CN116463565A - Pre-strain cryogenic aging method for improving comprehensive performance of aluminum-lithium alloy - Google Patents

Pre-strain cryogenic aging method for improving comprehensive performance of aluminum-lithium alloy Download PDF

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CN116463565A
CN116463565A CN202310292808.0A CN202310292808A CN116463565A CN 116463565 A CN116463565 A CN 116463565A CN 202310292808 A CN202310292808 A CN 202310292808A CN 116463565 A CN116463565 A CN 116463565A
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aluminum
lithium alloy
cryogenic
aging
alloy
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CN116463565B (en
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陈俊锋
邱宇潇
刘严
池海涛
陈玉龙
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Fujian Xiangxin Light Alloy Manufacturing Co ltd
Fuzhou University
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Fujian Xiangxin Light Alloy Manufacturing Co ltd
Fuzhou University
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/04Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/002Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working by rapid cooling or quenching; cooling agents used therefor
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

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  • Crystallography & Structural Chemistry (AREA)
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  • Mechanical Engineering (AREA)
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  • Organic Chemistry (AREA)
  • Testing Resistance To Weather, Investigating Materials By Mechanical Methods (AREA)
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Abstract

The invention discloses a pre-strain cryogenic aging method for improving comprehensive performance of aluminum lithium alloy, which comprises the steps of firstly carrying out 0-6% of pre-strain treatment on the aluminum lithium alloy, then putting the aluminum lithium alloy into liquid nitrogen for cryogenic treatment, immediately putting a sample subjected to cryogenic treatment into high-temperature dimethyl silicone oil for heat preservation, cooling the sample to room temperature in an air cooling mode, and finally carrying out aging treatment. The method can effectively improve the mechanical property and corrosion resistance of the aluminum alloy, and has the advantages of simple process flow, low operation difficulty, low cost and good popularization.

