CN107452458B - Iron alloy magnetic material and preparation method thereof - Google Patents
Iron alloy magnetic material and preparation method thereof Download PDFInfo
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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
- H01F1/147—Alloys characterised by their composition
- H01F1/14766—Fe-Si based alloys
- H01F1/14791—Fe-Si-Al based alloys, e.g. Sendust
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
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- C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
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- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/34—Ferrous alloys, e.g. steel alloys containing chromium with more than 1.5% by weight of silicon
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F27/00—Details of transformers or inductances, in general
- H01F27/24—Magnetic cores
- H01F27/255—Magnetic cores made from particles
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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
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Abstract
The invention discloses a ferroalloy magnetic material and a preparation method thereof, wherein the raw materials for preparing the ferroalloy magnetic material comprise the following simple substance components in percentage by mass: 85.5 to 93.0 percent of Fe, 3.0 to 6.5 percent of Cr, 3.0 to 7.0 percent of Al3, 0.5 to 2.0 percent of Si and 0.1 to 0.8 percent of Mn. The preparation method comprises the following steps: (1) mixing: mixing the raw materials of the iron alloy magnetic material, the process control agent and the grinding balls; (2) ball milling: performing ball milling in a protective atmosphere to obtain alloy powder; (3) and (3) granulation: adding an organic solvent and resin into the powder, continuing ball milling to obtain slurry, drying the slurry, crushing, and sieving to obtain the ferroalloy magnetic material. The obtained iron alloy magnetic material has uniform components, high strength and high insulation property, and meets the requirements of power inductance on the strength and the insulation property of a magnetic core.
Description
Technical Field
The invention relates to the technical field of ferroalloy materials, in particular to a ferroalloy magnetic material and a preparation method thereof.
Background
At present, ferroalloy magnetic materials are widely applied to electronic products, and along with the rapid development of the electronic industry, the requirements of fast-consumption intelligent terminal products on processing speed and capacity enable the densification of circuits to be a necessary trend, which directly leads to the development of inductance type components in the direction of small size, and the strength problem caused by the miniaturization of the products is one of the key points of inductance application; meanwhile, the alloy power inductor generally adopts the process modes of Ag termination, Ni electroplating and Sn plating to realize the manufacture of subsequent products, and if the surface insulation property of the material is poor in the electroplating process, the creeping plating phenomenon can occur in the electroplating process, so that the development of the material with high insulation property plays an important role in the development of the products needing to be subjected to the electroplating treatment process.
The existing magnetic alloy materials mainly used mainly comprise Fe-Si, FeSiAl, FeSiCr, FeNi, FeNiMo and the like, but the Fe-Si, FeSiAl, FeSiCr, Fe-Ni and the like have poor strength or insulation performance after heat treatment, although the magnetic permeability is high, the mechanical reliability problem is easy to exist in the using process, or the Fe-Ni and the like cannot be directly used for relevant electroplating treatment, so that the development of the iron alloy magnetic material with high strength and high insulation performance is necessary.
Disclosure of Invention
The invention provides a ferroalloy magnetic material and a preparation method thereof, wherein the ferroalloy magnetic material has high strength and high insulation property and meets the requirements of power inductance on the strength and the insulation property of a magnetic core.
The invention adopts the following technical scheme:
a raw material for preparing the iron alloy magnetic material comprises the following elementary substance components in percentage by mass: 85.5 to 93.0 percent of Fe, 3.0 to 6.5 percent of Cr, 3.0 to 7.0 percent of Al, 0.5 to 2.0 percent of Si and 0.1 to 0.8 percent of Mn0.
Preferably, in the raw material, the mass percentage of Si is 0.5% -1.0%.
Preferably, in the raw materials, the mass percent of Mn is 0.1% -0.5%.
Preferably, the average particle diameters of Fe, Cr, Al, Si and Mn in the raw materials are 5 to 20 μm, 5 to 15 μm, 10 to 30 μm, 3 to 15 μm and 2 to 15 μm, respectively.
