CN117778803A - MnBiSn permanent magnet alloy with low activation energy and preparation method thereof - Google Patents
MnBiSn permanent magnet alloy with low activation energy and preparation method thereof Download PDFInfo
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 62
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- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 20
- 239000000843 powder Substances 0.000 claims abstract description 19
- 238000002844 melting Methods 0.000 claims abstract description 11
- 230000008018 melting Effects 0.000 claims abstract description 11
- 239000000203 mixture Substances 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 8
- 239000011572 manganese Substances 0.000 claims description 37
- 239000002994 raw material Substances 0.000 claims description 21
- 238000004519 manufacturing process Methods 0.000 claims description 11
- 238000010791 quenching Methods 0.000 claims description 9
- 230000000171 quenching effect Effects 0.000 claims description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- 239000011261 inert gas Substances 0.000 claims description 8
- 229910052748 manganese Inorganic materials 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 5
- 229910052718 tin Inorganic materials 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 229910052797 bismuth Inorganic materials 0.000 claims description 4
- 238000012216 screening Methods 0.000 claims description 4
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 3
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 3
- 229910001004 magnetic alloy Inorganic materials 0.000 claims description 3
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 2
- 229910016629 MnBi Inorganic materials 0.000 abstract description 20
- 230000005291 magnetic effect Effects 0.000 abstract description 16
- 239000000463 material Substances 0.000 abstract description 12
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- 150000002910 rare earth metals Chemical class 0.000 description 6
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
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- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
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Abstract
The invention disclosesMnBiSn permanent magnet alloy with low activation energy and preparation method thereof, wherein the composition of the MnBiSn permanent magnet alloy is Mn 55 Bi 45－x Sn x Wherein x is more than 0 and less than or equal to 2. The preparation method comprises the following steps: alloy powders were prepared using vacuum induction melting techniques and subsequently annealed at 300 ℃ for 3 hours. According to the invention, by doping a proper amount of Sn element, the Sn element occupies the Bi atoms and vacancies of the MnBi crystal, the apparent activation energy required by the formation reaction of a MnBi low-temperature phase is reduced, the lattice parameter is optimized, the permanent magnetic performance is finally regulated, and the maximum magnetic energy product of the alloy material is greatly improved after testing; the preparation process is simple and easy to implement, and has great application prospect. The permanent magnet alloy prepared by the invention has excellent magnetic performance, and the permanent magnet material with excellent and stable performance can be prepared by simple smelting reaction, heat treatment process and ball milling.
Description
Technical Field
The invention belongs to the technical field of permanent magnet materials, and particularly relates to a MnBiSn permanent magnet alloy with low activation energy and a preparation method thereof.
Background
In recent years, permanent magnetic materials are widely applied to electromagnetic devices, motors, sensors and other equipment as key materials for converting electric energy, magnetic energy and mechanical energy. Currently, the permanent magnet market mainly comprises ferrite permanent magnet materials with low price and rare earth permanent magnet materials with excellent performance. Ferrite permanent magnetic materials have the advantages of low price, good stability and the like, but the lower magnetic energy product limits the application of the ferrite permanent magnetic materials in miniaturized and lightweight device equipment. Rare earth permanent magnet materials have excellent permanent magnet performance, but increasingly failure and expensive rare earth resources limit the wide application. In addition, in order to improve the high-temperature performance of the rare earth permanent magnet material, expensive heavy rare earth elements are added into alloy components, which inevitably increases the cost of the rare earth permanent magnet material greatly. Therefore, under the dual standards of performance and cost, there is an urgent need to develop a permanent magnetic material with low cost and performance between ferrite and rare earth permanent magnetic material.
