Materials Science and Engineering A355 (2003) 201 /207 www.elsevier.

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An investigation on the microstructure of an AM50 magnesium alloy

R.M. Wang a,b,*, A. Eliezer b, E.M. Gutman b
a

Electron Microscopy Laboratory and State Key Laboratory for Mesoscopic Physics, School of Physics, Peking University, Beijing 100871, PR China b Ben-Gurion University of the Negev, P.O. Box 853, Beer Sheba 84105, Israel Received 23 September 2002; received in revised form 13 January 2003; accepted 17 January 2003

Abstract The microstructure and the dislocation arrangement in the die cast AM50 magnesium alloy as well as in the stressed states have been investigated using conventional transmission electron microscopy (TEM), high-resolution TEM and energy dispersive X-ray analysis. The microstructure of the die cast AM50 alloy is found to mainly consist of a-Mg, b-Mg17Al12 and Al8Mn5 phases. Two kinds of b-Mg17Al12 particles with different sizes have been found in the stressed AM50 magnesium alloy. Besides the normal bMg17Al12 particles with size around several micrometers as in the die-cast AM50 magnesium alloy, some finer b-Mg17Al12 particles in the stressed states of the AM50 alloy have also been found. The finer b-Mg17Al12 particles are found to be only about tens of nanometers with oval or rod-like morphology, which may be formed during deformation. Dislocation pile-ups have been found in the stressed AM50 alloy for the first time. The spacing between each parallel dislocation in the pile-ups is only several nanometers. The dislocations are confined in the slip planes and piled up against grain boundaries. Dislocations in the networks are found to increase with deformation of the alloy. Also, dislocation networks have been found in the b-Mg17Al12 and Al8Mn5 phases as well as in the matrix in the deformed AM50 magnesium alloy. However, the dislocation pile-ups are found to be almost identical from 1.3% deformation to rupture, which explains the stable tensile yield strength of the AM50 magnesium alloy during the deformation. # 2003 Elsevier Science B.V. All rights reserved.
Keywords: Dislocation; Microstructure; AM50 magnesium alloy; Mechanical properties

1. Introduction The attractive mechanical properties of magnesium and its alloys increase their use for many technical applications [1,2], i.e. automobile, aeronautical and aerospace [3], housing utensils [4], electronic industries, etc. However, its poor galvanic corrosion resistance has been a major obstacle to its growth in structural application despite its other desirable physical and mechanical properties. Moreover, the problem of stress corrosion is becoming a major one today in Mg-alloys [5]. The susceptibility to intergranular stress corrosion cracking of magnesium base alloys depends strongly on alloy composition and heat treatment, and thus on the microstructure of the alloys. However, the fundamental factors that render an alloy susceptible are still far from

being understood. A lot of work has been done in aluminum alloys and dislocation pile-ups against the grain boundaries in the bands have been found. This finding has been used to predict the susceptibility to stress corrosion cracking [6]. We have studied the microstructure and dislocation arrangement in the AZ91D magnesium alloys and found dislocation pileups against the grain boundaries [7]. In this paper, the microstructure in the AM50 magnesium alloys and the dislocation arrangement in the stressed states were studied using conventional transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM) and energy dispersive X-ray (EDX) analysis.

2. Experimental procedures The specimen of AM50 Mg-alloy used for this study was die cast in a 200 t cold chamber machine. Round (gauge length of 75 mm and diameter of 5.9 mm)

* Corresponding author. Tel.: '/86-106275-5266; fax: '/86-1062751615. E-mail address: rmwang@pku.edu.cn (R.M. Wang).

