CN113223802B - High-temperature-resistant neodymium-iron-boron magnet and preparation method thereof - Google Patents
High-temperature-resistant neodymium-iron-boron magnet and preparation method thereof Download PDFInfo
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Abstract
The application relates to the technical field of neodymium iron boron magnets, in particular to a high-temperature-resistant neodymium iron boron magnet and a preparation method thereof. The high-temperature-resistant neodymium iron boron magnet is prepared from the following raw materials in parts by weight: 160-210 parts of praseodymium-neodymium alloy, 360-420 parts of iron, 20-40 parts of boron, 4-18 parts of a grain boundary alloy material, 1-6 parts of a first high-temperature resistant material and 2-8 parts of a second high-temperature resistant material, wherein the grain boundary alloy material is one or a combination of two of iron-cobalt-vanadium alloy and gadolinium-iron alloy. The preparation method of the high-temperature-resistant neodymium-iron-boron magnet comprises the following steps: (1) primary smelting; (2) re-smelting; (3) hydrogen crushing to prepare powder; (4) pressing and forming; (5) and (4) sintering and tempering. The high-temperature-resistant neodymium iron boron magnet and the preparation method thereof have the advantage of improving the high-temperature resistance of the neodymium iron boron magnet.
Description
Technical Field
The application relates to the technical field of neodymium iron boron magnets, in particular to a high-temperature-resistant neodymium iron boron magnet and a preparation method thereof.
Background
The neodymium-iron-boron magnet is a permanent magnet material with excellent magnetic property, is widely applied to the fields of electronics, electric machinery, medical instruments, toys, packaging, hardware machinery, aerospace and the like, and is commonly used as a permanent magnet motor, a loudspeaker, a magnetic separator, a computer disk driver, a magnetic resonance imaging equipment instrument and the like.
In the related art, the traditional neodymium iron boron magnet mainly comprises the following raw materials: 29-32 parts of rare earth metal neodymium, 64-69 parts of metal element iron and 1.1-1.2 parts of non-metal element boron, and the conventional sintering method of the neodymium-iron-boron magnet is to directly perform smelting, hydrogen breaking, pressing and sintering on the rare earth metal neodymium, the metal element iron and the non-metal element boron in sequence.
In view of the above-mentioned problems, the inventors believe that when the ndfeb magnet is used in a device, the temperature of the device due to long-term operation will continue to heat the ndfeb material, and the high temperature is very easy to demagnetize the ndfeb magnet, so that the high temperature resistance of the ndfeb magnet still needs to be improved.
Disclosure of Invention
In order to improve the high temperature resistance of the neodymium iron boron magnet, the application provides the high temperature resistant neodymium iron boron magnet and the preparation method thereof.
In a first aspect, the present application provides a high temperature resistant neodymium iron boron magnet, which adopts the following technical scheme:
a high-temperature resistant neodymium-iron-boron magnet is prepared from the following raw materials in parts by weight: 160-210 parts of praseodymium-neodymium alloy, 360-420 parts of iron, 20-40 parts of boron, 4-18 parts of a grain boundary alloy material, 1-6 parts of a first high-temperature resistant material and 2-8 parts of a second high-temperature resistant material, wherein the grain boundary alloy material is one or a combination of two of iron-cobalt-vanadium alloy and gadolinium-iron alloy.
Through adopting above-mentioned technical scheme, owing to adopt iron cobalt vanadium alloy and gadolinium ferroalloy as the grain boundary alloy material, and iron cobalt vanadium alloy and gadolinium ferroalloy have higher orientation degree for iron cobalt vanadium alloy and gadolinium ferroalloy improve the microstructure of high temperature resistant neodymium iron boron magnet, and then effectively reduce hole and loose degree in the microstructure of high temperature resistant magnet, and effectively improve the intrinsic coercive force of high temperature resistant neodymium iron boron magnet, consequently, obtain the high temperature resistance performance effect of improving neodymium iron boron magnet.
In addition, the Curie temperature of the high-temperature resistant magnet is relatively reduced due to the fact that the large amount of the grain boundary alloy material is added, and therefore the high-temperature resistant performance effect of the neodymium iron boron magnet can be indirectly improved in a mode that the grain boundary alloy material is added in a small amount.
Preferably, the grain boundary alloy material is prepared from the following raw materials in parts by weight: 2-9 parts of iron-cobalt-vanadium alloy and 2-9 parts of gadolinium-iron alloy.
