CN114628104A - Planar anisotropic soft magnetic material and preparation method thereof - Google Patents
Planar anisotropic soft magnetic material and preparation method thereof Download PDFInfo
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- CN114628104A CN114628104A CN202111535658.9A CN202111535658A CN114628104A CN 114628104 A CN114628104 A CN 114628104A CN 202111535658 A CN202111535658 A CN 202111535658A CN 114628104 A CN114628104 A CN 114628104A
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- 239000000696 magnetic material Substances 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title abstract description 10
- 238000000498 ball milling Methods 0.000 claims abstract description 40
- 239000000463 material Substances 0.000 claims abstract description 27
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000000956 alloy Substances 0.000 claims abstract description 14
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 12
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052802 copper Inorganic materials 0.000 claims abstract description 8
- 239000010949 copper Substances 0.000 claims abstract description 8
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000010936 titanium Substances 0.000 claims abstract description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical group [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 3
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical group [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 3
- 239000010941 cobalt Substances 0.000 claims abstract description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical group [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 3
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical group [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims abstract description 3
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 3
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 3
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical group [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910052721 tungsten Chemical group 0.000 claims abstract description 3
- 239000010937 tungsten Chemical group 0.000 claims abstract description 3
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 3
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical group [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 3
- 229910052751 metal Inorganic materials 0.000 claims description 13
- 239000002184 metal Substances 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 7
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 5
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 5
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 5
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 5
- 239000005642 Oleic acid Substances 0.000 claims description 5
- 229910052772 Samarium Inorganic materials 0.000 claims description 5
- 239000002270 dispersing agent Substances 0.000 claims description 5
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 5
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 5
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical group [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 claims description 5
- 229910052742 iron Inorganic materials 0.000 claims description 4
- 238000005266 casting Methods 0.000 claims 2
- 238000004519 manufacturing process Methods 0.000 claims 2
- 239000000203 mixture Substances 0.000 claims 1
- 230000005291 magnetic effect Effects 0.000 abstract description 18
- 230000035699 permeability Effects 0.000 abstract description 6
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 6
- 150000002910 rare earth metals Chemical class 0.000 abstract description 5
- 238000000227 grinding Methods 0.000 abstract description 4
- 238000005303 weighing Methods 0.000 abstract description 4
- 239000000843 powder Substances 0.000 description 11
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 8
- 238000003723 Smelting Methods 0.000 description 6
- 230000005415 magnetization Effects 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000005280 amorphization Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 2
- 230000005347 demagnetization Effects 0.000 description 2
- 238000009987 spinning Methods 0.000 description 2
- 241000656145 Thyrsites atun Species 0.000 description 1
- 230000004075 alteration Effects 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
- 230000000694 effects Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000005294 ferromagnetic effect Effects 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 238000002074 melt spinning Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 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
- H01F1/12—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
-
- 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
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention relates to the field of soft magnetic materials, and provides a planar anisotropic soft magnetic material with Sm as a component aiming at the problem that the magnetic permeability of an alloy soft magnetic material is difficult to improve due to the limitation of saturation magnetization1‑xREx(Fe0.8X0.2)12‑yMyWherein RE is zirconium element, X is selected from cobalt, manganese, nickel, aluminum and copper element, and M is selected from titanium, vanadium and tungsten element. The magnetic permeability and the natural resonant frequency of the soft magnetic material with the plane anisotropy can be further improved. The invention also provides a preparation method of the planar anisotropic soft magnetic material, which comprises the steps of weighing the raw materials in proportion, mixing, preparing an alloy strip, grinding the strip firstly and then ball-milling, and preparing the soft magnetic material with the planar anisotropic sheet shape. The invention prepares the material into the easy-to-surface soft magnetic material with plane anisotropy by ball milling and non-crystallizing, the preparation method is simple, and the prepared rare earth soft magnetic material can haveEffectively improve the magnetic performance of the soft magnetic material.
Description
Technical Field
The invention relates to the field of soft magnetic materials, in particular to a planar anisotropic soft magnetic material and a preparation method thereof.
Background
According to the Snoek limit formula proposed in 1947, the magnetic permeability (magnetic loss performance) and the natural resonant frequency of the material are proportional to the saturation magnetization of the material. For the alloy soft magnetic material, the saturation magnetization can not be increased without limit, and the magnetic loss performance of the material and the promotion space of the natural resonance frequency fr (generally <3GHz) are limited. The bottleneck problem causes the electromagnetic loss performance of related materials in a high frequency band to be sharply reduced, and the engineering application development is severely restricted. However, for a material with planar anisotropy, the magnetic permeability and natural resonant frequency of the material can be further improved because the in-plane anisotropy field is generally smaller than the out-of-plane anisotropy field. Therefore, it is necessary to study a soft magnetic material having plane anisotropy. In addition, 4f-3d orbital electronic coupling between rare earth and transition metal elements is beneficial to enhancing the ferromagnetic exchange effect of the magnetic material, so that the research on the rare earth soft magnetic material and the regulation and control of the microstructure of the rare earth soft magnetic material are reliable means for improving the magnetic performance of the soft magnetic material.
