CN112030085B - Al-Cu-Mg-Si series alloy deformation heat treatment process - Google Patents
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Abstract
The invention relates to the technical field of high-performance corrosion-resistant aluminum alloy design, in particular to an Al-Cu-Mg-Si alloy thermomechanical treatment process. The thermomechanical treatment process designed by the invention comprises two schemes, wherein the first scheme is as follows: firstly carrying out solid solution treatment, then carrying out primary aging, and then assisting with pre-stretching deformation after the primary aging; then, matching with secondary aging to obtain a product in a secondary aging state; or, firstly carrying out solid solution treatment, then assisting with pre-stretching deformation, and then sequentially carrying out primary aging and secondary aging to obtain a product in a secondary aging state; and carrying out three-stage aging treatment on the product in the second-stage aging state to obtain a finished product. The invention has reasonable process design, simple and controllable preparation process, and excellent mechanical property and corrosion resistance of the obtained product, and is suitable for the field of aerospace or civil transportation.
Description
Technical Field
The invention relates to the technical field of high-performance corrosion-resistant aluminum alloy design, in particular to an Al-Cu-Mg-Si alloy thermomechanical treatment process.
Background
The Al-Cu-Mg-Si alloy is an aging-strengthening aluminum alloy, has the advantages of high strength, good welding performance and processing performance and the like, and is widely applied to the fields of aerospace and civil transportation. The alloy sheet is subjected to solution quenching, pre-stretching deformation is generally adopted to eliminate residual stress generated in the processing process, then single-stage peak value aging is carried out, and the alloy is applied to actual engineering in a peak value aging state. The pre-cooling deformation introduced before aging can eliminate residual stress in the material, and can regulate and control the subsequent aging precipitation process, thereby having great influence on the performance of the alloy. It is known that when the pre-cooling deformation is small, the deformation has small influence on the appearance of alloy grains, wherein the dislocation introduced by the pre-deformation plays a main role. The pre-stretching deformation after the solution quenching has a promoting effect on the aging precipitation of the aluminum alloy, can improve the alloy strength, but can also sacrifice the plasticity and the toughness of the material while improving the alloy strength. Therefore, a heat treatment process needs to be developed for the Al-Cu-Mg-Si alloy, and the strength, the plasticity and the toughness of the alloy can be improved at the same time.
To solve this problem, the subject group proposed a new heat treatment process in the already filed patent (application No. 2020106622047) to improve the impact toughness and corrosion resistance of the alloy while maintaining the mechanical properties of the alloy substantially unchanged or even improved. In order to further widen the application field of the alloy, improve the strength-elongation rate platform of the alloy and form a high-strength impact-resistant corrosion-resistant structure. The invention provides a novel thermomechanical treatment process on the basis of the alloy plate, a pre-stretching deformation process is added, the alloy plate is more suitable for processing procedures in actual production, and the strength, impact toughness and corrosion resistance of the alloy plate are improved.
Disclosure of Invention
Aiming at the defects of the prior art, the invention firstly provides an Al-Cu-Mg-Si alloy thermomechanical treatment process; the obtained aluminum alloy product has excellent mechanical property and corrosion resistance, and the preparation method and the application thereof.
The invention relates to an Al-Cu-Mg-Si series alloy thermomechanical treatment process; the alloy comprises the following components in percentage by mass: 3.9-4.2% of Cu, 0.4-0.6% of Mg, 0.6-0.9% of Si, 0.6-0.8% of Mn, less than 0.05% of each of inevitable impurity elements, less than 0.15% of total amount of impurity elements and the balance of Al;
the thermomechanical treatment strengthening and toughening process comprises one of the following two schemes;
scheme one
The method comprises the following steps: solid solution heat treatment, namely placing the extruded alloy in a resistance furnace, heating to 503 +/-2 ℃ at the speed of 5-10 ℃/min, and preserving heat for 2.5-3.5 h; water quenching, wherein the quenching transfer time is less than 10s, and a solid solution product is obtained;
step two: first-stage aging heat treatment, heating the alloy in a solid solution quenching state from room temperature to 160 +/-3 ℃, wherein the heating rate is 5-10 ℃/min, and keeping the temperature for 2.5-3.5 h; water quenching to obtain a first-stage aging product;
step three: and (3) performing pre-stretching deformation treatment at room temperature, wherein the product obtained in the step two is subjected to pre-stretching deformation, and the pre-deformation amount is 1.5% -3.0%.
