CN114551077B - Method for optimizing microstructure of sintered NdFeB magnet - Google Patents
Method for optimizing microstructure of sintered NdFeB magnet Download PDFInfo
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- CN114551077B CN114551077B CN202111573870.4A CN202111573870A CN114551077B CN 114551077 B CN114551077 B CN 114551077B CN 202111573870 A CN202111573870 A CN 202111573870A CN 114551077 B CN114551077 B CN 114551077B
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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
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- 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
-
- 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
- H01F41/0286—Trimming
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
Abstract
The utility model discloses a method for optimizing sintered neodymium-iron-boron magnet microstructure, which comprises the steps of crushing an original cast piece in a mechanical crushing mode, crushing the original cast piece to an ideal size, obtaining a crushed cast piece with length and width being larger than 1mm and smaller than 10mm in any direction, separating out the original cast piece with large thickness (with thickness being more than 0.5 mm), sieving and sorting hydrogen crushed coarse powder obtained after hydrogen crushing successively, separating out coarse powder exceeding a certain size range, and improving the particle size distribution of fine powder after subsequent grinding; the method has the advantages that impurities with large size can be filtered out, impurities with smaller size can be filtered out, the degree of crushing after hydrogen absorption is different based on different microstructure cast pieces, coarse powder with different sizes obtained by crushing the separated cast pieces after hydrogen absorption is different, and therefore the effect of separating cast pieces with different microstructures is achieved, and the microstructure optimizing effect is good.
Description
Technical Field
The utility model relates to a method for optimizing a sintered NdFeB magnet, in particular to a method for optimizing the microstructure of the sintered NdFeB magnet.
Background
The neodymium-iron-boron permanent magnet material has been vigorously developed for nearly 40 years, the application field is continuously expanded, and the neodymium-iron-boron permanent magnet material has a great supporting effect on the development of green energy sources from a voice coil motor, a nuclear magnetic resonance imager, a driving motor and an industrial motor, especially for nearly ten years. However, in order to realize efficient energy conversion, the technical magnetic performance requirements on the neodymium iron boron permanent magnet material are also higher and higher. The technical magnetic performance of the sintered NdFeB permanent magnet is a magnetic parameter sensitive to a microstructure, and good technical magnetic performance cannot be obtained without meeting the required microstructure. That is to say, under the same condition, different technologies are adopted, the microstructure of the sintered NdFeB permanent magnet is different, and the technical magnetic performance can be greatly changed.
The sintered NdFeB permanent magnet is prepared by smelting, hydrogen crushing, grinding, forming, sintering and the like, and the material forms a scaly cast sheet with a certain microstructure after smelting, however, the microstructure consistency of the cast sheet is very poor under the restrictions of the flow of molten liquid, cooling conditions and the like in the casting process, and meanwhile, impurities such as a crucible, furnace dust, slag and the like are accompanied in the cast sheet, so that the obtaining of the high-performance sintered NdFeB permanent magnet is greatly restricted.
In order to obtain an ideal microstructure, thereby obtaining the sintered NdFeB permanent magnet with high remanence, high intrinsic coercivity and high magnetic energy product, the process from casting sheet to powder must be considered how to obtain crystal grains with consistent size. Because of the difference of casting sheets in casting and cooling processes, the obtained casting sheets are inconsistent in size, the microstructure of the casting sheets is also greatly different due to cooling at different positions of a copper roller, the casting sheets with poor microstructure are required to be filtered, and non-NdFeB impurities such as furnace dust, slag and the like in the production process are also filtered from the casting sheets.
