Effect of Sn on the microstructural evolution of quasicrystal-reinforced Mg–Zn

Abstract

The effect of Sn content on the microstructure evolution of the as-cast, as-extruded and as-aged Mg-8Zn-2Y-xSn alloys were systematically investigated. The results show that addition of Sn not only refines the grains but also promotes the precipitation of quasicrystal I-phase and the formation of Sn₃Y₅. The phase transformations during solidification were also studied in detail. After extrusion, the broken second phase particles (I-phase) are more uniformly and densely distributed in the matrix with Sn addition. Moreover, ultra-fine dynamically recrystallized grains are obtained in extruded Mg-8Zn-2Y-0.5Sn alloy. In addition, high density nano-scale precipitates are uniformly dispersed by aging, and these precipitates are identified to be Mg-Zn particles, I phase and mixture of the Mg-Zn precipitates and I-phase.

Keywords

I-phase Sn addition phase transformations

Introduction

As the lightest commercial structural material, magnesium alloy has the advantages of high specific strength, specific stiffness and excellent damping performance, which has been used in aerospace, automobile and electronic communication fields [1 -3]. However, the low strength and plasticity of magnesium alloys greatly limit its application. The icosahedral quasicrystal phase (I-phase) has high hardness, thermal stability and low interface energy with Mg matrix. It is deemed that dispersed and tiny I-phase particles in the matrix can not only prevent dislocation movement during deformation, but also promote dynamic recrystallization, helping to refine the grains of the α-Mg matrix during hot working (such as hot rolling and hot extrusion) [4 -6]. Moreover, the excellent interface relationship between matrix and I-phase makes no crack initiation observed at the interface of two phases during deformation [7 -10].

The results show that the stable I-phase (Mg₃Zn₆Y) of Mg-Zn-Y alloy can be obtained by traditional casting. In as-cast Mg-Zn-Y alloy, I-phase easily forms at grain boundaries as coarse and continuous lamellar eutectic phase, which has no remarkable effect to improve the mechanical properties [11]. Singh et al. [12] found yield strengths up to about 400 MPa have been achieved by chill casting and direct extrusion of Mg₉₃Zn₆Y (at.-%) alloy containing I-phase. At the same time, there is W-phase- Mg₃Zn₃Y₂ (space group Fm3m and lattice parameter α = 0.685 nm) in Mg-Zn-Y ternary alloy. However, owing to the cubic structure of W-phase and the incoherency between W-phase and Mg matrix, the atomic bonding between W-phase and Mg matrix is very weak [13]. Therefore, with W-phase increasing, the mechanical properties of the alloys degraded greatly [9]. The formation temperature of W phase is higher than that of I-phase, deleterious crystalline phase W competes strongly with the strengthening phase. Therefore, the promotion and modification of phase structures are crucial to the performance of the alloy. Liu et al. found the formation of I-phase particles at the W/Mg interfaces through a solid-state phase transformation in Mg₉₅Zn_4.2Y_0.7 (at.-%) alloy using in situ heating TEM techniques [14]. But only a small part of W phase transformation was observed. Other method, such as Mg-6Zn-1.4Y the alloy formed by rheo-squeeze casting after ultrasonic vibration treatment, still unable to change its phase composition and has a large volume fraction of W phase [15].

Gao et al. found that the addition of Sn significantly increased the volume fraction of 18R LPSO phase by adding 0.3 wt-% Sn to Mg-6Y-2Zn alloy [16]. In addition, the precipitate strengthening of the second-phase MgZn₂ and β-Mg₂Sn phases is found in a Mg-1.6Zn-0.16Y-0.8Sn (at.-%) alloy [17]. Revealing the influence of alloying elements on phase transformation, second phase particle distribution and grain size change is helpful to understand the change of alloy properties. So far, the influence mechanism of alloying element Sn in Mg-Zn-Y alloy is still unclear [18,19]. In this work, Mg-8Zn-2Y-xSn (x = 0, 0.5 and 1 wt-%) alloys were designed to understand the evolution of the microstructure of the Mg-Zn-Y alloy with Sn addition. Especially, the modification effect of Sn element on the I-phase in the Mg-Zn-Y alloy was studied.