Through adopting above-mentioned technical scheme, owing to adopt and carry out the mode of cooperative use with iron cobalt vanadium alloy and gadolinium ferroalloy for use iron cobalt vanadium alloy and gadolinium ferroalloy alone, to the promotion of high temperature resistant neodymium iron boron magnet's intrinsic coercive force and all optimize by a wide margin to curie temperature's reduction degree, further improve neodymium iron boron magnet's high temperature resistant performance effect.
Preferably, the first high-temperature-resistant powder is one or a combination of copper, aluminum and titanium.
By adopting the technical scheme, as the copper, the aluminum and the titanium are adopted as the first high-temperature-resistant powder, the copper, the aluminum and the titanium can improve the intrinsic coercive force of the high-temperature-resistant neodymium iron boron magnet, and further the high-temperature-resistant performance effect of the neodymium iron boron magnet is improved.
In addition, the Curie temperature of the high-temperature-resistant neodymium-iron-boron magnet is relatively reduced due to the addition of a large amount of copper, aluminum and titanium, so that the high-temperature-resistant performance effect of the neodymium-iron-boron magnet can be indirectly improved by adding a small amount of copper, aluminum and titanium.
Preferably, the first high-temperature resistant powder is prepared from the following raw materials in parts by weight: 0.1-0.3 part of copper, 0.5-3 parts of aluminum and 0.4-2.7 parts of titanium.
Through adopting above-mentioned technical scheme, can effectively improve the curie temperature reduction degree of high temperature resistant neodymium iron boron magnet when copper and aluminium carry out the cooperation use under above-mentioned proportion, indirectly improve the high temperature resistance performance effect of neodymium iron boron magnet.
When copper and aluminum are used in cooperation, coarse particles are usually formed at the intersection of grain boundaries, so that the increase of a peripheral stray field is promoted, the coercive force of the high-temperature-resistant neodymium-iron-boron magnet is weakened, and after titanium is added between copper and aluminum according to the proportion, the generation of the stray field and the coarse particles can be effectively reduced, and the high-temperature-resistant performance effect of the neodymium-iron-boron magnet is indirectly improved.
Preferably, the second high-temperature resistant material is one or a mixture of more of tantalum, dysprosium and zirconium.
By adopting the technical scheme, the temperature stability and the engineering temperature range of the high-temperature-resistant neodymium-iron-boron magnet can be effectively improved due to the tantalum, the dysprosium and the zirconium, and the high-temperature-resistant performance effect of the neodymium-iron-boron magnet is further effectively improved.
In addition, the tantalum, dysprosium and zirconium can also play a role in refining crystal grains and improving the exchange coupling field, so that the magnetic flux loss rate of the magnet caused by temperature rise is obviously reduced, the service temperature of the high-temperature-resistant neodymium iron boron magnet is further improved, and the high-temperature-resistant performance effect of the neodymium iron boron magnet is effectively improved.
Preferably, the second high-temperature resistant material is prepared from the following raw materials in parts by weight: 1-4 parts of dysprosium, 0.5-2 parts of tantalum and 0.5-2 parts of zirconium.
By adopting the technical scheme, because the magnetic distances of the dysprosium and the tantalum are arranged in an anti-parallel manner, the synergistic use of the dysprosium and the tantalum not only can effectively improve the coercive force and the temperature resistance of the high-temperature-resistant neodymium-iron-boron magnet, but also can slightly reduce the magnetic performance of the high-temperature-resistant neodymium-iron-boron magnet, and when the zirconium is added between the dysprosium and the tantalum in the proportion, the coercive force and the temperature resistance of the high-temperature-resistant neodymium-iron-boron magnet can be improved, and the magnetic performance reduction degree of the high-temperature-resistant neodymium-iron-boron magnet can be effectively improved.
Preferably, the mesh number of the praseodymium-neodymium alloy, the iron, the boron, the grain boundary alloy material, the first high temperature resistant material and the second high temperature resistant material is between 600-1000.
By adopting the technical scheme, because the mesh number of the praseodymium-neodymium alloy, iron, boron, the grain boundary alloy material, the first high-temperature resistant material and the second high-temperature resistant material is in the range, the stray field and coarse particles at the grain boundary intersection of the high-temperature resistant neodymium-iron-boron magnet are effectively reduced, the coercive force of the high-temperature resistant neodymium-iron-boron magnet is effectively improved, and the high-temperature resistant performance effect of the neodymium-iron-boron magnet is effectively improved.
