CN113930644B - Heat-resistant Al-Fe-Si aluminum alloy and preparation method thereof - Google Patents
Heat-resistant Al-Fe-Si aluminum alloy and preparation method thereof Download PDFInfo
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Abstract
The invention provides a heat-resistant Al-Fe-Si aluminum alloy and a preparation method thereof, wherein the Al-Fe-Si aluminum alloy comprises the following components in percentage by mass: 4.5 to 5.5 percent of iron, 2.8 to 3.5 percent of silicon, and the balance of Al and inevitable impurities, wherein the total amount of the impurities is less than or equal to 0.06 percent. The preparation method comprises the steps of remelting an Al-Fe-Si alloy ingot at 750-820 ℃ in a vacuum environment, and then chilling to obtain the heat-resistant Al-Fe-Si aluminum alloy, wherein the chilling speed is not less than 300 ℃/s. According to the invention, the Al-Fe-Si aluminum alloy with 100% of iron-containing phase being eutectic alpha-AlFeSi is obtained through component control and synergistic remelting chilling treatment, and the eutectic alpha-AlFeSi has extremely excellent enhancement effect, so that the Al-Fe-Si aluminum alloy has the characteristics of high tissue thermal stability and excellent strength and toughness performance. The method can be applied to parts which are in service at higher temperature, such as an engine shell, a piston and the like.
Description
Technical Field
The invention relates to a heat-resistant Al-Fe-Si aluminum alloy, belonging to the technical field of aluminum alloy preparation.
Background
Al-Si alloy is a material commonly used for automobile engines, and pure Al-Si alloy has low strength, so that a small amount of Cu and Mg elements are usually added into the alloy to improve the strength of the alloy. The main strengthening mechanism is aging precipitation strengthening, and the aging heat treatment temperature is below 200 ℃. These Mg-containing, cu precipitated phases coarsen after being kept at a temperature of 200 ℃ or higher for a long time (100 hours or longer), and the size increases, the number density decreases, the ability to inhibit dislocation movement decreases, and the strength of the alloy decreases. Whereas the operating temperature of an automobile engine is about 200 deg.c, which is detrimental to the strength of the Al-Si alloy. Therefore, it is necessary to develop an aluminum alloy which can be used at higher temperature to make up for the deficiencies of the existing Al-Si alloy.
The common novel heat-resistant aluminum alloy at present mainly comprises alloy systems of Al-Ni, al-Ce and the like. The alloy relies mainly on Al being stable at high temperatures 3 Ni，Al 11 Ce 3 The phases are used as strengthening phases of the alloy, the sizes of the phases are generally below 200nm, and the phases are uniformly distributed, so that the alloy has higher strength and elongation. However, the cost of the reinforcing elements of the heat-resistant aluminum alloy is relatively high.
Patent CN113416870A discloses an Al-Ce series high-strength heat-resistant aluminum alloy, wherein the addition amount of Ce reaches 12-16%, and in addition, 0.3-0.8% of Sc and 0.15-0.32% of Zr are added. The addition of these alloying elements greatly increases the cost of the alloy. Where Ce is more than 5 times as monovalent as Fe, and Sc is more expensive per kilogram (32000 yuan/kg). The addition of 0.3-0.8% adds 10-25 million to the cost per ton of alloy, which is not commercially viable.
The formation temperature of the alpha-AlFeSi phase is over 600 ℃, and the diffusion speed of Fe element in an aluminum matrix is slow, so that the alpha-AlFeSi has high stability at high temperature. And the needed elements Fe and Si are low-cost additive elements, so that the research on the alloy taking the fine alpha-AlFeSi eutectic as the strengthening phase is one direction for obtaining the low-cost heat-resistant aluminum alloy. However, the Al-Fe-Si system involves three elements, and the formed iron-containing phase is various, so that an alloy with the iron-containing phase being completely alpha-AlFeSi cannot be obtained under normal conditions, and flaky Al is inevitably generated 13 Fe 4 And a beta-AlFeSi detrimental phase. At present, an alloy with an iron-containing phase and a microstructure of all alpha-AlFeSi eutectic is not obtained.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide the Al-Fe-Si heat-resistant aluminum alloy with the iron-containing phase being alpha-AlFeSi and the preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention relates to a heat-resistant Al-Fe-Si aluminum alloy, wherein 100% of an iron-containing phase in the Al-Fe-Si aluminum alloy is eutectic alpha-AlFeSi, and the Al-Fe-Si aluminum alloy comprises the following components in percentage by mass: 4.5 to 5.5 percent of iron, 2.8 to 3.5 percent of silicon, and the balance of Al and inevitable impurities, wherein the total content of the impurities is less than or equal to 0.06 percent.
