CN108097977B - Plasma atomization preparation method of Fe-Si-Al soft magnetic alloy powder - Google Patents

Plasma atomization preparation method of Fe-Si-Al soft magnetic alloy powder Download PDF

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CN108097977B
CN108097977B CN201810101374.0A CN201810101374A CN108097977B CN 108097977 B CN108097977 B CN 108097977B CN 201810101374 A CN201810101374 A CN 201810101374A CN 108097977 B CN108097977 B CN 108097977B
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master alloy
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strip
silicon
iron
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CN108097977A (en
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徐有为
蔡勇
唐中飞
范海强
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Guangdong Mirrack Micro Metal Magnetoelectric Technology Co ltd
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Guangdong Mirrack 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)
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  • Organic Chemistry (AREA)
  • Nanotechnology (AREA)
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Abstract

The invention provides a plasma atomization preparation method of Fe-Si-Al soft magnetic alloy powder, which comprises the following steps: after smelting and homogenizing pure iron, metal silicon and an electrolytic aluminum ingot according to the standard components of Sendust, continuously casting to form a master alloy plate or strip, wherein the thickness of the plate or strip is less than 10 mm, the steel casting temperature must be controlled between 1380 and 1480 ℃, a casting die is a water-cooling copper die and the like which are easy to rapidly condense molten steel, the aim is to ensure that the grain size of the formed master alloy is less than 1 mm, avoid the component segregation of three elements of iron-silicon-aluminum due to the crystallization process, ensure that the components of subsequent atomized powder are consistently controlled in the Sendust standard components, namely: 9.6% + -0.2% of silicon, 5.4% + -0.2% of aluminum and the balance of iron. The invention adopts a method of preheating the master alloy by high frequency, solves the power problem that a plasma generator is difficult to melt a large amount of metal in a short time, and the required power of the plasma generator only needs 80 kilowatts without adopting an imported ultrahigh power plasma generator.