Experimental

The Mg-8Zn-2Y-xSn (x = 0, 0.5 and 1 wt-%) alloys were prepared from commercial pure Mg (99.95 wt-%), Zn (99.95 wt-%), Sn (99.99 wt-%) and Mg-30 wt-% Y master alloy. Vacuum induction furnace was used for melting. The stuffs were put into a mild steel crucible with a diameter of 85 mm and a length of 300 mm, filled with argon gas to prevent the oxidation. The crucible was heated to 740°C for melting. And then the melt was stirred well at 720°C for 25 min to ensure a homogeneous composition. After that the crucible was quenched into the saline water. The ingots was cut into cylinders with 80 in diameter and 50 in length, and then directly extruded into 16 mm diameter rods, with a ratio of 25:1 at a temperature of 350°C. Subsequently, a part of the extruded rods were annealed in a vacuum furnace at the temperatures of 160°C. The compositional analysis was carried out on the XRF-1800CCD X-ray fluorescence spectrophotometer (XRF). The actual compositions are given in Table 1.

Table 1

The designation and chemical composition of the as-cast alloy (wt-%).

		Measured composition
Alloy	Nominal composition	Mg	Zn	Y	Sn
ZW82	Mg-8Zn-2Y	Bal.	7.7	1.859	/
ZW82-0.5Sn	Mg-8Zn-2Y-0.5Sn	Bal.	7.95	1.99	0.5
ZW82-1Sn	Mg-8Zn-2Y-1Sn	Bal.	8.1579	2.2137	1.1193

The microstructure of the specimens was studied using the metallographic optical microscope (OM, Axiovert 40 MAT), the scanning electron microscope (SEM, TESCAN VEGA3) equipped with an X-ray energy-dispersive spectrometer (EDS). Specimens for OM and SEM observation were mechanically polished and etched with nital solution (4% nitric acid in ethanol, volume fraction). The phase constitutions of the as-cast alloy were analysed on a Rigaku D/max-2500 PC X-ray diffraction (XRD) instrument with Cu-Ka and a scanning rate of 4/min on the scanning angles between 10° and 90°. The DSC scan was carried out at a constant heating rate of 15°C/min under nitrogen atmosphere. For further studies on the precipitates in the aging process, a transmission electron microscope (TEM, JEOL 2100F) was used for observation. Thin foil specimens for TEM observation were prepared using a Gatan695 low temperature ion thinning apparatus. Vickers hardness was measured by HV-1000T digital microhardness tester under 50 gf load.

Results and discussion

Microstructure of the as-cast alloys

Optical micrographs of as-cast ZW82-xSn alloys are shown in Figure 1. It shows that the matrixes of three alloys with different contents of Sn addition are composed of dendrites. With the addition of Sn, the average grain size decreases. Particularly, as shown in Figure 1(b), with 0.5 wt-% Sn addition, ZW82-0.5Sn has the smallest grain size and the secondary dendrite spacing is 4.5 μm. The average secondary dendrite spacing in Figure 1(a–c) are 7.5, 4.5 and 6 μm, respectively. The results show that the grain can be refined by adding Sn, and the effect of 0.5 wt-% Sn is the most obvious.

Figure 1

Optical micrographs of as-cast ZW82-xSn alloys: (a) x = 0, (b) x = 0.5 and (c) x = 1.

Figures 2–3 show the XRD analyses of as-cast alloys. The pattern reveals that ZW82 alloy with no Sn addition is mainly composed of α-Mg, I-phase and W-phase, which is similar to the previous studies [15]. Moreover, with the addition of Sn, W-phase disappears. New characteristic peaks corresponding to Sn₃Y₅ are simultaneously detected, and the intensity of Sn₃Y₅ diffraction peaks enhanced when Sn is added to 1 wt-%. In short, the ZW82-0.5Sn and ZW82-1Sn alloys have the similar phase composition (I-phase, Sn₃Y₅ and α-Mg).

