CN112877622A - Non-isothermal heat treatment method of 7000 series aluminum alloy - Google Patents
Non-isothermal heat treatment method of 7000 series aluminum alloy Download PDFInfo
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Abstract
The invention provides a non-isothermal heat treatment method of 7000 series aluminum alloy; the method comprises high-temperature forced solution treatment, quenching treatment, pre-stretching treatment, cryogenic treatment and non-isothermal aging treatment, and can realize that the alloy strength of the high-alloying 7000 series aluminum alloy reaches or even exceeds the T6 state while the corrosion resistance of the alloy is improved, thereby avoiding the problem of strength loss after the alloy is subjected to the traditional aging heat treatment process (such as T77).
Description
Technical Field
The invention belongs to the technical field of aging heat treatment of 7000 series hard aluminum alloy, and relates to a non-isothermal heat treatment method of 7000 series aluminum alloy, in particular to high-alloying 7000 series aluminum alloy.
Background
The 7000 series aluminum alloy belongs to high-strength/ultrahigh-strength heat-treatable strengthened aluminum alloy, is widely applied to the field of aerospace, and has the characteristics of light weight, high specific strength, good toughness and good processability. With the higher and higher requirements of design units on the mechanical and corrosion resistance of aluminum alloy materials, the series of alloys are gradually and intensively developed in the directions of high alloying, large specification, integral manufacturing and the like.
As the key development direction of 7000 series aluminum alloys, the higher the alloying degree and the larger the semi-finished product specification, the more serious the local segregation of the alloy, and the more the intermediate phase exists in the matrix after the thermal deformation, and the higher the requirements for the solution quenching and aging process of the alloy. The traditional forced high-temperature solution quenching process cannot meet the conversion requirement of opposite supersaturated solid solutions of the middle phase of the high-alloying 7000 series aluminum alloy, the traditional aging processes of T6, T76 and T77 cannot meet the requirements on the mechanical property and the corrosion resistance of the series aluminum alloy, and the development of a novel solution quenching and aging heat treatment process is very important.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a non-isothermal heat treatment method of 7000 series aluminum alloy, which comprises high-temperature forced solution treatment, quenching treatment, pre-stretching treatment, cryogenic treatment and non-isothermal aging treatment, and can realize that the corrosion resistance of the high-alloying 7000 series aluminum alloy is improved, and simultaneously, the alloy strength (tensile strength and yield strength) reaches or even exceeds the T6 state, thereby avoiding the problem of strength loss of the alloy after the traditional T77 aging heat treatment process.
The purpose of the invention is realized by the following technical scheme:
a method of non-isothermal heat treatment of a 7000 series aluminum alloy, said method comprising the steps of:
(1) performing high-temperature forced solution treatment on a sample to be treated, wherein the high-temperature forced solution treatment comprises the steps of performing primary heat preservation on the sample to be treated by using a first temperature platform, then linearly heating the sample to be treated to a second temperature platform for secondary heat preservation, and then linearly heating the sample to a third temperature platform for tertiary heat preservation;
(2) sequentially carrying out quenching treatment, pre-stretching treatment and deep cooling treatment on the sample subjected to the high-temperature forced solution treatment;
(3) and carrying out non-isothermal aging treatment on the sample after cryogenic treatment, wherein the non-isothermal aging treatment comprises non-isothermal temperature rise primary aging treatment, linear temperature rise secondary regression aging treatment, quenching treatment and non-isothermal temperature reduction tertiary aging treatment.
In the present invention, the term "linear temperature rise" refers to a process of raising the temperature using a linear temperature rise rate. For example, "linearly increasing the temperature from the first temperature plateau to the second temperature plateau" means that the temperature increase process between the first temperature plateau and the second temperature plateau employs a linear temperature increase.
In the present invention, the term "non-isothermal" refers to a treatment process performed under a condition of a constant temperature change, and specifically, the term "non-isothermal temperature-raising primary aging treatment" refers to an aging treatment performed under a condition of a constant temperature rise, the term "non-isothermal temperature-lowering tertiary aging treatment" refers to an aging treatment performed under a condition of a constant temperature fall, and the term "linear temperature-raising secondary regression aging treatment" refers to an aging treatment performed after reaching a secondary aging temperature by linearly raising the temperature after the primary aging treatment is completed.
According to an embodiment of the present invention, in the step (1), the sample to be treated is, for example, 7000-series aluminum alloy, preferably 7000-series aluminum alloy after hot rolling.
According to an embodiment of the present invention, the 7000-series aluminum alloy is a 7000-series aluminum alloy conventional in the art; illustratively, the 7000 series aluminum alloy is selected from at least one of 7055 alloy, 7085 alloy, 7150 alloy, 7a55 alloy, 7a85 alloy, 7B50 alloy, 7050 alloy, and 7010 alloy.
