CN112489915A - Corrosion-resistant high-coercivity neodymium-iron-boron permanent magnet material and preparation method thereof - Google Patents
Corrosion-resistant high-coercivity neodymium-iron-boron permanent magnet material and preparation method thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 99
- 238000005260 corrosion Methods 0.000 title claims abstract description 55
- 230000007797 corrosion Effects 0.000 title claims abstract description 53
- 229910001172 neodymium magnet Inorganic materials 0.000 title claims abstract description 47
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims description 20
- 239000002245 particle Substances 0.000 claims abstract description 59
- -1 rare earth hydride Chemical class 0.000 claims abstract description 27
- 239000011777 magnesium Substances 0.000 claims abstract description 23
- 238000004321 preservation Methods 0.000 claims abstract description 23
- 238000005245 sintering Methods 0.000 claims abstract description 22
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 17
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 16
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000011282 treatment Methods 0.000 claims description 45
- 238000000498 ball milling Methods 0.000 claims description 33
- 238000005496 tempering Methods 0.000 claims description 29
- 238000010438 heat treatment Methods 0.000 claims description 26
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 24
- 239000001257 hydrogen Substances 0.000 claims description 24
- 229910052739 hydrogen Inorganic materials 0.000 claims description 24
- 238000002156 mixing Methods 0.000 claims description 23
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 16
- 239000000347 magnesium hydroxide Substances 0.000 claims description 16
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 16
- 239000003607 modifier Substances 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 13
- 239000002994 raw material Substances 0.000 claims description 12
- 238000010521 absorption reaction Methods 0.000 claims description 11
- 239000011159 matrix material Substances 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 238000005303 weighing Methods 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 9
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- 239000002002 slurry Substances 0.000 claims description 9
- 238000000227 grinding Methods 0.000 claims description 8
- 229910052771 Terbium Inorganic materials 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 238000000465 moulding Methods 0.000 claims description 7
- 238000005498 polishing Methods 0.000 claims description 7
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 claims description 7
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- 239000007788 liquid Substances 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 abstract description 16
- 229910052751 metal Inorganic materials 0.000 abstract description 9
- 239000002184 metal Substances 0.000 abstract description 9
- 229910052782 aluminium Inorganic materials 0.000 abstract description 7
- 239000012071 phase Substances 0.000 abstract description 6
- 238000006243 chemical reaction Methods 0.000 abstract description 5
- 239000000395 magnesium oxide Substances 0.000 abstract description 4
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 abstract description 4
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 abstract description 4
- 230000005389 magnetism Effects 0.000 abstract description 4
- 230000009467 reduction Effects 0.000 abstract description 4
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- 239000003638 chemical reducing agent Substances 0.000 abstract description 2
- 238000002844 melting Methods 0.000 abstract description 2
- 230000008018 melting Effects 0.000 abstract description 2
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 abstract description 2
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- 230000001808 coupling effect Effects 0.000 description 5
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- 238000005520 cutting process Methods 0.000 description 4
- 230000005347 demagnetization Effects 0.000 description 4
- 229910052733 gallium Inorganic materials 0.000 description 4
- 239000000696 magnetic material Substances 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 150000002910 rare earth metals Chemical class 0.000 description 4
- 239000007779 soft material Substances 0.000 description 4
- 238000001514 detection method Methods 0.000 description 3
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- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
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- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 2
- 238000010892 electric spark Methods 0.000 description 2
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
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- 238000011161 development Methods 0.000 description 1
- 230000005662 electromechanics Effects 0.000 description 1
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- 230000001737 promoting effect Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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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
- H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
- H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
- H01F1/0576—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together pressed, e.g. hot working
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/02—Making ferrous alloys by powder metallurgy
- C22C33/0207—Using a mixture of prealloyed powders or a master alloy
- C22C33/0228—Using a mixture of prealloyed powders or a master alloy comprising other non-metallic compounds or more than 5% of graphite
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/02—Making ferrous alloys by powder metallurgy
- C22C33/0257—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/10—Ferrous alloys, e.g. steel alloys containing cobalt
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/12—Ferrous alloys, e.g. steel alloys containing tungsten, tantalum, molybdenum, vanadium, or niobium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/14—Ferrous alloys, e.g. steel alloys containing titanium or zirconium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/16—Ferrous alloys, e.g. steel alloys containing copper
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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
- 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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- 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
Abstract
The application relates to the field of permanent magnet materials, and particularly discloses a corrosion-resistant high-coercivity neodymium iron boron permanent magnet material which comprises the following elements in percentage by weight: 1-8% of rare earth hydride particles, 10-15% of PrNd, 1.0-1.5% of B, 2-3% of Co, 0.1-0.3% of Cu, 0.5-1.0% of Nb, 0.1-0.2% of Zr, 1-2% of Al, 0-1% of Ga, and the balance of Fe, wherein the particle size of the rare earth hydride particles is 1000 meshes. This application makes metal aluminium be the reductant through high temperature environment earlier before the heat preservation sintering, metal magnesium is prepared to the direct reduction magnesium oxide, through adding magnesium element, under hot and humid environment, thereby reduce the oxidation of Nd with oxygen reaction, make the magnet keep good magnetism, because magnesium has lower melting point, can promote the sintering of magnet liquid phase, it is more even to make rich neodymium phase distribution, even rich Nd phase can improve the magnetic property of magnet, the inside corrosion properties of permanent-magnet material has been improved simultaneously.
