CN108831648A - The method of spray drying preparation performance Nd Fe B sintered magnet - Google Patents

The method of spray drying preparation performance Nd Fe B sintered magnet Download PDF

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Publication number
CN108831648A
CN108831648A CN201810643365.4A CN201810643365A CN108831648A CN 108831648 A CN108831648 A CN 108831648A CN 201810643365 A CN201810643365 A CN 201810643365A CN 108831648 A CN108831648 A CN 108831648A
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powder
spray drying
alloys
rare earth
heavy rare
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贺琦军
林建强
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NINGBO ZHAOBAO MAGNET Co Ltd
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NINGBO ZHAOBAO MAGNET Co Ltd
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    • 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

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  • 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)

Abstract

The invention discloses a kind of methods of spray drying preparation performance Nd Fe B sintered magnet, include the following steps:1) nearly just dividing than 2:14:Nd Fe B alloys rapid-hardening flake is made using strip casting in 1 Nd Fe B alloys raw material;2) above-mentioned alloy rapid-hardening flake is subjected to powder processed, obtains Nd Fe B alloys powder;3) by Nd Fe B alloys powder and heavy rare earth metal powder or heavy rare earth compound powder according to mass ratio (100~150):1 is dissolved in 25~35min of ultrasonic disperse in a certain amount of ether, obtains slurries;4) dry composite powder is made by spray drying in above-mentioned slurries;5) above-mentioned composite powder is subjected to magnetic field orientating molding, waits static pressure, Nd-Fe-B permanent magnet is made in vacuum-sintering and tempering heat treatment.Gained magnet coercivity of the invention greatly improves, and remanent magnetism and magnetic energy product reduction are unobvious, and simultaneous spray drying carries out in closed container, and raw material producing level is high, and required heavy rare earth raw material is few, significant effect.

