Amelioration of Mechanical Properties of Rolled Mg-4.5Al-2.5Zn Alloy by Cryogenic Cycling Treatment

doi:10.1007/s40195-025-01871-9

Abstract

Abstract:

In this study, cryogenic cycling treatment was used to process the hot-rolled Mg-4.5Al-2.5Zn alloy sheets to research the influence on mechanical properties and microstructure. Optical microscopy, electron back-scatter diffraction and transmission electron microscopy were applied to characterize the microstructures and analyze the mechanisms. The consequences indicate that the cryogenic cycling treatment has significantly influence on improving the mechanical properties. With the cycle of cryogenic cycling treatment increasing to 5 cycles, the sample processed by 3 cycles presents the highest ductility (~ 18.6%), while the 4-cycle one shows the highest strength (~ 311.8 MPa). The improvement can be attributed to fine grains, introduced high-density dislocation, 9.8%-fraction low-angle grain boundaries (LAGBs), the precipitation of Mg₁₇Al₁₂ phase and the texture with the intensity of 17.5. Although the average grain sizes of the samples processed by cryogenic cycling treatment have no obvious difference, internal stress variations induced by cryogenic cycling treatment significantly influence LAGBs, the basal texture evolution, and the prismatic < a > slip, pyramidal < c > slip and pyramidal < c + a > slip activation.

Key words: Mg-4.5Al-2.5Zn alloy, Cryogenic cycling treatment, Microstructure, Mechanical properties

Haoran Pang, Liwei Lu, Gongji Yang, Xiaojun Wang, Wen Wang, Hua Zhang, Yujuan Wu. Amelioration of Mechanical Properties of Rolled Mg-4.5Al-2.5Zn Alloy by Cryogenic Cycling Treatment[J]. Acta Metallurgica Sinica (English Letters), 2025, 38(8): 1436-1452.

Figures/Tables 17

Fig. 1 Schematic diagram of experimental process

Fig. 2 Engineering stress-strain curves of the Mg-4.5Al-2.5Zn alloy samples

Table 1 Data of tensile mechanical property of Mg-4.5Al-2.5Zn alloy at different states

Samples	UTS (MPa)	EL (%)
Initial sample	278.5	15.8
1-cycle	303	15.7
2-cycle	311	15
3-cycle	302	18.6
4-cycle	311.8	17.8
5-cycle	306	15.7
AC	296.7	14

Fig. 3 Optical microstructures of the samples treated by various processes: a initial sample, b 1-cycle, c 2-cycle, d 3-cycle, e 4-cycle, f 5-cycle, g AC

Fig. 4 EBSD maps and grain size distributions of Mg-4.5Al-2.5Zn alloy samples: a, b AC, c, d 4-cycle, e, f 5-cycle

Fig. 5 Typical grain G selected in Fig. 4a: a IPF map, b KAM map, c the corresponding KAM relative frequency and average KAM value, d (0001) pole figure, e inverse pole figures along the ND, f SF distribution map, g SF distribution map of S1, h SF distribution map of S2, i SF distribution map of S3

Fig. 6 DRX behavior in the typical region R1 selected in Fig. 4c: a DRX map, b misorientation angle accumulated along the arrow AB, c misorientation angle accumulated along the arrow CD, d (0001) pole figure, e inverse pole figures along the ND

Fig. 7 Characteristic regions R2 and R3 selected in Fig. 4e: a, c IPF map, b, d KAM map, e the corresponding KAM relative frequency and average KAM values, f, g (0001) pole figure, h, i SF distribution map; a, b, f, h R2, c, d, g, i R3

Fig. 8 LAGB statistics and IGMAs figures of: a-c AC, d-f 4-cycle, and g-i 5-cycle samples

Fig. 9 Pole figures: a-c AC samples, d-f 4-cycle samples, g-i 5-cycle samples

Fig. 10 Inverse pole figures and SF distribution of the major grains of PTC1, PTC2, PTC3 and PTC4 selected in Fig. 9a, d, g: a, b PTC1, c, d PTC2, e, f PTC3, g, h PTC4

Table 2 Average SF values of PTC1, PTC2, PTC3 and PTC4

Slip system	PTC1	PTC2	PTC3	PTC4
Basal slip	0.08	0.08	0.13	0.23
Prismatic < a > slip	0.47	0.47	0.24	0.45
Pyramidal < a > slip	0.38	0.39	0.40	0.45
Pyramidal < c + a > slip	0.44	0.44	0.42	0.40

Fig. 11 SF distributions of PT1 and PT2: a PT1, b PT2

Fig. 12 TEM images of microstructure morphology and dislocations of the three samples: a, b 4-cycle, c 5-cycle, d AC

Fig. 13 TEM images of precipitations in: a 4-cycle, and b 5-cycle samples

Fig. 14 Two-beam bright-field TEM micrographs of Mg-4.5Al-2.5Zn alloy: AC a, c, e and 4-cycle b, d, f

Fig. 15 KAM maps of different samples: a 4-cycle, b 5-cycle, c AC, and d the corresponding KAM relative frequency and average KAM value

