CN111933375A - Novel samarium-iron-carbon-based anisotropic magnetic powder - Google Patents
Novel samarium-iron-carbon-based anisotropic magnetic powder Download PDFInfo
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- CN111933375A CN111933375A CN202010656991.4A CN202010656991A CN111933375A CN 111933375 A CN111933375 A CN 111933375A CN 202010656991 A CN202010656991 A CN 202010656991A CN 111933375 A CN111933375 A CN 111933375A
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- H—ELECTRICITY
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- 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
- H01F1/058—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IVa elements, e.g. Gd2Fe14C
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- 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
- H01F1/06—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 in the form of particles, e.g. powder
- H01F1/08—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 in the form of particles, e.g. powder pressed, sintered, or bound together
- H01F1/086—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 in the form of particles, e.g. powder pressed, sintered, or bound together sintered
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Abstract
The invention discloses novel samarium-iron-carbon-based anisotropic magnetic powder. Samarium iron nitrogen magnetic powder molecular formula be: (Sm)1‑x,REx)u(Fe1‑y‑z,Ty,Mz)vCw. Wherein RE is the combination of Ce/Y/Nd/La or Ce/Y/Nd/La and other rare earth elements, and x is more than or equal to 0.01 and less than or equal to 0.99; t is one or more 3d or 4d transition elements, y is more than or equal to 0 and less than or equal to 0.60; m is one or more of C, Si, Al, S, P, Cl, F, Ga, Sn and Sc, and z is more than or equal to 0 and less than or equal to 0.60; u is more than or equal to 1.7 and less than or equal to 2.3, v is more than or equal to 16 and less than or equal to 18, and w is more than or equal to 1.8 and less than or equal to 6; the atomic ratio of Fe in Fe, T and M is more than or equal to 40 at.%. The samarium-iron-carbon-based magnetic powder has higher maximum magnetic energy product, coercive force, residual magnetic induction strength and high-temperature service performance.
Description
Technical Field
The invention belongs to the field of rare earth permanent magnet materials, and relates to novel samarium-iron-carbon-based anisotropic magnetic powder which is mainly used for preparing anisotropic bonded permanent magnets and can also be used for preparing sintered magnets.
Background
Samarium iron nitrogen compound has uniaxial anisotropy, high saturation magnetization and high Curie temperature, and completely has the foundation of making permanent magnet. However, samarium iron nitrogen also has its fatal disadvantages: it is obtained by low-temperature nitriding by gas-solid phase reaction, and thus cannot be obtained by direct smelting of raw materials or conventional powder metallurgy processes. Therefore, they are metastable and completely decompose into α -Fe and rare earth nitrides at a temperature of about 700 ℃ or less, without returning to the original compound structure, and thus it is difficult to manufacture a high-performance magnet.
Prior to the discovery of rare earth nitrides, much research has been conducted on rare earth iron carbides. The direct smelting method can prepare rare earth iron carbide with low carbon content, and although the rare earth iron carbide also has the foundation for preparing permanent magnets, the carbon content is low, so that the local temperature of the magnets is low, the anisotropy field is not high, and high-performance magnets cannot be obtained. And samarium iron carbide with high carbon content has room temperature anisotropy field up to 15 +/-0.5T which is far higher than that of neodymium iron boron magnet, but the carbide obtained by the method is unstable like nitride due to the adoption of the gas-solid phase reaction method, and brings serious difficulty to the preparation of high-performance permanent magnet.
Meanwhile, the storage amount of Sm in the crust of the earth is only 1/5 of Nd, and the proportion of Sm in all rare earth is 3.2%. The problem of Sm shortage will manifest once samarium iron carbon is used on a large scale. Ce is the most abundant rare earth element in the earth crust and accounts for 30.2 percent of the earth crust. Meanwhile, the rare earth resource is accompanied to the fact that Nd and the like are utilized and meanwhile Ce is accumulated in a large amount. The substitution of Sm by the abundant rare earth Ce in samarium-iron carbon is of great significance.
