CN104036903B - A kind of preparation method of ferrum tantnickel powder core - Google Patents
A kind of preparation method of ferrum tantnickel powder core Download PDFInfo
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- CN104036903B CN104036903B CN201410246068.8A CN201410246068A CN104036903B CN 104036903 B CN104036903 B CN 104036903B CN 201410246068 A CN201410246068 A CN 201410246068A CN 104036903 B CN104036903 B CN 104036903B
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Abstract
The invention discloses a kind of ferrum tantnickel powder core and preparation method thereof.Comprise the steps: 1) use vacuum induction melting ferrum silicon nickel alloy ingot casting；2) by above-mentioned alloy cast ingot through Mechanical Crushing, ball is clayed into power and is placed in argon atmosphere annealing；3) take ferrum tantnickel powder, carry out grain size proportion according to a certain percentage；4) it is passivated processing toward addition passivator in the ferrum tantnickel powder prepared；5) add magnetic particle colloid and the insulating compound of acetone dilution, stir, carry out insulation adhesive cladding；6) lubricant releasing agent is added, mix homogeneously, compression molding；7) compressing sample is positioned in protective atmosphere makes annealing treatment, furnace cooling, spraying, obtain target product.In alloy powder of the present invention, Ni content is relatively low, and cost is relatively low；By the rational size distribution proportioning to alloy powder, packed density can be made to reach maximum, improve the saturation induction density of powder core, and reduce its power attenuation.
Description
Technical field
The present invention relates to the manufacturing technology field of a kind of magnetic material, be specifically related to the preparation side of a kind of ferrum tantnickel powder core
Method.
Background technology
Metal magnetic powder core be by ferromagnetic particle is mixed with insulating wrapped agent compacting magnetics, magnetic powder it
Between separated by non magnetic dielectric, between granule and granule insulate, therefore powder core eddy-current loss under medium-high frequency is the least,
Its pcrmeability is less but has the preferable linearity, and has higher saturation induction density, can be applicable to high frequency occasion.Magnetic
The magnetic property of powder core and the material of magnetic powder own, magnetic powder particle size, insulating wrapped agent kind and consumption, pressing pressure and heat treatment
The many factors such as process are correlated with, and can be obtained with the ratio of insulating wrapped agent by adjustment powder size proportioning, magnetisable material
There is the powder core of different soft magnet performance.
According to the difference of the composition of magnetic powder own, metal magnetic powder core substantially can be divided into ferrocart core, ferrum silica magnetic particle core, ferrum sial
Powder core, ferrum tantnickel powder core, high magnetic flux powder core, MPP powder core and amorphous nano-crystalline powder core, all kinds of powder cores have it
Respective feature and application.Along with information technology and the fast development of electromechanical industries, it is desirable to magnetic device is toward high frequency, little
Type and intelligent direction development, it is strong that this just requires to have high saturation induction as the metal magnetic powder core of magnetic device core
Degree, excellent D.C. magnetic biasing ability and relatively low high-frequency loss.
The Chinese invention patent of Publication No. CN102314986 discloses the manufacture method of a kind of ferrum-silicon alloy magnetic powder core,
Comprise the following steps: a) join powder: taking appropriate ferrum Si powder, wherein the weight content of Si is 2% ~ 8%, and surplus is Fe；B) powder is fried: will
Prepare ferrum silica flour roast to temperature reach 50 DEG C ~ 150 DEG C time add phosphoric acid diluent carry out surface process, roast to be dried
After, add phenolic resin and continue to roast to being dried；C) compressing: pressure is 15 ~ 26 t/cm2；D) heat treatment: at thermotropism
It is passed through hydrogen in reason stove or nitrogen carries out heat treatment；E) face coat: use epoxy resin paint to be coated in the surface of powder core.
Although the ferrum silica magnetic particle core technique prepared by this technical scheme is simple, cost is relatively low, but it is disadvantageous in that: ferrum silica magnetic particle core
Power attenuation in high frequency is excessive, it is impossible to be applied to high frequency occasion.
