DSC and TEM Investigation of Precipitation Behavior in a Cold-Rolled Pre-Aged Al-Mg-Si-Cu Alloy
Abstract
1. Introduction
2. Materials and Experimental Methods
3. Results and Discussion
3.1. Hardness Evolution as a Function of Aging Time and Deformation Levels
3.2. Analysis of Precipitation Kinetics and Phase Transformation Using DSC
3.3. TEM Characterization of Microstructure and Precipitate Evolution
4. Conclusions
- -
- Hardness measurements show that increasing cold-rolling reduction significantly improves both the peak hardness and the aging kinetics. The undeformed sample exhibits a peak hardness of approximately 100 HV (increased from ~78 HV after pre-aging), whereas the 30%, 60%, and 80% cold-rolled samples reach peak hardness values of about 120 HV, 131 HV, and 142 HV, respectively. In addition, the time to reach peak hardness is greatly reduced, with the 80% cold-rolled sample reaching peak hardness within ~6 h, compared to ~1 week for the undeformed condition.
- -
- DSC analysis indicates that all precipitation peaks shift toward lower temperatures with increasing deformation. This is accompanied by a reduction in activation energy and a decrease in the full width at half-maximum of the main precipitation peak, demonstrating that cold rolling accelerates precipitation kinetics and lowers the energy barrier for phase transformation.
- -
- TEM observations reveal that cold rolling introduces a high density of dislocations, which act as preferential nucleation sites for precipitates. Consequently, precipitates increasingly form along dislocations, resulting in a higher number density and finer size distribution with increasing deformation.
Author Contributions
Funding
Data Availability Statement
Acknowledgments
Conflicts of Interest
References
- Miller, W.S.; Zhuang, L.; Bottema, J.; Wittebrood, A.; De Smet, P.; Haszler, A.; Vieregge, A.J. Recent development in aluminium alloys for the automotive industry. Mater. Sci. Eng. A 2000, 280, 37–49. [Google Scholar] [CrossRef] [Scilit]
- Sabirov, I.; Murashkin, M.Y.; Valiev, R.Z. Nanostructured aluminium alloys produced by severe plastic deformation: New horizons in development. Mater. Sci. Eng. A 2013, 560, 1–24. [Google Scholar] [CrossRef] [Scilit]
- Wang, S.H.; Liu, C.H.; Chen, J.H.; Li, X.L.; Zhu, D.H.; Tao, G.H. Hierarchical nanostructures strengthen Al–Mg–Si alloys processed by deformation and aging. Mater. Sci. Eng. A 2013, 585, 233–242. [Google Scholar] [CrossRef] [Scilit]
- Liu, C.; Ma, Z.; Ma, P.; Zhan, L.; Huang, M. Multiple precipitation reactions and formation of θ’-phase in a pre-deformed Al–Cu alloy. Mater. Sci. Eng. A 2018, 733, 28–38. [Google Scholar] [CrossRef] [Scilit]
- Jin, S.; Ngai, T.; Li, L.; Jia, S.; Zhai, T.; Ke, D. Aging response and precipitation behavior after 5% pre-deformation of an Al-Mg-Si-Cu alloy. Materials 2018, 11, 1422. [Google Scholar] [CrossRef] [Scilit]
- Cao, L.; Paul, A.R.; Malcolm, J.C. Clustering behaviour in an Al–Mg–Si–Cu alloy during natural ageing and subsequent under-ageing. Mater. Sci. Eng. A 2013, 559, 257–261. [Google Scholar] [CrossRef] [Scilit]
- Ren, J.; Chen, Z.; Peng, J.; Ma, W.; Ringer, S.P. An initial report on achieving high comprehensive performance in an Al-Mg-Si alloy via novel thermomechanical processing. J. Alloys Compd. 2018, 764, 679–683. [Google Scholar] [CrossRef] [Scilit]
- Zheng, R.; Sun, Y.; Ameyama, K.; Ma, C. Optimizing the strength and ductility of spark plasma sintered Al 2024 alloy by conventional thermo-mechanical treatment. Mater. Sci. Eng. A 2014, 590, 147–152. [Google Scholar] [CrossRef] [Scilit]
