CN113421762B - Preparation method of high-performance samarium-iron-nitrogen magnet - Google Patents
Preparation method of high-performance samarium-iron-nitrogen magnet Download PDFInfo
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- CN113421762B CN113421762B CN202110748890.4A CN202110748890A CN113421762B CN 113421762 B CN113421762 B CN 113421762B CN 202110748890 A CN202110748890 A CN 202110748890A CN 113421762 B CN113421762 B CN 113421762B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
- H01F41/026—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 protecting methods against environmental influences, e.g. oxygen, by surface treatment
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
- H01F41/0266—Moulding; Pressing
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
- H01F41/0293—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 diffusion of rare earth elements, e.g. Tb, Dy or Ho, into permanent magnets
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Abstract
The invention discloses a preparation method of a high-performance samarium-iron-nitrogen magnetThe method belongs to the technical field of magnetic materials. The preparation method comprises the following steps: by preparing Sm 2 Fe 17 Carrying out nitriding aging treatment on the alloy cast ingot to obtain a samarium-iron-nitrogen alloy cast ingot; a high-entropy alloy rapid quenching belt is obtained by a melt rapid quenching method, and the rapid quenching belt is crushed by a planetary ball milling process to obtain a mixed solution; in-process that carries out the high-energy ball-milling at samarium iron nitrogen alloy ingot casting to the mode of spraying is sprayed the mixed solution to samarium iron nitrogen alloy powder, makes the effective cladding of high entropy alloy powder on samarium iron nitrogen powder surface, effectively promotes the area of contact between diffuser and magnetic, improves diffusion efficiency, and through N 2 And (4) carrying out nitriding tempering heat treatment under protection to obtain the high-performance samarium-iron-nitrogen magnet. The method has the advantages of simple process and easy operation, and is favorable for the application of the high-performance samarium-iron-nitrogen magnet in more permanent magnet devices so as to meet the market demand.
Description
Technical Field
The invention relates to the technical field of magnetic materials, in particular to a preparation method of a high-performance samarium-iron-nitrogen magnet.
Background
The rare earth permanent magnetic material is an alloy formed by elements such as rare earth Nd, sm, pr and the like and some transition metal elements, is a special material with permanent magnetic property and is prepared by a specific process, and is widely applied to motors, generators, nuclear magnetic resonance imagers, microwave communication technologies, instruments and other devices and equipment which need permanent magnetic fields at present. At present, the most widely used rare earth permanent magnet materials are mainly: smCo 5 Type Sm 2 Co 17 Type and NdFeB system permanent magnets. Meanwhile, smFeN permanent magnet materials are valued by people due to the excellent magnetic property and good temperature stability since the coming of the world, and become one of the research hotspots of rare earth permanent magnet materials at home and abroad as the only permanent magnet which can exceed NdFeB in performance. The high-entropy alloy has a plurality of composition elements, so that various unique effects such as a high-entropy effect, a lattice distortion effect, a delayed diffusion effect, a cocktail effect and the like are endowed to the high-entropy alloy, and meanwhile, the mechanical properties of the high-entropy alloy are most extensively and deeply researched at present. High entropy alloys tend to have very high strength and hardness due to the solid solution strengthening effect and strong lattice distortion effect of the atoms within the alloy.
Therefore, in the process of carrying out high-energy ball milling on the samarium iron nitrogen alloy ingot, the invention sprays the mixed solution of FeCoNiMnGa powder and gasoline into the samarium iron nitrogen alloy powder in a spraying mode, ball milling and spraying are carried out simultaneously, so that the FeCoNiMnGa powder is effectively coated on the surface of the samarium iron nitrogen powder, the contact area between a diffuser and magnetic powder is effectively increased, the diffusion efficiency is improved, and the N is used for 2 And performing primary and secondary nitriding tempering heat treatment under protection to obtain the high-performance samarium-iron-nitrogen magnet.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a preparation method of a high-performance samarium-iron-nitrogen magnet.