According to the embodiment of the invention, in the step (1), the traditional high-temperature forced solution treatment adopts the technical processes of first temperature platform heat preservation → rapid temperature rise (the temperature rise rate is more than 30 ℃/h and is nonlinear temperature rise (the temperature rise rate is a curve and is increased and then decreased)) to second temperature platform heat preservation → rapid temperature rise (the temperature rise rate is more than 30 ℃/h and is nonlinear temperature rise (the temperature rise rate is a curve and is increased and then decreased)) to third temperature platform heat preservation, belongs to the process design of a crossing temperature platform, and aims at the problems that the high-alloyed alloy is easy to have unsatisfactory intermediate phase redissolution degree, and the improper operation of equipment is easy to have the problems of alloy overburning or insufficient furnace temperature uniformity caused by high temperature rushing and falling; the high-temperature forced solution treatment adopts the technical process of first temperature platform heat preservation → linear temperature rise (the temperature rise rate is 5-30 ℃/h) to second temperature platform heat preservation → linear temperature rise (the temperature rise rate is 5-30 ℃/h) to third temperature platform heat preservation, and particularly when aiming at high-alloying 7000 series aluminum alloy, the high-temperature forced solution treatment can remarkably improve the solid solution degree of a mesophase, improve the supersaturation degree of a matrix, and simultaneously avoid the problems of alloy overburning or furnace temperature uniformity insufficiency and the like caused by high temperature rush fall-back.
According to an embodiment of the present invention, in the step (1), the high temperature forced solution treatment is performed in a heat treatment furnace, which is a heat treatment furnace known in the art.
According to an embodiment of the present invention, in step (1), the first temperature plateau is (460 to 465) ° c ± 3 ℃, such as 460 ℃ ± 3 ℃, 461 ℃ ± 3 ℃, 462 ℃ ± 3 ℃, 463 ℃ ± 3 ℃, 464 ℃ ± 3 ℃, 465 ℃ ± 3 ℃; the first-stage heat preservation time is 1 to 2 times the minutes of the thickness (unit mm) of the sample, for example, 1 time, 1.5 times or 2 times; the temperature of the first-stage heat preservation is the temperature of the first temperature platform.
The number of minutes of the sample thickness is the corresponding incubation time, i.e., the thickness (unit mm) of the sample, and illustratively, the incubation time is 25min when the thickness of the sample is 25 mm.
According to an embodiment of the present invention, in step (1), the second temperature plateau is (466 to 470) ° c ± 3 ℃, such as 466 ℃ ± 3 ℃, 467 ℃ ± 3 ℃, 468 ℃ ± 3 ℃, 469 ℃ ± 3 ℃, 470 ℃ ± 3 ℃; the time of the second-stage heat preservation is 1 to 2 times the minutes of the thickness (unit mm) of the sample, for example, 1 time, 1.5 times or 2 times; the temperature of the second-stage heat preservation is the temperature of the second temperature platform.
According to an embodiment of the present invention, in step (1), the third temperature plateau is (471 to 475) ° c ± 3 ℃, such as 471 ℃ ± 3 ℃, 472 ℃ ± 3 ℃, 473 ℃ ± 3 ℃, 474 ℃ ± 3 ℃, 475 ℃ ± 3 ℃; the third-stage heat preservation time is 1-2 times of the minutes plus 60min of the thickness (unit mm) of the sample, for example, 1 time of the minutes plus 60min of the thickness of the sample, 1.5 times of the minutes plus 60min of the thickness of the sample, or 2 times of the minutes plus 60min of the thickness of the sample; the temperature of the third stage heat preservation is the temperature of the third temperature platform.
According to the embodiment of the invention, in the step (1), the temperature rise rate of the linear temperature rise to the second temperature platform is 5-30 ℃/h, such as 5 ℃/h, 8 ℃/h, 10 ℃/h, 15 ℃/h, 18 ℃/h, 20 ℃/h, 22 ℃/h, 25 ℃/h, 28 ℃/h, 30 ℃/h; the temperature rise rate of the linear temperature rise to the third temperature platform is 5-30 ℃/h, such as 5 ℃/h, 8 ℃/h, 10 ℃/h, 15 ℃/h, 18 ℃/h, 20 ℃/h, 22 ℃/h, 25 ℃/h, 28 ℃/h and 30 ℃/h.
According to an embodiment of the present invention, in the step (2), the sample after the high-temperature forced solution treatment is subjected to room-temperature water quenching treatment, and the temperature of the room-temperature water is, for example, 20 to 35 ℃.
According to an embodiment of the present invention, in the step (2), the sample after the high-temperature forced solution treatment is preferably subjected to a room-temperature water quenching treatment within 10 to 20 seconds, and preferably within 10 seconds, 15 seconds, or 20 seconds.
According to an embodiment of the present invention, in the step (2), the temperature of the sample after the quenching treatment is 20 to 35 ℃.
According to an embodiment of the present invention, in the step (2), the sample after the quenching treatment is subjected to pre-stretching in an amount of 1 to 3%. The pre-stretching treatment is preferably completed within 30min after the quenching treatment.
