CN115491617B - Method for refining aluminum and aluminum alloy grains by micro-alloying Si and Er - Google Patents
Method for refining aluminum and aluminum alloy grains by micro-alloying Si and Er Download PDFInfo
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- CN115491617B CN115491617B CN202211076681.0A CN202211076681A CN115491617B CN 115491617 B CN115491617 B CN 115491617B CN 202211076681 A CN202211076681 A CN 202211076681A CN 115491617 B CN115491617 B CN 115491617B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
- C22F1/053—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon of alloys with zinc as the next major constituent
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- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
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- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
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Abstract
A method for refining aluminum and aluminum alloy grains by micro-alloying Si and Er belongs to the technical field of aluminum alloy materials. According to the method, si and Er composite microalloying is adopted, a proper amount of Si and Er microalloying elements are added in the alloy preparation process, and through subsequent homogenization, hot rolling and solution treatment, a grain boundary precipitation phase rich in Er and Si elements is precipitated at a recrystallization grain boundary of the alloy, so that the growth of recrystallized grains is prevented, and the grains are obviously refined.
Description
Technical Field
The invention relates to a method for refining aluminum alloy grains, mainly relates to the effect of Si and Er microalloying elements on aluminum and aluminum alloy refined grains, and belongs to the technical field of alloy materials.
Technical Field
The aluminum alloy has excellent properties such as high strength and corrosion resistance, and is widely applied to the fields of aerospace, automobile manufacturing and the like. With the continuous development of aluminum alloy and the continuous increase of the application of the aluminum alloy in the high and new technical field, the aluminum alloy also has higher requirements on the structure and the performance of the aluminum alloy.
The size of recrystallized grains can obviously influence the performance of the alloy, and researches on the alloy have found that the alloy is restrained from recrystallization, and dynamic recrystallization during the hot working of the alloy is promoted, so that the alloy can generate extremely fine grains, and the superplasticity of the alloy is possible while the performance of the material is improved.
In the aspect of recrystallization grain refinement research at present, the alloy recrystallization is further inhibited mainly by improving the heat treatment process, so as to play a role in refining the recrystallization grains. Specific processes include solution quenching, overaging, intermediate temperature deformation, intermediate temperature transformation (ITMT) process for solution recrystallization treatment, recrystallization annealing, pre-deformation, low temperature annealing, rolling, recrystallization annealing, solution treatment for seven-system alloy, rolling deformation, continuous rolling deformation, recrystallization treatment, and the like. Although the above process can refine the recrystallized grains of the alloy, the process has the defects of large energy consumption, difficult operation, complex process, small application range of the process and the like.
Aiming at the complexity and the limitation of the heat treatment process, it is particularly important to design a recrystallization grain refinement mode without the limitation of the heat treatment process. Numerous researches show that microalloying can have a favorable influence on the grain structure and mechanical properties of the aluminum alloy, and trace Si elements are added into Al-Cu-Mg to inhibit the growth of precipitated phases in the alloy, so that the precipitated phases in a matrix are refined and uniformly distributed, the aging strengthening of the alloy is accelerated, and the mechanical properties of the alloy are improved. Meanwhile, researches show that the addition of trace Er into the A1-Mg alloy can effectively refine the as-cast crystal grains of the alloy, increase the thermal stability of the alloy and increase the recrystallization temperature by about 50 ℃. Therefore, the effect of the microalloying by the common addition of Si and Er elements on the size of the recrystallized grains of the alloy is discussed, and the comprehensive performance of the alloy is further improved.
Based on the technical background, the invention adopts a homogenization-rolling heat treatment process through Si and Er microalloying, so that the grain boundary precipitation phase rich in Er and Si elements is precipitated at the recrystallization grain boundary of the final alloy, thereby refining the recrystallization structure of the aluminum alloy, obtaining the aluminum alloy with more excellent mechanical properties, and meeting the higher requirements on the structure and the performance of the aluminum alloy in the industrial field.
Disclosure of Invention
The invention aims to invent a method for refining aluminum alloy grains, which adds or composites Si and Er microalloying elements into aluminum and aluminum alloy through a microalloying method widely used at present, precipitates a grain boundary precipitation phase rich in Er and Si elements at a recrystallization grain boundary of the rolled alloy through a homogenization-rolling subsequent heat treatment process, plays a role in refining the aluminum alloy recrystallization grains, and improves the mechanical property of the final aluminum alloy at the same time, so that the aluminum alloy with excellent comprehensive performance is prepared.
