CN103839642A - Neu flux core material with permeability being 75 and preparing method thereof - Google Patents
Neu flux core material with permeability being 75 and preparing method thereof Download PDFInfo
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- 239000000843 powder Substances 0.000 claims abstract description 58
- 229910052742 iron Inorganic materials 0.000 claims abstract description 53
- 238000003723 Smelting Methods 0.000 claims abstract description 21
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 16
- 239000010703 silicon Substances 0.000 claims abstract description 16
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- 229910002058 ternary alloy Inorganic materials 0.000 claims abstract description 8
- 238000012545 processing Methods 0.000 claims abstract description 4
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- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 30
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 19
- 238000002844 melting Methods 0.000 claims description 17
- 230000008018 melting Effects 0.000 claims description 17
- 238000002360 preparation method Methods 0.000 claims description 17
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 15
- XWHPIFXRKKHEKR-UHFFFAOYSA-N iron silicon Chemical compound [Si].[Fe] XWHPIFXRKKHEKR-UHFFFAOYSA-N 0.000 claims description 15
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 14
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
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- 239000003795 chemical substances by application Substances 0.000 claims description 10
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- 229910052759 nickel Inorganic materials 0.000 claims description 7
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- 229910002027 silica gel Inorganic materials 0.000 claims description 7
- 239000011248 coating agent Substances 0.000 claims description 5
- 238000000576 coating method Methods 0.000 claims description 5
- 239000003822 epoxy resin Substances 0.000 claims description 5
- 238000013467 fragmentation Methods 0.000 claims description 5
- 238000006062 fragmentation reaction Methods 0.000 claims description 5
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- 229920000647 polyepoxide Polymers 0.000 claims description 5
- 239000004922 lacquer Substances 0.000 claims description 4
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 4
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 3
- 241000790917 Dioxys <bee> Species 0.000 claims description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 3
- 238000000889 atomisation Methods 0.000 claims description 3
- 229910052796 boron Inorganic materials 0.000 claims description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims description 3
- 239000011733 molybdenum Substances 0.000 claims description 3
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 2
- 238000011017 operating method Methods 0.000 claims description 2
- KSIIOJIEFUOLDP-UHFFFAOYSA-N [Si].[Fe].[Ni] Chemical compound [Si].[Fe].[Ni] KSIIOJIEFUOLDP-UHFFFAOYSA-N 0.000 abstract description 3
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- 235000013312 flour Nutrition 0.000 description 2
- UGKDIUIOSMUOAW-UHFFFAOYSA-N iron nickel Chemical compound [Fe].[Ni] UGKDIUIOSMUOAW-UHFFFAOYSA-N 0.000 description 2
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- 229910052751 metal Inorganic materials 0.000 description 2
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- 229910052758 niobium Inorganic materials 0.000 description 2
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Abstract
The invention discloses a method for preparing a neu flux core material with permeability being 75. The method comprises the steps of primarily smelting 82-91 wt% of iron and 4-8 wt% of silicon, adding 5-10 wt% of nickel powder into the mixture of the iron and the silicon, carrying out secondary smelting to form iron silicon nickel ternary alloy and carrying out spraying and powder preparing, surface processing, compression molding, thermal treatment and surface paint spraying, and then the neu flux core material is obtained. The invention further discloses the neu flux core material with permeability being 75, wherein the neu flux core material with permeability being 75 is obtained according to the preparing method. A prepared magnetic core is low in cost and loss, and high in direct current bias performance.
Description
Technical field
The present invention relates to soft magnetic material technical field, especially relate to a kind of μ 75 iron tantnickel powder core materials and preparation method thereof.
Background technology
Metal magnetic powder core has the advantages such as high saturated magnetic induction, high-curie temperature and permanent magnetic conduction, is widely used in super-current power unit.Along with the popularization gradually of solar power generation, wind power generation, magnetic core used in inverter requires to have high DC stacked characteristic, low-loss and good frequency stability.The magnetic core that is widely used at present this field is mainly iron silica magnetic particle core, iron silica magnetic particle core, and cost is low, and DC stacked performance is high, but loss is high, generally has Pcv=2100mw/cm
3(100k, 100mT), generates heat more serious, is unfavorable for device efficient energy-saving.
