Effect of Heat Treatment on Microstructure and Mechanical Properties of Mg-Gd-Zn-Ti-xAl AlloysAbstract
The microstructure evolution and mechanical properties of Mg-12Gd-1Zn-0.6Ti-xAl alloys under different heat treatment conditions were studied. The results show that the as-cast Mg-12Gd-1Zn-0.6Ti alloy is composed of the α-Mg matrix and (Mg,Zn)3Gd phase. With the increase of Al element, Mg12Gd(Al,Zn) (18R-LPSO), Al2Gd and Al11Gd3 phases are formed in the microstructure. Following the homogenization process, the phases of (Mg,Zn)3Gd, 18R-LPSO, and a portion of Al11Gd3 undergo a transformation into the more stable Mg12Gd(Al,Zn) (14H-LPSO) phases at elevated temperatures. As the Al content increases from 0 to 0.8wt%, the proportion of 14H-LPSO phase significantly increases. The Al2Gd, 14H-LPSO, and Al11Gd3 phases exhibit excellent high-temperature stability. In the peak-aged alloy, the precipitated β′ phases can effectively suppress substrate slip and cause precipitation hardening, thereby improving strength. The Mg-12Gd-1Zn-0.6Ti-0.8Al alloy subjected to peak aging treatment exhibits a good combination of mechanical properties, with a yield strength of 187 MPa, a tensile strength of 290 MPa, and an elongation of 6.8%.
Keywords:
Mg-Gd-Zn-Ti-Al alloy; rare earth magnesium alloy; heat treatment; mechanical properties
1. Introduction
Magnesium (Mg) alloys are renowned for their low density, robust electromagnetic shielding, superior shock absorption, and high specific strength, making them a popular choice in industries such as biomedical devices, automotive, consumer electronics (3C) and aerospace1-4. However, their limited mechanical properties, especially in terms of plasticity and strength, hinder their broader application. Studies have shown that the incorporation of rare earth elements such as Y, Nd, Ce, and Gd can effectively enhance the plasticity and strength of Mg alloys5-8. Among them, Mg-Gd-Zn alloys are particularly promising, achieving a good balance between creep resistance, ductility and strength9,10. The excellent mechanical properties are attributed to the combined effect of β′ and LPSO (long-period stacking ordered) phases.
Microalloying and heat treatment are important methods to improve the strength of Mg alloys11-14. The addition of some alloying elements to Mg alloys has a large influence on the stacking fault energy. Generally, it is easier to form the LPSO phase at a lower stacking fault energy14. In particular, precipitation of the β′ phase, which is often observed in Mg alloys with a high RE content, can effectively enhance the mechanical properties13. Increasing the level of Zn leads to the formation of the LPSO phase and decreases the volume fraction of the β phase14. The high solubility of Y and Gd at elevated temperatures causes an easy dissolution of the β phase into the α-Mg matrix and the separation of the β′ phase after aging treatment15. Homma et al.15 showed that the UTS (ultimate tensile strength), YS (yield strength) and elongation of Mg-10Gd-5.7Y-1.6Zn-0.6Zr alloy after deformation and heat treatment reached 542 MPa, 473 MPa and 6%, respectively. This impressive strength is primarily attributed to the LPSO and β′ phases16. Recent studies have successfully used the E2EM model to explain why the formation of Al2RE phase has a profound grain refinement effect on Mg-RE alloys17,18. The addition of 0.6-1.0wt % Al can reduce the grain size of 180 μm in Mg-Y alloy to 36 μm, and Al2Y particles are identified as active nuclei by crystallographic calculation19,20. Furthermore, Al2Y and Al2Gd particles endow Mg-RE alloys with comparable grain refining efficiency to the well-recognized Zr elements. Moreover, the refined grains in Mg-RE alloys containing Al have better thermal stability than those containing Zr21.
Rationally adjusting the distribution, volume fraction, size, and morphology of strengthening phases plays a significant role in optimizing the mechanical properties of alloys. So far, there are few details about how Al element affects the formation of LPSO phase and how it affects the grain size in Mg-RE-Zn alloys. In this study, the microstructure and mechanical properties of Mg-12Gd-1Zn-0.6Ti-xAl under different heat treatment conditions were comprehensively studied to illustrate the effect of Al on Mg-RE-Zn alloys.
