CN112435820A - High-performance sintered neodymium-iron-boron magnet and preparation method thereof - Google Patents
High-performance sintered neodymium-iron-boron magnet and preparation method thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 15
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- 239000006247 magnetic powder Substances 0.000 claims abstract description 55
- 238000005245 sintering Methods 0.000 claims abstract description 46
- 238000005266 casting Methods 0.000 claims abstract description 36
- 230000008719 thickening Effects 0.000 claims abstract description 34
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000001257 hydrogen Substances 0.000 claims abstract description 32
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- 238000005496 tempering Methods 0.000 claims abstract description 22
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- 229910052802 copper Inorganic materials 0.000 claims description 15
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- 229910052733 gallium Inorganic materials 0.000 claims description 6
- 229910052684 Cerium Inorganic materials 0.000 claims description 3
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- 229910000905 alloy phase Inorganic materials 0.000 description 1
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- LGQXXHMEBUOXRP-UHFFFAOYSA-N tributyl borate Chemical compound CCCCOB(OCCCC)OCCCC LGQXXHMEBUOXRP-UHFFFAOYSA-N 0.000 description 1
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 1
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
- B22F3/04—Compacting only by applying fluid pressure, e.g. by cold isostatic pressing [CIP]
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1017—Multiple heating or additional steps
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
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- B22F9/00—Making metallic powder or suspensions thereof
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- B22F9/023—Hydrogen absorption
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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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
- H01F1/0555—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 pressed, sintered or bonded together
- H01F1/0557—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 pressed, sintered or bonded together sintered
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- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
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- 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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- 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
- H01F41/0266—Moulding; Pressing
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- B22—CASTING; POWDER METALLURGY
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/044—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by jet milling
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Abstract
The invention provides a preparation method of a high-performance sintered neodymium-iron-boron magnet, which comprises the following steps: (1) preparing raw materials according to the composition of the matrix alloy A, and smelting and casting the raw materials to obtain a casting sheet A; filling hydrogen into the cast piece A for crushing, sieving in an inert atmosphere to obtain coarse crushed powder A, and then grinding in an airflow mill protected by the inert atmosphere to obtain airflow mill magnetic powder A; (2) preparing raw materials according to the components of the grain boundary thickening alloy B, and smelting and casting the raw materials to obtain an ingot B; filling hydrogen into the cast ingot B for crushing, sieving in an argon protection box to obtain coarse crushed powder B, and then grinding in an airflow mill under the protection of argon atmosphere to obtain airflow mill magnetic powder B; (3) mixing the jet mill magnetic powder A and the jet mill magnetic powder B, adding a lubricant, stirring for 2-6 hours, then performing orientation molding, and performing isostatic pressing; (4) the blank after isostatic pressing treatment enters a sintering furnace, is subjected to dehydrogenation treatment, and then is subjected to presintering, high-temperature sintering and tempering heat treatment.
Description
Technical Field
The invention belongs to the field of rare earth permanent magnet material preparation, and relates to a high-performance sintered neodymium-iron-boron magnet and a preparation method thereof.
Background
Since the sintered neodymium iron boron appeared in 1983, the sintered neodymium iron boron is widely applied to the fields of IT, medical treatment, household appliances, new energy automobiles and the like due to the excellent magnetic property. With the development of the market, the sintered nd-fe-b magnet is required to have high magnetic property and high heat resistance, that is, the magnet is required to have a high maximum energy product and a high intrinsic coercive force. Therefore, it becomes a hot spot in technical research and development to improve the coercive force of the magnet while ensuring the magnetism of the magnet.
