd filed Critical Anhui Jihua New Material Co ltd
Priority to CN202110439465.7A priority Critical patent/CN113205938B/en
Publication of CN113205938A publication Critical patent/CN113205938A/en
Application granted granted Critical
Publication of CN113205938B publication Critical patent/CN113205938B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032Magnets 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
    • H01F1/04Magnets 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
    • H01F1/047Alloys characterised by their composition
    • H01F1/053Alloys characterised by their composition containing rare earth metals
    • H01F1/055Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/057Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
    • H01F1/0571Alloys 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
    • H01F1/0575Alloys 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
    • H01F1/0576Alloys 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 pressed, e.g. hot working
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032Magnets 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
    • H01F1/04Magnets 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
    • H01F1/047Alloys characterised by their composition
    • H01F1/053Alloys characterised by their composition containing rare earth metals
    • H01F1/055Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/057Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
    • H01F1/0571Alloys 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
    • H01F1/0575Alloys 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
    • H01F1/0577Alloys 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
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0253Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
    • H01F41/0266Moulding; Pressing
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0253Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
    • H01F41/0273Imparting anisotropy

Landscapes

  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Hard Magnetic Materials (AREA)
  • Manufacturing Cores, Coils, And Magnets (AREA)

Abstract

The invention provides a low-cost high-performance sintered neodymium iron boron permanent magnet material and a preparation process thereof, and relates to the technical field of rare earth magnetic functional materials. The low-cost high-performance sintered neodymium iron boron permanent magnet material is mainly prepared from YCeCo5 type magnetic powder and N38 neodymium iron boron magnet powder, and the main preparation process comprises the following steps: the method comprises the steps of material preparation, rapid hardening and sheet casting, hydrogen crushing treatment, airflow grinding, mixed powder cooling, magnetic field orientation compression, microwave high-temperature sintering, magnetic field heat treatment and the like. The invention overcomes the defects of the prior art, and the neodymium iron boron magnet has higher anisotropy by adding a certain amount of single-phase micro powder of YCeCo5 into the Nd-Fe-B material, thereby obtaining the low-cost high-coercivity neodymium iron boron magnet.

