CN108335897B - NdCeFeB isotropic compact permanent magnet and preparation method thereof - Google Patents
NdCeFeB isotropic compact permanent magnet and preparation method thereof Download PDFInfo
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- H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
- H01F1/0577—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together sintered
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Abstract
The invention discloses an NdCeFeB isotropic compact permanent magnet and a preparation method thereofx(FeCo)94‑x‑y‑zNbyGazB6Alloy thin strip, preparing the sputtering target material of Cu-Ce alloy and Ce-Co alloy, and plating the prepared sputtering target material on Ndx(FeCo)94‑x‑y‑zNbyGazB6The invention takes NdFeB as a matrix, and diffuses light rare earth alloys CeCu and CeCo into the matrix by adopting a hot pressing technology, thereby improving the coercive force of the magnet and obtaining the permanent magnet with good magnetic property.
Description
Technical Field
The invention relates to the technical field of magnetic material preparation, in particular to an NdCeFeB isotropic compact permanent magnet and a preparation method thereof.
Background
The neodymium iron boron permanent magnetic alloy has excellent permanent magnetic performance and is widely applied to a plurality of fields of new energy, electronics, automobiles, rail transit, national defense industry and the like.
Along with the development of intelligent automobiles, electric automobiles, rail transit and new energy industries in recent years, the social demand for high-performance neodymium-iron-boron permanent magnets is increased dramatically year by year. Because the curie temperature of the neodymium iron boron permanent magnet alloy is low, the working temperature of the neodymium iron boron permanent magnet alloy is low, and in order to increase the working temperature as much as possible, a large amount of rare earth elements, especially heavy rare earth elements are often required to be added into the existing alloy so as to greatly improve the alloy straighteningThe toughness, which results in a significant increase in the cost of alloy manufacture. In order to fully utilize the low-cost light rare earth elements such as Ce, people are trying to prepare Ce2Fe14The magnetic performance of the B permanent magnet alloy is far lower than that of the NdFeB alloy, so that the B permanent magnet alloy cannot be practically applied.
Disclosure of Invention
In order to solve the technical problems, the invention provides an NdCeFeB isotropic compact permanent magnet and a preparation method thereof.
The technical scheme is as follows: the preparation method of the NdCeFeB isotropic dense permanent magnet is characterized by comprising the following steps of:
(1) preparing Nd according to atomic percentagex(FeCo)94-x-y-zNbyGazB6The alloy thin strip is characterized in that x is 8-14, y is 0-1, and z is 0-0.5;
(2) respectively preparing a copper-cerium alloy and a cerium-cobalt alloy, and respectively preparing the copper-cerium alloy and the cerium-cobalt alloy into sputtering targets;
(3) plating the sputtering target material on the Ndx(FeCo)94-x-y-zNbyGazB6Obtaining a mixed thin strip on the alloy thin strip;
(4) and crushing the mixed thin strip, and performing hot pressing treatment on the obtained powder to obtain the NdCeFeB isotropic compact permanent magnet.
By adopting the technical scheme, the light rare earth alloy CeCu and CeCo is diffused into the matrix by adopting the traditional NdFeB as the matrix and adopting the hot pressing technology, so that the coercive force of the magnet is improved, the prepared permanent magnet has high coercive force, the traditional heavy rare earth element is not adopted at all, and the production cost is effectively reduced.
The ratio of cerium to copper in the copper-cerium alloy is 7:3 in terms of atomic percentage.
The ratio of cerium to cobalt in the cerium-cobalt alloy is 7:3 calculated by atomic percentage.
The sputtering target material accounts for 10-30% of the total weight of the mixed thin strip by mass percentage.
The hot-pressing temperature of the hot-pressing treatment is 650-.
When x is less than or equal to 12, the pressure of the hot pressing treatment is 150MPa, and when x is more than 12, the pressure of the hot pressing treatment is less than 150 MPa. When the content of Nd is lower, the prepared permanent magnet can be densified better by matching with high-pressure treatment, and when the content of Nd is higher, the permanent magnet with higher density can be obtained at lower pressure.
The hot pressing treatment method is spark plasma sintering. The hot pressing treatment mode can be vacuum induction hot pressing or the like besides spark plasma sintering, and is not limited to spark plasma sintering.
A dense NdCeFeB isotropic permanent magnet is characterized in that: prepared by the preparation method.
