CN114512327B - Preparation method of high-coercivity composite magnet - Google Patents
Preparation method of high-coercivity composite magnet Download PDFInfo
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- CN114512327B CN114512327B CN202210228541.4A CN202210228541A CN114512327B CN 114512327 B CN114512327 B CN 114512327B CN 202210228541 A CN202210228541 A CN 202210228541A CN 114512327 B CN114512327 B CN 114512327B
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- 239000002131 composite material Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 229910002546 FeCo Inorganic materials 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 21
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 14
- 230000008569 process Effects 0.000 claims abstract description 14
- 229910016629 MnBi Inorganic materials 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 238000011065 in-situ storage Methods 0.000 claims abstract description 9
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 7
- 238000005215 recombination Methods 0.000 claims abstract description 6
- 230000006798 recombination Effects 0.000 claims abstract description 6
- 238000000151 deposition Methods 0.000 claims description 21
- 230000008021 deposition Effects 0.000 claims description 21
- 239000013077 target material Substances 0.000 claims description 11
- 238000000137 annealing Methods 0.000 claims description 10
- 239000000758 substrate Substances 0.000 claims description 6
- 238000004544 sputter deposition Methods 0.000 claims description 5
- 239000000696 magnetic material Substances 0.000 abstract description 3
- 238000000465 moulding Methods 0.000 abstract 1
- 239000011572 manganese Substances 0.000 description 16
- KYAZRUPZRJALEP-UHFFFAOYSA-N bismuth manganese Chemical compound [Mn].[Bi] KYAZRUPZRJALEP-UHFFFAOYSA-N 0.000 description 3
- 229910001152 Bi alloy Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910001172 neodymium magnet Inorganic materials 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000005477 sputtering target Methods 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
- C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
- C23C14/5806—Thermal treatment
-
- 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
-
- 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
- H01F1/12—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 soft-magnetic materials
- H01F1/14—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 soft-magnetic materials metals or alloys
- H01F1/147—Alloys characterised by their composition
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Metallurgy (AREA)
- Mechanical Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Dispersion Chemistry (AREA)
- Electromagnetism (AREA)
- Manufacturing & Machinery (AREA)
- Thermal Sciences (AREA)
- Thin Magnetic Films (AREA)
- Manufacturing Cores, Coils, And Magnets (AREA)
Abstract
The invention discloses a preparation method of a high-coercivity composite magnet, and belongs to the technical field of magnetic materials. The preparation method comprises the following steps: the Bi layer, the Mn layer and the FeCo layer are deposited by magnetron sputtering, the (Bi/Mn/FeCo) multiplied by N multilayer sandwich structure film is prepared, N=1-5, and then the multilayer film is subjected to magnetic field heat treatment in situ, so that the formation of LTP MnBi phase and soft magnetic FeCo phase and the effective recombination between the two phases are realized, and finally the high-coercivity composite magnet is obtained. The method has simple process, easy molding, reduced cost and contribution to the application of the high-performance magnet in more permanent magnet devices.
Description
Technical Field
The invention relates to the technical field of magnetic materials, in particular to a preparation method of a high-coercivity composite magnet.
Background
In recent years, with the increasing reduction of rare earth resources and the rapid increase of price in the world, research on rare earth-free permanent magnet materials has become a hot spot. The MnBi permanent magnet has the advantages of low price, difficult corrosion, good mechanical property and the like, and particularly has positive coercive force temperature coefficient in a certain temperature range, so that the defect of the NdFeB permanent magnet can be overcome. However, as the MnBi low-temperature phase is formed by peritectic reaction, single-phase alloy is extremely difficult to prepare, so that the magnetic property of the MnBi low-temperature phase is low, and the application of the material is greatly limited. Therefore, how to obtain the high-performance pure single-phase manganese bismuth alloy and improve the magnetic property of the manganese bismuth alloy becomes a key problem of widening the application range of the manganese bismuth permanent magnetic material.
Therefore, the Bi layer, the Mn layer and the FeCo layer are deposited by magnetron sputtering to prepare the (Bi/Mn/FeCo) multiplied by N multilayer sandwich structure film, N=1-5, and then the multilayer film is subjected to magnetic field heat treatment in situ to realize the formation of LTP MnBi phase and soft magnetic FeCo phase and the effective recombination between the two phases, and finally the high-coercivity composite magnet is obtained.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention aims to provide a preparation method of a high-coercivity composite magnet.