Description

Low-cost high-performance sintered neodymium-iron-boron permanent magnet material and preparation process thereof
Technical Field
The invention relates to the technical field of rare earth magnetic functional materials, in particular to a low-cost high-performance sintered neodymium iron boron permanent magnet material 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 magnetic 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 coercivity of a sintered nd-fe magnet is only 1/5 to 1/3 of the theoretical value, and various efforts have been made to obtain a magnet having high coercivity and high stability, and the most effective method is to add heavy rare earth elements such as Dy and Tb. However, heavy rare earth resources are limited and 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 about 150 Koe) of Dy2Fe14B is about 2 times higher than the magnetocrystalline anisotropy field Ha (Ha about 70 Koe) of Nd2Fe14B, YCo5 also has higher magnetocrystalline anisotropy field Ha (Ha about 129 Koe), ceCo5 also has higher magnetocrystalline anisotropy field Ha (Ha about 200 Koe), and therefore, the coercive force of the neodymium iron boron magnet can be theoretically and greatly improved by adding the YCeCo5 type magnetic powder into the neodymium iron boron magnetic powder by adopting a proper process technology. And Y and Ce are rich in raw materials and low in price, and the use of YCeCo5 for improving the coercive force of the magnet has important application value.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a low-cost high-performance sintered neodymium iron boron permanent magnet material and a preparation process thereof, and a certain amount of YCeCo5 single-phase micro powder is added into an Nd-Fe-B material, so that the neodymium iron boron magnet has higher anisotropy, and the low-cost high-coercivity neodymium iron boron magnet is obtained.
In order to achieve the purpose, the technical scheme of the invention is realized by the following technical scheme:
the low-cost high-performance sintered NdFeB permanent magnet material comprises the following substances in percentage by mass: 4-16% of YCeCo5 type magnetic powder, 0.03% of lubricant, 0.12% of No. 120 aviation gasoline and the balance of N38 neodymium iron boron magnet powder reach 100%, wherein the YCeCo5 type magnetic powder is prepared according to the following atomic ratio: y is x Ce y Co z Mo m Ga n Wherein x =4.17-12.50, y =4.17-12.50, z =69.33-77.83, m =2.5-7.5, n =3-9.
The preparation process of the sintered neodymium-iron-boron permanent magnet material with low cost and high performance comprises the following steps:
(1) Preparing materials: compounding YCeCo5 type magnetic powder according to the atomic ratio;
(2) Quick-setting casting piece: placing the raw materials in the step (1) in a smelting and melt-spinning furnace, vacuumizing until the vacuum degree is less than 3Pa, drying the materials, filling argon to smelt the raw materials when the vacuum degree is less than 5Pa, continuously refining after the metals are completely melted until the temperature is increased to 1430-1450 ℃, adjusting the rotating speed of a water-cooled copper roller to 45rpm, and then controlling the water inlet temperature to 10-15 ℃ to start casting to obtain sheet alloys 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 milling: putting the HD powder brushed in the step (3) into an airflow milling machine, and performing airflow milling to obtain YCeCo5 fine powder for later use;
(5) And (3) mixed powder cooling: adding a lubricant and 120 # aviation gasoline into a mixing tank, mixing the YCeCo5 fine powder with N38 neodymium iron boron magnet powder, adding into the mixing tank, and carrying out cold treatment for 3 hours in a refrigerating chamber at about 0-5 ℃ in an argon protection environment;
(6) Magnetic field orientation profiling: placing the powder after the cold treatment into a fully-sealed magnetic field forming press with the field strength of 2.0T and the oxygen content of less than 10ppm, and performing orientation forming to obtain a formed green body for later use;
(7) Microwave high-temperature sintering: placing the green body obtained in the step (6) in a high-temperature microwave vacuum sintering furnace for high-temperature sintering, then carrying out air cooling to below 30 ℃ under the protection of argon gas, and discharging to obtain a sintered product;