According to the samarium-iron-carbon magnetic powder, 1 at% -99 at% of rare earth elements Ce/Y/Nd/La or Ce/Y/Nd/La and other rare earth elements are used for replacing Sm, so that the samarium-iron-carbon magnetic powder has high maximum magnetic energy product, coercive force and residual magnetic induction. Particularly, the maximum magnetic energy product of the samarium-iron-carbon-based rare earth permanent magnet powder prepared by partially replacing Sm with a combination of rare earth elements Ce/Y/Nd/La or Ce/Y/Nd/La and other rare earth elements is higher than that of pure samarium-iron-carbon rare earth permanent magnet powder. This is because, when Sm is partially replaced by a combination of a rare earth element Ce/Y/Nd/La or Ce/Y/Nd/La and other rare earth elements, the anisotropy of the samarium-iron-carbon based rare earth permanent magnet powder is reduced from the viewpoint of intrinsic magnetic energy, but the saturation magnetization is increased. Therefore, the coercive force of the magnetic powder is slightly reduced, the residual magnetic induction strength is improved, and the maximum magnetic energy product of the samarium-iron-carbon based rare earth permanent magnetic powder is maintained as a result of the combined action of the magnetic powder and the residual magnetic induction strength. Meanwhile, the addition of T and M can further inhibit or offset the reduction of magnetic powder anisotropy caused by the addition of RE. Thus, the synergistic effect of the addition of RE, T and M is to increase the saturation magnetization of the magnetic powder, slightly weakening, maintaining or even increasing the anisotropy of the magnetic powder, which still maintains a high curie temperature. Finally, the samarium-iron-carbon-based magnetic powder substituted by the high-abundance rare earth element Ce/Y/Nd/La or the combination of Ce/Y/Nd/La and other rare earth elements has high performance, namely, higher maximum magnetic energy product, coercive force, residual magnetic induction strength and high-temperature use performance.
The samarium-iron-carbon-based rare earth permanent magnet powder with high maximum magnetic energy product is prepared by partially replacing Sm with a combination of high-abundance rare earth elements Ce/Y/Nd/La or Ce/Y/Nd/La and other rare earth elements, and has important significance for expanding the application of high-abundance rare earth in rare earth permanent magnet materials and balancing the use of the rare earth elements.
Disclosure of Invention
The invention aims to provide a novel samarium-iron-carbon-based anisotropic magnetic powder aiming at the defects in the prior art.
The samarium-iron-carbon magnetic powder comprises the following components expressed by molecular formula: (Sm)1-x,REx)u(Fe1-y-z,Ty,Mz)vCw
In the formula, RE is the combination of rare earth elements Ce/Y/Nd/La or Ce/Y/Nd/La and other rare earth elements, and x is more than or equal to 0.01 and less than or equal to 0.99; t is one or more 3d or 4d transition elements, and y is more than or equal to 0 and less than or equal to 0.60; m is one or more of C, Si, Al, S, P, Cl, F, Ga, Sn and Sc, and z is more than or equal to 0 and less than or equal to 0.60. U is more than or equal to 1.7 and less than or equal to 2.3, v is more than or equal to 16 and less than or equal to 18, and w is more than or equal to 1.8 and less than or equal to 6.
The atomic ratio of Fe in Fe, T, and M should be 40 at.% or more.
The samarium-iron-carbon-based powder is obtained by partially substituting samarium by the combination of rare earth elements Ce/Y/Nd/La or Ce/Y/Nd/La and other rare earth elements. Although the substitution of Ce/Y/Nd/La causes the decrease of the coercive force of the magnetic powder, the remanence of the magnetic powder is improved. Therefore, the magnetic powder still has higher maximum energy product after partial replacement. Explained from the viewpoint of intrinsic magnetic properties, the addition of RE results in an increase in the saturation magnetization of the magnetic powder, with a slight decrease in anisotropy, and the addition of T and M serves to suppress or offset the decrease in anisotropy of the magnetic powder caused by the addition of RE. Thus, the synergistic effect of the addition of RE, T and M is to increase the saturation magnetization of the magnetic powder, slightly weakening, maintaining or even increasing the anisotropy of the magnetic powder, which still maintains a high curie temperature. Finally, the samarium-iron-carbon-based magnetic powder substituted by the high-abundance rare earth Ce/Y/Nd/La or the combination of Ce/Y/Nd/La and other rare earth elements has higher maximum magnetic energy product, coercive force, residual magnetic induction strength and high-temperature service performance, and has better comprehensive performance.
