CN108097977A - A kind of plasma atomization preparation method of iron-silicon-aluminum soft magnet alloy powder - Google Patents

A kind of plasma atomization preparation method of iron-silicon-aluminum soft magnet alloy powder Download PDF

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Publication number
CN108097977A
CN108097977A CN201810101374.0A CN201810101374A CN108097977A CN 108097977 A CN108097977 A CN 108097977A CN 201810101374 A CN201810101374 A CN 201810101374A CN 108097977 A CN108097977 A CN 108097977A
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iron
plasma
master alloy
silicon
soft magnet
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CN108097977B (en
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徐有为
蔡勇
唐中飞
范海强
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Guangdong Rick Micro Metal Magnetoelectric Technology Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/14Making metallic powder or suspensions thereof using physical processes using electric discharge
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/06Metallic powder characterised by the shape of the particles
    • B22F1/065Spherical particles
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/02Ferrous alloys, e.g. steel alloys containing silicon
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/06Ferrous alloys, e.g. steel alloys containing aluminium

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  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Nanotechnology (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

A kind of plasma the present invention provides iron-silicon-aluminum soft magnet alloy powder is atomized preparation method, comprises the following steps:Pure iron, metallic silicon and electrolysis aluminium ingot are by the standard component of Sendust after melting homogenizes, direct casting forms master alloy plate or band, plate or thickness of strip are less than 10 millimeters, pouring steel temperature must control between 1,380 1480 DEG C, pouring mold easily makes the design of molten steel rapid condensation for water cooled copper mould etc., purpose be make to be formed the grain size of master alloy is less than 1 millimeter, the composition segregation that three kinds of elements of iron sial is avoided to be generated due to crystallization process, ensure that the composition of subsequent atomized powder unanimously controls the standard component in Sendust, i.e.,:Silicone content 9.6% ± 0.2%, aluminium content 5.4% ± 0.2%, remaining as iron.Present invention employs the methods that high frequency preheats master alloy, it is difficult the power problem for melting a large amount of metals in a short time to solve plasma generator, the power of required plasma generator only needs 80 kilowatts, it is not necessary to using the special ultra high power plasma generator of import.