(8) Magnetic field heat treatment: and (4) carrying out magnetic field heat treatment on the sintered product obtained in the step (7), then carrying out air cooling to below 30 ℃ under the protection of argon gas, and discharging to obtain the sintered neodymium iron boron permanent magnet material. In the step (2), the material drying power is 200KW, the material drying time is 30min, the smelting power is 520KW, the refining power is 500KW, the refining time is 5min, and the thickness of the sheet alloy is controlled to be 0.15-0.25mm.
Preferably, the specific process of hydrogen crushing in the step (3) is to place the sheet alloy in a reaction kettle of a rotary hydrogen explosion furnace and then carry out vacuum pumping treatment, when the vacuum degree reaches below 0.5Pa, argon is filled to normal pressure, then vacuum pumping is carried out, high-purity industrial hydrogen with the purity of 99.99% is filled, saturated hydrogen absorption is carried out, when the pressure loss of the absorbed hydrogen is less than or equal to 0.02Mpa/5min, the hydrogen absorption is finished, the temperature is ensured to be below 100 ℃ in the hydrogen absorption process, after the hydrogen absorption is finished, the furnace is closed and heated to 550 ℃, dehydrogenation is carried out until the vacuum degree reaches below 40Pa, dehydrogenation is finished, and finally, water cooling treatment is carried out, so that the temperature is reduced to be below 30 ℃.
Preferably, the oxygen content of the milling process in the step (4) is controlled to be below 5PPm, the whole jet mill is operated under the protection of nitrogen, the milling pressure is controlled to be between 0.60 and 0.62Mpa, the nitrogen inlet temperature is controlled to be between 5 and 10 ℃, the temperature of the cooling circulating water outside the milling chamber is controlled to be between 5 and 10 ℃, and fine powder with the particle size distribution of X10=0.6 and 0.7 μm, X50=1.20 and 1.30 μm, X90 =2.75 and 2.85, D [3,2] =1.2 and 1.4 μm is obtained.
Preferably, in the step (5), the YCeCo5 fine powder and the N38 NdFeB magnet powder are mixed and then screened by a 100-mesh sieve.
Preferably, the positive and negative pulse magnetic field is adopted for multiple orientations in the step (6), and the green density is 4.4-4.5g/cm 3
Preferably, the high-temperature sintering process in the step (7) is to put the green body into a sintering furnace, heat the green body to 570-600 ℃ when the vacuum is pumped to 5.0E-1Pa, preserve the temperature for 10min, finally heat the green body to 800-950 ℃ and preserve the temperature for 20-60min, wherein the microwave frequency is 1.5-4.0Kw.
Preferably, the temperature of the magnetic field heat treatment in the step (8) is 485-525 ℃, the heat preservation is 1.5-4 h, and the magnetic field intensity is 1.5-4T.
The invention provides a low-cost high-performance sintered NdFeB permanent magnet material and a preparation process thereof, and compared with the prior art, the sintered NdFeB permanent magnet material has the advantages that:
the invention relates to a method for preparing YCeCo5 type magnetic powder Y x Ce y Co z Mo m Ga n Mix N38 neodymium iron boron magnet powder, through the mixed sintering heat treatment of a plurality of steps for the magnet material who makes has better high coercivity, reduces the cost expenditure of material simultaneously, promotes the economic benefits of material.
Drawings
FIG. 1: is the XRD pattern of the powder in example 2 of the invention;
FIG. 2 is a schematic diagram: is a data analysis chart of example 1 of the present invention;
FIG. 3: is a data analysis chart of example 2 of the present invention;
FIG. 4 is a schematic view of: is a data analysis chart of example 3 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 described below clearly and completely 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
The preparation method of the sintered neodymium-iron-boron permanent magnet material with low cost and high performance comprises the following steps: the preparation process of the sintered neodymium-iron-boron permanent magnet material with low cost and high performance comprises the following steps:
(1) Preparing materials: the YCeCo5 type powder is prepared by the following atomic ratio of Y 12.50 Ce 4.17 Co 77.83 Mo 2.5 Ga 3
(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 30min, charging argon gas and increasing the power to 520KW for smelting when the vacuum degree is less than 5Pa, adjusting the power to 500KW for refining for 5min after all metal is melted, adjusting the rotating speed of a water-cooling copper roller to 45rpm when the temperature reaches 1430-1450 ℃, and starting to cast at the water inlet temperature of 10-15 ℃ to obtain a 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 550 ℃ for dehydrogenation until the vacuum degree reaches below 40Pa, finishing the 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 X10=0.6-0.7 μm, X50=1.20-1.30 μm, X90 =2.75-2.85, D2 [3,2] =1.2-1.4 μm;
