CN114918428B - Manufacturing method for manufacturing self-assembled aluminum nickel cobalt magnet based on additive - Google Patents
Manufacturing method for manufacturing self-assembled aluminum nickel cobalt magnet based on additive Download PDFInfo
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 92
- 239000000654 additive Substances 0.000 title claims abstract description 67
- 230000000996 additive effect Effects 0.000 title claims abstract description 67
- -1 aluminum nickel cobalt Chemical compound 0.000 title claims abstract description 8
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 190
- 239000000956 alloy Substances 0.000 claims abstract description 190
- 239000000843 powder Substances 0.000 claims abstract description 126
- 230000005291 magnetic effect Effects 0.000 claims abstract description 65
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- 238000002844 melting Methods 0.000 claims abstract description 24
- 230000008018 melting Effects 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 24
- 238000005516 engineering process Methods 0.000 claims abstract description 18
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- 229910000828 alnico Inorganic materials 0.000 claims description 158
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 63
- 239000002994 raw material Substances 0.000 claims description 45
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
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- 238000012216 screening Methods 0.000 claims description 13
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- FFBHFFJDDLITSX-UHFFFAOYSA-N benzyl N-[2-hydroxy-4-(3-oxomorpholin-4-yl)phenyl]carbamate Chemical compound OC1=C(NC(=O)OCC2=CC=CC=C2)C=CC(=C1)N1CCOCC1=O FFBHFFJDDLITSX-UHFFFAOYSA-N 0.000 description 3
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Classifications
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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
- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/20—Direct sintering or melting
- B22F10/28—Powder bed fusion, e.g. selective laser melting [SLM] or electron beam melting [EBM]
-
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
-
- 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
- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/60—Treatment of workpieces or articles after build-up
- B22F10/64—Treatment of workpieces or articles after build-up by thermal means
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y10/00—Processes of additive manufacturing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y40/00—Auxiliary operations or equipment, e.g. for material handling
- B33Y40/20—Post-treatment, e.g. curing, coating or polishing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y80/00—Products made by additive manufacturing
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/023—Alloys based on nickel
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/07—Alloys based on nickel or cobalt based on cobalt
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
- C22C30/02—Alloys containing less than 50% by weight of each constituent containing copper
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/10—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
Abstract
The invention discloses a manufacturing method for manufacturing a self-assembled aluminum-nickel-cobalt magnet based on additive manufacturing. The method is based on additive manufacturing technology by self-assembly alpha 1 And alpha 2 Method of producing a magnet from an alloy, wherein alpha 1 The alloy has the atomic percentage composition of Fe x Co y Ni z Al u Ti v Cu w Nb t ，α 2 The alloy has the atomic percentage composition of Fe a Co b Ni c Al d Ti e Cu f Nb g The method comprises the steps of carrying out a first treatment on the surface of the Melting using selective laserThe technology carries out composite printing on two kinds of powder, alpha 1 And alpha is 2 The composite mass ratio of the alloy is 1:1-3:1, the coercive force of the magnet after heat treatment is 855.6-2174.4 Oe, the remanence is 9.4-15.7 kGs, and the maximum magnetic energy product is 4.2-13.2 MGOe. The invention overcomes the defects of the existing similar products that the two-phase component and content are difficult to regulate and control, the magnetic performance is still lower, and the parts with complex shapes are difficult to produce.
Description
Technical Field
The technical scheme of the invention relates to an aluminum nickel cobalt metal permanent magnet material, in particular to a manufacturing method for manufacturing a self-assembled aluminum nickel cobalt magnet based on additive manufacturing.
Background
The metal permanent magnet material Alnico (Alnico) has been widely used in high temperature devices since 1931, and is considered as a very promising rare earth-free permanent magnet due to its excellent thermal stability and high saturation magnetization, so that the manufacturing cost of certain high temperature applications can be greatly reduced, and the permanent magnet material has the best magnetic properties before the rare earth permanent magnet is made. The Alnico alloy is a permanent magnet mainly composed of Al, ni, co, fe and other elements, the Curie temperature is as high as 850 ℃, and the maximum working temperature is 538 ℃. Good magnetic properties of Alnico alloy are derived from amplitude modulation decomposition alpha-alpha 1 +α 2 The formed two-phase structure, wherein alpha phase is high-saturation solid solution phase, alpha 1 The phase is a ferromagnetic phase rich in Fe-Co, alpha 2 The phase is a weak magnetic phase or a non-magnetic phase rich in Al-Ni, alpha 1 Phase sum alpha 2 The composition, shape, distribution and number of phases are key factors in determining the permanent magnetic properties of the alloy.
The grades of Alnico alloys are defined as Alnico 1 to Alnico 9 total of 9 alloys depending on the alloy composition and processing conditions, with Alnico 5 and Alnico 8 being most commonly used, and the magnetic properties of Alnico alloys of different grades being dependent mainly on alpha determined by the different compositions 1 Phase sum alpha 2 Phase shape, size, volume fraction, arrangement, and branch type, etc. Zhou and Rehman et al (L.Zhou. Microstructure and magnetic property evolution with different heat-treatment conditions in an Alnico alloy [ J)].Acta Materialia,2017,133:73-80；S.U.Rehman.Synthesis,microstructures,magnetic properties and thermal stabilities of isotropic Alnico ribbons[J]Journal of Magnetism and Magnetic Materials,2018, 466:277-282.) in theory, when α 1 The phase is 5nm in diameter and 150nm longWhen the volume fraction is 2/3 of the rod shape, the magnetic energy product may double. Zhao et al (J.T.Zhao.the study on abnormal perature characteristics of coercivity in Alnico alloy [ J)]Journal of Magnetism and Magnetic Materials,2020, 508:166865.) it was found that Alnico 8alloys underwent amplitude modulated decomposition, α, upon annealing 1 The phase is bar-shaped, has a transverse direction of 25-28 nm, has a longitudinal direction of more than 300nm, and can improve alpha after heat treatment at 400 DEG C 1 The aspect ratio of the phases leads to an increase in shape anisotropy and thus magnetic properties.
Currently, the preparation process of the Alnico magnet is single, the process is complex, and the cost is high. Directionally solidified castings require the grains to be aligned in a particular direction, which is quite costly, time and complexity. Furthermore, alnico magnets produced by directional solidification must undergo extensive machining to obtain the final near net shape; once defective in the casting, it must be reworked and even scrapped directly, further increasing the production costs and also increasing the waste of material. In the current research, many researchers have tried to manufacture Alnico magnets using additive manufacturing methods. Compared with the traditional manufacturing method, the magnetic performance is improved to a different extent and the materials are saved. The advantages of the metal additive manufacturing (also called 3D printing) technology in material preparation are that the near net shape of the product with complex shape and difficult processing can be realized, which is beneficial to saving resources, reducing energy consumption and improving production efficiency. Especially, the permanent magnet material is prepared by using additive manufacturing technology, so that near net shaping of the magnet with the complex shape can be realized. White et al (e.m. H. White. Net shape processing of Alnico magnets by additive manufacturing [ J ]. IEEE Transactions on Magnetics,2017,53 (11): 1-6.) prepared an Alnico magnet using a laser near net shaping technique (LENS), found that an Alnico magnet processed by LENS had a remanence as high as 9kGs, a coercivity as high as 2.03kOe, a remanence approaching 10.6kGs of a directionally solidified, highly textured anisotropic cast Alnico 9, a coercivity matching 2.02kOe of sintered Alnico 8H. White et al (E.white. Processing of Alnico magnets by additive manufacturing [ J ]. Applied Sciences,2019,9 (22): 4843.) explored the feasibility of manufacturing Alnico magnets using laser near net shape forming techniques (LENS), directed Energy Deposition (DED), and electron beam fused powder bed fusion (EBM/PBF). It was found that the DED samples achieved the highest coercivity values for Alnico for additive manufacturing, much higher than for EBM/PBF samples of similar composition. However, the loss of Al and Cu in the EBM/PBF sample is an important factor in causing a decrease in coercivity. The EBM/PBF samples achieved the highest remanence at lower magnetic field annealing (MA) temperatures and were independent of MA time, but the composition changes of Al and Cu might contribute to higher remanence. Yang et al (Xiao-Shan Yang. Effect of remelting on microstructure and magnetic properties of Fe-Co-based alloys produced by laser additive manufacturing [ J ]. Journal of Physics and Chemistry of Solids,2019, 130:210-216.) prepared Fe-Co-based alloys with good saturation magnetization by laser additive manufacturing and laser remelting, which was found to improve the magnetic properties of the material and make the microstructure of the material denser.
