CN107134338B - Neodymium-iron-boron bonded magnetic powder compositely added with zinc and gadolinium and preparation method thereof - Google Patents
Neodymium-iron-boron bonded magnetic powder compositely added with zinc and gadolinium and preparation method thereof Download PDFInfo
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- 239000006247 magnetic powder Substances 0.000 title claims abstract description 75
- 239000011701 zinc Substances 0.000 title claims abstract description 48
- 229910052688 Gadolinium Inorganic materials 0.000 title claims abstract description 38
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 229910001172 neodymium magnet Inorganic materials 0.000 title claims abstract description 36
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 229910052725 zinc Inorganic materials 0.000 title claims abstract description 35
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical group [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000002131 composite material Substances 0.000 claims abstract description 10
- 229910052751 metal Inorganic materials 0.000 claims description 36
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 34
- 238000002425 crystallisation Methods 0.000 claims description 30
- 230000008025 crystallization Effects 0.000 claims description 30
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 28
- 229910045601 alloy Inorganic materials 0.000 claims description 26
- 239000000956 alloy Substances 0.000 claims description 26
- 239000002184 metal Substances 0.000 claims description 26
- 238000010791 quenching Methods 0.000 claims description 22
- 230000000171 quenching effect Effects 0.000 claims description 22
- 238000002844 melting Methods 0.000 claims description 19
- 230000008018 melting Effects 0.000 claims description 19
- 229910052786 argon Inorganic materials 0.000 claims description 14
- 239000002994 raw material Substances 0.000 claims description 13
- 229910052779 Neodymium Inorganic materials 0.000 claims description 8
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 claims description 8
- 238000003723 Smelting Methods 0.000 claims description 7
- 230000006698 induction Effects 0.000 claims description 7
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 6
- 229910052796 boron Inorganic materials 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 238000011049 filling Methods 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 5
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 13
- 238000012545 processing Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 34
- 230000005291 magnetic effect Effects 0.000 description 14
- 230000007797 corrosion Effects 0.000 description 8
- 238000005260 corrosion Methods 0.000 description 8
- 238000000227 grinding Methods 0.000 description 5
- 239000000696 magnetic material Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 230000006399 behavior Effects 0.000 description 3
- 230000002195 synergetic effect Effects 0.000 description 3
- 229910000583 Nd alloy Inorganic materials 0.000 description 2
- RKLPWYXSIBFAJB-UHFFFAOYSA-N [Nd].[Pr] Chemical compound [Nd].[Pr] RKLPWYXSIBFAJB-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 230000002411 adverse Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000003822 epoxy resin Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 229920000647 polyepoxide Polymers 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 1
- 230000001808 coupling effect Effects 0.000 description 1
- 230000005347 demagnetization Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000005293 ferrimagnetic effect Effects 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
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- 150000002739 metals Chemical class 0.000 description 1
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- 238000012986 modification Methods 0.000 description 1
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- 150000002910 rare earth metals Chemical class 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000009044 synergistic interaction Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
- H01F1/0571—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
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- B22F1/0003—
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/142—Thermal or thermo-mechanical treatment
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
- H01F1/0571—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
- 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 relates to the technical field of permanent magnet material processing, in particular to neodymium iron boron bonded magnetic powder added with zinc and gadolinium in a composite mode and a preparation method thereof.
Description
Technical Field
The invention relates to the technical field of permanent magnet material processing, in particular to neodymium iron boron bonded magnetic powder with composite added zinc and gadolinium and a preparation method thereof.
Background
The Nd-Fe-B permanent magnetic material has been widely researched and paid attention to due to its high magnetic energy and coercive force, and has been widely applied in the fields of electronics, electric power, machinery, medical apparatus and the like, but due to its hard magnetic phase Nd2Fe14The Curie temperature of B is low, and the temperature coefficient of remanence and the temperature coefficient of coercive force are high, so that the application of B in certain fields with high working temperature is limited.