A preparation method of the iron alloy magnetic material comprises the following steps:
(1) mixing: mixing the raw materials for preparing the ferroalloy magnetic material, a process control agent and grinding balls, wherein the addition amount of the process control agent is 0.5-3 wt% of the weight of the raw materials, and the mass ratio of powder to the grinding balls is 1:8-1: 20;
(2) ball milling: performing ball milling in a protective atmosphere to obtain alloy powder;
(3) and (3) granulation: adding an organic solvent and resin into the powder, continuing ball milling to obtain slurry, wherein the addition amount of the organic solvent is enough to disperse the powder, the addition amount of the resin is 2-10 wt% of the weight of the powder, drying the slurry, crushing, and sieving to obtain the ferroalloy magnetic material.
Preferably, in the step (1), the grinding balls are a mixture of small balls with the diameter of 1-4mm and large balls with the diameter of 5-10mm, and the mass ratio of the small balls to the large balls is 4: 1-2: 1.
Preferably, in the step (2), the rotation speed of the ball milling is 350-500rpm, and the ball milling time is 40-80 h.
Preferably, in the step (3), the screening is performed by using a 60-300 mesh screen.
Preferably, in step (1), the process control agent is ethanol; in the step (3), the organic solvent is at least one of ethanol, acetone and butanone; in the step (3), the resin is at least one of epoxy resin, furfural resin, polyvinyl alcohol and silicon resin.
An inductor is prepared from the iron alloy magnetic material.
The beneficial effects of the invention include: the iron alloy magnetic material has uniform components, has the characteristics of high strength (not less than 200MPa) and high insulation (more than 500M omega), and can meet the requirements of power inductance on the strength and the insulation performance of a magnetic core.
Drawings
Fig. 1 is an XRD pattern of a ferroalloy magnetic material obtained in a manufacturing process according to an embodiment of the present invention.
Detailed Description
The invention will be further described with reference to the accompanying drawings and preferred embodiments. It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict.
The invention provides a ferroalloy magnetic material, and in a specific embodiment, raw materials for preparing the ferroalloy magnetic material comprise the following elementary substance components in percentage by mass: 85.5 to 93.0 percent of Fe, 3.0 to 6.5 percent of Cr3, 3.0 to 7.0 percent of Al3, 0.5 to 2.0 percent of Si and 0.1 to 0.8 percent of Mn.
In a preferred embodiment, one or more of the following schemes may also be used in combination:
in the raw materials, the mass percent of Si is 0.5-1.0%.
In the raw materials, the mass percent of Mn is 0.1-0.5%.
In the raw materials, the average grain diameters of Fe, Cr, Al, Si and Mn are respectively 5-20 μm, 5-15 μm, 10-30 μm, 3-15 μm and 2-15 μm.
The formulations (in g) of the iron alloy magnetic materials in preferred examples 1 to 4 and comparative examples 1 to 2 of the present invention are illustrated below in the form of tables.
Table 1:
| elemental composition | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Comparative example 1 | Comparative example 2 |
| Fe | 91.9 | 91.7 | 92.5 | 86.8 | 87 | 87.3 | 92.4 |
| Cr | 4.5 | 3.5 | 3.0 | 5.0 | 6.5 | 5.5 | 5.0 |
| Al | 3.0 | 4.0 | 3.5 | 7.0 | 5.0 | 4.5 | 2.0 |
| Si | 0.5 | 0.6 | 0.7 | 0.8 | 1.0 | 2.2 | 0.4 |
| Mn | 0.1 | 0.2 | 0.3 | 0.4 | 0.5 | 0.5 | 0.2 |
The invention also provides a preparation method of the iron alloy magnetic material, which comprises the following steps:
(1) mixing: mixing the raw materials for preparing the ferroalloy magnetic material, a process control agent and grinding balls, wherein the addition amount of the process control agent is 0.5-3 wt% of the weight of the raw materials, and the mass ratio of powder to the grinding balls is 1:8-1: 20;
(2) ball milling: performing ball milling in a protective atmosphere to obtain alloy powder;
(3) and (3) granulation: adding an organic solvent and resin into the powder, fully ball-milling and mixing to obtain slurry, wherein the addition amount of the organic solvent is enough to disperse the powder, the addition amount of the resin is 2-10 wt% of the weight of the powder, drying the slurry, crushing, and sieving to obtain the ferroalloy magnetic material.