The Alnico alloy is very sensitive to heat treatment, and the Alnico alloy prepared directly undergoes amplitude modulation decomposition during annealing to form alpha 1 And alpha 2 Other phases that are detrimental to magnetic properties, such as Cu-rich phases, may also occur, resulting in reduced magnetic properties.
Disclosure of Invention
The invention aims at overcoming the defects in the prior art, and provides a manufacturing method of a self-assembled AlNiCo magnet based on additive manufacturing, wherein the Alnico magnet is a two-phase composite magnet, and the traditional method for controlling the structure and the performance of an alloy in one direction by the components of an initial Alnico alloy is changed into the method for optimally designing alpha in the Alnico magnet 1 And alpha 2 Phase composition, and according to design alpha 1 And alpha 2 Constituent composition of phases for preparing the corresponding alpha respectively 1 And alpha 2 Alloy powder; secondly, changing the preparation method, adopting additive manufacturing technology, and adopting alpha in the manufacturing process 1 And alpha 2 Alloy powder remelting and realizing self-assembly fusion, and the alloy powder is directly formed into the alloy powder with rich alpha respectively in the rapid cooling process 1 And is rich in alpha 2 A two-phase structure of the phase components; finally, the preparation process is carried out by adjusting alpha 1 And alpha 2 The compounding proportion of the alloy powder is regulated and controlled to control the assembly of the compound magnet and two phasesThe relative content; designed alpha 1 And alpha 2 The components of the alloy powder give consideration to the alpha required by the corresponding magnetic property in the final alloy 1 And alpha 2 The composition characteristics of the phases take into account alpha 1 And alpha 2 The upward slope diffusion characteristic required by inter-phase amplitude modulation decomposition, and alpha 1 And alpha 2 The compounding ratio of the alloy powder directly changes alpha in the magnet 1 And alpha 2 Proportion of phases; the Alnico composite magnet is directly self-assembled and manufactured by using a metal additive manufacturing technology to obtain finer initial grains in a master alloy, and then nano-scale alpha is obtained by controlling amplitude modulation decomposition in the heat treatment process 1 Phase sum alpha 2 The phase overcomes the defects of the existing similar products that the two-phase component and the content are difficult to regulate and control, the magnetic performance is still lower, and the parts with complex shapes are difficult to produce.
The technical scheme adopted by the invention for solving the technical problems is as follows:
manufacturing method for manufacturing self-assembled Alnico magnet based on additive manufacturing technology, wherein Alnico magnet is manufactured through self-assembly alpha based on additive manufacturing technology 1 And alpha 2 Magnet prepared by the method of alloying, wherein alpha 1 The alloy has the atomic percentage composition of Fe x Co y Ni z Al u Ti v Cu w Nb t The subscript symbols x, y, z, u, v, w and t in the formula represent the atomic percent of the defined element composition range, wherein x is more than or equal to 38 and less than or equal to 50, y is more than or equal to 30 and less than or equal to 42,6 and less than or equal to 12, z is more than or equal to 30 and less than or equal to 12, u is more than or equal to 4 and less than or equal to 10,0.3 and less than or equal to 1.5,0.3 and w is more than or equal to 1.2,0.3 and less than or equal to 1, and the atomic percent is as follows: x+y+z+u+v+w+t=100; and alpha is 2 The alloy has the atomic percentage composition of Fe a Co b Ni c Al d Ti e Cu f Nb g The subscript symbols a, b, c, d, e, f and g in the formula represent the atomic percentages of the element composition ranges, namely, a is more than or equal to 12 and less than or equal to 16, b is more than or equal to 20 and less than or equal to 35, c is more than or equal to 18 and less than or equal to 32, d is more than or equal to 15 and less than or equal to 30, e is more than or equal to 7 and less than or equal to 14,1.5 and f is more than or equal to 5,0.3 and less than or equal to 0.8, and the atomic percentages are calculated to satisfy a+b+c+d+e+f+g=100; composite printing of two powders using Selective Laser Melting (SLM), alpha 1 And alpha is 2 The composite mass ratio of the alloy is 1:1-3:1, and the alloy is prepared by the following stepsThe coercive force of the magnet after heat treatment is 855.6-2174.4 Oe, the remanence is 9.4-15.7 kGs, and the maximum magnetic energy product is 4.2-13.2 MGOe.
The manufacturing method of the self-assembled Alnico magnet based on additive manufacturing comprises the steps of preparing alpha 1 And alpha is 2 The two alloy powders are compounded, and the Alnico magnet is prepared by self-assembly through a metal additive manufacturing technology, and the preparation method comprises the following specific steps:
firstly, smelting to prepare a master alloy cast ingot:
according to alpha 1 Atomic percent composition Fe of alloy x Co y Ni z Al u Ti v Cu w Nb t And alpha is 2 Atomic percent composition Fe of alloy a Co b Ni c Al d Ti e Cu f Nb g The mass ratio of the raw materials of the components required by the two alloys is calculated respectively, and the bulk pure Fe, the pure Co, the pure Ni, the pure Al, the pure Ti, the pure Cu and the pure Nb are weighed according to the mass percentage to complete the preparation of the two alloy raw materials; vacuum degree is better than 10 -2 Arc or induction melting furnace of Pa respectively to prepare alpha 1 Alloy and alpha 2 Melting alloy raw material of alloy into alpha 1 Master alloy ingot and alpha 2 Ingot casting of master alloy;
wherein, in the general formula, the symbols x, y, z, u, v, w and t represent the atomic percent of the composition range of the limiting elements, x is more than or equal to 38 and less than or equal to 50, y is more than or equal to 30 and less than or equal to 42,6 and less than or equal to 12, z is more than or equal to 30 and less than or equal to 12, u is more than or equal to 4 and less than or equal to 10,0.3 and less than or equal to 1.5,0.3 and w is more than or equal to 1.2,0.3 and less than or equal to 1, and the atomic percent is as follows: x+y+z+u+v+w+t=100; the symbols a, b, c, d, e, f and g represent the atomic percentages of the defined element composition ranges, wherein a is more than or equal to 12 and less than or equal to 16, b is more than or equal to 20 and less than or equal to 35, c is more than or equal to 18 and less than or equal to 32, d is more than or equal to 15 and less than or equal to 30, e is more than or equal to 7 and less than or equal to 14,1.5 and f is more than or equal to 5,0.3 and g is less than or equal to 0.8, and the atomic percentages satisfy a+b+c+d+e+f+g=100;
secondly, pulverizing:
respectively preparing spherical powder from the two master alloy ingots prepared in the first step by using atomizing powder making equipment, wherein the particle size of the powder ranges from 1 mu m to 150 mu m;
thirdly, screening spherical powder:
alpha obtained in the second step 1 And alpha is 2 The two alloy spherical powders are respectively screened, and alpha with the grain diameter of 38-90 mu m is selected 1 Alloy powder and alpha 2 Alloy powder according to alpha 1 :α 2 Compounding according to the mass ratio of h to 1 (h=1-3), and mixing for 2-30 min by using a mixer;
fourth step, additive manufacturing:
filling the spherical powder screened in the third step into a bin of additive manufacturing equipment, filling inert gas nitrogen or argon for protection, applying a selective laser melting technology (SLM), controlling the laser power to be 100-300W, the scanning speed to be 600-1200 mm/s, and paving the powder to be 0.3-0.5 mm for additive manufacturing to obtain an Alnico magnet;
fifth, solution treatment:
carrying out solution treatment on the Alnico magnet prepared in the fourth step for 20-60 min at 1150-1350 ℃ and then carrying out water cooling to obtain a solid solution Alnico magnet;
sixth, heat treatment and aging of the magnetic field:
and (3) carrying out magnetic field heat treatment on the solid solution Alnico magnet obtained in the fifth step under a magnetic field of 2-10 kOe at 800-900 ℃ for 10-60 min, and then carrying out aging treatment at 600-400 ℃ for 6-30 h to finally obtain the Alnico magnet product.