In the industry, a method for improving the coercive force by partially replacing Nd in an original magnet by using heavy rare earth metal elements such as Dy or Tb and the like can obtain the obviously improved coercive force, but the Dy or Tb can enter a main phase to greatly reduce the magnetism of the magnet while improving the coercive force along with the increase of the replacement amount of the Dy or Tb; on the other hand, heavy rare earth metals such as Dy and Tb are more expensive than Nd, and therefore, partial substitution of Nd with Dy or Tb also increases the cost of the magnet. In order to overcome the defects, in recent years, heavy rare earth is distributed at the crystal grain boundary of the magnet by a thermal diffusion mode of the sintered magnet crystal grain boundary, so that the aim of improving the coercive force can be achieved by using a small amount of Dy and Tb, and the magnetic property of the magnet is reduced little. However, the grain boundary diffusion technology exists: 1. the large-scale production technology is difficult, expensive equipment needs to be configured, and corresponding technical support is needed; 2. the method has the limit to the size of the magnet and is not suitable for producing large-block magnets. Therefore, research on more suitable technology is needed to prepare the ndfeb magnet in the cost-effective and full-application field.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a high-performance sintered neodymium iron boron magnet and a preparation method thereof.
The invention provides a high-performance sintered neodymium-iron-boron magnet, which is prepared from the raw materials of a matrix alloy A and a grain boundary thickening alloy B;
the composition component of the base alloy A is RxTyMzB(1-x-y-z)Wherein R is one or more of Nd, Pr, La, Ce, Dy and Tb, M is one or more of Cu, Al and Ga and one or two of Nb and Zr, T is Fe and Co, and the mass ratio of Fe to Co is (40-100): 1, x is 28 to 33 wt%, y is 58 to 72 wt%, and z is 0 to 2.0 wt%.
The component R of the alloy B with thickened grain boundaryxM(1-x), wherein R is one or more of Nd, Pr, Dy and Tb, M is one or more of Cu, Al and Ga, and x is 80-95 wt%.
The invention provides a preparation method of the high-performance sintered neodymium-iron-boron magnet, which comprises the following steps:
(1) preparing raw materials according to the composition of the matrix alloy A, and smelting and casting the raw materials by adopting a rapid hardening process to obtain a cast piece A; placing the cast piece A in a hydrogen breaking furnace, filling hydrogen for breaking, sieving in inert atmosphere to obtain coarse broken powder A, and then grinding the coarse broken powder A in an airflow mill protected by inert atmosphere to obtain airflow mill magnetic powder A;
(2) preparing raw materials according to the components of the grain boundary thickening alloy B, and smelting and casting the raw materials to obtain an ingot B; placing the ingot B in a hydrogen breaking furnace, filling hydrogen for breaking, sieving in an argon protection box to obtain coarse broken powder B, and then grinding the coarse broken powder B in a jet mill protected by argon atmosphere to obtain jet mill magnetic powder B;
(3) mixing the jet mill magnetic powder A and the jet mill magnetic powder B, adding a lubricant, stirring for 2-6 hours, then carrying out orientation molding in an inert atmosphere, and then carrying out isostatic pressing treatment;
(4) and (3) feeding the blank subjected to isostatic pressing treatment into a sintering furnace, preserving heat for 2-5 hours at 550-600 ℃ for dehydrogenation treatment, and then performing presintering, high-temperature sintering and tempering heat treatment.
The smelting temperature of the step (1) and the step (2) is 1450-1500 ℃, and the casting temperature is 1400-1450 ℃; when the rapid hardening process is adopted, the rotating speed of the copper roller is 1.2-1.5 m/s, and the average thickness of the obtained cast sheet A is 0.2-0.4 mm.
The average particle size of the jet milling magnetic powder A in the step (1) is 4-5 mu m.
The average particle size of the jet milling magnetic powder B in the step (2) is 1-2 μm.
And (4) in the mixture of the jet milling magnetic powder A and the jet milling magnetic powder B in the step (3), the content of the jet milling magnetic powder B is 1-5 wt%.
The magnetic field intensity of the orientation forming in the step (3) is 1.0-1.5T, and the isostatic pressure treatment pressure is 150-220 MPa.
The pre-sintering in the step (4) is carried out at the temperature of 800-1000 ℃ for 10-15 h.
The pre-sintering in the step (4) is carried out for 12-15 h at 850-950 ℃.