In a preferred embodiment, one or more of the following schemes may also be used in combination:
in the step (1), grinding balls are a mixture of small balls with the diameter of 1-4mm and large balls with the diameter of 5-10mm, and the mass ratio of the small balls to the large balls is 4: 1-2: 1; the grinding balls can be made of zirconia or hard steel balls, and the process control agent is added in the mixing process to reduce the wall sticking phenomenon of the ball mill, so that the ball milling efficiency is improved.
In the step (2), the rotation speed of ball milling is 350-500rpm, and the ball milling time is 40-80 h; the protective atmosphere may be N2Or other inert gas such as Ar.
In the step (3), a sieve with 60-300 meshes is adopted for sieving.
In the step (1), the process control agent is ethanol.
In the step (3), the organic solvent is at least one of ethanol, acetone and butanone.
In the step (3), the resin is at least one of epoxy resin, furfural resin, polyvinyl alcohol and silicon resin.
Wherein, the raw material is also powder, but the average grain diameter of the alloy powder obtained after ball milling in the step (2) is smaller than that of the raw material, for example, the average grain diameter of the added raw material Fe is 5-20 μm, and the average grain diameter is less than 5 μm after ball milling.
In the granulation in the step (3), the adding sequence of the organic solvent and the resin is not limited, for example, the organic solvent may be added first for ball milling and mixing for 30-60min, and then the resin is added for ball milling and mixing for 30-90min, or the resin is added first for ball milling and mixing, then the organic solvent is added for ball milling and mixing, or the organic solvent and the resin are added simultaneously and then ball milling and mixing for 60-150min, and the ball milling speed in the step is also between 350 and 500 rpm.
The drying in step (3) may be carried out by air drying, and then drying at 120-250 ℃.
The preparation is illustrated by way of example with the formulation of example 1 as follows:
(1) mixing: weighing the following simple substance raw material powders: 90.6g of Fe, 4.5 g of Cr, 4.0g of Al, 0.7g of Si and 0.2g of Mn (the mass is 100g in total), and the components required by ball milling are weighed according to the proportion of ball materials
And
the zirconia balls (ball-to-material ratio is 10:1, mass ratio of large zirconia balls to small zirconia balls is 1:3) are mixed and put into a ball milling pot, and 2 wt% (2g) of absolute ethyl alcohol is dripped as a process control agent.
(2) Vacuumizing the ball milling tank, and introducing N2And (3) serving as ball milling protective atmosphere, then placing the mixture in a planetary ball mill for ball milling, setting the ball milling rotation speed and the ball milling time to be 400rpm and 50h respectively, and taking out the alloy powder after the ball milling tank is completely cooled.
(3) And (3) granulation: mixing the alloy powder obtained by ball milling with absolute ethyl alcohol, placing the mixture in a ball milling tank for mixing for 30min, then adding 8 wt% (namely 8g) of epoxy resin, continuing ball milling for 1h, filtering out zirconia balls, placing the slurry in air for air drying, placing the slurry in an oven for further drying after drying, and selecting the temperature to be 200 ℃; and after the powder is completely dried, crushing the powder and sieving the powder by using a 60-300-mesh sieve to obtain the iron alloy magnetic material. As shown in fig. 1, which is an XRD pattern of the alloy powder obtained during ball milling, wherein curve 2 is the alloy powder obtained after ball milling for 10h (wherein a is the peak of Fe), and curve 1 is the alloy powder obtained after ball milling for 50h, the disappearance of the peak (as shown by the dotted circle) and the decrease and broadening of the peak intensity appear in curve 1, compared to curve 2, which indicates that the alloying effect appears when the elements such as Cr and Al enter the crystal lattice of Fe metal after ball milling for 50 h.
