CN111312509B - Process method for carrying out dysprosium and terbium permeation on high-end neodymium iron boron product - Google Patents
Process method for carrying out dysprosium and terbium permeation on high-end neodymium iron boron product Download PDFInfo
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- H01F41/00—Apparatus 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
- H01F41/02—Apparatus 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
- H01F41/0253—Apparatus 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
- H01F41/0293—Apparatus 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 diffusion of rare earth elements, e.g. Tb, Dy or Ho, into permanent magnets
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- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- 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
- 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
- H01F1/0576—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 pressed, e.g. hot working
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- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- 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
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- 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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- H01F41/00—Apparatus 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
- H01F41/02—Apparatus 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
- H01F41/0253—Apparatus 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
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Abstract
The invention relates to the technical field of dysprosium and terbium penetration of neodymium iron boron products, in particular to a process method for dysprosium and terbium penetration of high-end neodymium iron boron products, which is characterized by comprising the following steps: (1) burdening and smelting; (2) preparing a spray liquid; (3) hydrogen crushing and airflow milling; (4) molding; (5) isostatic pressing; (6) dysprosium or terbium is added into the product prepared by the sintering and tempering steps in a spraying mode before hydrogen breaking, and the product has the advantages of simple process, energy conservation, great improvement on neodymium iron boron performance and the like.
Description
Technical Field
The invention relates to the technical field of dysprosium and terbium permeation of neodymium iron boron products, in particular to a process method for carrying out dysprosium and terbium permeation on high-end neodymium iron boron products, which has the advantages of simple process, energy conservation and greatly improved neodymium iron boron performance.
Background
As is well known, the nd-fe-b, which is one of rare earth permanent magnetic materials, has very high magnetic energy and coercive force, and the advantage of high energy density makes the nd-fe-b permanent magnetic material widely used in modern industry and electronic technology, so that it is possible to miniaturize, lighten and thin instruments and meters, electroacoustic motors, magnetic separation and magnetization, and other devices. In order to improve the coercive force of the ndfeb magnet, a certain amount of dysprosium or terbium is usually added into the ndfeb magnet or a certain amount of combination of the dysprosium or terbium is added into the ndfeb magnet, but in the existing method for adding the dysprosium or terbium into the ndfeb magnet, the depth of the dysprosium or terbium is generally shallow, the usage amount of the dysprosium is large, the influence is caused on the magnetism of the ndfeb magnet, the resource waste of the dysprosium is also caused, the cost of the dysprosium or terbium is increased, particularly, the step of carrying out the dysprosium or terbium infiltration is generally carried out after sintering in the existing process, so that the energy waste is caused by the multiple sintering and tempering, and the performances such as the coercive force of the obtained product are not ideal.
The prior infiltration process in the industry has the defects that: 1. dy or Tb still can be added in the burdening process, and the production process has high cost. 2. The thickness of the sintered product penetration hardly exceeds 4mm and the uniformity may be deteriorated. 3, after infiltration, vacuum sintering is needed to achieve the purpose of improving the performance, and the process of re-sintering needs about 6-10 hours.
The main effect of Dy or Tb in the sintered permanent magnet material is to improve the coercive force Hcj, the coercive force Hcj is one of the most important parameters for judging the performance of the permanent magnet material, the improvement of the coercive force can improve the maximum energy product (BH) m of the magnet, the demagnetization resistance of the permanent magnet in use can be improved, the stability of the magnet is improved, and the high-end permanent magnet motor, wind power generation, aerospace, medical industry and the like have very strict requirements on the Hcj of the sintered neodymium iron boron.
Moreover, the medical field and the aviation field have higher requirements on the comprehensive performance of neodymium iron boron products, such as EH, UH and other series, the coercive force is higher, particularly, cutting is needed after the products are prepared, and the dysprosium penetration or terbium penetration effect and the consistency are ensured to be good, so the squareness HK/Hcj is also required to be higher.