The manufacturing method of the self-assembled Alnico magnet based on additive manufacturing comprises the step of screening spherical powder for alpha in the third step 1 And alpha 2 The powder with the particle size of 48-80 μm is selected as the alloy powder with the best fluidity.
According to the manufacturing method for manufacturing the self-assembled Alnico magnet based on the additive, raw materials Fe, co, ni, al, ti, cu, nb are all commercial products, and the purities of the raw materials are more than or equal to 99.5% in mass percent; the equipment and processes used are all conventional equipment and processes well known in the art.
The manufacturing method of the self-assembled Alnico magnet based on additive manufacturing can be any one of metal additive manufacturing methods.
The invention has the substantial characteristics that:
the invention is thatIn component design, a biphase composite idea is adopted, and the biphase component and the biphase proportion are independently designed to enable the biphase component and the biphase proportion to be fused and self-assembled and composited in situ, so that alpha in the Alnico magnet prepared by the traditional method is broken through 1 Phase sum alpha 2 The phase composition and content are uncontrollable. Additive manufacturing is a novel preparation technology, namely a lamination preparation technology for quickly melting and quickly cooling metal powder under the action of high heat energy, and is helpful for obtaining fine initial grains due to the process of quick heating, quick cooling and lamination thermal cycle. In addition, the finally formed alpha in the Alnico alloy 1 Phase sum alpha 2 The composition, shape, distribution and quantity of the phases are essentially determined by the composition of the constituents of the initial Alnico alloy, which is then controlled by controlling the preparation parameters 1 Phase sum alpha 2 The composition, shape, distribution and quantity of the phases are difficult, and the adjustable amplitude is small. In particular, there has been no report to date on the use of additive manufacturing techniques to produce two-phase content and composition tunable Alnico magnets. The invention uses the self-assembled Alnico magnet prepared by the additive manufacturing technology to lead alpha to 1 Phase sum alpha 2 The proportion of phases is controlled by increasing alpha 1 The phase content obviously improves the saturation magnetization and remanence of the magnet, thereby improving the maximum magnetic energy product; finer initial grain structure can be obtained, and the printed magnet is compact and has few internal defects; compared with other methods, the preparation method is simpler and more convenient, saves materials, reduces the cost of production raw materials, has fewer defects in additive manufacturing of the magnet and is denser compared with casting of Alnico; the long sintering process is reduced compared to sintering an Alnico magnet. Compared with the Alnico alloy with the same component prepared by the traditional method, the magnetic performance is improved.
The beneficial effects of the invention are as follows:
(1) The self-assembled Alnico magnet has good hard magnetic property, the coercive force is 855.6-2174.4 Oe, the residual magnetism is 9.4-15.7 kGs, and the maximum magnetic energy product is 4.2-13.2 MGOe, which are all higher than those of the Alnico magnet prepared by the prior art.
(2) The Alnico product of the invention has low cost because of not containing expensive rare earth elements.
(3) The preparation method of the invention adopts a dual-phase composite method and then improves the magnetic performance of the Alnico magnetic alloy by a metal additive manufacturing technology, and compared with the magnet manufactured by the traditional technology such as casting, the method has fewer defects, higher performance and high preparation success rate, and reduces the material waste and the energy consumption.
(4) The preparation method of the invention can prepare the magnet with any complex shape which is near net shape.
Drawings
The invention will be further described with reference to the drawings and examples.
FIG. 1 is an X-ray diffraction pattern of an Alnico composite magnet type 1:1 of example 1.
FIG. 2 is the demagnetization curve of the type 1:1 Alnico composite magnet of example 1.
FIG. 3 is an X-ray diffraction pattern of the type 1.2:1 Alnico composite magnet of example 2.
FIG. 4 is a 1.2:1 Alnico composite magnet transmission electron microscopy image of example 2.
Fig. 5 is a demagnetization curve of the type 1.2:1 Alnico composite magnet of example 2.
FIG. 6 is an X-ray diffraction pattern of the type 1.5:1 Alnico composite magnet of example 3.
FIG. 7 is a 1.5:1 Alnico composite magnet scanning electron microscope image of example 3.
FIG. 8 is the demagnetization curve of the type 1.5:1 Alnico composite magnet of example 3.
FIG. 9 is an X-ray diffraction pattern of the type 1.8:1 Alnico composite magnet of example 4.
FIG. 10 is a transmission electron microscope image of the type 1.8:1 Alnico composite magnet of example 4.
FIG. 11 is the demagnetization curve of the type 1.8:1 Alnico composite magnet of example 4.
FIG. 12 is a sample profile of an Alnico composite magnet, type 2.1:1, of example 5.
FIG. 13 is a transmission electron microscope image of an Alnico composite magnet of type 2.1:1 of example 5.
FIG. 14 is a plot of demagnetization versus magnetic energy product for the 2.1:1 Alnico composite magnet of example 5.
FIG. 15 is a sample morphology of the type 2.3:1 Alnico composite magnet of example 6.
FIG. 16 is an X-ray diffraction pattern of an Alnico composite magnet type 2.3:1 of example 6.
FIG. 17 is a demagnetization curve of example 6 for an Alnico composite magnet type 2.3:1.
FIG. 18 is an X-ray diffraction pattern of an Alnico composite magnet of type 2.5:1 of example 7.
FIG. 19 is a scanning electron microscope image of an Alnico composite magnet type 2.5:1 of example 7.
FIG. 20 is a demagnetization curve of example 7 for an Alnico composite magnet type 2.5:1.
FIG. 21 is an X-ray diffraction pattern of an Alnico composite magnet of type 2.8:1 of example 8.
FIG. 22 is a transmission electron microscope image of a type 2.8:1 Alnico composite magnet of example 8.
FIG. 23 is a demagnetization curve of example 8 for an Alnico composite magnet type 2.8:1.
FIG. 24 is an X-ray diffraction pattern of the type 3:1 Alnico composite magnet of example 9.
FIG. 25 is a transmission electron microscope image of the type 3:1 Alnico composite magnet of example 9.
FIG. 26 is a demagnetization curve of the type 3:1 Alnico composite magnet of example 9.