The invention provides the Al-Fe-Si aluminum alloy with the iron phase being eutectic alpha-AlFeSi for the first time, and the Al-Fe-Si aluminum alloy does not have flaky Al 13 Fe 4 And beta-AlFeSi, so that the Al-Fe-Si aluminum alloy provided by the invention has excellent strength and elongation, and the microstructure heat resistance is excellent.
In the present invention, the mass percentage of Al-Fe-Si aluminum alloy is important, and if the content is not within the range of the present invention, the content cannot be adjustedThe iron-containing phases are all eutectic alpha-AlFeSi. When the iron content is too high or the silicon content is too low, coarse flaky or flower-like Al is generated in the alloy 13 Fe 4 Phase, impairing the strength and elongation of the alloy. When the iron content is too low or the silicon content is too high, coarse flaky beta-AlFeSi is precipitated, which causes stress concentration and deteriorates the strength and elongation of the alloy.
Preferably, the Al-Fe-Si aluminum alloy comprises the following components in percentage by mass: 4.8 to 5.5 percent of iron, 3.0 to 3.5 percent of silicon, and the balance of Al and inevitable impurities, wherein the total content of the impurities is less than or equal to 0.06 percent.
Preferably, the crystal grain of the alpha-AlFeSi is less than or equal to 200nm.
The Al-Fe-Si aluminum alloy provided by the invention contains alpha-AlFeSi with the iron phase of 200nm or less, the morphology of the alpha-AlFeSi is labyrinth or Chinese character, and the inventor finds that the morphology of the alpha-AlFeSi is labyrinth or Chinese character-shaped, and the morphology of the alpha-AlFeSi is matched with Al of the reinforcing phase in the Al-Ce eutectic alloy 11 Ce 3 The appearance is very similar, and the enhancement effect is obvious.
Preferably, the microstructure of the Al-Fe-Si aluminum alloy is an Al/alpha-AlFeSi eutectic cluster, and the diameter of the Al/alpha-AlFeSi eutectic cluster is 20-40 μm.
Preferably, the tensile strength of the Al-Fe-Si aluminum alloy is 240-260MPa, and the elongation is 15-20%.
The invention relates to a preparation method of a heat-resistant Al-Fe-Si aluminum alloy, which comprises the following steps:
remelting the Al-Fe-Si alloy ingot at 750-820 ℃ in a vacuum environment, and then chilling to obtain the heat-resistant Al-Fe-Si aluminum alloy, wherein the chilling speed is not less than 300 ℃/s, and preferably 400 ℃/s.
The inventor finds that the Al-Fe-Si alloy ingot meeting the component proportion of the designed formula is remelted and then is chilled, so that the iron-containing phase is fully alpha-AlFeSi.
In the present invention, the means for chilling is not limited as long as the cooling rate can satisfy the requirement, but if the cooling rate is too low, al is generated 13 Fe 4 And β -AlFeSi phase, which impairs the strength and elongation of the alloy.
Preferably, the remelting temperature is 780-800 ℃, and the heat preservation time is 20-40min.
The invention relates to a preparation method of a heat-resistant Al-Fe-Si aluminum alloy, which comprises the following steps:
and (2) carrying out machining on the Al-Fe-Si alloy ingot to obtain an Al-Fe-Si alloy short rod, packaging the Al-Fe-Si alloy short rod in a vacuum quartz tube, remelting the Al-Fe-Si alloy short rod at 750-820 ℃, preferably 780-800 ℃, preserving heat for 20-40min to obtain a remelted Al-Fe-Si alloy, then clamping and breaking the quartz tube, directly dropping the remelted Al-Fe-Si alloy into cooling water, and chilling to obtain the Al-Fe-Si alloy, wherein the temperature of the cooling water is less than or equal to 20 ℃.
In the process, the remelted Al-Fe-Si alloy is directly dropped into cooling water, about 2S is obtained, and the Al-Fe-Si alloy cooled to room temperature is obtained, wherein the cooling speed is not less than 300 ℃/S. The inventor finds that the Al-Fe-Si aluminum alloy obtained by the preparation process has the best final performance.
Preferably, the method for obtaining the Al-Fe-Si alloy ingot comprises the following steps: and (2) preparing an Al source, an Fe source and an Si source according to a designed proportion, smelting to obtain a melt, and casting and molding the melt to obtain the Al-Fe-Si alloy ingot.