The high-temperature sintering temperature in the step (4) is 1030-1100 ℃, and the sintering time is 4-6 h; the tempering heat treatment comprises the following steps: the primary tempering temperature is 800-920 ℃, and the tempering time is 2-4 hours; the secondary tempering temperature is 460-560 ℃, and the tempering time is 4-6 hours.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention adopts double alloy components: the crystal boundary thickening alloy B and the matrix alloy A are respectively cast, crushed and then co-sintered, the crystal boundary thickening alloy B is uniformly and dispersedly distributed around the matrix alloy A crystal grains, the crystal boundary is thickened, the structure and the distribution of the crystal boundary phase of the magnet are regulated, the magnetostatic coupling effect among the crystal grains is reduced, and the performance of the magnet is improved;
(2) according to the invention, the oxidation resistance of the crystal boundary thickening alloy B in the sintering process is effectively improved through the processes of casting the crystal boundary thickening alloy B into an ingot, removing hydrogen after hydrogen crushing, filling argon for protection and the like, and the crystal boundary thickening alloy B is uniformly dispersed around matrix phase crystal grains through pre-sintering, so that the effects of thickening the crystal boundary and improving the performance of a magnet are exerted;
(3) the average particle size of the jet mill magnetic powder B crushed by the crystal boundary thickening alloy B is controlled to be 1-2 mu m, so that the crystal boundary thickness is effectively improved, and the performance of a magnet is improved;
(4) according to the invention, the content of the jet mill magnetic powder B in the mixture of the jet mill magnetic powder A and the jet mill magnetic powder B is controlled to be 1-5 wt%, so that a crystal boundary thickening phase is generated, and components are prevented from entering a matrix phase, thereby effectively improving the performance of the magnet.
Drawings
Fig. 1 is a structural view of a sintered nd-fe-b magnet according to example 1 of the present invention;
FIG. 2 is a structural view of a sintered NdFeB magnet according to a comparative example 3 of the present invention;
Detailed Description
The high-performance sintered ndfeb magnet and the method for manufacturing the same according to the present invention will be described in detail below, and technical terms or scientific terms used at this time have meanings that are generally understood by those skilled in the art of the present invention, if not defined otherwise.
The embodiment of the invention provides a high-performance sintered neodymium-iron-boron magnet, which is prepared from the raw materials of a matrix alloy A and a grain boundary thickening alloy B;
the composition component of the base alloy A is RxTyMzB(1-x-y-z)Wherein R is one or more of Nd, Pr, La, Ce, Dy and Tb, M is one or more of Cu, Al and Ga and one or two of Nb and Zr, T is Fe and Co, and the mass ratio of Fe to Co is (40-100): 1, x is 28 to 33 wt%, y is 58 to 72 wt%, and z is 0 to 2.0wt％。
The component R of the alloy B with thickened grain boundaryxM(1-x)Wherein R is one or more of Nd, Pr, Dy and Tb, M is one or more of Cu, Al and Ga, and x is 80-95 wt%.
The crystal boundary thickening alloy B is uniformly and dispersedly distributed around the crystal grains of the matrix alloy A, so that the crystal boundary is thickened, the magnetostatic coupling effect among the crystal grains is reduced, and the intrinsic coercive force of the magnet is improved.
Another embodiment of the present invention provides a method for preparing a high-performance sintered ndfeb magnet, including the steps of:
(1) preparing raw materials according to the composition of the matrix alloy A, and smelting and casting the raw materials by adopting a rapid hardening process to obtain a cast piece A; placing the cast piece A in a hydrogen breaking furnace, filling hydrogen for breaking, sieving in inert atmosphere to obtain coarse broken powder A, and then grinding the coarse broken powder A in an airflow mill protected by inert atmosphere to obtain airflow mill magnetic powder A;
(2) preparing raw materials according to the components of the grain boundary thickening alloy B, and smelting and casting the raw materials to obtain an ingot B; placing the ingot B in a hydrogen breaking furnace, filling hydrogen for breaking, sieving in an argon protection box to obtain coarse broken powder B, and then grinding the coarse broken powder B in a jet mill protected by argon atmosphere to obtain jet mill magnetic powder B;
(3) mixing the jet mill magnetic powder A and the jet mill magnetic powder B, adding a lubricant, stirring for 2-6 hours, then carrying out orientation molding in an inert atmosphere, and then carrying out isostatic pressing treatment;
(4) and (3) feeding the blank subjected to isostatic pressing treatment into a sintering furnace, preserving heat for 2-5 hours at 550-600 ℃ for dehydrogenation treatment, and then performing presintering, high-temperature sintering and tempering heat treatment.