0921-5093/03/$ - see front matter # 2003 Elsevier Science B.V. All rights reserved. doi:10.1016/S0921-5093(03)00065-0

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specimen was produced at casting temperatures of 660 8C, injection rate of 57 m s (1 and die casting temperature of 200 8C. Their chemical compositions are given in Table 1. All tensile tests were performed at 25 8C and strain rate of 7 )/10(4 s(1 on Zwick-1445 machine (Zwick GmbH & Co., Germany) on 5 /7 specimens. Fig. 1 shows the typical strain /stress curve for AM50 alloy. The tested mechanical properties of the AM50 alloys stressed up to rupture are summarized in Table 2. Specimens for TEM and HRTEM analyses were prepared as follows. First, slices with diameter of 6 mm and thickness of 0.2 mm were cut from the center of the stressed AM50 specimen where the stress was concentrated. Then, they were mechanical polished and cut into 3 mm disks, and dimpled to about 10 mm in the center. Final preparation of the specimens was ion milling on a Gatan precision ion polishing system 691 under conditions of 5.0 kV and incident angle of 6 / 48. Conventional TEM and HRTEM analysis were conducted on a JEOL 2010 TEM equipped with a Gatan Multiscan CCD digital camera. The software for the CCD camera is Digital Micrograph 2.5.8. EDX spectroscopy was performed using an X-ray analysis with TIA integrated system for Tecnai attached to Tecnai F30 field emission TEM (FEI Company, USA).

Fig. 1. Typical strain /stress curve for AM50 alloy.

3. Results and discussion 3.1. Microstructure of the die cast AM50 magnesium alloy From the Mg /Al phase diagram, the AM50 magnesium alloy consists of a-Mg (hexagonal crystal structure, space group P 63/mmc, a 0/0.32094 nm and c 0/0.52105 nm) and b-Mg17Al12 (cubic crystal structure, Space 3 m, a 0/1.056 nm) phases. With the addition group I 4 of 0.57% (mass.) Mn, some Al8Mn5 (hexagonal crystal structure, a 0/1.273 nm and c 0/1.588 nm) particles have also been found in the AM50 magnesium alloy. Fig. 2 shows typical microstructure of the die-cast AM50 magnesium alloy. The b-Mg17Al12 precipitates, as shown in Fig. 2(a), are found to have typical lamellar structure and distribute in the matrix rather homogenously. The length of the lamellar b-Mg17Al12 precipitate ranges from hundreds of nanometers to several micrometers and the width is about tens of nanometers. However, the Al8Mn5 precipitates are found to have
Table 1 Chemical composition of the AM50 alloy (mass.%) Elements Chemical composition Al 5.1 Mn 0.57 Zn 0.15 Si 0.013

typical polygonal morphology with hundreds of nanometers in size. Moreover, the distribution of the Al8Mn5 precipitates is different from that of the bMg17Al12 ones. In some cases, only one or two precipitates can be found in the observation field, while in some other cases, several precipitates segregate in the observation field with the same magnification zoom, as shown in Fig. 2(b). The interfaces between the Al8Mn5 phase and the matrix are found to be sharp and clean. Some defects, such as stacking faults or twins, have also been found in the Al8Mn5 particles. The dislocation density of the a-Mg in the die cast AM50 magnesium alloy tends to be rather high, which is due to the fast cooling under geometric constraint that was experienced by the die cast specimens. As shown in Fig. 2(c), many of the dislocations are arranged in networks indicating that considerable recovery has also occurred during cooling to room temperature. The average dislocation spacing is measured to be about 100 nm ranging from about 10 nm to about 1 mm. Fig. 2(d) gives a high-resolution image of the a-Mg in the die cast AM50 magnesium alloy. The incident beam is parallel with [0 0 1] axis of the a-Mg matrix. The 0) and (1 0 0) interplannar spacing between each (/1 1 planes of the a-Mg phase is equal to 0.278 nm. The slight difference of the contrast in the high-resolution image comes from the nano-scale strains induced distortion in the alloy. Inside the circle in Fig. 2(d), one dislocation can also be found with an excessive atom plane. The nano-scale strains and dislocations in the alloy are due to the fast cooling under geometric constraint that was experienced by the die cast specimens.