2. Materials and Methods
Mg-12Gd-1Zn-0.6Ti-xAl alloys were cast from commercial pure Mg, pure Al, pure Zn, Mg-30% Y ( wt % ) and Mg-30% Gd ( wt % ) master alloy blocks and pure Ti powder. Samples manufactured based on Al content are labeled as 0Al, 0.4Al, 0.8Al, and 1.2Al. The chemical composition of these alloys was summarized in Table 1. The alloys melted in a medium frequency induction furnace filled with Ar atmosphere, and then the castings were cooled in saltwater. The obtained ingots were homogenized at 500 °C for 8 h and then quenched in water at 20 °C. Afterwards, the homogenized samples were aged at 220 °C for different durations.
The heat treatment furnace was the SX2-12-16A box resistance furnace. The microstructures were analyzed by the JSM-6610 scanning electron microscopy (SEM). The image mode used to capture microscopic images is BSE, and the acceleration voltage is 5 kV. The phases were identified by the AL-2700B X-ray diffractometer (XRD). The elemental composition of each microarea was observed and analyzed by energy-dispersive spectroscopy (EDS). Vickers hardness tests were performed at least 6 times using a DHV-1000 ZCCD machine under a pressure of 1.96 N for 15 s. The tensile mechanical properties were tested by the WDW-100D precision universal testing machine and the tensile strain rate was 0.2 mm/min. The YS, UTS, and elongation are the average values obtained from testing at least three specimens.
3. Results and Discussion
3.1. Initial microstructure
Figure 1 shows the SEM micrographs of the as-cast Mg-12Gd-1Zn-0.6Ti-xAl alloys. The eutectic phases of alloy 0Al are continuously distributed along grain boundarys in the form of island. In alloy 0.4Al, a large number of bright and gray eutectic phases distributed along grain boundaries have been observed, as well as a small amount of cluster phases, as shown in Figure 1b. Compared with alloys 0Al and 0.4Al, the bright island phase and gray phase in alloys 0.8Al and 1.2Al are significantly reduced, and the cluster phase is increased. At the same time, some small particle phases appeared in the matrix, which was the most in the alloy 1.2Al.
sem images of the as-cast mg-12gd-1zn-0.6ti-xal alloys: (a) alloy 0al (b) alloy 0.4al (c) alloy 0.8al (d) alloy 1.2al.
Figure 2 shows magnified SEM micrographs of the as-cast Mg-12Gd-1Zn-0.6Ti-xAl alloys, and Table 2 summarizes the corresponding EDS results. Referring to the XRD patterns shown in Figure 3, the gray phase is Mg12Gd(Al, Zn), the island phase is (Mg,Zn)3Gd, the cluster phase is Al11Gd3 and the particle phase is Al2Gd. According to previous studies, the gray Mg12Gd(Al,Zn) phase in Al-containing alloys is usually 18R-LPSO22-24. Most of the particle Al2Gd and cluster Al11Gd3 phases are distributed in the center of the matrix, as shown in Figures 2c and 2d.
magnified sem images of the as-cast mg-12gd-1zn-0.6ti-xal alloys: (a) alloy 0al (b) alloy 0.4al (c) alloy 0.8al (d) alloy 1.2al.
It is generally believed that as-cast Mg-Gd-Zn alloys do not contain LPSO phase25-27, which is consistent with the results of this experiment. Obviously, due to the addition of Al, the microstructure of Mg-Gd-Zn alloys changes significantly. In particular, a large number of 18R-LPSO phases are formed in the as-cast alloy with the addition of 04Al. Trace Al can easily lead to lattice distortion in Mg alloys due to the difference in atomic radius between Mg (0.160 nm) and Al (0.143 nm). Therefore, a large number of stacking faults are generated, and then evolved into LPSO phase23,28,29. However, as the Al element increased to 0.8 and 1.2, the LPSO phase significantly decreased, while the Al11Gd3 and Al2Gd phases increased. This indicates a clear competitive demand for Al and Gd elements in the forming process of LPSO phases and Al-Gd phases.