Detailed Description
Example 1
Firstly, smelting to prepare a master alloy cast ingot:
according to alpha 1 Atomic percent composition Fe of alloy 38.0 Co 42.0 Ni 9.0 Al 8.0 Ti 1.2 Cu 0.8 Nb 1.0 And alpha is 2 Atomic percent composition Fe of alloy 16.0 Co 35.0 Ni 18.0 Al 15.0 Ti 13.5 Cu 2.0 Nb 0.5 The mass ratio of the required component raw materials is calculated respectively, and the required component blocky raw materials are weighed according to the mass percentage: pure Fe, pure Co, pure Ni, pure Al, pure Ti, pure Cu and pure Nb are used for preparing two alloy raw materials, and the vacuum degree is superior to 10 -2 Pa vacuum arc melting furnace at 1500 ℃ to the upper partPrepared alpha is respectively carried out within 1670 DEG C 1 Alloy and alpha 2 Alloy raw materials of the alloy are respectively smelted into alpha 1 Master alloy ingot and alpha 2 Ingot casting of master alloy;
secondly, pulverizing:
preparing spherical powder from the two master alloy ingots prepared in the first step by using HERMIGA-100-20 high-pressure atomization powder preparation equipment of UK PSI (program specific information) company in 1650 ℃ and high-purity argon atmosphere, wherein the particle size of the powder ranges from 1 mu m to 150 mu m;
thirdly, screening spherical powder:
alpha obtained in the second step 1 And alpha is 2 The two alloy spherical powders are respectively screened, and alpha with the grain diameter of 38-90 mu m is selected 1 Alloy powder and alpha 2 Compounding alloy powder in a mass ratio of 1:1, and mixing for 2min at a rotating speed of a 28r/min charging barrel by using a double-motion efficient mixing type mixer for a laboratory;
fourth step, additive manufacturing:
filling spherical powder selected by the powder screened in the third step into a bin of Siam platinum S200 type additive manufacturing equipment, introducing a built cylindrical model phi 10mm multiplied by 10mm into the equipment, filling inert gas argon for protection, controlling the laser power to be 180W, controlling the scanning speed to be 800mm/S, and performing additive manufacturing with the powder spreading thickness of 0.3mm to obtain an Alnico magnet;
fifth, solution treatment:
the Alnico magnet prepared in the fourth step is subjected to water cooling after heat preservation for 25min at 1200 ℃ to obtain a solid solution Alnico magnet;
sixth, heat treatment and aging of the magnetic field:
and (3) carrying out magnetic field heat treatment on the solid solution Alnico magnet obtained in the fifth step under the magnetic field of 6kOe at 835 ℃ for 40min, and then respectively carrying out heat preservation at 600 ℃ at 500 ℃ at 400 ℃ for 4h, 6h and 10h to finally obtain the Alnico magnet product.
FIG. 1 shows an Alnico composite magnet Fe prepared in this example 26.69 Co 38.40 Ni 13.63 Al 11.60 Ti 7.52 Cu 1.42 Nb 0.74 Is amplified, each of which is observedThe peaks are composed of two superimposed peaks, and respectively correspond to the peak values of the amplitude modulation decomposition alpha-alpha 1 +α 2 Alpha of the formed ferromagnetic Fe-Co-rich 1 Phase and weakly magnetic Al-Ni rich alpha 2 And (3) phase (C).
FIG. 2 shows an Alnico composite magnet Fe prepared in this example 26.69 Co 38.40 Ni 13.63 Al 11.60 Ti 7.52 Cu 1.42 Nb 0.74 The demagnetizing curve of (a) shows that its coercive force (Hc) is 2174.4Oe, remanence (Br) is 10.6kGs, and maximum magnetic energy product ((BH) max ) 8.6MGOe.
Example 2
Firstly, smelting to prepare a master alloy cast ingot:
according to alpha 1 Atomic percent composition Fe of alloy 40.0 Co 38.5 Ni 11.0 Al 7.3 Ti 1.5 Cu 1.2 Nb 0.5 And alpha is 2 Atomic percent composition Fe of alloy 15.0 Co 23.0 Ni 22.0 Al 29.4 Ti 7.0 Cu 3.0 Nb 0.6 The mass ratio of the required component raw materials is calculated respectively, and the required component blocky raw materials are weighed according to the mass percentage: pure Fe, pure Co, pure Ni, pure Al, pure Ti, pure Cu and pure Nb are used for preparing two alloy raw materials, and the vacuum degree is superior to 10 -2 Smelting in Pa vacuum induction smelting furnace at 1500-1660 deg.c for 30min to prepare alpha 1 Alloy and alpha 2 Melting alloy raw material of alloy into alpha 1 Master alloy ingot and alpha 2 Ingot casting of master alloy;
secondly, pulverizing:
preparing spherical powder from the two master alloy ingots prepared in the first step by using HERMIGA-100-20 high-pressure atomization powder preparation equipment of UK PSI (program specific information) company in 1650 ℃ and high-purity nitrogen atmosphere, wherein the particle size of the powder ranges from 1 mu m to 150 mu m;
thirdly, screening spherical powder:
alpha obtained in the second step 1 And alpha is 2 The two alloy spherical powders are respectively screened, and alpha with the grain diameter of 48-80 mu m is selected 1 Alloy powder, alpha of 38-48 mu m 2 Alloy powderCompounding at a mass ratio of 1.2:1, and mixing for 10min at a cylinder rotation speed of 20r/min by using a laboratory mixer with a volume of 5L;
fourth step, additive manufacturing:
filling spherical powder selected by the powder screened in the third step into a bin of Siam platinum S200 type additive manufacturing equipment, introducing a built cylindrical model phi 10mm multiplied by 10mm into the equipment, filling inert gas nitrogen for protection, controlling the laser power to be 200W, controlling the scanning speed to be 850mm/S, and performing additive manufacturing with the powder spreading thickness of 0.4mm to obtain an Alnico magnet;
fifth, solution treatment:
the Alnico magnet prepared in the fourth step is subjected to water cooling after heat preservation for 30min at 1150 ℃ to obtain a solid solution Alnico magnet;
sixth, heat treatment and aging of the magnetic field:
and (3) carrying out heat preservation for 20min at 835 ℃ on the solid solution Alnico magnet obtained in the fifth step under a magnetic field of 2kOe, and then carrying out aging treatment at 600 ℃, 500 ℃ and 400 ℃ for 5h respectively, thereby finally obtaining the Alnico magnet product.
FIG. 3 shows an Alnico composite magnet Fe prepared in this example 27.82 Co 30.95 Ni 16.36 Al 18.07 Ti 4.18 Cu 2.08 Nb 0.55 After the X-ray diffraction pattern is amplified, three main peaks are obviously divided into two peaks which respectively correspond to the alpha-alpha decomposed by amplitude modulation 1 +α 2 Alpha formed 1 Phase sum alpha 2 And (3) phase (C).
FIG. 4 shows an Alnico composite magnet Fe prepared in this example 27.82 Co 30.95 Ni 16.36 Al 18.07 Ti 4.18 Cu 2.08 Nb 0.55 In the transmission electron microscope image of (2), most of crystal grains have the size smaller than 1 micron and no crystal boundary phase, and each crystal grain is internally provided with nanocrystalline alpha with two lining degrees 1 Phase alpha 2 Phase composition.
FIG. 5 shows an Alnico composite magnet Fe prepared in this example 27.82 Co 30.95 Ni 16.36 Al 18.07 Ti 4.18 Cu 2.08 Nb 0.55 Is a demagnetizing curve of (2)Hc 945.7Oe and Br 9.5kGs, giving (BH) max 5.1MGOe.