The preparation method of the high-performance samarium-iron-nitrogen magnet comprises the following steps:
(1) Preparing Sm as nominal component by arc melting 2 Fe 17 Then casting the alloy ingot with N at 300 to 700 DEG C 2 Nitriding aging treatment is carried out in gas protection, wherein the nitriding aging treatment time is 2 to 15 hours, and a samarium-iron-nitrogen alloy cast ingot is obtained;
(2) Preparing a high-entropy alloy rapid quenching belt with nominal component FeCoNiMnGa by a melt rapid quenching method, wherein the rotating speed of a copper roller is 10-50 m/s; then crushing the rapid quenching zone under the protection of gasoline by a planetary ball milling process to prepare a mixed solution with the powder particle size of 10 to 30 mu m, wherein the ball milling time is 2 to 10 hours;
(3) Carrying out high-energy ball milling on the samarium iron nitrogen alloy cast ingot obtained in the step (1), and simultaneously spraying the mixed solution of FeCoNiMnGa powder and gasoline obtained in the step (2) into the samarium iron nitrogen alloy powder in a spraying manner, and carrying out ball milling and spraying at the same time until the ball milling is finished; the mixed liquid of the FeCoNiMnGa powder and the gasoline accounts for 5 to 30 percent of the weight of the samarium-iron-nitrogen alloy ingot, wherein the FeCoNiMnGa powder accounts for 5 to 30 percent of the total weight of the mixed liquid;
(4) Preparing a pressed blank by the mixed powder obtained in the step (3) through a magnetic field orientation forming low-temperature auxiliary technology;
(5) Putting the pressed blank obtained in the step (4) in N 2 And performing primary and secondary nitriding tempering heat treatment in gas protection to obtain the high-performance samarium-iron-nitrogen magnet.
Further, the time of the high-energy ball milling in the step (3) is 2 to 8 hours.
Further, the magnetic field intensity of the magnetic field orientation molding low-temperature auxiliary technology in the step (4) is 1 to 3T, the pressure is 20 to 150 MPa, and the temperature is 50 to 150 ℃.
Further, the temperature of the first-stage tempering heat treatment of the first-stage and second-stage nitriding tempering heat treatments in the step (5) is 600 to 950 ℃, the heating rate is 1 to 10 ℃/min, the heat preservation time is 5 to 15 h, and then the mixture is rapidly cooled to room temperature; the temperature of the secondary tempering heat treatment is 300-600 ℃, the heating rate is 1-10 ℃/min, the heat preservation time is 1-5 h, and then the temperature is rapidly cooled to the room temperature.
Compared with the prior art, the invention has the following advantages and beneficial effects: in the process of carrying out high-energy ball milling on the samarium-iron-nitrogen alloy ingot, the mixed solution of FeCoNiMnGa powder and gasoline is sprayed into the samarium-iron-nitrogen alloy powder in a spraying manner, ball milling and spraying are carried out simultaneously, so that the FeCoNiMnGa powder is effectively coated on the surface of the samarium-iron-nitrogen alloy powder, and the component elements of FeCoNiMnGa high-entropy alloy are regularly and multi-compositely added in a samarium-iron-nitrogen magnet; meanwhile, the spraying mode in the process effectively improves the contact area between the diffuser and the magnetic powder, improves the diffusion efficiency, and passes through N 2 And performing primary and secondary nitriding and tempering heat treatment under protection to obtain the high-performance samarium-iron-nitrogen magnet.
Detailed Description
The present invention will be described in further detail with reference to examples, but the present invention is not limited to only the following examples.
