CN112614685B - Sintered neodymium-iron-boron permanent magnet oxygen control preparation method and prepared neodymium-iron-boron permanent magnet - Google Patents
Sintered neodymium-iron-boron permanent magnet oxygen control preparation method and prepared neodymium-iron-boron permanent magnet Download PDFInfo
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- 239000001301 oxygen Substances 0.000 title claims abstract description 105
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 105
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 104
- 229910001172 neodymium magnet Inorganic materials 0.000 title claims abstract description 51
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000000843 powder Substances 0.000 claims abstract description 106
- 238000005245 sintering Methods 0.000 claims abstract description 30
- 238000000034 method Methods 0.000 claims abstract description 29
- 238000005496 tempering Methods 0.000 claims abstract description 28
- 238000000462 isostatic pressing Methods 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000000463 material Substances 0.000 claims abstract description 25
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000001257 hydrogen Substances 0.000 claims abstract description 22
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 22
- 238000003801 milling Methods 0.000 claims abstract description 16
- 238000012360 testing method Methods 0.000 claims abstract description 12
- 238000007792 addition Methods 0.000 claims abstract description 11
- 238000003723 Smelting Methods 0.000 claims abstract description 10
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 10
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 10
- 239000000314 lubricant Substances 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 238000009740 moulding (composite fabrication) Methods 0.000 claims abstract description 4
- 238000005070 sampling Methods 0.000 claims abstract description 4
- 230000009469 supplementation Effects 0.000 claims abstract description 4
- 239000002245 particle Substances 0.000 claims description 25
- 238000000465 moulding Methods 0.000 claims description 23
- 238000009826 distribution Methods 0.000 claims description 9
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 4
- 239000002994 raw material Substances 0.000 abstract description 10
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 4
- 150000002910 rare earth metals Chemical class 0.000 abstract description 4
- 238000000354 decomposition reaction Methods 0.000 abstract description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 52
- 238000010438 heat treatment Methods 0.000 description 28
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 27
- 229910052786 argon Inorganic materials 0.000 description 26
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 22
- 238000001816 cooling Methods 0.000 description 18
- 238000011049 filling Methods 0.000 description 18
- 239000007789 gas Substances 0.000 description 13
- 239000000203 mixture Substances 0.000 description 12
- 238000004321 preservation Methods 0.000 description 12
- 241001062472 Stokellia anisodon Species 0.000 description 11
- 229910052757 nitrogen Inorganic materials 0.000 description 11
- 229910052742 iron Inorganic materials 0.000 description 10
- 239000000047 product Substances 0.000 description 10
- 239000013589 supplement Substances 0.000 description 8
- 238000005303 weighing Methods 0.000 description 8
- 229910052689 Holmium Inorganic materials 0.000 description 7
- 229910052796 boron Inorganic materials 0.000 description 7
- 238000005266 casting Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
- 229910052802 copper Inorganic materials 0.000 description 7
- 229910052733 gallium Inorganic materials 0.000 description 7
- 229910052726 zirconium Inorganic materials 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 229910045601 alloy Inorganic materials 0.000 description 6
- 239000000956 alloy Substances 0.000 description 6
- 238000006356 dehydrogenation reaction Methods 0.000 description 6
- 238000007599 discharging Methods 0.000 description 6
- 239000010439 graphite Substances 0.000 description 6
- 229910002804 graphite Inorganic materials 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 239000006247 magnetic powder Substances 0.000 description 6
- 239000002985 plastic film Substances 0.000 description 6
- 229920006255 plastic film Polymers 0.000 description 6
- 238000007670 refining Methods 0.000 description 6
- 229920006395 saturated elastomer Polymers 0.000 description 6
- 238000009461 vacuum packaging Methods 0.000 description 6
- RKLPWYXSIBFAJB-UHFFFAOYSA-N [Nd].[Pr] Chemical compound [Nd].[Pr] RKLPWYXSIBFAJB-UHFFFAOYSA-N 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 238000011068 loading method Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000000227 grinding Methods 0.000 description 4
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000010902 jet-milling Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000005481 NMR spectroscopy Methods 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000013213 extrapolation Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- RYZCLUQMCYZBJQ-UHFFFAOYSA-H lead(2+);dicarbonate;dihydroxide Chemical compound [OH-].[OH-].[Pb+2].[Pb+2].[Pb+2].[O-]C([O-])=O.[O-]C([O-])=O RYZCLUQMCYZBJQ-UHFFFAOYSA-H 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- 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
- H01F1/0573—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 obtained by reduction or by hydrogen decrepitation or embrittlement
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- 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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- 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 belongs to the technical field of rare earth permanent magnet materials, and particularly relates to a sintered neodymium iron boron permanent magnet oxygen control preparation method and a prepared neodymium iron boron permanent magnet. The method comprises the steps of preparing raw materials, smelting, carrying out hydrogen crushing to obtain coarse powder, adding an antioxidant into the coarse powder, carrying out airflow milling to prepare powder under the condition of no oxygen supplementation, adding a lubricant into the obtained fine powder, sampling to test the oxygen content in the fine powder, adding water into the fine powder, uniformly stirring to obtain powder, and carrying out forming, isostatic pressing, sintering and tempering to obtain the neodymium-iron-boron permanent magnet. The addition amount of water is calculated according to the test result of the oxygen content of the fine powder and the target oxygen content, the oxygen supplementation amount is accurately controlled, and after the water and the fine powder are uniformly mixed, oxygen generated by decomposition in the sintering process is uniformly combined with the neodymium iron boron, so that the oxygen content in the magnet is uniformly and stably distributed, and the coercive force and the overall performance of the magnet are further improved.