According to an embodiment of the present invention, in the step (2), the deep cooling treatment is a deep cooling treatment of the pre-stretched sample, and preferably the sample is placed in a deep cooling furnace for heat preservation treatment, wherein the heat preservation temperature is (-80 to-120) DEG C + -10 ℃, for example, -80℃ + -10 ℃, -85℃ + -10 ℃, -90℃ + -10 ℃, -95℃ + -10 ℃, -100℃ + -10 ℃, -105℃ + -10 ℃, -110℃ + -10 ℃, -115℃ + -10 ℃, -120℃ + -10 ℃; the heat preservation time is 30-120 min, such as 60 min.
According to the embodiment of the present invention, in the step (2), the temperature of the sample after the deep cooling treatment is (-80 to-120) ° c + -10 ℃.
According to the embodiment of the invention, in the step (2), the pre-stretching treatment and the cryogenic treatment can reduce the natural aging process while slowly releasing the quenching stress.
According to the embodiment of the invention, in the step (2), the non-isothermal aging treatment is carried out after the cryogenic treatment is finished.
According to an embodiment of the invention, in the step (3), the non-isothermal temperature-rise primary aging treatment is that the sample after deep cooling treatment is loaded into a heat treatment furnace with the temperature of 90 +/-5 ℃, then the sample is heated to (110-130) ° c +/-5 ℃ at a linear heating rate of 5-10 ℃/h and then is subjected to heat preservation, the total heat preservation time is 18-36 h, the total heat preservation time is the sum of the heating time of the sample loaded into the heat treatment furnace with the temperature of 90 +/-5 ℃ to the temperature of (110-130) ° c +/-5 ℃ and the heat preservation time of heat preservation at the temperature of (110-130) ° c +/-5 ℃, namely the total heat preservation time comprises the time of a heating stage and the time of a heat preservation stage.
According to an embodiment of the present invention, in the step (3), the linear temperature-increasing second-order regression aging treatment is performed by increasing the temperature to (175-185) ° c ± 5 ℃ at a linear temperature-increasing rate of 200-240 ℃/h, and then performing heat preservation, wherein the heat preservation time is 1-2 h, and the heat preservation time is only the time for increasing the temperature to (175-185) ° c ± 5 ℃ and then performing heat preservation. The linear heating rate of 200-240 ℃/h is selected to ensure that the temperature can be rapidly raised to the pre-heat preservation temperature, prevent the strengthening phase dispersed and precipitated in the primary aging process from growing up in the heating process, realize the purpose of regression heat treatment and obtain the ideal alloy performance.
According to an embodiment of the present invention, in the step (3), the quenching treatment is preferably a room temperature water quenching treatment, and the temperature of the room temperature water is, for example, 20 to 35 ℃.
According to an embodiment of the present invention, in the step (3), the temperature of the sample after the quenching treatment is 20 to 35 ℃.
According to the embodiment of the invention, in the step (3), the non-isothermal temperature-reduction three-stage aging treatment is to load the sample after quenching treatment into a heat treatment furnace with the temperature of (130-150) ± 5 ℃, then linearly reduce the temperature to (115-135) ° c ± 5 ℃ at 5-10 ℃/h, carry out heat preservation, carry out air cooling after the heat preservation is completed, and carry out the heat preservation for 12-24 h, wherein the total heat preservation time is the sum of the temperature reduction time of the sample loaded into the heat treatment furnace with the temperature of (130-150) ± 5 ℃ to reduce the temperature to (115-135) ° c ± 5 ℃ and the heat preservation time of carrying out the heat preservation at (115-135) ° c ± 5 ℃, namely the total heat preservation time comprises the time of the temperature reduction stage and the time of the heat preservation stage.
According to an embodiment of the present invention, in step (3), the aging temperature of the tertiary aging treatment is higher than the aging temperature of the primary aging treatment.
According to the embodiment of the invention, in the step (3), the traditional T77 aging treatment process is a regression aging process of performing rapid temperature rise to a higher temperature for heat preservation and then performing rapid quenching in two T6 aging (long-time heat preservation with the same temperature) processes, while the non-isothermal aging treatment of the invention is a process of performing non-isothermal temperature rise first-stage aging, linear temperature rise second-stage regression aging, quenching and non-isothermal temperature reduction third-stage aging, the aging temperature of the first-stage and third-stage aging treatments is slightly higher than that of the first-stage aging treatment while the non-isothermal processes are adopted, after the non-isothermal aging treatment of the invention, the aim of improving the corrosion resistance of the alloy can be achieved, the strengthening dispersed phase can be forcedly separated out, the alloy strength even exceeding the T6 state can be achieved, and the alloy is prevented from being subjected to the traditional T77 heat treatment process, a problem of strength loss occurs.