Description

A kind of plasma atomization preparation method of iron-silicon-aluminum soft magnet alloy powder
Technical field
The invention belongs to the metal soft magnetic alloy materials in functional material, and in particular to a kind of iron-silicon-aluminum soft magnet alloy powder Plasma atomization preparation method.
Background technology
Metal soft magnetic alloy powder is serial because having extremely low power loss characteristic and preferable DC superposition characteristic, Extensive use on the household electrical appliance such as photovoltaic inversion, direct-current charging post, pfc circuit, energy-saving frequency conversion air-conditioning, meets electronic component It is efficient, energy saving and miniaturization demand.
Wherein iron silica-alumina material has minimum power loss characteristic and relatively low cost advantage, but in some new light During lying prostrate inversion, the use of energy-saving frequency conversion air-conditioning, its DC superposition characteristic only has 45%-50%, and (magnetic conductivity 60, superposition are straight Flow field 100Oe, similarly hereinafter) cause resistance to large current characteristic bad, the requirement of design is not achieved;There is iron silicon materials outstanding direct current to fold Add characteristic, up to 70%-76%, but its power attenuation is larger, easily generates Wen Sheng, is used so as to affect;Iron nickel material With relatively low power attenuation, it may have excellent DC superposition characteristic (75%-80%) simply contains higher expensive material Nickel is affected and promoted the use of, therefore a kind of while have relatively low power attenuation, outstanding DC superposition characteristic, have a price The powder body material of lattice competitiveness, it is extremely important for the design of new energy magnet assembly.
At present the technical solution adopted is that, iron sial is obtained using nitrogen high-pressure atomization iron sial high-temperature molten steel Spherical powder, and produced in batches.But due in iron silica-alumina material, containing the gold for being relatively easy to oxidation at high temperature Belong to aluminium, content, so if in the case of without atmosphere protection, carries out alloy melting, due to the oxygen of aluminium in 5.0%-5.6% To change so that the viscosity of molten steel increases, and mobility is deteriorated, during by the leting slip a remark of 4-8 mm pore sizes, easy plug-hole, steel Water no longer flows down so that aerosolization operation stops.Therefore it can smoothly flow out and let slip a remark to iron sial molten steel, it is necessary to iron sial Molten steel carries out the processing of air-isolation, such as vacuum melting, atmosphere protection etc., so that and smelting operation is cumbersome, it is difficult to It continuously and efficiently produces, exception sometimes occurs, can operation be stopped completely, cost increases.
The domestic report being also related to using plasma atomization iron sial plasma atomization and research, but same problem It is, if iron sial high-temperature molten steel decontamination is not net or cools down, the factors such as molten steel viscosity height, in molten steel by 4-8 millimeters of leakages During mouth, there is a situation where blocking package is equally higher probability, cause the increase of production cost, the decline of yield, investment Cost is also more huge.
The content of the invention
The shortcomings that it is a primary object of the present invention to overcome the prior art and deficiency, provide a kind of iron-silicon-aluminum soft magnet alloyed powder The plasma atomization preparation method at end, steadily high-volume efficiently can produce iron-silicon-aluminum soft magnet alloy powder, the pole of acquisition Good powder sphericity.
In order to achieve the above object, the present invention uses following technical scheme:
A kind of plasma atomization preparation method of iron-silicon-aluminum soft magnet alloy powder of the present invention, comprises the following steps:
S1, by pure iron, metallic silicon and electrolysis aluminium ingot by Sendust standard component by melting it is uniform, direct casting shape Into master alloy plate or band, the control of steel temperature is poured between 1380-1480 DEG C, pours mold easily to make pouring for molten steel rapid condensation Mold designs so that the grain size for forming master alloy plate or band is less than 1 millimeter;
S2, by autoloader, the continuous iron sial master alloy band or plate step-by-step movement of formation are sent into high frequency Heating interval between master alloy is heated rapidly to 900-1100 DEG C, avoids the heating time long oxygen content for causing master alloy Increase, subsequently into the plasma nebulization region of argon medium;
S3, after the iron sial master alloy between high frequency is heated rapidly to 900-1100 degree enters plasma range of atomization, Using 80-150 kilowatts of plasma generator, as medium, spray gun alignment master alloy carries out injection heating for argon gas or nitrogen;
S4, spray gun do straight reciprocating motion, and the direction of motion is vertical with master alloy step direction, and torch flame mouth leaves female conjunction Between the distance of gold is 3-15 millimeters;
S5, the stepping rate of iron sial master alloy are matched with the translational speed of plasma spraying rifle, and pass through adjusting The power and argon flow amount of gas occur for plasma, to adjust the granularity of iron sial atomized powder and its distribution, in order to improve atomization Efficiency, the maximum particle diameter of iron sial atomized powder is 97 microns, obtains optimal magnetic core Bs;