Description
Technical Field
The invention belongs to the technical field of rare earth permanent magnet materials, and particularly relates to an oxygen control preparation method of a sintered neodymium iron boron permanent magnet and the prepared neodymium iron boron permanent magnet.
Background
Neodymium iron boron (NdFeB) is a rare earth permanent magnet material with the strongest magnetism at present, has good coercive force (Hcj), high magnetic energy product (8MGOe-64MGOe) and high temperature resistance, and related products are widely applied to the fields of electric automobiles, wind power generation, variable frequency air conditioners, nuclear magnetic resonance, optical disk drivers, instruments and meters, mineral separation, toys and the like. During the process of manufacturing the sintered Nd-Fe-B permanent magnet material, oxygen inevitably enters the sintered Nd-Fe-B permanent magnet from the atmosphere, although the ultra-pure raw materials are used, the pure ternary sintered Nd-Fe-B-O permanent magnet cannot be manufactured, actually, the quaternary Nd-Fe-B-O permanent magnet is a permanent magnet, and the oxygen brought in the preparation process has the performance on the sintered Nd-Fe-B permanent magnet material, especially the performance of HcjThere is a significant impact. At present, the preparation of the high-performance sintered Nd-Fe-B permanent magnet usually adopts a low-oxygen process route, but for the sintered Nd-Fe-B magnet with high rare earth total (more than 33 percent), the oxygen content of the magnet is HcjIs not that the lower the oxygen, the better, the magnetHcjWill increase with increasing oxygen content and decrease after increasing to a certain level. It has been shown that an appropriate oxygen content can improve the magnetic properties and stability of the magnet. Therefore, the control of the oxygen content is of great significance to the manufacture of high-performance sintered Nd-Fe-B permanent magnets and is also a great technical problem which troubles the production of sintered Nd-Fe-B permanent magnet materials.
At present, certain oxygen is mainly added in the air flow milling process in China, and the purpose of oxygen control is realized by isolating and controlling the oxygen (reducing the oxygen content in the subsequent production process as much as possible) in the subsequent production, for example, pure oxygen is absorbed into the air flow milling machine in the air flow milling and crushing process in the invention application with the publication number of CN108133818A, so that the direct adsorption and oxidation of air and water vapor are avoided, and the magnetic performance of the sintered neodymium iron boron magnet is improved. However, the oxygen content of the sintered nd-fe-b permanent magnet is not only influenced by the temperature and humidity of the working environment, but also related to the specific surface area of the powder particles, and the finer the particles, the larger the specific surface area, the easier the particles are oxidized. Because of the influence of the microstructure of the smelting cast piece and the hydrogen crushing process, the particle size of coarse powder is difficult to control during the air flow milling, and the retention time of the coarse powder in a milling chamber during the air flow milling also influences the oxygen absorption content of magnetic powder. In the process of milling powder by the jet mill, the particle size of the powder is reduced after the powder collides with each other, the specific surface area is increased, a large amount of heat can be released to increase the temperature of the magnetic powder, and the higher the temperature is, the more violent the oxygen absorption of the magnetic powder is. Therefore, the uniformity of the oxygen content of the neodymium iron boron magnetic powder is difficult to realize by adding oxygen through the jet mill, and the consistency of the oxygen content on the microscopic level is difficult to realize even if the later-stage powder is stirred. To obtain a high-performance sintered ndfeb permanent magnet, not only the oxygen content of the magnet needs to be controlled within a stable range, but also the oxygen distribution in the magnetic powder needs to be uniform to ensure the consistency of the magnet performance in molding, pressing and sintering.
Disclosure of Invention
Aiming at the technical problems, the invention aims to provide an oxygen control preparation method of a sintered neodymium iron boron permanent magnet, so that the uniform, stable and controllable oxygen content in the sintered neodymium iron boron magnet is realized.