(5) Mixed powder cooling treatment: adding the alloy micro powder obtained in the step (4) into commercial N38 powder according to the proportion of 4%, 8%, 12% and 16% for mixing, adding 0.03% of lubricant and 0.12% of 120 # aviation gasoline into a mixing tank before mixing, then putting the fine powder into a charging tank under the protection of argon after passing through a 100-mesh screen, and putting the charging tank into a refrigerating chamber at the temperature of about 0-5 ℃ for cooling treatment for 3 hours;
(6) Magnetic field orientation profiling: placing the fine powder in the step (5) into a fully-sealed magnetic field forming press with the oriented magnetic field intensity of 2.0T and 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 powder orientation degree is further improved, and the density of a formed green body is 4.4-4.5g/cm 3
(7) Microwave high-temperature sintering: putting the green body obtained in the step (6) into a high-temperature microwave vacuum sintering furnace with adjustable microwave power of 0.0-5.0Kw under the protection of argon gas for high-temperature sintering, wherein the specific process is that the green body is put into a sintering furnace, is heated to 570 ℃ when the vacuum is pumped to 5.0E-1Pa, is insulated for 10min, is heated to 950 ℃ at last, and is insulated for 20min, and the microwave frequency is 4.0Kw; after the heat preservation is finished, air cooling is carried out to below 30 ℃ under the protection of argon gas, and the mixture is discharged;
(8) Magnetic field heat treatment: performing magnetic field heat treatment on the product after microwave high-temperature sintering, wherein the temperature of the magnetic field heat treatment is 510 ℃, the heat preservation is performed for 1.5 h, the magnetic field intensity is 1.5T, after the heat preservation is completed, the product is air-cooled to below 30 ℃ under the protection of argon, and then the sintered neodymium iron boron permanent magnet material is obtained for detection, and the specific detection results are shown in the following table 1:
TABLE 1
Figure 256451DEST_PATH_IMAGE002
Example 2
The preparation method of the sintered neodymium-iron-boron permanent magnet material with low cost and high performance comprises the following steps: the preparation process of the sintered neodymium-iron-boron permanent magnet material with low cost and high performance comprises the following steps:
(1) Preparing materials: the YCeCo5 type powder is prepared by the following atomic ratio of Y 8.34 Ce 8.33 Co 69.33 Mo 5.0 Ga 9
(2) Adopting a ZDL-600 vacuum melt-spun furnace produced by Aifa Ke 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 30min, filling argon, increasing the power to 520KW for smelting when the vacuum degree is less than 5Pa, adjusting the power to 500KW for refining for 5min after all metal is melted, adjusting the rotating speed of a water-cooling copper roller to be 45rpm when the temperature reaches 1430-1450 ℃, and starting to cast at the water inlet temperature of 10-15 ℃ to obtain a 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 550 ℃ for dehydrogenation until the vacuum degree reaches below 40Pa, finishing the 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 X10=0.6-0.7 μm, X50=1.20-1.30 μm, X90 =2.75-2.85, D2 [ 2, 3,2] =1.2-1.4 μm;
(5) And (3) mixed powder chilling treatment: adding the alloy micro powder obtained in the step (4) into commercial N38 powder according to the proportion of 4%, 8%, 12% and 16% for mixing, adding 0.03% of lubricant and 0.12% of 120 # aviation gasoline into a mixing tank before mixing, then putting the fine powder into a charging tank under the protection of argon after passing through a 100-mesh screen, and putting the charging tank into a refrigerating chamber at the temperature of about 0-5 ℃ for cooling treatment for 3 hours;
(6) Magnetic field orientation profiling: placing the fine powder in the step (5) into a fully-sealed magnetic field forming press with the oriented magnetic field intensity of 2.0T and 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 powder orientation degree is further improved, and the density of a formed green body is 4.4-4.5g/cm 3