According to an embodiment of the invention, the method comprises the steps of:
1) and (3) carrying out high-temperature forced solution treatment: charging at 462 +/-3 ℃, keeping the temperature for 1 time of minutes of plate thickness, linearly heating to 467 +/-3 ℃ at 20 ℃/h after the heat preservation is finished, keeping the temperature for 1 time of minutes of plate thickness, linearly heating to 472 +/-3 ℃ at 20 ℃/h after the heat preservation is finished, and keeping the temperature for 1 time of minutes plus 60 min;
2) after the heat preservation is finished, quenching with room temperature water within 15s, and finishing the pre-stretching within 30min after the quenching is finished, wherein the pre-stretching amount is 1-3%;
3) immediately putting the pre-stretched material into a deep cooling furnace for heat preservation at the temperature of minus 100 +/-10 ℃ for 60 min;
4) and (3) after the heat preservation is finished, carrying out non-isothermal aging treatment: putting the sample obtained in the step 3) into a heat treatment furnace at 90 +/-5 ℃, linearly heating to 120 +/-5 ℃ at the speed of 10 ℃/h, and then carrying out heat preservation for 24 h; after the heat preservation is finished, linearly heating to 175 +/-5 ℃ at the speed of 240 ℃/h, and then preserving the heat for 60 min; carrying out quenching treatment at room temperature after heat preservation; putting the quenched sample into a heat treatment furnace at the temperature of 130 +/-5 ℃, linearly cooling to 120 +/-5 ℃ at the speed of 10 ℃/h, and then carrying out heat preservation for 16 h; taking out of the furnace and air cooling after the heat preservation is finished;
the above method is applicable to 7000 series aluminum alloys, such as 7050 aluminum alloy, having Zn ≦ 8%.
According to an embodiment of the invention, the method comprises the steps of:
1) and (3) carrying out high-temperature forced solution treatment: charging at 465 +/-3 ℃, keeping the temperature for minutes which are 1.5 times of the plate thickness, linearly heating to 470 +/-3 ℃ at 10 ℃/h after the heat preservation is finished, keeping the temperature for minutes which are 1.5 times of the plate thickness, linearly heating to 475 +/-3 ℃ at 20 ℃/h after the heat preservation is finished, and keeping the temperature for minutes which are 1.5 times of the plate thickness plus 60 min;
2) after the heat preservation is finished, quenching with room temperature water within 15s, and finishing the pre-stretching within 30min after the quenching is finished, wherein the pre-stretching amount is 1-3%;
3) immediately putting the pre-stretched material into a deep cooling furnace for heat preservation at the temperature of minus 100 +/-10 ℃ for 60 min;
4) and (3) after the heat preservation is finished, carrying out non-isothermal aging treatment: putting the sample obtained in the step 3) into a heat treatment furnace at 90 +/-5 ℃, linearly heating to 120 +/-5 ℃ at the speed of 5 ℃/h, and then carrying out heat preservation for 24 h; after the heat preservation is finished, linearly heating to 185 +/-5 ℃ at the speed of 240 ℃/h, and then preserving the heat for 60 min; carrying out quenching treatment at room temperature after heat preservation; putting the quenched sample into a heat treatment furnace at the temperature of 130 +/-5 ℃, linearly cooling to 120 +/-5 ℃ at the speed of 5 ℃/h, and then carrying out heat preservation for 16 h; taking out of the furnace and air cooling after the heat preservation is finished;
the above method is suitable for a high-alloying 7000 series aluminum alloy with Zn ≧ 8%, such as 7A95 aluminum alloy.
In the present invention, the quenching treatment is a process for maintaining the high-temperature or low-temperature structural characteristics of the structure at room temperature by rapidly cooling the structure at high temperature or low temperature to room temperature. When the temperature of the center of the sample after quenching treatment reaches a room temperature state, generally 20 to 35 ℃, the quenching treatment is considered to be finished.
The invention also provides a preparation method of the 7000 series aluminum alloy plate, which comprises the following steps:
(a) subjecting 7000 series aluminum alloy cast ingots to homogenization treatment and hot rolling treatment in sequence to obtain a test material;
(b) and (b) subjecting the sample obtained in step (a) to non-isothermal heat treatment by the above-mentioned non-isothermal heat treatment method for 7000-series aluminum alloy to obtain the 7000-series aluminum alloy plate.
According to the embodiment of the invention, the thickness of the 7000 series aluminum alloy plate is 6 mm-60 mm.
According to the embodiment of the invention, the 7000 series aluminum alloy plate adopts high-temperature forced solution treatment, then the intermediate phase formed after thermal deformation can be re-dissolved in the matrix to form a solid solution exceeding saturation, and after rapid quenching to room temperature, pre-stretching treatment, cryogenic treatment and non-isothermal aging treatment are immediately carried out, so that the corrosion resistance target of the alloy can be improved, and the alloy strength can reach or even exceed the T6 state.