Has the advantages that: the invention takes NdFeB as a matrix, and diffuses the light rare earth alloy CeCu and CeCo into the matrix by adopting a hot pressing technology, thereby improving the coercive force of the magnet, obtaining the permanent magnet with good magnetic performance, simultaneously adopting a liquid diffusion mode as an alloy adding mode, not needing to be smelted again when preparing the alloy, directly treating the existing NdFeB magnetic powder, having simple preparation process and low cost of used raw materials, and being suitable for large-scale production.
Drawings
FIG. 1 is a graph showing demagnetization curves of samples 1 to 5 and a reference 1;
FIG. 2 is a graph showing demagnetization curves of samples 6 to 10 and comparative sample 1;
FIG. 3 is a graph showing demagnetization curves of samples 11 to 12 and comparative sample 2;
fig. 4 is a graph showing demagnetization curves of sample 13 and control 3.
Detailed Description
The invention is further illustrated by the following examples and figures.
Example 1, an NdCeFeB isotropic dense permanent magnet prepared according to the following steps:
(1) preparation of Nd13Fe74Co7B6Alloy thin strip: according to atomic percentage, the nominal component is Nd13Fe74Co7B6Gold (II) ofBelongs to raw materials, alloy cast ingots are obtained by vacuum melting and are repeatedly melted for three times to ensure that the components of the alloy cast ingots are uniform, the melted alloy cast ingots are crushed and then subjected to vacuum melt spinning at the melt spinning speed of 30m/s to obtain Nd13Fe74Co7B6An alloy thin strip;
(2) preparing a mixed thin strip: according to the atomic percentage, the Ce is prepared by vacuum melting7Cu3Alloying, preparing a sputtering target material with the diameter of 2 inches, and then adopting magnetron sputtering to prepare Ce7Cu3Alloy is plated on the Nd13Fe74Co7B6On the alloy thin strip, controlling Ce by controlling sputtering time7Cu3In amounts such that they represent about 10%, 20% and 30% by weight of the total weight, respectively, to obtain three mixed ribbons;
(3) preparation of NdCeFeB isotropic dense permanent magnet: respectively crushing the three mixed thin strips into 80-mesh powder in a glove box, respectively filling the obtained powder into a die, and performing hot pressing treatment by using discharge plasma sintering at the hot pressing temperature of 700 ℃ and the pressure of 50MPa for 3min to obtain three NdCeFeB isotropic compact permanent magnets which are respectively named as sample 1 (containing 10% of Ce)7Cu3) Sample 2 (containing 20% Ce)7Cu3) And sample 3 (containing 30% Ce)7Cu3) The demagnetization curves of samples 1 to 3 were measured, respectively, and the results are shown in FIG. 1.
Example 2, an NdCeFeB isotropic dense permanent magnet prepared according to the following steps: the present embodiment is different from embodiment 1 in that: obtaining 10% Ce sputtered in step (2)7Cu3After the alloy is mixed into a thin strip, the heat preservation time is controlled to be 5min and 10min in the step (3), a sample 4 (heat preservation time of 5min) and a sample 5 (heat preservation time of 10min) are obtained respectively, then demagnetization curves of the samples 4 and 5 are measured respectively, and the influence of the heat preservation time on the performance of the magnet is researched, and the result is shown in figure 1.
Comparative example 1 preparation of NdFeB Isotropic dense permanent magnet as blank control, nominal composition Nd in atomic percent13Fe74B6The metal raw material is subjected to vacuum melting to obtain an alloy ingot, andrepeatedly smelting for three times to ensure that the components of the alloy cast ingot are uniform, crushing the smelted alloy cast ingot, and then carrying out vacuum melt spinning at the melt spinning speed of 30m/s to obtain Nd13Fe74B6An alloy thin strip prepared by forming the Nd13Fe74B6The alloy thin strip is crushed into 80-mesh powder in a glove box, the obtained powder is loaded into a die, hot pressing treatment is carried out by utilizing discharge plasma sintering, the hot pressing temperature is 700 ℃, the pressure is 50MPa, the temperature is kept for 3min to obtain a reference product 1, and the demagnetization curve of the reference product 1 is measured, wherein the result is shown in figure 1.
As is clear from FIG. 1, in comparative example 1, since the CeCu alloy was not added, the coercive force of the magnet was only 5.94kOe, and the density of the magnet was 7.20g/cm3(ii) a In sample 1, 10% Ce was added7Cu3After the alloy is hot-pressed, the coercive force of the magnet is increased to 12.46kOe, and the density of the magnet is also greatly increased to 7.49g/cm3(ii) a In sample 2, 20% of Ce was added7Cu3After the alloy is hot-pressed, the coercive force of the magnet is 12.86kOe, and the density of the magnet is 7.53g/cm3(ii) a In sample 3, with Ce7Cu3The alloy content is gradually increased to 30 percent, the coercive force of the magnet is slightly changed, but the change amplitude is small, and the density of the magnet is increased to 7.55g/cm3。
As can also be seen from FIG. 1, sample 5 has a slightly larger coercive force than sample 4, and the magnet density of sample 5 rises to 7.54g/cm3This indicates that the magnet performance is gradually improved with the increase of the holding time within a certain range. However, the research also finds that if the heat preservation time is too long, the crystal grains grow seriously, and the performance of the magnet is reduced.