Currently, many methods for improving the microstructure of sintered neodymium-iron-boron permanent magnets are presented. For example, a crushing and sorting device for original neodymium iron boron cast sheets disclosed in chinese patent publication No. CN 111701654A (hereinafter referred to as utility model 1), a sintered neodymium iron boron coarse powder screening device disclosed in chinese patent publication No. CN 205673045U (hereinafter referred to as utility model 2), an air mill suitable for neodymium iron boron alloy disclosed in chinese patent publication No. CN 112138827a and a method for using the same (hereinafter referred to as utility model 3). According to the utility model, a cast sheet crushing and sorting mode is adopted, cast sheets are crushed firstly, then cast sheets with different sizes and weights are subjected to vibration mode, and meanwhile, a soot blowing mechanism is added, so that nonmetallic impurities in the cast sheets are reduced, and the difference of microstructure consistency of the cast sheets is ignored. The coarse powder sieving device of utility model 2 is added to the upper part of the air flow mill bin, and can filter coarse powder and impurity with larger size, but omits coarse powder and impurity with very small size. In the utility model 3, when grinding, a mechanism of a rotary turntable is adopted to realize automatic nozzle replacement and reduce contact between a grinding chamber and air. Both utility model 1 and utility model 2 have been invented from the standpoint of filtering impurities which are not favorable for obtaining high-performance magnets, but have certain unilaterality, because the size of the impurities is uncontrollable, i.e. crucible fragments, slag and the like with larger sizes exist, and furnace dust with smaller sizes and slag at the end of casting also exist, the problems cannot be well solved by the above two patents. In addition, the two patents neglect that the microstructure consistency of the cast sheet is poor due to the melt flow difference in the casting process and the difference in the cooling process at different positions of the copper roller, and the difference has an important influence on obtaining high-performance magnets. While the utility model 3 can avoid the risk of mixing impurities in the powder during the pulverizing stage, the impurities that have been mixed into the coarse powder before the pulverizing stage cannot be removed. Therefore, the three patents can filter impurities in the casting stage or filter impurities in the powder stage, but the filtering effect is limited, so that the microstructure optimization effect of the sintered NdFeB magnet is poor.
Disclosure of Invention
The utility model aims to solve the technical problem of providing the method for optimizing the microstructure of the sintered NdFeB magnet, which not only can filter out impurities with large size, but also can filter out impurities with smaller size, is based on different abilities of the cast pieces with different microstructures to absorb hydrogen, and has different crushing degrees after absorbing hydrogen.
The technical scheme adopted for solving the technical problems is as follows: a method of optimizing the microstructure of a sintered neodymium-iron-boron magnet, comprising the steps of:
step (1), smelting and casting raw materials required for preparing a sintered NdFeB magnet to prepare an original cast sheet;
crushing the original cast sheet obtained in the step (1) in a mechanical crushing mode to obtain a crushed cast sheet with the length and the width being more than 1mm and less than 10mm, and simultaneously primarily filtering out impurities in the crushed cast sheet and the crushed cast sheet with the thickness being more than 0.5mm to obtain a primary filtering cast sheet;
step (3), the primary filtering casting pieces are subjected to hydrogen crushing by using a rotary hydrogen crushing furnace to obtain hydrogen crushing coarse powder with the particle size ranging from 3 mu m to 2000 mu m, wherein the obtained hydrogen crushing coarse powder comprises the following coarse powder: coarse powder composed of finely divided coarse powder and furnace dust, coarse powder composed of rare earth-rich phase particles, coarse powder with a microstructure of dendrites, coarse powder composed of impurity particles, coarse powder composed of spherical particles with a poor microstructure, and other coarse powder; wherein, the grain size of coarse powder composed of fine coarse powder and furnace dust is less than 70 μm, the coarse powder with microstructure of dendrite is in the form of cast piece which is insufficiently hydrogen crushed, and is still in the form of scale, the length or width is more than 1mm and less than 10mm, but the thickness is less than 0.5mm, spherical particles with poor microstructure are crushed due to the failure of hydrogen absorption, and the size is more than 1mm;
screening the hydrogen crushed coarse powder through a 200-mesh screen, filtering coarse powder with the particle size lower than 70 mu m to obtain first screened coarse powder, screening the first screened coarse powder through a 16-mesh screen, filtering coarse powder with the particle size lower than 1000 mu m to obtain second screened coarse powder, marking the coarse powder filtered at the moment as coarse powder A, screening the second screened coarse powder through a roller with a gap of 0-1mm, filtering coarse powder with the particle size larger than 1000 mu m and spherical particles and impurities with the diameter larger than 1000 mu m, dropping coarse powder and impurities with the thickness direction smaller than 1000 mu m from gaps of the roller, marking the dropped coarse powder as separated coarse powder, re-separating the separated coarse powder through a rotary magnetic roller, marking the residual coarse powder after impurity filtering as coarse powder B, wherein the coarse powder A and the coarse powder B are powder of sintered neodymium iron boron magnets.