(7) Microwave high-temperature sintering: putting the green body obtained in the step (6) into a high-temperature microwave vacuum sintering furnace with adjustable microwave power of 0.0-5.0Kw under the protection of argon gas for high-temperature sintering, wherein the specific process is that the green body is put into the sintering furnace, is vacuumized to 5.0E-1Pa, is heated to 570 ℃, is subjected to heat preservation for 10min, is heated to 900 ℃ at last, and is subjected to heat preservation for 30min, and the microwave frequency is 3.5Kw; after the heat preservation is finished, air cooling is carried out to below 30 ℃ under the protection of argon gas, and the mixture is discharged;
(8) Magnetic field heat treatment: carrying out magnetic field heat treatment on the product subjected to microwave high-temperature sintering, wherein the temperature of the magnetic field heat treatment is 525 ℃, keeping the temperature for 3 hours, and the magnetic field intensity is 3.0T, after the heat preservation is finished, carrying out air cooling to below 30 ℃ under the protection of argon, and discharging the product to obtain a sintered neodymium iron boron permanent magnet material for detection, wherein the specific detection results are shown in the following table 2:
TABLE 2
Figure 767067DEST_PATH_IMAGE004
Example 3
The preparation method of the sintered NdFeB permanent magnet material with low cost and high performance comprises the following steps: the preparation process of the sintered neodymium-iron-boron permanent magnet material with low cost and high performance comprises the following steps:
(1) Preparing materials: the YCeCo5 type powder is prepared by the following atomic ratio of Y 4.17 Ce 12.50 Co 69.83 Mo 7.5 Ga 6
(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 30min, charging argon gas and increasing the power to 520KW for smelting when the vacuum degree is less than 5Pa, adjusting the power to 500KW for refining for 5min after all metal is melted, adjusting the rotating speed of a water-cooling copper roller to 45rpm when the temperature reaches 1430-1450 ℃, and starting to cast at the water inlet temperature of 10-15 ℃ to obtain a 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 550 ℃ for dehydrogenation until the vacuum degree reaches below 40Pa, finishing the 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 X10=0.6-0.7 μm, X50=1.20-1.30 μm, X90 =2.75-2.85, D2 [ 2, 3,2] =1.2-1.4 μm;
(5) And (3) mixed powder chilling treatment: adding the alloy micro powder obtained in the step (4) into commercial N38 powder according to the proportion of 4%, 8%, 12% and 16% for mixing, adding 0.03% of lubricant and 0.12% of 120 # aviation gasoline into a mixing tank before mixing, then putting the fine powder into a charging tank under the protection of argon after passing through a 100-mesh screen, and putting the charging tank into a refrigerating chamber at the temperature of about 0-5 ℃ for cooling treatment for 3 hours;
(6) Magnetic field orientation profiling: placing the fine powder in the step (5) into a fully-sealed magnetic field forming press with the orientation magnetic field intensity of 2.0T and 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 powder orientation degree is further improved, and the density of a formed green body is 4.4-4.5g/cm 3
(7) Microwave high-temperature sintering: putting the green body obtained in the step (6) into a high-temperature microwave vacuum sintering furnace with adjustable microwave power of 0.0-5.0Kw under the protection of argon gas for high-temperature sintering, wherein the specific process is that the green body is put into a sintering furnace, the temperature is raised to 600 ℃ when the vacuum is pumped to 5.0E-1Pa, the temperature is kept for 10min, finally the temperature is raised to 800 ℃ of sintering temperature, and the microwave frequency is 1.5Kw for 60min of heat preservation time; after the heat preservation is finished, air cooling is carried out to below 30 ℃ under the protection of argon gas, and the mixture is discharged;
(8) Magnetic field heat treatment: carrying out magnetic field heat treatment on the product after microwave high-temperature sintering, wherein the temperature of the magnetic field heat treatment is 485 ℃, the heat preservation is carried out for 4 hours, the magnetic field intensity is 4T, after the heat preservation is finished, the product is air-cooled to below 30 ℃ under the protection of argon, and then the sintered neodymium iron boron permanent magnet material is obtained for detection, and the specific detection result is shown in the following table 3:
TABLE 3
Figure DEST_PATH_IMAGE006
In conclusion, the neodymium iron boron permanent magnet material prepared by the invention has good high coercive force.
It should be noted that, in this document, relational terms such as first and second, and the like are 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, 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 (8)