Step four: secondary aging heat treatment, namely placing the product obtained in the step three in an aging furnace for heat treatment for 1-21d at 69-85 ℃, and performing water quenching to obtain a secondary aging product;
step five: performing third-stage aging heat treatment, namely placing the product obtained in the fourth step in an aging furnace, performing heat treatment at the temperature of 160 +/-3 ℃ for 0.5-14h, and performing water quenching to obtain a third-stage aging product;
scheme two
Step A: solid solution heat treatment, namely placing the extruded alloy in a resistance furnace, heating to 503 +/-2 ℃ at the speed of 5-10 ℃/min, and preserving heat for 2.5-3.5 h; water quenching, wherein the quenching transfer time is less than 10s, and a solid solution product is obtained;
and B: performing pre-stretching deformation treatment at room temperature, namely performing pre-stretching deformation on the product obtained in the step A, wherein the pre-deformation amount is 1.5-3.0%;
and C: first-stage aging heat treatment, heating the alloy in a solid solution quenching state from room temperature to 160 +/-3 ℃, wherein the heating rate is 5-10 ℃/min, and keeping the temperature for 2.5-3.5 h; water quenching to obtain a first-stage aging product;
step D: and D, secondary aging heat treatment, namely placing the product obtained in the step C into an aging furnace, performing heat treatment for 1-21d at 69-85 ℃, and performing water quenching to obtain a secondary aging product.
Step E: d, three-stage aging heat treatment, namely placing the product obtained in the step D into an aging furnace, performing heat treatment at the temperature of 160 +/-3 ℃ for 0.5-14h, and performing water quenching to obtain a three-stage aging product;
preferably, the alloy comprises the following components in percentage by mass: 4.17% of Cu, 0.42% of Mg, 0.7% of Si, 0.63% of Mn, less than 0.05% of each of inevitable impurity elements, less than 0.15% of total amount of impurity elements, and the balance of Al.
Preferably, the invention relates to a thermomechanical treatment process of an Al-Cu-Mg-Si alloy; in step three or step B, the deformation amount of the pre-stretching deformation is 2.5%.
Preferably, the invention relates to a thermomechanical treatment process of an Al-Cu-Mg-Si alloy; : in the fourth step or the step D, the furnace temperature is controlled at 80 +/-3 ℃ during the secondary aging.
Preferably, the invention relates to an Al-Cu-Mg-Si series alloy thermomechanical treatment process; in step four or step D, the heat treatment time is 21D.
Preferably, the invention relates to a thermomechanical treatment process of an Al-Cu-Mg-Si alloy; and (5) placing the product obtained in the fifth step in an aging furnace, performing heat treatment for 12h at the temperature of 160 +/-3 ℃, and performing water quenching to obtain a three-stage aging-state product.
Preferably, the invention relates to a thermomechanical treatment process of an Al-Cu-Mg-Si alloy; and E, placing the product obtained in the step E in an aging furnace, performing heat treatment for 14h at the temperature of 160 +/-3 ℃, and performing water quenching to obtain a three-stage aging-state product.
The invention relates to an Al-Cu-Mg-Si series alloy thermomechanical treatment process; the obtained Al-Cu-Mg-Si alloy has tensile strength of 541-542MPa, yield strength of 489-502MPa, elongation of 10.48-11.69% and impact toughness of 12.85-13.46J-cm2The maximum depth of intergranular corrosion is 183 μm or less, and the degree of denudation is PB level or more. The details of the relevant experiments are as follows: each set of room temperature tensile specimens was tested on an Instron model 3369 tensile tester with a loading rate of 2 mm/min. The length direction of a sample of a room temperature pendulum impact (Charpy impact) experiment is sampled along the material extrusion direction, the sample is prepared according to GB/T229-. And performing a spalling corrosion test on the aging-state sample according to the requirements of GB/T22639-. The surface to be etched is ground and polished, and then the treated sample is placed in a test solution (234g/L NaCl +50g/L KNO)3+6.5ml/L HNO3Aqueous solution of (d), the ratio of volume to sample experimental area is 27: 1, controlling the temperature at (25 +/-1) DEG C, soaking for 96h, photographing the corroded surface at intervals, recording and grading. And performing intercrystalline corrosion test on the aging-state sample according to the requirements of GB/T7998-. The surface to be etched was buffed and polished, and the treated sample was then placed in the test solution (57g/L NaCl +10ml H)2O2) And carrying out suspension soaking corrosion for 12h, taking out a corroded sample, grinding and polishing, and observing the corrosion depth of the T-S surface.
