CN115821173A - High-abundance rare earth element-based nano dual-phase composite material and preparation method thereof - Google Patents
High-abundance rare earth element-based nano dual-phase composite material and preparation method thereof Download PDFInfo
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Abstract
The inventionProvides a high-abundance rare earth element-based nano dual-phase composite material and a preparation method thereof, wherein the composite material has a general formula of RE x (Fe 1‑y Co y ) 95‑x‑z M z B 5 The composition represented, wherein RE is a high-abundance rare earth element, M is a transition group element, and the composition ratios x, y, and z satisfy inequalities: x is more than or equal to 7 atom percent and less than or equal to 11 atom percent, y is more than or equal to 0.1 atom percent and less than or equal to 0.35 atom percent, and z is more than or equal to 0 atom percent and less than or equal to 1 atom percent. The high-abundance rare earth element RE is one or more of La, ce and Y. The transition group element M is one or more of Cu, cr, nb, ti and Zr. The high-abundance rare earth element-based nano two-phase composite material prepared by the invention has the advantages of low cost, high remanence, low coercive force, good squareness of a magnetic hysteresis loop and the like, and meets the magnetic performance requirement of the nano two-phase composite material for the magnetic control reactor.
Description
Technical Field
The invention relates to the technical field of rare earth magnetic materials, in particular to a preparation method of a high-abundance rare earth element-based nano two-phase composite material.
Background
The nano biphase composite material is prepared by exchange coupling of soft magnetic phase and hard magnetic phase in nano scaleThe novel magnetic materials formed were first reported by Coehoorn et al (Coehoorn R., de Mooij D.B., de Waard C.Meltsputter magnetic materials relating Fe 3 Journal of Magnetic and Magnetic Materials,1989,80, 101-104). The material not only has the characteristics of high coercive force of a hard magnetic phase and high saturation magnetization of a soft magnetic phase, and the theoretical magnetic energy product can reach 1MJ/m at most 3 And the rare earth has the advantages of low cost, high temperature stability, strong heat resistance, excellent oxidation resistance and the like due to low rare earth content, has very high practical performance, and can be widely applied to the industries of motors, electronics, instruments, automation, computers, automobiles, medical treatment, household appliances and the like.
In recent years, researchers have focused on the development of nano-sized two-phase composite materials, mainly on the improvement of magnetic properties and engineering applications. In the aspect of improving the magnetic performance, the reasonable design of the alloy components is an effective way for obtaining high magnetic performance of the nano dual-phase composite material. The adjustment of alloy components can improve the intrinsic characteristics of the magnet such as magnetocrystalline anisotropy, saturation magnetization and the like, and can also improve the magnetic performance by improving the microstructure of crystal grains.
In the aspect of engineering application, the nano dual-phase composite material has the dual characteristics of soft magnetic materials and hard magnetic materials, has an almost reversible magnetization characteristic curve, has good magnetizing and demagnetizing performances, shows a strong remanence enhancement effect and a potential maximum magnetic energy product, and can realize permanent magnet maintenance in closing. Based on these advantages, li Yue et al (Li Yue, cai Zhiyuan, wang Shuai, design of 308A nano two-phase composite permanent magnet contactor electrical switch, 2012, 1.
The magnetically controlled reactor is an electromagnetic device for reactive power compensation for new energy grid connection, and has obvious advantages for solving the problems of reactive power regulation, transient overvoltage, light line load loss and the like of a long-distance and large-capacity power transmission line and coping with severe tidal current change caused by centralized access of new energy power transmission. The traditional magnetically controlled reactor mostly adopts silicon steel materials to manufacture iron cores, and has the problems of high loss, high cost, complex structure and the like. The nano dual-phase composite material is adopted to replace a silicon steel material to serve as the iron core of the magnetically controlled reactor, so that the iron core has a remarkable energy-saving effect, and long-term stable service of a device is ensured due to high corrosion resistance and excellent temperature stability. The novel nano biphase composite material for the magnetic control reactor is required to have the characteristics of high remanence and low coercive force, so that the material can provide a larger constant magnetic field and can realize the function conversion of a hard magnetic phase and a soft magnetic phase with smaller energy consumption. However, the existing reports about Pr/Nd-based nano two-phase composite materials show lower remanence and large coercive force, and the magnetic characteristics are not matched with the application requirements of the magnetically controlled reactor and are difficult to apply.