Description
Technical Field
The application relates to the field of permanent magnet materials, in particular to a corrosion-resistant high-coercivity neodymium iron boron permanent magnet material and a preparation method thereof.
Background
The permanent magnetic material is used as an important information functional material and is widely applied to the fields of communication, electromechanics, information, robots, intelligent manufacturing and the like. The coercive force of the permanent magnetic material is generally larger than 4kA/m, and the strong magnetism can still be kept for a long time by removing an external magnetic field when the technical magnetization is saturated. At present, most of motors such as automobile starting motors, electric bicycle motors, computer driving motors, wind driven generators and the like adopt permanent magnet motors. The sintered Nd-Fe-B permanent magnet is small in size and high in performance, can well reduce the motor quality, improves the motor efficiency, is more suitable for the miniaturization and the light weight of automobiles, and provides a material basis for the development of novel industries.
The related technology is Chinese invention patent with publication number CN110808158A and discloses a method for improving the coercive force of a sintered neodymium iron boron magnet and the sintered neodymium iron boron magnet, the scheme discloses a method for improving the coercive force of the sintered neodymium iron boron magnet, which comprises the steps of RM alloy preparation, RM adhesion layer preparation, heat treatment and the like; the invention also provides the sintered neodymium-iron-boron magnet prepared by the method. According to the invention, the RM alloy is adhered to the surface of the magnet through friction collision, and the redundant adhering RM alloy on the surface can be removed through collision of medium particles, so that an RM adhesion layer with good consistency and strong binding force is formed, and meanwhile, adhesion is avoided; the residual RM alloy particles and medium particles can be recycled, and the utilization rate of rare earth is high; in the rotary heating process, the thickness of the RM alloy layer can be controlled, so that the diffusion quantity is controlled, and the requirements of sintered neodymium iron boron magnets with different properties are met.
In view of the above-mentioned related technologies, the inventor believes that in the scheme of simply adhering the rare earth alloy material on the surface of the base material through collision friction and then improving the coercivity of the material through high-temperature diffusion, because a good dispersion effect cannot be formed between the diffusion material and the base material, the uniformity of the neodymium iron boron material is affected, and thus the coercivity of the neodymium iron boron material cannot be effectively improved.
Disclosure of Invention
In order to improve the internal structure of the neodymium iron boron material and improve the coercive force and corrosion resistance of a magnet, in a first aspect, the application provides a corrosion-resistant high-coercive force type neodymium iron boron permanent magnet material and a preparation method thereof, wherein the corrosion-resistant high-coercive force type neodymium iron boron permanent magnet material comprises the following elements in percentage by weight: 1-8% of rare earth hydride particles, 10-15% of PrNd, 1.0-1.5% of B, 2-3% of Co, 0.1-0.3% of Cu, 0.5-1.0% of Nb, 0.1-0.2% of Zr, 1-2% of Al, 0-1% of Ga, and the balance of Fe, wherein the particle size of the rare earth hydride particles is 1000 meshes.
By adopting the technical scheme, the particle size of the rare earth diffusion material is optimized, so that a good dispersion structure can be formed after the rare earth diffusion material is added into the permanent magnet base material, and a structure of a coating form is formed by good combination of the dispersion particles and the main body base material, so that the crystal boundary structure is improved, the crystal grain coupling effect is inhibited, the coupling effect coefficient is reduced, the nucleation and growth of a dispersion field are inhibited, and the demagnetization factor is reduced, thereby effectively improving the coercive force of the neodymium iron boron permanent magnet material and further improving the corrosion resistance of the permanent magnet material.