1. The sintered NdFeB permanent magnet material with low cost and high performance is characterized by comprising the following substances in percentage by mass: 4-16% of YCeCo5 type magnetic powder, 0.03% of lubricant, 0.12% of No. 120 aviation gasoline and the balance of N38 neodymium iron boron magnet powder reach 100%, wherein the YCeCo5 type magnetic powder is prepared according to the following atomic ratio: y is x Ce y Co z Mo m Ga n Wherein x =4.17-12.50, y =4.17-12.50, z =69.33-77.83, m =2.5-7.5, n =3-9;
the preparation process of the sintered neodymium-iron-boron permanent magnet material with low cost and high performance comprises the following steps:
(1) Preparing materials: subjecting YCeCo5 type magnetic powder to Y treatment x Ce y Co z Mo m Ga n Atomic ratio of (2)Burdening;
(2) Quick-setting casting piece: placing the raw materials in the step (1) in a smelting and melt-spinning furnace, vacuumizing until the vacuum degree is less than 3Pa, drying the materials, filling argon to smelt the raw materials when the vacuum degree is less than 5Pa, continuously refining after the metals are completely melted until the temperature is increased to 1430-1450 ℃, adjusting the rotating speed of a water-cooled copper roller to 45rpm, and then controlling the water inlet temperature to 10-15 ℃ to start casting to obtain sheet alloys 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 milling: putting the HD powder brushed in the step (3) into an airflow milling machine, and performing airflow milling to obtain YCeCo5 fine powder for later use;
(5) And (3) mixed powder cooling: adding a lubricant and 120 # aviation gasoline into a mixing tank, mixing the YCeCo5 fine powder with N38 neodymium iron boron magnet powder, adding into the mixing tank, and carrying out cold treatment for 3 hours in a refrigerating chamber at 0-5 ℃ in an argon protection environment;
(6) Magnetic field orientation profiling: placing the powder after the cold treatment into a fully-sealed magnetic field forming press with the field strength of 2.0T and the oxygen content of less than 10ppm, and performing orientation forming to obtain a formed green body for later use;
(7) Microwave high-temperature sintering: placing the green body obtained in the step (6) in a high-temperature microwave vacuum sintering furnace for high-temperature sintering, then carrying out air cooling to below 30 ℃ under the protection of argon gas, and discharging to obtain a sintered product;
(8) Magnetic field heat treatment: and (4) carrying out magnetic field heat treatment on the sintered product obtained in the step (7), then carrying out air cooling to below 30 ℃ under the protection of argon gas, and discharging to obtain the sintered neodymium iron boron permanent magnet material.
2. The low-cost high-performance sintered NdFeB permanent magnet material as claimed in claim 1, wherein: in the step (2), the material drying power is 200KW, the material drying time is 30min, the smelting power is 520KW, the refining power is 500KW, the refining time is 5min, and the thickness of the sheet alloy is controlled to be 0.15-0.25mm.
3. The low-cost high-performance sintered NdFeB permanent magnet material as claimed in claim 1, wherein: the specific process of hydrogen crushing in the step (3) is to place the sheet alloy in a reaction kettle of a rotary hydrogen explosion furnace and then carry out vacuum pumping treatment, when the vacuum degree reaches below 0.5Pa, argon is filled to normal pressure, then high-purity industrial hydrogen with the purity of 99.99 percent is filled in the reaction kettle, the reaction kettle is vacuumized, saturated hydrogen absorption is carried out, when the pressure loss of the hydrogen absorption is less than or equal to 0.02Mpa/5min, the hydrogen absorption is finished, the temperature is ensured to be below 100 ℃ in the hydrogen absorption process, after the hydrogen absorption is finished, the furnace is closed and heated to 550 ℃, dehydrogenation is carried out until the vacuum degree reaches below 40Pa, dehydrogenation is finished, and finally, water cooling treatment is carried out, so that the temperature is reduced to be below 30 ℃.
4. The low-cost high-performance sintered NdFeB permanent magnet material as claimed in claim 1, wherein: the oxygen content of the milling process in the step (4) is controlled below 5PPm, the whole jet mill is operated under the protection of nitrogen, the milling pressure is controlled between 0.60 and 0.62MPa, the nitrogen inlet temperature is controlled between 5 and 10 ℃, the temperature of the cooling circulating water outside the milling chamber is controlled between 5 and 10 ℃, and fine powder with the particle size distribution of X10=0.6 and 0.7 μm, X50=1.20 and 1.30 μm, X90 =2.75 and 2.85, D2, 3,2 =1.2 and 1.4 μm is obtained.
5. The low-cost high-performance sintered NdFeB permanent magnet material as claimed in claim 1, wherein: and (3) mixing the YCeCo5 fine powder and the N38 NdFeB magnet powder in the step (5) and then sieving the mixture through a 100-mesh sieve.
6. The low-cost high-performance sintered NdFeB permanent magnet material as claimed in claim 1, wherein: in the step (6), positive and negative pulse magnetic fields are adopted for multiple orientations, and the density of the green body is 4.4-4.5g/cm 3
7. The low-cost high-performance sintered NdFeB permanent magnet material as claimed in claim 1, wherein: and (3) the high-temperature sintering process in the step (7) comprises the steps of putting the green body into a sintering furnace, vacuumizing to 5.0E-1Pa, heating to 570-600 ℃, preserving heat for 10min, finally heating to 800-950 ℃ of sintering temperature, preserving heat for 20-60min, and controlling the microwave frequency to be 1.5-4.0Kw.
8. The low-cost high-performance sintered NdFeB permanent magnet material as claimed in claim 1, wherein: in the step (8), the temperature of the magnetic field heat treatment is 485-525 ℃, the heat preservation is 1.5-4 h, and the magnetic field intensity is 1.5-4T.
CN202110439465.7A 2021-04-23 2021-04-23 Low-cost high-performance sintered neodymium-iron-boron permanent magnet material and preparation process thereof Active CN113205938B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202110439465.7A CN113205938B (en) 2021-04-23 2021-04-23 Low-cost high-performance sintered neodymium-iron-boron permanent magnet material and preparation process thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202110439465.7A CN113205938B (en) 2021-04-23 2021-04-23 Low-cost high-performance sintered neodymium-iron-boron permanent magnet material and preparation process thereof