Description

The method of spray drying preparation performance Nd Fe B sintered magnet
Technical field
The present invention relates to technical field of magnetic materials, prepare high performance sintered neodymium more specifically, it relates to be spray-dried The method of iron boron magnet.
Background technique
True benevolence in assistant river of nineteen eighty-three Japan et al. uses on the basis of study extensively to RE-Fe-X ternary alloy three-partalloy Powder metallurgical technique prepares magnetic energy product and is up to 290kJ/m3Neodymium iron boron (Nd-Fe-B) sintered magnet, it is dilute to have started the third generation Native permanent-magnet material.Sintered NdFeB magnet since the invention, is obtained with its excellent comprehensive performance and the price of relative moderate It is widely applied.In recent years, with the accelerated development of science and technology, Sintered NdFeB magnet is in new-energy automobile, frequency-changeable compressor and wind The promotion rate and application range of the high-end fields such as power power generation expand rapidly.These fields, which are required to Sintered NdFeB magnet, to be had Higher comprehensive magnetic energy has high remanent magnetism and high coercivity.
Sintered NdFeB magnet is with Nd2Fe14B compound is main phase, is around coated with the structure of Nd-rich phase.It is main Technical indicator include remanent magnetism Br, maximum magnetic energy product (BH) max, coercivity H j, Curie temperature Tc.By 20 years of researches Development has devised reasonable alloying component and mature preparation process, the remanent magnetism Br of magnet is made to have reached the 96% of theoretical value More than, magnetic energy product can reach 474kJ/m3, approached theoretical magnetic energy product 512kJ/m393%.Although coercivity obtains The promotion of certain depth, but for its theoretical value 5600kA/m, still have very big gap, can achieve at present Level is probably the 1/10~1/3 of its coercivity theoretical value.Neodymium iron boron magnetic body is thus greatly limited in high work temperature It is applied under degree environment.
In order to solve this problem, scientific worker has been engaged in a large amount of research, studies have shown that seeping in neodymium iron boron magnetic body The coercivity of magnet can be improved by entering Dy or Tb, and existing technological means mainly includes heavy rare earth alloy or Nd displacement Dy/Tb oxygen Compound/fluoride, but these technologies all there is a problem of it is more or less, as the former is due to the anti-magnetic of heavy rare earth atom and iron atom Property coupling, the indexs such as the remanent magnetism of magnet and maximum magnetic energy product will be greatly reduced, the Nd and Dy or Tb at the latter's main phase grain edge Oxide or fluoride directly replace, replacing velocity is very slow, thus make seep Dy, seep Tb efficiency it is very low, the production time It is long.And dysprosium used in the above method/terbium dosage is big, it is at high cost.
Summary of the invention
The object of the present invention is to provide a kind of methods of spray drying preparation performance Nd Fe B sintered magnet, by spraying Nd Fe B alloys are made in drying process and powder containing heavy rare earth element is uniformly dispersed and is adsorbed on Nd Fe B alloys powder particle table Performance Nd Fe B sintered magnet is made by sintering densification in the mixed powder in face, embodies heavy rare earth element and improves magnet magnetism The best use of energy.
To achieve the above object, it is realized by following technological means:A kind of spray drying prepares high performance sintered neodymium-iron-boron The method of magnet, includes the following steps:
1) nearly just dividing than 2:14:Nd Fe B alloys rapid-hardening flake is made using strip casting in 1 Nd Fe B alloys raw material;
2) above-mentioned alloy rapid-hardening flake is subjected to powder processed, obtains Nd Fe B alloys powder;First alloy cast ingot is carried out rough and torn It is broken, the antioxidant of 0.02wt%-0.70wt% is added, then air-flow is milled into the Nd Fe B alloys that average grain diameter is 3~5 μm Powder.Wherein antioxidant is sodium sulfite, sodium pyrosulfite, dibutylphenol, sodium hydrogensulfite, sodium thiosulfate, tertiary fourth One of base p-hydroxyanisole.
3) by Nd Fe B alloys powder and heavy rare earth metal powder or heavy rare earth compound powder according to mass ratio (100~ 150):1 is dissolved in 25~35min of ultrasonic disperse in a certain amount of ether, obtains slurries;The heavy rare earth metal powder or again The granularity of rare earth compound powder is less than or equal to 10 microns, the heavy rare earth metal be dysprosium, in three kinds of elements of terbium and holmium extremely Few one kind, the heavy rare earth compound are the heavy rare earth compound containing at least one of dysprosium, three kinds of elements of terbium and holmium.
4) dry composite powder is made by spray drying in above-mentioned slurries;
5) above-mentioned composite powder is subjected to magnetic field orientating molding, waits static pressure, neodymium iron is made in vacuum-sintering and tempering heat treatment Boron permanent magnet.The magnetic field orientating molding, 1.6~2T of magnetic field;The described equal static pressure, pressure is 200~300MPa;Described is true Sky sintering, sintering temperature are 1040~1080 DEG C, and vacuum degree is at least 1 × 10-2Pa, sintering time are 2~4 hours;Described time Burning hot processing is 2 grades of tempering, and level-one is tempered 850~900 DEG C, and 450~550 DEG C of second annealing, the time is 2~4 hours.
The beneficial effects of the present invention are:The Nd Fe B alloys rapid-hardening flake of phase is prepared into through strip casting, by coarse crushing With tiny Nd Fe B alloys particle is obtained after airflow milling, it is then mixed with heavy rare earth metal powder or heavy rare earth compound powder Close that spray drying obtains heavy rare earth metal powder or heavy rare earth compound powder is dispersed in mixing between Nd Fe B alloys particle Powder structure, mixed powder structure remain heavy rare earth metal powder or heavy rare earth compound powder more in the subsequent sintering process It is dispersed in the intracorporal structure of magnet block, forms rich rare earth Grain-Boundary Phase, to improve the coercivity of magnet, that is, improves the magnetism of magnet Energy.