Further preferably, the Al source is at least one selected from pure aluminum, aluminum-iron alloy, and aluminum-silicon alloy, the iron source is at least one selected from pure iron and aluminum-iron alloy, and the silicon source is at least one selected from pure silicon and aluminum-silicon alloy.
In actual operation, after processing an Al-Fe-Si alloy ingot into a short rod, polishing the short rod by using abrasive paper to remove surface processing marks, cleaning the short rod by using alcohol, putting the processed short rod into a cylindrical corundum crucible, and then sealing the crucible and a sample into a vacuum quartz tube.
The prominent substantive features and remarkable progress of the invention are mainly reflected in that:
(1) The Al-alpha-AlFeSi eutectic aluminum alloy is obtained by reasonably adjusting components and controlling the cooling speed, and a new heat-resistant aluminum alloy system is explored. In the Al-Fe-Si aluminum alloy obtained by the invention, 100% of the iron-containing phase is eutectic alpha-AlFeSi, and the effect of the alpha-AlFeSi in the Al-Fe-Si aluminum alloy is equivalent to that of eutectic Al in the Al-Ce eutectic alloy 11 Ce 3 Or eutectic Al-Ni alloyEutectic Al in (1) 3 Ni, eutectic Al thereof 11 Ce 3 The alloy has a similar labyrinth lamellar structure, and the width of the sheet is less than 200nm, so that the alloy has a good enhancement effect on the mechanical property of the alloy.
(2) The alloy obtained by the invention can realize excellent performances of 247MPa of tensile strength and 19% of elongation without adding other precipitation strengthening elements.
(3) The alloy obtained by the invention has the characteristics of high structure thermal stability and excellent strength and toughness performance. The method can be applied to parts which are in service at higher temperature, such as an engine shell, a piston and the like.
(4) The Fe and Si elements contained in the alloy have obvious price advantages compared with Ce and Ni, and the alloy is more suitable for commercialization.
Drawings
FIG. 1 is a schematic view of a vacuum tube seal.
FIG. 2 is an SEM image of the microstructure of the Al-Fe-Si aluminum alloy of example 1.
FIG. 3 shows the microstructure of the Al-Fe-Si aluminum alloy sheet of example 1 after heat treatment at 520 ℃ for 0, 2, 4, and 8 hours.
FIG. 4 is an SEM image of the microstructure of the Al-Fe-Si aluminum alloy of example 2.
FIG. 5 is an SEM image of the microstructure of Al-Fe-Si aluminum alloy of example 3.
FIG. 6 is an SEM image of the microstructure of the Al-Fe-Si aluminum alloy of comparative example 1.
FIG. 7 is an SEM image of the microstructure of the Al-Fe-Si aluminum alloy of comparative example 2.
FIG. 8 is a tensile stress-strain curve of Al-Fe-Si aluminum alloys in example 1 and comparative examples 1 and 2.
Detailed Description
The invention relates to a heat-resistant Al-Fe-Si aluminum alloy and a preparation method thereof, wherein the heat-resistant Al-Fe-Si aluminum alloy comprises the following components in percentage by mass: 4.5 to 5.5 percent of iron, 2.8 to 3.5 percent of silicon, and the balance of Al and inevitable impurities, wherein the total amount of the impurities is less than or equal to 0.06 percent. Preferably the alloy composition is: 4.8 to 5.5 percent of iron, 3 to 3.5 percent of silicon, and the balance of Al and inevitable impurities, wherein the total amount of the impurities is less than or equal to 0.06 percent.
The invention also provides a corresponding processing technology:
(1) Alloy smelting and casting: the preparation method comprises the steps of proportioning pure aluminum and intermediate alloy according to the mass fraction of 4.8-5.5% of iron, 3-3.5% of silicon and the balance of Al and inevitable impurities, then placing the alloy into a graphite crucible, casting the alloy into an aluminum rod, wherein the induced current in the alloy casting process is 260A, and after the casting is finished, pouring the aluminum rod into a copper mold to obtain an alloy ingot.
(2) Machining: cutting the alloy ingot by wire electrical discharge machining to obtain a short rod with the diameter of 12mm and the height of 20mm, polishing by abrasive paper to remove surface processing marks, and cleaning alcohol for later use.
(3) Vacuum tube sealing: putting the treated short rod into a cylindrical corundum crucible with the inner diameter of 13mm, and then sealing the crucible into a vacuum quartz tube; pumping the tube to below 50Pa on a vacuum tube sealing machine, and burning a quartz tube to form an annular neck at a position 2cm higher than the crucible; and then taking out and putting the quartz plug, pumping the tube to below 50Pa on a tube sealing machine, and sintering the quartz tube and the quartz plug together to form a vacuum closed space in the tube.