Herein, the ingot and the cast slab are those conventionally defined in the art, that is, the ingot is obtained by casting the alloy raw material after melting into a water-cooled mold, and the cast slab is obtained by casting the alloy raw material after melting onto a copper roller with a certain rotating speed.
In the invention, the smelting temperature of the step (1) and the step (2) is 1450-1500 ℃, and the casting temperature is 1400-1450 ℃; when the cast sheet is prepared, the rotating speed of a copper roller is 1.2-1.5 m/s, and the average thickness of the prepared cast sheet A is 0.2-0.4 mm; when the thickness of the cast piece is too small, ultrafine crystal grains are easily generated, and when the thickness of the cast piece is too large, the crystal grains are too large and a hetero-phase is generated.
The average thickness of the cast piece is defined herein as the average of the measured data of any 100 cast pieces, and the measuring tool can be a vernier caliper or a micrometer screw.
In the general preparation process of the sintered neodymium iron boron magnet, a casting sheet is cast, and the performance of the magnet is improved by sintering in the form of the casting sheet. The crystal boundary thickening alloy B is cast into an ingot and is co-sintered with the base alloy A in the form of a cast sheet. The reason is that the grain boundary thickening alloy B is a rare earth alloy, is easy to oxidize in the preparation process of the magnet, and can effectively resist oxidation when being cast into an ingot form. In addition, in order to further reduce the oxidation effect of the crystal boundary thickening alloy B, after the ingot B is charged with hydrogen and crushed, dehydrogenation treatment is not carried out, and the hydrogen component of the alloy is kept to better isolate the oxidation caused by the reaction of the alloy and oxygen in the powder preparation process; meanwhile, after being charged with hydrogen and crushed, the ingot B is sieved in an argon protection box and ground in an airflow mill in argon atmosphere, so that the crystal boundary thickening alloy B is not easy to oxidize in argon atmosphere.
In order to ensure the uniform dispersion of the grain boundary thickening alloy B at the grain boundary, the invention carries out a pre-sintering process before high-temperature sintering: and (3) preserving the heat for 10-15 hours at 800-1000 ℃, and preserving the heat for a certain time at the temperature to ensure that the crystal boundary thickening alloy B becomes a liquid phase and fully flows among crystal grains of the matrix phase. The pre-sintering process is preferably carried out at 850-950 ℃ for 12-15 h, so that the activity of crystal grains can be increased, the flow of the liquid phase alloy can be improved, and the crystal grains cannot grow.
The invention effectively improves the oxidation resistance of the crystal boundary thickening alloy B in the sintering process by casting the crystal boundary thickening alloy B into an ingot, removing hydrogen after hydrogen crushing, filling argon for protection and other processes, and uniformly disperses the crystal boundary thickening alloy B around matrix phase crystal grains by pre-sintering, thereby playing the roles of thickening the crystal boundary and improving the performance of a magnet.
And after the grain boundary thickening alloy B is milled by an air jet mill, controlling the average grain size of the air jet mill magnetic powder B to be 1-2 mu m. The average particle size of the jet mill magnetic powder B is controlled based on two points: 1. the thickness of the normal grain boundary phase of the sintered neodymium iron boron magnet is 5-50nm, and the average grain diameter of the sintered neodymium iron boron magnet is larger than the thickness of the normal grain boundary phase as an alloy phase which needs to play a role in thickening the grain boundary; 2. if the average grain size of the grain boundary thickening phase is too large, more grains wrap the same matrix phase grains, resulting in a decrease in the number of matrix phases and a decrease in magnetic properties. Therefore, the average particle size of the jet mill magnetic powder B is controlled to be 1-2 mu m, the grain boundary thickness is effectively improved, and the magnet performance is improved.
Herein, the average particle diameter of the jet-milled magnetic powder is defined as a median diameter of a volume-based particle diameter distribution measured by a laser diffraction scattering method.
And controlling the content of the jet milling magnetic powder B to be 1-5 wt% in the mixture of the jet milling magnetic powder A and the jet milling magnetic powder B. The jet milling magnetic powder B is used for forming a crystal boundary thickening phase, the content is not easy to be excessive, and the excessive content can cause components to enter a matrix phase to reduce the performance of the magnet.