S6, an argon gas circulating cooling system is set, bottom is arranged into gas, and plasma spraying position is past inside atomisation tower It is down nitrogen gas outlet, cooling cycle wind achievees the purpose that cooling through over-heat-exchanger, while argon gas after cooling or nitrogen can Cooling and nodularization process are formed to the iron aluminum silicon powder body after plasma jet atomization.
As preferred technical solution, in step S1, the standard component of the Sendust is as follows:
Silicone content 9.6% ± 0.2%, aluminium content 5.4% ± 0.2%, remaining as iron.
As preferred technical solution, in step S1, the mold that pours is water cooled copper mould.
As preferred technical solution, in step S1, the casting forms the thickness of master alloy plate or band in 5-30 Between millimeter.
As preferred technical solution, in step S2, the master alloy plate or band are using high-frequency heating mode, rapidly 1000 DEG C are heated to, reduces the output power of plasma generator.
As preferred technical solution, in step S6, the flow of circulating cooling wind is provided at 300-1200 cubic meters/hour.
Compared with prior art, the present invention having the following advantages that and advantageous effect:
1st, the present invention innovatively makes iron sial plate or banding master alloy using traditional casting process, controls master alloy Thickness be less than 10 millimeters, master alloy is evenly sent by heating zone by autoloader, mode of heating uses high-frequency heating, Master alloy is rapidly heated to 900-1100 degree, then enters back into plasma range of atomization, argon gas after plasma gun by forming High-temperature plasma air-flow forms high-temperature injection, since sendust has been preheated to the iron sial master alloy after heating 900-1100 degree, all iron sial master alloys are easily created liquid metal, at this time liquid iron sial be brought rapidly up to 1360-1500 degree or so, and be atomized by high-temperature plasma injection stream, the iron sial by atomization is gradually cooled down in spray chamber, cold But the phenomenon that during due to surface tension, continuous cooling meat globulate powder.This technique passes through 4-8 due to avoiding molten steel The throttle orifice of millimeter, there is no the phenomenon that blocking package, simultaneously because employing the method that high frequency preheats master alloy, solve etc. from Electronic generator is difficult the power problem for melting a large amount of metals in a short time, and the power of required plasma generator only needs 80 kilowatts, it is not necessary to using the special ultra high power plasma generator of import.
2nd, present invention obviates the current limliting leak that iron sial molten steel has to pass through 4-8 millimeters, blocking package phenomenon will not be generated, no Stringent vacuum or atmosphere protection melting and casting are needed, can continuously carry out atomization production, improves production effect Rate;
Description of the drawings
Fig. 1 is the structure diagram of plasma atomization device for making of the present invention.
Fig. 2 is plasma atomization preparation method flow chart of the present invention.
Specific embodiment
With reference to embodiment and attached drawing, the present invention is described in further detail, but embodiments of the present invention are unlimited In this.
Embodiment 1
The plasma atomization preparation method of iron-silicon-aluminum soft magnet alloy powder, pure iron, metallic silicon and electrolytic aluminium in the present embodiment For ingot by the standard component of Sendust after melting homogenizes, direct casting forms master alloy plate or band, plate or band Thickness is less than 10 millimeters, and pouring steel temperature must control between 1380-1480 DEG C, and pour mold easily makes molten steel fast for water cooled copper mould etc. The design that quickly cooling is coagulated, it is therefore an objective to make to be formed the grain size of master alloy is less than 1 millimeter, avoid three kinds of elements of iron sial due to crystallization The composition segregation that process generates ensures that the composition of subsequent atomized powder unanimously controls the standard component in Sendust, i.e.,:Silicon Content 9.6% ± 0.2%, aluminium content 5.4% ± 0.2%, remaining as iron.
As shown in Figure 1, in the plasma atomising device that the present embodiment 1 uses, by autoloader 1, by the company of formation Continuous iron sial master alloy band or plate step-by-step movement are sent into high-frequency heating section 2, and master alloy is heated rapidly to 900-1100 Between DEG C, the increase of the heating time long oxygen content for causing master alloy is avoided, is atomized subsequently into the plasma of argon medium Region 3, between plasma gun leaves most preferably 15-45 millimeters of the distance of master alloy, plasma gun moves back and forth, and is closed with mother The direction that gold advances is vertical in 90 degree, and master alloy is constantly atomized into powder by plasma jet, by coordinating master alloy feeding fast.
As shown in Fig. 2, the present embodiment comprises the following steps:
S1, pure iron, metallic silicon and electrolysis aluminium ingot are pressed into the standard component of Sendust (i.e.:Silicone content 9.6% ± 0.2%, Aluminium content 5.4% ± 0.2%, remaining as iron) it is uniform by melting, direct casting forms master alloy plate or band, plate or At 5~30 millimeters, pouring steel temperature must control between 1380-1480 DEG C thickness of strip, and pour mold easily makes for water cooled copper mould etc. The grain size for the master alloy that the design of molten steel rapid condensation is formed is less than 1 millimeter;