Further, the corrosion-resistant high-coercivity neodymium iron boron permanent magnet material also comprises Mg with the same mass as Cu and Al with the mass of 1/10 of Mg weight2O3。
By adopting the technical scheme, as Mg and Al are added into the permanent magnet material2O3Because of the addition of magnesium element, the density of Mg is very small and the activity of nano Mg powder is very high, Mg is easier to react with oxygen than Nd in hot and humid environments, thereby reducing the oxidation of Nd and keeping the magnet to have good magnetism, promoting the liquid phase sintering of the magnet through the formed alumina particles, enabling the distribution of the Nd-rich phase to be more uniform, and the uniform Nd-rich phase can improve the magnetic performance of the magnet, thereby optimizing the structural characteristics of the neodymium-iron-boron material and improving the corrosion resistance of the neodymium-iron-boron permanent magnet material.
Further, the preparation method of the corrosion-resistant high-coercivity neodymium iron boron permanent magnet material comprises the following steps:
s1, mixing the raw materials: weighing each element according to the formula, collecting the mixed particles, performing ball milling and mixing, and collecting the ball milling mixed matrix particles; s2, blank pressing: respectively weighing 45-50 parts by weight of ball-milling mixed matrix particles, 10-15 parts by weight of anti-corrosion modification liquid and 10-15 parts by weight of coercive force modifier, stirring and mixing, grinding and dispersing to obtain dispersed slurry, adding the dispersed slurry into a mold, and performing cold press molding; s3, heating and sintering: placing the cold-pressed blank in a vacuum sintering furnace, carrying out heat preservation treatment after temperature programming, and carrying out secondary temperature programming and heat preservation sintering; s4, secondary tempering: and (3) after standing and cooling to room temperature, carrying out tempering treatment twice, standing and cooling to room temperature, thus obtaining the corrosion-resistant high-coercivity neodymium iron boron permanent magnet material.
By adopting the technical scheme, because the corrosion-resistant high-coercivity neodymium iron boron permanent magnet material is prepared by adopting the one-step forming sintering preparation scheme, namely, the modified materials are prepared firstly and then mixed to prepare a blank, the blank is heated firstly, the magnesium oxide generated by reducing the magnesium hydroxide by the metal aluminum is reduced, the reduced magnesium permeates and is coated into the raw material of the permanent magnet material, the corrosion resistance of the material is improved by filling the metal magnesium, and the blank is sintered and formed again after secondary temperature programming, and the coercivity modifier filled in the blank permeates into the pores of the permanent magnet material under the high-temperature environment through secondary tempering treatment, so that the coercivity modifier forms more uniform load in the permanent magnet material, the structure of the soft material is improved, the corrosion resistance of the soft material is improved, and the optimized preparation scheme not only can effectively reduce the preparation time of the permanent magnet material, the preparation efficiency of the permanent magnetic material is improved, and meanwhile, the scheme of one-step molding and sintering improves the structural performance inside the permanent magnetic material, so that the service life is further improved.
Further, the anticorrosion modification liquid in the step S2 is prepared by mixing, by mass, 1: 3: 100 is prepared by mixing and dispersing nanometer aluminum powder, nanometer magnesium hydroxide particles and deionized water.
By adopting the technical scheme, as the nano aluminum powder and the nano magnesium hydroxide particles are dispersed in the deionized water to form the sol suspension of the colloidal material for addition, the dispersion performance among the components is improved, meanwhile, the aluminum powder and the magnesium hydroxide particles can be effectively filled into the material for reaction, the structural characteristics of the neodymium iron boron material are optimized, and the corrosion resistance of the neodymium iron boron permanent magnet material is improved.
Further, the coercivity modifier in step S2 is terbium hydride.
By adopting the technical scheme, because the terbium hydride is adopted for carrying out the coercive force modification treatment, the crystal boundary organization of the magnet in the permanent magnet material is improved, the crystal boundary is more continuous and smooth, the exchange coupling effect coefficient is improved, and meanwhile, the terbium hydride can wet crystal boundary smooth grains in the permanent magnet material, so that the demagnetization factor is reduced, and the coercive force of the magnet is improved.
Further, the preparation method of the coercivity modifier comprises the following steps: (1) taking pure terbium, polishing, washing, drying, carrying out ball milling treatment, collecting ball-milled particles, placing the ball-milled particles in a hydrogen crushing furnace, and carrying out hydrogen absorption treatment in a hydrogen atmosphere; (2) vacuumizing, heating, heat-preserving and sintering, and then performing ball milling treatment to obtain the coercivity modifier.