The inert atmosphere of the present invention is nitrogen or argon.
The lubricant of the invention is a lubricant which is conventionally used in the field for sintering neodymium iron boron magnets, such as paraffin, glycerol, silicate ester, silicone oil, stearic acid, zinc stearate, tributyl borate and the like. The addition amount of the lubricant is 0.2-0.5 wt% of the mixture of the jet mill magnetic powder A and the jet mill magnetic powder B.
Hereinafter, the technical solution of the present invention will be further described and illustrated by specific examples and drawings. However, these embodiments are exemplary, and the present disclosure is not limited thereto. Unless otherwise specified, the raw materials used in the following specific examples of the present invention are those commonly used in the art, and the methods used in the examples are those conventional in the art.
Example 1
The preparation method of the sintered neodymium-iron-boron magnet comprises the following steps:
(1) nd according to the composition A of the base alloy28.0Fe69.57Co1.0Cu0.1Al0.1Ga0.2Zr0.05B0.98Proportioning, smelting raw materials by adopting a rapid hardening process, and casting the raw materials on a copper roller with the rotating speed of 1.5m/s to obtain a casting sheet A with the average thickness of 0.3mm, wherein the smelting temperature is 1460 ℃, and the casting temperature is 1420 ℃; placing the cast piece A in a hydrogen breaking furnace, filling hydrogen for breaking, sieving in nitrogen protection to obtain coarse broken powder A with the granularity of less than or equal to 300 mu m, and then grinding the coarse broken powder A in an airflow mill protected by nitrogen atmosphere to obtain airflow mill magnetic powder A with the average particle size of 4 mu m;
(2) according to the constituent Pr of the alloy B with the grain boundary thickened23.75Nd71.25Cu3.0Al2.0Burdening, namely smelting and casting the raw materials into a water-cooled mold to obtain an ingot B, wherein the smelting temperature is 1460 ℃, and the casting temperature is 1410 ℃; placing the ingot B in a hydrogen breaking furnace, filling hydrogen for breaking, sieving in an argon protection box to obtain coarse broken powder B with the granularity of less than or equal to 300 mu m, and then grinding the coarse broken powder B in a jet mill protected by argon atmosphere to obtain jet mill magnetic powder B with the average particle size of 2 mu m;
(3) mixing the jet milling magnetic powder A and the jet milling magnetic powder B according to the mass ratio of 96:4, adding 0.3 wt% of lubricant stearic acid, stirring for 4 hours, then carrying out orientation molding in a magnetic field with the magnetic field intensity of 1.4T in an argon atmosphere, and pressing into a green body in a water isostatic pressing at 200 MPa;
(4) and sintering the green body in a vacuum sintering furnace, preserving heat for 3h at 580 ℃ for dehydrogenation treatment, sintering at 900 ℃ for 15h, heating to 1030 ℃ for sintering for 5h, cooling to room temperature, heating to 900 ℃ for primary tempering for 2.5h, cooling to 500 ℃ for secondary tempering for 4.5h, and preparing the sintered neodymium-iron-boron magnet.