Theories and practices show that the magnetic property of the product can be improved by adding certain alloy elements, and the temperature characteristic of the neodymium-iron-boron permanent magnetic material can be obviously improved, so that the use temperature of the neodymium-iron-boron permanent magnetic material is improved. However, because different metal elements have different crystallization behaviors, the influence and mechanism on the ndfeb permanent magnet material are also different, the improvement on the comprehensive performance of the ndfeb permanent magnet material is usually realized by the composite addition of multiple metal elements, and the addition of the metal elements has a decisive effect on the performance modification of the ndfeb permanent magnet material, if the addition is not properly selected, the adverse effect is even caused, so how to select the proper metal elements, and select the proper addition, the low-cost Curie temperature of the ndfeb is improved, the heat resistance and the comprehensive magnetic performance of the ndfeb permanent magnet material are improved, and the technical problem which needs to be solved at present is solved urgently.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide the neodymium iron boron bonded magnetic powder added with zinc and gadolinium compositely, which takes a neodymium iron boron permanent magnet as a main body and is doped with metal elements such as gadolinium and zinc, reduces the cost, improves the heat resistance and the corrosion resistance of the bonded magnetic powder and has excellent comprehensive performance.
Meanwhile, the invention also provides a preparation method of the neodymium iron boron bonded magnetic powder compounded with the zinc and the gadolinium.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a composite neodymium iron boron bonded magnetic powder added with zinc and gadolinium comprises the following elements in percentage by weight: 10-11% of Nd, 1.0-2.6% of GdB, 6-7% of B, 0.2-0.5% of Zn, and the balance of Fe.
Preferably, the neodymium iron boron bonded magnetic powder with zinc and gadolinium added compositely comprises the following elements in percentage by weight: 10.5% of Nd, 2% of Gd, 6% of B, 0.5% of Zn and the balance of Fe.
Optionally, the Nd element source is pure neodymium metal with a purity of more than 99.0% or a praseodymium-neodymium alloy with a neodymium content of more than 80%; the Fe element source is industrial pure iron with 99.8 percent of content and ferroboron alloy with boron content more than 19 percent; the source of the B element is ferroboron containing more than 19 percent of boron; the Gd element is sourced from metal gadolinium with the purity of more than 99 percent; the Zn element source is metal zinc with the purity of more than 99 percent.
The preparation method of the neodymium iron boron bonded magnetic powder added with zinc and gadolinium comprises the following operation steps:
1) taking raw materials according to the weight percentage of each element, adding the raw materials into a vacuum melting furnace, and controlling the melting temperature to be less than 4 × 10-2Smelting into an alloy ingot under the vacuum state of Pa;
2) crushing the alloy ingot smelted in the step 1), adding the crushed alloy ingot into a vacuum induction quick quenching furnace, wherein the vacuum degree reaches 5 × 10-2Filling argon after Pa, melting an alloy ingot crushed at 1450-1500 ℃ in an argon environment into molten metal, controlling the rapid quenching speed to be 25-33 m/s, and rapidly quenching the molten metal into uniform strips with the thickness of 50 +/-5 mu m;
3) crushing the uniform strips prepared in the step 2) into magnetic powder of 40 meshes;
4) magnetic powder prepared in the step 3)4.5 to 5.5 × 10-2And (3) carrying out crystallization treatment under the vacuum degree of Pa and the temperature of 600-700 ℃ and at the rotating speed of 20 r/s and the blanking speed of 20-25 kg/h of the crystallization furnace, thus completing the crystallization treatment.
Optionally, the step 4) further includes filling argon gas into the crystallization furnace, and then adding the magnetic powder prepared in the step 3) into the crystallization furnace for crystallization.