The advantages of the present invention over the prior art are that:1) spray drying using high pressure by solvent or diluent after being atomized, with In the contact of hot-air, ether rapid vaporization, powder disperses rapidly in the sky, and degree of scatter is high, and high production efficiency obtains composite powder Body is uniformly mixed, and disperse phase is evenly distributed in magnet;2) spray drying carries out in closed container, and raw material producing level is high, institute Need heavy rare earth raw material few, significant effect;3) gained magnet coercivity greatly improves, and remanent magnetism and magnetic energy product reduction are unobvious.
Specific embodiment
Invention is described in further detail below by specific embodiment, it is not to limit that following embodiment, which is descriptive, Protection scope of the present invention of property.
Embodiment 1
A method of spray drying preparation performance Nd Fe B sintered magnet includes the following steps:
1) design is based on 2:14:The Nd Fe B alloys ingredient Nd11.76Fe82.36B5.88 (atomic percentage) of 1 phase, is pressed According to the ingredient composition of design, the raw metal that purity is 99.9wt% is put into rapid hardening furnace and gets rid of band and is made with a thickness of 0.25mm's Nd Fe B alloys thin slice;
2) then rapid hardening thin slice is put into hydrogen broken furnace, leads to hydrogen stream 70ml/min, reacted 4 hours, hydrogen is broken to obtain 60 mesh Powder particle;Then the antioxidant of 0.05wt% is added, is transferred to and grinds 2 hours Nd Fe B alloys for being made 5 μm in airflow milling Powder.Wherein antioxidant selects sodium sulfite.
3) Nd Fe B alloys powder and granularity are less than or equal to 10 microns of DyF3Powder is according to mass ratio 150:1 is dissolved in Ultrasonic disperse 25min, obtains slurries in a certain amount of ether;The additional amount (in mass) of the ether is Nd Fe B alloys powder 2.5 times.
4) dry composite powder is made by spray drying in above-mentioned slurries;
5) above-mentioned composite powder is subjected to magnetic field orientating molding, waits static pressure, neodymium iron is made in vacuum-sintering and tempering heat treatment Boron permanent magnet.The magnetic field orientating molding, magnetic field 1.6T;The equal static pressure, pressure 200MPa;The vacuum-sintering, Sintering temperature is 1040~1080, and vacuum degree is at least 1 × 10-2Pa, when sintering time is 2;The tempering heat treatment is 2 grades and returns Fire, level-one are tempered 850 DEG C, and 450 DEG C of second annealing, the time is 2 hours.
Comparative example 1
It by purity is 99.9wt%'s according to the proportion that alloying component is Nd11.76Fe82.36B5.88 (atomic percentage) Raw metal carries out rapid hardening, hydrogen breaking, airflow milling, and magnetic field orientating molding waits static pressure, vacuum-sintering and tempering heat treatment, above-mentioned Procedure parameter selection is identical as the parameter in embodiment 1, and traditional handicraft magnet sample as a comparison is made.
1 gained magnet of embodiment and 1 gained magnet of comparative example are subjected to magnetism testing, the results are shown in Table 1.
1 embodiment 1 of table and magnet magnetic property in comparative example 1
Embodiment 2
A method of spray drying preparation performance Nd Fe B sintered magnet includes the following steps:
1) design is based on 2:14:The Nd Fe B alloys ingredient Nd11.76Fe80.36B5.88Cu2 (atomic percentage) of 1 phase, According to the ingredient composition of design, the raw metal that purity is 99.9wt% is put into rapid hardening furnace and gets rid of band and is made with a thickness of 0.25mm Nd Fe B alloys thin slice;
2) above-mentioned alloy rapid-hardening flake is put into hydrogen broken furnace, leads to hydrogen stream 75ml/min, reacted 4 hours, hydrogen is broken to obtain 60 Mesh powder particle;Then the antioxidant of 0.15wt% is added, is transferred to and grinds the neodymium iron boron conjunction for being made 5 μm for 2 hours in airflow milling Bronze end carries out powder processed, obtains Nd Fe B alloys powder, and antioxidant therein is sodium pyrosulfite;
3) the DyH3 powder by Nd Fe B alloys powder and granularity less than or equal to 10 microns is according to mass ratio 140:1 is dissolved in Ultrasonic disperse 30min, obtains slurries in a certain amount of ether;
4) dry composite powder is made by spray drying in above-mentioned slurries;
5) above-mentioned composite powder is subjected to magnetic field orientating molding, waits static pressure, neodymium iron is made in vacuum-sintering and tempering heat treatment Boron permanent magnet.The magnetic field orientating molding, magnetic field 1.8T;The equal static pressure, pressure 220MPa;The vacuum-sintering, Sintering temperature is 1050 DEG C, and vacuum degree is at least 1 × 10-2Pa, sintering time are 2.5 hours;The tempering heat treatment is 2 grades and returns Fire, level-one are tempered 860 DEG C, and 470 DEG C of second annealing, the time is 2.5 hours.
Comparative example 2
It is by purity according to the proportion that alloying component is Nd11.76Fe80.36B5.88Cu2 (atomic percentage) The raw metal of 99.9wt% carries out rapid hardening, hydrogen breaking, airflow milling, and magnetic field orientating molding waits static pressure, vacuum-sintering and tempering heat Processing, above process parameter selection is identical as the parameter in embodiment 2, and traditional handicraft magnet sample as a comparison is made.
2 gained magnet of embodiment and 2 gained magnet of comparative example are subjected to magnetism testing, the results are shown in Table 2.
2 embodiment 2 of table and magnet magnetic property in comparative example 2
Embodiment 3
A method of spray drying preparation performance Nd Fe B sintered magnet includes the following steps:
1) design is based on 2:14:The Nd Fe B alloys ingredient Nd9.76Pr2Fe80.36B5.88Al2 (atomic percent of 1 phase Number), according to the ingredient composition of design, the raw metal that purity is 99.9wt% is put into rapid hardening furnace get rid of band be made with a thickness of The Nd Fe B alloys thin slice of 0.25mm;
2) above-mentioned alloy rapid-hardening flake is subjected to powder processed, obtains Nd Fe B alloys powder;First alloy cast ingot is carried out rough and torn It is broken, the antioxidant of 0.30wt% is added, then air-flow is milled into the Nd Fe B alloys powder that average grain diameter is 3 μm, therein Antioxidant is dibutylphenol;
3) the DyF3 powder by Nd Fe B alloys powder and granularity less than or equal to 10 microns is according to mass ratio 130:1 is dissolved in Ultrasonic disperse 27min, obtains slurries in a certain amount of ether;
4) dry composite powder is made by spray drying in above-mentioned slurries;