Description

Plasma atomization preparation method of Fe-Si-Al soft magnetic alloy powder
Technical Field
The invention belongs to a metal soft magnetic alloy material in a functional material, and particularly relates to a plasma atomization preparation method of Fe-Si-Al soft magnetic alloy powder.
Background
The metal soft magnetic alloy powder series has extremely low power loss characteristic and good direct current superposition characteristic, is widely applied to household appliances such as photovoltaic inversion, direct current charging piles, PFC circuits, energy-saving variable frequency air conditioners and the like, and meets the requirements of high efficiency, energy conservation and miniaturization of electronic components.
The iron-silicon-aluminum material has the characteristics of lowest power loss and lower cost, but in the use process of some new photovoltaic inversion and energy-saving variable frequency air conditioners, the direct current superposition characteristics of the iron-silicon-aluminum material are only 45% -50% (magnetic permeability 60, superposition direct current field 100Oe, the same below) so that the high-current resistance characteristics are poor and the design requirements cannot be met; the iron-silicon material has excellent direct current superposition characteristics which reach 70% -76%, but the iron-silicon material has large power loss and is easy to generate temperature rise, thereby influencing the use; the iron-nickel material has low power loss and excellent direct current superposition characteristics (75% -80%), only contains high-cost material nickel, and influences popularization and use, so that the powder material which has low power loss, excellent direct current superposition characteristics and certain price competitiveness simultaneously is very important for the design of new energy magnetic components.
The technical scheme adopted at present is that ferrosilicon aluminum spherical powder is obtained by atomizing ferrosilicon aluminum high-temperature molten steel under high pressure by using nitrogen, and batch production is obtained. However, since the ferrosilicon aluminum material contains metallic aluminum which is easily oxidized at a high temperature, and the content is 5.0% to 5.6%, if alloy smelting is carried out without atmosphere protection, the viscosity of molten steel is increased and the fluidity is deteriorated due to the oxidation of aluminum, and during the process of passing through a nozzle with a hole diameter of 4 to 8 mm, the hole is easily blocked, the molten steel does not flow down any more, and the gas atomization operation is stopped. Therefore, in order to make the sendust water smoothly flow out of the discharge spout, air-isolation treatment such as vacuum melting, atmosphere protection and the like must be performed on the sendust water, so that the melting operation is troublesome, continuous and efficient production is difficult, and sometimes, an abnormality occurs, so that the operation is completely stopped, and the cost is increased.
The report and research about plasma atomization by adopting plasma atomization of Fe-Si-Al are also reported and researched in China, but the same problem is that if impurities of Fe-Si-Al high-temperature molten steel are not completely removed, or the molten steel is cooled, the viscosity of the molten steel is high, and the probability of package blockage is high in the process that the molten steel passes through a 4-8 mm discharge spout, so that the production cost is increased, the yield is reduced, and the investment cost is huge.
Disclosure of Invention
The invention mainly aims to overcome the defects of the prior art and provide a plasma atomization preparation method of Fe-Si-Al soft magnetic alloy powder, which can stably produce Fe-Si-Al soft magnetic alloy powder in a large scale and high efficiency and obtain excellent powder sphericity.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention relates to a plasma atomization preparation method of Fe-Si-Al soft magnetic alloy powder, which comprises the following steps:
s1, smelting pure iron, metallic silicon and an electrolytic aluminum ingot uniformly according to the standard components of Sendust, continuously casting to form a master alloy plate or strip, controlling the steel casting temperature to be 1380-1480 ℃, and designing a casting mold which is easy to rapidly condense molten steel so that the grain size of the formed master alloy plate or strip is less than 1 mm;
s2, feeding the formed continuous iron-silicon-aluminum master alloy strip or plate into a high-frequency heating region step by step through an automatic feeder, rapidly heating the master alloy to 900-1100 ℃ to avoid the increase of the oxygen content of the master alloy caused by overlong heating time, and then feeding the master alloy into a plasma atomization region of an argon medium;
s3, after the Fe-Si-Al master alloy which is rapidly heated to 900-1100 ℃ by high frequency enters a plasma atomization zone, a plasma generator of 80-150 kilowatt is adopted, argon or nitrogen is used as a medium, and a spray gun is aligned to the master alloy for spray heating;
s4, the spray gun makes linear reciprocating motion, the motion direction is vertical to the stepping direction of the master alloy, and the distance between the flame opening of the spray gun and the master alloy is 3-15 mm;
s5, matching the stepping speed of the Fe-Si-Al master alloy with the moving speed of a plasma spray gun, and adjusting the particle size and the distribution of Fe-Si-Al atomized powder by adjusting the power of plasma generated gas and the flow of argon gas, wherein in order to improve the atomization efficiency, the maximum particle size of the Fe-Si-Al atomized powder is 97 microns, and the optimal magnetic core Bs is obtained;
s6, an argon circulating cooling system is arranged in the atomizing tower, the bottom of the argon circulating cooling system is arranged to be gas inlet, the plasma spraying part is downward to be a nitrogen gas outlet, cooling circulating air passes through a heat exchanger to achieve the cooling purpose, and meanwhile, cooled argon or nitrogen can form a cooling and spheroidizing process on the iron-silicon-aluminum powder after plasma spraying and atomizing.
As a preferred technical solution, in step S1, the standard components of Sendust are as follows:
9.6% + -0.2% of silicon, 5.4% + -0.2% of aluminum and the balance of iron.
Preferably, in step S1, the casting mold is a water-cooled copper mold.
Preferably, in step S1, the thickness of the plate or strip of the mother alloy formed by casting is between 5 and 30 mm.
Preferably, in step S2, the master alloy sheet or strip is rapidly heated to 1000 ℃ by high frequency heating, and the output power of the plasma generator is reduced.
Preferably, in step S6, the flow rate of the circulating cooling air is defined to be 300-1200 cubic/hour.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1. the invention innovatively adopts the traditional casting process to manufacture the Fe-Si-Al plate-shaped or strip-shaped master alloy, controls the thickness of the master alloy to be less than 10 mm, the mother alloy is sent into the heating zone at a constant speed through the automatic feeder, the heating mode adopts high-frequency heating, the mother alloy is rapidly heated to 900-1100 ℃, then enters a plasma atomization area, argon forms high-temperature plasma airflow after passing through a plasma spray gun, the heated Fe-Si-Al master alloy is sprayed at high temperature, all the Fe-Si-Al master alloy is easy to form liquid metal because the Fe-Si-Al alloy is preheated to 900-1100 ℃, at the moment, the liquid Fe-Si-Al alloy is quickly heated to 1360-1500 ℃, and atomized by high-temperature plasma jet flow, the atomized sendust is gradually cooled in the atomizing chamber, and is continuously cooled and contracted into spherical powder in the cooling process due to the surface tension phenomenon. The process avoids molten steel from passing through a flow-limiting port of 4-8 mm, so that the phenomenon of blockage is avoided, and simultaneously, the power problem that a plasma generator is difficult to melt a large amount of metal in a short time is solved by adopting a method of preheating the master alloy by high frequency, the required power of the plasma generator only needs 80 kilowatts, and an imported ultrahigh-power plasma generator is not needed.