CN101425355B discloses a Pr/Nd-based biphase nano composite permanent magnetic material and a preparation method of a block thereof, and the general formula of the material composition is (Pr 101425355B) w Nd 100-w ) x Fe 100-x-y-z-m-n R y Ti z Q m B n Wherein Q is any one of V, mo, zr, si, W and Au, and after the raw materials are smelted, quickly quenched in vacuum and processed at ultrahigh pressure, the finally obtained magnet has the advantages of excellent magnetic performance, strong oxidation resistance, good machining performance and the like, and the optimal magnetic performance is as follows: b is r ＝0.84T，H c ＝879.82kA/m，(BH) max ＝159.1kJ/m 3 . CN1858861A discloses a RE-Fe-B-based high-performance nano composite permanent magnet material containing Ti and C. Said material having the general formula RE x Fe 100-x-y-z-w B y Ti z C w The composition shown in the specification, wherein RE is at least one rare earth element excluding La and Ce, the composite addition of Ti and C refines the grain size and remarkably improves the magnetic property, and B r ＞0.7T、H c Not less than 500kA/m. The two types of nano dual-phase composite materials both use a precious rare earth metal RE (such as Pr, nd and the like) base 2.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to overcome the defect of the magnetic property of the existing nano two-phase composite material for the magnetic control reactor, and the invention aims to provide the high-abundance rare earth element-based nano two-phase composite material which has the advantages of low cost, high remanence, low coercive force, good squareness of a hysteresis loop and the like and meets the magnetic property requirement of the nano two-phase composite material for the magnetic control reactor.
A high-abundance rare earth element-based nano two-phase composite material with a general formula of RE x (Fe 1-y Co y ) 95-x-z M z B 5 The composition represented, wherein RE is a high-abundance rare earth element, M is a transition group element, and the composition ratios x, y, and z satisfy inequalities: x is more than or equal to 7 atom percent and less than or equal to 11 atom percent, Y is more than or equal to 0.1 atom percent and less than or equal to 0.35 atom percent, z is more than or equal to 0 atom percent and less than or equal to 1 atom percent, and the high-abundance rare earth element RE is one or more of La, ce and Y.
Further, the high-abundance rare earth element-based nano-two-phase composite material also meets at least one of A, B as follows:
A. the transition group element M is one or more of Cu, cr, nb, ti and Zr;
B. the high-abundance rare earth element-based nano two-phase composite material is selected from Y x (Fe 1-y Co y ) 95-x-z M z B 5 (I)、(La 1-m Y m ) x (Fe 1-y Co y ) 95-x-z M z B 5 (II) or (La) 1-m-n Ce n Y m ) x (Fe 1-y Co y ) 95-x-z M z B 5 (III), in the formulas (I) to (III), in the formula (II), m is 0 to 1; in the formula (III), n is 0.1-0.4, and m is 0.05-0.2.
Further preferably, in formula (II), m is 0 to 0.5; in the formula (III), n is 0.4, and m is 0.1.
Further, the preparation method comprises the following steps:
s1, a step: smelting raw materials, namely proportioning Fe, co, B, a rare earth element RE and a transition group element M according to the atomic percentage, carrying out induction smelting on the raw materials under the protection of inert gas to obtain a melt, and then cooling to obtain an ingot;
and S2, a step: melt rapid quenching;
and S3, a step: crystallization treatment;
and S4, a step: performing hot pressing deformation;
and S5, a step: ball milling;
and S6, a step: and (3) bonding and molding in a magnetic field, mixing the magnetic powder with a bonding agent, pressing and molding under the magnetic field, and curing to obtain the nano two-phase composite material magnet.
And further, the melt rapid quenching in the step S2 is to crush the ingot and put the ingot into a quartz tube of a melt rapid quenching furnace, remelt the ingot under the protection of inert gas, and overflow the ingot onto a cooling copper roller for melt rapid quenching to form a uniform thin strip with the thickness of 20-40 mu m and the width of 1-2 mm.
More preferably, the rotation speed of the melt rapid quenching is 40-50 m/s.
Further, the step S3 of crystallization treatment is to put the rapid quenching strip into a vacuum heat treatment furnace, raise the temperature to the crystallization temperature at the speed of 5-20 ℃/min and keep the temperature for 5-10 min.
Still more preferably, the crystallization temperature is 650 to 800 ℃.
Further, the S4 step hot pressing deformation is to heat the strip to a hot pressing temperature and then apply a pressure of 400-600 MPa in a direction parallel to the thickness direction of the strip to thermally deform the strip.