The invention has the beneficial effects that:
the invention provides a non-isothermal heat treatment method of 7000 series aluminum alloy; the method comprises high-temperature forced solution treatment, quenching treatment, pre-stretching treatment, cryogenic treatment and non-isothermal aging treatment, and can realize that the alloy strength of the high-alloying 7000 series aluminum alloy reaches or even exceeds the T6 state while the corrosion resistance of the alloy is improved, thereby avoiding the problem of strength loss after the alloy is subjected to the traditional aging heat treatment process (such as T77).
Drawings
FIG. 1 is a process flow diagram of a non-isothermal heat treatment method according to a preferred embodiment of the present invention.
FIG. 2 is a process flow diagram of a heat treatment method of a conventional process (multi-stage solid solution + pre-stretching + T77 three-stage aging treatment) in the prior art.
Detailed Description
The preparation method of the present invention will be described in further detail with reference to specific examples. It is to be understood that the following examples are only illustrative and explanatory of the present invention and should not be construed as limiting the scope of the present invention. All the technologies realized based on the above-mentioned contents of the present invention are covered in the protection scope of the present invention.
The experimental methods used in the following examples are all conventional methods unless otherwise specified; reagents, materials and the like used in the following examples are commercially available unless otherwise specified.
Comparative example 1:
the 7050 aluminum alloy 25mm thick plate is treated by adopting a traditional heat treatment process, and the process flow is as follows: performing three-stage high-temperature forced solution treatment, wherein the process is 462 ℃ multiplied by 30min +467 ℃ multiplied by 30min +472 ℃ multiplied by 90min (rapid temperature rise is adopted for each stage of temperature platform change, and the rapid temperature rise rate is 100 ℃/h); after the heat preservation is finished, quenching with room temperature water within 15s, and finishing the pre-stretching within 30min after the quenching is finished, wherein the pre-stretching amount is 1.5%; after the pre-stretching is completed, a conventional T77 treatment is carried out: the temperature is 120 ℃ multiplied by 24h (the temperature is preserved after the material is put into a heat treatment furnace at 120 ℃, the heat preservation time is 24 h) +175 ℃ multiplied by 60min (the temperature is preserved after the material is linearly heated to 175 ℃ at 240 ℃/h), the heat preservation time is 60 min) + quenching +120 ℃ multiplied by 24h (the material is put into the heat treatment furnace at 120 ℃, the heat preservation time is 24 h), and the material is taken out of the furnace and cooled in air after the temperature is reached.
Comparative example 2:
the 7050 aluminum alloy 25mm thick plate is treated by adopting a solid solution and traditional T6 heat treatment process, and the process flow is as follows: and (3) carrying out high-temperature forced solution treatment:
462 ℃ multiplied by 25min +467 ℃ multiplied by 25min +472 ℃ multiplied by 85min (each stage of temperature platform changes by adopting linear temperature rise of 20 ℃/h); after the heat preservation is finished, quenching with room temperature water within 15s, and finishing the pre-stretching within 30min after the quenching is finished, wherein the pre-stretching amount is 1.5%; immediately putting the pre-stretched material into a deep cooling furnace for heat preservation at the temperature of-100 ℃ for 60min after pre-stretching; and (4) carrying out T6 treatment after the heat preservation is finished: and (3) placing the mixture into a heat treatment furnace at 120 ℃, preserving heat for 24 hours, taking the mixture out of the furnace after the temperature is reached, and cooling the mixture in the air.
Comparative example 3:
the 7A95 aluminum alloy 25mm thick plate is treated by adopting a traditional heat treatment process, and the process flow is as follows: and (2) carrying out three-stage high-temperature forced solution treatment, wherein the process comprises 465 ℃ multiplied by 30min, 470 ℃ multiplied by 30min, 475 ℃ multiplied by 90min (rapid heating is adopted for each stage of temperature platform change, the rapid heating rate is 100 ℃/h, after the heat preservation is finished, room-temperature water quenching is carried out within 15s, pre-stretching is finished within 30min after quenching, the pre-stretching amount is 1.5%, after pre-stretching is finished, the traditional T77 treatment is carried out, namely 120 ℃ multiplied by 24h (heat preservation is carried out after the pre-stretching is finished, the heat preservation time is 24h after the pre-stretching is finished, the heat preservation time is 175 ℃ multiplied by 60min (heat preservation is carried out after the pre-stretching is finished), the heat preservation time is 60min after the pre-stretching is finished, the heat preservation time is carried out after the pre-stretching is finished, the.
Comparative example 4:
the 7A95 aluminum alloy 25mm thick plate is treated by adopting a solid solution and traditional T6 heat treatment process, and the process flow is as follows: and (3) carrying out high-temperature forced solution treatment:
465 ℃ multiplied by 25min +470 ℃ multiplied by 25min +475 ℃ multiplied by 85min (each stage of temperature platform changes adopt 10 ℃/h linear temperature rise); after the heat preservation is finished, quenching with room temperature water within 15s, and finishing the pre-stretching within 30min after the quenching is finished, wherein the pre-stretching amount is 1.5%; immediately putting the pre-stretched material into a deep cooling furnace for heat preservation at the temperature of-100 ℃ for 60min after pre-stretching; and (4) carrying out T6 treatment after the heat preservation is finished: and (4) placing the mixture into a heat treatment furnace at 135 ℃, preserving heat for 16 hours, taking the mixture out of the furnace after the temperature is reached, and cooling the mixture in the air.