3.2. Microstructural evolution via homogenization
Figure 4 shows the SEM micrographs of Mg-12Gd-1Zn-0.6Ti-xAl alloys homogenized at 500°C for 8h. It is evident that the (Mg,Zn)3Gd phases in the as-cast alloys has completely disappeared. The grains of alloys 0Al and 0.4Al increase significantly during homogenization treatment, while the grains of alloys 0.8Al and 1.2Al show almost no change. Many bulk phases are discontinuously distributed along grain boundaries, as shown in Figures 4a and 4b. However, in addition to the bulk phase, alloys 0.8Al and 1.2Al contain a large number of parallel layered phases distributed within the crystal, as well as the initial state of the Al2Gd and Al11Gd3 phases, as shown in Figures 4c and 4d. Numerous studies have shown that the second phase in the homogenized Mg-Gd-Zn-Ti-Al alloy is the Mg12Gd(Al,Zn) (14H-LPSO) phase, and exists in bulk and layered30-32. Therefore, it is indicated that the island (Mg,Zn)3Gd, some cluster Al11Gd3, and gray 18R-LPSO phases have transformed into 14H-LPSO phases. Obviously, with the increase of Al content from 0wt% to 0.4wt% and then to 0.8wt%, the proportion of 14H-LPSO phase increases. It shows that the 14H-LPSO phase has excellent stability at high temperature. As shown in Figure 4a, many rectangular phases are mainly distributed along grain boundaries, and this rectangular phase has been confirmed to be a compound with high Gd content31,33. For the as-homogenized alloys 0.8Al and 1.2Al, there are still some cluster Al11Gd3 and Al2Gd particles in the matrix, indicating that Al11Gd3 and Al2Gd phases also have good high-temperature stability.
sem images of the as-homogenized mg-12gd-1zn-0.6ti-xal alloys: (a) alloy 0al (b) alloy 0.4al (c) alloy 0.8al (d) alloy 1.2al.
3.3. Mechanical properties of the as-cast and as-homogenized alloys
Figure 5 shows the mechanical properties of the as-cast Mg-12Gd-1Zn-0.6Ti-xAl alloys. Among the four alloys, the as-cast alloy 0.4Al has the best tensile properties, the UTS is 218 MPa, the YS is 149 MPa, and the elongation is 4.5%. The excellent mechanical properties of 0.4Al alloy are mainly due to the large amount of 18R-LPSO phase in the alloy, which has high hardness and stiffness34. For the as-cast alloy 1.2Al, its mechanical properties are the worst, with UTS, YS and elongation of 187 MPa, 126 MPa and 2.3%, respectively. This is attributed to the existence of most of Al2Gd and Al11Gd3 phases in the alloy 1.2Al, which leads to stress concentration and brittle fracture of the alloy.
Figure 6 shows the mechanical properties of the as-homogenized Mg-12Gd-1Zn-0.6Ti-xAl alloys. The mechanical properties of as-cast Mg-12Gd-1Zn-0.6Ti-xAl alloys were improved after homogenization treatment at 500 °C for 8 h, which can be explained by the second phase strengthening of 14H-LPSO and the solid solution strengthening of Gd element35. Among the four alloys, the mechanical properties of the as-homogenized alloy 1.2Al are the best, and its UTS, YS and elongation are 249 MPa, 158 MPa and 12.0%, respectively. In addition, the mechanical properties of the as-homogenized 0Al alloy are improved the most, which indicates that a large number of solid solution Gd elements and block LPSO phases can effectively enhance the strength.
3.4. Age hardening behaviors
Figure 7 shows the age hardening behaviors of the as-homogenized Mg-12Gd-1Zn-0.6Ti-xAl alloys at 220 °C. Alloy 0.8Al exhibits the most significant age hardening response, with a rapid increase in hardness within 4-26 h and reaching a peak of 120 HV after 34 h. The as-homogenized alloy 0.4Al reaches its peak hardness of 113 HV after 22 h. Alloy 1.2Al reaches a peak hardness of 115 HV after 26 h. However, the as-homogenized alloy 0Al exhibited the worst age hardening behavior, reaching a peak hardness of only 108.3 HV after 8 h. The reason for the increase in hardness during the 220 °C aging treatment of the as-homogenized alloys is the precipitation of a large amount of β' precipitates31. The fine β' precipitates form a semi-coherent structure with the α-Mg matrix, which is beneficial to restrain the substrate slip and improve strength36,37.