2. The invention avoids that the iron-silicon-aluminum molten steel must pass through a flow-limiting leak orifice of 4-8 mm, does not generate the phenomenon of blockage, does not need strict vacuum or atmosphere protection smelting and casting, can continuously carry out atomization production, and improves the production efficiency;
drawings
FIG. 1 is a schematic view of a plasma atomization production apparatus according to the present invention.
FIG. 2 is a flow chart of the plasma atomization production method of the present invention.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the present invention is not limited thereto.
Example 1
In the plasma atomization preparation method of the Sendust soft magnetic alloy powder in the embodiment, pure iron, metal silicon and an electrolytic aluminum ingot are smelted and homogenized according to the standard components of Sendust, and then are continuously cast to form a mother alloy plate or strip, wherein the thickness of the plate or strip is less than 10 mm, the steel casting temperature must be controlled between 1380-1480 ℃, and a casting mold is a design that a water-cooling copper mold and the like are easy to rapidly condense molten steel, so that the grain size of the formed mother alloy is less than 1 mm, the component segregation of three elements of the Sendust due to the crystallization process is avoided, the component uniformity of the subsequent atomized powder is controlled in the Sendust standard components, namely: 9.6% + -0.2% of silicon, 5.4% + -0.2% of aluminum and the balance of iron.
As shown in fig. 1, in the plasma atomization apparatus adopted in this embodiment 1, the formed continuous fe-si-al master alloy strip or plate is fed into the high-frequency heating zone 2 step by the automatic feeding machine 1, the master alloy is rapidly heated to 900-.
As shown in fig. 2, the present embodiment includes the following steps:
s1, smelting pure iron, metallic silicon and an electrolytic aluminum ingot uniformly according to Sendust standard components (namely, silicon content is 9.6% +/-0.2%, aluminum content is 5.4% +/-0.2%, and the balance is iron), continuously casting to form a master alloy plate or strip, wherein the thickness of the plate or strip is 5-30 mm, the steel casting temperature must be controlled between 1380 + 1480 ℃, and the casting die is a water-cooling copper die and the like, so that the grain size of the master alloy formed by the design of easily and quickly condensing molten steel is less than 1 mm;
s2, feeding the formed continuous iron-silicon-aluminum master alloy strip or plate into a high-frequency heating region step by step through an automatic feeder, rapidly heating the master alloy to 900-1100 ℃ to avoid the increase of the oxygen content of the master alloy caused by overlong heating time, and then feeding the master alloy into a plasma atomization region of an argon medium;
s3, after the Fe-Si-Al master alloy which is rapidly heated to 900-1100 ℃ by high frequency enters a plasma atomization zone, a plasma generator of 80-150 kilowatt is adopted, argon or nitrogen is used as a medium, and a spray gun is aligned to the master alloy for spray heating;
s4, the spray gun makes linear reciprocating motion, the motion direction is vertical to the stepping direction of the master alloy, and the distance between the flame opening of the spray gun and the master alloy is 3-15 mm;
s5, matching the stepping speed of the Fe-Si-Al master alloy with the moving speed of a plasma spray gun, and adjusting the particle size and the distribution of Fe-Si-Al atomized powder by adjusting the power of plasma generated gas and the flow of argon gas, wherein in order to improve the atomization efficiency, the maximum particle size of the Fe-Si-Al atomized powder is 97 microns, and the optimal magnetic core Bs is obtained;
s6, arranging an argon gas circulating cooling system in the atomizing tower, setting the bottom as gas inlet, setting the plasma spraying part as a nitrogen gas outlet, setting the flow of circulating cooling air required by the patent at 300-1200 cubic/h, cooling the circulating air by a heat exchanger to achieve the purpose of cooling, and simultaneously cooling and spheroidizing the ferrosilicon aluminum powder after plasma spraying and atomizing by using the cooled argon gas or nitrogen gas.
Example 2
The plasma atomizing apparatus of example 2 was the same as that of example 1, and the technical features were the same as those of example 1 except for the following technical features.
The plasma atomization preparation method of the embodiment 2 comprises the following specific steps: taking an iron-silicon-aluminum master alloy plate with the thickness of 20 mm and the width of 200 mm, passing the plate through a high-frequency heating zone at a stepping speed of 5 mm/10 s/time, wherein the temperature of the heated master alloy is 950-. The internal recycle cooling argon flow was 400 cubic meters per hour.
The results of plasma spray atomization were: the powder collecting speed reaches 50 kg/h, the weight of the undersize is 46 kg after the powder passes through a 150-mesh screen, the apparent density of the spherical sendust reaches 4.2-4.4 g/cc, the sphericity is very good, and the oxygen content of the powder is 500-600ppm.
The magnetic core is made of the iron-silicon-aluminum powder after plasma atomization, the weight of a magnetic ring is 26.9 g, the magnetic permeability is 61, under the test condition of 50Khz @100mT, the measured power loss is 256mW/cm3, under the condition of an external direct current field of 100Oe, the inductance is reduced to 64.1 percent of the original inductance, and the magnetic core performance is very excellent.
Example 3
The plasma atomizing apparatus of example 3 was the same as that of example 1, and the technical features were the same as those of example 1 except for the following technical features.
The plasma atomization preparation method of the embodiment 3 specifically comprises the following steps: the thickness of the iron-silicon-aluminum master alloy plate is 20 mm, the width of the iron-silicon-aluminum master alloy plate is 200 mm, the iron-silicon-aluminum master alloy plate passes through a high-frequency heating zone at a stepping speed of 5 mm/5 s/time, the temperature of the heated master alloy is 950-. In this example, compared to example 1, 2 plasma spray guns were mainly used to increase the plasma atomization rate and increase the throughput.
The results of plasma spray atomization were: the powder collecting speed reaches 80-100 kg/h, the weight of the undersize is 70-85 kg after the powder passes through a 150-mesh screen, the apparent density of the spherical sendust reaches 4.2-4.4 g/cc, the sphericity is very good, and the oxygen content of the powder is 450-580ppm.
The magnetic core is made of the iron-silicon-aluminum powder after plasma atomization, the weight of a magnetic ring is 27.02 g, the magnetic permeability is 63, the power loss is 263mW/cm3 under the test condition of 50Khz @100mT, the inductance is reduced to 62.4 percent of the original inductance under the condition of an external direct current field of 100Oe, and the magnetic core performance is very excellent.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.