In order to test the properties of the iron alloy magnetic materials, the iron alloy magnetic materials of the above examples and comparative examples were press-molded into magnetic rings or magnetic strips using a powder molding press with a pressing density controlled at 5.6g/cm3～6.0g/cm3In between (6.0 g/cm in this example)3) The size of the pressed magnetic ring is 8.0mm 5.0mm 2.0mm in Outside Diameter (OD) and Inside Diameter (ID), and the size of the pressed magnetic strip is 8.0mm 5.0mm 2.0mm in length (L) × width (b) × mm height (h) 32mm 4mm 3 mm.
In this example, the performance of a sintered FeCrAlSiMn magnetic ring was evaluated, the number of winding turns N was 26Ts turns, and the initial permeability of the magnetic ring sample was tested using a 3260B LCR tester; testing the insulation and voltage resistance of a sample by using a CH-333 type insulation voltage resistance tester for an electronic universal tester; the samples were tested for spectral characteristics using E4991A. The performance ratios of the examples and comparative examples are shown in table 2 below:
TABLE 2
| Test items | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Comparative example 1 | Comparative example 2 |
| Magnetic permeability | 52 | 53 | 50 | 50 | 51 | 46 | 48 |
| Insulation (M omega) | 675 | 650 | 600 | 513 | 520 | 450 | 87 |
| Withstand voltage (V) | 506 | 500 | 480 | 426 | 435 | 300 | 108 |
| Strength (MPa) | 213 | 208 | 200 | 225 | 230 | 160 | 137 |
The strength and the electromagnetic property of the materials obtained by comparing the examples and the comparative examples show that the comprehensive properties of the materials obtained by the examples are better than those of the comparative examples: the magnetic permeability mu of the material (FeCrAlSiMn alloy material) in the embodiment is 50 +/-8%, the insulation is more than 500M omega, the withstand voltage is more than 400V, and the strength can reach more than 200 MPa.
The foregoing is a more detailed description of the invention in connection with specific preferred embodiments and it is not intended that the invention be limited to these specific details. To those skilled in the art to which the invention relates, numerous changes, substitutions and alterations can be made without departing from the spirit of the invention, and these changes are deemed to be within the scope of the invention as defined by the appended claims.
Claims (10)
1. The ferroalloy magnetic material is characterized in that raw materials for preparing the ferroalloy magnetic material comprise the following simple substance components in percentage by mass: 85.5 to 93.0 percent of Fe, 3.0 to 6.5 percent of Cr, 3.0 to 7.0 percent of Al, 0.5 to 2.0 percent of Si and 0.1 to 0.8 percent of Mn; the ferroalloy magnetic material is prepared by the following steps:
(1) mixing: mixing a raw material of a ferroalloy magnetic material, a process control agent and a grinding ball, wherein the addition amount of the process control agent is 0.5-3 wt% of the weight of the raw material, and the mass ratio of powder to the grinding ball is 1:8-1: 20;
(2) ball milling: performing ball milling in a protective atmosphere to obtain alloy powder;
(3) and (3) granulation: adding an organic solvent and resin into the powder, continuously performing ball milling to obtain slurry, wherein the addition amount of the organic solvent is enough to disperse the powder, the addition amount of the resin is 2-10 wt% of the weight of the powder, drying the slurry, crushing the dried slurry, and sieving the crushed slurry to obtain ferroalloy magnetic material powder;
(4) and pressing and molding the iron alloy magnetic material powder into a magnetic ring or a magnetic strip, and sintering the magnetic ring or the magnetic strip in the air, wherein the sintering temperature is controlled to be 700-750 ℃, and the heat preservation time is 100-200 min.
2. The iron alloy magnetic material as claimed in claim 1, wherein the raw material contains Si in an amount of 0.5 to 1.0% by mass.
3. The iron alloy magnetic material as claimed in claim 1 or 2, wherein the mass percentage of Mn in the raw material is 0.1-0.5%.
4. A ferrous alloy magnetic material as claimed in claim 1 or 2, characterized in that the average grain sizes of Fe, Cr, Al, Si and Mn in the raw material are 5 μm-20 μm, 5 μm-15 μm, 10 μm-30 μm, 3 μm-15 μm and 2-15 μm, respectively.
