CN103824670B - A kind of iron silica magnetic particle core and preparation method thereof - Google Patents
A kind of iron silica magnetic particle core and preparation method thereof Download PDFInfo
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- CN103824670B CN103824670B CN201410037762.9A CN201410037762A CN103824670B CN 103824670 B CN103824670 B CN 103824670B CN 201410037762 A CN201410037762 A CN 201410037762A CN 103824670 B CN103824670 B CN 103824670B
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Abstract
The invention discloses a kind of preparation method of iron silica magnetic particle core. The present invention adds micro-element Ni or Co on the basis of iron silicon, adopts aeroponics to prepare iron silica flour, and wherein Si accounts for 5～7%, Ni or Co accounts for 0.1～1.5%, and all the other are Fe; The present invention adopts permanganate to make passivator, and epoxy resin and phenolic resins mixture are made binding agent, and it is good that the iron silica magnetic particle core making has DC superposition characteristic, and magnetic loss is low, and iron silica magnetic particle core density is high, smooth surface, the features such as good moldability.
Description
Technical field
The invention belongs to soft magnetic materials technical field, be specifically related to a kind of iron silica magnetic particle core and preparation method thereof.
Background technology
Along with the continuous progress of science and technology, electronic product is to high accuracy, high sensitivity and large capacity, small-sizedThat changes will seek development, and the metal magnetic powder core being applied in all kinds of electronic products is also had higher requirement.Iron silica magnetic particle core is owing to adopting powder metallurgical technique to be prepared from, and its resistivity is far above alloy soft magnetics such as silicon steelMaterial, therefore its eddy-current loss is less, can work in upper frequency; Meanwhile, the DC stacked spy of its excellenceProperty and low-loss just filled up the space of ferrocart core and other alloy magnetic powder core.
At present, the preparation technology of ferro-silicium powder mainly contains three kinds of water atomization, aerosolization and mechanical crushing methods.Along with the increase of silicone content, there is alloy structure ordering in ferro-silicium, it is hard and crisp that alloy becomes, and makes machineProcessing characteristics sharply worsens, and is difficult to use conventional method roll forming. Water atomized powder is due to its out-of-shape,Surface irregularity, is difficult for being coated, inter-adhesive when powder corner angle morphological feature makes powder compaction again, insulationFilm is compared with destructible, and eddy-current loss is higher; Aerosolization powder particles is spherical in shape, and content of surface oxygen is few.
Chinese patent CN102294474B discloses the preparation side of a kind of iron silicon materials and u50 iron silica magnetic particle coreMethod, improves the magnetic property of alloy by adding a small amount of Nb and V. Nb and V element add main orderBe the growing up of tissue of suppressing ferro-silicium in heat treatment process, can not effectively improve iron silica magnetic particle coreDC superposition characteristic. The iron silicon that Chinese patent CN102360660A discloses a kind of magnetic conductivity u=50 closesGold powder core and preparation method thereof, employing phosphoric acid is passivator, is that binding agent makes magnetic conductance by phenolic resinsRate is 50 iron silica magnetic particle core. Because ferro-silicium powder is done in the process of passivator at employing phosphoric acid, meeting and phosphorusAcid reaction generates the oxide of red iron, and this red material is semiconductor, make powder particle and particle itBetween can not effectively keep apart, make its loss higher.
Summary of the invention
The object of this invention is to provide a kind of preparation method of iron silica magnetic particle core, the iron that utilizes the method to be prepared intoThe features such as it is good that silica magnetic particle core has DC superposition characteristic, and magnetic loss is low, good moldability, the present invention also provides and adoptsThe iron silica magnetic particle core obtaining by the method.
Above-mentioned purpose is achieved through the following technical solutions:
A preparation method for iron silica magnetic particle core, comprises the following steps:
1) get iron silica flour, add 0.01～1% permanganate as passivator, then heating water dilution mixesRear fried dry;
2) to the binding agent that adds 0.5～3% in the good iron silica flour of passivation, mix rear fried dry;
3) to step 2) add 0.6～1% stearate in the iron silica flour that obtains, mix rear dry-pressing and becomeDensity >=6.4g/cm3Green compact;
4) green compact are incubated after 1～5h at 200～400 DEG C, then are warming up to 600～800 DEG C of insulation 0.5～1h, coldBut, be cooled to room temperature with the cooling velocity of 5～10 DEG C/min,
Described iron silica flour is grouped into by the one-tenth of following weight proportioning: Si5～7%, and Ni or Co0.1～1.5%, itsRemaining is Fe.
