CN116571721A - Method for regulating and controlling precipitation position of iron-rich intermetallic compound by using magnetic field - Google Patents

Method for regulating and controlling precipitation position of iron-rich intermetallic compound by using magnetic field Download PDF

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Publication number
CN116571721A
CN116571721A CN202310548332.2A CN202310548332A CN116571721A CN 116571721 A CN116571721 A CN 116571721A CN 202310548332 A CN202310548332 A CN 202310548332A CN 116571721 A CN116571721 A CN 116571721A
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China
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magnetic field
iron
alloy
rich
intermetallic compound
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CN202310548332.2A
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Inventor
帅三三
马金哲
王江
任忠鸣
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University of Shanghai for Science and Technology
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University of Shanghai for Science and Technology
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Priority to CN202310548332.2A priority Critical patent/CN116571721A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22DCASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D21/00Casting non-ferrous metals or metallic compounds so far as their metallurgical properties are of importance for the casting procedure; Selection of compositions therefor
    • B22D21/02Casting exceedingly oxidisable non-ferrous metals, e.g. in inert atmosphere
    • B22D21/04Casting aluminium or magnesium

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The invention provides a method for regulating and controlling precipitation positions of iron-rich intermetallic compounds by utilizing a magnetic field, and belongs to the technical fields of material solidification and magnetic field application. Comprising the following steps: and melting the iron-rich alloy ingot and horizontally rotating and solidifying under a magnetic field. The invention applies a magnetic field in the alloy solidification process, utilizes the thermo-magnetic effect of the magnetic field to regulate the precipitation position of the iron-rich intermetallic compound, and after the magnetic field is applied, the iron-rich intermetallic compound is only formed and grown on the oxide film at the edge of the alloy, and the intermetallic compound formed on the surrounding oxide film can continuously obtain solutes required for growth and growth, which also results in low solute concentration in the center of the alloy and the alloy center is basically free from intermetallic compound formation.