By adopting the technical scheme, pure terbium is adopted and polished, and the coercivity modifier is prepared by hydrogen absorption modification, so that the magnetic property of the neodymium iron boron material can be effectively improved, and the coercivity of the magnet is improved by the coercivity modifier.
Further, the hydrogen absorption treatment is as follows: introducing hydrogen to 0.05-0.08 MPa under the vacuum degree of 0.1-0.5 Pa, heating to 250-300 ℃, and preserving heat for 3-5 h for hydrogen absorption treatment.
By adopting the technical scheme, the temperature and the pressure of hydrogen absorption treatment are optimized, so that terbium can better react with hydrogen to generate terbium hydride for carrying out coercive force modification treatment.
Further, the programmed heating and heat preservation treatment in the step S3 is to heat the temperature to 850-920 ℃ at a rate of 1 ℃/min, and to carry out heat preservation treatment for 45-60 min.
Through adopting above-mentioned technical scheme, this application makes metal aluminium be the reductant through high temperature environment earlier before heat preservation sintering, magnesium is prepared to direct reduction magnesium oxide, because what adopt in this application scheme is nanometer level particulate material, so this application final reduction formed magnesium can effectively permeate to permanent magnet material inside and form the dispersion cladding, thereby through adding magnesium element, under hot and humid environment, thereby reduce the oxidation of Nd with oxygen reaction, make the magnet keep good magnetism, because magnesium has lower melting point, can promote magnet liquid phase sintering, make rich neodymium phase distribution more even, even rich Nd phase can improve the magnetic property of magnet, the inside corrosion behavior of permanent magnet material has been improved simultaneously.
Further, the two tempering treatments in the step S4 are to control the primary tempering temperature to be 850-880 ℃, perform the primary tempering for 100-110 min, and perform the heat preservation tempering at 480-500 ℃ for 3-5 h.
By adopting the technical scheme, the secondary tempering treatment is adopted, the internal stress is reduced, the ductility or the toughness of the alloy is improved, and meanwhile, in the secondary tempering process, the material in the coercivity modifier is subjected to good intercrystalline diffusion, so that the uniform diffusion performance of a crystal piece is improved.
In summary, the present application includes at least one of the following beneficial technical effects:
firstly, preparing each modified material, then mixing to prepare a blank, firstly heating to reduce magnesium oxide generated by magnesium hydroxide from metal aluminum, penetrating and coating the reduced magnesium into the permanent magnet material raw material, improving the corrosion resistance of the material by filling the metal magnesium, sintering again after secondary temperature programming, and penetrating the coercivity modifier filled in the permanent magnet material into pores of the permanent magnet material by secondary tempering to form more uniform load in the permanent magnet material, thereby improving the structure of the soft material and improving the corrosion resistance of the soft material.
Secondly, terbium hydride is adopted to carry out coercive force modification treatment, so that the crystal boundary organization of the magnet in the permanent magnet material is improved, the crystal boundary is more continuous and smooth, the exchange coupling effect coefficient is improved, and meanwhile, terbium hydride can wet crystal boundary smooth grains in the permanent magnet material, so that the demagnetization factor is reduced, and the coercive force of the magnet is improved.
Thirdly, the permanent magnet material is prepared through a one-time program scheme, so that the preparation time of the permanent magnet material can be effectively shortened, the preparation efficiency of the permanent magnet material is improved, and meanwhile, the structural performance in the permanent magnet material is improved through a one-time molding and sintering scheme, so that the service life is further prolonged.
Drawings
Fig. 1 is a flow chart of a corrosion-resistant high-coercivity neodymium iron boron permanent magnet material and a preparation method thereof provided by the application.
Detailed Description
The present application will be described in further detail with reference to the following drawings and examples.
In the embodiment of the present application, the used apparatuses and raw materials and auxiliary materials are as follows, but not limited thereto:
a machine: CHI604D electrochemical workstation, wire cut electric discharge machine, pulse magnetizing machine, high temperature permanent magnet measuring instrument NIM-500C.