Example 2
The preparation method of the sintered neodymium-iron-boron magnet comprises the following steps:
(1) nd according to the composition A of the base alloy30.0Fe67.3Co1.1Cu0.15Al0.12Nb0.08B1.25Proportioning, smelting raw materials by adopting a rapid hardening process, and casting the raw materials on a copper roller with the rotating speed of 1.5m/s to obtain a casting sheet A with the average thickness of 0.3mm, wherein the smelting temperature is 1480 ℃, and the casting temperature is 1420 ℃; placing the casting sheet A in hydrogenCharging hydrogen into a crushing furnace, crushing, sieving in nitrogen protection to obtain coarse crushed powder A with the particle size of less than or equal to 300 mu m, and then grinding the coarse crushed powder A in a jet mill protected by nitrogen atmosphere to obtain jet mill magnetic powder A with the average particle size of 5 mu m;
(2) dy is the component of alloy B with thickened grain boundary10.65Nd83.35Cu4.0Ga2.0Burdening, namely smelting and casting the raw materials into a water-cooled mold to obtain an ingot B, wherein the smelting temperature is 1460 ℃, and the casting temperature is 1410 ℃; placing the ingot B in a hydrogen breaking furnace, filling hydrogen for breaking, sieving in an argon protection box to obtain coarse broken powder B with the granularity of less than or equal to 300 mu m, and then grinding the coarse broken powder B in a jet mill protected by argon atmosphere to obtain jet mill magnetic powder B with the average particle size of 1 mu m;
(3) mixing the jet milling magnetic powder A and the jet milling magnetic powder B according to the mass ratio of 97:3, adding 0.3 wt% of lubricant stearic acid, stirring for 5 hours, then carrying out orientation molding in a magnetic field with the magnetic field intensity of 1.4T in an argon atmosphere, and pressing into a green body in a water isostatic pressing at 180 MPa;
(4) and sintering the green body in a vacuum sintering furnace, preserving heat for 4h at 560 ℃ for dehydrogenation treatment, sintering at 850 ℃ for 14h, heating to 1040 ℃ for sintering for 4h, cooling to room temperature, heating to 890 ℃ for primary tempering for 2h, cooling to 510 ℃ for secondary tempering for 5h, and preparing the sintered neodymium-iron-boron magnet.
Example 3
Example 3 differs from example 1 only in that the mean particle size of the jet mill magnetic powder B is 4 μm, and other steps are the same and are not repeated here.
Example 4
Example 4 differs from example 1 only in that the jet-milled magnetic powder a and the jet-milled magnetic powder B were mixed at a mass ratio of 92:8, and other steps are the same and are not described herein.
Example 5
The difference between the embodiment 5 and the embodiment 1 is only that the pre-sintering of the embodiment 5 is sintering at 850 ℃ for 8h, and other steps are the same as those of the embodiment 1 and are not repeated herein.
Example 6
The difference between the embodiment 6 and the embodiment 1 is only that the pre-sintering of the embodiment 6 is sintering at 850 ℃ for 18h, and other steps are the same as those of the embodiment 1 and are not repeated herein.
Comparative example 1
Comparative example 1 differs from example 1 only in that the grain boundary thickening alloy B of comparative example 1 was cast into a cast slab according to the rapid solidification process of the matrix alloy a, i.e., according to the composition Pr of the grain boundary thickening alloy B23.75Nd71.25Cu3.0Al2.0And (3) burdening, smelting the raw materials by adopting a rapid hardening process, casting the raw materials on a copper roller with the rotating speed of 1.5m/s to obtain a casting sheet B with the average thickness of 0.3mm, wherein the smelting temperature is 1460 ℃, the casting temperature is 1420 ℃, and other steps are the same as those in the embodiment 1 and are not repeated.
Comparative example 2
The difference between the comparative example 2 and the example 1 is only that the comparative example 2 is not pre-sintered, the temperature is kept at 580 ℃ for 3h for dehydrogenation treatment, then the temperature is directly raised to 1030 ℃ for sintering for 5h, and other steps are the same as those of the example 1 and are not repeated.
Comparative example 3
Comparative example 3 the composition Nd of the base alloy A in example 1 was directly used28.0Fe69.57Co1.0Cu0.1Al0.1Ga0.2Zr0.05B0.98And Dy as the constituent of alloy B with thickened grain boundary10.65Nd83.35Cu4.0Ga2.0Mixing according to the mass ratio of 96:4, namely according to Pr0.950Nd29.730Fe66.787Co0.960Cu0.216Al0.176Ga0.192Zr0.048B0.941The components are proportioned, the raw materials are smelted and cast on a copper roller with the rotating speed of 1.5m/s by adopting a rapid hardening process to obtain a casting sheet with the average thickness of 0.3mm, the smelting temperature is 1460 ℃, and the casting temperature is 1420 ℃; placing the cast piece in a hydrogen breaking furnace, filling hydrogen for breaking, sieving in nitrogen protection to obtain coarse broken powder with the granularity of less than or equal to 300 mu m, and then grinding the coarse broken powder in an airflow mill in nitrogen atmosphere protection to obtain airflow mill magnetic powder with the average particle size of 4 mu m; adding 0.3 wt% of lubricant stearic acid into jet mill magnetic powder, stirring for 4h, and then stirring in argonCarrying out orientation forming in a magnetic field with the magnetic field intensity of 1.4T in the atmosphere, and pressing into a green body in a water isostatic pressing at 200 MPa; and sintering the green body in a vacuum sintering furnace, preserving heat for 3h at 580 ℃ for dehydrogenation treatment, sintering at 900 ℃ for 15h, heating to 1030 ℃ for sintering for 5h, cooling to room temperature, heating to 900 ℃ for primary tempering for 2.5h, cooling to 500 ℃ for secondary tempering for 4.5h, and preparing the sintered neodymium-iron-boron magnet.