5) above-mentioned composite powder is subjected to magnetic field orientating molding, waits static pressure, neodymium iron is made in vacuum-sintering and tempering heat treatment Boron permanent magnet.The magnetic field orientating molding, magnetic field 2T;The equal static pressure, pressure 240MPa;The vacuum-sintering is burnt Junction temperature is 1060 DEG C, and vacuum degree is at least 1 × 10-2Pa, sintering time are 3 hours;The tempering heat treatment is 2 grades of tempering, Level-one is tempered 870 DEG C, and 490 DEG C of second annealing, the time is 3 hours.
Comparative example 3
It is by purity according to the proportion that alloying component is Nd9.76Pr2Fe80.36B5.88Al2 (atomic percentage) The raw metal of 99.9wt% carries out rapid hardening, hydrogen breaking, airflow milling, and magnetic field orientating molding waits static pressure, vacuum-sintering and tempering heat Processing, above process parameter selection is identical as the parameter in embodiment 3, and traditional handicraft magnet sample as a comparison is made.
3 gained magnet of embodiment and 3 gained magnet of comparative example are subjected to magnetism testing, the results are shown in Table 3.
3 embodiment 3 of table and magnet magnetic property in comparative example 3
Embodiment 4
A method of spray drying preparation performance Nd Fe B sintered magnet includes the following steps:
1) design is based on 2:14:The Nd Fe B alloys ingredient Dy1Nd9.76Pr1Fe81.36B5.88Al0.5Ga0.5 of 1 phase The raw metal that purity is 99.9wt% is put into rapid hardening furnace according to the ingredient composition of design and gets rid of band system by (atomic percentage) At the Nd Fe B alloys thin slice with a thickness of 0.25mm;
2) above-mentioned alloy rapid-hardening flake is subjected to powder processed, obtains Nd Fe B alloys powder;First alloy cast ingot is carried out rough and torn It is broken, the antioxidant of 0.40wt% is added, then air-flow is milled into the Nd Fe B alloys powder that average grain diameter is 4 μm.It is therein Antioxidant is sodium hydrogensulfite.
3) the Dy2O3 powder by Nd Fe B alloys powder and granularity less than or equal to 10 microns is according to mass ratio 120:1 dissolution Ultrasonic disperse 35min, obtains slurries in a certain amount of ether;
4) dry composite powder is made by spray drying in above-mentioned slurries;
5) above-mentioned composite powder is subjected to magnetic field orientating molding, waits static pressure, neodymium iron is made in vacuum-sintering and tempering heat treatment Boron permanent magnet.The magnetic field orientating molding, magnetic field 1.8T;The equal static pressure, pressure 250MPa;The vacuum-sintering, Sintering temperature is 1070 DEG C, and vacuum degree is at least 1 × 10-2Pa, sintering time are 4 hours;The tempering heat treatment is 2 grades and returns Fire, level-one are tempered 890 DEG C, and 520 DEG C of second annealing, the time is 4 hours.
Comparative example 4
It will according to the proportion that alloying component is Dy1Nd9.76Pr1Fe81.36B5.88Al0.5Ga0.5 (atomic percentage) The raw metal that purity is 99.9wt% carries out rapid hardening, hydrogen breaking, airflow milling, and magnetic field orientating molding waits static pressure, vacuum-sintering and Tempering heat treatment, above process parameter selection is identical as the parameter in embodiment 4, and traditional handicraft magnet sample as a comparison is made.
4 gained magnet of embodiment and 4 gained magnet of comparative example are subjected to magnetism testing, the results are shown in Table 4.
4 embodiment 4 of table and magnet magnetic property in comparative example 4
Embodiment 5
A method of spray drying preparation performance Nd Fe B sintered magnet includes the following steps:
1) design is based on 2:14:The Nd Fe B alloys ingredient of 1 phase Dy1Nd9.76Pr1Fe80.86B5.88Al0.5Ga0.5Co0.5 (atomic percentage), according to the ingredient composition of design, by purity It is put into for the raw metal of 99.9wt% and gets rid of band in rapid hardening furnace Nd Fe B alloys thin slice with a thickness of 0.25mm is made;
2) above-mentioned alloy rapid-hardening flake is subjected to powder processed, obtains Nd Fe B alloys powder;First alloy cast ingot is carried out rough and torn It is broken, the antioxidant of 0.70wt% is added, then air-flow is milled into the Nd Fe B alloys powder that average grain diameter is 4 μm.It is therein Antioxidant is sodium thiosulfate.
3) the TbF3 powder by Nd Fe B alloys powder and granularity less than or equal to 10 microns is according to mass ratio 110:1 is dissolved in Ultrasonic disperse 35min, obtains slurries in a certain amount of ether;
4) dry composite powder is made by spray drying in above-mentioned slurries;
5) above-mentioned composite powder is subjected to magnetic field orientating molding, waits static pressure, neodymium iron is made in vacuum-sintering and tempering heat treatment Boron permanent magnet.The magnetic field orientating molding, magnetic field 1.8T;The equal static pressure, pressure 250MPa;The vacuum-sintering, Sintering temperature is 1080 DEG C, and vacuum degree is at least 1 × 10-2Pa, sintering time are 2 hours;The tempering heat treatment is 2 grades and returns Fire, level-one are tempered 900 DEG C, and 550 DEG C of second annealing, the time is 2 hours.
Comparative example 5
It is matching for Dy1Nd9.76Pr1Fe80.86B5.88Al0.5Ga0.5Co0.5 (atomic percentage) according to alloying component Than the raw metal that purity is 99.9wt% is carried out rapid hardening, hydrogen breaking, airflow milling, magnetic field orientating molding waits static pressure, and vacuum is burnt Knot and tempering heat treatment, above process parameter selection is identical as the parameter in embodiment 5, and traditional handicraft magnet is made as a comparison Sample.
5 gained magnet of embodiment and 5 gained magnet of comparative example are subjected to magnetism testing, the results are shown in Table 5.
5 embodiment 5 of table and magnet magnetic property in comparative example 5
From the analysis of the data of above-described embodiment and comparative example it is found that the spray-dried magnet obtained for mixing heavy rare earth element Magnetic property especially coercivity compared to improving a lot with magnet made from conventional method, i.e., using the method for spray drying I High-performance neodymium iron boron sintered magnet has been made.
The above is only a preferred embodiment of the present invention, protection scope of the present invention is not limited merely to above-mentioned implementation Example, all technical solutions belonged under thinking of the present invention all belong to the scope of protection of the present invention.It should be pointed out that for the art Those of ordinary skill for, several improvements and modifications without departing from the principles of the present invention, these improvements and modifications It should be regarded as protection scope of the present invention.