- Lan, J.; Han, Z.; Hua, L. Effects of cold deformations on strength and ductility of extruded Al-Cu-Mg-Si alloy. Mater. Lett. 2021, 300, 130188. [Google Scholar] [CrossRef] [Scilit]
- Zhang, Z.; Yang, Y.; Gao, Y.; Wang, G.; Shi, W. Performance analysis of 7075 aluminum alloy strengthened by cavitation water jet peening at different scanning speeds. Crystals 2022, 12, 1451. [Google Scholar] [CrossRef] [Scilit]
- Koshino, Y.; Aruga, Y.; Mukai, J.; Kaneko, K. Relationship among elongation, work hardening behavior and dislocation characteristics of Al–Mg–Si series alloys. Mater. Trans. 2019, 60, 68–73. [Google Scholar] [CrossRef] [Scilit]
- Rhee, Y.; Thronsen, E.; Ryggetangen, O.; Marioara, C.D.; Holmestad, R.; Kobayashi, E. Effect of Pre-Deformation on Precipitation in Al–Zn–Mg–Cu Alloy. Met. Mater. Int. 2024, 30, 3294–3310. [Google Scholar] [CrossRef] [Scilit]
- Cui, M.; Jo, Y.H.; Kayani, S.H.; Kim, H.W.; Lee, J.H. Effects of Cu additions on the precipitation activation energy and mechanical properties of prestrained Al–Mg–Si alloys. J. Mater. Res. Technol. 2022, 20, 2629–2637. [Google Scholar] [CrossRef] [Scilit]
- Zhai, H.; Zhang, L.; Xing, S.; Hou, H.; Wang, Z.; Liu, S. The Effect of Pre-Deformation on the Microstructure and Hardness of Al-Zn-Mg-Cu Alloy. Coatings 2025, 15, 283. [Google Scholar] [CrossRef] [Scilit]
- Gleiter, H.; Hansen, N.; Horsewell, A.; Leffers, T.; Lilholt, H. Deformation of polycrystals: Mechanisms and microstructures. In Proceedings of the 2nd RISO Symposium on Metallurgy and Materials Science, Roskilde, Denmark, 14–18 September 1981; pp. 15–21. [Google Scholar]
- Gazizov, M.; Marioara, C.D.; Friis, J.; Wenner, S.; Holmestad, R.; Kaibyshev, R. Unique hybrid precipitate structures forming in an Al–Cu–Mg–Si alloy. J. Alloys Compd. 2020, 826, 153977. [Google Scholar] [CrossRef] [Scilit]
- Vu, N.H.; Lee, S.; Tsuchiya, T.; Katsumi, T.; Kita, K.; Matsuda, K. Effect of pre-aging temperature on hardening behavior and precipitation response of deformed Al–1.0% Cu–0.96% Mg–0.36% Si (wt.%) alloy. Arch. Metall. Mater. 2025, 70, 1287–1293. [Google Scholar] [CrossRef] [Scilit]
- He, L.; Zhang, H.; Cui, J. Effects of pre-ageing treatment on sub- sequent artificial ageing characteristics of an Al-1.01Mg-0.68Si-1.78Cu alloy. J. Mater. Sci. Technol. 2010, 26, 141–145. [Google Scholar] [CrossRef] [Scilit]
- Kirekawa, N.; Saito, K.; O, M.; Kobayashi, E. Effect of Cold Rolling on Cluster(1) Dissolvability during Artificial Aging and Formability during Natural Aging in Al-0.6Mg-1.0Si-0.5Cu Alloy. Metals 2022, 12, 92. [Google Scholar] [CrossRef] [Scilit]
- Xie, Y.; Liu, S.; Guo, X.; He, X.; Liang, C.; Deng, Y. Modulation of precipitation behavior by dislocations and alloying for superior strength-ductility balance in Al-Cu-Li alloys. J. Alloys Compd. 2025, 1010, 177334. [Google Scholar] [CrossRef] [Scilit]
- Ringer, S.P.; Caraher, S.K.; Polmear, I.J. Response to comments on cluster hardening in an aged Al-Cu-Mg alloy. Scr. Mater. 1998, 39, 1559–1567. [Google Scholar] [CrossRef] [Scilit]
- Esin, V.A.; Briez, L.; Sennour, M.; Köster, A.; Gratiot, E.; Crépin, J. Precipitation-hardness map for Al–Cu–Mg alloy (AA2024-T3). J. Alloys Compd. 2021, 854, 157164. [Google Scholar] [CrossRef] [Scilit]
- Abis, S. Characteristics of an aluminium alloy/Alumina Metal Matrix composite. Compos. Sci. Technol. 1989, 35, 1–11. [Google Scholar] [CrossRef] [Scilit]
- Riontino, G.; Abis, S.; Bottero, C. A DSC Study of Precipitation in Al-Cu-Mg Alloys. Alum. Alloys 1998, 2, 903–908. [Google Scholar]