Ni 0.0006

Cu 0.0007

Fe 0.0040

Be 0.0013

Mg Rest

R.M. Wang et al. / Materials Science and Engineering A355 (2003) 201 /207 Table 2 Mechanical properties of the AM50 alloys stressed up to rupture Samples M1 M7 M2 TYS (MPa) 124.4 119.9 117.5 TYS0.2% (MPa) 132.1 128.2 126.7 Stressmax (MPa) 146.9 166.4 194.8 Strain (%) 1.3 3.6 6.8 State No rupture No rupture Rupture

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Fig. 3 shows the EDX spectrums of the phases that exist in the AM50 alloy. Many points with different sizes range from 10 nm to 1 mm in diameter have been detected and the results are found to be identical. The analyzed results are summarized in Table 3. The chemical composition of the matrix obtained from the EDX is consistent with the nominal one with little aberration. The Mn content in the matrix is found to be apparently less than the nominal one, which indicates that most of the Mn in the alloy exists in the Al8Mn5 form. The Mg/Al ratio (67.14/32.76) of the b-Mg17Al12 phase is found to be a bitter higher than the normal ratio 17/12, which may be influenced by the matrix. In similarity, the little amount of Mg in the Al8Mn5 phase

comes from the matrix. The Al/Mn ratio (57.94/37.08) of the Al8Mn5 phase is very close to the stiometrochemistry 8/5. The results indicate that chemical composition obtained from the EDX analyses fit the nominated chemical composition of the alloy and the stiometrochemistry of the phases in the alloy very well. 3.2. Microstructures and dislocations in the stressed AM50 magnesium alloys After tensile test performed at 25 8C and strain rate of 7 )/10(4 s (1, the microstructures and dislocations in the stressed alloys were found to change apparently with deformation. The density, state and distribution of the

Fig. 2. Typical microstructures of the die cast AM50 alloy. (a) Bimodal distribution of a-Mg and b-Mg17Al12, (b) distribution of Al8Mn5 precipitates, (c) dislocation networks, (d) high resolution image of the a-Mg matrix showing dislocation and nano-scale strains.

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Fig. 3. EDX spectrum of the phases in the AM50 alloy.

Table 3 Analyzed chemical composition of the phases shown in Fig. 3 (at.%) Phase Matrix (a-Mg) b-Mg17Al12 Al8Mn5 Mg 94.65 67.14 4.98 Al 5.25 32.76 57.94 Mn 0.1 0.10 37.08

dislocations as well as the interface between the matrix and the secondary phases, such as b-Mg17Al12, Al8Mn5 etc. were found to be related to the deformation states. Fig. 4 shows typical bright field images of the dislocation arrangements in the AM50 magnesium alloy after 1.3% deformation. The dislocation network in Fig. 4(a) corresponds to that shown in Fig. 2(c), which forms during cooling to room temperature. After the tensile test, the dislocations density increases apparently. The dislocation arrangements in the networks become more complex and tangled with each other. The average dislocation spacing in the network is measured to be about 40 /100 nm, which is less than that in the die case AM50 alloy, indicating higher dislocation density. One remarkable characteristic of the dislocation arrangements in the stressed AM50 magnesium is the existence of straight and parallel dislocations, as shown in Fig. 4(b /d). Such straight and parallel dislocations form in series and are confined in the slip plane and pile up against the grain boundary. In Fig. 4(b), the straight and parallel dislocations are confined within a grain of the AM50 alloy. The dislocation lengths are chiefly hundreds of nanometers and the spacing between them are ranging from ten to several hundred nanometers. However, in Fig. 4(c), the dislocation pile-ups are found to exist along the interface between two grains in the AM50 magnesium alloy. The sizes are smaller and the density is even higher. High magnification image of such