Drawings
FIG. 1 is an XRD pattern of the magnetic powder of example 1.
FIG. 2 is a hysteresis loop obtained by testing magnetic powder with VSM in example 1.
Figure 3 is an XRD pattern of the magnetic powder of example 2.
FIG. 4 is a hysteresis loop obtained by testing magnetic powder with VSM in example 2.
Figure 5 is an XRD pattern of the magnetic powder of example 3.
FIG. 6 is a hysteresis loop obtained by testing magnetic powder with VSM in example 3.
Figure 7 is an XRD pattern of the magnetic powder of example 7.
FIG. 8 is a hysteresis loop obtained by testing magnetic powder with VSM in example 7.
Figure 9 is an XRD pattern of the magnetic powder of example 8.
FIG. 10 is a hysteresis loop obtained by testing magnetic powder with VSM in example 8.
Detailed Description
The invention is further examined with the aid of specific examples and with the aid of the accompanying drawings.
In the following examples 1.8. ltoreq. w.ltoreq.6.
Example 1
Placing Sm, Ce, Fe and graphite as raw materials in a ball milling tank, milling for 5 hours, carrying out vacuum annealing at 850 ℃, placing in the ball milling tank again for 30 minutes, milling for 1 hour, and carrying out vacuum annealing at 600 ℃ for 30 minutes to obtain (Sm)0.7Ce0.3)2Fe17CwAnd (3) granules.
(Sm0.7Ce0.3)2Fe17CwThe maximum magnetic energy product, remanence and coercive force of the magnetic powder were 45.4MGOe, 20.1kGs and 7.8kOe, respectively. FIG. 1 is an XRD pattern of the magnetic powder of example 1. FIG. 2 is a hysteresis loop obtained by testing magnetic powder with VSM in example 1.
In contrast, Sm2Fe17CwThe maximum magnetic energy product, remanence and coercive force of the magnetic powder were 41.8MGOe, 12.3kGs and 8.3kOe, respectively. Sm prepared by the same process of maximum magnetic energy product and remanence ratio of high-abundance rare earth Ce-doped magnetic powder2Fe17CwThe magnetic powder is higher. The subsequent powder metallurgy process can be used for processing (Sm)0.7Ce0.3)2Fe17CwAnd manufacturing the magnetic powder into a sintered magnet.
Example 2
Using Sm, La, Fe, Ti and graphene as raw materials, carrying out arc melting to obtain an ingot, carrying out vacuum annealing at 850 ℃ for 30min, crushing, putting into a ball milling tank, carrying out milling for 1 hour, and carrying out vacuum annealing at 600 ℃ for 30min to obtain (Sm)0.5La0.5)2(Fe0.85Ti0.15)17CwAnd (3) granules. (Sm)0.5La0.5)2(Fe0.85Ti0.15)17CwThe maximum magnetic energy product, remanence and coercive force of the magnetic powder are respectively 62.8MGOe and 18.6kGs and 9.0 kOe. Figure 3 is an XRD pattern of the magnetic powder of example 2. FIG. 4 is a hysteresis loop obtained by testing magnetic powder with VSM in example 2.
In contrast, Sm2Fe17CwThe maximum magnetic energy product, remanence and coercive force of the magnetic powder were 41.8MGOe, 12.3kGs and 8.3kOe, respectively. Sm obtained by the process with the same maximum magnetic energy product, remanence and coercive force ratio of high-abundance rare earth La-doped magnetic powder2Fe17CwThe magnetic powder is higher. The subsequent injection molding and sintering of the handle (Sm) can be carried out0.6La0.4)2(Fe0.85Ti0.15)17CwAnd manufacturing the magnetic powder into a sintered magnet.
Example 3
Using Sm, Y, Fe, Zr and graphite as raw materials, obtaining an ingot by induction melting, crushing after vacuum annealing at 850 ℃ for 30min, then placing the ingot in a ball milling tank, grinding for 1 hour, and vacuum annealing at 600 ℃ for 30min to obtain (Sm)0.4Y0.6)2Fe15Zr2CwAnd (3) granules. (Sm)0.4Y0.6)2Fe15Zr2CwThe maximum magnetic energy product, remanence and coercive force of the magnetic powder were 42.1MGOe, 14.8kGs and 8.9kOe, respectively. Figure 5 is an XRD pattern of the magnetic powder of example 3. FIG. 6 is a hysteresis loop obtained by testing magnetic powder with VSM in example 3.