- Jena, A.K.; Gupta, A.K.; Chaturvedi, M.C. A differential scanning calorimetric investigation of precipitation kinetics in the Al-1.53 wt% Cu-0.79 wt% Mg alloy. Acta Metall. 1989, 37, 885–895. [Google Scholar] [CrossRef] [Scilit]
- Kissinger, H.E. Reaction Kinetics in Differential Thermal Analysis. Anal. Chem. 1957, 29, 1702–1706. [Google Scholar] [CrossRef] [Scilit]
- Zhang, X. Applications of kinetic methods in thermal analysis: A review. Eng. Sci. 2020, 14, 1–3. [Google Scholar] [CrossRef] [Scilit]
- Wendlandt, W.W. Thermal Methods of Analysis, 3rd ed.; Wiley: New York, NY, USA, 1986. [Google Scholar]
- Zheng, K.; Li, Y.; Yang, S.; Fu, K.; Zheng, J.; He, Z.; Yuan, S. Investigation and modeling of the preheating effects on precipitation and hot flow behavior for forming high strength AA7075 at elevated temperatures. J. Manuf. Mater. Process. 2020, 4, 76. [Google Scholar] [CrossRef] [Scilit]
- Irmer, D.; Moussa, C.; Belkacemi, L.T.; Sennour, M.; Vaissière, A.; Esin, V.A. Effect of cold rolling on nucleation, growth and coarsening of S-phase precipitates in Al-Cu-Mg alloy (AA2024): From heterogeneous nucleation to homogeneous spatial distribution. J. Alloys Compd. 2023, 963, 171162. [Google Scholar] [CrossRef] [Scilit]
- Matsuda, K.; Kawai, A.; Watanabe, K.; Lee, S.; Marioara, C.D.; Wenner, S.; Nishimure, K.; Matsuzaki, T.; Nunomura, N.; Sato, T.; et al. Extra electron diffraction spots caused by fine precipitates formed at the early stage of aging in Al-Mg-X (X = Si, Ge, Zn)-Cu alloys. Mater. Trans. 2017, 58, 167–175. [Google Scholar] [CrossRef] [Scilit]
- Hai, V.N.; Ahmed, A.; Lee, S.; Tsuchiya, T.; Zou, Y.; Katsumi, T.; Kita, K.; Khanh, P.M.; Holmestad, R.; Marioara, C.D.; et al. A comparative investigation of microstructure and mechanical properties in a deformed and aged Al-Mg-Si alloy with high Cu content. Mater. Des. 2025, 260, 115172. [Google Scholar] [CrossRef] [Scilit]
- Gazizov, M.; Marioara, C.D.; Friis, J.; Wenner, S.; Holmestad, R.; Kaibyshev, R. Precipitation behavior in an Al–Cu–Mg–Si alloy during ageing. Mater. Sci. Eng. A 2019, 767, 138369. [Google Scholar] [CrossRef] [Scilit]
- Niu, F.J.; Chen, J.H.; Duan, S.Y.; Ming, W.Q.; Lu, J.B.; Wu, C.L.; Le, Z. The effect of pre-deformation on the precipitation behavior of AlCuMg (Si) alloys with low Cu/Mg ratios. J. Alloys Compd. 2020, 823, 153831. [Google Scholar] [CrossRef] [Scilit]
- Weng, Y.Y.; Jia, Z.H.; Ding, L.P.; Liao, J.; Zhang, P.P.; Xu, Y.Q.; Liu, Q. Effect of pre-straining on structure and formation mechanism of precipitates in Al–Mg–Si–Cu alloy. Trans. Nonferr. Met. Soc. China 2022, 32, 447. [Google Scholar] [CrossRef] [Scilit]
- Yuan, Z.; Lu, C.; Ding, L.; Xiang, K.; Weng, Y.; Liu, Q.; Jia, Z. The interactive effect of alloy composition and pre-straining on the precipitation behavior of Al–Mg–Si–Cu alloys. Mater. Sci. Eng. A 2022, 849, 143495. [Google Scholar] [CrossRef] [Scilit]
- Ding, L.; Yang, Y.; Zheng, Y.; Yin, T.; Huang, H.; Weng, Y. Effect of Pre-Deformation on Microstructure and Mechanical Properties of a Mg-Rich High-Cu Al-Mg-Si-Cu Alloy. Metals 2026, 16, 366. [Google Scholar] [CrossRef] [Scilit]
- Shao, D.; Zhang, P.; Zhang, J.Y.; Liu, G.; Wang, R.H.; Liu, W.Q.; Sha, G.; Sun, J. Effect of pre-strain on the solute clustering, mechanical properties, and work-hardening of a naturally aged Al-Cu-Mg alloy. Metall. Mater. Trans. A 2017, 48, 4121–4134. [Google Scholar] [CrossRef] [Scilit]
- Marioara, C.D.; Andersen, S.J.; Stene, T.N.; Hasting, H.; Walmsley, J.; Van Helvoort, A.T.J.; Holmestad, R. The effect of Cu on precipitation in Al–Mg–Si alloys. Philos. Mag. 2007, 87, 3385–3413. [Google Scholar] [CrossRef] [Scilit]