According to the composite zinc and gadolinium added neodymium iron boron bonded magnetic powder, zinc and gadolinium are doped into a neodymium iron boron permanent magnet material, so that the cost is reduced, the corrosion resistance, the residual magnetic induction strength, the intrinsic coercive force and the Curie temperature of the magnetic powder are improved, and the bonded magnetic powder has good heat resistance and is specifically embodied as follows:
gadolinium is used as a heavy rare earth element, the atomic magnetic moment of gadolinium is coupled with the 3d metal atomic magnetic moment in a ferrimagnetic manner, gadolinium is doped into a neodymium iron boron magnetic material, on one hand, the neodymium iron boron bonded magnet prepared by adding the gadolinium element has higher orientation degree, the defects of gaps, looseness and the like in the microstructure of the magnet are reduced, neodymium-rich phase is uniformly distributed, and gadolinium enters the neodymium-rich phase to form Gd2Fe14B is favorable for improving the chemical stability of the material, and the Curie temperature point of the material is 660K, the anisotropy field Ha is 1910KAm, and the Curie temperature point is higher than Nd2Fe14The temperature point B can improve the heat resistance and the coercive force of the magnet, effectively improve the corrosion resistance of the magnet and increase the intrinsic coercive force and the square degree of a demagnetization curve of the magnet; on the other hand, the gadolinium is added to partially replace the position of neodymium in the crystal phase, so that the production cost of the product can be greatly reduced, and the comprehensive utilization of rare earth resources is promoted;
incorporation of zinc, the zinc being able to enter Nd on the one hand2Fe14The lattice of the B phase occupies the position of Fe atoms, so that the actual Nd content in the alloy is increased, and meanwhile, the NdFeB alloy with the lower than normal component mainly consists of Nd due to the inhibition of α -Fe precipitation by zinc2Fe14B single phase composition, can completely suppress Nd3Fe62B14The generation of metastable phase, the amorphous crystallization process is changed from two-step crystallization to one-step crystallization, thus realizing heterogeneous and isothermal crystallization and remarkably improving the magnetic performance of the rapidly quenched NdFeB magnetic powder; on the other hand, zinc forms one on the surface at normal temperatureA protective film is formed to improve corrosion resistance;
therefore, the compound addition of zinc and gadolinium can reduce the temperature coefficient of the magnet, improve the crystallization temperature of α -Fe, simultaneously separate α -Fe and Nd2Fe14B during the crystallization of the rapidly quenched NdFeB alloy, avoid the first separation and growth of α -Fe, refine grains, enhance the exchange coupling effect among the grains, increase effective pinning positions, effectively improve the Hcj and Hk of the bonded magnetic powder, and improve the corrosion resistance of the prepared bonded magnetic powder by the synergistic effect of zinc and gadolinium and the internal and external combination.
In addition, it is known that when the performance of the neodymium iron boron permanent magnet material is improved by doping metal elements, the content of the doped metal elements has a decisive effect on the improvement of the performance, even if the amount is improperly selected, the adverse effect can be achieved, however, when the types of the doped metal are two or more, the influence of different metal elements on the crystallization behavior of the neodymium iron boron permanent magnet material is different, and the mutual restriction or synergistic effect also exists between the different metal elements, when two or more different metals are doped, the interaction between the different metal elements needs to be considered, and since the prior art does not exist that when the gadolinium and the zinc are combined and doped into the neodymium iron boron permanent magnet material, the selection of the doping amount should follow any principle and law, the weight percentage content of each metal element is defined in the invention, the magnetic powder can well exert synergistic effect, the cost is reduced, simultaneously, the high temperature resistance and various magnetic properties of the bonded magnetic powder are improved, the corrosion resistance of the bonded magnetic powder is improved, and creative labor is inevitably needed.
The crystallization behavior of the raw material can be influenced by the parameter control of the melting temperature, the vacuum degree, the rapid quenching speed, the crystallization treatment temperature, the vacuum degree and the like of the metal raw material in the preparation process of the bonded magnetic powder, further influencing the microstructure such as grain size of the prepared magnetic powder and finally influencing the magnetic properties such as coercive force of the magnetic powder, so that the preparation method of the bonded magnetic powder, according to the performance characteristics of the raw materials, a proper smelting vacuum environment and smelting temperature are selected, a vacuum induction quick quenching device is adopted to intelligently control the vacuum environment and the quick quenching speed of the quick quenching, and a proper vacuum environment and temperature for vacuum crystallization treatment are selected, especially the whole preparation process is carried out under the protection of argon, the crystal grain structure of the product is further refined, the orientation degree of the magnetic powder is influenced, and the high temperature resistance, the corrosion resistance and various magnetic properties of the magnetic powder are further improved under the combined action of the selection of various parameters.
Detailed Description
The technical solution of the present invention will be described in detail by specific examples.
The following Nd element sources are pure neodymium metal with the purity of more than 99.0 percent or praseodymium-neodymium alloy with the neodymium content of more than 80 percent; the Fe element source is industrial pure iron with 99.8 percent and ferroboron alloy with boron more than 19 percent; the B element source is ferroboron containing more than 19 percent of boron; the Gd element is sourced from metal gadolinium with the purity of more than 99 percent; the Zn element is derived from metal zinc with the purity of more than 99 percent.
Example 1
A neodymium iron boron bonded magnetic powder added with zinc and gadolinium compositely comprises the following elements in percentage by weight: 10.5% of Nd, 2% of Gd, 6% of B, 0.5% of Zn and the balance of Fe.