Mn-based permanent magnet materials are attracting attention because of their low cost, excellent performance and the like. In particular, mnBi permanent magnet alloys have a large magnetic energy product, a high coercivity and a positive coercivity temperature characteristic. The unique performance makes the hybrid electric vehicle and the wind driven generator applied to the high-temperature fields such as hybrid electric vehicles, wind driven generators and the like. Therefore, mnBi permanent magnet alloy is one of the most applicable rare earth-free permanent magnet materials at present. However, the maximum magnetic energy product of MnBi alloy is much smaller than its theoretical value. The maximum magnetic energy product of a MnBi alloy is mainly related to remanence and coercivity. The MnBi low-temperature phase is generated through peritectic reaction between Mn element and Bi element, and Mn element is easy to oxidize and segregate in the solidification process, so that the formation of the MnBi low-temperature phase is inhibited, and the saturation magnetization and the remanence of the MnBi alloy are lower. Regarding the coercive force, grains can be refined by ball milling or the like to improve the coercive force, but decomposition of the low-temperature phase of MnBi can also be caused. Therefore, how to reduce the activation energy of the low-temperature reaction, promote the generation of MnBi low-temperature phase, and ensure the saturation magnetization value while increasing the coercive force is a problem that is urgently needed to be studied at present.
Disclosure of Invention
This section is intended to outline some aspects of embodiments of the invention and to briefly introduce some preferred embodiments. Some simplifications or omissions may be made in this section as well as in the description summary and in the title of the application, to avoid obscuring the purpose of this section, the description summary and the title of the invention, which should not be used to limit the scope of the invention.
The present invention has been made in view of the above and/or problems occurring in the prior art.
Therefore, the invention aims to overcome the defects in the prior art and provide a MnBiSn permanent magnetic alloy with low activation energy, which is characterized in that: the composition of the MnBiSn permanent magnet alloy is Mn 55 Bi 45－x Sn x Wherein x is more than 0 and less than or equal to 2.
In order to solve the technical problems, the invention provides the following technical scheme: a preparation method of MnBiSn permanent magnetic alloy powder with low activation energy comprises the steps of,
according to the composition Mn 55 Bi 45－x Sn x Preparing raw materials, wherein x is more than 0 and less than or equal to 2;
fully melting the raw materials under the protection of inert gas, and cooling to obtain an alloy ingot;
remelting the alloy ingot and then carrying out single-roller spin quenching to obtain an alloy strip;
performing heat treatment on the alloy strip to obtain the MnBiSn permanent magnet alloy with low activation energy;
crushing, grinding and screening the prepared MnBiSn permanent magnet alloy strips by a mesh screen to obtain MnBiSn permanent magnet alloy powder.
As a preferred embodiment of the preparation process according to the invention, there is provided: the composition Mn 55 Bi 45－x Sn x Preparing raw materials, whereinThe raw materials are high-purity manganese tablets, bismuth ingots and tin particles with the purity not lower than 99.97 percent.
As a preferred embodiment of the preparation process according to the invention, there is provided: and fully melting the raw materials under the protection of inert gas, and cooling to obtain an alloy ingot, wherein the inert gas is high-purity argon.
As a preferred embodiment of the preparation process according to the invention, there is provided: the raw materials are fully melted under the protection of inert gas and then cooled to prepare an alloy ingot, wherein the melting temperature is 1200-1300 ℃ and the melting time is 10min.
As a preferred embodiment of the preparation process according to the invention, there is provided: carrying out single-roller spin quenching after remelting the alloy ingot, wherein the remelting times are at least twice; the rotation speed of the single-roller spin quenching is 15m/s.
As a preferred embodiment of the preparation process according to the invention, there is provided: the melting and remelting are both carried out under vacuum, wherein the vacuum degree is 10 -3 Pa or below.
As a preferred embodiment of the preparation process according to the invention, there is provided: the alloy strip is subjected to heat treatment, wherein the heat treatment is performed in vacuum, and the vacuum degree is 10 -5 Pa; the heating temperature is 300 ℃, the heating rate is 5 ℃/min, and the heating time is 4 hours.
As a preferred embodiment of the preparation process according to the invention, there is provided: crushing, grinding and screening the prepared MnBiSn permanent magnet alloy strips through a mesh screen, wherein the mesh number of the mesh screen is 800 meshes; the particle size of the MnBiSn stripe broken powder is not more than 22 mu m.