The aim of the invention can be achieved by the following technical scheme: a preparation method of a high-coercivity composite magnet is characterized in that a pure Bi target, a pure Mn target and Fe are arranged on a Si sheet substrate by utilizing a magnetron sputtering process 50 Co 50 The target material is sequentially sputtered on a Si sheet to prepare a (Bi/Mn/FeCo) multiplied by N multilayer sandwich structure film, wherein the deposition thickness of a Bi layer is 4 nm-8 nm, the deposition thickness of a Mn layer is 2 nm-6 nm, the deposition thickness of a FeCo layer is 10 nm-16 nm, and then the multilayer film is subjected to in-situ magnetic field heat treatment to realize the formation of an LTP MnBi phase and a soft magnetic FeCo phase and the effective recombination between the two phases, and finally the high-coercivity composite magnet is obtained.
Further, the vacuum degree of the vacuum chamber in the sputtering process is 4×10 -4 Pa~4×10 -3 Pa, magnetron sputtering current is 15-35A, and deposition rate of the target is 0.015-nm/s-0.099-nm/s.
Further, the magnetic field strength is 0.5T-1T, the annealing temperature is 500-850 ℃, and the annealing time is 15-60 min.
Compared with the prior art, the invention has the following advantages and beneficial effects: the invention uses the magnetron sputtering technology to make the pure Bi target material, the pure Mn target material and Fe on the Si sheet substrate 50 Co 50 Sputtering target materials on Si sheets sequentially to prepare a (Bi/Mn/FeCo) multiplied by N multilayer sandwich structure film, wherein N=1-5, and performing in-situ magnetic field heat treatment on the multilayer film to finally obtain the high-coercivity composite magnet; the improvement of magnetic performance is realized by about exchange coupling between the MnBi low-temperature phase and the soft magnetic FeCo phase; the method has the advantages of simple process, low process cost and low energy consumption.
Description of the embodiments
The present invention will be described in further detail with reference to examples, but the present invention is not limited to the following examples.
Example 1
Pure Bi target material, pure Mn target material and Fe on Si sheet substrate by utilizing magnetron sputtering process 50 Co 50 The targets are sputtered on the Si sheet in sequence, and the sputtering processThe vacuum degree of the medium vacuum chamber is 5 multiplied by 10 -4 Pa, magnetron sputtering current is 15A, and deposition rate of the target is 0.099 nm/s; preparing a (Bi/Mn/FeCo) x 2 double-layer sandwich structure film, wherein the deposition thickness of the Bi layer is 4 nm, the deposition thickness of the Mn layer is 2 nm, and the deposition thickness of the FeCo layer is 10 nm; and then carrying out in-situ magnetic field heat treatment on the multilayer film, wherein the magnetic field strength is 0.5 and T, the annealing temperature is 550 ℃, and the annealing time is 60 minutes, so that the formation of an LTP MnBi phase and a soft magnetic FeCo phase and the effective recombination between the two phases are realized, and finally, the high-coercivity composite magnet is obtained.
The high-coercivity composite magnet prepared by the method has a coercivity of 16.5 kOe and a magnetic energy product of 9.8 MGOe through magnetic property test.
Example 2
Pure Bi target material, pure Mn target material and Fe on Si sheet substrate by utilizing magnetron sputtering process 50 Co 50 The targets are sputtered on Si sheets in sequence, and the vacuum degree of a vacuum chamber in the sputtering process is 5 multiplied by 10 -4 Pa, magnetron sputtering current of 25A, and deposition rate of the target of 0.055 nm/s; preparing a (Bi/Mn/FeCo) x 3 three-layer sandwich structure film, wherein the deposition thickness of the Bi layer is 6 nm, the deposition thickness of the Mn layer is 4 nm, and the deposition thickness of the FeCo layer is 12 nm; and then carrying out in-situ magnetic field heat treatment on the multilayer film, wherein the magnetic field strength is 0.8 and T, the annealing temperature is 650 ℃, and the annealing time is 35 min, so that the formation of an LTP MnBi phase and a soft magnetic FeCo phase and the effective recombination between the two phases are realized, and finally, the high-coercivity composite magnet is obtained.
The high-coercivity composite magnet prepared by the method has coercivity of 17.5 kOe and magnetic energy product of 10.7 MGOe through magnetic property test.