Examples
Example 1
According to the mass ratio of 1: 3: 100, mixing nano aluminum powder and nano magnesium hydroxide particles, placing the mixture into deionized water, stirring and mixing the mixture at room temperature for 15min, and then performing ultrasonic dispersion at 200W for 10min to obtain a dispersion suspension;
taking pure terbium, polishing to remove a surface oxide layer, washing for 3 times by using absolute ethyl alcohol, naturally drying, placing in a ball milling tank, carrying out ball milling treatment, collecting ball milling particles, placing the ball milling particles in a hydrogen crushing furnace, introducing hydrogen to 0.05MPa under the vacuum degree of 0.1Pa, heating to 250 ℃, preserving heat for 3 hours, carrying out hydrogen absorption treatment, vacuumizing, heating again, preserving heat for 3 hours, standing, cooling to room temperature, carrying out ball milling treatment by using absolute ethyl alcohol as ball milling graft according to the ball-to-material ratio of 10:1 at room temperature, and sieving by using a 1000-mesh sieve to obtain modified powder;
weighing the following elements in percentage by weight: 1% of rare earth hydride particles, 10% of PrNd, 1.5% of B, 2% of Co, 0.1% of Cu, 0.5% of Nb, 0.1% of Zr, 1% of Al and the balance of Fe, stirring, mixing, ball-milling, collecting ball-milled mixed matrix particles, respectively weighing 45 parts of ball-milled mixed matrix particles, 10 parts of dispersed suspension and 10 parts of modified powder according to weight parts, stirring, mixing, grinding and dispersing in a grinding machine for 1h to obtain dispersed slurry, adding the dispersed slurry into a mold, cold-pressing, molding, placing in a vacuum sintering furnace, firstly heating to 850 ℃ according to a heating rate of 1 ℃/s, carrying out heat preservation treatment for 45min, then heating to 1150 ℃ according to a speed of 3 ℃/s, standing, cooling and tempering twice at room temperature after carrying out heat preservation sintering for 2h, controlling the tempering temperature to 850 ℃ for 100min, then carrying out heat preservation tempering for 3h at 480 ℃, standing, cooling to room temperature to obtain a calcined matrix, and the corrosion-resistant high-coercivity neodymium iron boron permanent magnet material can be prepared.
Example 2
According to the mass ratio of 1: 3: 100, mixing nano aluminum powder and nano magnesium hydroxide particles, placing the mixture into deionized water, stirring and mixing the mixture at room temperature for 17min, and then performing ultrasonic dispersion at 250W for 12min to obtain a dispersion suspension;
taking pure terbium, polishing to remove a surface oxide layer, washing for 4 times by using absolute ethyl alcohol, naturally drying, placing in a ball milling tank, carrying out ball milling treatment, collecting ball milling particles, placing the ball milling particles in a hydrogen crushing furnace, introducing hydrogen to 0.06MPa under the vacuum degree of 0.2Pa, heating to 275 ℃, preserving heat for 4 hours, carrying out hydrogen absorption treatment, vacuumizing, heating again, preserving heat for 4 hours, standing, cooling to room temperature, carrying out ball milling treatment by using absolute ethyl alcohol as ball milling graft according to the ball-to-material ratio of 10:1 at room temperature, and sieving by using a 1000-mesh sieve to obtain modified powder;
weighing the following elements in percentage by weight: 2% of rare earth hydride particles, 12% of PrNd, 1.2% of B, 2% of Co, 0.2% of Cu, 0.7% of Nb, 0.4% of Zr, 1% of Al, 0.5% of Ga and the balance of Fe, stirring, mixing and ball milling, collecting ball milling mixed matrix particles, respectively weighing 47 parts of ball milling mixed matrix particles, 12 parts of dispersed suspension and 12 parts of modified powder according to weight parts, stirring, mixing, grinding and dispersing in a grinding machine for 1h to obtain dispersed slurry, adding the dispersed slurry into a mold, cold press molding, placing in a vacuum sintering furnace, heating to 875 ℃ at a heating rate of 1 ℃/s, carrying out heat preservation treatment for 47min, heating to 1162 ℃ at a speed of 4 ℃/s, carrying out heat preservation sintering for 2h, standing, cooling and tempering twice at room temperature, controlling the tempering temperature to 875 ℃ for 105min, carrying out heat preservation tempering at 490 ℃ for 4h, standing, cooling to room temperature, and (4) obtaining a calcined substrate, and thus obtaining the corrosion-resistant high-coercivity neodymium iron boron permanent magnet material.