- Torsæter, M.; Ehlers, F.J.H.; Marioara, C.D.; Andersen, S.J.; Holmestad, R. Applying precipitate–host lattice coherency for compositional determination of precipitates in Al–Mg–Si–Cu alloys. Philos. Mag. 2012, 92, 3833–3856. [Google Scholar] [CrossRef] [Scilit]
- Thronsen, E.; Marioara, C.D.; Sunde, J.K.; Minakuchi, K.; Katsumi, T.; Erga, I.; Matsuda, K.; Holmestad, R. The effect of heavy deformation on the precipitation in an Al-1.3 Cu-1.0 Mg-0.4 Si wt.% alloy. Mater. Des. 2020, 186, 108203. [Google Scholar] [CrossRef] [Scilit]
- Weng, Y.; Li, R.; Zheng, L.; Zhao, R.; Zhou, Y.; Chen, J.; Ding, L. Effects of pre-deformation on microstructure evolution and hemming performance for Al-Mg-Si-Cu alloys. J. Mater. Res. Technol. 2025, 35, 2840–2851. [Google Scholar] [CrossRef] [Scilit]
- Wang, X.; Pan, Q.; Wang, W.; Huang, Z.; Chen, J.; Pan, B.; Liu, X. Effects of pre-strain and aging treatments on the mechanical property and corrosion resistance of the spray formed ultra-high strength Al-Zn-Mg-Cu alloy. Mater. Charact. 2022, 194, 112381. [Google Scholar] [CrossRef] [Scilit]











| Conditions | Heat Treatment |
|---|---|
| 0% CR | SHT + Pre-aging 35 °C + cold-rolling 0% + final aging 160 °C |
| 30% CR | SHT + Pre-aging 35 °C + cold-rolling 30% + final aging 160 °C |
| 60% CR | SHT + Pre-aging 35 °C + cold-rolling 60% + final aging 160 °C |
| 80% CR | SHT + Pre-aging 35 °C + cold-rolling 80% + final aging 160 °C |
| Peak | Condition | |||
|---|---|---|---|---|
| 0% CR | 30% CR | 60% CR | 80% CR | |
| A | 96.5 | 67.5 | 62.55 | 60.1 |
| B | 181.3 | 170.2 | 168.10 | 170.4 |
| C | 250.2 | 233.87 | 220.15 | 218.3 |
| D | 312.0 | 305.85 | 277.5 | 270.1 |
| E | 330.4 | 340.45 | 319.15 | 311.1 |
| F | 382.4 | 382.4 | 365.21 | 350.4 |
| G | 448.5 | 435.1 | 435.1 | 434.1 |
Disclaimer/Publisher’s Note: The statements, opinions and data contained in all publications are solely those of the individual author(s) and contributor(s) and not of MDPI and/or the editor(s). MDPI and/or the editor(s) disclaim responsibility for any injury to people or property resulting from any ideas, methods, instructions or products referred to in the content. |
© 2026 by the authors. Licensee MDPI, Basel, Switzerland. This article is an open access article distributed under the terms and conditions of the Creative Commons Attribution (CC BY) license.
Share and Cite
Hai, V.N.; Lee, S.; Tsuchiya, T.; Katsumi, T.; Kita, K.; Matsuda, K. DSC and TEM Investigation of Precipitation Behavior in a Cold-Rolled Pre-Aged Al-Mg-Si-Cu Alloy. J. Manuf. Mater. Process. 2026, 10, 167. https://doi.org/10.3390/jmmp10050167
Hai VN, Lee S, Tsuchiya T, Katsumi T, Kita K, Matsuda K. DSC and TEM Investigation of Precipitation Behavior in a Cold-Rolled Pre-Aged Al-Mg-Si-Cu Alloy. Journal of Manufacturing and Materials Processing. 2026; 10(5):167. https://doi.org/10.3390/jmmp10050167
Chicago/Turabian StyleHai, Vu Ngoc, Seungwon Lee, Taiki Tsuchiya, Tetsuya Katsumi, Kazuhiko Kita, and Kenji Matsuda. 2026. "DSC and TEM Investigation of Precipitation Behavior in a Cold-Rolled Pre-Aged Al-Mg-Si-Cu Alloy" Journal of Manufacturing and Materials Processing 10, no. 5: 167. https://doi.org/10.3390/jmmp10050167
APA StyleHai, V. N., Lee, S., Tsuchiya, T., Katsumi, T., Kita, K., & Matsuda, K. (2026). DSC and TEM Investigation of Precipitation Behavior in a Cold-Rolled Pre-Aged Al-Mg-Si-Cu Alloy. Journal of Manufacturing and Materials Processing, 10(5), 167. https://doi.org/10.3390/jmmp10050167