Example 3
Firstly, smelting to prepare a master alloy cast ingot:
according to alpha 1 Atomic percent composition Fe of alloy 41.5 Co 35.0 Ni 12.0 Al 10.0 Ti 0.7 Cu 0.3 Nb 0.5 And alpha is 2 Atomic percent composition Fe of alloy 14.0 Co 20.0 Ni 32.0 Al 23.5 Ti 8.2 Cu 1.5 Nb 0.8 The mass ratio of the required component raw materials is calculated respectively, and the required component blocky raw materials are weighed according to the mass percentage: pure Fe, pure Co, pure Ni, pure Al, pure Ti, pure Cu and pure Nb are used for preparing two alloy raw materials, and the vacuum degree is superior to 10 -2 The arc melting furnace of Pa respectively prepares alpha 1 Alloy and alpha 2 Melting alloy raw material of alloy into alpha 1 Master alloy ingot and alpha 2 Ingot casting of master alloy;
secondly, pulverizing:
preparing spherical powder from the two master alloy ingots prepared in the first step by using HERMIGA-100-20 high-pressure atomization powder preparation equipment of UK PSI (program specific information) limited company in 1660 ℃ and high-purity nitrogen atmosphere, wherein the particle size of the powder ranges from 1 mu m to 150 mu m;
thirdly, screening spherical powder:
alpha obtained in the second step 1 And alpha is 2 The two alloy spherical powders are respectively screened, and alpha with the grain diameter of 48-80 mu m is selected 1 Alloy powder, alpha of 38-48 mu m 2 Compounding alloy powder in a mass ratio of 1.5:1, and mixing for 10min at a rotating speed of a charging barrel of 20r/min by using a mixer;
fourth step, additive manufacturing:
filling spherical powder selected by the powder screened in the third step into a bin of Siam platinum S200 type additive manufacturing equipment, introducing a built cylindrical model phi 10mm multiplied by 10mm into the equipment, filling inert gas nitrogen for protection, controlling the laser power to be 100W, controlling the scanning speed to be 600mm/S, and performing additive manufacturing with the powder spreading thickness of 0.5mm to obtain an Alnico magnet;
fifth, solution treatment:
carrying out solution treatment on the Alnico magnet prepared in the fourth step at 1150 ℃ for 20min, and then carrying out water cooling to obtain a solid solution Alnico magnet;
sixth, heat treatment and aging of the magnetic field:
and (3) carrying out heat treatment on the solid solution Alnico magnet obtained in the fifth step by heat preservation at 800 ℃ for 50min under a magnetic field of 10kOe, and then respectively carrying out three-stage aging treatment at 600 ℃, 500 ℃ and 400 ℃ for 4h, 6h and 10h to finally obtain the Alnico magnet product.
FIG. 6 shows an Alnico composite magnet Fe prepared in this example 29.97 Co 28.71 Ni 20.39 Al 15.66 Ti 3.84 Cu 0.80 Nb 0.63 Can observe that three main peaks are obviously divided into two peaks which respectively correspond to alpha-alpha decomposed by amplitude modulation 1 +α 2 Alpha formed 1 Phase sum alpha 2 And (3) phase (C).
FIG. 7 shows an Alnico composite magnet Fe prepared in this example 29.97 Co 28.71 Ni 20.39 Al 15.66 Ti 3.84 Cu 0.80 Nb 0.63 The scanning electron microscope image of (2) can be seen to be divided into gray contrast and white contrast, and the white area has slightly high Fe content and is alpha with two different components 1 Phase alpha 2 A special microstructure embedded with each other.
FIG. 8 shows an Alnico composite magnet Fe prepared in this example 29.97 Co 28.71 Ni 20.39 Al 15.66 Ti 3.84 Cu 0.80 Nb 0.63 Shows Hc of 855.6Oe and Br of 9.4. 9.4kGs, resulting in (BH) max 4.2MGOe.
Example 4
Firstly, smelting to prepare a master alloy cast ingot:
according to alpha 1 Atomic percent composition Fe of alloy 44.0 Co 37.0 Ni 9.0 Al 8.1 Ti 0.8 Cu 0.5 Nb 0.6 And alpha is 2 Atomic percent composition Fe of alloy 13.5 Co 30.0 Ni 23.5 Al 18.0 Ti 12.0 Cu 2.5 Nb 0.5 The mass ratio of the required component raw materials is calculated respectively, and the required component blocky raw materials are weighed according to the mass percentage: pure Fe, pure Co, pure Ni, pure Al, pure Ti, pure Cu and pure Nb are used for preparing two alloy raw materials, and the vacuum degree is superior to 10 -2 The induction melting furnace of Pa respectively prepares alpha 1 Alloy and alpha 2 Melting alloy raw material of alloy into alpha 1 Master alloy ingot and alpha 2 Ingot casting of master alloy;
secondly, pulverizing:
preparing spherical powder from the two master alloy ingots prepared in the first step by using HERMIGA-100-20 high-pressure atomization powder preparation equipment of UK PSI (program specific information) limited company in 1680 ℃ and high-purity nitrogen atmosphere, wherein the particle size of the powder ranges from 1 mu m to 150 mu m;
thirdly, screening spherical powder:
alpha obtained in the second step 1 And alpha is 2 The two alloy spherical powders are respectively screened, and alpha with the grain diameter of 48-80 mu m is selected 1 Alloy powder and alpha with particle diameter of 38-62 mu m 2 Compounding alloy powder in a mass ratio of 1.8:1, and mixing for 10min at a rotating speed of a charging barrel of 20r/min by using a mixer;
fourth step, additive manufacturing:
filling spherical powder selected by the powder screened in the third step into a bin of Siam platinum S200 type additive manufacturing equipment, introducing a built cylindrical model phi 10mm multiplied by 10mm into the equipment, filling inert gas argon for protection, controlling the laser power to be 250W, controlling the scanning speed to be 1050mm/S, and performing additive manufacturing with the powder spreading thickness of 0.3mm to obtain an Alnico magnet;
fifth, solution treatment:
carrying out water cooling on the Alnico magnet prepared in the fourth step after heat preservation for 30min at 1250 ℃ for solid solution treatment to obtain a solid solution Alnico magnet;
sixth, heat treatment and aging of the magnetic field:
and (3) carrying out heat treatment on the solid solution Alnico magnet obtained in the fifth step by heat preservation at 850 ℃ for 15min under a magnetic field of 6kOe, and then respectively carrying out three-stage aging treatment at 600 ℃, 500 ℃ and 400 ℃ for 2h, thereby finally obtaining the Alnico magnet product.
FIG. 9 shows an Alnico composite magnet Fe prepared in this example 32.65 Co 34.40 Ni 14.39 Al 11.78 Ti 4.97 Cu 1.24 Nb 0.56 Each peak is observed to have a fine bifurcation due to amplitude modulation decomposition alpha-alpha during the magnetic field heat treatment 1 +α 2 I.e. the alpha phase breaks down into alpha 1 Phase sum alpha 2 And (3) phase (C).
FIG. 10 shows an Alnico composite magnet Fe prepared in this example 32.65 Co 34.40 Ni 14.39 Al 11.78 Ti 4.97 Cu 1.24 Nb 0.56 Is a Fe-Co rich alpha in white region 1 The black region is Al-Ni rich alpha 2 And (3) phase (C).
FIG. 11 shows an Alnico composite magnet Fe prepared in this example 32.65 Co 34.40 Ni 14.39 Al 11.78 Ti 4.97 Cu 1.24 Nb 0.56 Shows that Hc is 1239.2Oe and Br is 11.8kGs, resulting in (BH) max 8.2MGOe.
Example 5
Firstly, smelting to prepare a master alloy cast ingot:
according to alpha 1 Atomic percent composition Fe of alloy 47.0 Co 35.5 Ni 7.4 Al 7.0 Ti 1.3 Cu 1.0 Nb 0.8 And alpha is 2 Atomic percent composition Fe of alloy 15.8 Co 28.0 Ni 23.0 Al 17.4 Ti 10.0 Cu 5.0 Nb 0.8 The mass ratio of the required component raw materials is calculated respectively, and the required component blocky raw materials are weighed according to the mass percentage: pure Fe, pure Co, pure Ni, pure Al, pure Ti, pure Cu and pure Nb are used for preparing two alloy raw materials, and the vacuum degree is superior to 10 -2 The induction melting furnace of Pa respectively prepares alpha 1 Alloy and alpha 2 Melting alloy raw material of alloy into alpha 1 Master alloy ingot and alpha 2 Ingot casting of master alloy;
secondly, pulverizing:
preparing spherical powder from the two master alloy ingots prepared in the first step by using HERMIGA-100-20 high-pressure atomization powder preparation equipment of UK PSI (program specific information) company in 1650 ℃ and high-purity argon atmosphere, wherein the particle size of the powder ranges from 1 mu m to 150 mu m;
thirdly, screening spherical powder:
alpha obtained in the second step 1 And alpha is 2 The two alloy spherical powders are respectively screened, and alpha with the grain diameter of 48-80 mu m is selected 1 Alloy powder and alpha with particle diameter of 45-75 mu m 2 Compounding alloy powder in a mass ratio of 2.1:1, and mixing for 10min at a cylinder rotating speed of 15r/min by using a mixer;
fourth step, additive manufacturing:
filling spherical powder selected by the powder of the third step into a bin of Siam platinum Lite BLT-S200 type additive manufacturing equipment, introducing a built cylindrical model with the diameter of phi of 10mm multiplied by 10mm into the equipment, filling inert gas argon for protection, controlling the laser power to be 220W, the scanning speed to be 1000mm/S, and carrying out additive manufacturing by paving the powder with the thickness of 0.4mm to obtain an Alnico magnet;
fifth, solution treatment:
carrying out water cooling on the Alnico magnet prepared in the fourth step after heat preservation for 40min at 1250 ℃ for solid solution treatment to obtain a solid solution Alnico magnet;
sixth, heat treatment and aging of the magnetic field:
and (3) carrying out magnetic field heat treatment on the solid solution Alnico magnet obtained in the fifth step under the magnetic field of 10kOe at 835 ℃ for 60min, and then respectively carrying out three-stage aging treatment at 600 ℃, 500 ℃ and 400 ℃ for 4h, 8h and 12h to finally obtain the Alnico magnet product.