Disclosure of Invention
The invention aims to solve the defects of the prior art and provides a process method for carrying out dysprosium and terbium permeation on a high-end neodymium iron boron product, which has the advantages of simple process, energy conservation and greatly improved neodymium iron boron performance.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a process method for dysprosium and terbium permeation of a high-end neodymium iron boron product is characterized by comprising the following steps:
(1) material preparation and smelting: mixing praseodymium-neodymium, aluminum, copper, gadolinium, zirconium, niobium, boron and iron to form neodymium-iron-boron alloy, then placing the neodymium-iron-boron alloy into a crucible, vacuumizing and heating to 1450 ℃ with the vacuum degree of 10 & lt 3 & gt PA, and casting to finally form a sheet of 0.2-0.35mm under the condition of Ar-filled protection;
(2) preparing a spray liquid: mixing pure dysprosium or pure terbium powder into suspension;
(3) hydrogen breaking and jet milling: putting 500 kg of slices in the step (1) into a hydrogen breaking furnace, rotating the hydrogen breaking furnace without sealing the hydrogen breaking furnace at the rotating speed of 1.5 r/min, spraying the suspension prepared in the step (2) into the hydrogen breaking furnace, covering a cover of the hydrogen breaking furnace, vacuumizing to maintain the vacuum degree of-1 pa for 30-40 min, injecting hydrogen, crushing the powder with the hydrogen to obtain powder with the diameter of 240 plus 260 mu m, heating the powder to a reaction kettle to obtain powder with the temperature of 530 plus 540 ℃, reacting and separating out the hydrogen in the powder, carrying the powder in a grinding chamber by compressed nitrogen through an airflow mill through 4 nozzles to form supersonic colliding powder, continuously crushing the powder, and finally grinding the powder into fine powder with the diameter of 3-5 mu m;
(4) molding: putting the fine powder obtained in the step (3) into a die, and then putting the die into a press for pressing, wherein the forming pressure of the press is 8-12MPa, and the density of the obtained green compact is 3.5-3.8 g/cm3Green bodies;
(5) isostatic pressing: wrapping the green body obtained in the step (4) with a plastic film, then putting the plastic film into an isostatic press for pressurization, wherein the pressure is 16-18MPa, the time is 10min, and the slurry is solidified on the surface of the green body to obtain the green body with the density of 4.0-4.2g/cm3The blank of (2);
(6) sintering and tempering: unpacking the blank obtained in the step (5) under the protection of nitrogen, stacking in a graphite material box, feeding the product into a sintering furnace, strictly controlling the oxygen content not to exceed 10PPM in the process, starting vacuumizing a locking furnace cover, starting heating the product when the vacuum degree reaches 1pa, reaching 750 ℃ at the speed of 5 ℃/min, and at the moment, performing an internal gas release stage of the product until the vacuum degree reaches 5.0 to 10 ×, wherein-1And pa, continuing heating, raising the temperature to 1092 ℃ at the speed of 5 ℃/min, maintaining for 6-8 hours, rapidly cooling to 70 ℃ or less, continuing heating for tempering, keeping the primary tempering temperature of 890-930 ℃ for 3-4 hours, belonging to alloy binary eutectic, cooling to 70 ℃ or less, performing secondary tempering, heating to 450-650 ℃ and at the time belonging to ternary eutectic state, keeping the temperature for 3-4 hours, cooling to 60 ℃ or less, and discharging the product.
In the step (2), the granularity of the pure dysprosium or the pure terbium is 2.8-3.2 mu m, the gasoline is No. 120 gasoline, and the pure dysprosium or the pure terbium is mixed with the gasoline according to the mass ratio of 1: 5.
The spraying speed of the suspension sprayed in the step (3) is 1 liter/3 minutes, and the suspension is sprayed in a mist shape, and the spraying amount is 0.6-1.2% of the total weight of the slices.
The invention has the advantages of simple process, energy saving, greatly improved neodymium iron boron performance and the like due to the adoption of the process steps.
Drawings
FIG. 1 is a schematic view of 9 cutting sites of the present invention.
