Effect of homogenization treatment on the morphology evolution of LPSO phase and the corresponding mechanical properties of Mg-8Gd-5Y-2.5Zn-0.6Zr alloys

ABSTRACT

The morphology of LPSO phase, mechanical properties and fracture behavior of Mg-8Gd-5Y-2.5Zn-0.6Zr (wt%) alloy were systematically studied. The microstructure of as-cast and homogenized alloys is mainly composed of α-Mg matrix and Mg₁₂(Gd,Y)Zn eutectic phase (LPSO phase). The as-cast alloy contains a large number of fine block 18R LPSO phases, which can be transformed into lamellar, rod-like and large block 14H LPSO phases after homogenization at 520°C for different time. Homogenization treatment can significantly improve the mechanical properties of Mg-8Gd-5Y-2.5Zn-0.6Zr alloy, especially the plasticity. The fine block and lamellar LPSO phases are prone to stress concentration, causing transgranular cleavage fracture, thereby damaging the mechanical properties of the alloy. The rod-like LPSO phase is easy to form pinning effect in the matrix, which can effectively improve the mechanical properties of the alloy and cause transgranular and dimple fracture, so that the alloy obtains the best ultimate tensile strength, yield strength and elongation, which are 252MPa, 214MPa and 17.2%, respectively.

Keywords:
Magnesium alloy; LPSO phase; Homogenization treatment; Microstructure; Mechanical property

1. INTRODUCTION

Magnesium alloys have broad application prospects in aerospace, military, biomedical devices and automotive industries due to their low density, high specific strength and good machinability [¹,²,³,⁴,⁵]. The existing commercial magnesium alloys for automobiles include AZ91D (Mg-9Al-0.7Zn), AM50A (Mg-5Al-0.4Mn) and AM60B (Mg-6Al-0.4Mn). These alloys have excellent combination of corrosion resistance and die castability [⁶, ⁷]. However, its low mechanical properties cannot meet the requirements of the current national defense and civil industry.

Some studies have shown that the addition of RE (rare earth elements) to magnesium alloys can improve the mechanical properties of alloys at room temperature and high temperature, and has better creep resistance than traditional Mg-Al series alloys, the most prominent of which is Mg-Gd-Y-Zr series alloys [⁸,⁹,¹⁰,¹¹]. Adding Zn element to Mg-Gd-Y-Zr alloy can significantly improve the strengthening effect of the alloy [¹², ¹³]. Many Mg-RE-Zn alloys are prone to form different types of long-period stacking ordered (LPSO) structures such as 18R, 24R, 10H, 14H during solution treatment or homogenization treatment [¹⁴,¹⁵,¹⁶]. As is well-known, the value of Zn/RE is an important parameter to evaluate the type of the second phase in Mg-Zn-RE alloys. When this value is close to 0.5, the second phase is the LPSO phase, as shown for the Mg₉₇Zn₁Y₂ alloy [¹⁷]. As this value increases to more than 1, the LPSO phase transforms to the W-Mg3Zn3RE2 phases and the I phase [¹⁸]. Mg₉₇Zn₁Y₂ (at.%) was developed by rapid solidification powder metallurgy method in 2001. It is a novel alloy excellent mechanical properties with ultimate tensile strength of 610MPa and elongation of 5%. The main reason for the excellent mechanical properties of these alloys is that the existence of LPSO structure improves the hardness and strength of magnesium alloys [¹⁹,²⁰,²¹,²²].

Many investigations related to the microstructure and mechanical properties of the Mg-Gd-Y-Zn-Zr system have been reported [²³,²⁴,²⁵]. However, little is known about the microstructure evolution of LPSO phase in Mg-Gd-Y-Zn-Zr alloy after homogenization treatment and the mechanical properties of the corresponding alloy, which limits its application. Therefore, this work aims to study the morphology evolution of LPSO phase, and comprehensively analyze the mechanical properties and fracture behavior of the corresponding alloys at room temperature.

2. EXPERIMENTAL PROCEDURES

In order to obtain Mg-8Gd-5Y-2.5Zn-0.6Zr alloy, Mg-30wt%Gd master alloy, Mg-30wt%Y master alloy, pure Zr and Mg were placed in a 98mm stainless steel crucible and melted in a medium frequency induction furnace under argon atmosphere at 780°C. After fully stirring, the stainless steel crucible containing the melt is immersed in room temperature brine and cooled. Homogenization was carried out in a vacuum furnace at 520°C for 0–64h, followed by water quenching immediately.

The samples analyzed by optical microscopy (OM) and scanning electron microscopy (SEM) were prepared using standard techniques of grinding with SiC sandpaper and polishing with a MgO suspension, followed by etching in a 4vol% nitric acid solution. Phase analysis was performed on a Rigaku D/MAX2500PC X-ray diffractometer with a copper target at a scanning speed of 15°/min and a scanning angle of 20° to 90°.