FIG. 12 shows 18 Alnico composite magnets Fe prepared at one time in this example 36.19 Co 32.90 Ni 12.81 Al 10.60 Ti 4.32 Cu 2.39 Nb 0.80 Is a sample outline of the sample.
FIG. 13 shows an Alnico composite magnet Fe prepared in this example 36.19 Co 32.90 Ni 12.81 Al 10.60 Ti 4.32 Cu 2.39 Nb 0.80 The transmission electron microscope image of the composite magnet has clear amplitude modulation structure and enhanced orientation relation, and bright alpha 1 Alpha of phase black 2 The phases are inlaid and distributed and are orderly arranged.
FIG. 14 shows an Alnico composite magnet Fe prepared in this example 36.19 Co 32.90 Ni 12.81 Al 10.60 Ti 4.32 Cu 2.39 Nb 0.80 Demagnetizing curve along magnetic field direction and magnetic energy product (BH) change curve, hc is 1935.5Oe, br is 15.7. 15.7kGs, resulting in (BH) max 13.2MGOe.
Example 6
Firstly, smelting to prepare a master alloy cast ingot:
according to alpha 1 Atomic percent composition Fe of alloy 47.6 Co 40.0 Ni 6.0 Al 4.5 Ti 1.0 Cu 0.5 Nb 0.4 And alpha is 2 Atomic percent composition Fe of alloy 12.2 Co 22.0 Ni 30.0 Al 24.5 Ti 9.5 Cu 1.3 Nb 0.5 The mass ratio of the required component raw materials is calculated respectively, and the required component blocky raw materials are weighed according to the mass percentage: pure Fe, pure Co, pure Ni, pure Al, pure Ti, pure Cu and pure Nb are used for preparing two alloy raw materials, and the vacuum degree is superior to 10 -2 The induction melting furnace of Pa respectively prepares alpha 1 Alloy and alpha 2 Melting alloy raw material of alloy into alpha 1 Master alloy ingot and alpha 2 Ingot casting of master alloy;
secondly, pulverizing:
preparing spherical powder from the two master alloy ingots prepared in the first step by using TekSphereo-15 powder making equipment of a Talcner plasma system company at 1650 ℃ respectively, wherein the particle size of the powder ranges from 1 mu m to 150 mu m;
thirdly, screening spherical powder:
alpha obtained in the second step 1 And alpha is 2 The two alloy spherical powders are respectively screened, and alpha with the grain diameter of 48-80 mu m is selected 1 Alloy powder and alpha with particle diameter of 45-75 mu m 2 Alloy powder compounded in a mass ratio of 2.3:1, high MK2 type laboratory was usedThe effective mixing type mixer mixes for 20min at the rotating speed of a charging barrel of 18 r/min;
fourth step, additive manufacturing:
filling spherical powder selected by the powder screened in the third step into a bin of Tianjin radiming LiM-X150A type additive manufacturing equipment, introducing a built cylindrical model with the diameter of 10mm multiplied by 10mm into the equipment, filling inert gas nitrogen for protection, controlling the laser power to be 280W, the scanning speed to be 1100mm/s, and carrying out additive manufacturing on the powder spread thickness to be 0.5mm to obtain an Alnico magnet;
fifth, solution treatment:
carrying out water cooling on the Alnico magnet prepared in the fourth step after heat preservation for 45min at 1350 ℃ for solid solution treatment to obtain a solid solution Alnico magnet;
sixth, heat treatment and aging of the magnetic field:
and (3) carrying out heat treatment on the solid solution Alnico magnet obtained in the fifth step by heat preservation at 860 ℃ for 10min under a magnetic field of 2kOe, and then carrying out tertiary aging treatment at 600 ℃, 500 ℃ and 400 ℃ for 4h, 8h and 12h respectively, thus finally obtaining the Alnico magnet product.
FIG. 15 shows an Alnico composite magnet Fe prepared in this example 35.97 Co 34.09 Ni 13.88 Al 11.07 Ti 3.79 Cu 0.76 Nb 0.43 Is a sample morphology of (a).
FIG. 16 shows an Alnico composite magnet Fe prepared in this example 35.97 Co 34.09 Ni 13.88 Al 11.07 Ti 3.79 Cu 0.76 Nb 0.43 The X-ray diffraction pattern of (2) can be observed to be obviously divided into two peaks, because elements in the alloy undergo sufficient uphill diffusion in the process of magnetic field heat treatment, and alpha phase is decomposed into alpha 1 Phase sum alpha 2 And (3) phase (C).
FIG. 17 shows an Alnico composite magnet Fe prepared in this example 35.97 Co 34.09 Ni 13.88 Al 11.07 Ti 3.79 Cu 0.76 Nb 0.43 Shows Hc is 1203.4Oe and Br is 13.8kGs to give (BH) max 10.9MGOe.
Example 7
Firstly, smelting to prepare a master alloy cast ingot:
according to alpha 1 Atomic percent composition Fe of alloy 50.0 Co 30.0 Ni 8.5 Al 9.0 Ti 0.9 Cu 0.6 Nb 1.0 And alpha is 2 Atomic percent composition Fe of alloy 15.7 Co 33.0 Ni 19.0 Al 16.0 Ti 14.0 Cu 2.0 Nb 0.3 The mass ratio of the required component raw materials is calculated respectively, and the required component blocky raw materials are weighed according to the mass percentage: pure Fe, pure Co, pure Ni, pure Al, pure Ti, pure Cu and pure Nb are used for preparing two alloy raw materials, and the vacuum degree is superior to 10 -2 The induction melting furnace of Pa respectively prepares alpha 1 Alloy and alpha 2 Melting alloy raw material of alloy into alpha 1 Master alloy ingot and alpha 2 Ingot casting of master alloy;
secondly, pulverizing:
preparing spherical powder from the two master alloy ingots prepared in the first step by using TekSphereo-15 powder making equipment of a Talcner plasma system company at 1680 ℃ respectively, wherein the particle size of the powder ranges from 1 mu m to 150 mu m;
thirdly, screening spherical powder:
alpha obtained in the second step 1 And alpha is 2 The two alloy spherical powders are respectively screened, and alpha with the grain diameter of 48-75 mu m is selected 1 Alloy powder and alpha with particle diameter of 38-48 mu m 2 Compounding alloy powder in a mass ratio of 2.5:1, and mixing for 20min at a cylinder rotating speed of 18r/min by using a laboratory efficient mixing type mixer;
fourth step, additive manufacturing:
filling spherical powder selected by the powder screened in the third step into a bin of Siamplatin powder S200 type additive manufacturing equipment, introducing a built cube model of 10mm multiplied by 10mm into the equipment, filling inert gas nitrogen for protection, controlling laser power to be 120W, scanning speed to be 700mm/S, and paving powder thickness to be 0.3mm for additive manufacturing to obtain an Alnico magnet;
fifth, solution treatment:
carrying out water cooling on the Alnico magnet prepared in the fourth step after heat preservation for 50min at 1300 ℃ for solid solution treatment to obtain a solid solution Alnico magnet;
sixth, heat treatment and aging of the magnetic field:
and (3) carrying out magnetic field heat treatment on the solid solution Alnico magnet obtained in the fifth step under the magnetic field of 6kOe at 835 ℃ for 15min, and then respectively carrying out three-stage aging treatment at 600 ℃, 500 ℃ and 400 ℃ for 8h, 10h and 12h to finally obtain the Alnico magnet product.