Compared with the prior art, the utility model has the advantages that the original cast piece is crushed by adopting a mechanical crushing mode, so that the original cast piece is crushed to an ideal size, the crushed cast piece with the length and the width being larger than 1mm and smaller than 10mm is obtained, the problem that the subsequent hydrogen absorption crushing is insufficient due to the fact that the original cast piece is too large in size is solved, good conditions are created for the subsequent hydrogen crushing, meanwhile, the original cast piece with large thickness (more than 0.5mm in thickness) is separated out, the original cast piece with the similar ingot with the large thickness and poor grain boundary distribution is prevented from influencing the microstructure of the sintered neodymium-iron-boron magnet after forming powder, the crushing degree is different due to the fact that the cast pieces with different microstructures have different hydrogen absorption capacities, the effect of separating the crushed coarse powder with different microstructures is realized by sieving and sorting, the problem that impurities are contained in the original cast piece is solved, the non-ferromagnetic substances except neodymium-rich phase are doped in the magnet, meanwhile, coarse powder exceeding a certain size range is separated, the grain size distribution of the subsequent sintered neodymium-iron-boron magnet is improved, and the sintered neodymium-boron fine powder is obtained, and the sintered neodymium-iron-boron fine powder has good particle size distribution is optimized.
Drawings
FIG. 1 is a schematic diagram of a hydrogen kibble sifting and sorting process in a method of optimizing sintered NdFeB magnet microstructure according to the present utility model;
FIG. 2 is a magnet microstructure diagram of test group one in an embodiment of the method of optimizing sintered NdFeB magnet microstructure of the present utility model;
FIG. 3 is a magnet microstructure diagram of test group two in an embodiment of the method of optimizing sintered NdFeB magnet microstructure of the present utility model;
fig. 4 is a magnet microstructure diagram of a control group in an embodiment of the method of optimizing sintered neodymium-iron-boron magnet microstructure of the utility model.
Detailed Description
The utility model is described in further detail below with reference to the embodiments of the drawings.
Examples: a method of optimizing the microstructure of a sintered neodymium-iron-boron magnet, comprising the steps of:
step (1), smelting and casting raw materials required for preparing a sintered NdFeB magnet to prepare an original cast sheet;
crushing the original cast sheet obtained in the step (1) in a mechanical crushing mode to obtain a crushed cast sheet with the length and the width being more than 1mm and less than 10mm, and simultaneously primarily filtering out impurities in the crushed cast sheet and the crushed cast sheet with the thickness being more than 0.5mm to obtain a primary filtering cast sheet;
step (3), the primary filtering casting pieces are subjected to hydrogen crushing by using a rotary hydrogen crushing furnace to obtain hydrogen crushing coarse powder with the particle size range of 3-2000 mu m, the rotary hydrogen crushing furnace rotates for 3min and stands for 10min for circulation until the hydrogen absorption times reach more than 40 times, and the obtained hydrogen crushing coarse powder comprises the following coarse powder: coarse powder composed of finely divided coarse powder and furnace dust, coarse powder composed of rare earth-rich phase particles, coarse powder with a microstructure of dendrites, coarse powder composed of impurity particles, coarse powder composed of spherical particles with a poor microstructure, and other coarse powder; wherein, the grain size of coarse powder composed of fine coarse powder and furnace dust is less than 70 μm, the coarse powder with microstructure of dendrite is in the form of cast piece which is insufficiently hydrogen crushed, and is still in the form of scale, the length or width is more than 1mm and less than 10mm, but the thickness is less than 0.5mm, spherical particles with poor microstructure are crushed due to the failure of hydrogen absorption, and the size is more than 1mm;
screening the hydrogen crushed coarse powder through a 200-mesh screen, filtering coarse powder with the particle size lower than 70 mu m to obtain first screened coarse powder, screening the first screened coarse powder through a 16-mesh screen, filtering coarse powder with the particle size lower than 1000 mu m to obtain second screened coarse powder, marking the coarse powder filtered at the moment as coarse powder A, screening the second screened coarse powder through a roller with a gap of 0-1mm, filtering coarse powder with the particle size larger than 1000 mu m and spherical particles and impurities with the diameter larger than 1000 mu m, dropping coarse powder and impurities with the thickness direction smaller than 1000 mu m from gaps of the roller, marking the dropped coarse powder as separated coarse powder, re-separating the separated coarse powder through a rotary magnetic roller, marking the residual coarse powder after impurity filtering as coarse powder B, wherein the coarse powder A and the coarse powder B are powder of sintered neodymium iron boron magnets.
The coarse powder A and the coarse powder B prepared by the method for optimizing the microstructure of the sintered NdFeB magnet respectively prepare a high-remanence magnet N58, wherein the high-remanence magnet N58 prepared by the coarse powder A is used as a test group I, and the high-remanence magnet N58 prepared by the coarse powder B is used as a test group II. In order to embody the superiority of the method for optimizing the microstructure of the sintered NdFeB magnet, a control group is arranged, coarse powder adopted by the control group is marked as coarse powder C, and the coarse powder C is hydrogen crushed coarse powder obtained by smelting and hydrogen crushing under the same conditions as those of the test group.