References 55

[1]	T. Wang, L. Yang, Z.F. Tang, L. Wu, H.Y. Yan, C. Liu, Y.Z. Ma, W.S. Liu, Z.J. Yu, Mater. Sci. Eng. A 844, 143042 (2022)
[2]	K. Sheng, L.W. Lu, Y. Xiang, M. Ma, Z.Q. Wu, J. Magnes. Alloy. 7, 717 (2019) DOI
[3]	X. Liu, D.D. He, B.W. Zhu, W.H. Liu, F. Ye, F.A. Wei, C.C. Xu, L.X. Li, Scr. Mater. 253, 116296 (2024)
[4]	W. Kang, L.W. Lu, L.B. Feng, F.C. Lu, C.L. Gan, X.H. Li, J. Magnes. Alloy. 11, 317 (2023)
[5]	D. Nugmanov, M. Knezevic, M. Zecevic, O. Sitdikov, M. Markushev, I.J. Beyerlein, Mater. Sci. Eng. A 713, 81 (2018)
[6]	R. Ma, Y. Lu, L. Wang, Y.N. Wang, Trans. Nonferrous Met. Soc. China 28,902 (2018)
[7]	J.R. Li, D.S. Xie, H.S. Yu, R.L. Liu, Y.Z. Shen, X.S. Zhang, C.L. Yang, L.F. Ma, H.C. Pan, G.W. Qin, J. Alloys Compd. 835, 155228 (2020)
[8]	D.H. Cho, J.H. Nam, B.W. Lee, K.M. Cho, I.M. Park, J. Alloys Compd. 676, 461 (2016)
[9]	Y.L. Xu, S. Gavras, F. Gensch, K.U. Kainer, N. Hort, JOM 72,517 (2020)
[10]	D. Pei, W. Li, T.L. Yan, X.L. Li, X. Wang, J. Alloys Compd. 929, 167224 (2022)
[11]	C.Q. Liu, H.W. Chen, C. He, Y.Y. Zhang, J.F. Nie, Mater. Charact. 113, 214 (2016)
[12]	A. Utiarahman, A.F. Alkaim, A.M. Aljeboree, S.Z. Venediktovna, C.O. Takhirovna, M. Alexander, Y. Abilmazhinov, Y. Zhu, Mater. Today Commun. 26, 101843 (2021)
[13]	H. Zheng, L. Zhu, S.S. Jiang, Y.G. Wang, F.G. Chen, J. Alloys Compd. 790, 529 (2019)
[14]	J. Jin, X.L. Ji, S. Cao, W.W. Zhu, Metall. Mater. Trans. A 53, 3404 (2022)
[15]	H.M. Zhai, Y. Du, X.Q. Li, W.S. Li, H.F. Wang, J. Mater. Sci. 56, 8276 (2021)
[16]	H.B. Kim, E.W. Jeong, D.H. Ko, B.M. Kim, Y.R. Cho, Korean. J. Mater. Res. 23, 18 (2013)
[17]	S. Hao, X.P. Guo, J.Y. Cui, P. Xue, R.Z. Xu, X.M. Guo, Mater. Sci. Eng. A 909, 146838 (2024)
[18]	H. Mirzadeh, J. Mater. Res. Technol. 25, 7050 (2023)
[19]	B. Che, L.W. Lu, J.L. Zhang, J.H. Zhang, M. Ma, L.F. Wang, F.G. Qi, Mater. Sci. Eng. A 832, 142475 (2022)
[20]	Y. Liu, S. Shao, C.S. Xu, X.S. Zeng, X.J. Yang, Mater. Sci. Eng. A 588, 76 (2013)
[21]	M.G. Jiang, C. Xu, H. Yan, G.H. Fan, T. Nakata, C.S. Lao, R.S. Chen, S. Kamado, E.H. Han, B.H. Lu, Acta Mater. 157, 53 (2018)
[22]	K. Takagi, M. Yamasaki, Y. Mine, K. Takashima, Scr. Mater. 178, 498 (2020)
[23]	Y.T. Fan, L.W. Lu, H.L. Zhao, Z.Q. Wu, Y. Xue, W. Wang, Acta Metall. Sin.-Engl. Lett. 36, 1649 (2023)
[24]	H. Yu, H. Liu, B.A. Jiang, W. Yu, S.M. Kang, W.L. Cheng, S. Park, D. Chen, F.X. Yin, K. Shin, J.Y. Mu, X.W. Cui, J.H. Li, Metals 11,838 (2021)
[25]	K. Zhang, J.H. Zheng, C. Hopper, J. Jiang, Mater. Sci. Eng. A 811, 141001 (2021)
[26]	S.B. Zhou, T.T. Liu, A.T. Tang H. Shi, X.R. Jing, P. Peng, J.Y. Zhang, F.S. Pan, Trans. Nonferrous Met. Soc. China 34,504 (2024)
[27]	N. Stanford, Mater. Sci. Eng. A 565, 469 (2013)
[28]	H.K. Zhang, H. Xiao, X.W. Fang, Q. Zhang, R.E. Loge, K. Huang, Mater. Des. 193, 108873 (2020)
