CN114156037A - Iron-silicon-chromium soft magnetic powder material - Google Patents
Iron-silicon-chromium soft magnetic powder material Download PDFInfo
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- 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
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- 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
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- 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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Abstract
The preparation method of the iron-silicon-chromium soft magnetic powder material comprises the following steps: (1) atomizing to prepare powder; (2) passivating; (3) and (6) granulating. The powder of the invention has fine and uniform granularity, and the magnetic conductivity mu of the prepared magnetic ring samplei[25℃]The inductance change of more than 35, 100kHz and 2000kHz is small, the insulation impedance is more than 3G omega, no crack exists, and the performance is excellent; in practical application of products, the device can be used at a very wide higher frequency; the invention can produce the gas atomized powder of the integrally formed inductance sample with high insulating property in large scale by a low-cost production mode.
Description
Technical Field
The invention relates to a soft magnetic powder material, in particular to an iron-silicon-chromium soft magnetic powder material.
Background
The iron-silicon-chromium powder on the market at present has the magnetic conductivity of 20-120, but the insulation impedance performance is low, so that the defects of low inductance, low energy conversion efficiency, poor stacking performance and the like can be caused in the use process of a product manufactured by using the iron powder core.
CN110148509A discloses a high-reliability Fe-Si-Cr-FeSiCr integrated inductance granule and a preparation method thereof, wherein the granule is made of FeSiCr insulating alloy powder, nano BN and nano SiO2The composite modified E20 epoxy resin is organically combined with two heating curing type latent curing agents with high temperature (not less than 80 ℃) and low temperature (near 50 ℃), and the composite modified E20 epoxy resin is prepared by baking for 60-80 minutes at 50-70 ℃; the granule prepared by the method has long storage time: the effective period is more than 180 days under the environment of lower than 30 ℃, more than 60 days under the environment of 30 ℃ to 35 ℃, the magnetic conductivity is 27 +/-2, the insulation resistance is more than or equal to 1G omega, and the prepared product has no crack, bright and clean appearance, flatness and uniform texture. However, the added coating agent and curing agent are more, so that the magnetic conductivity of the water-gas combined atomized powder is low, and the loss of the atomized powder is large.
CN105895290A discloses a preparation method of high-temperature-resistant magnetic powder, which is characterized in that iron, silicon and chromium are used as main materials, epoxy resin and phenolic resin are added, and then the formed product is cured through a reasonable baking and sintering process, the process steps are simple, the operability is strong, the production cost is low, and the obtained product not only has excellent electromagnetic properties, but also has excellent high-temperature resistance, and can be used in a high-temperature environment of 190 ℃. But its coating insulation performance is poor.
CN1516204 discloses a method for manufacturing soft magnetic inductance iron core from sendust powder. The method comprises the following steps: smelting of iron-silicon-aluminum alloy, coarse crushing of iron-silicon-aluminum alloy ingots, heat treatment, fine crushing of iron-silicon-aluminum alloy ingots into alloy powder, annealing treatment, granularity proportioning, passivation treatment, addition of insulating agents, bonding agents and release agents into the alloy powder, compression molding, heat treatment and surface coating, and is characterized in that: the adhesive added after the passivation treatment is epoxy adhesive; and tempering after compression molding, namely preserving the temperature of the molded alloy powder core for at least 30 minutes in a nitrogen, argon or vacuum environment at 600-800 ℃. The method has small influence on the magnetic performance, and the manufactured soft magnetic powder core is not pulverized, cracked and high in mechanical strength, has good alternating current and direct current superposed dropping performance, but has low insulation resistance performance.
The FeSiAl alloy powder is introduced into CN103214233A, and although the saturation magnetic induction density Bs of the material can be effectively improved, the magnetic permeability of the invented material is not high, and the temperature-pressure performance and the insulation characteristic are not mentioned.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects in the prior art and provide the iron-silicon-chromium soft magnetic powder, the material has small inductance change at the frequency of 100kHz and 2000kHz, and the output stability of the inductor can be improved.