In a second aspect, the application provides a method for preparing a high-temperature-resistant neodymium-iron-boron magnet, which adopts the following technical scheme: a preparation method of a high-temperature-resistant neodymium-iron-boron magnet comprises the following steps:
(1) carrying out vacuum melting on the praseodymium-neodymium alloy, iron and boron at the temperature of 800-plus-900 ℃ to obtain a neodymium-iron-boron magnet base material;
(2) carrying out vacuum melting on the crystal boundary alloy material, the first high-temperature-resistant material, the second high-temperature-resistant material and the neodymium iron boron magnet base material at the temperature of 1500-;
(3) hydrogen crushing the raw material of the high-temperature resistant neodymium iron boron magnet, and then finely grinding to obtain high-temperature resistant neodymium iron boron magnetic powder;
(4) pressing the high-temperature-resistant neodymium iron boron magnetic powder in a vacuum environment to obtain a high-temperature-resistant neodymium iron boron magnet rough blank;
(5) the method comprises the steps of firstly sintering the crude blank of the high-temperature resistant neodymium iron boron magnet in vacuum at the temperature of 1000-plus-one 1100 ℃ and preserving heat for 1-3h, then carrying out vacuum tempering at the temperature of 800-plus-one 900 ℃ and preserving heat for 1-3h, then carrying out vacuum tempering at the temperature of 400-plus-one 500 ℃ and preserving heat for 1-3h, and finally cooling to obtain the high-temperature resistant neodymium iron boron magnet.
Through adopting above-mentioned technical scheme, because in (1) and (2), at first with praseodymium-neodymium alloy, iron and boron carry out the primary smelting and obtain neodymium iron boron magnet base material, later to the grain boundary alloy material, first high temperature resistant material, second high temperature resistant material and neodymium iron boron magnet base material smelting, and then impel praseodymium-neodymium alloy, iron, boron, grain boundary alloy material, the distribution of first high temperature resistant material and second high temperature resistant material more even, and effectively reduce the stray field of high temperature resistant neodymium iron boron magnet grain boundary junction, effectively improve the coercive force of high temperature resistant neodymium iron boron magnet, and then effectively improve the high temperature resistance performance effect of neodymium iron boron magnet.
In addition, in the step (5), when the high-temperature resistant neodymium iron boron magnet is prepared, heat preservation operation is performed during sintering and tempering, so that connection of the praseodymium-neodymium alloy, iron, boron, the grain boundary alloy material, the first high-temperature resistant material and the second high-temperature resistant material is enabled to be more stable, stray fields at the grain boundary intersection of the high-temperature resistant neodymium iron boron magnet are reduced, the coercive force of the high-temperature resistant neodymium iron boron magnet is effectively improved, and the high-temperature resistant performance effect of the neodymium iron boron magnet is further effectively improved.
Preferably, in (1), the praseodymium-neodymium alloy, iron, boron, the grain boundary alloy material, the first high temperature resistant material, and the second high temperature resistant material are first subjected to an acidification and degreasing treatment.
By adopting the technical scheme, in the step (1), the praseodymium-neodymium alloy, the iron, the boron, the crystal boundary alloy material, the first high-temperature-resistant material and the second high-temperature-resistant material are firstly acidified and deoiled, so that the influence of impurities on the raw materials is reduced, the coercive force and the service temperature of the high-temperature-resistant neodymium-iron-boron magnet are indirectly improved, and the high-temperature-resistant performance effect of the neodymium-iron-boron magnet is effectively improved.
In summary, the present application has the following beneficial effects:
1. because this application adopts iron cobalt vanadium alloy and gadolinium ferroalloy as the grain boundary alloy material for iron cobalt vanadium alloy improves the microstructure of high temperature resistant neodymium iron boron magnet with gadolinium ferroalloy, consequently, obtains the high temperature resistance performance effect that improves the neodymium iron boron magnet.
2. Preferentially adopt iron cobalt vanadium alloy and gadolinium ferroalloy to carry out the mode of cooperative use in this application for promotion of iron cobalt vanadium alloy and gadolinium ferroalloy to the intrinsic coercive force of high temperature resistant neodymium iron boron magnet and the degree of cutting down to curie temperature all optimize by a wide margin, obtained the high temperature resistant performance effect of further improvement neodymium iron boron magnet.
3. According to the method, the NdFeB magnet base material is obtained by primarily smelting the praseodymium-neodymium alloy, the iron and the boron, and then the crystal boundary alloy material, the first high-temperature-resistant material, the second high-temperature-resistant material and the NdFeB magnet base material are smelted, so that stray fields at the crystal boundary intersection of the high-temperature-resistant NdFeB magnet are effectively reduced, and the effect of improving the high-temperature resistance of the NdFeB magnet is obtained.