Example 3, an NdCeFeB isotropic dense permanent magnet prepared by the following steps:
(1) preparation of Nd13Fe74Co7B6Alloy thin strip: the same as example 1;
(2) preparing a mixed thin strip: according to the atomic percentage, the Ce is prepared by vacuum melting7Co3Alloying, preparing a sputtering target material with the diameter of 2 inches, and then adopting magnetron sputtering to prepare Ce7Co3Alloy is plated on the Nd13Fe74Co7B6On the alloy thin strip, controlling Ce by controlling sputtering time7Co3In amounts such that they represent about 10%, 20% and 30% by weight of the total weight, respectively, to obtain three mixed ribbons;
(3) preparation of NdCeFeB isotropic dense permanent magnet: respectively crushing the three mixed thin strips into 80-mesh powder in a glove box, respectively filling the obtained powder into a die, and performing hot pressing treatment by using discharge plasma sintering at the hot pressing temperature of 700 ℃ and the pressure of 50MPa for 3min to obtain three NdCeFeB isotropic compact permanent magnets which are respectively named as sample 6 (containing 10% of Ce)7Co3) Sample 7 (containing 20% Ce)7Co3) And sample 8 (30% Ce)7Co3) The demagnetization curves of the samples 6 to 8 were measured and compared with the demagnetization curve of the control 1, respectively, and the results are shown in fig. 2.
Example 4, an NdCeFeB isotropic dense permanent magnet prepared according to the following steps: the present embodiment is different from embodiment 3 in that: obtaining 10% Ce sputtered in step (2)7Co3After the alloy is mixed into a thin strip, the heat preservation time is controlled to be 5min and 10min in the step (3), a sample 9 (heat preservation time is 5min) and a sample 10 (heat preservation time is 10min) are respectively obtained, then demagnetization curves of the samples 9 and 10 are respectively measured, the influence of the heat preservation time on the performance of the magnet is researched, and the result is shown in fig. 2.
As can be seen from FIG. 2, Ce was not added7Co3The magnet coercive force of the alloy reference 1 is only 5.94 kOe; in sample 6, 10% Ce was added7Co3After the alloy is hot-pressed, the coercive force of the magnet is increased to 13.65kOe, and the density of the magnet is increased to 7.50g/cm3(ii) a In sample 7, 20% Ce was added7Co3After the alloy is hot-pressed, the coercive force of the magnet is increased to 12.58kOe, and the density of the magnet is 7.54g/cm3(ii) a In sample 8, Ce7Co3The content of the alloy is gradually increased to 30 percent, the coercive force of the magnet is 12.54kOe, and the density of the magnet is 7.60g/cm3。
It can also be seen that, as the holding time is prolonged to 10min, the coercivity of sample 10 is increased to 14.31kOe, which is a large improvement compared with sample 9The density of the magnet was 7.55g/cm3This indicates that the coercive force of the magnet gradually increases with the increase of the holding time within a certain range. However, the research also finds that if the heat preservation time is too long, the crystal grains grow seriously, the performance of the magnet is reduced, and the density of the magnet is smaller if the heat preservation time is too short.
Example 5, an NdCeFeB isotropic dense permanent magnet prepared according to the following steps:
(1) preparation of Nd11Fe81.5Nb1Ga0.5B6Alloy thin strip: according to atomic percentage, the nominal component is Nd11Fe81.5Nb1Ga0.5B6The metal raw material is subjected to vacuum melting to obtain an alloy ingot, the alloy ingot is repeatedly melted for three times to ensure that the components of the alloy ingot are uniform, the melted alloy ingot is crushed and then subjected to vacuum melt spinning at the melt spinning speed of 30m/s to obtain Nd11Fe81.5Nb1Ga0.5B6An alloy thin strip;
(2) preparing a mixed thin strip: according to the atomic percentage, the Ce is prepared by vacuum melting7Cu3Alloying, preparing a sputtering target material with the diameter of 2 inches, and then adopting magnetron sputtering to prepare Ce7Cu3Alloy is plated on the Nd11Fe81.5Nb1Ga0.5B6On the alloy thin strip, controlling Ce by controlling sputtering time7Cu3In an amount such that about 10% by weight of the total weight of the ribbon is mixed to form a thin ribbon;
(3) preparation of NdCeFeB isotropic dense permanent magnet: the mixed ribbon was crushed into 80 mesh powder in a glove box, the obtained powder was charged into a mold, and hot pressing was performed by spark plasma sintering at a hot pressing temperature of 680 ℃ under a pressure of 150MPa for 3min to obtain an NdCeFeB isotropic dense permanent magnet, which was designated as sample 11, and the demagnetization curve of this sample was measured, and the result is shown in fig. 3.