Feeding coarse powder A, coarse powder B and coarse powder C into an air flow mill respectively to finish grinding to obtain powder A, powder B and powder C respectively, forming and sintering the powder A, the powder B and the powder C under the same technological conditions to obtain high-remanence magnets N58 respectively, and then detecting magnetic properties of the three obtained high-remanence magnets N58 respectively under the same conditions, wherein magnetic property detection data are shown in table 1:
TABLE 1
Analysis of table 1 shows that: the combined magnetic properties of the high remanence magnets N58 of the first and second test groups are better than those of the high remanence magnet N58 of the control group, and the combined magnetic properties of the high remanence magnet N58 of the first test group are optimal.
The microstructure of the high remanence magnet N58 of the first test group and the high remanence magnet N58 of the second test group and the microstructure of the high remanence magnet N58 of the control group are observed by adopting a scanning electron microscope, wherein the microstructure of the high remanence magnet N58 of the first test group is shown in fig. 2, the microstructure of the high remanence magnet N58 of the second test group is shown in fig. 3, and the microstructure of the high remanence magnet N58 of the control group is shown in fig. 4. Analysis of fig. 2 shows that: the high remanence magnet N58 of the test group I has uniform grain size, uniform neodymium-rich phase distribution, no non-neodymium-iron-boron impurities and excellent microstructure. Analysis of fig. 3 shows that: although part of neodymium-rich phases are agglomerated at the grain boundary, non-neodymium-iron-boron impurities are not present, and the whole microstructure is good. Analysis of fig. 4 shows that: some non-neodymium-iron-boron impurities are entrained inside the magnet, resulting in a relatively poor microstructure. Therefore, the method for optimizing the microstructure of the sintered NdFeB magnet can obviously improve the microstructure of the sintered NdFeB magnet and improve the comprehensive magnetic performance of the sintered NdFeB magnet.
Claims (1)
1. The method for optimizing the microstructure of the sintered NdFeB magnet is characterized by comprising the following steps of:
step (1), smelting and casting raw materials required for preparing a sintered NdFeB magnet to prepare an original cast sheet;
crushing the original cast sheet obtained in the step (1) in a mechanical crushing mode to obtain a crushed cast sheet with the length and the width being more than 1mm and less than 10mm, and simultaneously primarily filtering out impurities in the crushed cast sheet and the crushed cast sheet with the thickness being more than 0.5mm to obtain a primary filtering cast sheet;
step (3), the primary filtering casting pieces are subjected to hydrogen crushing by using a rotary hydrogen crushing furnace to obtain hydrogen crushing coarse powder with the particle size ranging from 3 mu m to 2000 mu m, wherein the obtained hydrogen crushing coarse powder comprises the following coarse powder: coarse powder composed of finely divided coarse powder and furnace dust, coarse powder composed of rare earth-rich phase particles, coarse powder with a microstructure of dendrites, coarse powder composed of impurity particles, coarse powder composed of spherical particles with a poor microstructure, and other coarse powder; wherein, the grain size of coarse powder composed of fine coarse powder and furnace dust is less than 70 μm, the coarse powder with microstructure of dendrite is in the form of cast piece which is insufficiently hydrogen crushed, and is still in the form of scale, the length or width is more than 1mm and less than 10mm, but the thickness is less than 0.5mm, spherical particles with poor microstructure are crushed due to the failure of hydrogen absorption, and the size is more than 1mm;
screening the hydrogen crushed coarse powder through a 200-mesh screen, filtering coarse powder with the particle size lower than 70 mu m to obtain first screened coarse powder, screening the first screened coarse powder through a 16-mesh screen, filtering coarse powder with the particle size lower than 1000 mu m to obtain second screened coarse powder, marking the coarse powder filtered at the moment as coarse powder A, screening the second screened coarse powder through a roller with a gap of 0-1mm, filtering coarse powder with the particle size larger than 1000 mu m and spherical particles and impurities with the diameter larger than 1000 mu m, dropping coarse powder and impurities with the thickness direction smaller than 1000 mu m from gaps of the roller, marking the dropped coarse powder as separated coarse powder, re-separating the separated coarse powder through a rotary magnetic roller, marking the residual coarse powder after impurity filtering as coarse powder B, and marking the coarse powder A and the coarse powder B as powder of sintered NdFeB magnets.
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