Drawings
Fig. 1 is a flowchart of a method for manufacturing a high temperature resistant ndfeb magnet provided herein.
Detailed Description
The present application will be described in further detail with reference to examples and comparative examples.
The neutralized feed components in this application are shown in table 1:
TABLE 1 sources of the raw material components
| Raw materials | Manufacturer of the product | Specification of |
| Praseodymium-neodymium alloy | GANZHOU JIATON TECHNOLOGY GROUP Co.,Ltd. | CAS：1314-36-9 |
| Iron | Shanghai barge science and technology Limited | CAS：7439-89-6 |
| Boron | Beijing Happy-minded Biotechnology Ltd | CAS：7440-42-8 |
| Iron-cobalt-vanadium alloy | Jiu Ming Special Steel Co, Jiangsu | Number 1J22(Co50V2) |
| Gadolinium-iron alloy | Ganzhou city Jiangjiang mining Co Ltd | XB/T403-2012 |
| Copper (Cu) | Shandong Bairui New materials Co Ltd | CAS：7440-50-8 |
| Aluminium | Longyuan county Mingyu aluminum industry Co., Ltd | CAS：7429-90-5 |
| Titanium (IV) | Xian Site Industrial and trade company Limited | CAS：7440-32-6 |
| Tantalum | NINGXIA ORIENT TANTALUM INDUSTRY Co.,Ltd. | CAS：7440-25-7 |
| Dysprosium | Sigma Aldrich trade, Inc | CAS：14692-17-2 |
| Zirconium | Beijing October New materials science and technology Co., Ltd | CAS：7440-67-7 |
Examples
Example 1
A high-temperature resistant neodymium iron boron magnet is prepared by the following steps:
(1) 188g of praseodymium-neodymium alloy, 391g of iron and 30.5g of boron are added into a vacuum induction rapid hardening furnace, and then vacuum smelting is carried out for 1h at the temperature of 850 ℃ to obtain a neodymium-iron-boron magnet base material;
(2) adding 8g of gadolinium-iron alloy, 3.5g of copper, 5g of dysprosium and neodymium-iron-boron magnet base material into a vacuum induction rapid hardening furnace, and then carrying out vacuum melting for 1h at the temperature of 1750 ℃ to obtain a high-temperature-resistant neodymium-iron-boron magnet raw material;
(3) carrying out fine grinding on the raw material of the high-temperature resistant neodymium iron boron magnet through a hydrogen crushing furnace and an airflow mill, and then obtaining high-temperature resistant neodymium iron boron magnetic powder with the mesh number of 800 meshes;
(4) pressing the high-temperature-resistant neodymium iron boron magnetic powder in a vacuum environment by using a magnetic field press to obtain a high-temperature-resistant neodymium iron boron magnet rough blank; (5) placing the high-temperature-resistant neodymium iron boron magnet rough blank in a vacuum sintering furnace, then carrying out vacuum sintering at 1050 ℃ and carrying out heat preservation for 2h, then carrying out vacuum tempering at 850 ℃ and carrying out heat preservation for 2h, then carrying out vacuum tempering at 450 ℃ and carrying out heat preservation for 2h, and finally cooling to room temperature to obtain the high-temperature-resistant neodymium iron boron magnet.
Examples 2 to 3
The difference from example 1 is that the weight of each component of the raw materials of examples 2-3 is different, as shown in Table 2.
TABLE 2 compositions and weights (g) of the respective raw materials in examples 1 to 3
| Composition of raw materials | Example 1 | Example 2 | Example 3 |
| Praseodymium-neodymium alloy | 188 | 210 | 160 |
| Iron | 391 | 360 | 420 |
| Boron | 30.5 | 20 | 40 |
| Gadolinium-iron alloy | 8 | 18 | 4 |
| Copper (Cu) | 3.5 | 1 | 6 |
| Dysprosium | 5 | 8 | 2 |
Example 4
The difference from example 1 is that the weight of the gadolinium-iron alloy is 18 g.
Example 5
The difference from example 1 is that the weight of the gadolinium-iron alloy is 4 g.
Example 6
The difference from example 1 is that the gadolinium-iron alloy is replaced by an equivalent amount of iron-cobalt-vanadium alloy.