The SEM micrograph of as-cast alloys is shown in Figure 4. For ZW82 alloy, two different morphologies of lamellar eutectic structure and granular particle can be found in Figure 4(a), and the magnification of the white rectangular area is shown in Figure 4(d), labelled as A and B, respectively. EDS results in Table 2 indicate that lamellar eutectic structure and granular particle both contain Mg, Zn and Y while the molar ratio of Zn and Y is closed to 3:2 and 6:1, respectively. They should be W-phase/α-Mg eutectic pockets and granular I-phase, which is consistent with XRD analysis results and will also be verified in the later SADP analysis. In addition, similar morphology was observed in the work [15]. When 0.5 wt-% Sn is added to ZW82 alloy, divorced granular I-phase disappears. There are irregular particles containing Sn and Y inside the grains and the molar ratio with molar ratio of Sn to Y is close 3:5. According to XRD results and the previous study, it should be Sn₃Y₅ [20]. It can also be seen that there are some Mg in Sn₃Y₅ from the EDS results. Zhao et al. indicted that Mg has a certain solid solubility in Sn₃Y₅ phase [21]. In addition, because Mg is the matrix, there will be some errors in EDS analysis. Hence, the remaining lamellar eutectic structure must be I-phase/α-Mg eutectic pockets, which are close to the atomic Zn/Y ratio of I-phase shown in Table 2. It is worth mentioning that the lamellar spacing of I-phase/α-Mg eutectic pockets in ZW82-0.5Sn is significantly smaller than that of ZW82 alloy without Sn addition. With the addition of 1 wt-% Sn, I-phase / α-Mg eutectic structure becomes discontinuous, and the lamellar spacing slightly increases compared with ZW82-0.5Sn alloy.

On the basis of the DSC patterns, XRD analysis and microstructure observations of as-cast alloys. The composition of phases in alloys changes a lot with the addition of Sn. Therefore, it is necessary to discuss the solidification process of the alloys:

Figure 2

DSC analysis of as-cast ZW82 and ZW82-0.5Sn alloys.

Figure 3

XRD patterns of the as-cast ZW82-xSn alloys(x = 0, 0.5 and 1 wt %).

Figure 4

SEM images of as-cast alloys microstructure: (a)ZW82, (b)ZW82-0.5Sn, (c) ZW82-1Sn; (d), (e), (f) magnification of the white rectangular area in (a), (b) and (c), respectively.

Table 2

EDS results of the points indicated in Figure 4.

	Elements (at.-%)
Point	Mg	Zn	Y	Sn	Phase
A	73.22	17.07	9.71	/	W-phase
B	98.02	1.62	0.35	/	I-phase
C	85.20	12.60	2.1	/	I-phase
D	24.24	1.81	45.11	26.83	Sn₃Y₅
E	78.26	18.58	3.15	/	I-phase
F	19.03	0.82	47.2	32.94	Sn₃Y₅

At first, primary α-Mg nucleates from liquid metal (Equation (1)). With the decrease of temperature, the reaction type and temperature of the second phase of the alloys with and without Sn change evidently. For ZW82(as shown in Figure 5(a)-(d)), Y and Zn would segregate in the solid–liquid interface and W-phase/α-Mg eutectics are easy to form and agglomerate along primary α-Mg dendrites at about 500°C (Equation (2)), and then the remaining small amount of liquid phase forms the granular I-phase passing through Equation (3) at about 450°C. The three endothermic troughs in DSC curve are also agreed with the reactions. Moreover, the same reaction is also supported by the study of Fang [15]. (1) (2) (3)

Figure 5

Schematics of solidification process of Mg-8Zn-2Y alloy without Sn addition (a, b, c, d) and with Sn addition (a, b, e, f):(a) Liquid state; (b) Beginning of primary α-Mg solidification; (c) Formation of W-phase/α-Mg eutectics; (d) Formation of granular I-phase; (e) Formation of Sn₃Y₅; (f) Formation of I-phase/α-Mg eutectics.