In contrast, Sm2Fe17CwThe maximum magnetic energy product, remanence and coercive force of the magnetic powder were 41.8MGOe, 12.3kGs and 8.3kOe, respectively. Sm obtained by the process with the same maximum magnetic energy product, remanence and coercive force ratio of high-abundance rare earth Y-doped magnetic powder2Fe17CwThe magnetic powder is higher. The subsequent additive manufacturing of the sintering handle (Sm)0.4Y0.6)2Fe15Zr2CwAnd manufacturing the magnetic powder into a sintered magnet.
Example 4
Using mixed rare earth of Sm, Fe, Cr, Al, graphite and lanthanum and cerium as raw material, placing the raw material in a ball-milling tank, milling for 5 hours, vacuum annealing at 850 deg.C, placing the raw material in the ball-milling tank again for 30 minutes, milling for 1 hour, vacuum annealing at 600 deg.C for 30 minutes to obtain (Sm)0.4Ce0.59La0.01)2(Fe0.4Cr0.3Al0.3)17CwAnd (3) granules. (Sm)0.4Ce0.59La0.01)2(Fe0.4Cr0.3Al0.3)17CwThe maximum magnetic energy product, remanence and coercive force of the magnetic powder were 49.9MGOe, 19.2kGs and 8.5kOe, respectively. Subsequently, the magnetic powder is subjected to an explosion method to obtain a sintered magnet.
Example 5
Using Sm, Nd, Fe, Mn, Ga, Ni, Cu and graphite powder as raw materials, placing the raw materials in a ball milling tank, milling for 5 hours, carrying out vacuum annealing at 850 ℃, placing the raw materials in the ball milling tank again for 30 minutes, milling for 1 hour, and carrying out vacuum annealing at 600 ℃ for 30 minutes to obtain (Sm)0.4Nd0.6)2(Fe0.8873Mn0.11Ga0.0009Ni0.0009Cu0.0009)17CwAnd (3) granules. (Sm)0.4Nd0.6)2(Fe0.8873Mn0.11Ga0.0009Ni0.0009Cu0.0009)17CwThe maximum magnetic energy product, remanence and coercive force of the magnetic powder were 53.3MGOe, 21.4kGs and 10.2kOe, respectively. And then, mixing the magnetic powder with polyamide resin, and performing injection molding to obtain the magnet.
Example 6
With Sm2O3、La2O3、Fe2O3、CoO2Glucose is used as a raw material, hydrogen is introduced into a tube furnace at 850 ℃ for heat preservation for 120min, then the raw material is placed into a ball milling tank for ball milling for 1 hour, and vacuum annealing is carried out at 600 ℃ for 30min to obtain (Sm)0.3La0.7)2(Fe0.4Co0.6)17CwAnd (3) granules. (Sm)0.3La0.7)2(Fe0.4Co0.6)17CwThe maximum magnetic energy product, remanence and coercive force of the magnetic powder were 60.9MGOe, 20.5kGs and 16.5kOe, respectively. And then, tamping the magnetic powder, and sealing in a copper-clad sleeve. Then the copper-clad sleeve is placed in a mould, and the copper-clad sleeve is struck by a flying body through the discharge of an explosion spray gun to obtain the magnet.
Example 7
Placing Sm, La, Fe and graphite as raw materials in a ball milling tank, milling for 5 hours, carrying out vacuum annealing at 850 ℃, placing in the ball milling tank again for 30 minutes, milling for 1 hour, and carrying out vacuum annealing at 600 ℃ for 30 minutes to obtain (Sm)0.9La0.1)2Fe17CwAnd (3) granules. (Sm)0.9La0.1)2Fe17CwThe maximum magnetic energy product, remanence and coercive force of the magnetic powder were 39.0MGOe, 13.6kGs and 11.2kOe, respectively. Figure 7 is an XRD pattern of the magnetic powder of example 7. FIG. 8 is a hysteresis loop obtained by testing magnetic powder with VSM in example 7.