Description

Pre-strain cryogenic aging method for improving comprehensive performance of aluminum-lithium alloy
Technical Field
The invention belongs to the technical field of aluminum lithium alloy material processing, and particularly relates to a pre-strain cryogenic aging method for improving the comprehensive performance of an aluminum lithium alloy.
Background
The increasing growth of energy and environmental crisis has prompted the development of structural lightweight, while lightweight high-strength structural materials are a constant theme in the aerospace field. The novel aluminum-lithium alloy has the advantages of low density, high specific strength, high elastic modulus and the like, and becomes a material with high strength, low carbon and wide application prospect. However, because the aluminum-lithium alloy is generally listed as the important development direction of aerospace structural materials, the service environment is complex and is easily influenced by stress, temperature, weather, corrosive media, scouring action, heterostructures and the like, and therefore, a plurality of key aluminum alloy components have high requirements on indexes such as toughness, corrosion resistance and the like besides high strength.
Traditional isothermal aging technology is limited to aluminum alloy simple aging strengthening, and fine regulation and control on microstructure such as aluminum alloy grain characteristics, precipitated phase scale and distribution are far from sufficient. Meanwhile, a great deal of researches show that the strength and the corrosion resistance of the aluminum alloy are contradictory, and the corrosion performance of the aluminum lithium alloy is often reduced by improving the strength of the aluminum lithium alloy, so that the requirement of high comprehensive performance of the aluminum lithium alloy plate in the future is difficult to meet by the traditional aging process. At present, most researches mainly focus on the aging process, and aluminum-lithium alloy performance is improved by optimizing the aging process.
In aluminum-lithium alloy, due to the fact that precipitates with different types and different sizes are separated out in the whole aging process, the types, the sizes and the distribution of the precipitates have important influences on the mechanical property and the corrosion property of the alloy. However, because the controllable parameters in the aging process of the aluminum-lithium alloy are smaller, the improvement of the strength of the aluminum alloy only through an aging process is very limited, and a learner obtains a fine-grain material through a few unusual methods such as severe plastic deformation (equal channel extrusion, high-pressure torsion and the like), so that the great improvement of the strength of the aluminum-lithium alloy is realized. However, the method requires the aluminum alloy to generate huge deformation, has large technical difficulty, is difficult to manufacture large-size products, has large gap from the processing capacity of the existing industrial production equipment, has high processing cost and is difficult to popularize and apply. Therefore, it is very significant to find a method which can not only improve the comprehensive performance of the aluminum-lithium alloy, but also adapt to the use of modern industrial equipment and reduce the production cost.
Prestrain is a commonly used and technically mature work hardening process for aluminum alloys. However, after stretching, the high strength necessarily sacrifices the plasticity of the alloy due to the presence of work hardening, and the elongated grains also impair the spalling corrosion resistance of the alloy, which is intolerable in production practice. In addition, the tensile deformation is too large, the shaping of the alloy is obviously reduced, the processing is troublesome, and the deformation is too small and enough deformation energy storage is not obtained to promote precipitation. The aging temperature has an important influence on the microstructure after aging, and when the aging temperature is too high, coarse T is obtained 1 Phase, and T 1 The phase density is also reduced and this microstructure is detrimental to the mechanical properties. Therefore, in order to improve the alloy comprehensive properties, further regulation of the dislocation and the type, size and distribution of the precipitates is necessary through regulation of the temperature and deformation amount in the strain aging process.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide a pre-strain cryogenic aging process for improving the comprehensive performance of aluminum-lithium alloy, which can better regulate and control the sizes and distribution of precipitated phases on an aluminum alloy matrix and a grain boundary, and particularly enable solute atoms to be fully dissolved into a crystal lattice to form a supersaturated solid solution, thereby effectively improving the strength and corrosion resistance of the aluminum alloy, and is simple and easy to operate.
In order to achieve the above purpose, the invention adopts the following technical scheme:
a pre-strain cryogenic aging method for improving comprehensive performance of aluminum-lithium alloy comprises the following steps:
1) Prestrain: pre-strain treatment is carried out on the aluminum-lithium alloy at a stretching rate of 1 mm/min, so that the pre-deformation amount is 0-6%;
2) Cryogenic cooling: placing the aluminum lithium alloy treated in the step 1) into liquid nitrogen at the temperature of-197 ℃ for heat preservation treatment for 1h to 2h h;
3) And (3) up-slope quenching: rapidly placing the aluminum-lithium alloy treated in the step 2) into dimethyl silicone oil at 140 ℃ for heat preservation treatment for 5 min;
4) Air cooling: cooling the aluminum-lithium alloy material quenched in the step 3) in an air cooling mode;
5) Aging: and (3) aging the aluminum-lithium alloy subjected to air cooling in the step (4) at 160-170 ℃ and 36-48 h).
The aluminum lithium aluminum alloy comprises 2A97 aluminum alloy.
The invention firstly carries out pre-strain treatment on the aluminum lithium alloy to generate obvious influence on nucleation and growth of a precipitated phase in the aluminum alloy, and introduces a part of dislocation with high density; then placing the material subjected to the pre-strain treatment into liquid nitrogen for heat preservation, and then immediately placing the material into dimethyl silicone oil at 140 ℃ for heating, so that the surface temperature is rapidly increased to generate expansion, the alloy is in a low-temperature state, and the internal stress generated in a sample and the residual stress existing in the alloy are combined under the action of the existence of temperature difference to cause the alloy to generate micro plastic deformation, so that a large number of dislocation loops or dislocation cells are generated, and the alloy is internally provided with dislocation with high density and uniform distribution; and after primary ascending quenching, the material is subjected to aging treatment, so that second phase particles are precipitated, a strengthening phase with a larger strengthening effect is formed, and the aluminum alloy is strengthened.
In the process, the pre-strain, the deep cooling and the ascending slope quenching are key steps. First, the aluminum alloy has a higher stacking fault energy, and after tensile deformation at room temperature, more dislocations and higher distortion energy are obtained, and a large number of dislocations and high distortion energy are expected during subsequent processing of the aluminum lithium alloy. Because the high-density dislocation formed after stretching has a strong driving effect on the precipitation of second phase particles of the material, and the material after pre-strain treatment is placed into liquid nitrogen for deep cooling treatment and heat preservation, the formed supersaturated solid solution state is immediately placed into dimethyl silicone oil at 140 ℃ for heating, so that the surface temperature is rapidly increased and expansion occurs, the alloy is still in a low-temperature state, and the internal stress generated in a sample and the residual stress existing in the alloy are combined due to the existence of temperature difference, so that the alloy is subjected to micro-plasticThe alloy is deformed to generate a large number of dislocation loops or dislocation cells, so that the alloy has high density and uniform dislocation distribution, and the second phase particles T are subjected to aging treatment 1 The phase nucleation sites are more, a large amount of phase are separated out, the phase density is increased, the size is reduced, and then dispersed T is obtained 1 Phase, which is the ideal microstructure characteristics for alloy strength, plasticity and corrosion resistance, can give aluminum alloys with very high strength and plasticity. Therefore, the invention adopts the treatment methods of pre-strain, ascending quenching and aging, so that the aluminum alloy can obtain excellent mechanical properties. After detection, the yield strength of the treated aluminum alloy can reach 573.7MPa, the tensile strength can reach 593.6MPa, the elongation at break still has 11.25%, the corrosion resistance of the aluminum alloy is improved on the basis of ensuring the mechanical strength, and the advantages of the aluminum alloy can be fully exerted.