Comparative example 4
Comparative example 4 base alloy A composition Nd according to example 2 directly30.0Fe67.3Co1.1Cu0.15Al0.12Nb0.08B1.25And Dy as the constituent of alloy B with thickened grain boundary10.65Nd83.35Cu4.0Ga2.0Mixing according to a mass ratio of 97:3, namely according to Nd31.601Dy0.320Fe65.281Co1.067Cu0.266Al0.116Ga0.06Nb0.078B1.211The components are proportioned, the raw materials are smelted and cast on a copper roller with the rotating speed of 1.5m/s by adopting a rapid hardening process to obtain a casting sheet with the average thickness of 0.3mm, the smelting temperature is 1480 ℃, and the casting temperature is 1420 ℃; placing the cast piece in a hydrogen breaking furnace, filling hydrogen for breaking, sieving in nitrogen protection to obtain coarse broken powder with the granularity of less than or equal to 300 mu m, and then grinding the coarse broken powder in an airflow mill in nitrogen atmosphere protection to obtain airflow mill magnetic powder with the average particle size of 5 mu m; adding 0.3 wt% of lubricant stearic acid into jet mill magnetic powder, stirring for 5h, then carrying out orientation forming in a magnetic field with the magnetic field intensity of 1.4T in the argon atmosphere, and pressing into a green body in a water isostatic pressing at 180 MPa; and sintering the green body in a vacuum sintering furnace, preserving heat for 4h at 560 ℃ for dehydrogenation treatment, sintering at 850 ℃ for 14h, heating to 1040 ℃ for sintering for 4h, cooling to room temperature, heating to 890 ℃ for primary tempering for 2h, cooling to 510 ℃ for secondary tempering for 5h, and preparing the sintered neodymium-iron-boron magnet.
Fig. 1 is a structural view of a sintered ndfeb magnet according to example 1, and fig. 2 is a structural view of a sintered ndfeb magnet according to comparative example 3. As can be seen from fig. 1 and 2, the grain boundaries between the grains of the sintered nd-fe-b magnet of example 1 are uniformly dispersed and have a large thickness, while the grain boundaries of comparative example 3 are non-uniform and have a small thickness.
The sintered nd-fe-b magnets prepared in examples 1-6 and comparative examples 1-4 were measured for magnetic properties using a magnetometer, and the data are shown in table 1 below.
TABLE 1 magnetic Properties of sintered NdFeB magnets of examples 1-6 and comparative examples 1-4
As shown in Table 1, examples 1 and 2 are preferred examples having higher Br, Hcj, (BH) m, Hk/Hcj values; comparative example 1 the grain boundary-thickened alloy B was cast into a cast piece, the oxidation resistance was reduced, and the magnetic properties were reduced; comparative example 2 is not pre-sintered, the grain boundary thickening alloy B is not uniformly dispersed at the grain boundary, the grain boundary thickening effect is greatly reduced, and partial components can enter the matrix phase to reduce the magnetic performance of the magnet; the comparative example 3 and the example 4 directly cast and crush the two alloy components at the same time, so that the grain boundary among the grains of the neodymium iron boron magnet is uneven, the thickness of the grain boundary is smaller, and the magnetic performance is greatly reduced.