Example 3
According to the mass ratio of 1: 3: 100, mixing nano aluminum powder and nano magnesium hydroxide particles, placing the mixture into deionized water, stirring and mixing the mixture at room temperature for 20min, and then performing ultrasonic dispersion at 300W for 15min to obtain a dispersion suspension;
taking pure terbium, polishing to remove a surface oxide layer, washing for 5 times by using absolute ethyl alcohol, naturally drying, placing in a ball milling tank, carrying out ball milling treatment, collecting ball milling particles, placing the ball milling particles in a hydrogen crushing furnace, introducing hydrogen to 0.08MPa under the vacuum degree of 0.5Pa, heating to 300 ℃, preserving heat for 5 hours, carrying out hydrogen absorption treatment, vacuumizing, heating again, preserving heat for 5 hours, standing, cooling to room temperature, carrying out ball milling treatment by using absolute ethyl alcohol as ball milling graft according to the ball-to-material ratio of 10:1 at room temperature, and sieving by using a 1000-mesh sieve to obtain modified powder;
weighing the following elements in percentage by weight: 8 percent of rare earth hydride particles, 15 percent of PrNd, 1.5 percent of B, 3 percent of Co, 0.3 percent of Cu, 1.0 percent of Nb, 0.2 percent of Zr, 2 percent of Al, 1 percent of Ga and the balance of Fe, stirring, mixing and ball-milling, collecting ball-milled mixed matrix particles, respectively weighing 50 parts of ball-milled mixed matrix particles, 15 parts of dispersed suspension and 15 parts of modified powder according to the weight parts, stirring, mixing, placing in a grinding machine, grinding and dispersing for 2 hours, obtaining dispersed slurry, adding in a mould, cold-press molding, placing in a vacuum sintering furnace, firstly heating to 920 ℃ according to the heating rate of 1 ℃/s, carrying out heat preservation treatment for 60min, then heating to 1180 ℃ according to the heating rate of 5 ℃/s, carrying out heat preservation treatment for 3 hours, standing, cooling and tempering for two times at room temperature, controlling the tempering temperature to 880 ℃, tempering for 110min, then carrying out heat preservation tempering for 5h at 500 ℃, standing, cooling to, and (4) obtaining a calcined substrate, and thus obtaining the corrosion-resistant high-coercivity neodymium iron boron permanent magnet material.
Example 4
In example 4, no dispersion suspension was added during the preparation, and the other conditions and component ratios were the same as in example 1.
Example 5
In example 5, 1000 mesh gallium hydride particles were used instead of 1000 mesh terbium hydride particles in example 1, and the other conditions and component ratios were the same as in example 1.
Performance test
The performance tests of examples 1 to 5 were performed, and the nd-fe-b permanent magnet materials prepared in examples 1 to 5 were tested to specifically test the corrosion resistance and thermal stability.
Detection method/test method
Corrosion resistance:
a test sample is cut into small magnetic blocks with the size of 10mm multiplied by 5mm by an electric spark wire cutting machine, then an electrode wire and the magnetic blocks are welded together, the corrosion potential and the corrosion current density of the sample are tested on a CHI604D electrochemical workstation, a standard three-electrode test system is adopted, the sample to be tested is a working electrode, a saturated calomel electrode is used as a reference electrode, and a platinum electrode is used as an auxiliary electrode. The corrosion medium is 3.5% NaCl and 0.005% H2SO4The test temperature of the solution is 25 +/-0.1 ℃, and the electrokinetic potential scanning speed is 2 mV/s.
Thermal stability performance:
cutting the test sample into small magnetic blocks of 10mm × 10mm × 5mm by a wire electric discharge machine, polishing and cleaning the surface, magnetizing the sample by a pulse magnetizing machine, and testing the magnetic properties of the magnetized magnet at different temperatures of 20 deg.C, 50 deg.C, 100 deg.C, 150 deg.C and 200 deg.C by a high temperature permanent magnet measuring instrument (NIM-500C).
The specific detection results are shown in the following tables 1-3:
TABLE 1 Performance test Table
TABLE 2 Performance test Table
TABLE 3 Performance test Table
The performance detection comparison in reference to tables 1-3 can find that:
the performances of the examples 1 to 3 are compared, wherein the corrosion resistance and the thermal stability of the example 3 are the best, because the proportion of the added materials in the example 3 is the highest, and the technical scheme of the application is reflected from the side surface to be practicable.
Comparing the performances of the embodiment 1 and the embodiment 4, since the dispersion suspension is not added in the preparation process in the embodiment 4, the permanent magnet material finally prepared in the application does not contain metal magnesium particles, so the corrosion resistance in the embodiment 4 is remarkably reduced, which shows that the technical scheme of the application not only improves the dispersion performance among the components, but also the aluminum powder and the magnesium hydroxide particles can be effectively filled in the material for reaction, thereby optimizing the structural characteristics of the neodymium iron boron material and improving the corrosion resistance of the neodymium iron boron permanent magnet material.