It is yet another object of the present invention to overcome the deficiencies of the prior art by providing a MnBiSn permanent magnet alloy powder having a low activation energy.
The invention has the beneficial effects that:
the permanent magnet alloy prepared by the method has excellent magnetic performance, and the permanent magnet material with excellent and stable performance can be prepared by simple smelting reaction, heat treatment process and ball milling.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the description of the embodiments will be briefly described below, it being obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art. Wherein:
FIG. 1 is an XRD pattern of the products prepared in examples 1 to 4 and comparative example;
FIG. 2 is a DSC graph of the products prepared in examples 1-4 and comparative examples;
FIGS. 3 (a-e) are graphs of the first endotherm peaks measured at various heating rates (5-40 ℃ C./min) for the products prepared in examples 1-4 and comparative examples, and the apparent activation energy change for the products prepared in comparative example of FIG. 3 (f);
FIG. 4 is a graph showing the change in saturation magnetization (Ms), coercive force (Hc), and maximum magnetic energy product [ (BH) max ] with the increase in Sn content of the products produced in examples 1 to 4 and comparative example.
Detailed Description
In order that the above-recited objects, features and advantages of the present invention will become more apparent, a more particular description of the invention will be rendered by reference to specific embodiments thereof which are illustrated in the appended drawings.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways other than those described herein, and persons skilled in the art will readily appreciate that the present invention is not limited to the specific embodiments disclosed below.
Further, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic can be included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
Example 1
Mn (Mn) 55 Bi 44.5 Sn 0.5 Permanent magnet alloy powderThe preparation method of (2) comprises the following steps:
(1) The elementary substances of three elements of manganese, bismuth and tin with purity not lower than 99.97 percent are Mn according to nominal compositions 55 Bi 44.5 Sn 0.5 (the atomic number ratio of Mn, bi, and Sn was 55:44.5:0.5) to prepare an alloy material, and 8wt.% Mn was added in consideration of volatilization of Mn element.
(2) Sequentially placing the raw materials prepared in the step (1) into a boron nitride crucible, placing the crucible into an induction coil in an induction smelting furnace, and vacuumizing a chamber of the smelting furnace to enable the vacuum degree to reach 10 -3 Pa, closing a vacuum pump, filling a proper amount of high-purity argon into the cavity, slowly lifting the induced current until the alloy is completely melted, preserving heat for 10min, pouring into a water-cooled copper mold, and taking out the alloy ingot after full cooling.
(3) Crushing the alloy ingot obtained in the step (2) into small blocks, putting the small blocks into a quartz tube, and carrying out single-roller spin quenching in a vacuum melt-spinning machine to prepare strips; the single roller spin quenching is as follows: the surface of an alloy ingot obtained by induction smelting is polished clean, then the alloy ingot is crushed into small blocks with the diameter of 1-2 cm, about 15g of alloy ingot is weighed and put into the bottom of a quartz spray pipe with the tip aperture of 0.3-0.5 mm, and a proper amount of argon is filled into an external air storage tank to form pressure difference with the inside of a cavity of a rotary quenching machine.
(4) Placing the strip obtained in the step (3) into a corundum crucible, placing into a vacuum tube furnace for heat treatment, and vacuumizing by a molecular pump to ensure that the vacuum degree in the quartz tube reaches 10 -5 Pa, then heating from room temperature to 300 ℃ at a heating rate of 5 ℃/min, preserving heat for 3 hours, and gradually cooling along with a furnace after the heat preservation is finished, so as to obtain the strip after heat treatment.
(5) Crushing the heat-treated strips obtained in the step (4), grinding into powder by using a mortar, and sieving by using a 800-mesh stainless steel mesh sieve to ensure that the particle size of the powder is not more than 22 mu m; performing low-energy ball milling on the raw powder, wherein zirconia balls with the diameter of 3mm are adopted in the ball milling process, the ball-material ratio is 15:1, the ball milling medium is absolute ethyl alcohol, the ball milling time is 5 hours, the ball milling rotating speed is set to 175rpm, and Mn with uniform particle size is obtained 55 Bi 44.5 Sn 0.5 Alloy powder.