The specific embodiments described herein are merely illustrative of the spirit 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 (10)
1. The high-performance sintered neodymium-iron-boron magnet is characterized in that the preparation raw materials of the high-performance sintered neodymium-iron-boron magnet comprise a matrix alloy A and a grain boundary thickening alloy B;
the composition component of the base alloy A is RxTyMzB(1-x-y-z)Wherein R is one or more of Nd, Pr, La, Ce, Dy and Tb, M is one or more of Cu, Al and Ga and one or two of Nb and Zr, T is Fe and Co, and the mass ratio of Fe to Co is (40-100): 1, x is 28-33 wt%, y is 58-72 wt%, and z is 0-2.0 wt%;
the component R of the alloy B with thickened grain boundaryxM(1-x)Wherein R is one or more of Nd, Pr, Dy and Tb, M is one or more of Cu, Al and Ga, and x is 80-95 wt%.
2. The method for preparing a high-performance sintered neodymium-iron-boron magnet according to claim 1, comprising the following steps:
(1) preparing raw materials according to the composition of the matrix alloy A, and smelting and casting the raw materials by adopting a rapid hardening process to obtain a cast piece A; placing the cast piece A in a hydrogen breaking furnace, filling hydrogen for breaking, sieving in inert atmosphere to obtain coarse broken powder A, and then grinding the coarse broken powder A in an airflow mill protected by inert atmosphere to obtain airflow mill magnetic powder A;
(2) preparing raw materials according to the components of the grain boundary thickening alloy B, and smelting and casting the raw materials to obtain an ingot B; placing the ingot B in a hydrogen breaking furnace, filling hydrogen for breaking, sieving in an argon protection box to obtain coarse broken powder B, and then grinding the coarse broken powder B in a jet mill protected by argon atmosphere to obtain jet mill magnetic powder B;
(3) mixing the jet milling magnetic powder A and the jet milling magnetic powder B, adding a lubricant, stirring for 2-6 h, then carrying out orientation forming in an inert atmosphere, and then carrying out isostatic pressing treatment;
(4) and (3) feeding the blank subjected to isostatic pressing treatment into a sintering furnace, preserving heat for 2-5 hours at 550-600 ℃ for dehydrogenation treatment, and then performing presintering, high-temperature sintering and tempering heat treatment.
3. The preparation method of the high-performance sintered neodymium-iron-boron magnet according to claim 2, wherein the smelting temperature in the step (1) and the step (2) is 1450-1500 ℃, and the casting temperature is 1400-1450 ℃; when the rapid hardening process is adopted, the rotating speed of the copper roller is 1.2-1.5 m/s, and the average thickness of the obtained cast sheet A is 0.2-0.4 mm.
4. The method for preparing a high-performance sintered NdFeB magnet according to claim 2, wherein the average particle size of the jet-milled magnetic powder A in the step (1) is 4-5 μm.
5. The method for preparing a high-performance sintered NdFeB magnet according to claim 2, wherein the average particle size of the jet-milled magnetic powder B in the step (2) is 1-2 μm.
6. The method for preparing a high-performance sintered neodymium-iron-boron magnet according to claim 2, wherein in the mixture of the jet milling magnetic powder A and the jet milling magnetic powder B in the step (3), the content of the jet milling magnetic powder B is 1-5 wt%.
7. The method for preparing a high-performance sintered NdFeB magnet according to claim 2, wherein the magnetic field strength of the orientation molding in the step (3) is 1.0-1.5T, and the isostatic pressure is 150-220 MPa.
8. The method for preparing the high-performance sintered neodymium-iron-boron magnet according to claim 2, wherein the pre-sintering in the step (4) is performed at 800-1000 ℃ for 10-15 hours.
9. The method for preparing a high-performance sintered NdFeB magnet according to claim 8, wherein the pre-sintering in the step (4) is performed by keeping the temperature at 850-950 ℃ for 12-15 h.
10. The preparation method of the high-performance sintered neodymium-iron-boron magnet according to claim 2, characterized in that the high-temperature sintering temperature in the step (4) is 1030-1100 ℃, and the sintering time is 4-6 h; the tempering heat treatment comprises the following steps: the primary tempering temperature is 800-920 ℃, and the tempering time is 2-4 hours; the secondary tempering temperature is 460-560 ℃, and the tempering time is 4-6 hours.
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