As a preference; the invention relates to an Al-Cu-Mg-Si series alloy thermomechanical treatment process; the extrusion ratio of the extruded alloy was 9:1, and the extrusion temperature was 440 ℃.
The invention relates to an Al-Cu-Mg-Si series alloy thermomechanical treatment process; the obtained product is used in the aerospace field or the civil vehicle field. Of course, the obtained product can be used as a structural member under high-load working conditions.
The process designed by the invention can synchronously improve the tensile strength, toughness and corrosion resistance of the product.
Principles and advantages
The primary aging heat treatment aims at aging the aluminum alloy in a solid solution quenching state to an underaging state, well utilizes a quenching vacancy, can precipitate more GP zones in a matrix, and the GP zones can be used as precursor phases of a subsequent aging strengthening phase. The energy difference between the inside of the crystal and the grain boundary is reduced due to the introduction of dislocation, the preferential precipitation tendency of the grain boundary is reduced, and meanwhile, the diffusion of solute atoms to the grain boundary is reduced due to the increase of the number of the precipitated phases in the crystal, so that the number of the precipitated phases in the grain boundary of the alloy is less, the distribution is more discontinuous, and the corrosion resistance of the alloy is improved.
Description of the drawings:
FIG. 1 is TEM images of the alloy in the crystal of examples one, two and comparative example one: (a) TEM image of A alloy; (b) TEM image of B alloy; (c) is a TEM image of the C alloy.
FIG. 2 is TEM images of the grain boundaries of alloys of examples I, II and comparative example I: (a) TEM image of A alloy; (b) TEM image of B alloy; (c) is a TEM image of the C alloy.
Table 1 toughness of the alloys obtained in the examples and comparative examples.
Table 2 corrosion resistance of the alloys obtained in the examples and comparative examples.
Detailed Description
The raw materials used in the examples and comparative examples of the present invention are Al-Cu-Mg-Si based alloys, which comprise the following components in mass percent: 3.9-4.2% of Cu, 0.4-0.6% of Mg, 0.6-0.9% of Si, 0.6-0.8% of Mn, less than 0.05% of each of inevitable impurity elements, less than 0.15% of total amount of impurity elements, and the balance of Al.
In the examples and comparative examples of the present invention, the raw material used was an Al-Cu-Mg-Si alloy, the extrusion ratio was 9:1, and the extrusion temperature was 440 ℃.
In the specific embodiment of the invention, the tensile property is based on the GB/T228.1-2010 standard, the impact property is based on the GB/T229-2007 standard, the spalling corrosion property is based on the GB/T22639-2008 standard, and the intergranular corrosion property is based on the GB/T7998-2005 standard.
Example one
Using an extruded Al-Cu-Mg-Si alloy as a raw material (the composition of which comprises, in mass percent, 4.17% of Cu, 0.42% of Mg, 0.70% of Si, 0.63% of Mn, and less than 0.05% of each of unavoidable impurity elements, less than 0.15% of total impurity elements, and the balance Al), and subjecting the raw material to the following heat treatment:
the method comprises the following steps: solid solution heat treatment, namely placing the extruded alloy in a resistance furnace, heating to 503 +/-2 ℃ at the speed of 5-10 ℃/min, and preserving heat for 3 hours; water quenching, wherein the quenching transfer time is less than 10s, and a solid solution product is obtained;
step two: first-stage aging heat treatment, heating the alloy in a solid solution quenching state from room temperature to 160 +/-3 ℃, wherein the heating rate is 5-10 ℃/min, and keeping the temperature for 3 hours; water quenching to obtain a first-stage aging product;
step three: and (3) pre-stretching deformation treatment at room temperature, namely pre-stretching deformation is carried out on the product obtained in the step two, the pre-deformation amount is 2.5%, and the deformation amount is finished on an Instron3369 type tensile testing machine at one time.
Step four: and (4) secondary aging heat treatment, namely placing the product obtained in the step three in an aging furnace, heating to 80 +/-3 ℃ at the speed of 5-10 ℃/min, preserving heat for 21d, and performing water quenching to obtain a secondary aging product.
Step five: and (3) carrying out third-stage aging heat treatment, namely placing the product obtained in the fourth step into an aging furnace, heating to 160 +/-3 ℃ at the speed of 5-10 ℃/min, keeping the temperature for 12h, and carrying out water quenching to obtain a third-stage aging product, wherein the product is abbreviated as A. The specific data of mechanical properties of the product in the three-stage aging state are shown in table 1, and the specific data of corrosion resistance of the product are shown in table 2. FIG. 1 is a TEM image of the inside of the alloy crystal after the aging treatment. FIG. 2 is a TEM image of the grain boundary of the alloy after the aging treatment.