Example 7
The difference from example 1 is that the gadolinium ferroalloy is replaced by a composition of equal amounts of iron cobalt vanadium alloy and gadolinium ferroalloy and the ratio of iron cobalt vanadium alloy to gadolinium ferroalloy is 1: 1.
Example 8
The difference from example 1 is that the gadolinium ferroalloy is replaced by a composition of equal amounts of iron cobalt vanadium alloy and gadolinium ferroalloy and the ratio of iron cobalt vanadium alloy to gadolinium ferroalloy is 1: 2.
Example 9
The difference from example 1 is that the gadolinium ferroalloy is replaced by an equal composition of iron cobalt vanadium alloy and gadolinium ferroalloy and the ratio of iron cobalt vanadium alloy to gadolinium ferroalloy is 2: 1.
Example 10
The difference from example 1 is that the weight of copper is 6 g.
Example 11
The difference from example 1 is that the weight of copper is 1 g.
Example 12
The difference from example 1 is that copper is replaced with an equal amount of aluminum.
Example 13
The difference from example 1 is that copper is replaced with an equal amount of titanium.
Example 14
The difference from example 1 is that copper was replaced with an equal amount of a combination of copper and titanium, and the ratio of copper to titanium was 1: 10.
Example 15
The difference from example 1 is that copper was replaced with an equal amount of copper to aluminum composition and the ratio of copper to aluminum was 1: 10.
Example 16
The difference from example 1 is that copper was replaced with an equal amount of copper to aluminum composition and the ratio of copper to aluminum was 1: 5.
Example 17
The difference from example 1 is that copper was replaced with an equal amount of copper to aluminum composition and the ratio of copper to aluminum was 1: 15.
Example 18
The difference from example 1 is that copper was replaced with a composition of equal amounts of copper, aluminum and titanium, and the ratio of copper, aluminum and titanium was 1:5: 5.
Example 19
The difference from example 1 is that copper was replaced with a composition of equal amounts of copper, aluminum and titanium, and the ratio of copper, aluminum and titanium was 1:3: 7.
Example 20
The difference from example 1 is that copper was replaced with a composition of equal amounts of copper, aluminum and titanium, and the ratio of copper, aluminum and titanium was 1:7: 3.
Example 21
The difference from example 1 was that the weight of dysprosium was 2 g.
Example 22
The difference from example 1 was that the weight of dysprosium was 8 g.
Example 23
The difference from example 1 is that dysprosium is replaced with an equal amount of tantalum.
Example 24
The difference from example 1 is that dysprosium is replaced with an equal amount of zirconium.
Example 25
The difference from example 1 was that dysprosium was replaced with a composition of equal amounts of dysprosium and zirconium, and the ratio of dysprosium to zirconium was 1: 1.
Example 26
The difference from example 1 is that dysprosium is replaced with an equal amount of a composition of dysprosium and tantalum, and the ratio of dysprosium to tantalum is 1: 1.
Example 27
The difference from example 1 is that dysprosium is replaced with an equal amount of a composition of dysprosium and tantalum, and the ratio of dysprosium to tantalum is 1: 2.
Example 28
The difference from example 1 is that dysprosium is replaced with an equal amount of a composition of dysprosium and tantalum, and the ratio of dysprosium to tantalum is 2: 1.
Example 29
The difference from example 1 is that dysprosium is replaced with a composition of equal amounts of dysprosium, tantalum and zirconium, and the ratio of dysprosium, tantalum and zirconium is 2:1: 1.
Example 30
The difference from example 1 was that dysprosium was replaced with a composition of equal amounts of dysprosium, tantalum and zirconium, and the ratio of dysprosium, tantalum and zirconium was 4:1: 3.
Example 31
The difference from example 1 is that dysprosium is replaced with a composition of equal amounts of dysprosium, tantalum and zirconium, and the ratio of dysprosium, tantalum and zirconium is 4:3: 1.
Example 32
The difference from the embodiment 1 is that, in (3), the mesh number of the high temperature resistant neodymium iron boron magnetic powder is 600 meshes.
Example 33
The difference from the embodiment 1 is that, in (3), the mesh number of the high temperature resistant neodymium iron boron magnetic powder is 1000 meshes.
Example 34
The difference from the example 1 is that the praseodymium-neodymium alloy, the iron, the boron, the gadolinium-iron alloy, the copper and the dysprosium are directly added into a vacuum induction rapid hardening furnace and vacuum melting is carried out for 1h at the temperature of 1750 ℃.