The Chinese invention patent of Publication No. CN100999021 discloses Fe-Ni50Series alloy powder and powder core manufacturer
Method, comprises the following steps: 1) a kind of soft-magnetic Fe-Ni50Series alloy powder manufacture method, including: Fe-Ni50Be alloy smelting-
Water atomization is sprayed into the heat treatment after powder-powder processing-processing；2) a kind of Fe-Ni50It is the manufacturer of alloy soft magnetic powder core
Method, including: screening powder particle carries out grain size proportion-Passivation Treatment-powder surface passivating treatment-in alloy powder and adds absolutely
Edge agent, lubricant, releasing agent-compression molding-heat treatment-face coat.Fe-Ni prepared by this technical scheme50Although powder core
Saturation induction density is high, and DC superposition characteristic is preferable, and power attenuation is relatively low, but it is disadvantageous in that: Fe-Ni50In magnetic powder
The content of Ni element is up to 50%, causes production cost higher, is unfavorable for use of large-scale production.
The Chinese invention patent of Publication No. CN102436895 discloses the preparation method of a kind of Fe-Si-Al magnetic core, bag
Include following steps: 1) take ferrum sial powder according to set grain size proportion；2) in the ferrum sial powder prepared, passivator is added
It is passivated processing；3) magnetic particle colloid that dilutes with acetone of addition and insulating compound after passivation, stir, carry out insulation adhesive bag
Cover；4) lubricant releasing agent is added, mix homogeneously, it is pressed into base sample；5) base sample be positioned in protective atmosphere carry out heat treatment,
Spraying, obtains target product.Although Fe-Si-Al magnetic core tensile strength prepared by this technical scheme is higher, direct current biasing characteristic is relatively
Good, power attenuation is relatively low, but it is disadvantageous in that the saturation induction density of powder core is relatively low, is not suitable in high-power condition
Lower use.
In sum, produce in the market and the powder core that uses has respective feature and application.The highest
Magnetic flux powder core has the saturation flux density of maximum, is lost relatively low, and comprehensive magnetic can be excellent.But the manufacturing cost of costliness limits
Make it to produce and application, and developing rapidly along with modern electronic technology, magnetic device is proposed in high-power lower application
Higher requirement, this works out a kind of low cost, high performance powder core to substitute high magnetic flux magnetic with regard to an urgent demand related personnel
Powder core.And ferrum tantnickel powder core is as the alloy magnetic powder core of a new generation, its saturation induction density is close with high magnetic flux powder core,
Loss ratio ferrum silica magnetic particle core is low by about one time, close with high magnetic flux powder core, and direct current biasing characteristic is better than ferrum silica magnetic particle core, is a kind of
Substitute the lower cost materials of high magnetic flux powder core.
Therefore, seek a set of suitable technological process to prepare low cost, high performance ferrum tantnickel powder core, have become as
The technical problem that those skilled in the art are urgently to be resolved hurrily.
Summary of the invention
The invention provides the preparation method of a kind of ferrum tantnickel powder core, solve existing powder core and be difficult to meet low one-tenth
Originally a, difficult problem for high performance requirements.