Still more preferably, the hot pressing temperature is 600 to 800 ℃.
Further, in the step S5, the ball milling adopts a vibration ball milling or rolling ball milling mode to crush the strip materials into powder with the particle size of 3-5 microns.
Further, the adhesive of the step S6 is one or more of epoxy resin, phenolic resin and novolac resin.
Further, the pressure of the magnetic field in the step S6 is 100-300 MPa, the size is 2-4T, the curing temperature is 60-180 ℃, and the curing time is 1-3 hours.
Further, the prepared high-abundance rare earth element-based nano two-phase composite material is applied to a magnetically controlled reactor.
Compared with the prior art, the invention has the following advantages:
1. the invention relates to a high-abundance rare earth element-based nano two-phase composite material, wherein the RE of the high-abundance rare earth element is one or more of La, ce and Y, and the content of the RE is 7-11 atomic percent. Compared with the common Pr and Nd elements in the nano two-phase composite material, the La, ce and Y elements have richer contents and lower price. Wherein, the prices of La and Ce are equivalent to about 1/10 of Pr and Nd, and the price of Y is about 1/2 of Pr and Nd. And (Pr, nd) commonly used in nano biphase composite material 2 Fe 14 Compared with B hard magnetic phase, the material formed by high-abundance rare earth elements La, ce and Y and Fe and B elements (such as RE) 2 Fe 14 B) Has a lower magnetocrystalline anisotropy field of (Pr, nd) 2 Fe 14 1/4 of the phase B, x is more than or equal to 7 atom percent and less than or equal to 11 atom percent, y is more than or equal to 0.1 atom percent and less than or equal to 0.35 atom percent, z is more than or equal to 0 atom percent and less than or equal to 1 atom percent, so that the content of Co is between 8.3 and 30.8 atom percent, and a proper amount of Co element replaces Fe in the nano two-phase composite material, thereby improving the Curie temperature of the magnet, enhancing the thermal stability, and simultaneously realizing the effects of reducing the coercive force and improving the remanence. Therefore, the nano biphase composite material has more advantages in meeting the magnetic performance requirements of high remanence and low coercive force of the nano biphase composite material for the magnetic control reactor. The content of the transition group element M is in the range of 0-1 atomic percent, and the doping of a small amount of the transition group element can promote the formation of RE on the one hand 2 (FeCo) 14 On the other hand, the B/alpha- (FeCo) nano biphase mixture can be strongly segregated at the grain boundary, so that the size of nano crystal grains is sharply reduced, the coupling effect between soft magnetic phase and hard magnetic phase is enhanced, the remanence enhancement effect is high, and the squareness of a hysteresis loop is good.
2. In the preparation method of the high-abundance rare earth element-based nano dual-phase composite material, the anisotropic nano dual-phase composite material strip is obtained by adopting a hot-pressing deformation mode, the residual amorphous tissue in the strip can be further subjected to nano crystallization in the process, the exchange coupling effect between soft and hard magnetic phases is improved, and the remanence enhancement effect is enlarged. Meanwhile, the nano-crystalline grains in the strip material are subjected to thermal deformation under the action of the hot pressure, and a texture is formed along the pressure direction, so that the strip material has anisotropy, and compared with an isotropic strip material, the anisotropic strip material has better squareness of a hysteresis curve, and has larger remanence and smaller coercive force in the direction of an easy magnetization axis.
3. In the preparation method of the high-abundance rare earth element-based nano two-phase composite material, the nano two-phase composite material magnet is obtained by adopting a magnetic field bonding forming method, compared with sintering forming, the magnet obtained by the bonding forming method has smaller nanocrystalline particle size, stronger exchange coupling effect between soft and hard magnetic phases and more obvious remanence enhancement effect. The magnetic field of 2-4T is applied in the bonding forming process and is far larger than the saturation magnetic induction intensity of the magnetic powder, so that the magnetic powder can be fully oriented along the magnetic field direction, the magnetic anisotropy is further improved, the magnetic field direction is vertical to the pressure direction, larger orientation factors can be obtained, the residual magnetism is higher, and the magnet meets the magnetic performance requirement of the nano two-phase composite material for the magnetic control reactor.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is Y 7 (Fe 0.9 Co 0.1 ) 87.9 Cu 0.1 B 5 XRD patterns of the cast ingot at different rapid quenching speeds;
FIG. 2 is Y 7 (Fe 0.9 Co 0.1 ) 87.9 Cu 0.1 B 5 XRD patterns of the rapid quenching strips at different crystallization treatment temperatures;
FIG. 3 is Y 7 (Fe 0.9 Co 0.1 ) 87.9 Cu 0.1 B 5 J-H curves of the nano biphase composite material magnet at different crystallization treatment temperatures;
FIG. 4 is Y 7 (Fe 0.9 Co 0.1 ) 87.9 Cu 0.1 B 5 Hysteresis loops of the strip in directions parallel and perpendicular to the hot deformation pressure.