Example 2
Mn (Mn) 55 Bi 44 Sn 1 The method for producing permanent magnet alloy powder differs from example 1 in the amount of raw materials added, the amount of raw materials added and Mn in this example 55 Bi 44 Sn 1 The ratio of Mn, bi, sn (atomic number ratio: 55:44:1) was set, and the other steps were the same as in example 1.
Example 3
Mn (Mn) 55 Bi 43.5 Sn 1.5 The method for producing permanent magnet alloy powder differs from example 1 in the amount of raw materials added, the amount of raw materials added and Mn in this example 55 Bi 43.5 Sn 1.5 The ratio of Mn, bi, and Sn (atomic number ratio: 55:43.5:1.5) was set, and the other steps were the same as in example 1.
Example 4
Mn (Mn) 55 Bi 43 Sn 2 The method for producing permanent magnet alloy powder differs from example 1 in the amount of raw materials added, the amount of raw materials added and Mn in this example 55 Bi 43 Sn 2 The ratio of Mn, bi, sn (atomic number ratio: 55:43:2) was set, and the other steps were the same as in example 1.
Comparative example
Mn (Mn) 55 Bi 45 The method for producing permanent magnet alloy powder differs from example 1 in the amount of raw materials added, the amount of raw materials added and Mn in this example 55 Bi 45 (atomic number ratio of Mn and Bi was 55:45), and the other steps were the same as in example 1.
Example 5
The products prepared in examples 1 to 4 and comparative examples were tested as follows:
(A) The thermal phase transition behavior of the heavy alloy ingots obtained in step (3) in examples 1 to 4 or comparative example was measured using a Differential Scanning Calorimeter (DSC).
(B) The microstructure, phase composition and lattice parameter of the permanent magnet alloy powders obtained in step (5) in examples 1 to 4 or comparative example were measured by X-ray diffraction analysis (XRD), and the measurement results of the phase composition and lattice parameter are shown in table 1.
(C) The magnetic properties at room temperature of the permanent magnet alloy powders obtained in step (5) in examples 1 to 4 or comparative example were measured using a Vibrating Sample Magnetometer (VSM).
Table 1 table of phase composition and lattice parameter of samples prepared in examples 1 to 4 and comparative example
In order to illustrate the effect of Sn element doping on the low temperature MnBi phase content, a change in its low temperature MnBi phase content can be observed. The contents of LTP-MnBi in comparative examples and examples 1 to 4 were 89.9wt.%, 92.8wt.% and 91.7wt.%,74.3wt.% and 65.6wt.%, respectively. It is known that doping with Sn element at a proper concentration can promote the formation of a ferromagnetic phase LTP-MnBi, and that if the doping concentration is high, the NiAs-type hexagonal structure of LTP-MnBi is destroyed to form a MnBiSn intermetallic phase.
In order to explain the effect of Sn doping on low-temperature MnBi phase generation, it was observed that all endothermic peaks gradually shift to a high-temperature region as the temperature increase rate increases. The invention is based on Kissinger
Equation the apparent activation energy of the samples prepared in examples 1 to 4 and comparative example was calculated:
t: phase transition onset temperature, beta: heating rate, R, gas constant (8.314 J.mol) -1 ·K -1 )，E α Apparent activation energy, v: a frequency factor; e (E) α The trend of variation at different Sn doping concentrations is shown in FIG. 3, and it can be seen that E α The change trend of increasing after decreasing is presented with the increase of the Sn concentration, and when the doping concentration is 0.5at percent, the Mn ratio of the master alloy is obtained 55 Bi 45 Smaller E α A value indicating that doping with Sn element at an appropriate concentration can reduce the apparent activation energy required for the reaction, such that LTP-MnBi is formed more easily.