S2, by autoloader, the continuous iron sial master alloy band or plate step-by-step movement of formation are sent into high frequency Heating interval between master alloy is heated rapidly to 900-1100 DEG C, avoids the heating time long oxygen content for causing master alloy Increase, subsequently into the plasma nebulization region of argon medium;
S3, after the iron sial master alloy between high frequency is heated rapidly to 900-1100 degree enters plasma range of atomization, Using 80-150 kilowatts of plasma generator, as medium, spray gun alignment master alloy carries out injection heating for argon gas or nitrogen;
S4, spray gun do straight reciprocating motion, and the direction of motion is vertical with master alloy step direction, and torch flame mouth leaves female conjunction Between the distance of gold is 3-15 millimeters;
S5, the stepping rate of iron sial master alloy are matched with the translational speed of plasma spraying rifle, and pass through adjusting The power and argon flow amount of gas occur for plasma, to adjust the granularity of iron sial atomized powder and its distribution, in order to improve atomization Efficiency, the maximum particle diameter of iron sial atomized powder is 97 microns, obtains optimal magnetic core Bs;
S6, an argon gas circulating cooling system is set, bottom is arranged into gas, and plasma spraying position is past inside atomisation tower Down for nitrogen gas outlet, the flow regulation of the circulating cooling wind of this patent requirement is at 300-1200 cubic meters/hour, cooling cycle wind Achieve the purpose that cooling through over-heat-exchanger, while argon gas after cooling or nitrogen can be to the iron sial after plasma jet atomization Powder forms cooling and nodularization process.
Embodiment 2
The plasma atomising device of the present embodiment 2 uses and the identical device of embodiment 1, in addition to following technical characteristics, His technical characteristic is same as Example 1.
The plasma atomization preparation method of the present embodiment 2 concretely comprises the following steps:Iron sial master alloy sheet metal thickness is taken as 20 millis Rice, 200 millimeters of width, with 5 millimeters/10 seconds/time of stepping rate by high-frequency heating area, the temperature after master alloy is heated is 950-1050 DEG C, for the power that plasma generator is set as 65 kilowatts, argon gas is medium, generates plasma high temperature gas flow and mother is closed Gold carries out jet atomization, and plasma gun at the uniform velocity moves, the movement of completion 200 millimeters/10 seconds, and the distance of spray gun and master alloy is 5 centimetres.Interior circulating cooling argon gas stream is 400 cubes of ms/h of
Plasma spraying atomization result be:The speed that powder is collected reaches 50 kgs/hour, and powder passes through 150 mesh sieves After net, screenings weight is 46 kilograms, and the apparent density of spherical iron sial powder has reached 4.2-4.4 grams/cc, spherical shape Degree is very good, and the oxygen content of powder is 500-600ppm.
Iron aluminum silicon powder system after being atomized with this plasma is made magnetic core, 26.9 grams of magnet ring weight, magnetic conductivity 61, Under the test condition of 50Khz@100mT, the power attenuation that measures is 256mW/cm3, in the case of the external dc field of 100Oe, Inductance drops to as the 64.1% of original inductance, and magnetic core performance is very outstanding.
Embodiment 3
The plasma atomising device of the present embodiment 3 uses and the identical device of embodiment 1, in addition to following technical characteristics, His technical characteristic is same as Example 1.
The plasma of the present embodiment 3 is atomized preparation method:Iron sial master alloy sheet metal thickness is 20 millimeters, width 200 millimeters, with 5 millimeters/5 seconds/time of stepping rate by high-frequency heating area, the temperature after master alloy is heated is 950-1050 DEG C, 2 plasma generators are designed, for the respective power set as 60 kilowatts, argon gas is medium, generates plasma high temperature gas flow Jet atomization, the at the uniform velocity mobile shifting done opposite uniform motion, complete 100 millimeters/5 seconds of 2 plasma guns are carried out to master alloy Dynamic, the distance of spray gun and master alloy is 5 centimetres.Interior circulating cooling argon gas stream is relatively real for 600 cubes of ms/h of the present embodiment It applies for example 1, mainly employs 2 plasma gunes, for improving plasma atomization speed, improve production capacity.
Plasma spraying atomization result be:The speed that powder is collected reaches 80-100 kgs/hour, and powder passes through 150 After mesh screen, screenings weight is 70-85 kilograms, and the apparent density of spherical iron sial powder has reached 4.2-4.4 grams/cube li Rice, sphericity is very good, and the oxygen content of powder is 450-580ppm.
Iron aluminum silicon powder system after being atomized with this plasma is made magnetic core, 27.02 grams of magnet ring weight, magnetic conductivity 63, Under the test condition of 50Khz@100mT, the power attenuation that measures is 263mW/cm3, in the case of the external dc field of 100Oe, Inductance drops to as the 62.4% of original inductance, and magnetic core performance is very outstanding.
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention and from above-described embodiment Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine, simplification, Equivalent substitute mode is should be, is included within protection scope of the present invention.