The tensile test of the above alloy samples was carried out at a tensile speed of 1.5mm/min with a standard cylindrical sample with a gauge distance of 25mm and a diameter of 5mm. All tensile tests were carried out on the Zwick/Roell Z020 tensile testing machine. All fracture morphologies were observed by SEM.

3. RESULTS AND DISCUSSION

3.1. Microstructural evolution

Figure 1 shows the X-ray diffraction (XRD) patterns of Mg-8Gd-5Y-2.5Zn-0.6Zr alloys obtained after homogenization at 520°C for different times, indicating that the alloys are mainly composed of α-Mg matrix and Mg₁₂(Gd,Y)Zn eutectic phase (LPSO phase). Many studies have shown that the LPSO phase usually exhibits an 18R-LPSO structure in as-cast alloys, and it will transform into a 14H-LPSO structure with high temperature stability after homogenization treatment [²⁶, ²⁷].

Figure 1
X-ray diffraction (XRD) patterns of the as-cast and homogenized alloy.

Figure 2 shows the optical micrographs of the as-cast and homogenized alloys at different holding times (4h–64h). It can be seen from Figure 2a and Figure 3a that the fine block LPSO phase is distributed along the α-Mg grain boundary. After homogenization treatment at 520°C for 4h, the fine block LPSO phase at the grain boundary becomes thinner obviously, and a small amount of lamellar LPSO phase precipitates at the grain boundary and within the grain, as shown in Figure 2b. After homogenization treatment at 520°C for 8h, it is almost difficult to find the block LPSO phase, and only lamellar LPSO phase can be seen at the grain boundaries and within the grains, as shown in Figure 2c and Figure 3b. This shows that the lamellar LPSO phase at the grain boundary is mainly transformed from the fine block LPSO phase, while the lamellar phase in the middle of the grain is mainly precipitated by the α-Mg supersaturated solid solution. From Figure 2d and Figure 3c, it can be seen that most of the lamellar LPSO phases are gathered together and transformed into rod-like LPSO phases. When the homogenization treatment reaches 16h, a part of the rod-like LPSO phase is obviously thickened, and the other part is transformed into a large block LPSO phase, as shown in Figure 2e. During the homogenization treatment from 16h to 64h, the microstructure of the alloy is mainly composed of rod-like and large block LPSO phases, and the size of the LPSO phase increases with the increase of homogenization treatment time, as shown in Figure 2e and Figure 2f. The microstructure of LPSO phase in as-cast and homogenized alloys at different holding time is summarized in Table 1.

Figure 2
Optical microstructure of the as-cast and homogenized alloy: (a) as-cast, (b) 520°C × 4h, (c) 520°C × 8h, (d) 520°C × 12h, (e) 520°C × 16h, and (f) 520°C × 64h.

Figure 3
SEM images of the as-cast alloy and homogenized alloy: (a) as-cast, (b) 520°C × 8h, (c) 520°C × 12h, and (d) magnified image of the region marked in (c).

Table 1
The morphology of the LPSO phase and the tensile properties of the corresponding as-cast alloy and the alloy homogenized for different times.

HOMOGENIZED CONDITION	MORPHOLOGY OF LPSO PHASE	YIELD STRENGTH/MPa	ULTIMATE TENSILE STRENGTH/MPa	ELONGATION/%
As-cast	Fine block LPSO	119	227	8.9
520°C × 4h	Fine block LPSO + lamellar LPSO	162	240	16.1
520°C × 8h	Lamellar LPSO	143	239	11.9
520°C × 12h	Rod-like LPSO	214	252	17.2
520°C × 16h	Rod-like LPSO + large block LPSO	144	231	11.7
520°C × 64h	Large block LPSO	/	/	/

Figure 3 shows the SEM micrographs of the as-cast Mg-8Gd-5Y-2.5Zn-0.6Zr alloy and homogenized at 520°C for 8h and 12h. The marked red rectangular area in Figure 3c is enlarged and shown in Figure 3d. The lamellar and rod-like LPSO phases can be clearly distinguished by observing Figure 3b and Figure 3c. Table 2 summarizes the EDS elemental analysis results of the corresponding points in Figure 3. The fine block phase (point A), lamellar phase (point C) and rod-like phase (point D) observed in the alloy have an ratio of (Y + Gd)/Zn (at%) about 4/3, which are all composed of LPSO phase. Some small white square phases such as point E and point F in Figure 3d can be determined to be rich in Gd and Y elements.

Table 2
EDS elemental analysis results of the corresponding points phase in Figure 3.