The technical solution adopted in the present invention is specific as follows:
The preparation method of a kind of ferrum tantnickel powder core comprises the steps:
1) vacuum melting furnace smelting iron silicon nickel alloy ingot casting, by percentage to the quality, the chemical composition of alloy cast ingot are used
Being Si 5 ~ 30%, Ni 3 ~ 20%, Al 0.01 ~ 0.2%, Ca 0.01 ~ 0.2%, C≤0.05%, surplus is Fe；
2) above-mentioned alloy cast ingot is positioned over indifferent gas after Mechanical Crushing, the ferrum tantnickel powder of ball milling one-tenth-100 mesh
Making annealing treatment in the heat-treatment furnace of body protective atmosphere, annealing temperature is 400 ~ 700 DEG C, and annealing time is 1 ~ 5 h；
3) by prepared ferrum tantnickel powder in following ratio :-100 mesh ~+200 mesh account for 10 ~ 30% ,-200 mesh of gross mass ~
+ 300 mesh account for the 35 ~ 50% of gross mass, and-300 mesh ~+400 mesh account for 15 ~ 35% ,-400 mesh of gross mass and account for the 5 ~ 20% of gross mass and enter
Row grain size proportion；
4) toward step 3) the ferrum tantnickel powder for preparing adds account for ferrum tantnickel powder quality 0.2 ~ 1.8% passivator and carry out blunt
Change processes；Described passivator is one or more in phosphoric acid, chromic acid or hydrogen peroxide；
5) after Passivation Treatment completes, the magnetic particle colloid accounting for ferrum tantnickel powder quality 0.2 ~ 2.0% of addition acetone as solvent
Solution and account for the insulating compound of ferrum tantnickel powder quality 0.02 ~ 1.0%, is sufficiently stirred for, carries out insulation adhesive cladding；Described insulation
Agent is one or more in Kaolin, mica powder or Pulvis Talci；
6) after insulating wrapped completes, adding the lubricant releasing agent accounting for ferrum tantnickel powder quality 0.1 ~ 1.5%, mixing is all
Even, at 12 ~ 28 t/cm2Pressure under compressing, obtain compressing sample；Described lubricant releasing agent is stearic acid
One or more in zinc, barium stearate, calcium stearate or molybdenum bisuphide；
7) compressing sample is positioned in inert gas shielding atmosphere, at 400 DEG C ~ 800 DEG C, is incubated 2 ~ 10 little
Time, furnace cooling, spraying, obtain ferrum tantnickel powder core.
Described passivator is phosphoric acid.Described insulating compound is Kaolin.Described lubricant releasing agent is 1:1 in mass ratio
The zinc stearate of ~ 1:5 mixing and barium stearate.Described step 2) and step 7) in noble gas be respectively nitrogen or argon.
The preparation method using the present invention can make the ferrum tantnickel powder core of μ=26 ~ 90, and its ring-like specification is ФOD=
6.35 ~ 132.54 mm, ФID=2.79 ~ 78.59 mm, Ht=2.79 ~ 25.40 mm(ФODFor powder core external diameter, ФIDFor magnetic powder
In-core footpath, HtFor powder core thickness).
The invention have the advantages that 1, processing technology simple, use equipment simple；2, in product Ni constituent content be 3 ~
20%, production cost higher flux powder core is substantially reduced；3 products adopting this method preparation, have the saturated magnetic strength of excellence
Answering intensity, when magnetic field intensity is 500 Oe, saturation induction density is up to 1.5T, good inductance value, higher quality factor and
Relatively low power attenuation, frequency is 50 kHz, BmWhen being 1000 Gs, loss is less than 400 mW/cm3.Product master prepared by the present invention
It is used for substituting high magnetic flux powder core, is widely used in the fields such as pfc circuit, power inductor, Switching Power Supply, UPS.
Accompanying drawing explanation
Fig. 1 is the SEM figure before the magnetic powder passivation that wet-grinding technology and relative device of the present invention prepares；
Fig. 2 is the SEM figure after the magnetic powder passivation that wet-grinding technology and relative device of the present invention prepares；
Fig. 3 is the SEM figure before the magnetic powder passivation that dry mill process of the present invention prepares；
Fig. 4 is the SEM figure after the magnetic powder passivation that dry mill process of the present invention prepares.
Detailed description of the invention
In the present invention, ferrum tantnickel powder uses ball-milling method powder process, and detailed process is as follows: by ingot iron, polysilicon, pure nickel
Join melting in vacuum melting furnace, obtain alloy cast ingot；Hammering alloy cast ingot is broken into 5 mm particles below, then will
Granule after Po Sui is put into and is carried out ball milling in planetary ball mill.Two kinds of different ball-milling technologies are used to prepare ferrum tantnickel powder:
1) using wet-grinding technology and relative device powder process, in ball grinder, addition ethanol is as grinding aid, and ball milling parameter is ratio of grinding media to material 10:1, and ball mill turns
Speed 300 r/min, Ball-milling Time 10 h；2) using dry mill process powder process, be not added with any grinding aid, ball milling parameter is ratio of grinding media to material 8:
1, drum's speed of rotation 300 r/min, Ball-milling Time 2 h.Ball milling obtains the alloy powder of-100 mesh after terminating, then by this alloy
In powder is positioned over the heat-treatment furnace of inert gas shielding, 400 ~ 700 DEG C of insulation 1 ~ 5 h carry out stress relief annealing process, are moved back
Ferrum tantnickel powder after fire.Ferrum tantnickel powder after annealing is carried out grain size proportion according to certain ratio, through Passivation Treatment
After, add compression molding after insulating adhesive and lubricant releasing agent, in inert gas shielding atmosphere, finally carry out destressing move back
Fire processes and i.e. can be made into ferrum tantnickel powder core.