Description

Method for regulating and controlling precipitation position of iron-rich intermetallic compound by using magnetic field
Technical Field
The invention relates to the technical field of material solidification and magnetic field application, in particular to a method for regulating and controlling precipitation positions of iron-rich intermetallic compounds by using a magnetic field.
Background
The aluminum alloy has good mechanical property and corrosion resistance, and is widely used in the fields of machinery, aviation and the like. However, iron impurities that are difficult to remove are inevitably produced during the casting and recycling of aluminum alloys. The inclusion of trace amounts of iron impurities within the Al-Si alloy results in hard and brittle intermetallic compounds such as alpha-Al 8 Fe 2 Si and beta-Al 5 Formation of FeSi. Closing deviceWhen the gold contains higher content of iron element, the brittle plate block-shaped beta-Al 5 The FeSi phase is the main precipitate in the alloy and precipitates inside the alloy. These beta phases are the primary sites of crack formation, which adversely affect the casting properties, machinability and final mechanical properties (in particular ductility) of the alloy.
Therefore, how to control the position of the alloy precipitated phase, reduce or avoid the precipitated phase from precipitating in the alloy, and improve the alloy performance becomes a difficult problem in the prior art.
Disclosure of Invention
The invention aims to provide a method for regulating and controlling precipitation positions of iron-rich intermetallic compounds by utilizing a magnetic field. The method provided by the invention can enable intermetallic compounds to be formed only at the alloy edges and substantially no alloy center.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a method for regulating and controlling precipitation positions of iron-rich intermetallic compounds by utilizing a magnetic field, which comprises the following steps:
and melting the iron-rich alloy ingot and horizontally rotating and solidifying under a magnetic field.
Preferably, the mass fraction of iron in the iron-rich alloy ingot is 0.5-1.5%.
Preferably, the melting temperature is 750-850 ℃.
Preferably, the melting and heat preserving time is 20-40 min.
Preferably, the rate of temperature rise to the melting temperature is 10 to 20 ℃/min.
Preferably, the direction of the magnetic field is a horizontal direction.
Preferably, the strength of the magnetic field is 0.05 to 9T.
Preferably, the horizontal rotation rate is 180 DEG/40-60 s.
Preferably, the cooling rate at the time of solidification is 2 to 4K/min.
The invention provides a method for regulating and controlling precipitation positions of iron-rich intermetallic compounds by using a magnetic field. According to the invention, the iron-rich alloy ingot is solidified under the action of a magnetic field after being melted, in the solidification process, due to the reduction of temperature, the alloy is solidified along the radial direction, intermetallic compounds and surrounding liquid components are different, the Seebeck effect can be generated, the temperature of the tip of the intermetallic compound is possibly higher than the temperature of the bottom of the intermetallic compound, a non-isothermal interface is formed, thermoelectric magnetic currents are generated, the thermoelectric magnetic currents act on the interface near the melt on a microscopic scale, the thermoelectric magnetic currents also cause directional flow of the melt, when only a transverse magnetic field in the same direction is applied, the transverse static magnetic field plays a role in promoting the flow of a liquid phase, unidirectional thermoelectromagnetic flow is generated, fe elements migrate along the flow direction of the liquid phase, fe solute is enriched on one side of a sample, so that the intermetallic compound formed at first on the edge of the sample continuously gets solute growth, and coarse plate-shaped intermetallic compound which is biased on one side of the sample is formed; when the method of the present invention is used, the sample is continuously rotated, and the Fe solute is continuously moved to the edge of the sample (before being moved to one side), and at this time, the intermetallic compound formed on the oxide film of the edge of the sample can continuously obtain the Fe solute required for growth and development, which also results in a lower concentration of Fe solute in the center of the sample, and the center of the sample is substantially free from intermetallic compound formation.
Drawings
FIG. 1 is a physical and internal schematic diagram of an apparatus for a method of controlling precipitation sites of iron-rich intermetallic compounds using a magnetic field according to the present invention;
FIG. 2 is an X-ray diagram of a solidified sample after application of a magnetic field in accordance with example 1 of the present invention;
FIG. 3 is a graph showing the three-dimensional reconstruction of a solidified sample after application of a magnetic field in example 1 of the present invention;
FIG. 4 is a schematic diagram showing the precipitation position of intermetallic compounds upon addition of a magnetic field according to the present invention;
FIG. 5 is an X-ray diagram of a solidified sample in comparative example 1 of the present invention without a magnetic field;
FIG. 6 is a graph showing the three-dimensional reconstruction of a solidified sample through ct when no magnetic field is applied in comparative example 1 of the present invention;
FIG. 7 is a schematic diagram showing the precipitation position of an intermetallic compound when a magnetic field is not added in the present invention.
Detailed Description
The invention provides a method for regulating and controlling precipitation positions of iron-rich intermetallic compounds by utilizing a magnetic field, which comprises the following steps:
and melting the iron-rich alloy ingot and horizontally rotating and solidifying under a magnetic field.
The source of each raw material is not particularly limited unless specifically stated, and commercially available products known to those skilled in the art may be used.
The invention preferably smelts the alloy raw materials to obtain the iron-rich alloy ingot.
In the present invention, the alloy is preferably an Al-Si-Fe alloy.
In the present invention, the mass fraction of Si in the Al-Si-Fe alloy is preferably 8 to 12%, more preferably 10%.