The aluminum-lithium alloy treated by the method has ideal precipitated structure morphology, content and distribution, not only can the comprehensive mechanical properties including strength and corrosion resistance be improved, but also the process flow is simple, the operation difficulty is low, the related treatment can be carried out by common industrial production equipment, the processing cost is low, and the popularization is good.
Drawings
FIG. 1 is a flow chart of the pre-strained cryogenic process of the present invention.
FIG. 2 is an SEM image of a fracture of a 2A97 aluminum alloy obtained by the process of example 1.
FIG. 3 is a graph showing room temperature stretch profiles of aluminum alloy samples obtained by the example and comparative example treatments.
FIG. 4 is a graph showing polarization curves of aluminum alloy samples obtained by the treatment of examples and comparative examples.
FIG. 5 is a graph showing the surface topography of samples of the aluminum alloys treated in the examples and comparative examples after electrochemical corrosion testing in a 3.5wt% neutral NaCl solution.
Detailed Description
In order to make the contents of the present invention more easily understood, the technical scheme of the present invention will be further described with reference to the specific embodiments, but the present invention is not limited thereto.
Example 1
A preparation process of a 2A97 aluminum alloy with good comprehensive performance comprises the following steps:
1) Prestrain: pre-strain treatment is carried out on the aluminum alloy at a stretching rate of 1 mm/min, so that the pre-deformation amount is 2%;
2) Cryogenic cooling: placing the aluminum alloy treated in the step 1) into liquid nitrogen at the temperature of-197 ℃ for heat preservation for 2 h;
3) And (3) up-slope quenching: rapidly placing the aluminum alloy treated in the step 2) into dimethyl silicone oil at 140 ℃ for preserving heat for 5 min;
4) Air cooling: cooling the aluminum alloy quenched in the step 3) in an air cooling mode;
5) Aging: and (3) aging the aluminum alloy subjected to air cooling in the step (4) at 160 ℃ and 48 and h.
Example 2
A preparation process of a 2A97 aluminum alloy with good comprehensive performance comprises the following steps:
1) Prestrain: pre-strain treatment is carried out on the aluminum alloy at a stretching rate of 1 mm/min, so that the pre-deformation amount is 4%;
2) Cryogenic cooling: placing the aluminum alloy treated in the step 1) into liquid nitrogen at the temperature of-197 ℃ for heat preservation for 2 h;
3) And (3) up-slope quenching: rapidly placing the aluminum alloy treated in the step 2) into dimethyl silicone oil at 140 ℃ for preserving heat for 5 min;
4) Air cooling: cooling the aluminum alloy quenched in the step 3) in an air cooling mode;
5) Aging: and (3) aging the aluminum alloy subjected to air cooling in the step (4) at 160 ℃ and 48 and h.
Comparative example 1
The 2A97 aluminum alloy is subjected to a traditional two-stage aging process, namely, firstly, aging treatment is carried out at 115 ℃ for 12 hours, then water cooling is carried out to room temperature, then aging treatment is carried out at 165 ℃ for 24 hours, then cooling is carried out to room temperature, and the aluminum alloy is immediately put into a refrigerator for storage.
Comparative example 2
The 2A97 aluminum alloy is subjected to a traditional two-stage aging process, namely, firstly, aging treatment is carried out at 115 ℃ for 24 hours, then water cooling is carried out to room temperature, then aging treatment is carried out at 165 ℃ for 24 hours, then cooling is carried out to room temperature, and the aluminum alloy is immediately put into a refrigerator for storage.
Comparative example 3
The 2A97 aluminum alloy is subjected to a traditional two-stage aging process, namely, firstly, aging treatment is carried out at 115 ℃ for 48 hours, then water cooling is carried out to room temperature, then aging treatment is carried out at 165 ℃ for 24 hours, then cooling is carried out to room temperature, and the aluminum alloy is immediately put into a refrigerator for storage.
The aluminum alloy samples obtained in the examples and the comparative examples were subjected to mechanical property test, room temperature tensile test, dynamic polarization test and soaking test under simulated seawater corrosion conditions by using the method of GB/T288.1-2010, and the results are shown in Table 1 and FIGS. 3-5, respectively.
Table 1 table comparing mechanical properties of aluminum alloy samples obtained by different processes with those of complicated multistage strain aging samples
Table 1 is a table comparing the mechanical properties of the inventive subzero aged samples with those of complex multi-stage deformation aged samples. As can be seen from the table, the yield strength and the tensile strength of the aluminum alloy samples obtained in the examples are higher than those of the complex multistage deformation aging samples, and the elongation is improved.
FIG. 3 is a drawing curve at room temperature of aluminum alloy samples obtained by the treatment of examples and comparative examples. As can be seen from the graph, the yield strength and the tensile strength of the aluminum alloy samples obtained in the examples are higher than those of the comparative examples, and the elongation is not quite different. The aluminum alloy obtained in the embodiment 2 has the best comprehensive mechanical properties of room-temperature stretching, the yield strength of the aluminum alloy can reach 573.7MPa, the breaking strength of the aluminum alloy can reach 593.6MPa, and the breaking elongation of the aluminum alloy is 14.3%.
FIG. 4 is a graph of polarization curves of samples of aluminum alloys obtained from the comparative and example treatments (the polarization curves were fitted to more clearly compare the corrosion behavior of the alloys at different pre-deformations). Generally, the lower the corrosion potential, the higher the corrosion current density and the poorer the corrosion resistance of the corresponding alloy. As is clear from fig. 4, the corrosion potential of the test sample treated by the process of the present invention is significantly improved, which indicates that the introduction of the pre-strain can effectively improve the corrosion resistance of the alloy, and the corrosion resistance thereof is enhanced with the increase of the pre-strain, thereby indicating that the present invention can effectively improve the stress corrosion resistance of the aluminum alloy compared with the conventional process.
FIG. 5 is a graph showing the surface topography of the aluminum alloy samples obtained in the examples and comparative examples after electrochemical corrosion testing in a 3.5% wt% neutral NaCl solution. As can be seen from fig. 5, as the degree of pre-strain increases, the degree of corrosion damage of the aluminum alloy sample also decreases, the corrosion profiles of the alloy pre-deformation amounts of 2% and 4% are almost the same, a plurality of corrosion pits with relatively small sizes are formed, the distribution of the corrosion pits is relatively dispersed, the corrosion degree of the sample is relatively light, the corrosion resistance is good, and the sample is superior to the peak aging sample of the conventional aging treatment (the soaking corrosion grade of the sample of the conventional aging treatment is EC grade, and the soaking corrosion grade of the sample of the example treatment is EA grade).
Comprehensive test results prove that the mechanical property and corrosion resistance of the aluminum lithium alloy treated by adopting the pre-strain deep cooling aging (pre-strain + deep cooling + ascending quenching) are obviously better than those of the aluminum lithium alloy treated by the traditional secondary aging treatment, and the aluminum lithium alloy is an ideal treatment method.
Although only the aluminum-lithium alloy with the mark of 2A97 is selected for testing, the strengthening form, the precipitation type and the precipitation rule of the aluminum-lithium alloy are basically consistent. Therefore, the invention can be applied to aluminum-lithium alloys of other brands by properly adjusting the technological parameters of the thermomechanical treatment within the technological parameter range disclosed by the invention.