Compared with ZW82, obvious differences in the phase transformations were observed with Sn addition (as shown in Figure 5(e)-(f)). An interesting phenomenon that either Y or Sn can be soluble in the α-Mg solid solution but they are not simultaneously soluble was proposed by Zhao et al. [21]. Thus, most of Y and Sn tend to be enriched at the solid–liquid interface, after nucleation of primary α-Mg. In addition, electronegative values of Mg, Zn, Sn, Y are 1.31, 1.65, 1.96 and 1.22, respectively [22]. According to the principle that the greater the electronegativity difference is, the easier it is to form compounds between elements, Sn₃Y₅ should nucleate earlier and more easily than other compounds [20] also shows that Sn₃Y₅ would form in Mg-1Sn-xY (wt-%) alloys (x less than 7) at 556°C by a reaction Equation (4). The absence of Sn₃Y₅ phase endothermic troughs in DSC curve may be attributed to low fraction of Sn₃Y₅ phase formation. At this point, with the further decrease of temperature, Y in the residual liquid would be suitable for the Zn/Y atomic ratio of eutectic reaction to obtain I-phase/α-Mg eutectic pockets (Equation (5)). (4) (5) According to a large number of studies, the grain refinement via alloying is mainly attributed to two factors in magnesium alloy. One is heterogeneous nucleation, and the other is the growth restriction factor (GRF), caused by solute elements segregation [22,23]. First, two conditions must be satisfied for the second phase particle to become the sites of heterogeneous nucleation during solidification: (i) the particle should precipitate from the liquid before the matrix; (ii) crystal surface structure of matrix and the particle in contact with each other. However, as shown in Figure 2, the DSC curve indicates that both ZW82 and ZW82-0.5Sn have three distinct endothermic troughs. Moreover, an endothermic trough at about 620°C in the two alloys, which should be the endothermic trough of the a-Mg matrix during solidification. Although the theoretical melting point of magnesium is 650°C, nucleation needs to take place in supercooled liquid. At the same time, the melting point of alloy is lower than that of pure metal. Hence, no phase can act as the sites of heterogeneous nucleation for the matrix during the solidification. Second, the per-unit GRF value corresponding to Sn in Mg is 1.47 according to the calculation results of Qian [23]. Another important reason is that most of Y and Sn tend to be enriched at the solid–liquid interface because of the addition of Sn according to the previous analysis, and Y even has a higher GRF than Sn. The supercooling caused by the enrichment of Sn and Y at the solid–liquid interface can hinder the grain growth and refine the grain.

Microstructure of the as-extruded alloys

As can be seen in Figure 6, the original dentritic structure of as-cast alloys is broken after extrusion. All alloys, excepting ZW82-1Sn, are mainly composed of fine equiaxed dynamic recrystallized grains and coarse elongated grains without dynamic recrystallization. The ultra-fine dynamic recrystallization grains, especially ZW82-0.5Sn alloy, are only 570 ± 60 nm. The average grain size of recrystallized grains in ZW82 and ZW82-1Sn are 810 ± 50 nm and 1.5 ± 0.3 μm, respectively. It is worth mentioning that the dynamic recrystallization process of the ZW82-1Sn alloy is the most complete with the uniform grain distribution.

Figure 6

Optical micrographs of as-extruded ZW82-xSn alloys: (a) x = 0, (b) x = 0.5 and (c) x = 1. Yellow wireframe indicates no recrystallization area.

Figure 7 shows the second phase distribution of the extruded alloy. Low magnification SEM micrographs (Figure 7(a–c)) indicate that the original the I-phase/α-Mg or W-phase/α-Mg eutectic pockets are broken into chains and distributed along the extrusion direction. After adding Sn, the volume fraction of the second phase particles is greatly increased. Compared with ZW82, the broken I-phase particles are more uniformly and densely distributed in the matrix. Simultaneously, the size of the particles is also greatly reduced with a size of 100–500 nm. Overall, the results indicate that adding Sn promotes the refinement and dispersion of the I-phase particles. Compare with ZW82, larger volume fraction and special structure of I-phase (about 1 μm) would effectively act as hard particles for stimulating recrystallization (PSN) [24,25]. Therefore, ZW82-0.5Sn shows the most effective grain refinement during hot deformation, which could be attributed to the small initial grain size, PSN effect of the fragmented I-phase particles [26]. And ZW82-1Sn shows the uniform grain distribution exhibits uniform grain distribution mainly attributed to the distribution of broken I-phase particles is more uniform than that of ZW82-0.5Sn alloy.

Figure 7

SEM images of as-extruded alloys microstructure: (a)ZW82, (b)ZW82-0.5Sn, (c) ZW82-1Sn; (d), (e), (f) magnification of the white rectangular area in (a), (b) and (c), respectively.

High magnification micrographs (see in Figure 7(e and f)) show that there are few large block particles in ZW82-0.5Sn and ZW82-1Sn alloy. The element distribution of one block particle is shown in Figure 8, and the result shows that it should be Sn₃Y₅, which satisfies the phase composition of as-cast alloy.

Figure 8

SEM micrograph and EDS results of the block phase in ZW82-0.5Sn alloy.