In the present invention, the mass fraction of iron in the iron-rich alloy ingot is preferably 0.5 to 1.5%, more preferably 1%.
In the present invention, the alloy raw material preferably includes pure iron, pure aluminum, and Al-12wt% Si-0.2wt% Fe master alloy.
In the invention, the smelting temperature is preferably 650-850 ℃, more preferably 700-800 ℃; the invention preferably keeps the temperature after the alloy raw materials are completely melted; the time for the heat preservation is preferably 5 to 15 minutes, more preferably 10 minutes. The invention preferably carries out stirring in the heat preservation process; the stirring rate is preferably 200 to 400rpm, more preferably 300rpm. The invention limits the smelting temperature, time and stirring rate in the above range, and can lead the solute distribution in the alloy to be more uniform, thus obtaining fine and uniform primary Si phase and compact matrix structure.
In the present invention, the smelting is preferably performed in high purity argon. In the invention, the high-purity argon can protect the alloy from oxidation and pollution.
In the present invention, the smelting is preferably performed in a vacuum induction furnace. In the invention, the smelting is preferably preceded by a purge with high purity argon to remove impurities and oxygen.
After smelting, the invention preferably carries out sequential cooling, cutting, polishing, washing and drying on the smelted product to obtain the iron-rich alloy ingot.
The cooling method is not particularly limited, and a smelting cooling method known to those skilled in the art may be employed.
In the present invention, the cutting is preferably performed by wire-cut electric discharge machining into round bars having a diameter of 2 to 4mm and a length of 50 to 70mm, and more preferably into round bars having a diameter of 3mm and a length of 60 mm. In the invention, the round bar structure is more suitable for rotation, so that the magnetic field is uniformly applied in the rotation process, and a more accurate result is obtained.
The polishing operation is not particularly limited in the present invention, and polishing operations well known to those skilled in the art may be employed.
In the present invention, the washing preferably includes alkali washing, water washing and organic solvent washing which are sequentially performed.
In the invention, the alkali liquor in alkali washing is preferably sodium hydroxide solution, potassium hydroxide solution or sodium carbonate solution; the mass concentration of the alkali liquor is preferably 5-15%, more preferably 10%; the temperature of the alkaline washing is preferably 70-90 ℃, more preferably 80 ℃; the time of the alkali washing is preferably 20 to 40 minutes, more preferably 30 minutes. The invention has no special limit to the dosage of the alkali liquor, and can be used for immersing the iron-rich alloy ingot. In the present invention, the alkali washing is used to remove residues after spark cutting.
The operation of the washing is not particularly limited, and the washing method can be carried out by adopting a technical scheme of washing which is well known to a person skilled in the art.
In the present invention, after the washing is completed, the surface of the alloy ingot is preferably inspected by a microscope to confirm whether there is any residual ablation trace or scale; the present invention preferably repeats the alkaline washing and the water washing, if any. The times of the alkaline washing and the water washing are not particularly limited, and the surface of the alloy ingot is ensured to have no residual ablation trace or oxide scale.
In the present invention, the organic solvent at the time of washing with the organic solvent is preferably one or more of acetone and alcohol; the organic solvent wash is preferably an ultrasonic wash; the power of the ultrasonic wave is preferably 50-200W, more preferably 100-150W; the time of the ultrasonic wave is preferably 10 to 30 minutes, more preferably 15 to 20 minutes. In the present invention, the organic solvent washing can further remove the residue after cutting.
In the present invention, the drying temperature is preferably 90 to 110 ℃, more preferably 100 ℃; the drying time is preferably 1 to 3 hours, more preferably 2 hours.
After drying is completed, the present invention preferably places the dried product in a dry environment to avoid reaction with moisture or other substances in the air.
After the iron-rich alloy ingot is obtained, the iron-rich alloy ingot is melted and then horizontally rotated and solidified under a magnetic field.
In the present invention, the melting temperature is preferably 750 to 850 ℃, more preferably 780 to 820 ℃; the melting heat preservation time is preferably 20-40 min, more preferably 30min; the rate of heating to the melting temperature is preferably 10 to 20℃per minute, more preferably 15℃per minute. The invention limits the melting temperature, time and the like in the above range, and can ensure that the iron-rich alloy ingot is completely melted.
In the present invention, the direction of the magnetic field is preferably a horizontal direction; the strength of the magnetic field is preferably 0.05 to 9T, more preferably 0.05 to 5T, and most preferably 0.05 to 1T. The present invention limits the direction and strength of the magnetic field to the above-described range, enabling the iron-rich intermetallic compound to sufficiently flow to the melt edge position.
In the present invention, the rate of the horizontal rotation is preferably 180 °/40 to 60s, more preferably 180 °/50s. In the present invention, the rotation can ensure that the iron-rich intermetallic compound formed during solidification moves to the alloy edge position.
In the present invention, the cooling rate at the time of solidification is preferably 2 to 4K/min, more preferably 3K/min. The present invention limits the rate of solidification to the above range, enabling the iron-rich intermetallic compound to have a smaller size.