POINT	COMPOSITION (at%)				POSSIBLE COMPOUND
	Mg	Gd	Y	Zn
A	91.81	2.39	2.04	3.35	Mg12(Gd,Y)Zn
B	99.28	0.32	0.19	0.31	α-Mg
C	89.73	2.81	3.32	4.15	Mg12(Gd,Y)Zn
D	91.50	2.20	2.14	4.16	Mg12(Gd,Y)Zn
E	53.64	33.86	10.46	2.04	Gd and Y-rich elements
F	64.31	23.52	8.23	3.06	Gd and Y-rich elements

3.2. Mechanical properties and fractography

Figure 4 shows the tensile properties of Mg-8Gd-5Y-2.5Zn-0.6Zr alloy after homogenization at 520°C for different time. The corresponding yield strength (YS), ultimate tensile strength (UTS) and elongation are summarized in Table 1. After homogenization treatment, the UTS and YS increased slightly, but the elongation increased significantly. When the alloy is homogenized at 520°C for 12h, the alloy exhibits the best mechanical properties due to the presence of a large number of rod-like LPSO phases. Its YS is 214MPa, UTS is 252MPa, and elongation is 17.2%.

Figure 4
Tensile properties of the alloy obtained by homogenization treatment at 520°C for different times.

It has been reported that the LPSO phase has high Youngʼs modulus, which can effectively hinder the movement of dislocations and improve the strength of magnesium alloys [²⁸]. At the same time, the LPSO phase can increase the critical shear stress of basal slip and activate non-basal slip, thereby simultaneously improving strength and ductility [²⁹, ³⁰]. During the homogenization treatment, the main change in the microstructure of the alloy is the morphology of the LPSO phase. The morphology of LPSO phase may be the key factor affecting the mechanical properties of the alloy after homogenization treatment. The maximum variation is the elongation of mechanical properties, as shown in Figure 4. The fine block LPSO phase in the as-cast alloy is distributed along the α-Mg grain boundary, which is easy to cause stress concentration at the grain boundary, resulting in poor plasticity of the as-cast alloy. The precipitation of a small amount of lamellar phase (Fine block LPSO phase + lamellar LPSO phase) can promote the mechanics properties, but a large number of lamellar phase (Lamellar LPSO phase) are more likely to form sharp morphology, which is easy to produce cracks in the matrix and reduce plasticity. The rod-like LPSO phase is easy to form a pinning effect in the matrix, which can effectively improve the mechanical properties of the alloy.

Figure 5 shows the fracture surface of the tensile specimen of Mg-8Gd-5Y-2.5Zn-0.6Zr alloy after homogenization treatment at 520°C for different time. Large cleavage planes, secondary cracks and tearing ridges are observed on the fracture surface in Figure 5a and 5c, indicating that the fracture mode is typical transgranular cleavage fracture. This proves that the fine block and lamellar LPSO phases are easy to form secondary cracks in the matrix. The fracture surface shown in Figure 5b is mainly composed of tearing ridges around the cleavage planes and a large number of river patterns, indicating that the fracture mode is transgranular cleavage fracture. When the homogenization treatment reaches 12h, a large number of dimples, cleavage planes and tearing ridges can be easily observed in Figure 5d, indicating that the fracture mode is transgranular and dimple fracture. These fracture morphologies show that the fine block LPSO phase and lamellar LPSO phase are easy to cause stress concentration, resulting in cracks and reducing the mechanical properties of the alloy, while the rod-like LPSO phase is more conducive to the mechanical properties of the alloy.

Figure 5
SEM images showing fracture surfaces of tensile samples: (a) as-cast, (b) 520°C × 4h, (c) 520°C × 8h, and (d) 520°C × 12h.

4. CONCLUSIONS

• [1]

  Homogenization treatment at 520°C has a significant effect on the microstructure evolution of Mg-8Gd-5Y-2.5Zn-0.6Zr alloy. The as-cast alloy contains a large number of fine block 18R LPSO phases distributed along the grain boundaries. The high temperature stable 14H LPSO phases of fine block + lamellar, lamellar, rod-like, rod-like + large block and large block can be obtained by homogenization at 520°C for 4h, 8h, 12h, 16h and 64h, respectively.

• [2]

  Homogenization treatment can significantly improve the mechanical properties of Mg-8Gd-5Y-2.5Zn-0.6Zr alloy, especially the plasticity. The rod-like LPSO phase is easy to form a pinning effect in the matrix, which can effectively improve the mechanical properties of the alloy and obtain the best mechanical properties. The ultimate tensile strength, yield strength and elongation are 252MPa, 214MPa and 17.2%, respectively.

• [3]

  The fine block and a large number of lamellar LPSO phases are easy to cause stress concentration, which causes secondary cracks in the matrix and reduces the mechanical properties of the alloy. Their fracture mode is mainly transgranular cleavage fracture. The rod-like LPSO phase is more conducive to the mechanical properties of the alloy, especially plasticity, and its fracture mode is transgranular and dimple fracture.

5. ACKNOWLEGEMENTS

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), 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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Publication Dates

• Publication in this collection
  07 Feb 2025
• Date of issue
  2025

History

• Received
  26 Nov 2024
• Accepted
  23 Dec 2024