The technical scheme adopted by the invention for solving the technical problems is as follows: the preparation method of the iron-silicon-chromium soft magnetic powder material comprises the following steps:
(1) gas atomization powder preparation: smelting raw materials of iron-silicon-chromium soft magnetic alloy powder to obtain alloy liquid; under the protection of nitrogen, preparing Fe-Si-Cr magnetically soft alloy powder by a gas atomization method;
(2) passivation: preparing a passivator by taking aluminum dihydrogen phosphate as a passivator main agent and taking a mixed solution of distilled water and acetone as a diluent; passivating the Fe-Si-Cr magnetically soft alloy powder by using the passivating agent, filtering out passivated Fe-Si-Cr magnetically soft alloy powder, and blowing the passivated Fe-Si-Cr magnetically soft alloy powder to be semi-dry by using high-pressure air;
(3) and (3) granulation: drying the semi-dry Fe-Si-Cr magnetically soft alloy powder to obtain dry Fe-Si-Cr magnetically soft alloy powder; adding a mixed solution of modified epoxy resin and phenolic resin into the dried Fe-Si-Cr magnetically soft alloy powder for granulation; screening out 50-350 meshes of particles, baking, cooling to room temperature along with a furnace, adding a lubricant, and uniformly mixing to obtain the Fe-Si-Cr soft magnetic powder material.
Preferably, in the step (1), the raw materials of the fe-si-cr magnetically soft alloy powder are: 4.5-6.5 parts of pure chromium, 2-6.5 parts of pure silicon, 0.3-1.5 parts of calcium silicate powder, 0.8-2.5 parts of calcium oxide, 0.05-0.1 part of aluminum nitride and 87.5-91.5 parts of industrial pure iron.
Preferably, in the step (1), the pure chromium, the pure silicon and the industrial pure iron are divided into two parts during smelting, one part of the pure chromium, the pure silicon and the iron are added at the bottom of the furnace, and the other part of the pure chromium, the pure silicon and the iron are added during the cleaning process; controlling the temperature of the molten steel to be 1620-1750 ℃, reducing the heating power, adding calcium silicate powder, calcium oxide and aluminum nitride, slagging, removing slag and purifying to obtain the alloy liquid.
Preferably, in the step (1), the gas atomization method uses low-pressure vortex gas as an atomization medium, and the pressure is 0.4-0.85 MPa.
The gas atomization method is a common preparation method of metal and alloy powder: the alloy liquid flows into a spray chamber, is sent into an atomizing tower to initially form larger metal molten drops, then acts on the larger metal molten drops through an atomizing medium, and strongly crushes the larger metal molten drops into a large amount of fine metal molten drops, and then is solidified into iron-silicon-chromium soft magnetic alloy spherical or subsphaeroidal powder under the action of surface tension in the precipitation cooling process.
Preferably, in the step (2), the diluent consists of distilled water and acetone in a volume ratio of 1: 0.8-1.2.
Preferably, in the step (2), the time of the passivation treatment is 20-60 min.
Preferably, in the step (2), the volume ratio of the main passivating agent to the diluent is 100: 5-10.
Preferably, in the step (2), the mass ratio of the main passivating agent to the Fe-Si-Cr magnetically soft alloy powder is 0.4-2: 100.
Preferably, in the step (3), the solvent of the mixed solution of the modified epoxy resin and the phenolic resin is acetone.
Preferably, in the step (3), the mass ratio of the modified epoxy resin to the Fe-Si-Cr magnetically soft alloy powder is 1.5-3.5: 100.
Preferably, in the step (3), the mass ratio of the phenolic resin to the iron-silicon-chromium magnetically soft alloy powder is 1-2: 100.
Preferably, in the step (3), the drying temperature is 100-150 ℃ and the drying time is 20-60 min.
Preferably, in the step (3), the baking temperature is 50-80 ℃, and the baking time is 60-120 min.
Preferably, in the step (3), the lubricant is nano magnesium stearate, and the mass of the nano magnesium stearate is 0.05-0.2 wt% of the mass of the granules.
The iron-silicon-chromium powder has excellent antirust performance, high saturation magnetic induction intensity, low loss characteristic and the like, and is widely applied to integrally formed inductors. The gas atomized iron-silicon-chromium powder has lower loss and better saturation characteristics, and good sphericity to ensure better insulation reliability of the integral inductor. The gas atomization powder preparation process has the performances of accurate component control, stable particle size distribution and the like.
The addition of Si and Cr in Fe can raise the resistivity of the material and thus reduce the loss Pe caused by eddy current. The invention obtains higher insulation resistance value and Bs value by increasing the content of Fe/Cr and reducing the content of Si, and the contents of Fe, Si and Cr are also needed to be matched and adjusted to realize the invention because certain excellent temperature and pressure performance needs to be kept. The contents of Fe, Si and Cr in the invention can simultaneously meet the requirements of high Bs, high insulation resistance, broadband performance and the like; when the Fe content is below the range of the present invention, Bs will be below 900 mT. When the content of Fe is higher than the range of the present invention, the insulation resistance is much lower than 1G Ω, so Bs and high resistance performance cannot be considered at the same time. When the Si content is 4.5 to 8.5 wt%, the resistivity of the material can reach 3G omega cm, and the resistivity can be further increased by further increasing the Si content, but the Ms of the material is also reduced, but the material becomes extremely brittle. When the Cr content is 3-7.5 wt%, the resistivity of the material can reach 3G omega cm, and the Ms of the material can be greatly reduced although the resistivity can be further increased by further increasing the Cr content.