The above object of the present invention is achieved by the following technical solutions:
an oxygen-controlling preparation method of a sintered neodymium-iron-boron permanent magnet comprises the steps of preparing materials, smelting, and carrying out hydrogen crushing to obtain coarse powder, adding an antioxidant into the coarse powder, carrying out airflow milling to prepare powder under the condition of no oxygen supplementation to obtain fine powder, then adding a lubricant, sampling to test the oxygen content in the fine powder, adding water into the fine powder, uniformly stirring to obtain powder, and carrying out forming, isostatic pressing, sintering and tempering to obtain the neodymium-iron-boron permanent magnet.
The particle size of the powder obtained by the airflow milling is small, the specific surface area is large, the powder is easy to oxidize, and at present, certain oxygen is supplemented in the powder making process to ensure that the powder is slightly passivated so as to prevent the over-high oxygen content caused by severe oxidation in the subsequent forming process. However, in the process of jet milling, the powder collides with each other to release heat, oxygen absorption is aggravated, the uniformity of the oxygen content in the magnetic powder is difficult to ensure by adding oxygen through the jet mill, and the oxygen supplement amount is difficult to control.
In the above preparation method, the amount of water added is calculated as follows: m × (w)0-w1) X 18/16; wherein M is the weight of the fine powder, w0Is the target oxygen content, w1Is the oxygen content in the fine powder, and w1≤w0。
When testing the oxygen content, firstly sampling, preparing a magnet sample by molding, isostatic pressing, sintering and tempering under the control of an oxygen-free process, and taking the central part of the magnet sample to test the oxygen content (w)1). According to the oxygen content test result and the target oxygen content (w) of the product2) And calculating the weight of the oxygen needing to be increased, and further obtaining the addition amount of the water. According to the invention, water with corresponding weight is accurately added according to the actual oxygen content after the powder is milled by the airflow mill, so that the oxygen content in the neodymium iron boron magnet tends to be stable and is controlled to be in a certain rangeWithin a constant range.
In the preparation method, the smelting comprises the following specific steps: putting raw materials into a crucible of a rapid hardening furnace, vacuumizing the rapid hardening furnace to below 1Pa, starting to dry the materials, setting the power of the dried materials to be 80-120 KW, setting the time to be 10-30 minutes, filling argon to be-0.07-0.055 MPa when the vacuum degree is lower than 3Pa, then increasing the power to 480-550 KW, and starting to smelt; after the raw materials are melted, continuously melting for 8-10 minutes, adjusting the power to 350-400 KW, and refining for 2-5 minutes; the surface of the alloy liquid turns silvery white, and casting is carried out to obtain a cast sheet.
In the preparation method, the hydrogen crushing comprises the following specific steps: and (3) putting the cast piece into a hydrogen crushing furnace, absorbing hydrogen until the cast piece is saturated, and then heating to 500-600 ℃ for dehydrogenation until the pressure is lower than 20Pa to obtain coarse powder.
In the preparation method, before the powder is prepared by the jet mill, the jet mill is required to be subjected to oxygen discharge until the oxygen concentration is not more than 5 ppm.
In the preparation method, the average particle diameter SMD of the fine powder is 2.5-3.0 μm, and the particle size distribution ratio is not more than (X90/X10) 5.0.
In the preparation method, in the powder preparation process of the jet mill, the addition amount of the antioxidant is 0.05-0.2% of the weight of the coarse powder, and the addition amount of the lubricant is 0.05-0.2% of the weight of the fine powder.
In the above preparation method, the molding specifically comprises: under the nitrogen atmosphere, the powder is placed in a magnetic field of a press with the temperature of more than 1.5T and is subjected to orientation forming to obtain the powder with the density of 3.6-4.2 g/cm3The green compact of (1).
In the forming process, the oxygen content of the nitrogen atmosphere is controlled to be less than 0.05 percent.
In the above preparation method, the isostatic pressing is specifically: wrapping the green body with a plastic film, vacuum packaging, placing into an isostatic pressing machine, and performing isostatic pressing treatment under the oil pressure of 150-300MPa to further increase the density of the blank to 4.4-4.8g/cm3。
In the above preparation method, the sintering specifically is: removing vacuum bag and film under nitrogen protection, placing in a graphite box, placing in a furnace, and vacuumizing to 5.0 × 10-1Pa or lessHeating to 800-900 deg.c, maintaining for 3-6 hr, and lowering the vacuum degree to 10-1And (4) continuously heating to 1000-1100 ℃ below Pa, and sintering for 2-10 hours.
In the above preparation method, the tempering specifically is: and cooling the sintered product to be below 100 ℃ by filling argon gas, heating the sintered product to 860 to 950 ℃, preserving the heat for 1 to 4 hours, performing primary tempering, cooling the sintered product to be below 80 ℃ by filling argon gas after heat preservation, heating the sintered product to be 440 to 520 ℃, preserving the heat for 3 to 6 hours, performing secondary tempering, cooling the sintered product to be below 60 ℃ by filling argon gas after heat preservation, and discharging the sintered product.