Detailed Description
Example 1
The high-abundance rare earth element-based nano two-phase composite material comprises the following components in percentage by formula: y is 7 (Fe 0.9 Co 0.1 ) 87.9 Cu 0.1 B 5 。
The preparation method of the nano two-phase composite material comprises the following steps:
s1, a step: smelting raw materials, namely preparing elemental iron, elemental cobalt, elemental copper, elemental boron and elemental yttrium with the purity of 99.9 percent according to the atomic percentage, putting the prepared raw materials into a crucible of a vacuum induction furnace, carrying out induction smelting on the raw materials for 5 times under the protection of inert gas argon to obtain a uniformly smelted melt, then putting the melt into a water-cooled copper crucible for cooling to obtain Y 7 (Fe 0.9 Co 0.1 ) 87.9 Cu 0.1 B 5 And (5) casting a mother alloy ingot.
And S2, a step: and (2) melt rapid quenching, namely crushing the ingot prepared in the step (S1) and then placing the crushed ingot into a quartz tube of a melt rapid quenching furnace, wherein the pressure difference of protective gas inside and outside the quartz tube is set to be 0.8MPa, the diameter of the quartz tube mouth is 0.3mm, and the distance from a nozzle to the surface of a copper roller is 0.75mm. Re-melting the cast ingot under the protection of inert gas argon, overflowing the cast ingot onto a cooling copper roller with the rotating speed of 50m/s for melt rapid quenching to obtain Y with the thickness of 30 mu m and the width of 1.5mm 7 (Fe 0.9 Co 0.1 ) 87.9 Cu 0.1 B 5 And (6) rapidly quenching the strip.
And S3, a step: and (3) performing crystallization treatment, namely putting the quick quenching strip prepared in the step (S2) into a vacuum heat treatment furnace, heating the furnace to 800 ℃ at the heating rate of 10 ℃/min, and keeping the temperature for 8min. And after the heat preservation is finished, cooling the strip to room temperature along with the furnace to obtain the nano two-phase composite strip.
And S4, a step: and (3) carrying out hot-pressing deformation, namely heating the nano two-phase composite material strip obtained in the step (S3) to 650 ℃, then applying 400MPa of pressure in a direction parallel to the thickness direction of the strip to deform the strip, and reducing the thickness to 20 mu m to obtain the anisotropic nano two-phase composite material strip.
And S5, a step: and (4) ball milling, namely crushing the belt material obtained in the step (S4) into powder with the diameter of about 3-5 mu m by adopting a rolling ball milling mode to obtain the nanometer double-phase composite material magnetic powder.
And S6, a step: and (3) magnetic field bonding molding, namely mixing the magnetic powder obtained in the step (S5) with an epoxy resin binder, uniformly mixing, injecting into a mold made of a non-magnetic material, performing magnetic field compression molding under the pressure of 100MPa, wherein the magnetic field is 2T, the direction of the magnetic field is vertical to the direction of the pressure, and curing for 2 hours at 170 ℃ to obtain the anisotropic nano two-phase composite material magnet.
Example 2
A series of high-abundance rare earth element-based nano two-phase composite materials comprise the following components in percentage by formula: (La) 1- m Y m ) 9 (Fe 0.9 Co 0.1 ) 85.9 Ti 0.1 B 5 Wherein m is 0, 0.1, 0.2, 0.3, 0.4, 0.5, 0.6, 07, 0.8, 0.9 and 1 respectively.
The preparation method of the nano two-phase composite material comprises the following steps:
s1, a step: smelting raw materials, namely preparing elemental iron, elemental cobalt, elemental titanium, elemental boron, elemental lanthanum and elemental yttrium with the purity of 99.9 percent according to the atomic percentage, putting the prepared raw materials into a crucible of a vacuum induction furnace, carrying out induction smelting on the raw materials for 5 times under the protection of inert gas argon to obtain a uniformly smelted melt, then putting the melt into a water-cooled copper crucible, and cooling to obtain (La) 1-m Y m ) 9 (Fe 0.9 Co 0.1 ) 85.9 Ti 0.1 B 5 And (5) casting a mother alloy ingot.