Embodiment 1
By dry mill process prepare ferrum tantnickel powder (containing Si 5%, Ni 20%, Al 0.01%, Ca 0.05%, C 0.02%,
Surplus is Fe), make annealing treatment in being positioned over the heat-treatment furnace of nitrogen protection atmosphere, annealing temperature is 700 DEG C, annealing time
It is 1 h.Ferrum tantnickel powder after annealing carries out proportioning according to following granularity: the granule of-100 mesh ~+200 mesh accounts for the 30% of total amount；-
The granule of 200 mesh ~+300 mesh accounts for the 40% of total amount；The granule of-300 mesh ~+400 mesh accounts for the 20% of total amount；Remaining is-400 purposes
Grain, accounts for the 10% of total amount.Add in the ferrum tantnickel powder prepared and account for the phosphoric acid of ferrum tantnickel powder quality 1.8% and be passivated place
Reason, the Kaolin add the magnetic particle colloid acetone soln accounting for ferrum tantnickel powder quality 0.5%, accounting for ferrum tantnickel powder quality 0.8%, stirs
Mix uniformly, carry out insulation adhesive cladding, be subsequently adding zinc stearate and the tristearin of 0.25% accounting for ferrum tantnickel powder quality 0.25%
Acid barium makees lubricant releasing agent, makes molding powder after mix homogeneously.Molding powder is positioned over 100 T hydraulic press for powder formation
On, at 20 t/cm2Pressure under be pressed into ring-like sample, the external diameter of magnet ring is 23.6 mm, and internal diameter is 14.4 mm, and thickness is
8.89 mm.Prepared ring-like sample average is divided into 5 parts, numbering 1 ~ 5, it is positioned in the heat-treatment furnace of argon atmosphere,
It is incubated 2 h, 4 h, 6 h, 8 h and 10 h, furnace cooling, spraying at 700 DEG C respectively, obtains target product.
After testing, the relevant electromagnetic parameter of target product such as table 1:
Table 1
Embodiment 2
By dry mill process prepare ferrum tantnickel powder (containing Si 10%, Ni 15%, Al 0.2%, Ca 0.01%, C 0.05%,
Surplus is Fe), make annealing treatment in being positioned over the heat-treatment furnace of nitrogen protection atmosphere, annealing temperature is 400 DEG C, annealing time
It is 5 h.Ferrum tantnickel powder after annealing carries out proportioning according to following granularity: the granule of-100 mesh ~+200 mesh accounts for the 10% of total amount；-
The granule of 200 mesh ~+300 mesh accounts for the 35% of total amount；The granule of-300 mesh ~+400 mesh accounts for the 35% of total amount；Remaining is-400 purposes
Grain accounts for the 20% of total amount.The ferrum tantnickel powder prepared is divided into 5 parts, numbering 1 ~ 5, it is separately added into and accounts for ferrum tantnickel powder quality
0.2%, the chromic acid of 0.6%, 1.0%, 1.4% and 1.8% is passivated processing, and adds the magnetic powder accounting for ferrum tantnickel powder quality 1.0%
Glue acetone soln, account for the mica powder of ferrum tantnickel powder quality 1.0%, stir, carry out insulation adhesive cladding, be subsequently adding and account for
The zinc stearate of ferrum tantnickel powder quality 0.25% and the barium stearate of 1.25% make lubricant releasing agent, make molding after mix homogeneously
Powder.Molding powder is positioned on 100 T hydraulic press for powder formation, at 28 t/cm2Pressure under be pressed into ring-like sample,
The external diameter of magnet ring is 23.6 mm, and internal diameter is 14.4 mm, and thickness is 8.89 mm.Finally magnet ring is positioned over argon atmosphere
Heat-treatment furnace in, be incubated 4 h at 700 DEG C, furnace cooling, spraying, obtain target product.