Claims (6)

1. the plasma atomization preparation method of a kind of iron-silicon-aluminum soft magnet alloy powder, which is characterized in that comprise the following steps:
S1, by pure iron, metallic silicon and electrolysis aluminium ingot by Sendust standard component by melting it is uniform, direct casting forms mother Sheet alloy or band pour the control of steel temperature between 1380-1480 DEG C, pour mold be easily make molten steel rapid condensation pour mold Design so that the grain size for forming master alloy plate or band is less than 1 millimeter;
S2, by autoloader, the continuous iron sial master alloy band or plate step-by-step movement of formation are sent into high-frequency heating Section between master alloy is heated rapidly to 900-1100 DEG C, avoids the increasing of the heating time long oxygen content for causing master alloy Add, subsequently into the plasma nebulization region of argon medium;
S3, after the iron sial master alloy between high frequency is heated rapidly to 900-1100 degree enters plasma range of atomization, use 80-150 kilowatts of plasma generator, argon gas or nitrogen carry out injection heating as medium, spray gun alignment master alloy;
S4, spray gun do straight reciprocating motion, and the direction of motion is vertical with master alloy step direction, and torch flame mouth leaves master alloy Between distance is 3-15 millimeters;
S5, the stepping rate of iron sial master alloy are matched with the translational speed of plasma spraying rifle, and pass through adjusting etc. from The power and argon flow amount of gas occur for son, to adjust the granularity of iron sial atomized powder and its distribution, in order to improve nebulization efficiency, The maximum particle diameter of iron sial atomized powder is 97 microns, obtains optimal magnetic core Bs;
One argon gas circulating cooling system is set inside S6, atomisation tower, and bottom is arranged into gas, and plasma spraying position is down Nitrogen gas outlet, cooling cycle wind achievees the purpose that cooling through over-heat-exchanger, while argon gas after cooling or nitrogen can equities Iron aluminum silicon powder body after ion jet atomization forms cooling and nodularization process.
2. the plasma atomization preparation method of iron-silicon-aluminum soft magnet alloy powder according to claim 1, which is characterized in that step In S1, the standard component of the Sendust is as follows:
Silicone content 9.6% ± 0.2%, aluminium content 5.4% ± 0.2%, remaining as iron.
3. the plasma atomization preparation method of iron-silicon-aluminum soft magnet alloy powder according to claim 1, which is characterized in that step In S1, the mold that pours is water cooled copper mould.
4. the plasma atomization preparation method of iron-silicon-aluminum soft magnet alloy powder according to claim 1, which is characterized in that step In S1, the thickness for forming master alloy plate or band of casting is between 5-30 millimeters.
5. the plasma atomization preparation method of iron-silicon-aluminum soft magnet alloy powder according to claim 1, which is characterized in that step In S2, the master alloy plate or band are heated rapidly to 1000 DEG C, are reduced plasma generator using high-frequency heating mode Output power.
6. the plasma atomization preparation method of iron-silicon-aluminum soft magnet alloy powder according to claim 1, which is characterized in that step In S6, the flow of circulating cooling wind is provided at 300-1200 cubic meters/hour.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114517015A (en) * 2020-11-20 2022-05-20 洛阳尖端技术研究院 Wave-absorbing composition, wave-absorbing material and preparation method thereof

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CN106115705A (en) * 2016-06-27 2016-11-16 乌克兰巴顿焊接研究所 A kind of infusibility tungsten carbide wc+W2the preparation method of C spherical powder
CN107175337A (en) * 2017-05-22 2017-09-19 加拿大艾浦莱斯有限公司 A kind of metal powder preparation method and its device based on plasma atomization technique

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CN103068731A (en) * 2010-05-18 2013-04-24 爱科控股公司 Spherical powder and its preparation
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Publication number Priority date Publication date Assignee Title
CN114517015A (en) * 2020-11-20 2022-05-20 洛阳尖端技术研究院 Wave-absorbing composition, wave-absorbing material and preparation method thereof

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