Claims (6)

1. A pre-strain cryogenic aging method for improving comprehensive performance of aluminum-lithium alloy is characterized by comprising the following steps of: the method comprises the following steps:
1) Prestrain: pre-strain treatment is carried out on the aluminum lithium alloy;
2) Cryogenic cooling: placing the aluminum-lithium alloy treated in the step 1) into liquid nitrogen for heat preservation treatment;
3) And (3) up-slope quenching: rapidly placing the aluminum-lithium alloy treated in the step 2) into a high-temperature solution for heat preservation treatment;
4) Air cooling: cooling the aluminum-lithium alloy quenched in the step 3) in an air cooling mode;
5) Aging: and (3) aging the aluminum-lithium alloy subjected to air cooling in the step (4).
2. The pre-strained cryogenic aging method for improving the comprehensive performance of aluminum-lithium alloy according to claim 1, which is characterized in that: the aluminum lithium aluminum alloy comprises 2A97 aluminum alloy.
3. The pre-strained cryogenic aging method for improving the comprehensive performance of aluminum-lithium alloy according to claim 1, which is characterized in that: the stretching rate of the pre-strain treatment in the step 1) is 1 mm/min, and the pre-deformation amount is 0-6%.
4. The pre-strained cryogenic aging method for improving the comprehensive performance of aluminum-lithium alloy according to claim 1, which is characterized in that: the temperature of the liquid nitrogen in the step 2) is-197 ℃; the heat preservation treatment time is 1h-2h.
5. The pre-strained cryogenic aging method for improving the comprehensive performance of aluminum-lithium alloy according to claim 1, which is characterized in that: step 3) the high-temperature solution is simethicone, and the temperature of the simethicone is 140 ℃; the heat preservation treatment time is 5min.
6. The pre-strained cryogenic aging method for improving the comprehensive performance of aluminum-lithium alloy according to claim 1, which is characterized in that: the temperature of the aging treatment in the step 4) is 160-170 ℃ and the time is 36-48 h.
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