The sintering of the Fe-Si-Cr alloy is performed completely in the ferrite phase region to grow ferrite grains, which contributes to lowering Hc and increasing μm. The magnetic performance can be further improved (about 10%) by using the modified epoxy resin process for coating. Because of high Bm and low Hc, the Fe-Si-Cr powder sintered soft magnet is very suitable for being applied to occasions requiring low iron loss Pc under an alternating current magnetic circuit or pulse current, and the working frequency can be from tens of kHz to thousands of kHz. The coating compounds have higher resistivity and are tightly combined with the base metal, can be continuously used as insulating coating layers, and the coated magnetic powder core has better high-frequency magnetic permeability and high insulating property. The Fe-Si-Cr soft magnetic powder can be used as a raw material of a miniature inductor or an integrally formed inductor.
The invention has the beneficial effects that:
(1) the powder of the invention has fine and uniform granularity;
(2) magnetic permeability mu of magnetic ring sample made of iron-silicon-chromium soft magnetic powder materiali[25℃]The inductance change of more than 35, 100kHz and 2000kHz is small, the insulation impedance is more than 3G omega, no crack exists, and the performance is excellent; in practical application of products, the device can be used at a very wide higher frequency;
(3) the invention can produce the gas atomized powder of the integrally formed inductance sample with high insulating property in large scale by a low-cost production mode.
Drawings
FIG. 1 is a diagram of the morphology of Fe-Si-Cr magnetically soft alloy powder prepared by a gas atomization method in example 1 of the present invention.
Detailed Description
The present invention will be further described with reference to the following examples and the accompanying drawings.
The starting materials used in the examples of the present invention were all obtained from conventional commercial sources.
The present invention is further illustrated by the following examples, which should not be construed as limiting the scope of the invention.
Unless otherwise specified, the chemical reagents used in the examples of the present invention were all commercially available in a conventional manner.
Example 1
The preparation method of the iron-silicon-chromium soft magnetic powder comprises the following steps:
(1) gas atomization powder preparation
Adding a raw material of iron-silicon-chromium soft magnetic alloy powder into a smelting crucible containing a medium-frequency induction furnace, and smelting to obtain an alloy liquid; under the protection of nitrogen, feeding the alloy liquid into an atomizing tower, preliminarily forming larger metal molten drops in the atomizing tower, acting low-pressure vortex gas with the pressure of 0.5MPa as an atomizing medium on the alloy liquid, strongly crushing the alloy liquid into a large number of fine metal molten drops, and then cooling and solidifying the fine metal molten drops into iron-silicon-chromium soft magnetic alloy powder; the morphology of the resulting aerosolized powder is shown in FIG. 1;
the iron-silicon-chromium soft magnetic alloy powder comprises the following raw materials in percentage by mass: 89 parts of industrial pure iron, 4.5 parts of pure silicon, 6.5 parts of pure chromium, 0.65 part of calcium silicate powder, 1.5 parts of calcium oxide and 0.08 part of aluminum nitride;
during smelting, dividing pure chromium, pure silicon and industrial pure iron into two parts, adding one part of pure chromium, pure silicon and iron at the bottom of the furnace, and adding the other part of pure chromium, pure silicon and iron in the process of clearing; controlling the temperature of the molten steel within the range of 1620-1750 ℃, reducing the heating power, adding calcium silicate powder, calcium oxide and aluminum nitride, slagging, removing slag and purifying to obtain an alloy liquid;
the alloy liquid is slowly poured into a tundish crucible, flows into a spray chamber through a current-limiting liquid guide pipe, is sent into an atomization tower, and then acts on the larger metal molten drops through an atomization medium of low-pressure vortex gas, the larger metal molten drops are powerfully crushed into a large number of small metal molten drops, and then the molten drops are solidified into iron-silicon-chromium soft magnetic alloy spherical or subsphaeroidal powder under the action of surface tension in the process of precipitation and cooling; the alloy powder has the following element composition: 89 wt% Fe, 4.5 wt% Si, 6.5 wt% Cr.