A process for refining Al and Al alloy grains by microalloying Si and Er features that the microalloying Si and Er elements are added to the matrix of pure Al or Al alloy, the ingot is homogenized, heat treated and rolled, and then heat treated to separate Si and Er out at the recrystallized grain boundary to prevent the grains from growing.
The aluminum alloy grain refining method provided by the invention is characterized in that Si and Er microalloying elements are added, the weight percentage of the Si element in the final alloy is 0.15-0.3%, and the weight percentage of the Er element in the final alloy is 0.1-0.25%.
And a proper amount of Si and Er microalloying elements are added into the pure aluminum in a compounding way, so that the weight percentage of the Si element in the final alloy is 0.15-0.3%, and the weight percentage of the Er element in the final alloy is 0.1-0.25%.
And a proper amount of Si and Er microalloying elements are compositely added into the aluminum alloy matrix, wherein the aluminum alloy matrix is preferably Al-Cu-Mg, al-Zn-Mg-Cu alloy and the like.
The aluminum alloy grain refining method provided by the invention is characterized in that the aluminum alloy obtained by casting is subjected to homogenization treatment at 440-460 ℃/6 h.
The aluminum alloy grain refinement method provided by the invention is characterized by comprising the following steps of heat treatment and rolling after homogenization treatment: heat treatment is carried out for 1-2 h at 430-460 ℃, and rolling is carried out at the heat treatment temperature, wherein the deformation is 65-80%, and preferably 1-pass rolling is carried out.
The aluminum alloy grain refining method provided by the invention is characterized in that the temperature of the heat treatment after rolling is 530-550 ℃.
The invention is realized by the following technical scheme: the method for refining aluminum alloy grains comprises the steps of (1) designing components of the alloy; (2) Smelting by a graphite crucible and casting by an iron mold to prepare an ingot alloy; (3) homogenizing the alloy; (4) hot rolling the alloy; (5) heat treating the alloy.
And (3) designing the components of the prepared aluminum alloy, and selecting proper amounts of microalloying elements, namely Si and Er, so as to obtain the aluminum alloy with fine grains and excellent performance.
The specific process for preparing the cast ingot alloy by adopting graphite crucible smelting and iron mold casting comprises the following steps: firstly, putting raw materials into a graphite crucible, heating and melting the raw materials in a high-temperature smelting furnace at 800+/-5 ℃, and keeping the temperature and standing the raw materials when the temperature is reached, if pure Mg needs to be added, thenAluminum foil is wrapped and added to reduce the burning loss of Mg, and then the mixture is fully stirred, and after the mixture is fully melted, C 2 Cl 6 Degassing, stirring, preserving heat, standing, and then casting by an iron mold to obtain the aluminum alloy cast ingot.
And (3) placing the cast ingot obtained by casting in a heat treatment furnace on the basis of the step (2), and carrying out homogenization treatment for 6 hours at 440-460 ℃.
And (4) carrying out heat treatment and heat preservation on the homogenized sample for 1-2 hours at 430-460 ℃ on the basis of the step (3), and rolling the sample at the heat treatment temperature until the deformation is 65-80%.
And (5) carrying out heat treatment at 530-550 ℃ on the basis of the step (4), heating from room temperature to 530-550 ℃, preserving heat for 1h, and then quenching to room temperature in 10 s.
According to the invention, after Er and Si are added into the aluminum alloy together, through subsequent homogenization-hot rolling and heat treatment processes, a grain boundary precipitation phase rich in Er and Si elements is precipitated at a recrystallization grain boundary of the alloy, and the growth of recrystallized grains is prevented, so that the recrystallization structure of the aluminum alloy is refined, and the aluminum alloy with excellent performance is obtained.
Description of the drawings:
fig. 1 (a): metallographic pictures of the Al-0.25Er alloy in example 1 after solution treatment.
Fig. 1 (b): metallographic pictures of the Al-0.25Er-0.3Si alloy of example 1 after solution treatment.
Fig. 2 (a): metallographic pictures of the Al-4Cu-0.5Mg alloy in example 2 after solution treatment.
Fig. 2 (b): metallographic pictures of the Al-4Cu-0.5Mg-0.15Si alloy in example 2 after solution treatment.
Fig. 2 (c): metallographic pictures of the Al-4Cu-0.5Mg-0.15Si-0.1Er alloy in example 2 after solution treatment.