The invention also aims to provide the sintered neodymium-iron-boron permanent magnet prepared by the preparation method.
The sintered Nd-Fe-B permanent magnet comprises the following chemical components in percentage by mass: PrNd: 28-33 wt%, Ho: 1-5 wt%, B: 0.92-1.1 wt%, Al: 0-0.8 wt%, Cu: 0.05-0.3 wt%, Co: 0.1 to 2 wt%, Ga: 0 to 0.5 wt%, Zr: 0 to 0.5 wt%, and the balance Fe.
In a preferred embodiment of the present invention, the sintered nd-fe-b permanent magnet comprises the following chemical components by mass: PrNd: 29 wt%, Ho: 4 wt%, B: 0.94 wt%, Al: 0.9 wt%, Cu: 0.2 wt%, Co: 0.2 wt%, Ga: 0.1 wt%, Zr: 0.1 wt%, and the balance Fe.
Compared with the prior art, the invention has the following advantages:
1. according to the invention, no oxygen is added in the powder preparation process of the air flow mill, water is added to supplement oxygen after the fine powder is prepared, and oxygen generated by decomposition in the sintering process is uniformly combined with the neodymium iron boron after the water and the fine powder are uniformly mixed, so that uniform oxygen control of the neodymium iron boron magnet can be realized.
2. The water addition amount is calculated according to the test result of the oxygen content of the fine powder and the target oxygen content, so that accurate oxygen supplement is realized, the supplemented oxygen is obtained through water decomposition instead of direct oxygen charging, the stability of the oxygen content in the neodymium iron boron permanent magnet can be controlled, and the consistency of the oxygen on microscopic distribution can be ensured.
3. The neodymium iron boron permanent magnet prepared by the invention carries out reasonable oxygen control through process optimization, so that the oxygen content in the magnet is uniform and stable, and the coercive force and the overall performance of the magnet are favorably improved.
Detailed Description
The technical solution of the present invention is further described and illustrated by the following specific examples. The raw materials used in the examples of the present invention are all those commonly used in the art, and the methods used in the examples are all those conventionally used in the art, unless otherwise specified. It should be understood that the specific embodiments described herein are merely to aid in the understanding of the invention and are not intended to limit the invention specifically.
Example 1
The embodiment provides a preparation method of a sintered neodymium iron boron permanent magnet, which comprises the following steps:
(1) preparing materials: weighing the following raw materials in percentage by weight: PrNd: 29 wt%, Ho: 4 wt%, B: 0.94 wt%, Al: 0.9 wt%, Cu: 0.2 wt%, Co: 0.2 wt%, Ga: 0.1 wt%, Zr: 0.1 wt%, the balance being Fe;
(2) smelting: sequentially loading finely crushed materials such as iron bars, ferroboron and the like and praseodymium-neodymium into a crucible of a rapid hardening furnace, vacuumizing the rapid hardening furnace to below 1Pa, starting to dry the materials, setting the power of the drying to be 100KW, setting the time to be 10 minutes, filling argon to-0.065 MPa when the vacuum degree is lower than 3Pa, increasing the power to 500KW, and starting to smelt; continuing to smelt for 10 minutes after the iron rod is completely smelted, adjusting the power to 360KW, and refining for 5 minutes; when the alloy liquid level is changed into silvery white, casting to obtain a cast sheet;
(3) hydrogen crushing: putting the cast sheet into a hydrogen crushing furnace, absorbing hydrogen until the cast sheet is saturated, and then heating the cast sheet to 550 ℃ for dehydrogenation until the temperature is lower than 20Pa to obtain coarse powder;
(4) milling: adding 0.105kg of antioxidant into 105kg of coarse powder, firstly carrying out oxygen discharge on an air flow mill until the oxygen concentration is less than or equal to 5ppm, then grinding the coarse powder into fine powder under the condition of no oxygen supplement, and then adding 0.105kg of lubricant into the fine powder; the volume average particle diameter SMD of the fine powder is 2.6 mu m and the particle size distribution ratio (X90/X10) is less than or equal to 5.0 measured by a Newpatakg laser particle size tester;
(5) and (3) testing the oxygen content: weighing 5kg of sample from the powder obtained in the step (4), and formingCarrying out type, isostatic pressing, sintering and tempering treatment to obtain a neodymium iron boron magnet sample, taking the central part of the sample, and measuring the oxygen content (w) in the sample by adopting an IRO-II type oxygen measuring instrument1) The result was 0.038%; wherein, the molding, isostatic pressing, sintering and tempering processes are the same as the steps (7) to (9);
(6) adding water and stirring: according to M x (w)0-w1) X 18/16 calculating Water addition amount, wherein, target oxygen content (w)0) 0.2 percent, and the weight (M) of the sampled fine powder is 100kg, 0.182kg of water is added into the fine powder, and the fine powder and the water are stirred for 8 hours on a three-dimensional American-like stirrer to be fully and uniformly mixed;