Example two
The first step is completely the same as the first step, except that the sequence of pre-stretching deformation and primary aging heat treatment in the second step is different from that in the first step.
Step two: and (3) pre-stretching deformation treatment at room temperature, namely pre-stretching deformation is carried out on the product obtained in the step two, the pre-deformation amount is 2.5%, and the deformation amount is finished on an Instron3369 type tensile testing machine at one time.
Step three: first-stage aging heat treatment, heating the alloy in a solid solution quenching state from room temperature to 160 +/-3 ℃, wherein the heating rate is 5-10 ℃/min, and keeping the temperature for 3 hours; water quenching to obtain a first-stage aging product;
step four: and (4) secondary aging heat treatment, namely placing the product obtained in the step three in an aging furnace, heating to 80 +/-3 ℃ at the speed of 10 ℃/min, preserving heat for 21d, and performing water quenching to obtain a secondary aging product.
Step five: and (3) performing third-stage aging heat treatment, namely putting the product obtained in the fourth step into an aging furnace, heating to 160 +/-3 ℃ at the speed of 5-10 ℃/min, keeping the temperature for 14h, and performing water quenching to obtain a third-stage aging product, which is abbreviated as B. The specific data of the mechanical properties of the product are shown in table 1, and the specific data of the corrosion resistance of the product are shown in table 2.
Comparative example 1
Alloys under conventional single stage peak aging (T8) regime
Using an extruded Al-Cu-Mg-Si alloy as a raw material (the composition of which comprises, in mass percent, 4.17% of Cu, 0.42% of Mg, 0.70% of Si, 0.63% of Mn, and less than 0.05% of each of unavoidable impurity elements, less than 0.15% of total impurity elements, and the balance Al), and subjecting the raw material to the following heat treatment:
the first step, the second step and the second example are completely the same, except that the first comparative example also performs the traditional single-stage peak aging treatment on the product obtained in the second step of the second example.
Step three: single-stage peak value aging heat treatment, namely placing the product obtained in the step one in an aging furnace, heating to 160 +/-3 ℃ at the speed of 5-10 ℃/min, and preserving heat for 14 h; water quenching to obtain a single-stage peak value aging-state product; the product is designated as C. The specific data of the mechanical properties of the product are shown in table 1, and the specific data of the corrosion resistance of the product are shown in table 2. FIG. 1 is a TEM image of the inside of the crystal of the aged alloy. FIG. 2 is a TEM image of the grain boundary of the alloy after the aging treatment.
The results in tables 1 and 2 show that compared with the traditional T8 process, the alloy obtained in the first example has improved tensile strength and yield strength, the elongation is improved by 22.43 percent, and the impact toughness is improved by 23.44 percent; the tensile strength and the yield strength of the alloy obtained in the second example are improved, the elongation is improved by 36.57%, and the impact toughness is improved by 17.85%. Therefore, the mechanical property of the alloy treated by the thermomechanical treatment process is greatly improved. In addition, the intergranular corrosion resistance and the spalling corrosion resistance of the alloy treated by the heat treatment process are improved compared with those of the traditional T8-state alloy. Meanwhile, as can be seen from fig. 1 and 2, the alloy treated by the thermomechanical treatment process of the present invention has a higher density of precipitation-strengthened phases, a small size, and mainly contains a large amount of theta' phases dispersed, the number of the precipitation phases in the alloy grain boundary is small, and the distance between the phases is large, which is the reason for improving the strength, toughness and corrosion resistance of the alloy.
As shown by the comparison of the comparative example and the example, after the thermomechanical treatment process disclosed by the invention is adopted, the tensile strength is 541-542MPa, the yield strength is 489-502MPa, the elongation is 10.48-11.69%, and the impact toughness is 12.85-13.46J-cm2The maximum depth of intergranular corrosion is less than 183 mu m, and the denudation degree is more than PB level.