Example 1
(1) Preparing Sm serving as nominal component by adopting electric arc melting 2 Fe 17 The alloy ingot of (2), followed by N-casting the alloy ingot at 300 DEG C 2 Nitriding aging treatment is carried out in gas protection, and the time of the nitriding aging treatment is 2 h, so that a samarium-iron-nitrogen alloy cast ingot is obtained;
(2) Preparing a high-entropy alloy rapid quenching belt with nominal components of FeCoNiMnGa by adopting a melt rapid quenching method, wherein the rotating speed of a copper roller is 10 m/s; then crushing the rapid quenching belt under the protection of gasoline by a planetary ball milling process to prepare mixed liquid with the powder particle size of 10 mu m, wherein the ball milling time is 2 hours;
(3) Carrying out high-energy ball milling on the samarium iron nitrogen alloy cast ingot obtained in the step (1), wherein the high-energy ball milling time is 2 h, and simultaneously spraying the mixed solution of FeCoNiMnGa powder and gasoline obtained in the step (2) into the samarium iron nitrogen alloy powder in a spraying manner, and carrying out ball milling and spraying at the same time until the ball milling is finished; the mixed liquid of FeCoNiMnGa powder and gasoline accounts for 5% of the weight of the samarium iron nitrogen alloy cast ingot, wherein the FeCoNiMnGa powder accounts for 5% of the total weight of the mixed liquid;
(4) Preparing a pressed blank by using the mixed powder magnetic field orientation forming low-temperature auxiliary technology obtained in the step (3), wherein the magnetic field intensity is 1T, the pressure is 30 MPa, and the temperature is 50 ℃;
(5) Putting the pressed blank obtained in the step (4) in N 2 Performing primary and secondary nitriding and tempering heat treatment in gas protection,
wherein the temperature of the first-stage tempering heat treatment is 680 ℃, the heating rate is 8 ℃/min, the heat preservation time is 5 h, and then the temperature is rapidly cooled to the room temperature; the temperature of the secondary tempering heat treatment is 600 ℃, the heating rate is 8 ℃/min, the heat preservation time is 1 h, then the secondary tempering heat treatment is carried out by quenching to the room temperature, and finally the samarium-iron-nitrogen magnet is obtained.
Through the tests of magnetic property and fracture toughness property, the samarium-iron-nitrogen magnet prepared by the invention has the coercive force of 1928 kA/m and the magnetic energy product of 235.2 kJ/m 3 The fracture toughness is 19.2 MN m -3/2 。
Example 2
(1) Preparing Sm as nominal component by arc melting 2 Fe 17 The alloy ingot of (2), followed by N at 500 ℃ of the alloy ingot 2 Nitriding aging treatment is carried out in gas protection, and the nitriding aging treatment time is 8 h, so that samarium-iron-nitrogen alloy cast ingots are obtained;
(2) Preparing a high-entropy alloy rapid quenching belt with nominal components of FeCoNiMnGa by adopting a melt rapid quenching method, wherein the rotating speed of a copper roller is 28 m/s; then crushing the rapid quenching zone under the protection of gasoline by a planetary ball milling process to prepare mixed liquor with the powder particle size of 20 microns, wherein the ball milling time is 6 hours;
(3) Carrying out high-energy ball milling on the samarium iron nitrogen alloy cast ingot obtained in the step (1), wherein the high-energy ball milling time is 6 h, and simultaneously spraying the mixed solution of FeCoNiMnGa powder and gasoline obtained in the step (2) into the samarium iron nitrogen alloy powder in a spraying manner, and carrying out ball milling and spraying at the same time until the ball milling is finished; the mixed solution of FeCoNiMnGa powder and gasoline accounts for 15% of the weight of the samarium-iron-nitrogen alloy ingot, wherein the FeCoNiMnGa powder accounts for 15% of the total weight of the mixed solution;
(4) Preparing a pressed blank by using the mixed powder magnetic field orientation forming low-temperature auxiliary technology obtained in the step (3), wherein the magnetic field intensity is 2T, the pressure is 80 MPa, and the temperature is 100 ℃;
(5) Putting the pressed blank obtained in the step (4) in N 2 Performing primary and secondary nitriding and tempering heat treatment in gas protection,
wherein the temperature of the first-stage tempering heat treatment is 780 ℃, the heating rate is 6 ℃/min, the heat preservation time is 10 h, and then the temperature is rapidly cooled to the room temperature; the temperature of the secondary tempering heat treatment is 400 ℃, the heating rate is 6 ℃/min, the heat preservation time is 3 h, and then the secondary tempering heat treatment is carried out by quenching to room temperature, thus obtaining the samarium-iron-nitrogen magnet.