Example 35
The difference from example 1 is that in (1), the praseodymium-neodymium alloy, iron, boron, gadolinium-iron alloy, copper and dysprosium are first pickled in 98% concentrated sulfuric acid and then degreased in dodecylbenzene.
Example 36
The difference from example 1 is that in (5), the heat-retaining operation was not performed.
Comparative example
Comparative example 1
The difference from example 1 is that comparative example 1 is the ndfeb magnet and the preparation method thereof described in the background art.
Comparative example 2
The difference from example 1 is that gadolinium-iron alloy is not included.
Comparative example 3
The difference from example 1 is that copper is not included.
Comparative example 4
The difference from example 1 is that dysprosium is not included.
Performance test
Test method
Three samples were taken from examples 1 to 36 and comparative examples 1 to 4, respectively, and then the following tests were performed at 20 ℃ and averaged.
First, magnetic Property test
The samples are detected by a magnetic test method in GB/T3217 permanent magnet (hard magnetic) material, and then intrinsic coercive force, maximum magnetic energy product and Curie temperature are obtained.
Test two, maximum operating temperature test
And (3) detecting the sample at the highest working temperature in GB/T13560-2017 sintered NdFeB permanent magnet materials, and then obtaining the highest working temperature.
And (3) detection results: the results of the tests of examples 1 to 36 and comparative examples 1 to 4 are shown in Table 3.
TABLE 3 test results of examples 1 to 36 and comparative examples 1 to 4
Combining examples 1-3 and comparative example 1 and combining table 3, it can be seen that, although the curie temperature of examples 1-3 is reduced compared to comparative example 1, the intrinsic coercivity, the maximum magnetic energy product and the maximum working temperature of examples 1-3 are all significantly increased, thereby demonstrating that the high temperature resistance of the high temperature resistant ndfeb magnet can be effectively improved by the raw materials of the high temperature resistant ndfeb magnet within the ratio range of examples 1-3.
Combining example 1, examples 4-5, and comparative example 2 with table 3, it can be seen that, although the curie temperature of example 4 is reduced compared to example 1, the intrinsic coercivity, the maximum magnetic energy product, and the maximum operating temperature of example 4 are all improved; although the curie temperature of example 5 was raised, the intrinsic coercivity, the maximum magnetic energy product, and the maximum operating temperature of example 5 were all lowered, while the curie temperature of comparative example 2 was further raised, and the intrinsic coercivity, the maximum magnetic energy product, and the maximum operating temperature of comparative example 2 were all further lowered.
Therefore, the gadolinium-iron alloy has the effects of improving the intrinsic coercive force and the maximum magnetic energy product of the high-temperature resistant neodymium-iron magnet, but the gadolinium-iron alloy also has the effect of reducing the curie temperature of the high-temperature resistant neodymium-iron-boron magnet, but relatively speaking, the gadolinium-iron alloy has the promotion effect on the high-temperature resistance of the high-temperature resistant neodymium-iron-boron magnet. And along with the increase of the amount of the gadolinium ferroalloy, the lifting effect gradually rises, but when the amount of the gadolinium ferroalloy is greater than that of the embodiment 1, the lifting effect gradually falls, so that the lifting effect of the gadolinium ferroalloy to the neodymium iron boron magnet is relatively excellent under the specific gravity of the embodiment 1.
Referring to example 1, example 6 and comparative example 1, and combining table 3, it can be seen that, compared to comparative example 1 and example 1, example 6 also has a certain promotion effect on the intrinsic coercivity, the maximum magnetic energy product and the maximum working temperature of the high temperature resistant ndfeb magnet, but the promotion effect is relatively poor compared with the gadolinium-iron alloy; in addition, example 6 also has certain weakening effect to the curie temperature of the high temperature resistant ndfeb magnet, but the weakening effect is lower, which shows that the fe-co-v alloy also has certain improvement effect to the high temperature resistant performance of the ndfeb magnet.
Referring to example 1, examples 7-9 and Table 3, it can be seen that the intrinsic coercivity and the maximum energy product of examples 7-9 are somewhat reduced, the Curie temperature and the maximum operating temperature of examples 7-9 are improved, and the improvement effect of example 7 is the best, compared to example 1.
Therefore, the synergistic use of the iron-cobalt-vanadium alloy and the gadolinium-iron alloy has the effect of improving the high-temperature resistance of the high-temperature-resistant neodymium-iron-boron magnet, and when the ratio of the iron-cobalt-vanadium alloy to the gadolinium-iron alloy is 1:1, the improvement effect is best.