(4) Remelting and chilling: raising the temperature from room temperature to 750-820 ℃ at a heating rate of less than 10 ℃/min, preserving the temperature for 20 minutes, taking out the sample, quickly moving the sample to the water surface by using a pliers, and clamping a quartz tube to break the quartz tube so that the sample directly falls into the water to obtain a quenched sample.
Example 1
The components of the heat-resistant Al-Fe-Si aluminum alloy in the embodiment 1 are as follows by mass percent: 5% of iron, 3% of silicon, and the balance of Al and inevitable impurities. The preparation method comprises the steps of taking pure aluminum, al-10Fe and Al-20Si intermediate alloy according to a designed proportion, carrying out smelting casting through the processes, sealing a tube in vacuum, remelting at 800 ℃, clamping a quartz tube after remelting, enabling a sample to directly fall into water with the temperature of about 20 ℃ for chilling, and cooling the alloy to the room temperature after about 2 s. Then obtaining a water-cooling sample, namely the Al-Fe-Si aluminum alloy. And then testing the mechanical property of the Al-Fe-Si aluminum alloy, wherein the tensile strength of the obtained alloy is 247MPa, and the elongation is 19%.
Cutting Al-Fe-Si aluminum alloy into sheets with the thickness of 1mm by electric spark wire cutting, putting 3 sheets into a 520 ℃ box furnace, and respectively carrying out heat treatment for 2 hours, 4 hours and 8 hours.
Fig. 2 is an SEM picture of the microstructure of the Al-Fe-Si aluminum alloy prepared in example 1, and it can be seen from the SEM picture that the microstructure of the alloy is all fine Al/α -AlFeSi eutectic clusters, and α -AlFeSi is distributed in a labyrinth shape and has a thickness of 200nm or less.
Fig. 3 shows the microstructure of the Al-Fe-Si aluminum alloy sheet obtained in example 1 after heat treatment at 520 ℃ for 0 hour, 2 hours, 4 hours, and 8 hours, and it can be seen that the a-AlFeSi phase uniformly distributed in the alloy can be maintained below 0.5 μm after heat preservation at 520 ℃ for 8 hours, and the alloy exhibits high structure thermal stability.
Example 2
The heat-resistant Al-Fe-Si aluminum alloy in example 2 comprises the following components in percentage by mass: 4.8% of iron, 3% of silicon, and the balance of Al and inevitable impurities. The preparation method comprises the steps of taking pure aluminum, al-10Fe and Al-20Si intermediate alloy according to a designed proportion, carrying out smelting casting through the processes, sealing a tube in vacuum, remelting at 800 ℃, clamping a quartz tube after remelting, enabling a sample to directly fall into water with the temperature of about 20 ℃ for chilling, and cooling the alloy to the room temperature after about 2 s.
And chilling to obtain a water-cooled sample, namely the Al-Fe-Si aluminum alloy, and testing the mechanical property of the alloy, wherein the tensile strength of the obtained alloy is 244MPa, and the elongation is 16%.
Fig. 4 is a SEM picture of the microstructure of example 2, and it can be seen that all iron-containing phases in the alloy are fine eutectic α -AlFeSi.
Example 3
The heat-resistant Al-Fe-Si aluminum alloy in example 3 comprises the following components in percentage by mass: 5% of iron, 3.5% of silicon, and the balance of Al and inevitable impurities. The intermediate alloy of pure aluminum, al-10Fe and Al-20Si is smelted and cast by the above-mentioned process, vacuum tube-sealing, remelting at 800 deg.C, after remelting, clamping quartz tube to make sample directly fall into water with about 20 deg.C, and chilling, and cooling to room temperature for about 2 s. And chilling to obtain a water-cooled sample, namely the Al-Fe-Si aluminum alloy. And then testing the mechanical property of the Al-Fe-Si aluminum alloy, wherein the tensile strength of the obtained alloy is 252MPa, and the elongation is 15%.
Fig. 5 is an SEM picture of the microstructure of example 3, from which it can be seen that all the iron-containing phases in the alloy are fine eutectic a-AlFeSi.