Microstructure of the as-aged alloys

The extruded samples were subjected to the artificial aging at 160°C (T5 treatment). According to the measurement of Vickers hardness tester, it is found that the peak aging time of the three alloys is about 46h. Figure 9 shows the Bright field TEM images obtained from the ZW82 and ZW82-1Sn after peak-aging. The chain like particles in Figure 8(a) should be obtained from the fragmentation of eutectic blocks during extrusion. The corresponding SAED pattern (insert) with the electron beam direction parallel to the zone axis reveals that they are W-phase with a face-centred cubic structure. We simultaneously find some isolated particles in ZW82 with a different lattice structure in Figure 9(b) and corresponding SAED pattern is shown in Figure 9(c). The isolated particle can be identified as an I-phase structure which has fivefold symmetry. It confirms that two types of particles correspond to W-phase/α-Mg eutectics and granular particles in cast ZW82 alloy. Figure 9(d) shows the TEM image and SAED pattern (insert) of ZW82-1Sn alloy, and those particles identified as I-phase by SADP pattern should be formed by fragmentation of I-phase/α-Mg eutectic blocks during extrusion.

Figure 9

Bright field TEM images of the ZW82 after peak- aging (a, b, c) and ZW82-1Sn (d): (a)and (d) Bright field TEM image and corresponding SAED patterns; (b) an isolated particle in ZW82 alloy and (c) corresponding SAED patterns.

High magnification TEM images of the ZW82 and ZW82-1Sn alloys after peak-aging are illustrated in Figure 10. In each alloy, very fine precipitation can be observed. Figure 10 (a) and (d) shows that some precipitates have a dark uniform contrast with a size about 50 nm and grey contrast with a size about 40 nm and less. In addition, some precipitates (marked by arrows) have a mixture of grey and black contrasts. Magnification of the mixture of grey and black contrasts and corresponding SAED patterns suggest that precipitates with a dark contrast should be I-phase. The report [4] pointed out that these precipitates are a mixture of the Mg-Zn precipitates and I-phase. In the meantime, Independent grwy contrast precipitates with a size of 5-50nm are identified to be MgZn₂ intermetallic compounds. Those precipitates should be precipitated during aging from a supersaturated matrix reported by Kima [27].

Figure 10

High magnification bright field TEM images of the ZW82 (a, b, c) and ZW82-1Sn (d) after peak- aging; (b) magnification of the mixture of grwy and black contrasts in ZW82 alloy and (c) corresponding SAED patterns.

Conclusions

In this paper, the effect of 0.5 wt-% Sn and 1 wt-% Sn addition on the microstructure evolution of the Mg-8Zn-2Y alloy under the as-cast, as-extruded and as-aged condition has been studied. The following conclusions are draw:

In as-cast alloy, 0.5 wt-% Sn has the most positive effect on the refinement of -Mg dendrites. Furthermore, composition of phases in alloys changes a lot with the addition of Sn. ZW82 alloy consists of -Mg, W-phase and a small number of granular I-phase, but increased volume fraction of l-phase and a few of Sn₃Y₅ phase form in ZW82-0.5Sn and ZW82-1Sn alloys.

Through the systematic analysis of the solidification mechanism of the three alloys, the difference of as-cast structure is caused by the phase transformations of L→Sn₃Y₅ + α-Mg and L→α-Mg + I owing to the change of solid–liquid interface composition.

After extrusion, the ultra-fine dynamic recrystallization grains with only 570 ± 60 nm and increased volume fraction of l-phase can be obtained from the ZW82-0.5Sn alloy.

Nano-scale I-phase, MgZn₂ and the mixture of the Mg-Zn precipitates and I-phase are uniformly precipitated from supersaturated matrix during aging.

Future recommendations

According to the above research, addition of Sn in Mg-8Zn-2Y not only refines the grains but also promotes the precipitation of quasicrystal I-phase. javascript:void(0);However, the effect of Sn addition on the mechanical properties of the alloy has not been revealed. Therefore, it is necessary to explore the mechanical properties of Mg-8Zn-2Y-xSn alloy as cast, extruded and aged, and explain the strengthening mechanism.

Footnotes

Disclosure statement

No potential conflict of interest was reported by the author(s).

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Effect of Sn on the microstructural evolution of quasicrystal-reinforced Mg–Zn–Y alloy

Abstract

Keywords

Introduction

Experimental

Results and discussion

Microstructure of the as-cast alloys

Microstructure of the as-extruded alloys

Microstructure of the as-aged alloys

Conclusions

Future recommendations

Footnotes

References