FIG. 18 shows an Alnico composite magnet Fe prepared in this example 39.82 Co 30.89 Ni 11.61 Al 11.08 Ti 4.79 Cu 1.02 Nb 0.79 It can be seen that each peak consists of two peaks due to amplitude modulation decomposition α→α occurring during the heat treatment 1 +α 2 I.e. the alpha phase breaks down into alpha 1 Phase sum alpha 2 And (3) phase (C).
FIG. 19 shows an Alnico composite magnet Fe prepared in this example 39.82 Co 30.89 Ni 11.61 Al 11.08 Ti 4.79 Cu 1.02 Nb 0.79 After magnetic field heat treatment, obvious amplitude modulation structure is formed inside the crystal grain, alpha 1 And alpha is 2 Mosaic distribution, fe-Co rich alpha at grey strip position 1 The black region is Al-Ni rich alpha 2 The white particles at the grain boundaries are Cu.
FIG. 20 shows an Alnico composite magnet Fe prepared in this example 39.82 Co 30.89 Ni 11.61 Al 11.08 Ti 4.79 Cu 1.02 Nb 0.79 Shows that Hc is 1528.8Oe and Br is 11.6kGs, resulting in (BH) max 9.1MGOe.
Example 8
Firstly, smelting to prepare a master alloy cast ingot:
according to alpha 1 Atomic percent composition Fe of alloy 46.6 Co 36.0 Ni 10.2 Al 6.0 Ti 0.5 Cu 0.4 Nb 0.3 And alpha is 2 Atomic percent composition Fe of alloy 12.0 Co 23.0 Ni 24.7 Al 30.0 Ti 7.3 Cu 2.7 Nb 0.3 The mass ratio of the required component raw materials is calculated respectively, and the required component blocky raw materials are weighed according to the mass percentage: pure Fe, pure Co, pure Ni, pure Al, pure Ti, pure Cu and pure Nb are used for preparing two alloy raw materials, and the vacuum degree is superior to 10 -2 The induction melting furnace of Pa respectively prepares alpha 1 Alloy and alpha 2 Melting alloy raw material of alloy into alpha 1 Master alloy ingot and alpha 2 Ingot casting of master alloy;
secondly, pulverizing:
preparing spherical powder from the two master alloy ingots prepared in the first step by using HERMIGA-100-20 high-pressure atomization powder preparation equipment of UK PSI (program specific information) company in 1650 ℃ and high-purity argon atmosphere, wherein the particle size of the powder ranges from 1 mu m to 150 mu m;
thirdly, screening spherical powder:
alpha obtained in the second step 1 And alpha is 2 The two alloy spherical powders are respectively screened, and alpha with the grain diameter of 48-75 mu m is selected 1 Alloy powder and alpha with particle diameter of 38-62 mu m 2 Compounding alloy powder in a mass ratio of 2.8:1, and mixing for 20min at a cylinder rotating speed of 23r/min by using a double-motion mixing type mixer;
fourth step, additive manufacturing:
filling spherical powder selected by the powder screened in the third step into a bin of Tianjin radiming LiM-X150A type additive manufacturing equipment, introducing a built round ring body model with the outer diameter phi of 16mm, the inner diameter phi of 10mm and the height of 10mm into the equipment, filling inert gas argon for protection, controlling the laser power to be 150W, the scanning speed to be 750mm/s, and the powder spreading thickness to be 0.4mm for additive manufacturing to obtain an Alnico magnet;
fifth, solution treatment:
carrying out water cooling on the Alnico magnet prepared in the fourth step after heat preservation for 35min at 1250 ℃ to carry out solution treatment, thus obtaining a solid solution Alnico magnet;
sixth, heat treatment and aging of the magnetic field:
and (3) carrying out heat treatment on the solid solution Alnico magnet obtained in the fifth step by heat preservation at 870 ℃ for 30min under a magnetic field of 10kOe, and then carrying out tertiary aging treatment at 600 ℃, 500 ℃ and 400 ℃ for 4h, 6h and 10h respectively, thus finally obtaining the Alnico magnet product.
FIG. 21 shows an Alnico composite magnet Fe prepared in this example 36.52 Co 32.22 Ni 14.42 Al 12.99 Ti 2.48 Cu 1.07 Nb 0.30 The X-ray diffraction pattern of (2) is observed to be obviously divided into two peaks, and the phenomenon is due to the improvement of alpha in the alloy 1 The content of the phases, so that the elements in the alloy undergo sufficient uphill diffusion during the heat treatment of the magnetic field, and the alpha phase is decomposed into alpha 1 Phase sum alpha 2 And (3) phase (C).
FIG. 22 shows an Alnico composite magnet Fe prepared in this example 36.52 Co 32.22 Ni 14.42 Al 12.99 Ti 2.48 Cu 1.07 Nb 0.30 Can be seen to be classified into gray and white contrast, bright white alpha 1 The phase is distributed in a strip shape in a dispersing way 2 Is a kind of medium.
FIG. 23 shows an Alnico composite magnet Fe prepared in this example 36.52 Co 32.22 Ni 14.42 Al 12.99 Ti 2.48 Cu 1.07 Nb 0.30 Shows Hc of 1422.3Oe, remanence of 12.3kGs and maximum magnetic energy product of 8.9MGOe.
Example 9
Firstly, smelting to prepare a master alloy cast ingot:
according to alpha 1 Atomic percent composition Fe of alloy 45.0 Co 41.0 Ni 9.0 Al 4.0 Ti 0.3 Cu 0.3 Nb 0.4 And alpha is 2 Atomic percent composition Fe of alloy 13.0 Co 26.7 Ni 28.0 Al 21.7 Ti 8.0 Cu 2.0 Nb 0.6 The mass ratio of the required component raw materials is calculated respectively, and the required component blocky raw materials are weighed according to the mass percentage: pure Fe, pure Co, pure Ni, pure Al, pure Ti, pure Cu and pure Nb are used for preparing two alloy raw materials, and the vacuum degree is superior to 10 -2 The induction melting furnace of Pa respectively prepares alpha 1 Alloy and alpha 2 Alloy raw material melt of alloyRefining to alpha 1 Master alloy ingot and alpha 2 Ingot casting of master alloy;
secondly, pulverizing:
preparing spherical powder from the two master alloy ingots prepared in the first step by using HERMIGA-100-20 high-pressure atomization powder preparation equipment of UK PSI (program specific information) company in 1650 ℃ and high-purity argon atmosphere, wherein the particle size of the powder ranges from 1 mu m to 150 mu m;
thirdly, screening spherical powder:
alpha obtained in the second step 1 And alpha is 2 The two alloy spherical powders are respectively screened, and alpha with the grain diameter of 48-90 mu m is selected 1 Alloy powder and alpha with particle diameter of 38-75 mu m 2 Compounding alloy powder in a mass ratio of 3:1, and mixing for 30min at a rotating speed of a 21r/min charging barrel by using a JHT-5 double-motion mixing type mixer;
fourth step, additive manufacturing:
filling spherical powder selected by the powder screened in the third step into a bin of Siam platinum S200 type additive manufacturing equipment, introducing a built cylindrical model phi 10mm multiplied by 10mm into the equipment, filling inert gas nitrogen for protection, controlling the laser power to 300W, controlling the scanning speed to 1200mm/S, and performing additive manufacturing with the powder spreading thickness of 0.5mm to obtain an Alnico magnet;
fifth, solution treatment:
carrying out water cooling on the Alnico magnet prepared in the fourth step after heat preservation for 60min at 1350 ℃ for solid solution treatment to obtain a solid solution Alnico magnet;
sixth, heat treatment and aging of the magnetic field:
and (3) carrying out heat treatment on the solid solution Alnico magnet obtained in the fifth step by heat preservation at 900 ℃ for 25min under a magnetic field of 6kOe, and then respectively carrying out three-stage aging treatment by heat preservation at 600 ℃, 500 ℃ and 400 ℃ for 5h, thereby finally obtaining the Alnico magnet product.