Detailed Description
The invention is further described below with reference to the accompanying drawings:
a process method for dysprosium and terbium permeation of a high-end neodymium iron boron product is characterized by comprising the following steps: (1) material preparation and smelting: praseodymium neodymium, aluminum, titanium,mixing copper, gadolinium, zirconium, niobium, boron and iron to form neodymium iron boron alloy, then placing the neodymium iron boron alloy into a crucible, vacuumizing and heating, wherein the vacuum degree is 10 & lt- & gt 3PA, heating to 1450 ℃, and casting under the condition of Ar protection to finally form a sheet with the thickness of 0.2-0.35 mm; (2) preparing a spray liquid: taking pure dysprosium or pure terbium powder with the granularity of 2.8-3.2 mu m, gasoline No. 120, and mixing the pure dysprosium or pure terbium powder and the gasoline according to the mass ratio of 1:5 to prepare suspension, (3) carrying out hydrogen crushing and airflow milling: putting 500 kg of the slices in the step (1) into a hydrogen breaking furnace, rotating the hydrogen breaking furnace without closing the furnace, wherein the rotating speed is 1.5 r/min, spraying the suspension prepared in the step (2) into the hydrogen breaking furnace at a spraying speed of 1 l/3 min in a mist state, wherein the spraying amount of the suspension is 0.6-1.2% of the total weight of the slices, covering the hydrogen breaking furnace with a cover, vacuumizing, maintaining the vacuum degree at-1 pa for 30-40 min, injecting hydrogen, crushing the powder with the hydrogen, wherein the diameter of the powder is 240-260 mu m, reacting and separating out the hydrogen in the powder at the temperature of 530-540 ℃ in a heating reaction kettle, carrying the powder in a grinding chamber by compressed nitrogen through an airflow mill through 4 nozzles, continuously crushing the powder with supersonic speed, and finally grinding the powder into 3-5 mu m fine powder; (4) molding: putting the fine powder obtained in the step (3) into a die, and then putting the die into a press for pressing, wherein the forming pressure of the press is 8-12MPa, and the density of the obtained green compact is 3.5-3.8 g/cm3Green bodies; (5) isostatic pressing: wrapping the green body obtained in the step (4) with a plastic film, then putting the plastic film into an isostatic press for pressurization, wherein the pressure is 16-18MPa, the time is 10min, and the slurry is solidified on the surface of the green body to obtain the green body with the density of 4.0-4.2g/cm3The blank of (2); (6) sintering and tempering: unpacking the blank obtained in the step (5) under the protection of nitrogen, stacking in a graphite material box, feeding the product into a sintering furnace, strictly controlling the oxygen content not to exceed 10PPM in the process, starting vacuumizing a locking furnace cover, starting heating the product when the vacuum degree reaches 1pa, reaching 750 ℃ at the speed of 5 ℃/min, and at the moment, performing an internal gas release stage of the product until the vacuum degree reaches 5.0 to 10 ×, wherein-1pa, continuously heating, raising the temperature to 1092 ℃ at the speed of 5 ℃/min, maintaining for 6-8 hours, quickly cooling to 70 ℃ or less, continuously heating and temperingThe primary tempering temperature is 890-930 ℃ and the heat is continuously preserved for 3-4 hours, which belongs to alloy binary eutectic, after the alloy binary eutectic is cooled to be less than or equal to 70 ℃, the secondary tempering is carried out, the alloy binary eutectic is heated to be 450-650 ℃, which belongs to ternary eutectic state, after the heat is continuously preserved for 3-4 hours, the air is cooled to be less than or equal to 60 ℃, and the product is discharged from the furnace.
According to the same formula, dysprosium or terbium is converted into molten dysprosium or terbium and added before hydrogen breaking, and although the total amount of the dysprosium and terbium is not changed, the performance is obviously improved.
The difference between the prior art and the present art;
the prior art comprises the following steps: proportioning (containing dysprosium/terbium), smelting, hydrogen crushing, milling, molding, isostatic pressing, sintering and machining.
The process comprises the following steps: proportioning, smelting (without dysprosium/terbium), spraying dysprosium terbium, crushing by hydrogen, pulverizing, molding, isostatic pressing, sintering and machining.
The products prepared by the prior art and the process are cut into 9 products according to 9 positions marked by a figure 1, the products at the 9 positions are subjected to performance testing, the performance tables of the prior art and the products prepared by the process are shown in the following table 1-table 4, wherein the table 1 is a terbium-infiltrated product performance table of the prior art (the mixture ratio of raw materials in the table indicates that the raw materials directly contain terbium), the table 2 is a terbium-infiltrated product performance table of the process (hydrogen breaking infiltration indicates that terbium is sprayed before the hydrogen breaking process), the table 3 is a dysprosium-infiltrated product performance table of the prior art (the mixture ratio of the raw materials in the table indicates that dysprosium is directly contained in the raw materials), and the table 4 is a dysprosium-infiltrated product performance table of the process (hydrogen breaking infiltration indicates that dysprosium is sprayed before the hydrogen breaking process).
Table 1: terbium-infiltrated product performance table of the prior art (the mixture ratio of the raw materials in the table indicates that the raw materials directly contain terbium)
Table 2: terbium permeability product performance table of the process (hydrogen breaking permeability means spraying terbium before hydrogen breaking process)
Table 3: dysprosium-doped product performance table in the prior art (raw material proportion in the table indicates that the raw materials contain dysprosium directly)
Table 4: dysprosium-infiltrated product performance meter of the process (Hydrogen-broken infiltration means that dysprosium is sprayed before hydrogen-broken process)
From the comparison between the above tables 1 and 2, it can be seen that: the coercive force Hcj of the terbium-infiltrated product prepared by the process is obviously improved, wherein the squareness HK/Hcj reaches 0.99, and the squareness of 9 parts is 0.99, so that the terbium-infiltrated product prepared by the process has good effect and consistent squareness, and is very suitable for the requirements of high-end permanent magnet motors, wind power generation, aerospace and medical industries on neodymium iron boron products.