As Chinese patent Granted publication number: CN102303115A, in the patent document of on 01 04th, 2012 Granted publication day, the preparation method of the iron silicon metal magnetic powder core of a kind of iron silicon materials and μ 26 is disclosed, in the iron silicon materials of the method, Si content is 6.4wt%～7.0wt%, add micro-Nb and V element, surplus is Fe, directly carries out melting powder by atomization and prepare μ 26 iron silicon magnetic cores in opening stove.In the method, mix micro-Nb and V element and can suppress the oxidation of ferro-silicium, prevent that oxide inclusions is in crystal grain inside, can reduce coercive force, reduce the magnetic hysteresis loss of magnetic core, but Nb and the mixing of V element of trace do not exert an influence substantially to the resistivity of ferro-silicium, and eddy current loss is higher, and therefore the overall losses of iron silicon magnetic core is higher.
Summary of the invention
The present invention is in order to solve the high weak point of general iron silica magnetic particle loss, and a kind of preparation method of low-loss μ 75 iron tantnickel powder core materials is provided.The present invention also provides a kind of μ being obtained by this preparation method 75 iron tantnickel powder core materials.
To achieve these goals, the present invention is by the following technical solutions:
A preparation method for μ 75 iron tantnickel powder core materials, operating procedure is:
(1) first melting: take the ingot iron of 82～91 weight portions and the silicon ingot of 4～8 weight portions, be placed in vacuum medium frequency induction furnace and carry out first melting, obtain iron silicon binary alloy;
(2) secondary smelting: by after cooling iron silicon binary alloy fragmentation, sneak into the nickel powder of 5～10 weight portions, be again placed in vacuum medium frequency induction furnace and carry out secondary smelting, obtain iron tantnickel ternary alloy three-partalloy;
(3) powder process: the iron tantnickel ternary alloy three-partalloy of melting is through the tundish of atomization plant, carries out powder by spraying with nitrogen;
(4) magnetic processing: the magnetic making is put into the acetone soln Passivation Treatment of phosphoric acid, constantly stirred until acetone volatilization is complete, phosphoric acid addition is 0.6～0.8% of magnetic weight;
(5) make powder core: magnetic after treatment, through compression molding, heat treatment and surface lacquer, is obtained to iron tantnickel powder core.
Iron tantnickel powder core material prepared by the present invention, compared with iron silica magnetic particle core, nickle atom solid solution is in ferro-silicium, cause silicon to decline in the inner solubility of ferro-silicium crystal grain, silicon is in grain boundaries enrichment, the Silicon-rich Grain-Boundary Phase that forms high resistivity is coated on around crystal grain, and resistivity of material is improved greatly, reduces magnetic core eddy current loss; Compared with iron nickel powder core, nickel content is low, and cost is low.The present invention utilizes above-mentioned preparation method to obtain iron tantnickel ternary-alloy material, has obtained iron silica magnetic particle core, iron nickel powder core advantage separately.
Iron tantnickel magnetic prepared by the present invention adopts two step vacuum melting methods, the benefit of two step meltings is in second step melting, and the nickel element adding on the one hand enters ferro-silicium crystal grain inside, makes silicon in grain boundaries enrichment, form the Grain-Boundary Phase of Silicon-rich, improve resistivity; Adopt on the other hand substep smelting iron silicon nickel alloy, can improve the solid solubility of silicon in the middle of alloy, be conducive to improve the resistivity of magnetic core.Vacuum can reduce the oxygen content of iron silicon nickel alloy, reduces material internal oxide particle impurity, is conducive to reduce material coercive force.
The present invention adopts the acetone soln of phosphoric acid as passivator, and the difficult generation of the magnetic of unpassivated processing plastic deformation causes powder core to be difficult for compressing and compacted density is very low, and formability is very poor.When passivation, select acetone to disperse phosphoric acid as solvent, utilize the volatile characteristic of acetone, make it naturally to volatilize and remove in whipping process, simplify the operation.Meanwhile, magnetic permeability and the factor of merit impact of the consumption of phosphoric acid on the powder core making is larger.Along with the increase of phosphoric acid consumption, magnetic permeability is on a declining curve, can utilize and control phosphoric acid consumption, obtains the powder core material of different magnetic permeabilitys.