Example 6, an NdCeFeB isotropic dense permanent magnet prepared by the following steps: this embodiment is different from embodiment 5 in that: the alloy prepared in the step (2) is Ce7Co3Prepared in this exampleThe NdCeFeB isotropic dense permanent magnet, designated as sample 12, was measured for demagnetization curve and the results are shown in fig. 3.
Comparative example 2, NdFeB isotropically dense permanent magnet was prepared as a blank control for samples 11 and 12, with Nd as a nominal component in atomic percent11Fe81.5Nb1Ga0.5B6The metal raw material is subjected to vacuum melting to obtain an alloy ingot, the alloy ingot is repeatedly melted for three times to ensure that the components of the alloy ingot are uniform, the melted alloy ingot is crushed and then subjected to vacuum melt spinning at the melt spinning speed of 30m/s to obtain Nd11Fe81.5Nb1Ga0.5B6An alloy thin strip prepared by forming the Nd11Fe81.5Nb1Ga0.5B6The alloy thin strip was crushed into 80 mesh powder in a glove box, the obtained powder was loaded into a mold, and hot pressing was performed by spark plasma sintering at 680 ℃ under 150MPa for 3min to obtain a reference 2, and the demagnetization curve of the reference 2 was measured, and the result is shown in FIG. 3.
As is clear from FIG. 3, in comparative example 2, since the cerium-copper alloy or the cerium-cobalt alloy was not added, the coercive force of the magnet was only about 9.1kOe, and the magnet density was 7.36g/cm3Compared with the reference product 1, the coercive force of the magnet is improved due to the addition of Nb and Ga elements; in sample 11, 10% Ce was added7Co3After the alloy is hot-pressed, the coercive force of the magnet is increased from 9.1kOe to 12.1kOe, and the density of the magnet is increased to 7.58g/cm3(ii) a In sample 12, 10% Ce was added7Cu3After the alloy is hot-pressed, the coercive force of the magnet is increased to 12.7kOe, and the density of the magnet is increased to 7.57g/cm3。
Example 7, an NdCeFeB isotropic dense permanent magnet prepared by the following steps:
(1) preparation of Nd12Fe81Nb1B6Alloy thin strip: according to atomic percentage, the nominal component is Nd12Fe81Nb1B6The metal raw material is subjected to vacuum melting to obtain an alloy ingot, the alloy ingot is repeatedly melted for three times to ensure that the components of the alloy ingot are uniform, and the melted alloy ingot is crushed and then subjected to vacuum meltingMelt-spinning at a speed of 30m/s to obtain Nd12Fe81Nb1B6An alloy thin strip;
(2) preparing a mixed thin strip: according to the atomic percentage, the Ce is prepared by vacuum melting7Cu3Alloying, preparing a sputtering target material with the diameter of 2 inches, and then adopting magnetron sputtering to prepare Ce7Cu3Alloy is plated on the Nd12Fe81Nb1B6On the alloy thin strip, controlling Ce by controlling sputtering time7Cu3In an amount such that about 10% by weight of the total weight of the ribbon is mixed to form a thin ribbon;
(3) preparation of NdCeFeB isotropic dense permanent magnet: the mixed ribbon was crushed into 80 mesh powder in a glove box, the obtained powder was charged into a mold, and hot pressing was performed by spark plasma sintering at a hot pressing temperature of 680 ℃ under a pressure of 150MPa for 3min to obtain an NdCeFeB isotropic dense permanent magnet, which was designated as sample 13, and the demagnetization curve of this sample was measured, and the result is shown in fig. 4.