Generally, common rare earth soft magnetic materials are axially anisotropic, and found by the great university of Lanzhou, Tao et al, to convert the Nd in the form of flakes2Co17After the material is ball-milled and crushed, the material is broken along a c-axis crystal plane, and the component of the magnetic conductivity meets mui'～1+p/((1-p)Nd) (p is the volume fraction of the magnetic material, NdIs a demagnetization factor), when the out-of-plane anisotropy field of the material is the sum of the demagnetization field and the c-axis anisotropy field, the magnetic loss performance and the natural resonance frequency (y.zhang, p.wang, t.ma, y.wang, l.qiao, t.wang, High-frequency electromagnetic properties of magnetic Nd) of the material are further improved2Co17micron flakes fractured along c crystal plane with natural resonance frequency exceeding 10GHz,Appl.Phys.Lett.108(2016)092406.)。
Disclosure of Invention
The invention provides a planar anisotropic soft magnetic material for overcoming the problem that the magnetic conductivity of an alloy soft magnetic material is limited by saturation magnetization intensity and is difficult to improve, the magnetic conductivity and the natural resonance frequency are improved, and the planar anisotropic soft magnetic material has stronger wave-absorbing performance and can be applied to the field of electromagnetic wave absorption.
In order to achieve the purpose, the invention adopts the following technical scheme:
a planar anisotropic soft magnetic material comprises Sm1-xREx(Fe0.8X0.2)12-yMyWherein Sm is samarium, RE is zirconium, Fe is ironX is selected from cobalt, manganese, nickel, aluminum and copper, M is selected from titanium, vanadium and tungsten, 0<x<1，0<y<12. The existing alloy soft magnetic material has a bottleneck due to saturation magnetization, so that the magnetic loss performance and the natural resonant frequency f of the material are limitedrThe magnetic permeability and the natural resonant frequency of the soft magnetic material with the plane anisotropy can be further improved.
The invention also provides a preparation method of the planar anisotropic soft magnetic material, which comprises the following steps: the raw materials are weighed according to the proportion, mixed and prepared into an alloy strip, and the strip is ground and then ball-milled to prepare the soft magnetic material with the planar anisotropy and the flake form. The invention prepares the material into the easy-to-surface soft magnetic material with plane anisotropy by ball milling and non-crystallizing, the preparation method is simple, and the magnetic performance of the prepared rare earth soft magnetic material is effectively improved.
Preferably, the raw materials are mixed and then melted into metal ingots with uniform components, and the metal ingots are crushed into small pieces and then prepared into alloy strips. As a further preference, the alloy strip is produced using a strip-spinning machine, wherein the copper roll speed is 30-55m/s and the strip-spinning vacuum is (4-6) × 10-3Pa. The material is pre-amorphized by melt spinning, which is beneficial to complete amorphization achieved by subsequent ball milling.
Preferably, the ribbon is first ground to 125 μm or less and then ball milled.
Preferably, the ball milling conditions are as follows: the ball-material ratio is 1 (65-75), the ball milling time is 24-96h, and oleic acid accounting for 1-10% of the total mass of the balls and the materials is added as a dispersing agent. More preferably, the ball milling time is 48 to 72 hours. More preferably, the solvent used for ball milling is n-hexane.
Therefore, the beneficial effects of the invention are as follows: (1) preparing the material into an easy-to-surface soft magnetic material with plane anisotropy by ball milling and amorphization; (2) the material is pre-amorphized by a melt-spun belt, so that the subsequent ball milling is facilitated to achieve complete amorphization; (3) the soft magnetic material with plane anisotropy is prepared, the magnetic conductivity and the natural resonance frequency are improved, meanwhile, the soft magnetic material is widely applied to the field of electromagnetic wave absorption, and the material prepared by the method has strong wave absorption performance.
Drawings
FIG. 1 is a diagram of the morphology of the powder after ball milling;
FIG. 2 is a diagram of the wave-absorbing performance of the powder after ball milling.
Detailed Description
The technical solution of the present invention is further illustrated by the following specific examples.
In the present invention, unless otherwise specified, all the raw materials and equipment used are commercially available or commonly used in the art, and the methods in the examples are conventional in the art unless otherwise specified.
Example 1
A planar anisotropic soft magnetic material consisting of: sm0.8Zr0.2(Fe0.8Co0.2)11.5Ti0.5Wherein Sm is samarium and Fe is iron. The preparation method comprises the following steps:
1) weighing the raw materials according to the proportion, mixing, and smelting the raw materials into metal ingots with uniform components by using a smelting furnace;
2) crushing the metal ingot into small blocks, preparing the metal ingot into an alloy strip by using a strip throwing machine, wherein the speed of a copper roller is 50m/s, and the strip throwing vacuum is 5 x 10-3Pa；
3) Grinding the obtained strip to be below 125 mu m, further crushing the strip into powder by using ball milling, wherein the ball milling ball material ratio is 1:70, the ball milling time is 24h, oleic acid accounting for 5 percent of the total mass of the ball and the material is added during ball milling as a dispersing agent, and the ball milling solvent is n-hexane, so that the soft magnetic material with the planar anisotropy and the flake form is prepared.