As preferably, the magnetic making is carried out to grading by-200 orders ,-150 orders ,-100 orders, then according to-200 orders :-150 orders :-100 orders=6:3:1 enters step (4) after mixing in step (3).
As preferably, the magnetic after step (4) Passivation Treatment is put into the acetone soln of siliceous gum resin, constantly stir until acetone volatilization is complete, silica gel resin amount is 1～2% of magnetic weight.Magnetic after passivation adds silica gel resin, bonding when on the one hand auxiliary magnetic moulding, increases on the other hand the resistant to elevated temperatures characteristic of powder core.
As preferably, the smelting temperature of vacuum medium frequency induction furnace is 1460 DEG C～1600 DEG C.
As preferably, in step (2), the granularity of nickel powder is-300 orders.
As preferably, when step (5) compression molding, adding the release agent that accounts for magnetic weight 0.3%～1%, described release agent is one or more in stearate, dioxy three boron, molybdenum bisuphide.Prevent that powder core and mould are bonding.
As preferably, in compression molding, briquetting pressure is 1800～2200MPa, and the dwell time is 9s～10s.Briquetting pressure in the present invention is higher than the briquetting pressure of other iron silica magnetic particle core material, and high pressure moulding can improve magnetic core density, thereby improves the saturation induction density of magnetic core.
As preferably, described heat treatment be by the powder core after moulding under nitrogen atmosphere, at 690 DEG C～750 DEG C temperature, be incubated 40～60min.
As preferably, described surface lacquer is to solidify after the spraying of magnetic surface epoxy resin coating.
A kind of μ 75 iron tantnickel powder core materials, described iron tantnickel powder core material is ternary alloy material, iron tantnickel powder core is made up of the silicon of 4～8wt%, nickel and the remaining iron of 5～10wt%.
Beneficial effect: the iron tantnickel powder core material that the present invention obtains: 1) cost is low, and loss is low; 2) in alloy melting process, oxygen content is low, and material coercive force is low; 3) substep melting, silicon solid solubility is high, improves resistivity; 4) iron tantnickel magnetic smooth surface, easy and phosphatase reaction generates dielectric film, and the magnetic core quality factor of acquisition are high.
Embodiment
Below in conjunction with embodiment, the present invention will be further described.
Embodiment 1
Take the industrial ingot iron of 86 weight portions and the silicon ingot of 6 weight portions, dropping into vacuum degree is 6.7 × 10
-3in the vacuum medium frequency induction furnace of Pa, carry out first melting, and add appropriate SiO
2, be used for removing the gred.Smelting temperature is 1460 DEG C, and smelting time is 1h, cooling with stove, obtains iron silicon binary alloy ingot casting.Iron silicon binary alloy ingot is carried out to fragmentation with disintegrating machine, obtaining the fragment of 3cm diameter, is-300 object nickel powders toward the granularity of evenly sneaking into 8 weight portions in fragment, frequently in induction furnace, carries out secondary smelting in a vacuum, smelting temperature is 1470 DEG C, and fusing time is 1.5h.After alloy melting is good, directly enter the tundish of vacuum gas-atomized powder machine, carry out powder by spraying with nitrogen, by aerosolization powder collection, sieve with vibrating screen, carry out classification storage by-200 orders ,-150 orders ,-100 object granule sizes.Then by-200 orders: the weight ratio of 150 orders :-100 orders=6:3:1 is chosen magnetic and carried out grain size proportion mixing.The magnetic mixing is put into the acetone soln Passivation Treatment of phosphoric acid, constantly stirs until acetone volatilization is complete, and phosphoric acid addition is 0.7% of magnetic weight, and acetone addition is 10% of magnetic weight.The magnetic after passivation is added in the acetone soln of siliceous gum resin again, constantly stir until acetone volatilization is complete, silica gel resin amount is 1% of magnetic weight, and acetone addition is 5% of magnetic weight.Before compression molding, add the release agent that accounts for magnetic weight 0.8%, release agent is stearate, and the magnetic mixing is placed in to mould, be pressed into the magnet ring of 27mm × 14.60mm × 11.2mm, briquetting pressure is 2000MPa, and the dwell time is 10s, obtains magnetic core blank.By the magnetic core after moulding at N
2under atmosphere, heat treatment 50min at 720 DEG C of temperature, cooling with stove.After coming out of the stove, magnetic core surface is carried out epoxy resin coating spraying, is solidified, and finally obtains μ 75 iron tantnickel powder cores.The magnetic property of the iron tantnickel powder core obtaining after testing, is as shown in table 1.