Example 1:
the 7050 aluminum alloy 25mm thick plate is treated by adopting a non-isothermal heat treatment process, which comprises the following process steps: and (3) carrying out high-temperature forced solution treatment: 459 ℃ multiplied by 25min +464 ℃ multiplied by 25min +469 ℃ multiplied by 85min (each stage of temperature platform changes and adopts 20 ℃/h linear temperature rise); after the heat preservation is finished, quenching with room temperature water within 15s, and finishing the pre-stretching within 30min after the quenching is finished, wherein the pre-stretching amount is 1.5%; immediately putting the pre-stretched material into a deep cooling furnace for heat preservation at the temperature of minus 90 ℃ for 60 min; and (3) carrying out non-isothermal aging treatment after the heat preservation is finished: and (2) putting the mixture into a heat treatment furnace at 85 ℃, linearly heating to 115 ℃ at a speed of 10 ℃/h, then preserving heat for 24h, linearly heating to 170 ℃ at a speed of 240 ℃/h after the heat preservation is finished, preserving heat for 60min, carrying out quenching treatment at room temperature after the heat preservation is finished, immediately putting the mixture into a heat treatment furnace at 125 ℃ after the quenching is finished, linearly cooling to 115 ℃ at a speed of 10 ℃/h, preserving heat for 16h, taking the mixture out of the furnace after the temperature is reached, and carrying out air cooling.
Example 2:
the 7050 aluminum alloy 25mm thick plate is treated by adopting a non-isothermal heat treatment process, which comprises the following process steps: and (3) carrying out high-temperature forced solution treatment: 465 ℃ multiplied by 25min +470 ℃ multiplied by 25min +475 ℃ multiplied by 85min (each stage of temperature platform changes adopts linear temperature rise of 20 ℃/h); after the heat preservation is finished, quenching with room temperature water within 15s, and finishing the pre-stretching within 30min after the quenching is finished, wherein the pre-stretching amount is 1.5%; immediately putting the pre-stretched material into a deep cooling furnace for heat preservation at the temperature of minus 110 ℃ for 60min after pre-stretching; and (3) carrying out non-isothermal aging treatment after the heat preservation is finished: and (2) putting the mixture into a heat treatment furnace at the temperature of 95 ℃, linearly heating to 125 ℃ at the speed of 10 ℃/h, then preserving heat for 24h, linearly heating to 180 ℃ at the speed of 240 ℃/h after the heat preservation is finished, preserving heat for 60min, carrying out quenching treatment at room temperature after the heat preservation is finished, immediately putting the mixture into a heat treatment furnace at the temperature of 135 ℃, linearly cooling to 125 ℃ at the speed of 10 ℃/h, preserving heat for 16h, taking the mixture out of the furnace after the temperature is reached, and carrying out air cooling.
Example 3:
the 7A95 aluminum alloy 25mm thick plate is processed by adopting a non-isothermal heat treatment process, which comprises the following steps: and (3) carrying out high-temperature forced solution treatment: 462 ℃ multiplied by 25min +467 ℃ multiplied by 25min +472 ℃ multiplied by 85min (each stage of temperature platform changes by adopting 10 ℃/h linear temperature rise); after the heat preservation is finished, quenching with room temperature water within 15s, and finishing the pre-stretching within 30min after the quenching is finished, wherein the pre-stretching amount is 1.5%; immediately putting the pre-stretched material into a deep cooling furnace for heat preservation at the temperature of minus 90 ℃ for 60 min; and (3) carrying out non-isothermal aging treatment after the heat preservation is finished: and (2) putting the mixture into a heat treatment furnace at 85 ℃, linearly heating to 115 ℃ at 5 ℃/h, then preserving heat for 24h, linearly heating to 180 ℃ at 240 ℃/h after the heat preservation is finished, preserving heat for 60min, carrying out quenching treatment at room temperature after the heat preservation is finished, immediately putting the mixture into a heat treatment furnace at 125 ℃ after the quenching is finished, linearly cooling to 115 ℃ at 5 ℃/h, preserving heat for 16h, taking the mixture out of the furnace after the temperature is reached, and carrying out air cooling.