Example 2
The difference from example 1 is that the ball milling time is 48 h.
Example 3
The difference from example 1 is that the ball milling time is 72 h.
Example 4
The difference from example 1 is that the ball milling time is 96 h.
Example 5
A planar anisotropic soft magnetic material consisting of: sm0.6Zr0.4(Fe0.8Mn0.2)10V2Wherein Sm is samarium and Fe is iron. The preparation method comprises the following steps:
1) weighing the raw materials according to the proportion, mixing, and smelting the raw materials into metal ingots with uniform components by using a smelting furnace;
2) crushing the metal ingot into small pieces, preparing the metal ingot into an alloy strip by using a strip throwing machine, wherein the speed of a copper roller is 30m/s, and the strip throwing vacuum is 6 x 10-3Pa；
3) Grinding the obtained strip to be below 125 mu m, further crushing the strip into powder by using ball milling, wherein the ball milling ball material ratio is 1:65, the ball milling time is 48h, oleic acid accounting for 1 percent of the total mass of the ball and the material is added during ball milling to be used as a dispersing agent, and the ball milling solvent is n-hexane, so that the soft magnetic material with the planar anisotropy and the flake form is prepared.
Example 6
A planar anisotropic soft magnetic material consisting of: sm0.7Zr0.3(Fe0.8Ni0.2)9.5W2.5Wherein Sm is samarium and Fe is iron. The preparation method comprises the following steps:
1) weighing the raw materials according to the proportion, mixing, and smelting the raw materials into metal ingots with uniform components by using a smelting furnace;
2) crushing the metal ingot into small pieces, preparing the metal ingot into an alloy strip by using a strip throwing machine, wherein the speed of a copper roller is 55m/s, and the vacuum of the strip throwing is 4 x 10-3Pa；
3) Grinding the obtained strip to be below 125 mu m, further crushing the strip into powder by using ball milling, wherein the ball milling ball material ratio is 1:75, the ball milling time is 48h, oleic acid accounting for 10 percent of the total mass of the ball and the material is added during ball milling as a dispersing agent, and the ball milling solvent is n-hexane, so that the soft magnetic material with the planar anisotropy and the flake form is prepared.
Performance testing
FIG. 1 is a graph of the morphology of the powder after ball milling in examples 1-4, and it can be seen that the powder after ball milling is obviously flaky, and the flaky powder is gradually thinned and reduced as the ball milling time is increased from 24h to 96h, but the reduction of the powder from 72h to 96h is not as significant as before. In combination with the wave-absorbing performance diagram of the powder after ball milling shown in FIG. 2, the wave-absorbing performance of the powder after ball milling for 48h is the best, and ball milling for 72h is the second best, so that in combination, the ball milling time is preferably between 48 and 72 h.
The following table lists the properties of the soft magnetic materials prepared in examples 1 to 4, which shows that the soft magnetic materials prepared by the present invention have planar anisotropy, and enhance magnetic permeability and natural resonant frequency.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (7)
1. A planar anisotropic soft magnetic material is characterized in that the component Sm1-xREx(Fe0.8X0.2)12-yMyWherein Sm is samarium, RE is zirconium, Fe is iron, X is selected from cobalt, manganese, nickel, aluminum and copper, M is selected from titanium, vanadium and tungsten, 0<x<1，0<y<12。
2. A method for preparing a planar anisotropic soft magnetic material according to claim 1, comprising the steps of: the raw materials are weighed according to the proportion, mixed and prepared into an alloy strip, and the strip is ground and then ball-milled to prepare the soft magnetic material with the planar anisotropy and the flake form.
3. The method for preparing a planar anisotropic soft magnetic material according to claim 2, wherein the raw materials are mixed and then melted into a metal ingot with uniform composition, and the metal ingot is crushed into small pieces and then prepared into an alloy strip.
4. A method for the production of a planar anisotropic soft magnetic material according to claim 2 or 3, wherein the alloy strip is produced using a strip casting machine, wherein the copper roll speed is 30-55m/s and the strip casting vacuum is (4-6) × 10-3Pa。
5. A method of manufacturing a planar anisotropic soft magnetic material according to claim 2, wherein the ribbon is ball milled after being milled to below 125 μm.
6. A method for preparing a planar anisotropic soft magnetic material according to claim 2 or 5, wherein the ball milling conditions are as follows: the ball-material ratio is 1 (65-75), the ball milling time is 24-96h, and oleic acid accounting for 1-10% of the total mass of the balls and the materials is added as a dispersing agent.
7. The method for preparing a planar anisotropic soft magnetic material according to claim 6, wherein the ball milling time is 48 to 72 hours.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202111535658.9A CN114628104A (en) | 2021-12-15 | 2021-12-15 | Planar anisotropic soft magnetic material and preparation method thereof |
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| CN202111535658.9A CN114628104A (en) | 2021-12-15 | 2021-12-15 | Planar anisotropic soft magnetic material and preparation method thereof |
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2021
- 2021-12-15 CN CN202111535658.9A patent/CN114628104A/en not_active Withdrawn
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Application publication date: 20220614 |