Comparing the performances of the embodiment 1 and the embodiment 5, because 1000-mesh gallium hydride particles are adopted to replace 1000-mesh terbium hydride particles in the embodiment 1, although the corrosion resistance of the permanent magnet material prepared from gallium hydride is not obviously reduced, the reduction speed of the absolute values of the coercive force temperature coefficient and the remanence temperature coefficient is slow, which shows that the thermal stability is reduced, because the terbium hydride is adopted to carry out coercive force modification treatment compared with terbium hydride, the crystal boundary structure of the magnet in the permanent magnet material is improved, the crystal boundary is more continuously and smoothly, the exchange coupling effect coefficient is improved, meanwhile, the terbium hydride can wet crystal boundary smooth grains in the permanent magnet material, and the demagnetization factor is reduced, thereby improving the coercive force of the magnet.
Comparative example
Comparative examples 1 to 3
In comparative examples 1 to 3, no rare earth hydride was added, and the other conditions and component ratios were the same as in examples 1 to 3.
Comparative examples 4 to 6
In comparative examples 4 to 6, the suspension prepared from nano zinc and nano magnesium hydroxide particles and water was used instead of the suspension prepared from nano aluminum powder, nano magnesium hydroxide particles and water, and the rest conditions and component ratios were the same as in examples 1 to 3.
Comparative examples 7 to 9
In comparative examples 7-9, one-time temperature programming and heat preservation treatment is adopted for 2-3 hours, and the rest conditions and component proportions are the same as those in examples 1-3.
Comparative examples 10 to 12
In comparative examples 10 to 12, when the permanent magnet material was prepared, the permanent magnet material was directly left to stand and cooled to room temperature without performing the secondary tempering treatment, and the other conditions and the component ratios were the same as those in examples 1 to 3.
Performance test
Respectively testing the performances of the neodymium iron boron permanent magnet materials prepared in comparative examples 1-12, and specifically testing the corrosion resistance and the thermal stability of the neodymium iron boron permanent magnet materials prepared in comparative examples 1-12.
Detection method/test method
Corrosion resistance:
a test sample is cut into small magnetic blocks with the size of 10mm multiplied by 5mm by an electric spark wire cutting machine, then an electrode wire and the magnetic blocks are welded together, the corrosion potential and the corrosion current density of the sample are tested on a CHI604D electrochemical workstation, a standard three-electrode test system is adopted, the sample to be tested is a working electrode, a saturated calomel electrode is used as a reference electrode, and a platinum electrode is used as an auxiliary electrode. The corrosion medium is 3.5% NaCl and 0.005% H2SO4The test temperature of the solution is 25 +/-0.1 ℃, and the electrokinetic potential scanning speed is 2 mV/s.
Thermal stability performance:
cutting the test sample into small magnetic blocks of 10mm × 10mm × 5mm by a wire electric discharge machine, polishing and cleaning the surface, magnetizing the sample by a pulse magnetizing machine, and testing the magnetic properties of the magnetized magnet at different temperatures of 20 deg.C, 50 deg.C, 100 deg.C, 150 deg.C and 200 deg.C by a high temperature permanent magnet measuring instrument (NIM-500C).
The specific detection results are shown in the following tables 1-3:
TABLE 4 Performance test Table
TABLE 5 Performance test Table
TABLE 6 Performance test Table
Referring to the comparison of the performance tests in tables 4-6, it can be found that:
comparing comparative examples 1-3 with examples 1-3, the rare earth hydride is not added in the formula of the comparative examples, and the comparison of the data in tables 5-6 shows that the thermal stability of the comparative examples 1-3 is remarkably reduced, which shows that the rare earth hydride added in the application can improve the grain boundary structure, thereby improving the coercive force of the neodymium iron boron permanent magnet material.
Comparing the comparative examples 4-6 with the examples 1-3, the suspension prepared from nano zinc and nano magnesium hydroxide particles and water is used in the comparative examples to replace the suspension prepared from nano aluminum powder, nano magnesium hydroxide particles and water, and the corrosion resistance in the comparative examples is obviously reduced, which shows that the nano aluminum powder and the nano magnesium hydroxide particles are dispersed in deionized water, the aluminum powder and the magnesium hydroxide particles can be effectively filled into the material for reaction, and the formed metal magnesium is reduced, so that the structural characteristics of the neodymium iron boron material can be optimized, and the corrosion resistance of the neodymium iron boron permanent magnet material can be improved.