The solidifying device is not particularly limited, and can be selected according to actual needs. In the present invention, the physical and schematic diagrams of the solidifying means are preferably as shown in fig. 1, which is performed using a resistance furnace with two independent heaters, the center of which is designed with a center hole into which an iron-rich alloy ingot can be inserted and rotated; the iron-rich alloy ingot is preferably placed in a boron nitride tube and then inserted into the central hole of the furnace; the central part of the outer surface of the furnace is a window which is made of boron nitride BN and has the height of 10mm and the width of 20mm so as to run X-ray penetration and facilitate later detection; the side wall of the central part of the furnace is provided with 2 thermocouples and 1 magnet, the thermocouples are used for controlling the temperature, and the top and the bottom of the furnace are respectively provided with one measuring thermocouple for measuring the temperature in the furnace.
The schematic diagram of the precipitation position of the intermetallic compound when the magnetic field is added is preferably shown as figure 4, and the intermetallic compound is distributed in a red annular shadow area under the action of the magnetic field; the schematic of the precipitation position of the intermetallic compound without the addition of the magnetic field is preferably as shown in fig. 7. As can be seen from fig. 4 and 7, when a magnetic field is applied, the diffusion of intermetallic compounds and the distribution of primary phases in the alloy are affected by the thermo-electromagnetic effect of the magnetic field during rotation, and thus the distribution of intermetallic compounds is regulated.
The technical solutions of the present invention will be clearly and completely described in the following in connection with the embodiments of the present invention. It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
(1) Using industrial pure iron, pure aluminum and Al-12wt.% Si-0.2wt.% Fe as raw materials, placing the raw materials into a corundum crucible according to the component proportion of Al-10wt.% Si-1wt.% Fe alloy, then placing the corundum crucible into a vacuum induction furnace, washing gas by high-purity argon, heating to 700 ℃ for smelting, stirring at 300rpm for 10min by adopting a magnetic stirring mode after the raw materials are completely melted, and cooling to obtain an alloy ingot, wherein the whole smelting process is carried out under the condition of high-purity argon;
(2) Cutting an alloy ingot into round bars with the diameter of 3mm and the length of 60mm by adopting wire electric discharge cutting, polishing the surface by using sand paper, then putting the round bars into NaOH solution with the mass concentration of 10%, keeping the temperature at 80 ℃ for 30min, then washing the round bars with water, wiping the round bars to dry, checking the surface by adopting a microscope that no ablation trace or oxide skin remains on the surface, putting the round bars into an oven at 100 ℃ for 2h, then putting the round bars into acetone, performing ultrasonic washing for 15min under the power of 100W, then drying the round bars, and putting the round bars into a boron nitride tube with the inner diameter of about 3mm and the outer diameter of about 6 mm;
(3) The boron nitride tube containing the alloy ingot is placed in the central hole of a resistance furnace, rotated at a speed of 180 DEG/50 s, the furnace is heated to 750 ℃ at a speed of 15 ℃/min, a magnetic field of 0.07T in the horizontal direction is applied, the temperature is maintained for 30min, and then the sample is cooled at a speed of 3K/min until the sample is completely solidified.
Comparative example 1
The magnetic field in example 1 was omitted and the other parameters were the same as in example 1.
The alloy sample solidified in example 1 was observed by X-ray, and as a result, the upper graph in fig. 2 shows an X-ray image of a slice, the lower graph shows an X-ray image of one side, the sample is a round bar, the upper graph corresponds to a view of the distribution of intermetallic compounds by cutting the round bar at the waist, and the lower graph corresponds to a view of the distribution of intermetallic compounds by cutting the round bar from the head down along the diameter of a circle. Example 1 an image of an alloy sample subjected to ct three-dimensional reconstruction is shown in fig. 3, and the overall distribution of intermetallic compounds in the sample can be seen from fig. 3, wherein the upper graph is that of the sample viewed from the top down, and the lower graph is that of the sample viewed from one side. The alloy sample after solidification of comparative example 1 was observed by X-rays, and the result is shown in FIG. 5, wherein the upper graph in FIG. 5 shows an X-ray image of a certain slice, and the lower graph shows an X-ray image of one side. As shown in fig. 6, which shows an image of the three-dimensional reconstruction of the alloy sample of comparative example 1, as seen from fig. 2 to 3 and fig. 5 to 6, the intermetallic compound is randomly generated in the sample without a magnetic field and covers the entire sample, and after the magnetic field is applied, the intermetallic compound is formed and grown only on the oxide film surface of the sample, and the center portion is hardly present.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.

Claims (9)

1. A method for controlling precipitation positions of iron-rich intermetallic compounds by using a magnetic field, comprising the following steps:
and melting the iron-rich alloy ingot and horizontally rotating and solidifying under a magnetic field.
2. The method of claim 1, wherein the mass fraction of iron in the iron-rich alloy ingot is 0.5-1.5%.
3. The method of claim 1, wherein the melting temperature is 750-850 ℃.
4. A method according to claim 1 or 3, wherein the incubation time for melting is 20 to 40 minutes.
5. A method according to claim 3, wherein the rate of rise of the temperature to the melting temperature is 10 to 20 ℃/min.
6. The method of claim 1, wherein the direction of the magnetic field is a horizontal direction.
7. The method according to claim 1 or 6, wherein the magnetic field has a strength of 0.05 to 9T.
8. The method according to claim 1, wherein the horizontal rotation is at a rate of 180 °/40-60 s.
9. The method according to claim 1, wherein the cooling rate upon solidification is 2 to 4K/min.
CN202310548332.2A 2023-05-16 2023-05-16 Method for regulating and controlling precipitation position of iron-rich intermetallic compound by using magnetic field Pending CN116571721A (en)

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CN116571721A true CN116571721A (en) 2023-08-11

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