Through magnetic performance and fracture toughness tests, the samarium-iron-nitrogen magnet prepared by the method has the coercive force of 2058 kA/m and the magnetic energy product of 248.7 kJ/m 3 The fracture toughness is 21.5 MN m -3/2 。
Example 3
(1) Preparing Sm serving as nominal component by adopting electric arc melting 2 Fe 17 The alloy ingot of (2) is subsequently subjected to N at 700 DEG C 2 Nitriding aging treatment is carried out in gas protection, and the time of the nitriding aging treatment is 15 h, so that a samarium-iron-nitrogen alloy cast ingot is obtained;
(2) Preparing a high-entropy alloy rapid quenching belt with nominal components of FeCoNiMnGa by adopting a melt rapid quenching method, wherein the rotating speed of a copper roller is 45 m/s; then crushing the rapid quenching belt under the protection of gasoline by a planetary ball milling process to prepare a mixed solution with the powder particle size of 30 mu m, wherein the ball milling time is 9 hours;
(3) Carrying out high-energy ball milling on the samarium iron nitrogen alloy cast ingot obtained in the step (1), wherein the high-energy ball milling time is 8 h, and simultaneously spraying the mixed solution of FeCoNiMnGa powder and gasoline obtained in the step (2) into the samarium iron nitrogen alloy powder in a spraying manner, and carrying out ball milling and spraying at the same time until the ball milling is finished; the mixed solution of FeCoNiMnGa powder and gasoline accounts for 28 percent of the weight of the samarium iron nitrogen alloy cast ingot, wherein the FeCoNiMnGa powder accounts for 28 percent of the total weight of the mixed solution;
(4) Preparing a pressed blank by using the mixed powder magnetic field orientation forming low-temperature auxiliary technology obtained in the step (3), wherein the magnetic field intensity is 3T, the pressure is 140 MPa, and the temperature is 150 ℃;
(5) Putting the green compact obtained in the step (4) in N 2 Performing primary and secondary nitriding and tempering heat treatment in gas protection,
wherein the temperature of the first-stage tempering heat treatment is 880 ℃, the heating rate is 2 ℃/min, the heat preservation time is 15 h, and then the temperature is rapidly cooled to the room temperature; the temperature of the secondary tempering heat treatment is 300 ℃, the heating rate is 2 ℃/min, the heat preservation time is 5 h, and then the secondary tempering heat treatment is carried out by quenching to room temperature, thus obtaining the samarium-iron-nitrogen magnet.
Through the magnetic performance and fracture toughness tests of the samarium iron nitrogen magnet prepared by the invention, the coercive force is 2199 kA/m, and the magnetic energy product is 255.1 kJ/m 3 The fracture toughness is 23.7 MN m -3/2 。
Claims (4)
1. A preparation method of a high-performance samarium-iron-nitrogen magnet is characterized by comprising the following steps:
(1) Preparing Sm serving as nominal component by adopting electric arc melting 2 Fe 17 Then casting the alloy ingot with N at 300 to 700 DEG C 2 Nitriding aging treatment is carried out in gas protection, and the time of the nitriding aging treatment is 2 to 15 hours, so that a samarium-iron-nitrogen alloy cast ingot is obtained;
(2) Preparing a high-entropy alloy rapid quenching belt with nominal component FeCoNiMnGa by a melt rapid quenching method, wherein the rotating speed of a copper roller is 10-50 m/s; then crushing the rapid quenching belt under the protection of gasoline by a planetary ball milling process to prepare a mixed solution with the powder particle size of 10 to 30 microns, wherein the ball milling time is 2 to 10 hours;
(3) Carrying out high-energy ball milling on the samarium iron nitrogen alloy ingot obtained in the step (1), and simultaneously spraying the mixed solution of FeCoNiMnGa powder and gasoline obtained in the step (2) into the samarium iron nitrogen alloy powder in a spraying manner, and carrying out ball milling and spraying at the same time until the ball milling is finished; the mixed solution of FeCoNiMnGa powder and gasoline accounts for 5 to 30 percent of the weight of the samarium-iron-nitrogen alloy cast ingot, wherein the FeCoNiMnGa powder accounts for 5 to 30 percent of the total weight of the mixed solution;
(4) Preparing a pressed blank by the mixed powder obtained in the step (3) through a magnetic field orientation forming low-temperature auxiliary technology;
(5) Putting the green compact obtained in the step (4) in N 2 And performing primary and secondary nitriding tempering heat treatment in gas protection to obtain the high-performance samarium-iron-nitrogen magnet.