After testing, the relevant electromagnetic parameter of target product such as table 2:
Table 2
Embodiment 3
The ferrum tantnickel powder prepared by wet-grinding technology and relative device is (containing Si 20%, Ni 8%, Al 0.05%, Ca 0.2%, C 0.02%, remaining
Amount is Fe), make annealing treatment in being positioned over the heat-treatment furnace of nitrogen protection atmosphere, annealing temperature is 500 DEG C, and annealing time is
3 h.Ferrum tantnickel powder after annealing carries out proportioning according to following granularity: the granule of-100 mesh ~+200 mesh accounts for the 20% of total amount；-
The granule of 200 mesh ~+300 mesh accounts for the 50% of total amount；The granule of-300 mesh ~+400 mesh accounts for the 15% of total amount；Remaining is-400 purposes
Grain accounts for the 15% of total amount.Add in the ferrum tantnickel powder prepared and account for the hydrogen peroxide of ferrum tantnickel powder quality 0.2% and be passivated place
Reason, the Kaolin add the magnetic particle colloid acetone soln accounting for ferrum tantnickel powder quality 1.5%, accounting for ferrum tantnickel powder quality 0.02%,
Stir, carry out insulation adhesive cladding, be subsequently adding the calcium stearate and the two of 0.25% accounting for ferrum tantnickel powder quality 0.25%
Molybdenum sulfide makees lubricant releasing agent, makes molding powder after mix homogeneously.Molding powder is positioned over 100 T hydraulic press for powder formation
On, at 12 t/cm2Pressure under be pressed into ring-like sample, the external diameter of magnet ring is 23.6 mm, and internal diameter is 14.4 mm, and thickness is
8.89 mm.Prepared sample average is divided into 5 parts, numbering 1 ~ 5, it is positioned in the heat-treatment furnace of argon atmosphere, exists respectively
It is incubated 2 h, furnace cooling, spraying at 400 DEG C, 500 DEG C, 600 DEG C, 700 DEG C and 800 DEG C, obtains target product.
After testing, the relevant electromagnetic parameter of target product such as table 3:
Table 3
Embodiment 4
By wet-grinding technology and relative device prepare ferrum tantnickel powder (containing Si 30%, Ni 3%, Al 0.05%, Ca 0.05%, C 0.02%,
Surplus is Fe), make annealing treatment in being positioned over the heat-treatment furnace of nitrogen protection atmosphere, annealing temperature is 500 DEG C, annealing time
It is 2 h.Ferrum tantnickel powder after annealing carries out proportioning according to following granularity: the granule of-100 mesh ~+200 mesh accounts for the 20% of total amount；-
The granule of 200 mesh ~+300 mesh accounts for the 40% of total amount；The granule of-300 mesh ~+400 mesh accounts for the 25% of total amount；Remaining is-400 purposes
Grain accounts for the 15% of total amount.Add in the ferrum tantnickel powder prepared and account for the phosphoric acid of ferrum tantnickel powder quality 1.0% and be passivated processing,
The Pulvis Talci add the magnetic particle colloid acetone soln accounting for ferrum tantnickel powder quality 2.0%, accounting for ferrum tantnickel powder quality 0.2%, stirring
Uniformly, carry out insulation adhesive cladding, be subsequently adding zinc stearate and the stearic acid of 0.75% accounting for ferrum tantnickel powder quality 0.25%
Barium makees lubricant releasing agent, makes molding powder after mix homogeneously.Molding powder is divided into 5 parts, numbering 1 ~ 5, it is positioned over
On 100T hydraulic press for powder formation, respectively at 12 t/cm2、16 t/cm2、20 t/cm2、24 t/cm2With 28 t/cm2Pressure
Under be pressed into ring-like sample, the external diameter of magnet ring is 23.6 mm, and internal diameter is 14.4 mm, and thickness is 8.89 mm.Finally magnet ring is put
It is placed in the heat-treatment furnace of argon atmosphere, is incubated 8 h, furnace cooling, spraying at 700 DEG C, obtains target product.