Fig. 3 (a): metallographic pictures of the Al-4.5Zn-1.5Mg-1.0Cu alloy in example 3 after solution treatment.
Fig. 3 (b): metallographic pictures of the Al-4.5Zn-1.5Mg-1.0Cu-0.35Si alloy in example 3 after solution treatment.
Fig. 3 (c): metallographic pictures of the Al-4.5Zn-1.5Mg-1.0Cu-0.35Si-0.1Er alloy in example 3 after solution treatment.
Fig. 4: TEM image of alloy after Er and Si elements are added together
The specific embodiment is as follows:
the present invention will be further illustrated with reference to the following examples, but the present invention is not limited to the following examples.
Example 1: two aluminum alloy cast ingots with different components are prepared by adopting graphite crucible smelting and iron mold casting, and the raw materials are high-purity aluminum, al-24% Si and Al-6% Er intermediate alloy. Firstly, calculating the mass of required experimental raw materials according to designed alloy components, putting high-purity aluminum into a graphite crucible, heating and melting in a high-temperature smelting furnace at 800+/-5 ℃, then adding Al-24% Si and Al-6% Er intermediate alloy after the pure aluminum is completely melted, fully stirring, and after the pure aluminum is fully melted, obtaining C 2 Cl 6 Degassing, stirring, preserving heat, standing, casting by using an iron mold, and air cooling the alloy to obtain an ingot. The two kinds of alloy materials Al-0.25Er and Al-0.25Er-0.3Si are prepared, the two kinds of as-cast alloy are homogenized for 6 hours at 450 ℃, hot rolled at 450 ℃ and the deformation amount is 80%, the alloy is water-cooled for solution treatment after heat preservation for 1 hour at 540 ℃, the finally treated sample is polished by sand paper, the surface of the sample is polished by polishing paste, and Keller reagent (95% H 2 O+2.5%HNO 3 +1.5% hcl+1.0% hf) and finally observing the grain size of the sample after the solution treatment process in a dry environment using a metallographic microscope. As shown in fig. 1 (a), a metallographic image of an Al-0.25Er solution treated was compared with a metallographic image of an Al-0.25Er-0.3Si alloy shown in fig. 1 (b), and the average particle size was counted to obtain table 1:
table 1: average grain size of alloy
The composite addition of Si and Er obviously reduces the average grain size of the alloy, and the recrystallization grain refinement effect is obvious, which shows that the microalloy effect of Si and Er has obvious effect on aluminum alloy grain refinement. As shown in FIG. 4, which is a TEM image of Al-0.25Er-0.3Si alloy grain boundary, it can be obviously observed that black precipitated phases containing Si and Er elements exist at the grain boundary, and the existence of the precipitated phases prevents the growth of recrystallized grains, so that the recrystallized grains of the alloy are refined.
Example 2: two aluminum alloy cast ingots with different components are prepared by adopting graphite crucible smelting and iron mold casting, and the raw materials are high-purity aluminum, pure magnesium, al-50% Cu, al-24% Si and Al-6% Er intermediate alloy. Firstly, calculating the mass of required experimental raw materials according to designed alloy components, firstly, putting high-purity aluminum into a graphite crucible, heating and melting in a high-temperature smelting furnace at 800+/-5 ℃, then adding Al-50% Cu, al-24% Si and Al-6% Er intermediate alloy after the pure aluminum is completely melted, adding Mg wrapped by aluminum foil after the furnace burden is completely melted, preserving the heat for about 10min, fully stirring, and after the pure aluminum is fully melted, carrying out C 2 Cl 6 Degassing, stirring, preserving heat, standing, casting by using an iron mold, and air cooling the alloy to obtain an ingot. Three alloy materials of Al-4Cu-0.5Mg, al-4Cu-0.5Mg-0.15Si and Al-4Cu-0.5Mg-0.15Si-0.1Er are prepared, three as-cast alloys are homogenized at 450 ℃ for 6 hours and then hot rolled, the deformation is 80 percent, then the alloys are subjected to water cooling after being kept at 540 ℃ for 12 hours and then subjected to solution treatment, an experimental sample is cut into small samples of 10mm multiplied by 5mm, the samples are polished by sand paper, the polished surfaces of the samples are polished by polishing paste, and Keller reagent (95% H) 2 O+2.5%HNO 3 +1.5% hcl+1.0% hf) and finally observing the grain size of the sample after the solution treatment process in a dry environment using a metallographic microscope. As shown in fig. 2 (a), 2 (b) and 2 (c), the metallographic pictures of three alloys, i.e., al-4Cu-0.5Mg-0.15Si-0.1Er, after solution treatment, were taken, and the average grain sizes of the three alloys were counted to obtain table 2:
table 2: average grain size of alloy
By comparing the average grain sizes of the three alloys, the single addition of Si reduces the recrystallized grain size of the alloy, and the composite addition of Si and Er obviously refines the recrystallized grain size of the alloy, which shows that the composite addition of Si and Er has obvious effect on refining the recrystallized grain of the alloy.