Comparative example 3 preparation of NdFeB isotropically dense permanent magnet as blank control for sample 13, with Nd as a nominal component in atomic percent12Fe81Nb1B6The metal raw material is subjected to vacuum melting to obtain an alloy ingot, the alloy ingot is repeatedly melted for three times to ensure that the components of the alloy ingot are uniform, the melted alloy ingot is crushed and then subjected to vacuum melt spinning at the melt spinning speed of 30m/s to obtain Nd12Fe81Nb1B6An alloy thin strip prepared by forming the Nd12Fe81Nb1B6The alloy thin strip was crushed into 80 mesh powder in a glove box, the obtained powder was loaded into a mold, and hot pressing was performed by spark plasma sintering at 680 ℃ under 150MPa for 3min to obtain a reference 3, and the demagnetization curve of the reference 3 was measured, and the result is shown in FIG. 4.
As is clear from FIG. 4, when 10% of Ce was added, the amount of Ce was larger than that of control 37Cu3After the alloy is hot-pressed, the coercive force of the magnet is increased from 6.0kOe to 9.3kOe, and the density is increased from 7.41g/cm3Raising the temperature to 7.56g/cm3Analysis of samples 11-13 revealed that addition of the single agent was performedThe coercive force of the magnet can be better improved by adding Nb or Ga or simultaneously adding the Nb or Ga or the Ga; in addition, at the same time in Ndx(FeCo)94-x-y-zNbyGazB6Sputtering Ce on the alloy thin strip7Cu3Alloy and Ce7Co3The alloy can also improve the coercive force and density of the magnet obviously.
Finally, it should be noted that the above-mentioned description is only a preferred embodiment of the present invention, and those skilled in the art can make various similar representations without departing from the spirit and scope of the present invention.
Claims (7)
1. A preparation method of an NdCeFeB isotropic dense permanent magnet is characterized by comprising the following steps:
(1) preparing Nd according to atomic percentagex(FeCo)94-x-y-zNbyGazB6The preparation method comprises the following steps of preparing the Nd thin strip, wherein the value of x is 8-14, the value of y is 0-1, and the value of z is 0-0.5x(FeCo)94-x-y-zNbyGazB6Preparing metal raw materials according to atomic percentage, obtaining an alloy ingot by vacuum melting, repeatedly melting for three times to ensure that the components of the alloy ingot are uniform, crushing the melted alloy ingot, and then performing vacuum melt spinning;
(2) respectively preparing a copper-cerium alloy or a cerium-cobalt alloy, and respectively preparing the copper-cerium alloy or the cerium-cobalt alloy into sputtering targets;
(3) plating the sputtering target material on the Ndx(FeCo)94-x-y-zNbyGazB6Obtaining a mixed thin strip on the alloy thin strip;
(4) and crushing the mixed thin strip, and performing hot pressing treatment on the obtained powder to obtain the NdCeFeB isotropic compact permanent magnet, wherein the hot pressing temperature of the hot pressing treatment is 650-750 ℃, the pressure is 50-150MPa, and the heat preservation is performed for 3-10 min.
2. The method for preparing an NdCeFeB isotropic dense permanent magnet according to claim 1, wherein the method comprises the following steps: the ratio of cerium to copper in the copper-cerium alloy is 7:3 in terms of atomic percentage.
3. The method for preparing an NdCeFeB isotropic dense permanent magnet according to claim 1, wherein the method comprises the following steps: the ratio of cerium to cobalt in the cerium-cobalt alloy is 7:3 calculated by atomic percentage.
4. A method for producing an NdCeFeB isotropic dense permanent magnet according to claim 1, 2 or 3, characterized in that: the sputtering target material accounts for 10-30% of the total weight of the mixed thin strip by mass percentage.
5. The method for preparing an NdCeFeB isotropic dense permanent magnet according to claim 1, wherein the method comprises the following steps: when x is less than or equal to 12, the pressure of the hot pressing treatment is 150MPa, and when x is more than 12, the pressure of the hot pressing treatment is less than 150 MPa.
6. The method for preparing an NdCeFeB isotropic dense permanent magnet according to claim 1, wherein the method comprises the following steps: the hot pressing treatment method is spark plasma sintering.
7. An NdCeFeB isotropic dense permanent magnet, characterized in that: prepared by the preparation method of any one of claims 1-3 or 5-6.
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EP4156210A1 (en) * | 2021-09-24 | 2023-03-29 | Yantai Dongxing Magnetic Materials Inc. | A low-cost rare earth magnet and corresponding manufacturing method thereof |
JP2023047305A (en) * | 2021-09-24 | 2023-04-05 | 煙台東星磁性材料株式有限公司 | Nd-Fe-B MAGNETIC MATERIAL AND METHOD FOR MANUFACTURING THE SAME |
JP7325921B2 (en) | 2021-09-24 | 2023-08-15 | 煙台東星磁性材料株式有限公司 | Nd--Fe--B system magnetic material and its manufacturing method |
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