And S2, a step: and (3) melt rapid quenching, namely crushing the ingot prepared in the step (S1), and then putting the ingot into a quartz tube of a melt rapid quenching furnace, wherein the pressure difference of protective gas inside and outside the quartz tube is set to be 0.8MPa, the diameter of the quartz tube nozzle is 0.3mm, and the distance from the nozzle to the surface of a copper roller is 0.75mm. The cast ingot is remelted under the protection of inert gas argonMelting, overflowing onto a cooled copper roller with rotation speed of 50m/s, and rapidly quenching to obtain (La) with thickness of 30 μm and width of 1.5mm 1-m Y m ) 9 (Fe 0.9 Co 0.1 ) 85.9 Ti 0.1 B 5 And (6) rapidly quenching the strip.
And S3, a step: and (3) performing crystallization treatment, namely putting the quick quenching strip prepared in the step (S2) into a vacuum heat treatment furnace, heating the furnace to 800 ℃ at the heating rate of 10 ℃/min, and keeping the temperature for 8min. And after the heat preservation is finished, cooling the strip to room temperature along with the furnace to obtain the nano two-phase composite strip.
And S4, a step: and (3) carrying out hot-pressing deformation, namely heating the nano two-phase composite material strip obtained in the step (S3) to 650 ℃, then applying 400MPa of pressure in a direction parallel to the thickness direction of the strip to deform the strip, and reducing the thickness to 20 mu m to obtain the anisotropic nano two-phase composite material strip.
And S5, a step: and (4) ball milling, namely crushing the strip material obtained in the step (S4) into powder with the diameter of about 3-5 mu m by adopting a rolling ball milling mode to obtain the nano double-phase composite material magnetic powder.
And S6, a step: and (3) magnetic field bonding molding, namely mixing the magnetic powder obtained in the step (S5) with an epoxy resin binder, uniformly mixing, injecting into a mold made of a non-magnetic material, performing magnetic field compression molding under the pressure of 100MPa, wherein the magnetic field is 2T, the direction of the magnetic field is vertical to the direction of the pressure, and curing for 2 hours at 170 ℃ to obtain the anisotropic nano two-phase composite material magnet.
Measured by Vibrating Sample Magnetometer (VSM) (La) 1-m Y m ) 9 (Fe 0.9 Co 0.1 ) 85.9 Ti 0.1 B 5 The magnetization curves of the magnets are listed in Table 1 (La) 1-m Y m ) 9 (Fe 0.9 Co 0.1 ) 85.9 Ti 0.1 B 5 As can be seen from the table, the coercive force of the magnet is changed within the range of 10-148 kA/m and is much smaller than the coercive force (H) of the Pr/Nd-based nano two-phase composite material c Not less than 500 kA/m), when m is 0-0.5, the remanence is changed in the range of 0.70-0.90T and is higher than that of Pr/Nd base nanometer biphase magnetic material (B) r = 0.7T), satisfies the magnetic control reactanceThe nanometer double-phase composite material has high remanence and low coercive force. The remanence and the coercive force of the rapid quenching strip are gradually reduced along with the gradual increase of the content of the Y element, and the value is represented by J when m =0 r ＝0.90T、H c J when =148kA/m decreases to m =1 r ＝0.35T、H c ＝10kA/m。
TABLE 1 (La) 1-m Y m ) 9 (Fe 0.9 Co 0.1 ) 85.9 Ti 0.1 B 5 Magnetic parameters of magnet
Example 3
A series of high-abundance rare earth element-based nano dual-phase composite materials comprise the following components in percentage by formula: (La) 1-m-n Ce n Y m ) 11 (Fe 0.7 Co 0.3 ) 83.9 Cu 0.1 B 5 . The values of m and n are shown in the following table.
The preparation method of the nano two-phase composite material comprises the following steps:
s1, a step: smelting raw materials, namely preparing simple substance iron, simple substance cobalt, simple substance copper, simple substance boron, simple substance lanthanum, simple substance cerium and simple substance yttrium with the purity of 99.9 percent according to the atomic percentage, putting the prepared raw materials into a crucible of a vacuum induction furnace, carrying out induction smelting on the raw materials for 5 times under the protection of inert gas argon to obtain a uniformly smelted melt, then putting the melt into a water-cooled copper crucible for cooling to obtain (La) 1-m-n Ce n Y m ) 11 (Fe 0.7 Co 0.3 ) 83.9 Cu 0.1 B 5 And (5) casting a mother alloy ingot.