Claims (7)

1. a kind of method of spray drying preparation performance Nd Fe B sintered magnet, which is characterized in that include the following steps:
1) nearly just dividing than 2:14:Nd Fe B alloys rapid-hardening flake is made using strip casting in 1 Nd Fe B alloys raw material;
2) above-mentioned alloy rapid-hardening flake is subjected to powder processed, obtains Nd Fe B alloys powder;
3) by Nd Fe B alloys powder and heavy rare earth metal powder or heavy rare earth compound powder according to mass ratio (100~150): 1 is dissolved in 25~35min of ultrasonic disperse in a certain amount of ether, obtains slurries;
4) dry composite powder is made by spray drying in above-mentioned slurries;
5) above-mentioned composite powder is subjected to magnetic field orientating molding, waits static pressure, neodymium iron boron is made forever in vacuum-sintering and tempering heat treatment Magnet.
2. the method for spray drying preparation performance Nd Fe B sintered magnet according to claim 1, which is characterized in that institute Stating flouring technology is that alloy cast ingot is first carried out coarse crushing, the antioxidant of 0.02wt%-0.70wt% is added, then airflow milling The Nd Fe B alloys powder that average grain diameter is 3~5 μm is made.
3. the method for spray drying preparation performance Nd Fe B sintered magnet according to claim 1, which is characterized in that institute The granularity of the heavy rare earth metal powder or heavy rare earth compound powder stated is less than or equal to 10 microns, and the heavy rare earth metal is At least one of three kinds of dysprosium, terbium and holmium elements, the heavy rare earth compound be containing in three kinds of dysprosium, terbium and holmium elements at least A kind of heavy rare earth compound.
4. the method for spray drying preparation performance Nd Fe B sintered magnet according to claim 1, which is characterized in that institute State magnetic field orientating molding, 1.6~2T of magnetic field.
5. the method for spray drying preparation performance Nd Fe B sintered magnet according to claim 1, which is characterized in that institute The equal static pressure stated, pressure are 200~300MPa.
6. the method for spray drying preparation performance Nd Fe B sintered magnet according to claim 1, which is characterized in that institute The vacuum-sintering stated, sintering temperature are 1040~1080 DEG C, and vacuum degree is at least 1 × 10-2Pa, sintering time are 2~4 hours.
7. the method for spray drying preparation performance Nd Fe B sintered magnet according to claim 1, which is characterized in that institute Stating tempering heat treatment is 2 grades of tempering, and level-one is tempered 850~900 DEG C, and 450~550 DEG C of second annealing, the time is 2~4 hours.
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CN111370215A (en) * 2020-01-06 2020-07-03 横店集团东磁股份有限公司 Efficient method for manufacturing ferrite rubber-plastic magnetic powder
CN113571280A (en) * 2021-07-23 2021-10-29 包头天和磁材科技股份有限公司 Neodymium iron boron magnet coarse powder auxiliary agent, preparation method and application thereof, and preparation method of magnet
CN115483016A (en) * 2022-10-13 2022-12-16 安徽省瀚海新材料股份有限公司 Preparation method of sintered neodymium-iron-boron magnet