FIG. 24 shows an Alnico composite magnet Fe prepared in this example 36.38 Co 37.15 Ni 14.12 Al 8.77 Ti 2.37 Cu 0.76 Nb 0.45 Can be observed to be clearly divided into two peaks due to amplitude-modulated decomposition of the alloy during heat treatmentAlpha phase decomposition into alpha 1 Phase sum alpha 2 And (3) phase (C).
FIG. 25 shows an Alnico composite magnet Fe prepared in this example 36.38 Co 37.15 Ni 14.12 Al 8.77 Ti 2.37 Cu 0.76 Nb 0.45 After heat treatment, the inside of the crystal grain forms an amplitude modulation structure alpha 1 And alpha is 2 Inlay distribution, bright color stripe position is Fe-Co rich alpha 1 The dark area is alpha rich in Al-Ni 2 。
FIG. 26 shows an Alnico composite magnet Fe prepared in this example 36.38 Co 37.15 Ni 14.12 Al 8.77 Ti 2.37 Cu 0.76 Nb 0.45 Shows Hc 1771.3Oe and Br 10.8kGs to give (BH) max 7.6MGOe.
The invention is not a matter of the known technology.
Claims (4)
1. A manufacturing method for manufacturing self-assembled AlNiCo magnet based on additive is characterized in that the method is based on additive manufacturing technology through self-assembly alpha 1 And alpha 2 Alloy method for preparing magnet, composite printing of two powders using selective laser melting technology SLM, alpha 1 And alpha is 2 The alloy composite mass ratio is 1:1-3:1, and the self-assembled aluminum nickel cobalt magnet is obtained;
wherein alpha is 1 The alloy has the atomic percentage composition of Fe x Co y Ni z Al u Ti v Cu w Nb t The subscript symbols x, y, z, u, v, w and t in the formula represent the atomic percent of the defined element composition range, wherein x is more than or equal to 38 and less than or equal to 50, y is more than or equal to 30 and less than or equal to 42,6 and less than or equal to 12, z is more than or equal to 30 and less than or equal to 12, u is more than or equal to 4 and less than or equal to 10,0.3 and less than or equal to 1.5,0.3 and w is more than or equal to 1.2,0.3 and less than or equal to 1, and the atomic percent is as follows: x+y+z+u+v+w+t=100; and alpha is 2 The alloy has the atomic percentage composition of Fe a Co b Ni c Al d Ti e Cu f Nb g The subscript a, b, c, d, e, f and g in the formula represent atomic percent of the element composition range, a is more than or equal to 12 and less than or equal to 16, b is more than or equal to 20 and less than or equal to 35, c is more than or equal to 18 and less than or equal to 32,d is 15-30, e is 7-14,1.5, f is 5,0.3-g is 0.8, and a+b+c+d+e+f+g=100.
2. The manufacturing method of the self-assembled aluminum-nickel-cobalt magnet based on additive manufacturing according to claim 1, wherein the coercive force of the self-assembled aluminum-nickel-cobalt magnet after heat treatment is 855.6-2174.4 Oe, the remanence is 9.4-15.7 kGs, and the maximum magnetic energy product is 4.2-13.2 MGOe.
3. The method for manufacturing the self-assembled alnico magnet based on additive manufacturing according to claim 1, comprising the steps of:
firstly, smelting to prepare a master alloy cast ingot:
according to alpha 1 Atomic percent composition Fe of alloy x Co y Ni z Al u Ti v Cu w Nb t And alpha is 2 Atomic percent composition Fe of alloy a Co b Ni c Al d Ti e Cu f Nb g The mass ratio of the raw materials of the components required by the two alloys is calculated respectively, and the bulk pure Fe, the pure Co, the pure Ni, the pure Al, the pure Ti, the pure Cu and the pure Nb are weighed according to the mass percentage respectively to finish the preparation of the two alloy raw materials; vacuum degree is better than 10 -2 Arc or induction melting furnace of Pa respectively to prepare alpha 1 Alloy and alpha 2 Melting alloy raw material of alloy into alpha 1 Master alloy ingot and alpha 2 Ingot casting of master alloy;
wherein, in the general formula, the symbols x, y, z, u, v, w and t represent the atomic percent of the composition range of the limiting elements, x is more than or equal to 38 and less than or equal to 50, y is more than or equal to 30 and less than or equal to 42,6 and less than or equal to 12, z is more than or equal to 30 and less than or equal to 12, u is more than or equal to 4 and less than or equal to 10,0.3 and less than or equal to 1.5,0.3 and w is more than or equal to 1.2,0.3 and less than or equal to 1, and the atomic percent is as follows: x+y+z+u+v+w+t=100; the symbols a, b, c, d, e, f and g represent the atomic percentages of the defined element composition ranges, wherein a is more than or equal to 12 and less than or equal to 16, b is more than or equal to 20 and less than or equal to 35, c is more than or equal to 18 and less than or equal to 32, d is more than or equal to 15 and less than or equal to 30, e is more than or equal to 7 and less than or equal to 14,1.5 and f is more than or equal to 5,0.3 and g is less than or equal to 0.8, and the atomic percentages satisfy a+b+c+d+e+f+g=100;
secondly, pulverizing:
respectively preparing spherical powder from the two master alloy ingots prepared in the first step by using atomizing powder making equipment, wherein the particle size of the powder ranges from 1 mu m to 150 mu m;
thirdly, screening spherical powder:
alpha obtained in the second step 1 And alpha is 2 The two alloy spherical powders are respectively screened, and alpha with the grain diameter of 38-90 mu m is selected 1 Alloy powder and alpha 2 Alloy powder according to alpha 1 :α 2 Compounding according to the mass ratio of h to 1, wherein h=1-3, and mixing for 2-30 min by using a mixer;
fourth step, additive manufacturing:
filling the spherical powder screened in the third step into a bin of additive manufacturing equipment, filling inert gas nitrogen or argon for protection, controlling the laser power to be 100-300W, the scanning speed to be 600-1200 mm/s, and paving the powder to be 0.3-0.5 mm for additive manufacturing to obtain an Alnico magnet;
fifth, solution treatment:
carrying out solution treatment on the Alnico magnet prepared in the fourth step for 20-60 min at 1150-1350 ℃ and then carrying out water cooling to obtain a solid solution Alnico magnet;
sixth, heat treatment and aging of the magnetic field:
and (3) carrying out magnetic field heat treatment on the solid solution Alnico magnet obtained in the fifth step under a magnetic field of 2-10 kOe at 800-900 ℃ for 10-60 min, and then carrying out aging treatment at 600-400 ℃ for 6-30 h to finally obtain the self-assembled AlNiCo magnet.
4. The method for manufacturing a self-assembled alnico magnet based on additive manufacturing according to claim 3, wherein in the third step of screening the spherical powder, for α 1 And alpha 2 The grain diameter of the alloy powder is 48-80 mu m.
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