S1, a step: and (2) melt rapid quenching, namely crushing the ingot prepared in the step (S1), putting the ingot into a quartz tube of a melt rapid quenching furnace, setting the pressure difference of protective gas inside and outside the quartz tube to be 0.8MPa, and setting the diameter of a quartz tube nozzle to be0.3mm and the distance from the nozzle to the surface of the copper roll was 0.75mm. Re-melting the cast ingot under the protection of inert gas argon, overflowing the cast ingot onto a cooling copper roller with the rotating speed of 50m/s for melt rapid quenching to obtain the (La) with the thickness of 30 mu m and the width of 1.5mm 1-m-n Ce n Y m ) 11 (Fe 0.7 Co 0.3 ) 83.9 Cu 0.1 B 5 And (4) rapidly quenching the strip.
And S3, a step: and (3) performing crystallization treatment, namely putting the quick quenching strip prepared in the step (S2) into a vacuum heat treatment furnace, heating the furnace to 800 ℃ at the heating rate of 10 ℃/min, and keeping the temperature for 8min. And after the heat preservation is finished, cooling the strip to room temperature along with the furnace to obtain the nano dual-phase composite strip.
And S4, a step: and (3) carrying out hot-pressing deformation, namely heating the nano two-phase composite material strip obtained in the step (S3) to 650 ℃, then applying 400MPa of pressure in a direction parallel to the thickness direction of the strip to deform the strip, and reducing the thickness to 20 mu m to obtain the anisotropic nano two-phase composite material strip.
And S5, a step: and (4) ball milling, namely crushing the strip material obtained in the step (S4) into powder with the diameter of about 3-5 mu m by adopting a rolling ball milling mode to obtain the nano double-phase composite material magnetic powder.
And S6, a step: and (3) magnetic field bonding molding, namely mixing the magnetic powder obtained in the step (S5) with an epoxy resin binder, uniformly mixing, injecting into a mold made of a non-magnetic material, performing magnetic field compression molding under the pressure of 100MPa, wherein the magnetic field is 2T, the direction of the magnetic field is vertical to the direction of the pressure, and curing for 2 hours at 170 ℃ to obtain the anisotropic nano two-phase composite material magnet. Table 2 lists (La) 1-m-n Ce n Y m ) 11 (Fe 0.7 Co 0.3 ) 83.9 Cu 0.1 B 5 As can be seen from the table, the magnetic performance of the strip is gradually increased with the increasing Ce content, and when the Ce content is 4.4 atomic%, the magnetic performance of the strip is the highest, at the moment, the coercive force is 183kA/m, the remanence is 1.10T, and the maximum magnetic energy product is 7.7MGOe. Compared with Pr/Nd base nanometer biphase composite material, the magnet has the advantages of large remanence and small coercive force, meets the magnetic performance requirement of the nanometer biphase composite material for the magnetic control reactor, and can be used as the magnetic control reactorA magnetically controlled reactor core material.
TABLE 2 (La) 1-m-n Ce n Y m ) 11 (Fe 0.7 Co 0.3 ) 83.9 Cu 0.1 B 5 Magnetic parameters of magnet
Experimental example 1
The experiment aims to investigate the influence of the ingot casting in the step S2 on the prepared composite material at different rapid quenching speeds, the material components and content and other process conditions and parameters are the same as those in the example 1, only the rapid quenching speed is 10-50 m/S, and the result is shown in figure 1.
FIG. 1 is Y 7 (Fe 0.9 Co 0.1 ) 87.9 Cu 0.1 B 5 The XRD pattern of the cast ingot under different rapid quenching speeds can be known, when the rapid quenching speed is 10-40 m/s, a plurality of diffraction peaks exist in the XRD pattern, which shows that nano-crystalline grains are separated out from the strip under the rapid quenching speed, and the subsequent crystallization treatment is not beneficial to obtaining a nano-crystalline structure with fine and uniform particle size. When the rapid quenching speed is 50m/s, the XRD pattern is a typical amorphous pattern, and a uniform nanocrystalline structure is easier to form through subsequent crystallization treatment. Therefore, in order to ensure that the rapid quenching strip obtains an ideal nanocrystalline structure in the subsequent crystallization treatment, the rapid quenching speed is controlled to be 40-50 m/s.