Publications (2)

Publication Number Publication Date
CN113205938A CN113205938A (en) 2021-08-03
CN113205938B true CN113205938B (en) 2022-10-14

Family

ID=77028018

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202110439465.7A Active CN113205938B (en) 2021-04-23 2021-04-23 Low-cost high-performance sintered neodymium-iron-boron permanent magnet material and preparation process thereof

Country Status (1)

Country Link
CN (1) CN113205938B (en)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113724956B (en) * 2021-08-27 2023-11-24 安徽吉华新材料有限公司 Double-main-phase rare earth permanent magnet material and preparation method thereof

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6350434A (en) * 1986-08-19 1988-03-03 トライバツハ−・ケミツシエ・ベルケ・アクチエンゲゼルシヤフト Production of rare earth metal and rare earth metal-containing alloy
JP2000315607A (en) * 1999-04-28 2000-11-14 Hitachi Metals Ltd Permanent magnet and fixing structure thereof
CN101499347A (en) * 2008-11-04 2009-08-05 北京倍力隆磁材料技术有限公司 Production method for composite anisotropic rare earth permanent magnetic material with good temperature characteristics
WO2014156592A1 (en) * 2013-03-25 2014-10-02 インターメタリックス株式会社 Sintered magnet production method
WO2019038371A1 (en) * 2017-08-25 2019-02-28 Sicpa Holding Sa Assemblies and processes for producing optical effect layers comprising oriented non-spherical oblate magnetic or magnetizable pigment particles
CN111243806A (en) * 2020-01-10 2020-06-05 太原科技大学 Preparation method of high-performance sintered neodymium-iron-boron magnet
CN111378907A (en) * 2020-04-08 2020-07-07 甘肃稀土新材料股份有限公司 Auxiliary alloy for improving coercive force of neodymium iron boron permanent magnet material and application method

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6872325B2 (en) * 2002-09-09 2005-03-29 General Electric Company Polymeric resin bonded magnets
US20060054245A1 (en) * 2003-12-31 2006-03-16 Shiqiang Liu Nanocomposite permanent magnets