From the comparison between the above tables 3 and 4, it can be seen that: the coercive force Hcj of the dysprosium infiltrated product prepared by the process is obviously improved, wherein the squareness HK/Hcj reaches 0.99, and the squareness of 9 parts is 0.99, which shows that the dysprosium infiltrated product prepared by the process has good dysprosium infiltrated effect and consistent squareness, and is very suitable for the requirements of high-end permanent magnet motors, wind power generation, aerospace and medical industries on neodymium iron boron products.
Claims (1)
1. A process method for dysprosium and terbium permeation of a high-end neodymium iron boron product is characterized by comprising the following steps:
(1) material preparation and smelting: mixing praseodymium-neodymium, aluminum, copper, gadolinium, zirconium, niobium, boron and iron to form neodymium-iron-boron alloy, then placing the neodymium-iron-boron alloy into a crucible, vacuumizing and heating to 1450 ℃ with the vacuum degree of 10 & lt 3 & gt PA, and casting to finally form a sheet of 0.2-0.35mm under the condition of Ar-filled protection;
(2) preparing a spray liquid: mixing pure dysprosium or pure terbium powder into a suspension, wherein the granularity of the pure dysprosium or the pure terbium is 2.8-3.2 mu m, the gasoline is No. 120 gasoline, and the pure dysprosium or the pure terbium is mixed with the gasoline according to the mass ratio of 1: 5;
(3) hydrogen breaking and jet milling: putting 500 kg of slices obtained in the step (1) into a hydrogen-breaking furnace, rotating the hydrogen-breaking furnace without sealing a cover, wherein the rotating speed is 1.5 revolutions per minute, then spraying the suspension prepared in the step (2) into the hydrogen-breaking furnace, then covering a cover of the hydrogen-breaking furnace, vacuumizing, maintaining the vacuum degree at-1 pa for 30-40 minutes, then injecting hydrogen, wherein the diameter of the powder is 240-260 mu m after the hydrogen is crushed, then passing through a heating reaction kettle, the temperature reaches 530-540 ℃, the hydrogen in the powder can react and be separated out, the powder is carried in a grinding chamber by compressed nitrogen through an airflow mill and passes through 4 nozzles to form supersonic speed colliding powder, the supersonic speed colliding powder is continuously crushed, and finally the supersonic speed colliding powder is ground into 3-5 mu m fine powder, the spraying speed of the spraying suspension is 1 liter/3 minutes, and the spraying amount is 0.6-1.2% of the total weight of the slices;
(4) molding: putting the fine powder obtained in the step (3) into a die, and then putting the die into a press for pressing, wherein the forming pressure of the press is 8-12MPa, and the density of the obtained green compact is 3.5-3.8 g/cm3Green bodies;
(5) isostatic pressing: wrapping the green body obtained in the step (4) with a plastic film, then putting the plastic film into an isostatic press for pressurization, wherein the pressure is 16-18MPa, the time is 10min, and the slurry is solidified on the surface of the green body to obtain the green body with the density of 4.0-4.2g/cm3The blank of (2);
(6) sintering and tempering: unpacking the blank obtained in the step (5) under the protection of nitrogen, stacking in a graphite material box, feeding the product into a sintering furnace, strictly controlling the oxygen content not to exceed 10PPM in the process, starting vacuumizing a locking furnace cover, starting heating the product when the vacuum degree reaches 1pa, reaching 750 ℃ at the speed of 5 ℃/min, and at the moment, performing an internal gas release stage of the product until the vacuum degree reaches 5.0 to 10 ×, wherein-1pa, continuously heating, raising the temperature to 1092 ℃ at the speed of 5 ℃/min, maintaining for 6-8 hours, rapidly cooling to 70 ℃ or less, continuously heating for tempering, keeping the primary tempering temperature of 890-650 ℃ for 3-4 hours, belonging to the alloy binary eutectic, cooling to 70 ℃ or less, performing secondary tempering, heating to 450-650 ℃ and keeping the temperature for 6-8 hoursThe temperature is kept for 3-4 hours, and then the product is discharged from the furnace after air cooling to be less than or equal to 60 ℃.
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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 |
| CN102347126B (en) * | 2010-07-30 | 2014-07-23 | 沈阳中北通磁科技股份有限公司 | High-performance sintered neodymium-iron-boron (Nd-Fe-B) rare-earth permanent magnet material and manufacturing method thereof |
| CN103757586A (en) * | 2014-01-13 | 2014-04-30 | 赣州诚正有色金属有限公司 | Method of infiltrating metal infiltrating agent to cerium-containing neodymium iron boron magnetic material |
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