3.5. Mechanical properties of peak-aged alloys
After homogenization treatment, peak aging treatment was performed on all Mg-12Gd-1Zn-0.6Ti-xAl alloys, and their tensile mechanical properties were tested. The tensile mechanical properties of the peak-aged Mg-12Gd-1Zn-0.6Ti-xAl alloys at ambient temperature are shown in Figure 8. The strength of Mg-12Gd-1Zn-0.6Ti-xAl alloys were significantly enhanced after peak aging treatment. However, the ductility has slightly decreased. The UTS and YS of 1.2Al alloy showed the greatest improvement, reaching 280 MPa and 185 MPa respectively. The mechanical properties of 0.8Al alloy are the best, and the YS, UTS and elongation are 187 MPa, 290 MPa and 6.8%, respectively. The 0Al alloy with larger grain size has a smaller aging hardening response, with YS, UTS, and elongation of 181 MPa, 265 MPa, and 4.2%, respectively The YS, UTS, and elongation of 0.4Al alloy are 184 MPa, 269 MPa, and 5.6%, respectively. After peak aging treatment, a large area of fine ellipsoidal β′ phases precipitated in the alloy will significantly enhance the comprehensive mechanical properties of the alloy26,38-40. Precipitation strengthening is the most dominant strengthening mechanism in the aging process. The β′ precipitated phase in the peak-aged alloy has a semi-coherent structure with α-Mg, which can effectively inhibit the basal slip and improve the tensile strength of the Mg alloy39,41,42. Interestingly, even if the tensile properties of the homogenized state are similar, the tensile properties of the peak-aged 0.8Al and 1.2Al alloys are significantly better than those of the 0Al and 0.4Al alloys. Moreover, the plasticity of the peak-aged Mg-12Gd-1Zn-0.6Ti-xAl alloys increases with the increase of Al element, and the elongation of the peak-aged alloy 1.2Al reaches 9.3%. This may be related to the Al11Gd3, 14H-LPSO and Al2Gd phases with high temperature stability.
4. Conclusions
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The second phase of as-cast Al-free alloy is composed of (Mg,Zn)3Gd phase. Adding trace amounts of Al to Mg-Gd-Zn-Ti alloy is beneficial for the formation of Mg12Gd(Al,Zn) phase (18R-LPSO). The (Mg,Zn)3Gd phase gradually decreases with the increase of Al, while Al2Gd and Al11Gd3 increase accordingly.
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The 18R-LPSO, (Mg,Zn)3Gd and some Al11Gd3 phases evolved into 14H-LPSO phase during homogenization treatment. When the Al content increases from 0 to 0.8wt %, the fraction of 14H-LPSO phase increases. The Al11Gd3, 14H-LPSO, and Al2Gd phases all exhibit excellent high temperature stability.
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The as-homogenized Mg-12Gd-1Zn-0.6Ti-0.8Al alloy exhibits the most significant age hardening response, with a rapid increase in hardness within 4-26 h and reaching a peak of 120 HV after 34 h. The precipitation of β′ precipitates in Mg-Gd-Zn-Ti(-Al) alloys is beneficial for suppressing substrate slip, leading to precipitation hardening and significantly enhancing strength. The 0.8Al alloy achieved the best mechanical properties, with YS, UTS, and elongation of 187 MPa, 290 MPa, and 6.8%, respectively.
5. Acknowledgments
This work was supported by the Hunan Provincial Natural Science Foundation of China (2022JJ50172), Key Scientific Research Project of Hunan Provincial Department of Education (24A0549), Shanxi Key Laboratory of Intelligent Casting and Advanced Forming for New Materials Open Fund Project (ICAF202505), Hunan Provincial Department of Education Higher Education Teaching Reform Research Project (HNJG-2022-1018), Science and Technology Innovation Guidance Project of Shaoyang (2022GX4073), Research Project on Degree and Graduate Teaching Reform at Shaoyang University (2022JGSY003).
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Data Availability
The data presented in this paper are part of the ongoing research initiatives. Revealing the data too early at this juncture may hinder the publication of follow-up research results. The data has not been publicly released. We take your understanding of this situation very seriously. We are firmly committed to making complete data accessible at the right time in the future. For users interested in accessing this data, it can be obtained by submitting a request to the corresponding author [Yuhong Zhao].
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Edited by
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Associate Editor:
Hugo Sandim.
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Editor-in-Chief:
Luiz Antonio Pessan.
Data availability
The data presented in this paper are part of the ongoing research initiatives. Revealing the data too early at this juncture may hinder the publication of follow-up research results. The data has not been publicly released. We take your understanding of this situation very seriously. We are firmly committed to making complete data accessible at the right time in the future. For users interested in accessing this data, it can be obtained by submitting a request to the corresponding author [Yuhong Zhao].
Publication Dates
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Publication in this collection
03 Nov 2025 -
Date of issue
2025
History
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Received
16 Feb 2025 -
Reviewed
25 Aug 2025 -
Accepted
31 Aug 2025