Embodiment 2
Take the industrial ingot iron of 82 weight portions and the silicon ingot of 8 weight portions, dropping into vacuum degree is 6.7 × 10
-3in the vacuum medium frequency induction furnace of Pa, carry out first melting, and add appropriate SiO
2, be used for removing the gred.Smelting temperature is 1600 DEG C, and smelting time is 1h, cooling with stove, obtains iron silicon binary alloy ingot casting.Iron silicon binary alloy ingot is carried out to fragmentation with disintegrating machine, obtaining the fragment of 6cm diameter, is-300 object nickel powders toward the granularity of evenly sneaking into 10 weight portions in fragment, frequently in induction furnace, carries out secondary smelting in a vacuum, smelting temperature is 1600 DEG C, and fusing time is 1.5h.After alloy melting is good, directly enter the tundish of air atomizing flour mill, carry out powder by spraying with nitrogen, aerosol powder is collected, sieve with vibrating screen, carry out classification storage by-200 orders ,-150 orders ,-100 object granule sizes.Then by-200 orders: the weight ratio of 150 orders :-100 orders=6:3:1 is chosen magnetic and carried out proportioning mixing.The magnetic mixing is put into the acetone soln Passivation Treatment of phosphoric acid, constantly stirs until acetone volatilization is complete, and phosphoric acid addition is 0.6% of magnetic weight, and acetone addition is 8% of magnetic weight.The magnetic after passivation is added in the acetone soln of siliceous gum resin again, constantly stir until acetone volatilization is complete, silica gel resin amount is 2% of magnetic weight, and acetone addition is the 6wt% of magnetic weight.Before compression molding, add the release agent that accounts for magnetic weight 0.3%, release agent is the mixture of stearate, dioxy three boron, and the magnetic mixing is placed in to mould, be pressed into the magnet ring of 27mm × 14.60mm × 11.2mm, briquetting pressure is 1800MPa, and the dwell time is 9s, obtains magnetic core blank.By the magnetic core after moulding at N
2under atmosphere, heat treatment 40min at 690 DEG C of temperature, cooling with stove.After coming out of the stove, magnetic core surface is carried out epoxy resin coating spraying, is solidified, and finally obtains μ 75 iron tantnickel powder cores.The magnetic property of the iron tantnickel powder core obtaining after testing, is as shown in table 1.
Embodiment 3
Take the industrial ingot iron of 91 weight portions and the silicon ingot of 4 weight portions, dropping into vacuum degree is 6.7 × 10
-3in the vacuum medium frequency induction furnace of Pa, carry out first melting, and add appropriate SiO
2, be used for removing the gred.Smelting temperature is 1500 DEG C, and smelting time is 1h, cooling with stove, obtains iron silicon binary alloy ingot casting.Iron silicon binary alloy ingot is carried out to fragmentation with disintegrating machine, obtaining the fragment of 4cm diameter, is-300 object nickel powders toward the granularity of evenly sneaking into 5 weight portions in fragment, frequently in induction furnace, carries out secondary smelting in a vacuum, smelting temperature is 1500 DEG C, and fusing time is 1.5h.After alloy melting is good, directly enter the tundish of air atomizing flour mill, carry out powder by spraying with nitrogen, aerosol powder is collected, sieve with vibrating screen, carry out classification storage by-200 orders ,-150 orders ,-100 object granule sizes.Then by-200 orders: the weight ratio of 150 orders :-100 orders=6:3:1 is chosen magnetic and carried out proportioning mixing.The magnetic mixing is put into the acetone soln Passivation Treatment of phosphoric acid, constantly stirs until acetone volatilization is complete, and phosphoric acid addition is 0.8% of magnetic weight, and acetone addition is 12% of magnetic weight.The magnetic after passivation is added in the acetone soln of siliceous gum resin again, constantly stir until acetone volatilization is complete, silica gel resin amount is 2% of magnetic weight, and acetone addition is the 6wt% of magnetic weight.Before compression molding, add the release agent that accounts for magnetic weight 1%, release agent is molybdenum bisuphide, and the magnetic mixing is placed in to mould, is pressed into the magnet ring of 27mm × 14.60mm × 11.2mm, and briquetting pressure is 2200MPa, and the dwell time is 10s, obtains magnetic core blank.By the magnetic core after moulding at N
2under atmosphere, heat treatment 60min at 750 DEG C of temperature, cooling with stove.After coming out of the stove, magnetic core surface is carried out epoxy resin coating spraying, is solidified, and finally obtains μ 75 iron tantnickel powder cores.The magnetic property of the iron tantnickel powder core obtaining after testing, is as shown in table 1.