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CN101615459B (en) * 2009-04-28 2011-11-23 中国科学院宁波材料技术与工程研究所 Method for improving performance of sintered Nd-Fe-B permanent magnetic material
CN105189805A (en) * 2013-04-24 2015-12-23 中央电气工业株式会社 Raw material alloy for R-T-B magnet
CN103646742A (en) * 2013-12-23 2014-03-19 湖南航天磁电有限责任公司 Neodymium-iron-boron magnet and preparation method thereof
CN104064346A (en) * 2014-05-30 2014-09-24 宁波同创强磁材料有限公司 NdFeB magnet and preparation method thereof
CN105427995A (en) * 2015-12-21 2016-03-23 浙江凯文磁业有限公司 Preparation method for improving NdFeB (neodymium iron boron) coercivity by organic heavy rare earth complex

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CN111370215A (en) * 2020-01-06 2020-07-03 横店集团东磁股份有限公司 Efficient method for manufacturing ferrite rubber-plastic magnetic powder
CN113571280A (en) * 2021-07-23 2021-10-29 包头天和磁材科技股份有限公司 Neodymium iron boron magnet coarse powder auxiliary agent, preparation method and application thereof, and preparation method of magnet
CN113571280B (en) * 2021-07-23 2024-02-13 包头天和磁材科技股份有限公司 Neodymium-iron-boron magnet coarse powder auxiliary agent, preparation method and application thereof, and preparation method of magnet
CN115483016A (en) * 2022-10-13 2022-12-16 安徽省瀚海新材料股份有限公司 Preparation method of sintered neodymium-iron-boron magnet

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