After testing, the relevant electromagnetic parameter of target product such as table 4:
Table 4
Claims (4)
1. the preparation method of a ferrum tantnickel powder core, it is characterised in that comprise the steps:
1) using vacuum melting furnace smelting iron silicon nickel alloy ingot casting, by percentage to the quality, the chemical composition of alloy cast ingot is Si
5 ~ 30%, Ni 3 ~ 20%, Al 0.01 ~ 0.2%, Ca 0.01 ~ 0.2%, C≤0.05%, surplus is Fe；
2) above-mentioned alloy cast ingot is positioned over nitrogen or argon after Mechanical Crushing, the ferrum tantnickel powder of ball milling one-tenth-100 mesh
Making annealing treatment in the heat-treatment furnace of protective atmosphere, annealing temperature is 400 ~ 700 DEG C, and annealing time is 1 ~ 5 h；
3) by prepared ferrum tantnickel powder in following ratio :-100 mesh ~+200 mesh account for 10 ~ 30% ,-200 mesh ~+300 of gross mass
Mesh accounts for the 35 ~ 50% of gross mass, and-300 mesh ~+400 mesh account for 15 ~ 35% ,-400 mesh of gross mass and account for the 5 ~ 20% of gross mass and carry out grain
Degree proportioning；
4) toward step 3) the ferrum tantnickel powder for preparing adds account for the passivator of ferrum tantnickel powder quality 0.2 ~ 1.8% and be passivated
Process；Described passivator is one or more in phosphoric acid, chromic acid or hydrogen peroxide；
5) after Passivation Treatment completes, the magnetic particle colloid solution accounting for ferrum tantnickel powder quality 0.2 ~ 2.0% of addition acetone as solvent
And account for the insulating compound of ferrum tantnickel powder quality 0.02 ~ 1.0%, it is sufficiently stirred for, carries out insulation adhesive cladding；Described insulating compound is
One or more in Kaolin, mica powder or Pulvis Talci；
6), after insulating wrapped completes, the lubricant releasing agent accounting for ferrum tantnickel powder quality 0.1 ~ 1.5% is added, mix homogeneously,
12~28 t/cm2Pressure under compressing, obtain compressing sample；Described lubricant releasing agent is zinc stearate, hard
One or more in fat acid barium, calcium stearate or molybdenum bisuphide；
7) compressing sample is positioned in nitrogen or argon atmosphere, at 400 DEG C ~ 800 DEG C, is incubated 2 ~ 10 little
Time, furnace cooling, spraying, obtain ferrum tantnickel powder core.
The preparation method of a kind of ferrum tantnickel powder core the most according to claim 1, it is characterised in that described passivator is
Phosphoric acid.
The preparation method of a kind of ferrum tantnickel powder core the most according to claim 1, it is characterised in that described insulating compound is
Kaolin.
The preparation method of a kind of ferrum tantnickel powder core the most according to claim 1, it is characterised in that described lubricating release
Agent is zinc stearate and the barium stearate of the mixing of 1:1 ~ 1:5 in mass ratio.
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| KR102068972B1 (en) * | 2015-05-14 | 2020-01-22 | 티디케이가부시기가이샤 | Soft magnetic metal powder and soft magnetic metal dust core |
| CN109680210B (en) * | 2018-12-18 | 2020-03-20 | 横店集团东磁股份有限公司 | Preparation method of mu = 150-250 sendust soft magnetic powder core |
| CN112652437A (en) * | 2021-01-15 | 2021-04-13 | 江苏瑞德磁性材料有限公司 | Preparation method of metal soft magnetic powder core with low forming pressure and high production efficiency |
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| US5755986A (en) * | 1995-09-25 | 1998-05-26 | Alps Electric Co., Ltd. | Soft-magnetic dielectric high-frequency composite material and method for making the same |
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