(7) molding: ensuring that the oxygen content of the seal box is less than 0.05 percent under the protection of nitrogen, and molding the powder in a mold with a magnetic field of a press machine more than 1.5T to obtain the molding density of 3.8g/cm3The green compact of (a);
(8) isostatic pressing: wrapping the green body with plastic film, vacuum packaging, placing into isostatic press, performing isostatic pressing treatment under 200MPa oil pressure to further increase the density of the green body to 4.7g/cm3；
(9) Sintering and tempering: removing vacuum bag and film under nitrogen protection, placing in a graphite box, placing in a furnace, and vacuumizing to 5.0 × 10-1Heating to 850 deg.C below Pa, maintaining for 4 hr, and reducing vacuum degree to 10-1Continuously heating to 1000 ℃ below Pa, and sintering for 8 hours; and cooling the mixture to below 100 ℃ by filling argon after sintering, heating the mixture to 920 ℃, preserving heat for 3 hours, carrying out primary tempering, cooling the mixture to below 80 ℃ by filling argon after heat preservation, heating the mixture to 460 ℃, preserving heat for 5 hours, carrying out secondary tempering, cooling the mixture to below 60 ℃ by filling argon after heat preservation, and discharging the mixture.
Example 2
The embodiment provides a preparation method of a sintered neodymium iron boron permanent magnet, which comprises the following steps:
(1) preparing materials: weighing the following raw materials in percentage by weight: PrNd: 29 wt%, Ho: 4 wt%, B: 0.94 wt%, Al: 0.9 wt%, Cu: 0.2 wt%, Co: 0.2 wt%, Ga: 0.1 wt%, Zr: 0.1 wt%, the balance being Fe;
(2) smelting: sequentially loading finely crushed materials such as iron bars, ferroboron and the like and praseodymium-neodymium into a crucible of a rapid hardening furnace, vacuumizing the rapid hardening furnace to below 1Pa, starting to dry the materials, setting the power of the drying to be 100KW, setting the time to be 10 minutes, filling argon to-0.065 MPa when the vacuum degree is lower than 3Pa, increasing the power to 500KW, and starting to smelt; continuing to smelt for 10 minutes after the iron rod is smelted, adjusting the power to 360KW, and refining for 5 minutes; when the alloy liquid level is changed into silvery white, casting to obtain a cast sheet;
(3) hydrogen crushing: putting the cast sheet into a hydrogen crushing furnace, absorbing hydrogen until the cast sheet is saturated, and then heating to 550 ℃ for dehydrogenation until the temperature is lower than 20Pa to obtain coarse powder;
(4) milling: adding 0.105kg of antioxidant into 105kg of coarse powder, firstly carrying out oxygen discharge on an air flow mill until the oxygen concentration is less than or equal to 5ppm, then grinding the coarse powder into fine powder under the condition of no oxygen supplement, and then adding 0.105kg of lubricant into the fine powder; the volume average particle diameter SMD of the fine powder is 2.6 mu m and the particle size distribution ratio (X90/X10) is less than or equal to 5.0 measured by a Newpatakg laser particle size tester;
(5) and (3) testing the oxygen content: weighing 5kg of sample from the powder obtained in the step (4), forming, isostatic pressing, sintering and tempering to obtain a neodymium-iron-boron magnet sample, measuring the oxygen content (w) in the sample by adopting an IRO-II type oxygen measuring instrument at the central part of the sample1) The result was 0.041%; wherein, the molding, isostatic pressing, sintering and tempering processes are the same as the steps (7) to (9);
(6) adding water and stirring: according to M x (w)0-w1) X 18/16 calculating Water addition amount, wherein, target oxygen content (w)0) When the weight of the fine powder is 0.3 percent and the weight (M) of the sampled fine powder is 100kg, 0.291kg of water is added into the fine powder, and the fine powder and the water are stirred for 8 hours on a three-dimensional American-like stirrer to be fully and uniformly mixed;
(7) molding: ensuring that the oxygen content of the seal box is less than 0.05 percent under the protection of nitrogen, and molding the powder in a mold with a magnetic field of a press machine more than 1.5T to obtain the molding density of 3.8g/cm3The green compact of (a);
(8) isostatic pressing: wrapping the green body with plastic film, vacuum packaging, placing into isostatic pressing machine, and performing isostatic pressing treatment under 200MPa oil pressure to further increase the density of the green bodyTo 4.7g/cm3；
(9) Sintering and tempering: removing vacuum bag and film under nitrogen protection, placing in a graphite box, placing in a furnace, and vacuumizing to 5.0 × 10-1Heating to 800 deg.C below Pa, maintaining for 5 hr, and reducing vacuum degree to 10-1Continuously heating to 1100 ℃ below Pa, and sintering for 6 hours; and cooling the mixture to below 100 ℃ by filling argon after sintering, heating the mixture to 920 ℃, preserving heat for 3 hours, carrying out primary tempering, cooling the mixture to below 80 ℃ by filling argon after heat preservation, heating the mixture to 460 ℃, preserving heat for 5 hours, carrying out secondary tempering, cooling the mixture to below 60 ℃ by filling argon after heat preservation, and discharging the mixture.