Example 4:
the 7A95 aluminum alloy 25mm thick plate is processed by adopting a non-isothermal heat treatment process, which comprises the following steps: and (3) carrying out high-temperature forced solution treatment: 468 ℃ is multiplied by 25min +473 ℃ is multiplied by 25min +478 ℃ is multiplied by 85min (each stage of temperature platform changes adopts 10 ℃/h linear temperature rise); after the heat preservation is finished, quenching with room temperature water within 15s, and finishing the pre-stretching within 30min after the quenching is finished, wherein the pre-stretching amount is 1.5%; immediately putting the pre-stretched material into a deep cooling furnace for heat preservation at the temperature of minus 110 ℃ for 60min after pre-stretching; and (3) carrying out non-isothermal aging treatment after the heat preservation is finished: and (2) placing the materials into a heat treatment furnace at the temperature of 95 ℃, linearly heating to 125 ℃ at the speed of 5 ℃/h, then preserving heat for 24h, linearly heating to 190 ℃ at the speed of 240 ℃/h after the heat preservation is finished, preserving heat for 60min, carrying out quenching treatment at room temperature after the heat preservation is finished, immediately placing the materials into a heat treatment furnace at the temperature of 135 ℃, linearly cooling to 125 ℃ at the speed of 5 ℃/h, then preserving heat for 16h, taking the materials out of the furnace after the materials reach the temperature, and carrying out air cooling.
Table 1 is a list of compositions of aluminum alloys used in the above examples and comparative examples, in which the contents of the respective elements were measured using methods known in the art.
TABLE 1 compositions of aluminum alloys used in examples and comparative examples
Table 2 shows the results of the performance tests of the treated aluminum alloy slabs of the examples and comparative examples, wherein the tensile strength, yield strength and elongation are measured by the GB/T228.1 test method using an electronic universal material tester for room temperature tensile tests, and the corrosion resistance is measured by the HB 5455 test method for immersion tests. The specific test results are detailed in table 2.
TABLE 2 results of performance test of the treated aluminum alloy slabs of examples and comparative examples
As can be seen from Table 2, the alloy thick plate prepared by the method of the invention has improved corrosion resistance and alloy strength even exceeding T6 state.
The embodiments of the present invention have been described above. However, the present invention is not limited to the above embodiment. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method of non-isothermal heat treatment of a 7000 series aluminum alloy, said method comprising the steps of:
1) performing high-temperature forced solution treatment on a sample to be treated, wherein the high-temperature forced solution treatment comprises the steps of performing primary heat preservation on the sample to be treated by using a first temperature platform, then linearly heating the sample to be treated to a second temperature platform for secondary heat preservation, and then linearly heating the sample to a third temperature platform for tertiary heat preservation;
(2) sequentially carrying out quenching treatment, pre-stretching treatment and deep cooling treatment on the sample subjected to the high-temperature forced solution treatment;
(3) and carrying out non-isothermal aging treatment on the sample after cryogenic treatment, wherein the non-isothermal aging treatment comprises non-isothermal temperature rise primary aging treatment, linear temperature rise secondary regression aging treatment, quenching treatment and non-isothermal temperature reduction tertiary aging treatment.
2. The method according to claim 1, wherein in the step (1), the sample to be processed is 7000 series aluminum alloy, and the 7000 series aluminum alloy is at least one selected from 7055 alloy, 7085 alloy, 7150 alloy, 7a55 alloy, 7a85 alloy, 7B50 alloy, 7050 alloy, and 7010 alloy.
3. The method according to claim 1, wherein in step (1), the first temperature plateau is (460-465) C ± 3 ℃; the first-stage heat preservation time is 1-2 times of minutes of the thickness of the sample, wherein the unit of the thickness of the sample is mm; and/or, in the step (1), the second temperature platform is (466-470) DEG C +/-3 ℃; the time of the second-stage heat preservation is 1-2 times of minutes of the thickness of the sample; the temperature of the second-stage heat preservation is the temperature of a second temperature platform, wherein the unit of the thickness of the sample is mm; and/or, in the step (1), the third temperature platform is (471-475) ° c +/-3 ℃; the third-stage heat preservation time is 1-2 times of the minutes of the thickness of the sample and 60 min; the temperature of the third stage heat preservation is the temperature of a third temperature platform, wherein the unit of the thickness of the sample is mm.
4. The method according to claim 1, wherein in the step (1), the temperature rise rate of the linear temperature rise to the second temperature platform is 5-30 ℃/h; the temperature rise rate of the platform for linearly rising the temperature to the third temperature is 5-30 ℃/h.
5. The method according to claim 1, wherein in the step (2), the quenching treatment is performed by subjecting the sample after the high-temperature forced solution treatment to water quenching treatment at room temperature within 10 to 20 seconds; and/or the temperature of the sample after the quenching treatment is 20 to 35 ℃.
6. The method according to claim 1, wherein in the step (2), the pre-stretching treatment is to pre-stretch the sample after the quenching treatment is completed, and the pre-stretching amount is 1-3%; and/or in the step (2), the deep cooling treatment is to put the sample after the pre-stretching treatment into a deep cooling furnace for heat preservation treatment, wherein the heat preservation temperature is (-80 to-120) DEG C +/-10 ℃; the heat preservation time is 30-120 min.