Experimental example 2
In order to investigate the influence of different crystallization treatment temperatures in the step S3 on the prepared high-abundance rare earth element-based composite material, the material components and content and other process conditions and parameters are the same as those in example 1, only the crystallization temperature is set to be 500-800 ℃, the XRD diagram is shown in FIG. 2, and the J-H curve is shown in FIG. 3.
FIG. 2 is Y 7 (Fe 0.9 Co 0.1 ) 87.9 Cu 0.1 B 5 The XRD pattern of the rapid quenching strip at different crystallization treatment temperatures can show that when the crystallization treatment temperature is less than 650 ℃, no plurality of diffraction peaks appear in the XRD patternIt is shown that no nano-crystalline grains are formed in the ribbon and therefore the crystallization treatment temperature should be greater than 650 c. After being hot-pressed and crystallized at 650-800 ℃, Y 7 (Fe 0.9 Co 0.1 ) 87.9 Cu 0.1 B 5 The rapid quenching strip shows a plurality of crystal diffraction peaks, which indicates that the rapid quenching alloy is crystallized. And the main precipitated phase is Y through the calibration of diffraction peak 2 Fe 14 B hard magnetic phase and alpha-Fe soft magnetic phase, which proves that the rapid quenching strip is a nano two-phase composite strip after the thermal compression crystallization treatment at 650-800 ℃.
FIG. 3 is Y 7 (Fe 0.9 Co 0.1 ) 87.9 Cu 0.1 B 5 The J-H curve of the magnet at different crystallization temperatures is shown in the figure, Y 7 (Fe 0.9 Co 0.1 ) 87.9 Cu 0.1 B 5 The magnetic hysteresis loop of the magnet has good squareness and shows single permanent magnetic performance, which shows that strong exchange coupling effect is generated between the soft magnetic phase and the hard magnetic phase in the magnet. Table 3 lists Y 7 (Fe 0.9 Co 0.1 ) 87.9 Cu 0.1 B 5 The coercive force of the magnetic performance parameters of the magnet after crystallization treatment at different temperatures is between 60 and 75kA/m and is far less than the coercive force (H) of the Pr/Nd-based nano two-phase composite material c ≥500kA/m)。
TABLE 3Y 7 (Fe 0.9 Co 0.1 ) 87.9 Cu 0.1 B 5 Magnetic performance parameters of magnet at different crystallization treatment temperatures
Experimental example 3
The experiment aims to investigate the influence of hot-pressing deformation in the step S4 on the magnetic performance of the prepared high-abundance rare earth element-based nano dual-phase composite material, the material components and content and other process conditions and parameters are the same as those in the example 1, and the result is shown in FIG. 4.
FIG. 4 is Y 7 (Fe 0.9 Co 0.1 ) 87.9 Cu 0.1 B 5 Hysteresis loops of the strip in directions parallel and perpendicular to the direction of the hot deformation pressure, wherein the hysteresis loops parallel to the hot deformation pressure are shown by solid lines and the hysteresis loops perpendicular to the direction of the hot deformation pressure are shown by dashed lines. As can be seen from the figure, after the hot-pressing deformation process, the hysteresis loops of the strip material in two directions are not overlapped, which shows that the hot-pressing deformation process can enable the strip material to have anisotropy, and the direction parallel to the hot-deformation pressure direction is the direction of the easy magnetization axis. Meanwhile, compared with a magnetic hysteresis loop perpendicular to the thermal deformation pressure direction, the magnetic hysteresis loop parallel to the thermal deformation pressure direction has the advantages of better squareness, large remanence and small coercive force, which shows that the easy magnetization axis direction of the anisotropic strip material is easier to obtain high remanence and low coercive force, and the magnetic performance requirement of the nano biphase composite material for the magnetic control reactor is met.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (14)
1. A high-abundance rare earth element-based nano dual-phase composite material with a general formula of RE x (Fe 1-y Co y ) 95-x-z M z B 5 The composition represented, wherein RE is a high-abundance rare earth element, M is a transition group element, and the composition ratios x, y, and z satisfy inequalities: x is more than or equal to 7 atom percent and less than or equal to 11 atom percent, Y is more than or equal to 0.1 atom percent and less than or equal to 0.35 atom percent, z is more than or equal to 0 atom percent and less than or equal to 1 atom percent, and the high-abundance rare earth element RE is one or more of La, ce and Y.