Example 3
Pure Bi target material, pure Mn target material and Fe on Si sheet substrate by utilizing magnetron sputtering process 50 Co 50 The targets are sputtered on Si sheets in sequence, and the vacuum degree of a vacuum chamber in the sputtering process is 5 multiplied by 10 -4 Pa, magnetron sputtering current is 35A, and deposition rate of the target is 0.021 nm/s; preparing a (Bi/Mn/FeCo) x 5 five-layer sandwich structure film, wherein the deposition thickness of the Bi layer is 8 nm, the deposition thickness of the Mn layer is 6 nm, and the deposition thickness of the FeCo layer is 16 nm; then to multiple layersAnd carrying out magnetic field heat treatment on the film in situ, wherein the magnetic field strength is 1T, the annealing temperature is 750 ℃, the annealing time is 15 min, the formation of LTP MnBi phase and soft magnetic FeCo phase and the effective combination between the two phases are realized, and finally, the high-coercivity composite magnet is obtained.
The high-coercivity composite magnet prepared by the method has coercivity of 18.5 kOe and magnetic energy product of 11.9 MGOe through magnetic property test.
Claims (3)
1. A preparation method of a high-coercivity composite magnet is characterized in that a pure Bi target, a pure Mn target and Fe are arranged on a Si sheet substrate by utilizing a magnetron sputtering process 50 Co 50 The target material is sequentially sputtered on a Si sheet to prepare a (Bi/Mn/FeCo) multiplied by N multilayer sandwich structure film, wherein the deposition thickness of a Bi layer is 4 nm-8 nm, the deposition thickness of a Mn layer is 2 nm-6 nm, the deposition thickness of a FeCo layer is 10 nm-16 nm, and then the multilayer film is subjected to in-situ magnetic field heat treatment to realize the formation of an LTP MnBi phase and a soft magnetic FeCo phase and the effective recombination between the two phases, and finally the high-coercivity composite magnet is obtained.
2. The method for preparing the high-coercivity composite magnet according to claim 1, which is characterized in that the process conditions of magnetron sputtering deposition are as follows: vacuum degree of vacuum chamber in sputtering process is 4×10 -4 Pa~4×10 -3 Pa, magnetron sputtering current is 15-35A, and deposition rate of the target is 0.015-nm/s-0.099-nm/s.
3. The method for preparing the high coercivity composite magnet according to claim 1, characterized in that the in-situ magnetic field heat treatment process conditions are as follows: the magnetic field strength is 0.5T-1T, the annealing temperature is 500-850 ℃, and the annealing time is 15-60 min.
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| CN202210228541.4A CN114512327B (en) | 2022-03-10 | 2022-03-10 | Preparation method of high-coercivity composite magnet |
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| CN202210228541.4A CN114512327B (en) | 2022-03-10 | 2022-03-10 | Preparation method of high-coercivity composite magnet |
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| CN114512327B true CN114512327B (en) | 2023-11-10 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002100028A (en) * | 2000-09-26 | 2002-04-05 | Sony Corp | Metal thin-film type magnetic recording medium |
| CN105081342A (en) * | 2014-05-06 | 2015-11-25 | 丰田自动车工程及制造北美公司 | Method to prepare hard-soft magnetic FeCo/SiO2/MnBi nanoparticles with magnetically induced morphology |
| CN105777107A (en) * | 2016-03-17 | 2016-07-20 | 江苏新浦电子科技有限公司 | Ceramic target for preparing conducting glass by aid of magnetron sputtering method |
| CN106567040A (en) * | 2015-10-10 | 2017-04-19 | 中国科学院上海硅酸盐研究所 | Magnetoelectric composite film and preparation method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5948033B2 (en) * | 2011-09-21 | 2016-07-06 | 株式会社日立製作所 | Sintered magnet |
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- 2022-03-10 CN CN202210228541.4A patent/CN114512327B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002100028A (en) * | 2000-09-26 | 2002-04-05 | Sony Corp | Metal thin-film type magnetic recording medium |
| CN105081342A (en) * | 2014-05-06 | 2015-11-25 | 丰田自动车工程及制造北美公司 | Method to prepare hard-soft magnetic FeCo/SiO2/MnBi nanoparticles with magnetically induced morphology |
| CN106567040A (en) * | 2015-10-10 | 2017-04-19 | 中国科学院上海硅酸盐研究所 | Magnetoelectric composite film and preparation method thereof |
| CN105777107A (en) * | 2016-03-17 | 2016-07-20 | 江苏新浦电子科技有限公司 | Ceramic target for preparing conducting glass by aid of magnetron sputtering method |
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