The preparation method of the bonded magnetic powder comprises the following operation steps:
1) taking raw materials according to the weight percentage of each element, adding the raw materials into a vacuum melting furnace, and controlling the melting temperature to be less than 4 × 10-2Smelting into an alloy ingot under the vacuum state of Pa;
2) crushing the alloy ingot smelted in the step 1), adding the crushed alloy ingot into a vacuum induction quick quenching furnace, wherein the vacuum degree reaches 5 × 10-2Introducing argon after Pa, melting an alloy ingot crushed at 1500 ℃ in an argon environment into molten metal, controlling the rapid quenching speed to be 25-33 m/s, and rapidly quenching the molten metal into uniform strips with the thickness of 50 +/-5 mu m;
3) crushing the uniform strip prepared in the step 2) into 40-mesh magnetic powder.
4) 4.5-5.5 × 10 g of the magnetic powder prepared in the step 3)-2And (3) setting the blanking speed of the crystallization furnace to be 25kg/h and the rotating speed to be 20 r/s under the vacuum degree of Pa and the temperature of 650 ℃, and performing vacuum crystallization treatment to complete the process.
Example 2
A neodymium iron boron bonded magnetic powder added with zinc and gadolinium compositely comprises the following elements in percentage by weight: 10% of Nd, 2.6% of Gd, 6.5% of B, 0.4% of Zn and the balance of Fe.
The preparation method of the bonded magnetic powder comprises the following operation steps:
1) taking raw materials according to the weight percentage of each element, adding the raw materials into a vacuum melting furnace, and controlling the melting temperature to be less than 4 × 10-2Smelting into an alloy ingot under the vacuum state of Pa;
2) crushing the alloy ingot smelted in the step 1), adding the crushed alloy ingot into a vacuum induction quick quenching furnace, wherein the vacuum degree reaches 5 × 10-2After Pa, filling argon, melting an alloy ingot crushed at 1450 ℃ in an argon environment into molten metal, controlling the rapid quenching speed to be 25-33 m/s, and rapidly quenching the molten metal into uniform strips with the thickness of 50 +/-5 mu m;
3) crushing the uniform strips prepared in the step 2) into magnetic powder of 40 meshes;
4) 4.5-5.5 × 10 g of the magnetic powder prepared in the step 3)-2And (3) carrying out crystallization treatment under the vacuum degree of Pa and the temperature of 600 ℃ and at the charging speed of 23kg/h and the rotating speed of 20 r/s of the crystallization furnace.
Example 3
A neodymium iron boron bonded magnetic powder added with zinc and gadolinium compositely comprises the following elements in percentage by weight: nd 11%, Gd1.0%, B7%, Zn 0.2%, and the balance of Fe.
The preparation method of the bonded magnetic powder comprises the following operation steps:
1) taking raw materials according to the weight percentage of each element, adding the raw materials into a vacuum melting furnace, and controlling the melting temperature to be less than 4 × 10-2Smelting into an alloy ingot under the vacuum state of Pa;
2) crushing the alloy ingot smelted in the step 1), adding the crushed alloy ingot into a vacuum induction quick quenching furnace, wherein the vacuum degree reaches 5 × 10-2Introducing argon after Pa, melting an alloy ingot crushed at the temperature of 1480 ℃ in an argon environment into molten metal, controlling the rapid quenching speed to be 25-33 m/s, and rapidly quenching the molten metal into molten metal with the thickness of 50 +/-5 mum uniform strips;
3) crushing the uniform strips prepared in the step 2) into magnetic powder of 40 meshes;
4) 4.5-5.5 × 10 g of the magnetic powder prepared in the step 3)-2And (3) carrying out crystallization treatment under the conditions of Pa vacuum degree and argon gas filling, at the temperature of 700 ℃, setting the blanking speed to be 20kg/h and the rotating speed to be 20 r/s.
Comparative example 1
The comparative bonded magnetic powder is different from the example 1 in that the bonded magnetic powder comprises the following elements in percentage by weight: 10.5% of Nd, 6% of B, 2.5% of Zn and the balance of Fe.
Comparative example 2
The comparative bonded magnetic powder is different from the example 1 in that the bonded magnetic powder comprises the following elements in percentage by weight: 12.5% of Nd, 6% of B, 0.5% of Zn and the balance of Fe.