TABLE 1
TABLE 2
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (8)
1. An Al-Cu-Mg-Si series alloy deformation heat treatment process is characterized in that; the alloy comprises the following components in percentage by mass: 3.9-4.2% of Cu, 0.4-0.6% of Mg, 0.6-0.9% of Si, 0.6-0.8% of Mn, less than 0.05% of each of inevitable impurity elements, less than 0.15% of total amount of impurity elements and the balance of Al;
the thermomechanical treatment strengthening and toughening process comprises one of the following two schemes;
scheme one
The method comprises the following steps: solid solution heat treatment, namely placing the extruded alloy in a resistance furnace, heating to 503 +/-2 ℃ at the speed of 5-10 ℃/min, and preserving heat for 2.5-3.5 h; water quenching, wherein the quenching transfer time is less than 10s, and a solid solution product is obtained;
step two: first-stage aging heat treatment, heating the alloy in a solid solution quenching state from room temperature to 160 +/-3 ℃, wherein the heating rate is 5-10 ℃/min, and keeping the temperature for 2.5-3.5 h; water quenching to obtain a first-stage aging product;
step three: performing pre-stretching deformation treatment at room temperature, namely performing pre-stretching deformation on the product obtained in the step two, wherein the pre-deformation amount is 1.5-3.0%;
step four: performing secondary aging heat treatment, namely placing the product obtained in the step three in an aging furnace at 80 +/-3 ℃, performing heat treatment for 21d, and performing water quenching to obtain a secondary aging product;
step five: performing three-stage aging heat treatment, namely putting the product obtained in the step four into an aging furnace, performing heat treatment at the temperature of 160 +/-3 ℃ for 0.5-14h, and performing water quenching to obtain a three-stage aging product;
scheme two
Step A: solid solution heat treatment, namely placing the extruded alloy in a resistance furnace, heating to 503 +/-2 ℃ at the speed of 5-10 ℃/min, and preserving heat for 2.5-3.5 h; water quenching, wherein the quenching transfer time is less than 10s, and a solid solution product is obtained;
and B: performing pre-stretching deformation treatment at room temperature, namely performing pre-stretching deformation on the product obtained in the step two, wherein the pre-deformation amount is 1.5-3.0%;
and C: first-stage aging heat treatment, heating the alloy in a solid solution quenching state from room temperature to 160 +/-3 ℃, wherein the heating rate is 5-10 ℃/min, and keeping the temperature for 2.5-3.5 h; water quenching to obtain a first-stage aging product;
step D: c, secondary aging heat treatment, namely placing the product obtained in the step C in an aging furnace at 80 +/-3 ℃, performing heat treatment for 21d, and performing water quenching to obtain a secondary aging product;
step E: and D, three-stage aging heat treatment, namely placing the product obtained in the step D into an aging furnace, performing heat treatment at the temperature of 160 +/-3 ℃ for 0.5-14h, and performing water quenching to obtain a three-stage aging product.
2. The Al-Cu-Mg-Si based alloy thermomechanical treatment process of claim 1, wherein: the alloy comprises the following components in percentage by mass: 4.17% of Cu, 0.42% of Mg, 0.7% of Si, 0.63% of Mn, less than 0.05% of each of inevitable impurity elements, less than 0.15% of total amount of impurity elements, and the balance of Al.
3. The Al-Cu-Mg-Si based alloy thermomechanical treatment process of claim 1, wherein: in step three or step B, the deformation amount of the pre-stretching deformation is 2.5%.
4. The Al-Cu-Mg-Si based alloy thermomechanical treatment process of claim 1, wherein: and (5) placing the product obtained in the fifth step in an aging furnace, performing heat treatment for 12h at the temperature of 160 +/-3 ℃, and performing water quenching to obtain a three-stage aging-state product.
5. The Al-Cu-Mg-Si based alloy thermomechanical treatment process of claim 1, wherein: and (5) placing the product obtained in the fifth step in an aging furnace, performing heat treatment for 14h at 160 +/-3 ℃, and performing water quenching to obtain a three-stage aging-state product.
6. The Al-Cu-Mg-Si based alloy thermomechanical treatment process of claim 4 or 5, characterized in that: the tensile strength of the obtained Al-Cu-Mg-Si alloy is 541-542MPa, yield strength of 489-502MPa, elongation of 10.48-11.69%, and impact toughness of 12.85-13.46 J.cm2The maximum depth of intergranular corrosion is below 183 microns, and the degree of denudation is above PB level.
7. The Al-Cu-Mg-Si based alloy thermomechanical treatment process of claim 1, wherein: the extrusion ratio of the extruded alloy was 9:1, and the extrusion temperature was 440 ℃.
8. The Al-Cu-Mg-Si based alloy thermo-mechanical treatment process according to any one of claims 1 to 7, wherein: the obtained product is used in the aerospace field or the civil vehicle field.
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