Preferably, the preparation method of described iron silica flour is: in proportion Si, Fe, Ni or Co are placed in to meltingIn stove, at 1500～1800 DEG C, be fused into molten steel, then the speed stream with 10～20 kilograms per minute by molten steelEnter atomizer, the high speed nitrogen producing by 40～100MPa high pressure is pulverized molten steel and is made iron silica flour.
Preferably, the size distribution of described iron silica flour is: 150 orders≤granularity <, 200 orders account for 10～20%; 200Order≤granularity < 325 orders account for 50～60%; Granularity >=325 order accounts for 30～40%.
Preferably, described binding agent is the mixture of epoxy resin and phenolic resins, described epoxy resin and phenolThe weight ratio of urea formaldehyde is 1: 2.
The iron silica magnetic particle core obtaining according to above-mentioned preparation method.
Percentage in the present invention is mass percent.
The invention has the beneficial effects as follows:
1) the present invention adds micro-element Ni or Co on the basis of iron silicon, can effectively improve iron silicon magneticThe DC superposition characteristic of powder core, reduces magnetic loss, and prepared iron silica magnetic particle core density is high, smooth surface,Good moldability.
2) the present invention adopts permanganate to make passivator, and epoxy resin and phenolic resins mixture are made binding agent,Because the high manganese ion comprising in permanganate has stronger oxidisability with respect to phosphoric acid,Iron silicon powder surface is easier to form complete insulating bag overlay film, makes the iron silica magnetic particle core magnetic loss that makes lower,Make the mouldability of iron silica magnetic particle core better simultaneously.
3) production cost of the present invention is low.
Brief description of the drawings
Fig. 1 is the influence curve figure of silicone content to iron silica flour soft magnet performance, in figure: λ s is saturation magnetostrictionCoefficient, ρ are that resistivity, Bs are that saturation induction density, κ 1 are that magnetocrystalline anisotropy constant, Tc are CurieTemperature.
Fig. 2 is the iron silica magnetic particle wicking surface outward appearance picture after embodiment 2 and comparative example 2 moulding.
Fig. 3 is the iron silica magnetic particle wicking surface outward appearance picture after embodiment 3 and comparative example 3 moulding.
Fig. 4 is the iron silica magnetic particle wicking surface outward appearance picture after embodiment 4 and comparative example 4 moulding.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1Si, Ni or the Co impact on iron silica flour soft magnet performance
1, the silicon of different content is mixed with iron, be placed in smelting furnace, at 1500～1800 DEG C, be fused into steelLiquid, then flows into atomizer by molten steel with the speed of 10～20 kilograms per minute, by 40～100MPa high pressureThe high speed nitrogen producing is pulverized molten steel and is made iron silica flour.
As can be seen from Figure 1, in the time that silicone content is 5～7%, magnetostriction coefficient λ s and the magnetic of its alloyκ 1 is lower for anisotropic crystalline constant, and electricalresistivityρ is higher, so loss is lower, its soft magnet performance is more excellent.
2, taking silicone content as 6% as example, in ferro-silicium, add Ni or the Co element of different content, fromIn following table 1, can find out and in ferro-silicium, add micro-Ni or Co element, the magnetostriction of its alloyCoefficient lambda s and magnetocrystalline anisotropy constant κ 1 obviously reduce, and electricalresistivityρ obviously raises, and its soft magnet performance obtainsTo significantly improving, still along with the increase of Ni or Co constituent content, in the time that its content is greater than 1.5%, thisSoft magnet performance improve trend tend towards stability, due to Co, Ni element in occurring in nature storage capacity compared with Fe elementFew, thus expensive, comprehensive cost performance, the content of determining Ni or Co is 0.1～1.5%.