Comparative example 3
The comparative bonded magnetic powder is different from the example 1 in that the bonded magnetic powder comprises the following elements in percentage by weight: 10.5% of Nd, 2.5% of Gd, 6% of B and the balance of Fe.
Comparative example 4
The comparative bonded magnetic powder is different from the example 1 in that the bonded magnetic powder comprises the following elements in percentage by weight: nd 11%, Gd 2%, B6%, and the balance of Fe.
Comparative example 5
The comparative bonded magnetic powder is different from the example 1 in that the bonded magnetic powder comprises the following elements in percentage by weight: 10.5% of Nd, 6% of B and the balance of Fe.
Comparative example 6
The comparative bonded magnetic powder is different from that of example 1 in that the melting temperature in step 2) is adjusted to 1600 ℃, the rapid quenching speed in step 2) is adjusted to 20m/s, the temperature in the crystallization treatment process in step 3) is adjusted to 800 ℃, the blanking speed is adjusted to 30kg/h, and the rotating speed is adjusted to 25 r/s, and the rest is the same as example 1.
Comparative example 7
The bonded magnetic powder of this comparative example is different from example 1 in that the melting temperature in step 1) is adjusted to 1400 ℃, the rapid quenching speed in step 2) is adjusted to 35m/s, the temperature in the crystallization process in step 3) is adjusted to 550 ℃, the blanking speed is adjusted to 15kg/h, and the rotation speed is adjusted to 15 rpm, and the same as example 1 is otherwise applied.
Test examples
Test method 1: the magnetic powders prepared in examples 1 to 3 and comparative examples 1 to 7 were mixed with an epoxy resin in a ratio of 98: 2, processed and pressed into a circular magnet having a diameter and a height of 10mm, and the magnetic properties and the curie temperature were measured by a magnetic property tester and a curie temperature tester model JZB-1, the results of which are shown in table 1 below:
TABLE 1
| Hcj | （BH）max | Curie temperature | Br | |
| Example 1 | 10.25kOe | 11.2MGOe | 390℃ | 9500Gs |
| Example 2 | 9.95kOe | 10.8MGOe | 380℃ | 9325Gs |
| Example 3 | 9.7kOe | 10.7MGOe | 370℃ | 9220Gs |
| Comparative example 1 | 9.6kOe | 10.5MGOe | 300℃ | 8520Gs |
| Comparative example 2 | 9.4kOe | 10.3MGOe | 290℃ | 8350Gs |
| Comparative example 3 | 8.95kOe | 10.1MGOe | 280℃ | 8200Gs |
| Comparative example 4 | 8.82kOe | 10.2MGOe | 275℃ | 8250Gs |
| Comparative example 5 | 8.54kOe | 9.8MGOe | 265℃ | 8100Gs |
| Comparative example 6 | 8.25kOe | 9.21MGOe | 350℃ | 7850Gs |
| Comparative example 7 | 8.80kOe | 10.35MGOe | 355℃ | 8960Gs |
From the results shown in Table 1 above, it is understood that the magnetic powder prepared in example 1 is superior in temperature resistance and magnetic properties to those of example 2 and example 3.
The results show that the magnetic powder prepared in the examples 1 to 3 has better properties than the comparative example 1, the comparative example 2, the comparative example 3, the comparative example 4 and the comparative example 5, and that gadolinium and zinc are simultaneously doped into the neodymium iron boron magnetic material to mutually act synergistically to improve Hcj (BH) of the bonded magnetic powdermaxBr and Curie temperature, and improve the comprehensive performance of the bonded magnetic powder.
The magnetic powder prepared in the embodiments 1 to 3 has various performances superior to those of the comparative example 7 and 6, and the results show that the high temperature resistance of the magnetic powder is further improved under the combined action of the selection of various parameters under the control of parameters such as melting temperature, vacuum degree, rapid quenching speed, crystallization treatment temperature, vacuum degree and the like defined by the invention, so that the prepared magnetic powder has excellent comprehensive performance.