Example 3
The embodiment provides a preparation method of a sintered neodymium iron boron permanent magnet, which comprises the following steps:
(1) preparing materials: weighing the following raw materials in percentage by weight: PrNd: 29 wt%, Ho: 4 wt%, B: 0.94 wt%, Al: 0.9 wt%, Cu: 0.2 wt%, Co: 0.2 wt%, Ga: 0.1 wt%, Zr: 0.1 wt%, the balance being Fe;
(2) smelting: sequentially loading finely crushed materials such as iron bars, ferroboron and the like and praseodymium-neodymium into a crucible of a rapid hardening furnace, vacuumizing the rapid hardening furnace to below 1Pa, starting to dry the materials, setting the power of the drying to be 100KW, setting the time to be 10 minutes, filling argon to-0.065 MPa when the vacuum degree is lower than 3Pa, increasing the power to 500KW, and starting to smelt; continuing to smelt for 10 minutes after the iron rod is completely smelted, adjusting the power to 360KW, and refining for 5 minutes; when the alloy liquid level is silver white, casting to obtain a cast sheet;
(3) hydrogen crushing: putting the cast sheet into a hydrogen crushing furnace, absorbing hydrogen until the cast sheet is saturated, and then heating the cast sheet to 550 ℃ for dehydrogenation until the temperature is lower than 20Pa to obtain coarse powder;
(4) milling: adding 0.105kg of antioxidant into 105kg of coarse powder, firstly carrying out oxygen discharge on an air flow mill until the oxygen concentration is less than or equal to 5ppm, then grinding the coarse powder into fine powder under the condition of no oxygen supplement, and then adding 0.105kg of lubricant into the fine powder; the volume average particle diameter SMD of the fine powder is 2.8 mu m and the particle size distribution ratio (X90/X10) is less than or equal to 5.0 measured by a Newpatakg laser particle size tester;
(5) and (3) testing the oxygen content: the powder obtained from step (4)Weighing 5kg of sample, molding, isostatic pressing, sintering and tempering to obtain a neodymium-iron-boron magnet sample, measuring the oxygen content (w) in the sample by an IRO-II type oxygen measuring instrument at the central part of the sample1) The result was 0.043%; wherein, the molding, isostatic pressing, sintering and tempering processes are the same as the steps (7) - (9);
(6) adding water and stirring: according to M x (w)0-w1) X 18/16 calculation of Water addition, wherein, target oxygen content (w)0) 0.4 percent, and the weight (M) of the sampled fine powder is 100kg, then 0.402kg of water is added into the fine powder, and the fine powder and the water are stirred for 8 hours on a three-dimensional American-like stirrer to be fully and uniformly mixed;
(7) molding: ensuring that the oxygen content of the seal box is less than 0.05 percent under the protection of nitrogen, and molding the powder in a mold with a magnetic field of a press machine more than 1.5T to obtain the molding density of 3.8g/cm3The green compact of (a);
(8) isostatic pressing: wrapping the green body with plastic film, vacuum packaging, placing into isostatic press, performing isostatic pressing treatment under 200MPa oil pressure to further increase the density of the green body to 4.7g/cm3；
(9) Sintering and tempering: removing vacuum bag and film under nitrogen protection, placing in a graphite box, placing in a furnace, and vacuumizing to 5.0 × 10-1Heating to 850 deg.C below Pa, maintaining for 4 hr, and reducing vacuum degree to 10-1Continuously heating to 1000 ℃ below Pa, and sintering for 8 hours; and cooling the gas filled with argon to below 100 ℃ after sintering, heating the gas filled with argon to 950 ℃, preserving the heat for 2 hours, carrying out primary tempering, cooling the gas filled with argon to below 80 ℃ after heat preservation, heating the gas filled with argon to 500 ℃, preserving the heat for 4 hours, carrying out secondary tempering, cooling the gas filled with argon to below 60 ℃ after heat preservation, and discharging the gas from the furnace.