(2) Passivation of
Aluminum dihydrogen phosphate is used as a main agent of a passivator, and a mixed solution (1:1) of distilled water and acetone is used as a diluent to prepare the passivator; passivating the Fe-Si-Cr soft magnetic alloy powder for 40min, filtering out the passivated Fe-Si-Cr soft magnetic alloy powder, and blowing the powder to be semi-dry by high-pressure air; the volume ratio of the main passivator agent to the diluent is 100:5, and the dosage ratio of the main passivator agent to the Fe-Si-Cr soft magnetic alloy powder is 1: 100;
(3) granulating
Drying at 120 ℃ for 30min to dry the semi-dry Fe-Si-Cr magnetically soft alloy powder to obtain dry Fe-Si-Cr magnetically soft alloy powder; adding a mixed solution of modified epoxy resin and phenolic resin into the dried Fe-Si-Cr magnetically soft alloy powder for granulation; screening out 50-350-mesh particles, baking for 90min at 70 ℃, cooling to room temperature along with a furnace, adding nano magnesium stearate accounting for 0.15 wt% of the mass of the particles as a lubricant, and uniformly mixing to obtain the Fe-Si-Cr soft magnetic powder material; the mass of the mixed solution of the modified epoxy resin and the phenolic resin is 3.0 wt% of the dry iron-silicon-chromium magnetically soft alloy powder, the solvent of the mixed solution of the modified epoxy resin and the phenolic resin is acetone, and the mass ratio of the modified epoxy resin to the iron-silicon-chromium magnetically soft alloy powder is 1.8: 100, the mass ratio of the phenolic resin to the FeSiCr magnetically soft alloy powder is 1.2: 100, and the mass ratio of the nano magnesium stearate to the FeSiCr magnetically soft alloy powder is 0.15: 100 as the lubricant.
Through detection, the apparent density of the Fe-Si-Cr soft magnetic powder material obtained in the embodiment is 2.67g/cm3Tap density of 4.2g/cm3The particle size distribution is D50: 10-22 μm, D90: 35-56 mu m, oxygen content less than 1500ppm, and pressing the green body under 400-600 MPa, wherein the annular inductance density is 6.15g/cm3。
The preparation methods of the examples 2 to 8 and the comparative examples 1 to 14 are basically the same as the example 1, and the differences are that the raw material proportion and the passivation and granulation process formula are different: some of the parameters selected in comparative examples 1 to 14 were too large or too small relative to the present invention. The details are shown in tables 1 and 2:
TABLE 1 raw materials for gas atomized powders of examples 1 to 8 and comparative examples 1 to 14
TABLE 2 powder compositions and passivation and granulation process recipes for examples 1-8 and comparative examples 1-14
The finished powders of the examples and comparative examples were prepared into test specimens and tested for performance:
1) warm-pressing and forming: respectively weighing 2.1g of powder, and pressing a magnetic ring green body sample with the outer diameter of 14mm and the inner diameter of 8mm under the pressure condition of 400-600 MPa;
2) baking: baking the sample at 160 ℃ for 180min, and cooling the sample to room temperature along with the furnace;
3) and (3) performance testing: and (3) carrying out inductance and Q value testing on the sample ring subjected to baking treatment by using an Agilent E4991A LCR tester of Agilent. The test conditions were respectively: testing inductance under the conditions that f is 100kHz, f is 2000kHz and u is 0.5v (power supply power is 50W) and converting the inductance into magnetic permeability; measuring inductance and Q value of the baked magnetic ring with the outer diameter 14 and the inner diameter 8 by Agilent E4991A at each frequency, and calculating magnetic permeability mu of the samplei[25℃]Using a Chroma 19053 insulation tester to detect the insulation resistance of a square sample DR4 multiplied by 1.5 mm; selecting a square sample DR4 multiplied by 1.5mm after baking after warm pressing and 50 test reliability tests, and recording the cracking number of 200 hours under the statistical test; results for each group are the average of 5 replicates. The results of the performance tests are shown in table 3.
TABLE 3 table of properties of test samples of examples 1-8 and comparative examples 1-14
As can be seen from Table 3, the magnetic ring sample prepared from the Fe-Si-Cr soft magnetic powder material obtained in the embodiment of the invention has magnetic permeability mui[25℃]: the inductance change of more than 35, 100kHz and 2000kHz is small, the insulation resistance is more than 3G omega, and the magnetic ring is not cracked, and is obviously superior to the magnetic ring sample prepared from the powder obtained by the comparative example.