2. The high abundance rare earth element-based nano-bi-phase composite of claim 1, wherein the high abundance rare earth element-based nano-bi-phase composite further satisfies at least one of A, B:
A. the transition group element M is one or more of Cu, cr, nb, ti and Zr;
B. the high-abundance rare earth element-based nano dual-phase composite material is selected from Y x (Fe 1-y Co y ) 95-x-z M z B 5 (I)、(La 1-m Y m ) x (Fe 1- y Co y ) 95-x-z M z B 5 (II) or (La) 1-m-n Ce n Y m ) x (Fe 1-y Co y ) 95-x-z M z B 5 (III) in the formulas (I) to (III), m in the formula (II) is 0 to 1, n in the formula (III) is 0.1 to 0.4, and m is 0.05 to 0.2.
3. The high abundance rare earth element-based nano biphasic composite of claim 2, wherein in formula (II), m is 0-0.5; in the formula (III), n is 0.4 and m is 0.1.
4. The method for preparing the high-abundance rare-earth-based nano-bi-phase composite material according to any one of claims 1 to 3, wherein the method comprises the following steps:
s1, a step: smelting raw materials, namely proportioning Fe, co, B, a rare earth element RE and a transition group element M according to the atomic percentage, carrying out induction smelting on the raw materials under the protection of inert gas to obtain a melt, and then cooling to obtain an ingot;
and S2, a step: melt rapid quenching;
and S3, a step: crystallization treatment;
and S4, a step: performing hot pressing deformation;
and S5, a step: ball milling;
and S6, a step: and (3) bonding and molding in a magnetic field, mixing the magnetic powder with a bonding agent, pressing and molding under the magnetic field, and curing to obtain the nano two-phase composite material magnet.
5. The method for preparing the high-abundance rare-earth-element-based nano dual-phase composite material according to claim 4, wherein the step S2 is melt-quenching, in which an ingot is crushed and then placed in a quartz tube of a melt-quenching furnace, the ingot is re-melted under the protection of inert gas, and then overflows onto a cooling copper roller for melt-quenching, so as to form a uniform thin strip with the thickness of 20-40 μm and the width of 1-2 mm.
6. The method for preparing the high-abundance rare-earth-element-based nano dual-phase composite material according to claim 5, wherein the rotation speed of the melt rapid quenching is 40-50 m/s.
7. The method for preparing the high-abundance rare-earth-element-based nano dual-phase composite material according to claim 4, wherein the S3 step of crystallization treatment is to put a rapid quenching strip into a vacuum heat treatment furnace, raise the temperature to the crystallization temperature at a rate of 5-20 ℃/min and keep the temperature for 5-10 min.
8. The method for preparing the high-abundance rare-earth-element-based nano dual-phase composite material according to claim 7, wherein the crystallization temperature is 650-800 ℃.
9. The method for preparing the high-abundance rare-earth-element-based nano dual-phase composite material according to claim 4, wherein the S4 step hot-pressing deformation is that the strip is heated to a hot-pressing temperature, and then a pressure of 400-600 MPa is applied in a direction parallel to the thickness direction of the strip to thermally deform the strip.
10. The method for preparing the high-abundance rare-earth-element-based nano dual-phase composite material according to claim 9, wherein the hot-pressing temperature is 600-800 ℃.
11. The preparation method of the high-abundance rare-earth-element-based nano two-phase composite material according to claim 4, wherein the ball milling in the step S5 is performed by adopting a vibration ball milling or rolling ball milling mode to crush the strip material into powder with the particle size of 3-5 μm.
12. The method for preparing the high-abundance rare-earth-element-based nano dual-phase composite material according to claim 4, wherein the binder in the S6 step is one or more of epoxy resin, phenolic resin and novolac resin.
13. The method for preparing the high-abundance rare-earth-element-based nano dual-phase composite material according to claim 4, wherein the pressure of the magnetic field in the step S6 is 100-300 MPa, the size is 2-4T, the curing temperature is 60-180 ℃, and the curing time is 1-3 hours.
14. Use of the high-abundance rare-earth-element-based nano-bi-phase composite according to any one of claims 1 to 3 or the high-abundance rare-earth-element-based nano-bi-phase composite prepared according to any one of claims 4 to 13 in a magnetically controlled reactor.
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