Table 1Ni or the impact of Co on iron silica flour soft magnet performance and cost
| Composition | FeSi6 | FeSi6(Ni/Co)0.1 | FeSi6(Ni/Co)1 | FeSi6(Ni/Co)1.5 | FeSi6(Ni/Co)2 |
| λs | 8×10-6 | 5×10-6 | 3×10-6 | 1×10-6 | 0.8×10-6 |
| κ1 | 3×10-7 | 2.5×10-7 | 2×10-7 | 1×10-7 | 0.9×10-7 |
| ρ | 100 | 150 | 200 | 250 | 270 |
| Cost | Low | Medium | Medium | Medium | Higher |
Embodiment 2
In the present embodiment, the composition of iron silica flour alloy is: Si5%, Ni1.5%, all the other are Fe. Adopt gasMist method is prepared from, and the concrete steps of described aeroponics are: Si, Ni, Fe are placed in to smelting furnace,At 1500～1800 DEG C, be fused into molten steel, then molten steel flowed into atomizer with the speed of 10～20 kilograms per minute,The high speed nitrogen producing by 40～100MPa high pressure is pulverized molten steel and is made iron silica flour. The granularity of described iron silica flourBe distributed as: 150 orders≤granularity <, 200 orders account for 10%; 200 orders≤granularity <, 325 orders account for 60%; Granularity >=325 orders account for 30%.
The preparation method of iron silica magnetic particle core is:
1) get iron silica flour, add 1% potassium permanganate as passivator, then heating water dilution mixes rear stir-fryDry;
2) to the binding agent that adds 3% in the good iron silica flour of passivation, described binding agent is epoxy resin and phenolic aldehydeThe mixture of resin, in described mixture, the weight ratio of epoxy resin and phenolic resins is 1: 2, mixesRear fried dry;
3) to step 2) add 1% stearate in the iron silica flour that obtains, mix rear dry-pressing and become density≥6.4g/cm3Green compact;
4) green compact are incubated after 5h at 200～400 DEG C, then are warming up to 600～800 DEG C of insulation 0.5h, cooling,Cooling velocity with 5 DEG C/min is cooled to room temperature.
Comparative example 2-1(is not containing trace element)
In this example, the composition of iron silica flour alloy is: Si5%, all the other are Fe, adopt aeroponics to be prepared from,The size distribution of iron silica flour is identical with embodiment 2.
The preparation method of iron silica magnetic particle core is identical with embodiment 2.
Comparative example 2-2(is containing trace element)
In this example, the composition of iron silica flour alloy is: Si5%, Nb1.5%, all the other are Fe, adopt aeroponicsBe prepared from, the size distribution of iron silica flour is identical with embodiment 2.
The preparation method of iron silica magnetic particle core is identical with embodiment 2.
The iron silica magnetic particle core performance comparison of table 2 embodiment 2 and comparative example 2
| Magnetic conductivity (%) | DC superposition characteristic (100 oersted) | Loss (500Gs/50kHz) | |
| Embodiment 2 | 60 | 80.3% | 150kW/cm3 |
| Comparative example 2-1 | 60 | 70.5% | 200kW/cm3 |
| Comparative example 2-2 | 60 | 71.2% | 193kW/cm3 |
The iron silica magnetic particle core processability comparison of table 3 embodiment 2 and comparative example 2
| Briquetting pressure | Compact density | Outward appearance | |
| Embodiment 2 | 18t/cm3 | 6.43g/cm3 | Smooth surface, without scaling |
| Comparative example 2-1 | 18t/cm3 | 6.2g/cm3 | Rough surface, scaling |
| Comparative example 2-2 | 18t/cm3 | 6.3g/cm3 | Rough surface |
Iron silica magnetic particle wicking surface outward appearance after moulding is shown in Fig. 2.
Embodiment 3
In the present embodiment, the composition of iron silica flour alloy is: Si7%, Co0.1%, all the other are Fe. Adopt gasMist method is prepared from, and the concrete steps of described aeroponics are: Si, Co, Fe are placed in to smelting furnace,At 1500～1800 DEG C, be fused into molten steel, then molten steel flowed into atomizer with the speed of 10～20 kilograms per minute,The high speed nitrogen producing by 40～100MPa high pressure is pulverized molten steel and is made iron silica flour. The granularity of described iron silica flourBe distributed as: 150 orders≤granularity <, 200 orders account for 20%; 200 orders≤granularity <, 325 orders account for 50%; Granularity >=325 orders account for 30%.