[29]	J.L. Zhang, L.W. Lu, W. Kang, B. Che, M.H. Li, Y.T. Fan, M. Min, J. Plast. Eng. 29, 126 (2022)
[30]	J.B. Jia, Y. Xu, Y. Yang, C. Chen, W.C. Liu, L.X. Hu, J.T. Luo, J. Alloys Compd. 721, 347 (2017)
[31]	R. Sarvesha, W. Alam, A. Gokhale, T.S. Guruprasad, S. Bhagavath, S. Karagadde, J. Jain, S.S. Singh, Mater. Sci. Eng. A 759, 368 (2019)
[32]	Y.H. Zhao, X.Z. Liao, Y.T. Zhu, Z. Horita, T.G. Langdon, Mater. Sci. Eng. A 410-411, 188 (2005)
[33]	Q.H. Wang, B. Jiang, A.T. Tang, C. He, D.F. Zhang, J.F. Song, T.H. Yang, G.S. Huang, F.S. Pan, Mater. Sci. Eng. A 746, 259 (2019)
[34]	T.S. Zhou, Z.H. Liu, D.L. Yang, S.J. Meng, Z. Jia, D.X. Liu, J. Alloys Compd. 873, 159880 (2021)
[35]	T.S. Zhou, B. Wang, M.J. Zhang, Y.Q. Li, S.W. Hu, X.Q. Li, D.X. Liu, Mater. Sci. Eng. A 899, 146469 (2024)
[36]	H.C. Pan, R. Kang, J.R. Li, H.B. Xie, Z.R. Zeng, Q.Y. Huang, C.L. Yang, Y.P. Ren, G.W. Qin, Acta Mater. 186, 278 (2020)
[37]	X.J. Chen, W.C. Liu, G.H. Wu, H.R.J. Nodooshan, X.F. Zhang, S. Zhang, K.H. Zhou, W.J. Ding, J. Mater. Res. 31, 419 (2016)
[38]	K. Bryła, M. Krystian, J. Horky, B. Mingle, K. Mroczka, P. Kurtyka, L. Litynska-Dobrzynska, Mater. Sci. Eng. A 737, 318 (2018)
[39]	J.Y. Xiong, Z.Y. Chen, L. Yi, S.H. Hu, T. Chen, C.M. Liu, Mater. Sci. Eng. A 590, 60 (2014)
[40]	F.M. Lu, A.B. Ma, J.H. Jiang, J. Chen, D. Song, Y.C. Yuan, J.Q. Chen, D.H. Yang, J. Alloys Compd. 643, 28 (2015)
[41]	L.P. Zhong, Y.J. Wang, Y.C. Dou, J. Magnes. Alloy. 7, 637 (2019)
[42]	M. Zha, X. Ma, H.L. Jia, Z.M. Hua, Z.X. Fan, Z.Z. Yang, Y.P. Gao, H.Y. Wang, Int. J. Plast. 167, 103682 (2023)
[43]	F. Mokdad, D.L. Chen, D.Y. Li, J. Alloys Compd. 737, 549 (2018)
[44]	L. Li, C. Zhang, H. Lv, C. Liu, Z. Wen, J. Jiang, J. Magnes. Alloy. 10, 249 (2022)
[45]	S.C. Li, X. Zhao, X.D. Wang, X.M. Mu, F.F. Yan, J. Alloys Compd. 1005, 176102 (2024)
[46]	L.Y. Zhao, H. Yan, R.S. Chen, E.H. Han, Mater. Charact. 170, 110697 (2020)
[47]	S.C. Li, Z. Wang, X. Zhao, X.D. Wang, J.M. Yu, J. Mater. Res. Technol. 33, 384 (2024)
[48]	X. Liu, Q.H. Wan, B.W. Zhu, W.H. Liu, L.X. Li, C.C. Xu, P.C. Guo, J. Mater. Sci. 59, 3662 (2024)
[49]	V.M. Miller, T.M. Pollock, Metall. Mater. Trans. 47, 1854 (2016)
[50]	Y.Y. He, G. Fang, J. Alloys Compd. 901, 163745 (2022)
[51]	W. Qiu, S.L. Li, Z.Y. Lu, S.M. Zhang, J. Chen, W. Chen, L. Gan, W. Li, Y.J. Ren, J. Luo, M.H. Yao, W. Xie, Acta Metall. Sin.-Engl. Lett. 38, 287 (2025)
[52]	G. Esteban-Manzanares, A.X. Ma, I. Papadimitriou, E. Martinez, J. Llorca, Model. Simul. Mater. Sc. 27, 075003 (2019)
[53]	D.D. Zhang, M.Y. Chen, X.R. Zhang, K. Li, L.Q. Wang, Z.Y. Zhao, P.K. Bai, D.Q. Fang, Acta Metall. Sin.-Engl. Lett. 37, 1830 (2024)
[54]	U.M. Chaudry, Y. Noh, K.A. Hamad, Mater. Res. Technol. 19, 3406 (2022)
[55]	B. Che, L.W. Lu, J.L. Zhang, J. Teng, L. Chen, Y. Xu, T. Wang, L. Huang, Z.Q. Wu, J. Mater. Res. Technol. 19, 4557 (2022)