Comparing the comparative examples 7-9 with the examples 1-3, the comparative examples 7-9 adopt one-time temperature programming and heat preservation treatment for 2-3 h in the preparation process, and the corrosion resistance in the comparative examples also shows a descending trend, because the magnesium metal cannot be effectively and completely reduced by one-time temperature raising scheme, the content of magnesium dispersed in the permanent magnet material is reduced, and the corrosion resistance is reduced compared with the examples 1-3.
Comparing the comparative examples 10-12 with the examples 1-3, the comparative examples 10-12 do not carry out secondary tempering treatment when the permanent magnet material is prepared, and directly stand and cool to room temperature, and the coercivity modifier material added in the application cannot be effectively diffused to form optimization due to the fact that secondary tempering treatment is not carried out, so that the coercivity of the material is reduced.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (9)
1. The corrosion-resistant high-coercivity neodymium-iron-boron permanent magnet material is characterized by comprising the following elements in percentage by weight: 1-8% of rare earth hydride particles, 10-15% of PrNd, 1.0-1.5% of B, 2-3% of Co, 0.1-0.3% of Cu, 0.5-1.0% of Nb, 0.1-0.2% of Zr, 1-2% of Al, 0-1% of Ga, and the balance of Fe, wherein the particle size of the rare earth hydride particles is 1000 meshes.
2. The corrosion-resistant high-coercivity NdFeB permanent magnet material as claimed in claim 1, further comprising Mg equal to Cu in mass and Al 1/10 in mass based on Mg weight2O3。
3. The preparation method of the corrosion-resistant high-coercivity neodymium iron boron permanent magnet material is characterized by comprising the following steps of:
s1, mixing the raw materials: weighing each element according to the formula, collecting the mixed particles, performing ball milling and mixing, and collecting the ball milling mixed matrix particles;
s2, blank pressing: respectively weighing 45-50 parts by weight of ball-milling mixed matrix particles, 10-15 parts by weight of anti-corrosion modification liquid and 10-15 parts by weight of coercive force modifier, stirring and mixing, grinding and dispersing to obtain dispersed slurry, adding the dispersed slurry into a mold, and performing cold press molding;
s3, heating and sintering: placing the cold-pressed blank in a vacuum sintering furnace, carrying out heat preservation treatment after temperature programming, and carrying out secondary temperature programming and heat preservation sintering;
s4, secondary tempering: and (3) after standing and cooling to room temperature, carrying out tempering treatment twice, standing and cooling to room temperature, thus obtaining the corrosion-resistant high-coercivity neodymium iron boron permanent magnet material.
4. The method for preparing the corrosion-resistant high-coercivity neodymium-iron-boron permanent magnet material according to claim 3, wherein the corrosion-resistant modifying solution in the step S2 is prepared by mixing, by mass, 1: 3: 100 is prepared by mixing and dispersing nanometer aluminum powder, nanometer magnesium hydroxide particles and deionized water.
5. The method for preparing the corrosion-resistant high-coercivity neodymium-iron-boron permanent magnet material according to claim 3, wherein the coercivity modifier in the step S2 is terbium hydride.
6. The preparation method of the corrosion-resistant high-coercivity neodymium-iron-boron permanent magnet material according to claim 5, wherein the coercivity modifier is prepared by the following steps:
(1) taking pure terbium, polishing, washing, drying, carrying out ball milling treatment, collecting ball-milled particles, placing the ball-milled particles in a hydrogen crushing furnace, and carrying out hydrogen absorption treatment in a hydrogen atmosphere;
(2) vacuumizing, heating, heat-preserving and sintering, and then performing ball milling treatment to obtain the coercivity modifier.
7. The method for preparing the corrosion-resistant high-coercivity neodymium-iron-boron permanent magnet material according to claim 6, wherein the hydrogen absorption treatment is as follows: introducing hydrogen to 0.05-0.08 MPa under the vacuum degree of 0.1-0.5 Pa, heating to 250-300 ℃, and preserving heat for 3-5 h for hydrogen absorption treatment.
8. The method for preparing a corrosion-resistant high-coercivity neodymium-iron-boron permanent magnet material according to claim 3, wherein the temperature programming and heat preservation treatment in the step S3 is to heat the neodymium-iron-boron permanent magnet material to 850-920 ℃ at a rate of 1 ℃/min, and the heat preservation treatment is performed for 45-60 min.
9. The method for preparing a corrosion-resistant high-coercivity neodymium-iron-boron permanent magnet material according to claim 3, wherein the two tempering treatments in the step S4 are to control the temperature of the first tempering at 850-880 ℃, perform the first tempering for 100-110 min, and perform the heat preservation tempering at 480-500 ℃ for 3-5 h.
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