2. The method for preparing a high performance samarium iron nitrogen magnet in accordance with claim 1, further comprising: the time of the high-energy ball milling in the step (3) is 2 to 8 hours.
3. The method for preparing a high performance samarium iron nitrogen magnet in accordance with claim 1, further comprising: the magnetic field strength of the magnetic field orientation molding low-temperature auxiliary technology in the step (4) is 1 to 3T, the pressure is 20 to 150 MPa, and the temperature is 50 to 150 ℃.
4. The method for preparing a high performance samarium iron nitrogen magnet in accordance with claim 1, further comprising: the temperature of the first-stage tempering heat treatment of the first-stage and second-stage nitriding tempering heat treatments in the step (5) is 600 to 950 ℃, the heating rate is 1 to 10 ℃/min, the heat preservation time is 5 to 15 h, and then the materials are quenched to room temperature; the temperature of the secondary tempering heat treatment is 300 to 600 ℃, the heating rate is 1 to 10 ℃/min, the heat preservation time is 1 to 5 h, and then the secondary tempering heat treatment is quenched to the room temperature.
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Citations (7)
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| JPH06204016A (en) * | 1992-03-18 | 1994-07-22 | Kinya Adachi | Manufacture of rare earth intermetallic compound magnetic material composed of rare earth compound |
| JP2006351688A (en) * | 2005-06-14 | 2006-12-28 | Sumitomo Metal Mining Co Ltd | Producing method of samarium-iron-nitrogen-based magnet fine powder |
| CN102184776A (en) * | 2011-02-24 | 2011-09-14 | 中国计量学院 | Preparation method of rare earth complex crystal boundary modification sintered neodymium-iron-boron magnetic body |
| CN109036752A (en) * | 2018-08-14 | 2018-12-18 | 徐靖才 | A kind of method that nitrogen class rare earth compounding prepares high-coercive force samarium iron nitrogen magnet |
| CN112382498A (en) * | 2020-11-23 | 2021-02-19 | 杨杭福 | Preparation method of high-coercivity and high-energy product diffusion samarium-iron-nitrogen magnet |
| CN112635145A (en) * | 2021-01-13 | 2021-04-09 | 泮敏翔 | Rare earth-free composite magnetic powder and preparation method thereof |
| CN112652433A (en) * | 2021-01-13 | 2021-04-13 | 泮敏翔 | Anisotropic composite magnet and preparation method thereof |
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2021
- 2021-07-02 CN CN202110748890.4A patent/CN113421762B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06204016A (en) * | 1992-03-18 | 1994-07-22 | Kinya Adachi | Manufacture of rare earth intermetallic compound magnetic material composed of rare earth compound |
| JP2006351688A (en) * | 2005-06-14 | 2006-12-28 | Sumitomo Metal Mining Co Ltd | Producing method of samarium-iron-nitrogen-based magnet fine powder |
| CN102184776A (en) * | 2011-02-24 | 2011-09-14 | 中国计量学院 | Preparation method of rare earth complex crystal boundary modification sintered neodymium-iron-boron magnetic body |
| CN109036752A (en) * | 2018-08-14 | 2018-12-18 | 徐靖才 | A kind of method that nitrogen class rare earth compounding prepares high-coercive force samarium iron nitrogen magnet |
| CN112382498A (en) * | 2020-11-23 | 2021-02-19 | 杨杭福 | Preparation method of high-coercivity and high-energy product diffusion samarium-iron-nitrogen magnet |
| CN112635145A (en) * | 2021-01-13 | 2021-04-09 | 泮敏翔 | Rare earth-free composite magnetic powder and preparation method thereof |
| CN112652433A (en) * | 2021-01-13 | 2021-04-13 | 泮敏翔 | Anisotropic composite magnet and preparation method thereof |
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