Claims (10)
1. The Fe-Si-Cr soft magnetic powder material is characterized in that the preparation method comprises the following steps:
(1) gas atomization powder preparation: smelting raw materials of iron-silicon-chromium soft magnetic alloy powder to obtain alloy liquid; under the protection of nitrogen, preparing Fe-Si-Cr magnetically soft alloy powder by a gas atomization method;
(2) passivation: preparing a passivator by taking aluminum dihydrogen phosphate as a passivator main agent and taking a mixed solution of distilled water and acetone as a diluent; passivating the Fe-Si-Cr magnetically soft alloy powder by using the passivating agent, filtering out passivated Fe-Si-Cr magnetically soft alloy powder, and blowing the passivated Fe-Si-Cr magnetically soft alloy powder to be semi-dry by using high-pressure air;
(3) and (3) granulation: drying the semi-dry Fe-Si-Cr magnetically soft alloy powder to obtain dry Fe-Si-Cr magnetically soft alloy powder; adding a mixed solution of modified epoxy resin and phenolic resin into the dried Fe-Si-Cr magnetically soft alloy powder for granulation; screening out 50-350 meshes of particles, baking, cooling to room temperature along with a furnace, adding a lubricant, and uniformly mixing to obtain the Fe-Si-Cr soft magnetic powder material.
2. The Fe-Si-Cr soft magnetic powder material according to claim 1, wherein in the step (1), the Fe-Si-Cr soft magnetic alloy powder comprises the following raw materials: 4.5-6.5 parts of pure chromium, 2-6.5 parts of pure silicon, 0.3-1.5 parts of calcium silicate powder, 0.8-2.5 parts of calcium oxide, 0.05-0.1 part of aluminum nitride and 87.5-91.5 parts of industrial pure iron.
3. The Fe-Si-Cr soft magnetic powder material according to claim 1 or 2, wherein in the step (1), pure Cr, pure Si and industrial pure Fe are divided into two parts during smelting, one part of pure Cr, pure Si and Fe is added at the bottom of the furnace, and the other part of pure Cr, pure Si and Fe is added during the cleaning process; controlling the temperature of the molten steel to be 1620-1750 ℃, reducing the heating power, adding calcium silicate powder, calcium oxide and aluminum nitride, slagging, removing slag and purifying to obtain the alloy liquid.
4. The Fe-Si-Cr soft magnetic powder material according to any one of claims 1 to 3, wherein in the step (1), the gas atomization method uses low-pressure vortex gas as an atomization medium, and the pressure is 0.4-0.85 MPa.
5. The Fe-Si-Cr soft magnetic powder material according to any one of claims 1 to 4, wherein in the step (2), the diluent consists of distilled water and acetone in a volume ratio of 1: 0.8-1.2; the time of the passivation treatment is 20-60 min.
6. The Fe-Si-Cr soft magnetic powder material according to any one of claims 1 to 5, wherein in the step (2), the volume ratio of the main passivating agent to the diluent is 100: 5-10; the mass ratio of the main agent of the passivating agent to the Fe-Si-Cr magnetically soft alloy powder is 0.4-2: 100.
7. The Fe-Si-Cr soft magnetic powder material according to any one of claims 1 to 6, wherein in the step (3), a solvent of a mixed solution of the modified epoxy resin and the phenolic resin is acetone.
8. The Fe-Si-Cr soft magnetic powder material according to any one of claims 1 to 7, wherein in the step (3), the mass ratio of the modified epoxy resin to the Fe-Si-Cr soft magnetic alloy powder is 1.5-3.5: 100; the mass ratio of the phenolic resin to the iron-silicon-chromium soft magnetic alloy powder is 1-2: 100.
9. The Fe-Si-Cr soft magnetic powder material according to any one of claims 1 to 8, wherein in the step (3), the temperature for drying is 100 to 150 ℃ and the time is 20 to 60 min; the baking temperature is 50-80 ℃, and the baking time is 60-120 min.
10. The Fe-Si-Cr soft magnetic powder material according to any one of claims 1 to 9, wherein in the step (3), the lubricant is nano magnesium stearate, and the used mass is 0.05 to 0.2 wt% of the mass of the particles.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115050566A (en) * | 2022-07-19 | 2022-09-13 | 横店集团东磁股份有限公司 | Iron-silicon-chromium soft magnetic composite material for injection molding and preparation method thereof |
| CN116100016A (en) * | 2023-03-27 | 2023-05-12 | 西南应用磁学研究所(中国电子科技集团公司第九研究所) | Method for preparing iron-silicon-chromium soft magnetic metal powder and application of prepared soft magnetic metal powder |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115050566A (en) * | 2022-07-19 | 2022-09-13 | 横店集团东磁股份有限公司 | Iron-silicon-chromium soft magnetic composite material for injection molding and preparation method thereof |
| CN116100016A (en) * | 2023-03-27 | 2023-05-12 | 西南应用磁学研究所(中国电子科技集团公司第九研究所) | Method for preparing iron-silicon-chromium soft magnetic metal powder and application of prepared soft magnetic metal powder |
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