Example 8
Placing Sm, Ce, Nd, Fe and graphite as raw materials in a ball milling tank, milling for 5 hours, carrying out vacuum annealing at 850 ℃, placing in the ball milling tank again for 30 minutes, milling for 1 hour, and carrying out vacuum annealing at 600 ℃ for 30 minutes to obtain (Sm)0.5Ce0.25Nd0.25)2Fe17CwAnd (3) granules. (Sm)0.5Ce0.25Nd0.25)2Fe17CwThe maximum magnetic energy product, remanence and coercive force of the magnetic powder were 38.4MGOe, 13.0kGs and 14.4kOe, respectively. Figure 9 is an XRD pattern of the magnetic powder of example 8. FIG. 10 is a hysteresis loop obtained by testing magnetic powder with VSM in example 8.
Example 9
Using mixed rare earth of Sm, Fe, Cr, Al, graphite and lanthanum and cerium as raw material, placing the raw material in a ball-milling tank, milling for 5 hours, vacuum annealing at 850 deg.C, placing the raw material in the ball-milling tank again for 30 minutes, milling for 1 hour, vacuum annealing at 600 deg.C for 30 minutes to obtain (Sm)0.4Ce0.4La0.2)2(Fe0.4Cr0.3Al0.3)17CwAnd (3) granules. (Sm)0.4Ce0.4La0.2)2(Fe0.4Cr0.3Al0.3)17CwThe maximum magnetic energy product, remanence and coercive force of the magnetic powder were 48.7MGOe, 18.1kGs and 8.2kOe, respectively.
The above embodiments are not intended to limit the present invention, and the present invention is not limited to the above embodiments, and all embodiments are within the scope of the present invention as long as the requirements of the present invention are met.
Claims (2)
1. The utility model provides a novel samarium iron carbon base anisotropic magnetic, its characterized in that samarium iron nitrogen magnetic is the composition that molecular formula shows is: (Sm)1-x,REx)u(Fe1-y-z,Ty,Mz)vCw；
In the formula, RE is the combination of rare earth elements Ce/Y/Nd/La or Ce/Y/Nd/La and other rare earth elements, and x is more than or equal to 0.01 and less than or equal to 0.99; t is one or more 3d or 4d transition elements, and y is more than or equal to 0 and less than or equal to 0.60; m is one or more of C, Si, Al, S, P, Cl, F, Ga, Sn and Sc, and z is more than or equal to 0 and less than or equal to 0.60; u is more than or equal to 1.7 and less than or equal to 2.3, v is more than or equal to 16 and less than or equal to 18, and w is more than or equal to 1.8 and less than or equal to 6;
the atomic ratio of Fe in Fe, T and M is more than or equal to 40 at.%.
2. The high abundance rare earth Ce/Y/Nd/La substituted samarium-iron-nitrogen based magnetic powder with high maximum energy product of claim 1, wherein T is one or more of Co, Ni, Cu, Mn, Cr, Mo, Ta, W, Hf, Nb, V, Zr, Ti, Zn, Ru, Rh, Pd, Pt.
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Citations (5)
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| JPH02145739A (en) * | 1988-11-28 | 1990-06-05 | Toshiba Corp | Permanent magnet material and permanent magnet |
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| CN1281055A (en) * | 1999-07-14 | 2001-01-24 | 中国科学院金属研究所 | Process for preparing permanent-magnetic material of Sm-Fe-C compound |
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2020
- 2020-07-09 CN CN202010656991.4A patent/CN111933375A/en active Pending
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| JPH02145739A (en) * | 1988-11-28 | 1990-06-05 | Toshiba Corp | Permanent magnet material and permanent magnet |
| CN1089385A (en) * | 1992-12-26 | 1994-07-13 | 中国科学院物理研究所 | A kind of high stable rare-earth-iron-permanent-magnetic carbide and preparation method thereof |
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| TRIBHUWAN PANDCY等: "Tuning the Magnetic Properties and Structural Stabilities of the 2-17-3 Magnets Sm2Fe17X3 (X =C, N) by Substituting La or Ce for Sm", 《PHYSICAL REVIEW APPLIED》 * |
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