Test method 2:
the magnetic powders prepared in examples 1 to 3 and comparative examples 1 to 5 were mixed with an epoxy resin in a ratio of 98: 2, which was processed and then pressed into a circular magnet having a diameter and a height of 10mm, and the magnet was placed at 85 ℃ and 80% RH for 180 days to observe the appearance of each magnet, the results of which are shown in table 2 below: wherein the mass loss is the ratio of the mass difference of the magnet before and after placement to the mass of the magnet before placement;
TABLE 2
| Pulverized state of magnet | |
| Example 1 | No obvious chalking phenomenon appears in the appearance, and the mass loss is less than 5 percent |
| Example 2 | No obvious chalking phenomenon appears in the appearance, and the mass loss is less than 5 percent |
| Example 3 | No obvious chalking phenomenon appears in the appearance, and the mass loss is less than 5 percent |
| Comparative example 1 | Obvious powdering phenomenon is visible in appearance, and the mass loss reaches about 10 percent |
| Comparative example 2 | Obvious powdering phenomenon is visible in appearance, and the mass loss reaches about 10 percent |
| Comparative example 3 | Obvious powdering phenomenon is visible in appearance, and the mass loss reaches about 10 percent |
| Comparative example 4 | Obvious powdering phenomenon is visible in appearance, and the mass loss reaches about 10 percent |
| Comparative example 5 | Obvious powdering phenomenon is visible in appearance, and the mass loss reaches about 10 percent |
From the results shown in table 2, it can be seen that, in the invention, by doping gadolinium and zinc into the neodymium iron boron magnet material in a composite manner, and by limiting the doping amount of each metal element, a synergistic interaction is generated between the gadolinium and the zinc, and the corrosion resistance of the prepared product is improved.
Claims (6)
1. The neodymium iron boron bonded magnetic powder added with zinc and gadolinium is characterized in that the magnetic powder comprises the following elements in percentage by weight: 10-11% of Nd, 1.0-2.6% of Gd, 6-7% of B, 0.2-0.5% of Zn and the balance of Fe;
the preparation method of the neodymium iron boron bonded magnetic powder added with zinc and gadolinium comprises the following operation steps:
1) taking raw materials according to the weight percentage of each element, adding the raw materials into a vacuum melting furnace, and controlling the melting temperature to be less than 4 × 10-2Smelting into an alloy ingot under the vacuum state of Pa;
2) crushing the alloy ingot smelted in the step 1), adding the crushed alloy ingot into a vacuum induction quick quenching furnace, wherein the vacuum degree reaches 5 × 10-2Filling argon after Pa, melting the mixture into molten metal at 1450-1500 ℃ in an argon environment, controlling the rapid quenching speed to be 25-33 m/s, and rapidly quenching the molten metal into uniform strips with the thickness of 50 +/-5 mu m;
3) crushing the uniform strips prepared in the step 2) into magnetic powder of 40 meshes;
4) setting the blanking speed of the crystallization furnace to be 20-25 kg/h and the rotating speed to be 20 r/s, and enabling the magnetic powder prepared in the step 3) to be 4.5-5.5 × 10-2And (3) carrying out crystallization treatment at the temperature of 600-700 ℃ under the vacuum degree of Pa, thus completing the process.
2. The composite zinc and gadolinium added neodymium iron boron bonded magnetic powder according to claim 1, wherein the magnetic powder comprises the following elements by weight percent: 10.5% of Nd, 2% of Gd, 6% of B, 0.5% of Zn and the balance of Fe.
3. The composite zinc and gadolinium added neodymium iron boron bonded magnetic powder according to claim 1, wherein the magnetic powder comprises the following elements by weight percent: 10% of Nd, 2.6% of Gd, 6.5% of B, 0.4% of Zn and the balance of Fe.
4. The composite zinc and gadolinium added neodymium iron boron bonded magnetic powder according to claim 1, wherein the magnetic powder comprises the following elements by weight percent: nd 11%, Gd1.0%, B7%, Zn 0.2%, and the balance of Fe.
5. The method for preparing neodymium-iron-boron bonded magnetic powder compositely added with zinc and gadolinium according to claim 1, wherein the step 4) further comprises the step of adding the magnetic powder prepared in the step 3) into a crystallization furnace for crystallization after argon is filled into the crystallization furnace.
6. The composite zinc and gadolinium added neodymium iron boron bonded magnetic powder according to any one of claims 1 to 4, wherein the Nd element source is pure neodymium metal with purity of more than 99.0%; the Fe element source is industrial pure iron with 99.8 percent of content and ferroboron alloy with boron content more than 19 percent; the source of the B element is ferroboron containing more than 19 percent of boron; the Gd element is sourced from metal gadolinium with the purity of more than 99 percent; the Zn element source is metal zinc with the purity of more than 99 percent.
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