Claims (2)

1. A plasma atomization preparation method of Fe-Si-Al soft magnetic alloy powder is characterized by comprising the following steps:
s1, smelting pure iron, metallic silicon and an electrolytic aluminum ingot uniformly according to standard components of Sendust, and continuously casting to form a master alloy plate or strip, wherein the thickness of the plate or strip is less than 10 mm, the steel casting temperature is controlled to be 1380-1480 ℃, a casting mold is designed for the casting mold which is easy to rapidly condense molten steel, so that the grain size of the formed master alloy plate or strip is less than 1 mm, the casting mold is a water-cooling copper mold, and the thickness of the cast master alloy plate or strip is 5-10 mm; the standard components of Sendust are as follows:
9.6 percent +/-0.2 percent of silicon, 5.4 percent +/-0.2 percent of aluminum and the balance of iron;
s2, feeding the formed continuous iron-silicon-aluminum master alloy strip or plate into a high-frequency heating region step by step through an automatic feeder, rapidly heating the master alloy to 900-1100 ℃ to avoid the increase of the oxygen content of the master alloy caused by overlong heating time, and then feeding the master alloy into a plasma atomization region of an argon medium;
s3, after the Fe-Si-Al master alloy which is rapidly heated to 900-1100 ℃ by high frequency enters a plasma atomization zone, a plasma generator of 80-150 kilowatt is adopted, argon or nitrogen is used as a medium, and a spray gun is aligned to the master alloy for spray heating;
s4, the spray gun makes linear reciprocating motion, the motion direction is vertical to the stepping direction of the master alloy, and the distance between the flame opening of the spray gun and the master alloy is 3-15 mm;
s5, matching the stepping speed of the Fe-Si-Al master alloy with the moving speed of a plasma spray gun, and adjusting the particle size and the distribution of Fe-Si-Al atomized powder by adjusting the power of plasma generated gas and the flow of argon gas, wherein in order to improve the atomization efficiency, the maximum particle size of the Fe-Si-Al atomized powder is 97 microns, and the optimal magnetic core Bs is obtained;
s6, arranging an argon circulating cooling system in the atomizing tower, arranging the bottom of the argon circulating cooling system as an inlet, arranging a nitrogen outlet at the downward position of the plasma spraying part, enabling cooling circulating air to pass through a heat exchanger to achieve the cooling purpose, enabling the cooled argon or nitrogen to form a cooling and spheroidizing process on the iron-silicon-aluminum powder subjected to plasma spraying and atomizing, and enabling the flow rate of the circulating cooling air to be regulated to 300 and 1200 cubic/hour.
2. The method for preparing sendust powder according to claim 1, wherein in step S2, the master alloy sheet or strip is heated rapidly to 1000 ℃ by high frequency heating, and the output power of the plasma generator is reduced.
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