5. A method for producing a ferroalloy magnetic material according to any one of claims 1 to 4, comprising the steps of:
(1) mixing: mixing a raw material for preparing the iron alloy magnetic material according to any one of claims 1 to 4, a process control agent and grinding balls, wherein the addition amount of the process control agent is 0.5 to 3 weight percent of the weight of the raw material, and the mass ratio of powder to grinding balls is 1:8 to 1: 20;
(2) ball milling: performing ball milling in a protective atmosphere to obtain alloy powder;
(3) and (3) granulation: adding an organic solvent and resin into the powder, continuously performing ball milling to obtain slurry, wherein the addition amount of the organic solvent is enough to disperse the powder, the addition amount of the resin is 2-10 wt% of the weight of the powder, drying the slurry, crushing the dried slurry, and sieving the crushed slurry to obtain ferroalloy magnetic material powder;
(4) and pressing and molding the iron alloy magnetic material powder into a magnetic ring or a magnetic strip, and sintering the magnetic ring or the magnetic strip in the air, wherein the sintering temperature is controlled to be 700-750 ℃, and the heat preservation time is 100-200 min.
6. The method according to claim 5, wherein in the step (1), the grinding balls are a mixture of small balls with a diameter of 1-4mm and large balls with a diameter of 5-10mm, and the mass ratio of the small balls to the large balls is 4: 1-2: 1.
7. The preparation method according to claim 5, wherein in the step (2), the rotation speed of the ball mill is 350-500rpm, and the ball milling time is 40-80 h.
8. The method according to claim 5, wherein in the step (3), the sieving is performed by using a 60-300 mesh sieve.
9. The method of claim 5, wherein in step (1), the process control agent is ethanol; in the step (3), the organic solvent is at least one of ethanol, acetone and butanone; in the step (3), the resin is at least one of epoxy resin, furfural resin, polyvinyl alcohol and silicon resin.
10. An inductor produced from the iron alloy magnetic material according to any one of claims 1 to 4.
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| JPS6160807A (en) * | 1984-09-01 | 1986-03-28 | Fukuda Kinzoku Hakufun Kogyo Kk | Production of metallic powder having narrow width of grain size |
| CN1690242A (en) * | 2004-04-27 | 2005-11-02 | 宝山钢铁股份有限公司 | Soft magnetic structural-steel-plate with excellent toughness under low temperature and method for making same |
| CN102177268A (en) * | 2008-10-10 | 2011-09-07 | 株式会社丰田自动织机 | Iron alloy, iron alloy member and manufacturing method therefor |
| CN102732800A (en) * | 2012-06-10 | 2012-10-17 | 电子科技大学 | Fe-Ni-Cr soft magnetic alloy and preparation method thereof |
| CN104036900A (en) * | 2013-03-05 | 2014-09-10 | 大同特殊钢株式会社 | Soft Magnetic Metal Powder And Powder Core |
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| WO2002084676A1 (en) * | 2001-04-13 | 2002-10-24 | Mitsui Chemicals, Inc. | Magnetic core and magnetic core-use adhesive resin composition |
| JP5368686B2 (en) * | 2007-09-11 | 2013-12-18 | 住友電気工業株式会社 | Soft magnetic material, dust core, method for producing soft magnetic material, and method for producing dust core |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6160807A (en) * | 1984-09-01 | 1986-03-28 | Fukuda Kinzoku Hakufun Kogyo Kk | Production of metallic powder having narrow width of grain size |
| CN1690242A (en) * | 2004-04-27 | 2005-11-02 | 宝山钢铁股份有限公司 | Soft magnetic structural-steel-plate with excellent toughness under low temperature and method for making same |
| CN102177268A (en) * | 2008-10-10 | 2011-09-07 | 株式会社丰田自动织机 | Iron alloy, iron alloy member and manufacturing method therefor |
| CN102732800A (en) * | 2012-06-10 | 2012-10-17 | 电子科技大学 | Fe-Ni-Cr soft magnetic alloy and preparation method thereof |
| CN104036900A (en) * | 2013-03-05 | 2014-09-10 | 大同特殊钢株式会社 | Soft Magnetic Metal Powder And Powder Core |
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