CN111230127A - Preparation method of composite magnetic powder - Google Patents
Preparation method of composite magnetic powder Download PDFInfo
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- CN111230127A CN111230127A CN202010116293.5A CN202010116293A CN111230127A CN 111230127 A CN111230127 A CN 111230127A CN 202010116293 A CN202010116293 A CN 202010116293A CN 111230127 A CN111230127 A CN 111230127A
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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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C12/00—Alloys based on antimony or bismuth
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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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- 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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
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Abstract
The invention discloses a preparation method of composite magnetic powder, which comprises the following steps: according to the nominal composition MnxBi100‑xMelting an alloy ingot (the mole fraction x =45,50, 55), and coarsely crushing the alloy ingot; mn to be produced by the inventionxBi100‑xPlacing the alloy ingot fragments into a mortar for coarse grinding, screening through a 100-mesh grid sieve after grinding, and obtaining MnxBi100‑xPerforming low-energy ball milling compounding on the alloy powder; the obtained MnxBi100‑xTaking a proper amount of alloy powder, putting the alloy powder into a ball milling tank, and simultaneously putting MnxBi100‑xα -Fe micron powder with 5 percent of the mass of the alloy powder, then adding a proper amount of ethanol and nonmagnetic steel balls with proper size, wherein the ethanol is used as a ball milling medium, and the mass of the steel balls and Mn arexBi100‑xQuality of alloy powderThe ratio of the magnetic powder to the magnetic powder is 10: 1, the magnetic powder is finally placed into a planetary ball mill, the ball milling time is set to be 1-6 hours after the magnetic powder is placed into the planetary ball mill, the ball milling rotating speed is 256 revolutions per minute, and the clockwise/anticlockwise rotation alternation time is 6 minutes to obtain the α -Fe/MnBi composite magnetic powder with high saturation magnetization.
Description
Technical Field
The invention provides a preparation method of high-performance α -Fe/MnBi composite magnetic powder, in particular to a method for preparing high-saturation magnetization α -Fe/MnBi composite magnetic powder by low-energy ball milling, belonging to the technical field of material science.
Background
With the rapid development of science and technology, especially in the fields of automobiles, aerospace and the like, under various extreme environmental conditions, more strict requirements are imposed on various materials. Permanent magnets are used as materials with the most important functions and are more and more widely applied in the fields of national economy and science and technology. Currently, Nd-Fe-B magnets are receiving attention due to their high magnetic properties and good mechanical properties. However, since the curie temperature of NdFeB magnets is only 318 ℃, the operating temperature is mostly below 200 ℃, and thus the use thereof at high temperatures is greatly limited. The Curie temperature of the Mn-Bi permanent magnetic alloy can reach 360 ℃, more importantly, the Mn-Bi permanent magnetic alloy has the characteristic of positive coercive force temperature coefficient, the intrinsic coercive force of the Mn-Bi permanent magnetic alloy can still reach 25.8kOe at 280 ℃, and the Mn-Bi permanent magnetic alloy is particularly suitable for being used in a high-temperature environment, so that the Mn-Bi permanent magnetic alloy is widely researched and paid attention to by people. However, Mn atoms of the MnBi alloy are easy to segregate from the MnBi liquid phase when the peritectic reaction occurs at 719K, so that pure single-phase MnBi is difficult to obtain, and the saturation magnetization of the MnBi alloy is directly influenced.
The invention provides a method for preparing high-performance α -Fe/MnBi composite magnetic powder by adopting a α -Fe compounding method, wherein the high-performance α -Fe/MnBi composite magnetic powder is prepared by adopting the α -Fe compounding method, so that a strong exchange coupling effect is formed between α -Fe phase and MnBi low-temperature phase (LTP) in a high-intensity collision process, and the saturation magnetization of the alloy powder is obviously improved.
Disclosure of Invention
The invention aims to provide a method for compounding α -Fe/MnBi composite magnetic powder by low-energy ball milling, which has the following specific technical scheme:
a method for low-energy ball milling α -Fe/MnBi composite magnetic powder comprises the following steps:
1) preparing materials: according to the nominal composition MnxBi100-x(the mole fraction x is 45,50,55), Mn and Bi alloy with the purity of more than 99.99 percent is adopted for weighing and proportioning;
2) smelting: the prepared raw materials are put into an electric arc furnace under the protection of argon by adopting an electric arc melting method, and are melted to obtain MnxBi100-xAlloy ingot casting;
3) preparation: the MnxBi prepared in the step 2) is added100-xPreparing coarse powder from the alloy ingot, and screening the coarse powder by using a 100-mesh sieve to obtain coarse powder;
4) assembling a ball milling tank: mn prepared in the step 3)xBi100-xTaking a proper amount of alloy coarse powder, putting the alloy coarse powder into a ball milling tank, and adding Mn simultaneouslyxBi100-xα -Fe micron powder with 5 percent of the mass of the alloy coarse powder is put into a nonmagnetic steel ball, a proper amount of ethanol is added, the ball-material ratio is 10: 1, and a ball milling tank is assembled and put into a planetary ball mill;
5) planetary ball milling, namely putting the assembled ball milling tank in the step 4) into a planetary ball mill, setting the ball milling time to be 1-6 hours, setting the rotating speed of the ball mill to be 256 r/min, and rotating clockwise/anticlockwise for alternative time to be 6 minutes to finally obtain the high saturation magnetization α -
Fe/MnBi composite magnetic powder;
compared with the prior art, the invention has the following advantages:
(1) α -Fe micron powder and MnxBi100-xThe alloy powder is subjected to low-energy ball milling compounding, α -Fe micron powder and MnxBi100-xThe alloy powder can be effectively collided, the strong exchange coupling effect of α -Fe soft magnetic phase and MnBiLTP phase can be realized in the ball milling process, the stability of the MnBiLTP phase is not influenced, the saturation magnetization intensity of the manganese-bismuth alloy is improved, and the maximum improvement amplitude reaches more than 150%;
(2) compared with the traditional low-temperature phase acquisition mode, the method has the advantages of simple process, easy operation and production cost reduction.
Detailed Description
The present invention is further described below.
Example 1
1) Preparing materials: according to the nominal composition Mn45Bi55Mn and Bi with the purity of more than 99.99 percent are taken as raw materials, and weighing and proportioning are carried out;
2) smelting: the prepared raw materials are put into an electric arc melting furnace under the protection of argon by adopting an electric arc melting method, and Mn is obtained by melting45Bi55Alloy (I)
3) Preparing coarse powder: mn prepared in the step 2)45Bi55Preparing coarse powder from the alloy ingot, and screening the coarse powder by using a 100-mesh sieve to obtain coarse powder;
4) assembling a ball milling tank: mn prepared in the step 3)45Bi55Taking a proper amount of alloy coarse powder, putting the alloy coarse powder into a ball milling tank, and adding Mn simultaneously45Bi55α -Fe micron powder with 5 percent of the mass of the alloy coarse powder is put into a nonmagnetic steel ball, added with proper amount of ethanol, and put into a planetary ball mill after being assembled with a ball milling tank, wherein the ball-to-material ratio is 10: 1;
5) and (3) planetary ball milling, namely putting the assembled ball milling tank in the step 4) into a planetary ball mill, setting the ball milling time for 1 hour, setting the rotating speed of the ball mill to be 256 revolutions per minute, and rotating clockwise/anticlockwise for 6 minutes alternately to finally obtain the α -Fe/MnBi composite magnetic powder with high saturation magnetization.
Comparative example 1
1) Preparing materials: according to the nominal composition Mn45Bi55Mn and Bi alloys with the purity of more than 99.99 percent are adopted for weighing and proportioning;
2) smelting: the prepared raw materials are put into an electric arc melting furnace under the protection of argon by adopting an electric arc melting method, and Mn is obtained by melting45Bi55Alloy ingot casting;
3) preparation: mn prepared in the step 2)45Bi55Preparing coarse powder from the alloy ingot, and screening the coarse powder by using a 100-mesh sieve to obtain coarse powder;
4) assembling a ball milling tank: mn prepared in the step 3)45Bi55Taking a proper amount of alloy coarse powder, putting the alloy coarse powder into a ball milling tank, putting nonmagnetic steel balls, adding a proper amount of ethanol, wherein the ball-material ratio is 10: 1, putting the assembled ball milling tank into the tankIn a planet ball mill;
5) planetary ball milling, namely putting the assembled ball milling tank in the step 4) into a planetary ball mill, setting the ball milling time to be 1 hour, setting the rotating speed of the ball mill to be 256 revolutions per minute, and rotating clockwise/anticlockwise for alternative time to be 6 minutes to finally obtain the high saturation magnetization α -
Fe/MnBi composite magnetic powder;
the magnetic properties of the samples prepared by the two methods were tested by using a vibrating sample magnetometer. The comparative results are shown in Table 1.
Serial number | Categories | Saturation magnetization Ms (emu/g) |
1 | α -Fe complex | 35.234 |
2 | Not compounded with α -Fe | 12.845 |
Table 1.
Example 2
1) Preparing materials: according to the nominal composition Mn50Bi50Mn and Bi with the purity of more than 99.99 percent are taken as raw materials, and weighing and proportioning are carried out;
2) smelting: the prepared raw materials are put into an electric arc melting furnace under the protection of argon by adopting an electric arc melting method, and Mn is obtained by melting50Bi50Alloy (I)
3) Preparing coarse powder: mn prepared in the step 2)50Bi50Preparing coarse powder from the alloy ingot, and screening the coarse powder by using a 100-mesh sieve to obtain coarse powder;
4) assembling a ball milling tank: mn prepared in the step 3)50Bi50Taking a proper amount of alloy coarse powder, putting the alloy coarse powder into a ball milling tank, and adding Mn simultaneously50Bi50α -Fe micron powder with 5 percent of the mass of the alloy coarse powder is put into a nonmagnetic steel ball, added with proper amount of ethanol, and put into a planetary ball mill after being assembled with a ball milling tank, wherein the ball-to-material ratio is 10: 1;
5) and (3) performing planetary ball milling, namely putting the assembled ball milling tank in the step 4) into a planetary ball mill, setting the ball milling time to be 3 hours, setting the rotating speed of the ball mill to be 256 revolutions per minute, and rotating clockwise/anticlockwise for 6 minutes alternately to finally obtain the α -Fe/MnBi composite magnetic powder with high saturation magnetization.
Comparative example 2
1) Preparing materials: according to the nominal composition Mn50Bi50Mn and Bi with the purity of more than 99.99 percent are taken as raw materials, and weighing and proportioning are carried out;
2) smelting: the prepared raw materials are put into an electric arc melting furnace under the protection of argon by adopting an electric arc melting method, and Mn is obtained by melting50Bi50Alloy (I)
3) Preparing coarse powder: mn prepared in the step 2)50Bi50Preparing coarse powder from the alloy ingot, and screening the coarse powder by using a 100-mesh sieve to obtain coarse powder;
4) assembling a ball milling tank: mn prepared in the step 3)50Bi50Taking a proper amount of alloy coarse powder, putting the alloy coarse powder into a ball milling tank, putting nonmagnetic steel balls, adding a proper amount of ethanol, wherein the ball-material ratio is 10: 1, assembling a ball milling tank and then putting the assembled ball milling tank into a planetary ball mill;
5) planetary ball milling, namely putting the assembled ball milling tank in the step 4) into a planetary ball mill, setting the ball milling time for 4 hours, setting the rotating speed of the ball mill to be 256 revolutions per minute, and rotating clockwise/anticlockwise for 6 minutes alternately to finally obtain α -Fe/MnBi composite magnetic powder with high saturation magnetization;
the magnetic properties of the samples prepared by the two methods were tested by using a vibrating sample magnetometer. The comparative results are shown in Table 2.
Serial number | Categories | Saturation magnetization Ms (emu/g) |
1 | α -Fe complex | 44.995 |
2 | Not compounded with α -Fe | 25.123 |
Table 2.
Example 3
1) Preparing materials: according to the nominal composition Mn55Bi45Mn and Bi with the purity of more than 99.99 percent are taken as raw materials, and weighing and proportioning are carried out;
2) smelting: the prepared raw materials are put into an electric arc melting furnace under the protection of argon by adopting an electric arc melting method, and Mn is obtained by melting55Bi45Alloy (I)
3) Preparing coarse powder: mn prepared in the step 2)55Bi45Preparing coarse powder from the alloy ingot, and screening the coarse powder by using a 100-mesh sieve to obtain coarse powder;
4) assembling a ball milling tank: mn prepared in the step 3)55Bi45Taking a proper amount of alloy coarse powder, putting the alloy coarse powder into a ball milling tank, and adding Mn simultaneously55Bi45α -Fe micron powder with 5 percent of the mass of the alloy coarse powder is put into a nonmagnetic steel ball, added with proper amount of ethanol, and put into a planetary ball mill after being assembled with a ball milling tank, wherein the ball-to-material ratio is 10: 1;
5) planetary ball milling, namely putting the assembled ball milling tank in the step 4) into a planetary ball mill, setting the ball milling time for 6 hours, setting the rotating speed of the ball mill to be 256 revolutions per minute, and rotating clockwise/anticlockwise for 6 minutes alternately to finally obtain the high saturation magnetization α -
Fe/MnBi composite magnetic powder.
Comparative example 3
1) Preparing materials: according to the nominal composition Mn55Bi45Mn and Bi with the purity of more than 99.99 percent are taken as raw materials, and weighing and proportioning are carried out;
2) smelting: the prepared raw materials are put into an electric arc melting furnace under the protection of argon by adopting an electric arc melting method, and Mn is obtained by melting55Bi45Alloy (I)
3) Preparing coarse powder: mn prepared in the step 2)55Bi45Preparing coarse powder from the alloy ingot, and screening the coarse powder by using a 100-mesh sieve to obtain coarse powder;
4) assembling a ball milling tank: mn prepared in the step 3)55Bi45Taking a proper amount of alloy coarse powder, putting the alloy coarse powder into a ball milling tank, putting nonmagnetic steel balls, adding a proper amount of ethanol, wherein the ball-material ratio is 10: 1, assembling a ball milling tank and then putting the assembled ball milling tank into a planetary ball mill;
5) planetary ball milling, namely putting the assembled ball milling tank in the step 4) into a planetary ball mill, setting the ball milling time for 3 hours, setting the rotating speed of the ball mill to be 256 revolutions per minute, and rotating clockwise/anticlockwise for 6 minutes alternately to finally obtain α -Fe/MnBi composite magnetic powder with high saturation magnetization;
the magnetic properties of the samples prepared by the two methods were tested by using a vibrating sample magnetometer. The comparative results are shown in Table 3.
Serial number | Categories | Saturation magnetization Ms (T) |
1 | α -Fe complex | 46.683 |
2 | Not compounded with α -Fe | 33.966 |
Table 3.
Claims (2)
1. The preparation method of the composite magnetic powder is characterized by comprising the following steps of:
1) preparing materials: according to the nominal composition MnxBi100-xThe molar fraction x =45,50,55, Mn and Bi alloy with the purity of more than 99.99 percent is adopted for weighing and proportioning;
2) smelting: the prepared raw materials are put into an electric arc furnace under the protection of argon by adopting an electric arc melting method, and are melted to obtain MnxBi100-xAlloy ingot casting;
3) preparation: the MnxBi prepared in the step 2) is added100-xPreparing coarse powder from the alloy ingot, and screening the coarse powder by using a 100-mesh sieve to obtain coarse powder;
4) assembling a ball milling tank: mn prepared in the step 3)xBi100-xTaking a proper amount of alloy coarse powder, putting the alloy coarse powder into a ball milling tank, and adding Mn simultaneouslyxBi100-xα -Fe micron powder with 5 percent of the mass of the alloy coarse powder is put into a nonmagnetic steel ball, a proper amount of ethanol is added as a ball milling medium, the ball-material ratio is 10: 1, and a ball milling tank is assembled and put into a planetary ball mill;
5) and (3) low-energy ball milling, namely putting the assembled ball milling tank in the step 4) into a planetary ball mill, setting the ball milling time to be 1-6 hours, setting the rotating speed of the ball mill to be 256 r/min, and rotating clockwise/anticlockwise for alternative time to be 6 minutes to finally obtain the α -Fe/MnBi composite magnetic powder with high saturation magnetization.
2. The method of preparing a composite magnetic powder of claim 1, wherein:
the ball milling process in step 5) is preferably as follows, with a ball milling time of 3 hours.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113517124A (en) * | 2021-04-22 | 2021-10-19 | 中国计量大学 | Preparation method of high-performance anisotropic rare-earth-free permanent magnet |
CN113782331A (en) * | 2021-09-18 | 2021-12-10 | 泮敏翔 | Preparation method of high-performance double-hard-magnetic-phase nano composite magnet |
CN113921261A (en) * | 2021-08-12 | 2022-01-11 | 泮敏翔 | Preparation method of high-performance high-resistivity composite magnet |
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CN113517124A (en) * | 2021-04-22 | 2021-10-19 | 中国计量大学 | Preparation method of high-performance anisotropic rare-earth-free permanent magnet |
CN113921261A (en) * | 2021-08-12 | 2022-01-11 | 泮敏翔 | Preparation method of high-performance high-resistivity composite magnet |
CN113921261B (en) * | 2021-08-12 | 2023-10-20 | 中国计量大学 | Preparation method of high-performance high-resistivity composite magnet |
CN113782331A (en) * | 2021-09-18 | 2021-12-10 | 泮敏翔 | Preparation method of high-performance double-hard-magnetic-phase nano composite magnet |
CN113782331B (en) * | 2021-09-18 | 2023-10-20 | 中国计量大学 | Preparation method of high-performance double-hard-magnetic-phase nanocomposite magnet |
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