Combining example 1, examples 10-11, and comparative example 3, and combining table 3, it can be seen that, although the curie temperature of example 10 is reduced compared to example 1, the intrinsic coercivity, the maximum magnetic energy product, and the maximum operating temperature of example 10 are all improved; although the curie temperature of example 11 was raised, the intrinsic coercivity, the maximum magnetic energy product, and the maximum operating temperature of example 11 were all lowered, while the curie temperature of comparative example 3 was further raised, and the intrinsic coercivity, the maximum magnetic energy product, and the maximum operating temperature of comparative example 3 were all further lowered.
Therefore, although copper has an effect of increasing the intrinsic coercivity and the maximum energy product of the high-temperature-resistant neodymium iron magnet, copper also has an effect of decreasing the curie temperature of the high-temperature-resistant neodymium iron boron magnet, relatively speaking, copper has an effect of promoting the high-temperature resistance of the high-temperature-resistant neodymium iron boron magnet. And the lifting effect gradually rises with the increase of the amount of copper, but when the amount of copper is greater than that of embodiment 1, the lifting effect gradually falls, so that the lifting effect of copper on the neodymium iron boron magnet is relatively excellent under the specific gravity of embodiment 1.
Referring to example 1, examples 12 to 13 and comparative example 1, and combining table 3, it can be seen that examples 12 to 13 also have a certain improvement effect on the intrinsic coercivity and the maximum magnetic energy product of the high temperature resistant ndfeb magnet, compared to comparative example 1 and example 1, but the improvement effect is poorer compared to copper; in addition, the curie temperature of the high-temperature resistant ndfeb magnet in example 11 is also weakened to a certain extent, but the weakening effect is almost zero, even equivalent to that in comparative example 1, while the curie temperature of the high-temperature resistant ndfeb magnet in example 12 is even improved to a certain extent, but overall, the high-temperature resistance of the ndfeb magnet is also improved by aluminum and titanium, and the improvement effect is slightly better than that of copper.
Referring to example 1 and examples 14-20 in combination with Table 3, it can be seen that the intrinsic coercivity and the maximum energy product of examples 14-20 are somewhat reduced, the Curie temperature and the maximum operating temperature of examples 14-20 are greatly increased, and the improvement effect of example 18 is the best, compared to example 1.
Therefore, the synergistic use of copper, aluminum and titanium has the effect of improving the high-temperature resistance of the high-temperature resistant neodymium-iron-boron magnet, and the improvement effect is best when the ratio of copper, aluminum and titanium is 1:5: 5.
Combining example 1, examples 21-22, and comparative example 4, and combining table 3, it can be seen that, although the curie temperature and intrinsic coercivity of example 21 are reduced, the maximum energy product of example 21 is reduced relative to example 1; while the curie temperature and intrinsic coercivity of example 22 were improved, the maximum magnetic energy product of example 22 was decreased, while the curie temperature and intrinsic coercivity of comparative example 4 were further decreased, and the maximum magnetic energy product of comparative example 4 was further increased.
Thus, although dysprosium has an effect of improving the intrinsic coercivity and the curie temperature of the high-temperature-resistant neodymium-iron magnet, dysprosium also has an effect of reducing the maximum energy product of the high-temperature-resistant neodymium-iron-boron magnet, and relatively speaking, dysprosium has an effect of promoting the high-temperature resistance of the high-temperature-resistant neodymium-iron-boron magnet. And the lifting effect gradually increases with the increase of the amount of dysprosium, but the lifting effect gradually decreases when the amount of dysprosium is greater than that of example 1, so that the lifting effect of dysprosium on the neodymium iron boron magnet is relatively excellent under the specific gravity of example 1.
Referring to example 1, examples 23 to 24 and comparative example 1, and combining table 3, it can be seen that, compared to comparative example 1 and example 1, examples 23 to 24 have substantially the same effect on the high temperature resistant ndfeb magnet as example 1, and therefore, tantalum and zirconium also have a certain improvement effect on the high temperature resistance of the ndfeb magnet, and the improvement effect is slightly better than that of copper.
Referring to example 1 and examples 25 to 31 in combination with table 3, it can be seen that, compared to example 1, examples 25 to 31 have greatly improved maximum operating temperature of the high temperature resistant ndfeb magnet, and example 29 has the best improvement effect.
Therefore, the synergistic use of dysprosium, tantalum and zirconium has the effect of improving the high-temperature resistance of the high-temperature-resistant neodymium-iron-boron magnet, and the improvement effect is best when the ratio of dysprosium, tantalum and zirconium is 2:1: 1.