Example 3: two aluminum alloy cast ingots with different components are prepared by adopting graphite crucible smelting and iron mold casting, and the used raw materials are high-purity aluminum, pure magnesium, pure zinc, al-50% Cu, al-24% Si and Al-6% Er intermediate alloy. Firstly, calculating the mass of required experimental raw materials according to designed alloy components, firstly, putting high-purity aluminum into a graphite crucible, heating and melting in a high-temperature smelting furnace at 800+/-5 ℃, then adding Al-50% Cu, al-24% Si and Al-6% Er intermediate alloy after the pure aluminum is completely melted, adding pure magnesium and pure zinc wrapped by aluminum foil after the furnace burden is completely melted, preserving heat for about 10min, fully stirring, and after the pure aluminum is fully melted, fully melting C 2 Cl 6 Degassing, stirring, preserving heat, standing, casting by using an iron mold, and air cooling the alloy to obtain an ingot. Three alloy materials of Al-4.5Zn-1.5Mg-1.0Cu, al-4.5Zn-1.5Mg-1.0Cu-0.35Si and Al-4.5Zn-1.5Mg-1.0Cu-0.35Si-0.1Er are prepared, three as-cast alloys are homogenized for 15 hours at 450 ℃, hot rolled at 450 ℃, the deformation amount is 80%, the alloy is kept at 540 ℃ for 1 hour, then water cooling is carried out, solution treatment is carried out on the alloy after the alloy is cooled, sand paper polishing is carried out on the treated alloy, polishing paste is used for polishing the surface of the sample, and Keller reagent (95% H 2 O+2.5%HNO 3 +1.5% hcl+1.0% hf) and finally observing the grain size of the sample after the solution treatment process in a dry environment using a metallographic microscope. As shown in fig. 3 (a), 3 (b) and 3 (c), the metallographic pictures after solution treatment of three alloys of Al-4.5Zn-1.5Mg-1.0Cu, al-4.5Zn-1.5Mg-1.0Cu-0.35Si and Al-4.5Zn-1.5Mg-1.0Cu-0.35Si-0.1Er are obviously observed by comparing the metallographic pictures, the addition of Si and Er elements reduces the size of recrystallized grains of the alloy, and the addition of trace Si leads to the refinement of the recrystallized grains of the alloy, and the fine grain effect after the composite addition of Si and Er is more obvious, similar to the result of example 2.
Claims (2)
1. A method for refining aluminum and aluminum alloy grains by micro-alloying Si and Er is characterized in that a proper amount of micro-alloying elements Si and Er are added into a pure aluminum or aluminum alloy matrix in a compounding way, an alloy ingot is subjected to heat treatment and rolling after homogenization, and then heat treatment is performed, and the grains are prevented from growing by precipitation of Si and Er at a recrystallization grain boundary;
adding Si and Er microalloying elements, wherein the weight percentage of the Si element in the final alloy is 0.15-0.3%, and the weight percentage of the Er element in the final alloy is 0.1-0.25%;
carrying out homogenization treatment at 440-460 ℃/6h on the aluminum alloy obtained by casting;
heat treatment and rolling after homogenization treatment: heat treatment is carried out for 1-2 h at 430-460 ℃, rolling is carried out at the heat treatment temperature, the deformation is 65-80%, and 1-pass rolling is carried out;
the temperature of the heat treatment after rolling is 530-550 ℃;
the aluminum alloy matrix is Al-Cu-Mg or Al-Zn-Mg-Cu alloy.
2. The method for refining aluminum and aluminum alloy grains by micro-alloying of Si and Er according to claim 1, wherein the heat treatment is carried out at 530-550 ℃, the temperature is raised from room temperature to 530-550 ℃, the heat is preserved for 1h, and then the water quenching is carried out for 10s to room temperature.
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