Comparative example 1
The alloy comprises 5% of iron, 3% of silicon, and the balance of Al and inevitable impurities. The pure aluminum, al-10Fe and Al-20Si intermediate alloy is smelted and cast by the process to obtain an as-cast sample, and the cooling speed of casting is less than or equal to 1 ℃/s. And then testing the mechanical property of the alloy, wherein the tensile strength of the obtained alloy is 126MPa, and the elongation is 1.6%.
FIG. 6 is a SEM photograph showing the microstructure of this comparative example, and it can be seen that the alloy contains a large amount of coarse flower/flake Al 13 Fe 4 These phases can lead to stress concentrations that impair the strength and elongation of the alloy. From this comparative example, the importance of cooling rate for the preparation of Al-a-AlFeSi eutectic heat resistant alloys can be seen.
Comparative example 2
The alloy comprises 5 percent of iron, 5 percent of silicon, and the balance of Al and inevitable impurities. The pure aluminum, al-10Fe and Al-20Si intermediate alloy is smelted and cast, the tube is sealed in vacuum, and the water-cooled sample is obtained after remelting and chilling according to the conditions of the embodiment 1. And then testing the mechanical property of the alloy, wherein the tensile strength of the obtained alloy is 184MPa, and the elongation is 2%.
Fig. 7 shows an SEM picture of the microstructure of the comparative example, from which it can be seen that the alloy containing a higher amount of silicon contains a large amount of coarse flaky β -AlFeSi, which is a recognized harmful phase and greatly impairs the mechanical properties of the alloy. The comparative example shows that the components should be within a certain range and the best within the scope of the patent requirement to obtain the Al-alpha-AlFeSi eutectic heat-resistant alloy.
It is noted that this patent is intended to protect the composition of the eutectic alloy that will yield a complete Al-a-AlFeSi alloy. The key to the preparation method is high cooling speed, and means for realizing rapid cooling include using a water-cooled mold, die casting, selective laser melting (3D printing, additive manufacturing) and the like. Any component that is within the scope of the present patent application is to be considered within the scope of the present patent application.
Claims (5)
1. A preparation method of heat-resistant Al-Fe-Si aluminum alloy is characterized by comprising the following steps: the method comprises the following steps: the method comprises the following steps of (1) carrying out machining on an Al-Fe-Si alloy ingot to obtain an Al-Fe-Si alloy short rod, packaging the Al-Fe-Si alloy short rod in a vacuum quartz tube, remelting at 750-820 ℃, carrying out heat preservation for 20-40min to obtain a remelted Al-Fe-Si alloy, then clamping the quartz tube, directly dropping the remelted Al-Fe-Si alloy into cooling water, and carrying out chilling to obtain the Al-Fe-Si aluminum alloy, wherein the temperature of the cooling water is less than or equal to 20 ℃, and the chilling speed is greater than or equal to 300 ℃/s; in the Al-Fe-Si aluminum alloy, 100% of an iron-containing phase is eutectic alpha-AlFeSi, and the Al-Fe-Si aluminum alloy comprises the following components in percentage by mass: 4.5 to 5.5 percent of iron, 2.8 to 3.5 percent of silicon, and the balance of Al and inevitable impurities, wherein the total content of the impurities is less than or equal to 0.06 percent;
the microstructure of the Al-Fe-Si aluminum alloy is Al/alpha-AlFeSi eutectic cluster, and the diameter of the Al/alpha-AlFeSi eutectic cluster is 20-40 mu m;
the crystal grain of the eutectic alpha-AlFeSi is less than or equal to 200nm.
2. The method for preparing a heat-resistant Al-Fe-Si aluminum alloy according to claim 1, wherein: the remelting temperature is 780-800 ℃, and the heat preservation time is 20-40min.
3. The method for preparing the heat-resistant Al-Fe-Si aluminum alloy according to claim 1, comprising the following steps: the method for obtaining the Al-Fe-Si alloy cast ingot comprises the following steps: and (2) preparing an Al source, an Fe source and an Si source according to a designed proportion, smelting to obtain a melt, and casting and molding the melt to obtain the Al-Fe-Si alloy ingot.
4. The method for preparing a heat-resistant Al-Fe-Si aluminum alloy according to claim 1, wherein: the Al-Fe-Si aluminum alloy comprises the following components in percentage by mass: 4.8 to 5.5 percent of iron, 3.0 to 3.5 percent of silicon, and the balance of Al and inevitable impurities, wherein the total content of the impurities is less than or equal to 0.06 percent.
5. The method for preparing a heat-resistant Al-Fe-Si aluminum alloy according to claim 1, wherein: the tensile strength of the Al-Fe-Si aluminum alloy is 240-260MPa, and the elongation is 15-20%.
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