Comparative example 1
The comparative example provides a method for preparing a sintered neodymium-iron-boron permanent magnet, comprising the following steps:
(1) preparing materials: weighing the following raw materials in percentage by weight: PrNd: 29 wt%, Ho: 4 wt%, B: 0.94 wt%, Al: 0.9 wt%, Cu: 0.2 wt%, Co: 0.2 wt%, Ga: 0.1 wt%, Zr: 0.1 wt%, the balance being Fe;
(2) smelting: sequentially loading finely crushed materials such as iron bars, ferroboron and the like and praseodymium-neodymium into a crucible of a rapid hardening furnace, vacuumizing the rapid hardening furnace to below 1Pa, starting to dry the materials, setting the power of the drying to be 100KW, setting the time to be 10 minutes, filling argon to-0.065 MPa when the vacuum degree is lower than 3Pa, increasing the power to 500KW, and starting to smelt; continuing to smelt for 10 minutes after the iron rod is completely smelted, adjusting the power to 360KW, and refining for 5 minutes; when the alloy liquid level is changed into silvery white, casting to obtain a cast sheet;
(3) hydrogen crushing: putting the cast sheet into a hydrogen crushing furnace, absorbing hydrogen until the cast sheet is saturated, and then heating the cast sheet to 550 ℃ for dehydrogenation until the temperature is lower than 20Pa to obtain coarse powder;
(4) milling: adding 0.105kg of antioxidant into 105kg of coarse powder, firstly carrying out oxygen discharge on an air flow mill until the oxygen concentration is less than or equal to 5ppm, then grinding the coarse powder into fine powder under the condition of no oxygen supplement, and then adding 0.105kg of lubricant into the fine powder; the volume average particle diameter SMD of the fine powder is 2.5 mu m and the particle size distribution ratio (X90/X10) is less than or equal to 5.0 measured by a Newpatakg laser particle size tester;
(5) molding: ensuring that the oxygen content of the seal box is less than 0.05 percent under the protection of nitrogen, and molding the powder in a mold with a magnetic field of a press machine more than 1.5T to obtain the molding density of 3.9g/cm3The green compact of (a);
(6) isostatic pressing: wrapping the green body with plastic film, vacuum packaging, placing into isostatic pressing machine, performing isostatic pressing under 200MPa oil pressure to further increase the density of the green body to 4.6g/cm3；
(7) Sintering and tempering: removing vacuum bag and film under nitrogen protection, placing in a graphite box, placing in a furnace, and vacuumizing to 5.0 × 10-1Heating to 850 deg.C below Pa, maintaining for 4 hr, and reducing vacuum degree to 10-1Continuously heating to 1000 ℃ below Pa, and sintering for 8 hours; and after sintering, cooling the gas filled with argon to be below 100 ℃, heating to 920 ℃, preserving heat for 3 hours, carrying out primary tempering, cooling the gas filled with argon to be below 80 ℃ after heat preservation, heating to 460 ℃, preserving heat for 5 hours, carrying out secondary tempering, cooling the gas filled with argon to be below 60 ℃ after heat preservation, and discharging.
Comparative example 2
The comparative example provides a method for preparing a sintered neodymium-iron-boron permanent magnet, comprising the following steps:
(1) preparing materials: weighing the following raw materials in percentage by weight: PrNd: 29 wt%, Ho: 4 wt%, B: 0.94 wt%, Al: 0.9 wt%, Cu: 0.2 wt%, Co: 0.2 wt%, Ga: 0.1 wt%, Zr: 0.1 wt%, the balance being Fe;
(2) smelting: sequentially loading finely crushed materials such as iron bars, ferroboron and the like and praseodymium-neodymium into a crucible of a rapid hardening furnace, vacuumizing the rapid hardening furnace to below 1Pa, starting to dry the materials, setting the power of the drying to be 100KW, setting the time to be 10 minutes, filling argon to-0.065 MPa when the vacuum degree is lower than 3Pa, increasing the power to 500KW, and starting to smelt; continuing to smelt for 10 minutes after the iron rod is completely smelted, adjusting the power to 360KW, and refining for 5 minutes; the surface of the strip alloy liquid turns silvery white, and a casting sheet is obtained by casting;
(3) hydrogen crushing: putting the cast sheet into a hydrogen crushing furnace, absorbing hydrogen until the cast sheet is saturated, and then heating to 550 ℃ for dehydrogenation until the temperature is lower than 20Pa to obtain coarse powder;
(4) powder preparation: adding 0.105kg of antioxidant into 105kg of coarse powder, performing jet milling to prepare powder, injecting pure oxygen into the jet mill in the process, wherein the supplement amount of the pure oxygen is 1.0-3.0L/h, and adding 0.105kg of lubricant into the prepared fine powder; the volume average particle diameter SMD of the fine powder is 2.7 mu m and the particle size distribution ratio (X90/X10) is less than or equal to 5.0 measured by a Newpatakg laser particle size tester;
(5) molding: ensuring that the oxygen content of the seal box is less than 0.05 percent under the protection of nitrogen, and molding the powder in a mold with a magnetic field of a press machine more than 1.5T to obtain the molding density of 3.8g/cm3Green compacts of (4);
(6) isostatic pressing: wrapping the green body with plastic film, vacuum packaging, placing into isostatic pressing machine, performing isostatic pressing under 200MPa oil pressure to further increase the density of the green body to 4.5g/cm3；
(7) Sintering and tempering: removing vacuum bag and film under nitrogen protection, placing in a graphite box, placing in a furnace, and vacuumizing to 5.0 × 10-1Heating to 850 deg.C below Pa, maintaining for 4 hr, and reducing vacuum degree to 10-1Continuously heating to 1000 ℃ below Pa, and sintering for 8 hours; after sintering, filling argon gas for cooling toHeating to 920 ℃ below 100 ℃, preserving heat for 3 hours for primary tempering, cooling to 80 ℃ below by filling argon after heat preservation, heating to 460 ℃ and preserving heat for 5 hours for secondary tempering, cooling to 60 ℃ below by filling argon after heat preservation, and discharging.