The preparation method of iron silica magnetic particle core is:
1) get iron silica flour, add 0.01% magnesium permanganate as passivator, after then heating water dilution mixesFried dry;
2) to the binding agent that adds 0.5% in the good iron silica flour of passivation, described binding agent is epoxy resin and phenolic aldehydeThe mixture of resin, in described mixture, the weight ratio of epoxy resin and phenolic resins is 1: 2, mixesRear fried dry;
3) to step 2) add 0.6% stearate in the iron silica flour that obtains, mix rear dry-pressing Cheng MiDegree >=6.4g/cm3Green compact;
4) green compact are heat-treated, after 200～400 DEG C of insulation 1h, then be warming up to 600～800 DEG C of insulations1h, cooling, be cooled to room temperature with the cooling velocity of 8 DEG C/min.
Comparative example 3-1(is not containing trace element)
In this example, the composition of iron silica flour alloy is: Si7%, all the other are Fe, adopt aeroponics to be prepared from,The size distribution of iron silica flour is identical with embodiment 3.
The preparation method of iron silica magnetic particle core is identical with embodiment 3.
Comparative example 3-2(is containing trace element)
In this example, the composition of iron silica flour alloy is: Si7%, V0.1%, all the other are Fe, adopt aerosol legal systemStandby forming, the size distribution of iron silica flour is identical with embodiment 3.
The preparation method of iron silica magnetic particle core is identical with embodiment 3.
The iron silica magnetic particle core performance comparison of table 4 embodiment 3 and comparative example 3
| Magnetic conductivity (%) | DC superposition characteristic (100 oersted) | Loss (500Gs/50kHz) | |
| Embodiment 3 | 75 | 69.8% | 120kW/cm3 |
| Comparative example 3-1 | 75 | 55% | 180kW/cm3 |
| Comparative example 3-2 | 75 | 60% | 160kW/cm3 |
The iron silica magnetic particle core processability comparison of table 5 embodiment 3 and comparative example 3
| Briquetting pressure | Compact density | Outward appearance | |
| Embodiment 3 | 18t/cm3 | 6.43g/cm3 | Smooth surface, without scaling |
| Comparative example 3-1 | 18t/cm3 | 6.15g/cm3 | Rough surface, scaling |
| Comparative example 3-2 | 18t/cm3 | 6.23g/cm3 | Rough surface |
Iron silica magnetic particle wicking surface outward appearance after moulding is shown in Fig. 3.
Embodiment 4
In the present embodiment, the composition of iron silica flour alloy is: Si6%, Ni1%, all the other are Fe. Adopt aerosolMethod is prepared from, and the concrete steps of described aeroponics are: Si, Ni, Fe are placed in to smelting furnace,At 1500～1800 DEG C, be fused into molten steel, then flow into atomizer with the speed of 10～20 kilograms, pass throughThe high speed nitrogen that 40～100MPa high pressure produces is pulverized, the then speed with 10～20 kilograms per minute by molten steelFlow into atomizer, the high speed nitrogen producing by 40～100MPa high pressure is pulverized molten steel and is made iron silica flour. DescribedThe size distribution of iron silica flour is: 150 orders≤granularity <, 200 orders account for 10%; 200 orders≤granularity <, 325 orders account for50%; Granularity >=325 order accounts for 40%.
The preparation method of iron silica magnetic particle core is:
1) get iron silica flour, add 0.1% zinc permanganate as passivator, then heating water dilution mixes rear stir-fryDry;
2) to the binding agent that adds 1.5% in the good iron silica flour of passivation, described binding agent is epoxy resin and phenolic aldehydeThe mixture of resin, in described mixture, the weight ratio of epoxy resin and phenolic resins is 1: 2, mixesRear fried dry;
3) to step 2) add 0.8% stearate in the iron silica flour that obtains, mix rear dry-pressing Cheng MiDegree >=6.4g/cm3Green compact;
4) green compact are heat-treated, after 200～400 DEG C of insulation 3h, then be warming up to 600～800 DEG C of insulations0.8h, cooling, be cooled to room temperature with the cooling velocity of 10 DEG C/min.