Claims (10)
1. a preparation method for μ 75 iron tantnickel powder core materials, is characterized in that, operating procedure is:
(1) first melting: take the ingot iron of 82～91 weight portions and the silicon ingot of 4～8 weight portions, be placed in vacuum medium frequency induction furnace and carry out first melting, obtain iron silicon binary alloy;
(2) secondary smelting: by after cooling iron silicon binary alloy fragmentation, sneak into the nickel powder of 5～10 weight portions, be again placed in vacuum medium frequency induction furnace and carry out secondary smelting, obtain iron tantnickel ternary alloy three-partalloy;
(3) powder process: the iron tantnickel ternary alloy three-partalloy of melting is through the tundish of atomization plant, carries out powder by spraying with nitrogen;
(4) magnetic processing: the magnetic making is put into the acetone soln Passivation Treatment of phosphoric acid, constantly stirred until acetone volatilization is complete, phosphoric acid addition is 0.6～0.8% of magnetic weight;
(5) make powder core: magnetic after treatment, through compression molding, heat treatment and surface lacquer, is obtained to iron tantnickel powder core.
2. the preparation method of a kind of μ 75 iron tantnickel powder core materials according to claim 1, it is characterized in that, the magnetic making in step (3) is carried out to grading by-200 orders ,-150 orders ,-100 orders, then according to-200 orders :-150 orders :-100 orders=6:3:1 enters step (4) after mixing.
3. the preparation method of a kind of μ 75 iron tantnickel powder core materials according to claim 1, it is characterized in that, the acetone soln of silica gel resin is joined in the magnetic after step (4) Passivation Treatment, constantly stir until acetone volatilization is complete, silica gel resin amount is 1～2% of magnetic weight.
4. the preparation method of a kind of μ 75 iron tantnickel powder core materials according to claim 1, is characterized in that, the smelting temperature of vacuum medium frequency induction furnace is 1460 DEG C～1600 DEG C.
5. the preparation method of a kind of μ 75 iron tantnickel powder core materials according to claim 1, is characterized in that, in step (2), the granularity of nickel powder is-300 orders.
6. the preparation method of a kind of μ 75 iron tantnickel powder core materials according to claim 1, it is characterized in that, when step (5) compression molding, adding the release agent that accounts for magnetic weight 0.3%～1%, described release agent is one or more in stearate, dioxy three boron, molybdenum bisuphide.
7. according to the preparation method of a kind of μ 75 iron tantnickel powder core materials described in claim 1 or 6, it is characterized in that, in compression molding, briquetting pressure is 1800～2200MPa, and the dwell time is 9s～10s.
8. the preparation method of a kind of μ 75 iron tantnickel powder core materials according to claim 1, is characterized in that, described heat treatment be by the powder core after moulding under nitrogen atmosphere, at 690 DEG C～750 DEG C temperature, be incubated 40～60min.
9. the preparation method of a kind of μ 75 iron tantnickel powder core materials according to claim 1, is characterized in that, described surface lacquer is to solidify after the spraying of magnetic surface epoxy resin coating.
10. the μ being obtained by the preparation method of μ 75 iron tantnickel powder core materials as claimed in claim 1 75 iron tantnickel powder core materials, it is characterized in that, described iron tantnickel powder core material is ternary alloy material, and iron tantnickel powder core is made up of the silicon of 4～8wt%, nickel and the remaining iron of 5～10wt%.
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| CN106571205B (en) * | 2016-11-03 | 2019-02-26 | 中国兵器科学研究院宁波分院 | The preparation method of low-loss iron tantnickel powder core composite material |
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