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6350434A (en) * 1986-08-19 1988-03-03 トライバツハ−・ケミツシエ・ベルケ・アクチエンゲゼルシヤフト Production of rare earth metal and rare earth metal-containing alloy
JP2000315607A (en) * 1999-04-28 2000-11-14 Hitachi Metals Ltd Permanent magnet and fixing structure thereof
CN101499347A (en) * 2008-11-04 2009-08-05 北京倍力隆磁材料技术有限公司 Production method for composite anisotropic rare earth permanent magnetic material with good temperature characteristics
WO2014156592A1 (en) * 2013-03-25 2014-10-02 インターメタリックス株式会社 Sintered magnet production method
WO2019038371A1 (en) * 2017-08-25 2019-02-28 Sicpa Holding Sa Assemblies and processes for producing optical effect layers comprising oriented non-spherical oblate magnetic or magnetizable pigment particles
CN111243806A (en) * 2020-01-10 2020-06-05 太原科技大学 Preparation method of high-performance sintered neodymium-iron-boron magnet
CN111378907A (en) * 2020-04-08 2020-07-07 甘肃稀土新材料股份有限公司 Auxiliary alloy for improving coercive force of neodymium iron boron permanent magnet material and application method

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
Preparation and microwave absorption properties of NdFeB alloys;XIONG Jilei 等;《JOURNAL OF RARE EARTHS》;20150531;全文 *

Also Published As

Publication number Publication date
CN113205938A (en) 2021-08-03

Similar Documents

Publication Publication Date Title
CN111430143B (en) Preparation method of rare earth neodymium iron boron permanent magnet
CN104599801A (en) Rare earth permanent magnetic material and preparation method thereof
CN104851545B (en) A kind of permanent-magnet material preparation method with grain boundary decision layer
CN111613402B (en) Process for remanufacturing high-performance permanent magnet by utilizing neodymium iron boron waste magnetic steel
TWI751788B (en) NdFeB MAGNET MATERIAL, RAW MATERIAL COMPOSITION, PREPARATION METHOD AND APPLICATION
CN113205936B (en) NdFeB/YCo5 type high-performance magnet and preparation process thereof
CN104575901A (en) Neodymium iron boron magnet added with terbium powder and preparation method thereof
CN107424701A (en) The superfine powder reuse method of sintered neodymium iron boron material
CN114864264B (en) Preparation process of low-weight rare earth high-coercivity rare earth neodymium-iron-boron permanent magnet
CN105355412A (en) Method for obtaining high-magnetism sintered NdFeB through sulfidizing
CN114724838A (en) Preparation process of waste neodymium iron boron magnetic steel regenerated new magnet
JP2022184672A (en) Neodymium-iron-boron permanent magnet and preparation method and use thereof
CN113205938B (en) Low-cost high-performance sintered neodymium-iron-boron permanent magnet material and preparation process thereof
CN114823027A (en) High-boron neodymium-iron-boron permanent magnet material and preparation method thereof
CN113948263A (en) Neodymium iron boron material and preparation method thereof
CN113205937B (en) Heavy-rare-earth-free high-performance sintered neodymium-iron-boron permanent magnet material and preparation process thereof
CN109243746A (en) Ultra-fine Grained sintered permanent magnet made of a kind of delay sintering of low temperature and preparation method thereof
CN114864263A (en) Cyclic preparation process of waste neodymium-iron-boron magnet
CN113724954B (en) High-coercivity permanent magnet without heavy rare earth and preparation process thereof
CN115881379A (en) High-remanence neodymium-iron-boron magnet and preparation method and application thereof
CN113724956B (en) Double-main-phase rare earth permanent magnet material and preparation method thereof
CN111968850B (en) Method for preparing high-coercivity neodymium-iron-boron permanent magnet material by discharge plasma sintering
CN107845467B (en) Sintered neodymium-iron-boron magnetic steel and preparation method thereof
CN111968815A (en) High-performance permanent magnet based on Bayan Obo mixed rare earth and preparation method thereof
CN115747611B (en) Auxiliary alloy cast sheet, high-remanence high-coercivity neodymium-iron-boron permanent magnet and preparation method

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant