CN111230127B - Preparation method of composite magnetic powder - Google Patents
Preparation method of composite magnetic powder Download PDFInfo
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- CN111230127B CN111230127B CN202010116293.5A CN202010116293A CN111230127B CN 111230127 B CN111230127 B CN 111230127B CN 202010116293 A CN202010116293 A CN 202010116293A CN 111230127 B CN111230127 B CN 111230127B
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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 MnxBi 100‑x Melting an alloy ingot (the mole fraction x =45,50,55), and coarsely crushing the alloy ingot; mn to be produced by the invention x Bi 100‑x Placing the alloy ingot fragments into a mortar for coarse grinding, screening through a 100-mesh grid sieve after grinding, and obtaining Mn x Bi 100‑x Performing low-energy ball milling compounding on the alloy powder; the obtained Mn x Bi 100‑x Taking a proper amount of alloy powder, putting the alloy powder into a ball milling tank, and simultaneously putting Mn x Bi 100‑x alpha-Fe micron powder accounting for 5 percent of the mass of the alloy powder is added with proper amount of ethanol and nonmagnetic steel balls with proper size, the ethanol is used as a ball milling medium, and the mass of the steel balls and Mn are x Bi 100‑x The mass ratio of the alloy powder is 10:1, finally putting the mixture into a planetary ball mill; after the mixture is put into a planetary ball mill, the ball milling time is set to be 1-6 hours, the ball milling rotating speed is 256 revolutions per minute, and the alternating time of clockwise rotation and anticlockwise rotation is 6 minutes to obtain the alpha-Fe/MnBi composite magnetic powder with high saturation magnetization. The process is simple and easy to operate, and reduces the production cost of the high-performance permanent magnet.
Description
Technical Field
The invention provides a preparation method of high-performance alpha-Fe/MnBi composite magnetic powder, in particular to a method for preparing high-saturation magnetization alpha-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.
Because the temperature difference between the melting points of the two metals of manganese and bismuth is large, the fluidity of molten metal is poor, so that the content of low-temperature phase is small, the content of low-temperature phase is often improved by long-time (more than 24 hours) low-temperature heat treatment annealing treatment, discharge plasma sintering and the like in actual production, manpower and material resources are wasted, and the saturation magnetization can not be ensured to reach an ideal value. The soft magnetic composite method is another method for increasing the saturation magnetization of MnBi. Wherein alpha-Fe recombination can improve saturation magnetization. The invention provides a method for preparing high-performance alpha-Fe/MnBi composite magnetic powder by adopting an alpha-Fe compounding method. In the high-intensity collision process, the alpha-Fe phase and the MnBi low-temperature phase (LTP) form a strong exchange coupling effect, and the saturation magnetization of the alloy powder is obviously improved.
Disclosure of Invention
The invention aims to provide a method for compounding alpha-Fe/MnBi composite magnetic powder by low-energy ball milling. The specific technical scheme is as follows:
a method for low-energy ball milling of alpha-Fe/MnBi composite magnetic powder comprises the following steps:
1) Preparing materials: mn as a nominal composition x Bi 100-x (the mole 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 MnxBi 100-x Alloy ingot casting;
3) Preparation: the MnxBi prepared in the step 2) is added 100-x Preparing 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) x Bi 100-x Taking a proper amount of alloy coarse powder, putting the alloy coarse powder into a ball milling tank, and adding Mn simultaneously x Bi 100-x And (2) placing alpha-Fe micron powder with 5% of alloy coarse powder by mass into a nonmagnetic steel ball, adding a proper amount of ethanol, wherein the ball-material ratio is 10:1, assembling a ball milling tank and putting the ball milling tank into a planetary ball mill;
5) Planetary ball milling: 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 revolutions per minute, and rotating clockwise/anticlockwise for alternative time to be 6 minutes, so as to finally obtain the high saturation magnetization alpha-Fe/MnBi composite magnetic powder;
compared with the prior art, the invention has the following advantages:
(1) Mixing alpha-Fe micron powder with Mn x Bi 100-x The alloy powder is subjected to low-energy ball milling compounding, and alpha-Fe micron powder and Mn x Bi 100-x The alloy powder can be effectively collided, the strong exchange coupling effect of the alpha-Fe soft magnetic phase and the MnBiLTP phase can be realized in the ball milling process, the stability of the MnBiLTP phase is not influenced, the saturation magnetization 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: mn as a nominal composition 45 Bi 55 Mn 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 melting 45 Bi 55 Alloy (I)
3) Preparing coarse powder: mn prepared in the step 2) 45 Bi 55 Preparing 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) 45 Bi 55 Taking a proper amount of alloy coarse powder, putting the alloy coarse powder into a ball milling tank, and adding Mn simultaneously 45 Bi 55 5% of alloy coarse powder by mass of alpha-Fe micronAnd (3) putting the powder into a nonmagnetic steel ball, adding a proper amount of ethanol, wherein the ball-material ratio is 10:1, assembling a ball milling tank and then putting the ball milling tank into a planetary ball mill;
5) Planetary ball milling: and (3) putting the assembled ball milling tank into a planetary ball mill in the step 4), 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, so as to finally obtain the high-saturation magnetization alpha-Fe/MnBi composite magnetic powder.
Comparative example 1
1) Preparing materials: according to the nominal composition Mn 45 Bi 55 Mn 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 melting 45 Bi 55 Alloy ingot casting;
3) Preparation: mn prepared in the step 2) 45 Bi 55 Preparing 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) 45 Bi 55 Taking 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 putting the ball milling tank into a planetary ball mill;
5) Planetary ball milling: 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 alternative time of 6 minutes to finally obtain high saturation magnetization 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;
table 1.
Example 2
1) Preparing materials: according to nominal compositionMn 50 Bi 50 Mn and Bi with the purity of more than 99.99 percent are taken as raw materials, and the raw materials are weighed and proportioned;
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 melting 50 Bi 50 Alloy (I)
3) Preparing coarse powder: mn prepared in the step 2) 50 Bi 50 Preparing 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) 50 Bi 50 Taking a proper amount of alloy coarse powder, putting the alloy coarse powder into a ball milling tank, and adding Mn simultaneously 50 Bi 50 And (2) placing alpha-Fe micron powder with 5% of alloy coarse powder by mass into a nonmagnetic steel ball, 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: and (3) putting the assembled ball milling tank into a planetary ball mill in the step 4), 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 alternative time to be 6 minutes, thereby finally obtaining the high saturation magnetization alpha-Fe/MnBi composite magnetic powder.
Comparative example 2
1) Preparing materials: according to the nominal composition Mn 50 Bi 50 Mn 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 melting 50 Bi 50 Alloy (II)
3) Preparing coarse powder: mn prepared in the step 2) 50 Bi 50 Preparing 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) 50 Bi 50 Taking 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 ball milling tank into a planetary ball mill;
5) Planetary ball milling: 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 alternative time of 6 minutes to finally obtain high saturation magnetization 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 2;
table 2.
Example 3
1) Preparing materials: according to the nominal composition Mn 55 Bi 45 Mn and Bi with the purity of more than 99.99 percent are taken as raw materials, and the raw materials are weighed and proportioned;
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 melting 55 Bi 45 Alloy (I)
3) Preparing coarse powder: mn prepared in the step 2) 55 Bi 45 Preparing 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) 55 Bi 45 Taking a proper amount of alloy coarse powder, putting the alloy coarse powder into a ball milling tank, and adding Mn simultaneously 55 Bi 45 And (2) placing alpha-Fe micron powder with 5% of the mass of the alloy coarse powder into a nonmagnetic steel ball, 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: and (3) putting the assembled ball milling tank into a planetary ball mill in the step 4), 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 alternative time of 6 minutes to finally obtain the high saturation magnetization alpha-Fe/MnBi composite magnetic powder.
Comparative example 3
1) Preparing materials: mn as a nominal composition 55 Bi 45 Mn 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 melting 55 Bi 45 Alloy (I)
3) Preparing coarse powder: mn prepared in the step 2) 55 Bi 45 Preparing 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) 55 Bi 45 Taking 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: 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 alternative time of 6 minutes to finally obtain high saturation magnetization MnBi composite magnetic powder;
the samples prepared by the above two methods were tested for their magnetic properties using a vibrating sample magnetometer. The comparative results are shown in table 3;
table 3.
Claims (1)
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 Mn x Bi 100-x The 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 melting furnace under the protection of argon by adopting an electric arc melting method, and Mn is obtained by melting x Bi 100-x Alloy ingot casting;
3) Preparation: the MnxBi prepared in the step 2) is added 100-x Preparing coarse powder from the alloy ingot, and screening the coarse powder by using a 100-mesh sieve to obtain coarse powder;
4) AssemblyBall-milling jar: mn prepared in the step 3) x Bi 100-x Taking a proper amount of alloy coarse powder, putting the alloy coarse powder into a ball milling tank, and adding Mn simultaneously x Bi 100-x And (2) placing alpha-Fe micron powder with 5% of alloy coarse powder by mass into a nonmagnetic steel ball, adding a proper amount of ethanol as a ball milling medium, wherein the ball-material ratio is 10:1, assembling a ball milling tank and putting the ball milling tank into a planetary ball mill;
5) Low-energy ball milling: and (3) putting the ball milling tank assembled 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 revolutions per minute, and rotating clockwise/anticlockwise for alternative time to be 6 minutes to finally obtain the high saturation magnetization alpha-Fe/MnBi composite magnetic powder.
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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 |
| CN113921261B (en) * | 2021-08-12 | 2023-10-20 | 中国计量大学 | Preparation method of high-performance high-resistivity 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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| CN102240810A (en) * | 2011-06-24 | 2011-11-16 | 北京工业大学 | Method for preparing high-coercivity manganese bismuth magnetic powder |
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| EP0706191B1 (en) * | 1994-04-14 | 1999-09-08 | Hitachi Maxell, Ltd. | Magnetic powder and its manufacture and application |
| JP3488761B2 (en) * | 1994-04-14 | 2004-01-19 | 日立マクセル株式会社 | MAGNETIC POWDER, ITS MANUFACTURING METHOD, MAGNETIC RECORDING MEDIUM USING MAGNETIC POWDER PRODUCED BY THIS MANUFACTURING METHOD, RECORDING / REPRODUCING METHOD AND RECORDING / REPRODUCING DEVICE FOR THIS MAGNETIC RECORDING MEDIUM |
| JPH10261514A (en) * | 1997-03-19 | 1998-09-29 | Hitachi Maxell Ltd | Magnetic material |
| CN102610346B (en) * | 2011-12-01 | 2015-10-28 | 中国计量学院 | A kind of Novel rare-earth-free nanometer composite permanent magnet material and preparation method thereof |
| CN102909381B (en) * | 2012-10-17 | 2014-06-18 | 北京工业大学 | Method for preparing high coercive force manganese-bismuth magnetic powder by doping cobalt nano-particles |
| CN105336488B (en) * | 2015-11-20 | 2018-10-26 | 中国计量学院 | Improve Fe3B/Nd2Fe14The preparation method of B series magnetic alloy intrinsic coercivity |
| CN108780688A (en) * | 2016-01-07 | 2018-11-09 | 户田工业株式会社 | MnBi based magnetic powders and its manufacturing method and bonded permanent magnet mixture, bonded permanent magnet, MnBi systems metallic magnet and its manufacturing method |
| CN105689726B (en) * | 2016-01-21 | 2017-12-29 | 中国计量学院 | A kind of preparation method for mixing rare earth high-coercive force manganese bismuth alloy magnetic |
| CN107297493A (en) * | 2017-06-13 | 2017-10-27 | 同济大学 | A kind of high-coercive force MnBi nano particles and preparation method thereof |
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| CN102240810A (en) * | 2011-06-24 | 2011-11-16 | 北京工业大学 | Method for preparing high-coercivity manganese bismuth magnetic powder |
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