Comparative example 4-1(is not containing trace element)
In this example, the composition of iron silica flour alloy is: Si6%, all the other are Fe, adopt aeroponics to be prepared from,The size distribution of iron silica flour is identical with embodiment 4.
The preparation method of iron silica magnetic particle core is identical with embodiment 4.
Comparative example 4-2(is containing trace element)
In this example, the composition of iron silica flour alloy is: Si6%, V1%, all the other are Fe, adopt aerosol legal systemStandby forming, the size distribution of iron silica flour is identical with embodiment 4.
The preparation method of iron silica magnetic particle core is identical with embodiment 4.
The iron silica magnetic particle core performance comparison of table 6 embodiment 4 and comparative example 4
| Magnetic conductivity (%) | DC superposition characteristic (100 oersted) | Loss (500Gs/50kHz) | |
| Embodiment 4 | 90 | 60.3% | 80kW/cm3 |
| Comparative example 4-1 | 90 | 49.3% | 143kW/cm3 |
| Comparative example 4-2 | 90 | 51.5% | 161kW/cm3 |
The iron silica magnetic particle core processability comparison of table 7 embodiment 4 and comparative example 4
| Briquetting pressure | Compact density | Outward appearance | |
| Embodiment 4 | 18t/cm3 | 6.41g/cm3 | Smooth surface, without scaling |
| Comparative example 4-1 | 18t/cm3 | 5.96g/cm3 | Rough surface, scaling |
| Comparative example 4-2 | 18t/cm3 | 6.0g/cm3 | Rough surface |
Iron silica magnetic particle wicking surface outward appearance after moulding is shown in Fig. 4.
Conclusion: can find out from the result of the test of embodiment 2-4, the present invention adds trace on the basis of iron siliconElement Ni or Co, can effectively improve the DC superposition characteristic of iron silica magnetic particle core, reduce magnetic loss, madeThe iron silica magnetic particle core density obtaining is high, smooth surface, good moldability.
Claims (5)
1. a preparation method for iron silica magnetic particle core, is characterized in that comprising the following steps:
1) get iron silica flour, add 0.01～1% permanganate as passivator, then heating water dilution mixesRear fried dry;
2) to the binding agent that adds 0.5～3% in the good iron silica flour of passivation, mix rear fried dry;
3) to step 2) add 0.6～1% stearate in the iron silica flour that obtains, mix rear dry-pressing and becomeDensity >=6.4g/cm3Green compact;
4) green compact are incubated after 1～5h at 200～400 DEG C, then are warming up to 600～800 DEG C of insulation 0.5～1h, coldBut, be cooled to room temperature with the cooling velocity of 5～10 DEG C/min,
Described iron silica flour is grouped into by the one-tenth of following weight proportioning: Si5～7%, and Ni or Co0.1～1.5%, itsRemaining is Fe.
2. the preparation method of iron silica magnetic particle core according to claim 1, is characterized in that: described iron silica flourPreparation method be: in proportion Si, Fe, Ni or Co are placed in to smelting furnace, molten at 1500～1800 DEG CChange into molten steel, then molten steel is flowed into atomizer with the speed of 10～20 kilograms per minute, by 40～100MPaThe high speed nitrogen that high pressure produces is pulverized molten steel and is made iron silica flour.
3. the preparation method of iron silica magnetic particle core according to claim 1, is characterized in that: described iron siliconThe size distribution of powder is: 150 orders≤granularity <, 200 orders account for 10～20%; 200 orders≤granularity <, 325 orders account for50～60%; Granularity >=325 order accounts for 30～40%.
4. the preparation method of iron silica magnetic particle core according to claim 1, is characterized in that: described bondingAgent is the mixture of epoxy resin and phenolic resins, and the weight ratio of described epoxy resin and phenolic resins is 1: 2.
5. the iron silica magnetic particle core that the preparation method described in any one obtains according to claim 1～4.
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| CN101236812A (en) * | 2007-12-14 | 2008-08-06 | 浙江大学 | Making method for electromagnetic wave interference resisting iron ,silicon, aluminum and nickel alloy |
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