Measurement of remanence B of sintered NdFeB magnets of examples 1 to 3 and comparative examples 1 to 2 with QT-800 fully automatic permanent magnet characteristic Rapid testerr(kGs) coercive force Hcj(kOe), maximum magnetic energy product (BH)max(MGOe) and the squareness Hk/Hcj of the extrapolation curve, the test results are shown in Table 1.
TABLE 1 magnetic Properties of NdFeB magnets of examples 1-3 and comparative examples 1-2
From the above results, it can be seen that the coercivity of the sintered nd-fe-b permanent magnet prepared in the embodiment of the present invention is significantly higher than that of the permanent magnets in comparative examples 1-2, and Hk/HcjAnd higher. Therefore, the method ensures that the oxygen content in the prepared neodymium iron boron magnet is stable and uniformly distributed through an effective oxygen control technology, so that the consistency of the magnet is better, and the overall performance of the neodymium iron boron permanent magnet is obviously improved.
The technical solutions claimed in the above embodiments are not exhaustive in terms of their values within the parameters and the equivalent substitutions for a single or multiple features in the technical solutions of the embodiments are also within the scope of the invention, and all the parameters involved in the technical solutions of the invention have no mutually exclusive combinations unless otherwise specified.
The specific embodiments described herein are merely illustrative of the spirit of the invention and do not limit the scope of the invention. Various modifications or additions may be made to the described embodiments or alternatives may be employed by those skilled in the art without departing from the spirit or ambit of the invention as defined in the appended claims.
Claims (7)
1. An oxygen control preparation method of a sintered neodymium iron boron permanent magnet is characterized by comprising the steps of preparing materials, smelting and carrying out hydrogen crushing to obtain coarse powder, adding an antioxidant into the coarse powder, carrying out airflow milling to prepare powder under the condition of no oxygen supplementation to obtain fine powder, then adding a lubricant, sampling to test the oxygen content in the fine powder, adding water into the fine powder, uniformly stirring to obtain powder, and carrying out forming, isostatic pressing, sintering and tempering to obtain the neodymium iron boron permanent magnet; the amount of water added was calculated as follows: m × (B)w 0 -w 1 ) X 18/16; wherein M is the weight of the fine powder,w 0 in order to obtain the target oxygen content,w 1 is the oxygen content in the fine powder, andw 1 ≤w 0 。
2. the method for preparing the sintered NdFeB permanent magnet according to claim 1, wherein the jet mill is subjected to oxygen discharge until the oxygen concentration is not more than 5ppm before the powder is milled by the jet mill.
3. The method for preparing the sintered NdFeB permanent magnet according to claim 1, wherein the average particle diameter (SMD) of the fine powder is 2.5-3.0 μm, and the particle size distribution ratio is not more than (X90/X10) 5.0.
4. The method for preparing the sintered NdFeB permanent magnet according to claim 1, wherein in the process of milling the powder by the jet mill, the addition amount of the antioxidant is 0.05-0.2% of the weight of the coarse powder, and the addition amount of the lubricant is 0.05-0.2% of the weight of the fine powder.
5. The method for preparing the sintered NdFeB permanent magnet according to claim 1, wherein the molding specifically comprises: and under the nitrogen atmosphere, placing the powder in a magnetic field of a press with the temperature of more than 1.5T, and performing orientation forming to obtain a green body.
6. The method for preparing the sintered NdFeB permanent magnet according to claim 5, wherein the oxygen content of the nitrogen atmosphere is controlled to be less than 0.05% during the forming process.
7. A sintered ndfeb permanent magnet characterized in that it is produced by the method of claim 1.
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