As can be seen from the combination of example 1, examples 32 to 33, and table 3, the maximum operating temperatures of examples 32 to 33 are all decreased compared to example 1, which shows that, when the mesh number of the high temperature ndfeb magnetic powder is 800, the effect of improving the high temperature resistance of the high temperature ndfeb is the best.
It can be seen from the combination of example 1 and examples 34 to 36 and the combination of table 3 that the maximum operating temperatures of examples 34 to 36 are all reduced compared to example 1, which shows that the respective melting, pickling, degreasing and heat-preserving operations all have certain improvement effects on the high-temperature resistance of the high-temperature ndfeb magnet.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (4)
1. The high-temperature-resistant neodymium-iron-boron magnet is characterized by being prepared from the following raw materials in parts by weight: 160-210 parts of praseodymium-neodymium alloy, 360-420 parts of iron, 20-40 parts of boron, 4-18 parts of grain boundary alloy material, 1-6 parts of first high-temperature resistant material and 2-8 parts of second high-temperature resistant material; the grain boundary alloy material is prepared from the following raw materials in parts by weight: 2-9 parts of iron-cobalt-vanadium alloy and 2-9 parts of gadolinium-iron alloy; the first high-temperature-resistant powder is prepared from the following raw materials in parts by weight: 0.1-0.3 part of copper, 0.5-3 parts of aluminum and 0.4-2.7 parts of titanium; the second high-temperature-resistant material is prepared from the following raw materials in parts by weight: 1-4 parts of dysprosium, 0.5-2 parts of tantalum and 0.5-2 parts of zirconium.
2. The high temperature resistant neodymium iron boron magnet of claim 1, characterized in that: the mesh number of the praseodymium-neodymium alloy, the iron, the boron, the grain boundary alloy material, the first high-temperature resistant material and the second high-temperature resistant material is between 600 and 1000.
3. The method for preparing the high-temperature-resistant neodymium-iron-boron magnet according to any one of claims 1 to 2, characterized by comprising the following steps:
(1) carrying out vacuum melting on the praseodymium-neodymium alloy, iron and boron at the temperature of 800-plus-900 ℃ to obtain a neodymium-iron-boron magnet base material;
(2) carrying out vacuum melting on the crystal boundary alloy material, the first high-temperature-resistant material, the second high-temperature-resistant material and the neodymium iron boron magnet base material at the temperature of 1500-;
(3) hydrogen crushing the raw material of the high-temperature resistant neodymium iron boron magnet, and then finely grinding to obtain high-temperature resistant neodymium iron boron magnetic powder;
(4) pressing the high-temperature-resistant neodymium iron boron magnetic powder in a vacuum environment to obtain a high-temperature-resistant neodymium iron boron magnet rough blank;
(5) the method comprises the steps of firstly sintering the crude blank of the high-temperature resistant neodymium iron boron magnet in vacuum at the temperature of 1000-plus-one 1100 ℃ and preserving heat for 1-3h, then carrying out vacuum tempering at the temperature of 800-plus-one 900 ℃ and preserving heat for 1-3h, then carrying out vacuum tempering at the temperature of 400-plus-one 500 ℃ and preserving heat for 1-3h, and finally cooling to obtain the high-temperature resistant neodymium iron boron magnet.
4. The method for preparing the high-temperature-resistant neodymium-iron-boron magnet according to claim 3, characterized by comprising the following steps: (1) firstly, carrying out acidification and degreasing treatment on praseodymium-neodymium alloy, iron, boron, a grain boundary alloy material, a first high-temperature resistant material and a second high-temperature resistant material.
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| CN101236815A (en) * | 2007-12-07 | 2008-08-06 | 烟台正海磁性材料有限公司 | A high-temperature resisting R-Fe-B agglomeration permanent magnetic material and its making method |
| CN110335733A (en) * | 2019-06-05 | 2019-10-15 | 宁波合力磁材技术有限公司 | A kind of neodymium iron boron magnetic body resistant to high temperature and preparation method thereof |
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| CN101236815A (en) * | 2007-12-07 | 2008-08-06 | 烟台正海磁性材料有限公司 | A high-temperature resisting R-Fe-B agglomeration permanent magnetic material and its making method |
| CN110335733A (en) * | 2019-06-05 | 2019-10-15 | 宁波合力磁材技术有限公司 | A kind of neodymium iron boron magnetic body resistant to high temperature and preparation method thereof |
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