In addition, in order to more intuitively reflect the influence of Sn element doping, fig. 4 lists the change curves of saturation magnetization, coercive force, and maximum magnetic energy product with increase in Sn content. The analysis revealed that the magnetocrystalline anisotropy was most remarkable and the most excellent overall magnetic properties were exhibited when the Sn element content was 0.5 at%. In Sn doped samples, mn 55 Bi 44.5 Sn 0.5 The samples showed the highest (BH) max value, reaching 11.36MGOe, relative to Mn in the comparative example 55 Bi 45 The sample improves the comprehensive magnetic performance by 5%, which shows that the doping of Sn element can obviously improve the maximum magnetic energy product of MnBi alloy.
In Sn doped samples, mn 55 Bi 43 Sn 2 The samples showed the highest (BH) max value, reaching 11.36MGOe, relative to Mn in the comparative example 55 Bi 45 The coercivity of the sample is improved by 17%.
The invention obviously reduces the apparent activation energy of the reaction by doping proper amount of Sn element into the MnBi alloy, promotes the generation of low-temperature MnBi phase, shows excellent comprehensive magnetic performance, and has important significance for the further development and wide application of the MnBi alloy.
It should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the same, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or substituted without departing from the spirit and scope of the technical solution of the present invention, and it should be covered in the scope of the present invention.
Claims (10)
1. A MnBiSn permanent magnet alloy with low activation energy, characterized in that: the composition of the MnBiSn permanent magnet alloy is Mn 55 Bi 45－x Sn x Wherein x is more than 0 and less than or equal to 2.
2. A method for preparing MnBiSn permanent magnetic alloy powder with low activation energy, which is characterized by comprising the following steps:
according to the composition Mn 55 Bi 45－x Sn x Preparing raw materials, wherein x is more than 0 and less than or equal to 2;
fully melting the raw materials under the protection of inert gas, and cooling to obtain an alloy ingot;
remelting the alloy ingot and then carrying out single-roller spin quenching to obtain an alloy strip;
performing heat treatment on the alloy strip to obtain the MnBiSn permanent magnet alloy with low activation energy;
crushing, grinding and screening the prepared MnBiSn permanent magnet alloy strips by a mesh screen to obtain MnBiSn permanent magnet alloy powder.
3. The method of manufacturing as claimed in claim 2, wherein: the composition Mn 55 Bi 45－x Sn x Preparing raw materials, wherein the raw materials are high-purity manganese tablets, bismuth ingots and tin particles with purity not lower than 99.97%.
4. The method of manufacturing as claimed in claim 2, wherein: and fully melting the raw materials under the protection of inert gas, and cooling to obtain an alloy ingot, wherein the inert gas is high-purity argon.
5. The method of manufacturing as claimed in claim 2, wherein: the raw materials are fully melted under the protection of inert gas and then cooled to prepare an alloy ingot, wherein the melting temperature is 1200-1300 ℃ and the melting time is 10min.
6. The method of manufacturing as claimed in claim 2, wherein: carrying out single-roller spin quenching after remelting the alloy ingot, wherein the remelting times are at least twice; the rotation speed of the single-roller spin quenching is 15m/s.
7. The method of manufacturing as claimed in claim 2, wherein: the melting and remelting are both carried out under vacuum, wherein the vacuum degree is 10 -3 Pa or below.
8. The method of claim 2The preparation method is characterized in that: the alloy strip is subjected to heat treatment, wherein the heat treatment is performed in vacuum, and the vacuum degree is 10 -5 Pa; the heating temperature is 300 ℃, the heating rate is 5 ℃/min, and the heating time is 4 hours.
9. The method of manufacturing as claimed in claim 2, wherein: crushing, grinding and screening the prepared MnBiSn permanent magnet alloy strips through a mesh screen, wherein the mesh number of the mesh screen is 800 meshes; the particle size of the MnBiSn stripe broken powder is not more than 22 mu m.
10. A MnBiSn permanent magnet alloy powder with low activation energy produced by the production method according to any one of claims 2 to 9.
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