7. The method according to claim 1, wherein in the step (3), the non-isothermal temperature-rise primary aging treatment is to load the sample after the deep cooling treatment into a heat treatment furnace with the temperature of 90 +/-5 ℃, then raise the temperature to (110-130) DEG C +/-5 ℃ at a linear temperature rise rate of 5-10 ℃/h, and then carry out heat preservation, wherein the total heat preservation time is 18-36 h; and/or the presence of a gas in the gas,
in the step (3), the linear heating secondary regression aging treatment is to heat the temperature to (175-185) ° c +/-5 ℃ at a linear heating rate of 200-240 ℃/h, and then to carry out heat preservation for 1-2 h; and/or the presence of a gas in the gas,
in the step (3), the non-isothermal cooling three-stage aging treatment is to load the quenched sample into a heat treatment furnace with the temperature of (130-150) +/-5 ℃, then linearly cool the sample to (115-135) +/-5 ℃ at the speed of 5-10 ℃/h, then keep the temperature, keep the total temperature for 12-24 h, and take the sample out of the furnace for air cooling after the temperature is kept for a while.
8. The method according to any one of claims 1-7, wherein the method comprises the steps of:
1) and (3) carrying out high-temperature forced solution treatment: charging at 462 +/-3 ℃, keeping the temperature for 1 time of minutes of plate thickness, linearly heating to 467 +/-3 ℃ at 20 ℃/h after the heat preservation is finished, keeping the temperature for 1 time of minutes of plate thickness, linearly heating to 472 +/-3 ℃ at 20 ℃/h after the heat preservation is finished, and keeping the temperature for 1 time of minutes plus 60 min;
2) after the heat preservation is finished, quenching with room temperature water within 15s, and finishing the pre-stretching within 30min after the quenching is finished, wherein the pre-stretching amount is 1-3%;
3) immediately putting the pre-stretched material into a deep cooling furnace for heat preservation at the temperature of minus 100 +/-10 ℃ for 60 min;
4) and (3) after the heat preservation is finished, carrying out non-isothermal aging treatment: putting the sample obtained in the step 3) into a heat treatment furnace at 90 +/-5 ℃, linearly heating to 120 +/-5 ℃ at the speed of 10 ℃/h, and then carrying out heat preservation for 24 h; after the heat preservation is finished, linearly heating to 175 +/-5 ℃ at the speed of 240 ℃/h, and then preserving the heat for 60 min; carrying out quenching treatment at room temperature after heat preservation; putting the quenched sample into a heat treatment furnace at the temperature of 130 +/-5 ℃, linearly cooling to 120 +/-5 ℃ at the speed of 10 ℃/h, and then carrying out heat preservation for 16 h; taking out of the furnace and air cooling after the heat preservation is finished; the method is suitable for 7000 series aluminum alloy with Zn less than or equal to 8 percent.
9. The method according to any one of claims 1-7, wherein the method comprises the steps of:
1) and (3) carrying out high-temperature forced solution treatment: charging at 465 +/-3 ℃, keeping the temperature for minutes which are 1.5 times of the plate thickness, linearly heating to 470 +/-3 ℃ at 10 ℃/h after the heat preservation is finished, keeping the temperature for minutes which are 1.5 times of the plate thickness, linearly heating to 475 +/-3 ℃ at 20 ℃/h after the heat preservation is finished, and keeping the temperature for minutes which are 1.5 times of the plate thickness plus 60 min;
2) after the heat preservation is finished, quenching with room temperature water within 15s, and finishing the pre-stretching within 30min after the quenching is finished, wherein the pre-stretching amount is 1-3%;
3) immediately putting the pre-stretched material into a deep cooling furnace for heat preservation at the temperature of minus 100 +/-10 ℃ for 60 min;
4) and (3) after the heat preservation is finished, carrying out non-isothermal aging treatment: putting the sample obtained in the step 3) into a heat treatment furnace at 90 +/-5 ℃, linearly heating to 120 +/-5 ℃ at the speed of 5 ℃/h, and then carrying out heat preservation for 24 h; after the heat preservation is finished, linearly heating to 185 +/-5 ℃ at the speed of 240 ℃/h, and then preserving the heat for 60 min; carrying out quenching treatment at room temperature after heat preservation; putting the quenched sample into a heat treatment furnace at the temperature of 130 +/-5 ℃, linearly cooling to 120 +/-5 ℃ at the speed of 5 ℃/h, and then carrying out heat preservation for 16 h; taking out of the furnace and air cooling after the heat preservation is finished; the method is suitable for the high-alloying 7000 series aluminum alloy with Zn being more than or equal to 8 percent.
10. A method of making a 7000 series aluminum alloy plate, the method comprising the steps of:
(a) subjecting 7000 series aluminum alloy cast ingots to homogenization treatment and hot rolling treatment in sequence to obtain a test material;
(b) subjecting the sample obtained in step (a) to non-isothermal heat treatment by the non-isothermal heat treatment method for 7000-series aluminum alloy according to any one of claims 1 to 9 to obtain the 7000-series aluminum alloy plate.
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