pile-ups is shown in Fig. 4(d). Hundreds of dislocations with about 100 nm in length pile up together. The spacing between each parallel dislocation is found to be almost identical, which is only several nanometers. Fig. 5 gives a high-resolution image of the Al8Mn5 and the matrix. The incident beam is parallel with [1 1 2] direction of Al8Mn5 phase. The interplannar spacing 0) and (/1 1 1) planes in the between the nearest two (/1 1 Al8Mn5 phase are measured to be about 1.1 and 0.51 nm, respectively. The spacing between the lines in the bottom of Fig. 5 is measured to be about 0.52 nm, which is very close to the spacing between each (0 0 1) plane of a-Mg (0.521 nm). Along the interface, some Moire fringes can be found at the bottom of Fig. 5. Some additional dark contrast in the Al8Mn5 phase indicates nano-scale strains at those areas. With higher deformation test, some very fine bMg17Al12 precipitates have been found in the AM50 magnesium alloy. Fig. 6 shows a typical microstructure and a corresponding selected area pattern of two kinds of b-Mg17Al12 precipitates in the AM50 magnesium alloy after 3.6% deformation. The incident beam is parallel to [1 1 1] direction of b-Mg17Al12 phase. The coarse precipitates, as shown in Fig. 6(a), is very large with dendritic or lamellar structure as those in the die cast state. The size is about several micrometers. However, the fine ones, as shown in Fig. 6(b), have typical oval or rod-like morphology with size of only tens of nanometers. The similar morphology and directional distribution of the very fine b-Mg17Al12 particles reveals that they are formed by the same mechanism, possibly during the deformation. Investigations also indicate that the density of the dislocations increase with deformation. Fig. 7 shows typical bright field images of the dislocation networks and pile-ups in the alloy after 3.6% deformation. In Fig. 7(a), many dislocations tangled together. The average dislocation spacing is only about 20 /50 nm. The lengths of the dislocation also become shorter with average about 100 nm. In Fig. 7(b), some dislocation pile-ups can be found at the interface between the Al8Mn5 phase and the matrix. Some dislocations can also be found within the Al8Mn5 phase. Moreover, it is found some bMg17Al12 particles have been broken to pieces during the deformation, as shown in Fig. 7(c). Fig. 8 shows typical dislocation arrangements in the AM50 alloy till rupture (6.8%). It can be seen that the dislocation density in network (shown in Fig. 8a) is very high. The spacing between the dislocations is only about 10 /30 nm. However, the spacing between each parallel dislocation within the dislocation pile-ups is found to be also several nanometers, which is much more stable when deformed from 1.3% to rupture. More detailed investigations indicate the distance between two successive dislocations decreases as the barrier. As shown Fig. 8(b) as arrow, the distance between the two in pile-up

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Fig. 4. Typical dislocation arrangements in the AM50 alloy after 1.3% deformation. (a) Dislocations network, (b /d) dislocation pile-ups.

which is more than two times than that near the dislocation core. From Table 2, it can be found that the tensile yield strength of the AM50 alloy is almost identical during 1.3% deformation to rupture with similar dislocation pile-ups. It is a prospective way to tailor the mechanical properties of the magnesium alloy by the control of dislocation pile-ups.

4. Conclusions The microstructure of the die cast AM50 alloy consists of a-Mg, b-Mg17Al12 and Al8Mn5 phases. The a-Mg and b-Mg17Al12 particles have a wide variety of morphologies while Al8Mn5 particles have typical polygonal morphologies. High-density dislocations in the aMg have been found in the die cast AM50 alloy. The dislocation networks form during cooling to room temperature. Dislocation pile-ups have been found in the stressed AM50 alloys. They are confined in the slip planes and are piled up against the grain boundary. The spacing between each parallel dislocation is found to be only

Fig. 5. High resolution image of the Al8Mn5 phase and the matrix in the AM50 alloy after 1.3% deformation.

near the dislocation core is measured to be only 4 /5 nm. The distance between the two successive dislocations increases gradually and at the end of the dislocation pile-ups, the distance is measured to be over 10 nm,

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Fig. 6. Two kinds of b-Mg17Al12 precipitates in the AM50 alloy after 3.6% deformation. (a) Coarse b-Mg17Al12, (b) ne b-Mg17Al12, (c) corresponding SAD pattern of the ne b-Mg17Al12 phase.

several nanometers and remains almost identical after 1.3% deformation to rupture. The distance between two successive dislocations is also found to decrease as the barrier.

The dislocation density in the networks increases with the amount of deformation of the alloy. Dislocations have also been found in the b-Mg17Al12 and Al8Mn5 phases as well as in the matrix in the deformed alloy.

Fig. 7. Dislocation arrangements in the AM50 alloy after 3.6% deformation. (a) Dislocation network, (b) dislocation pile-ups, (c) dislocations in bMg17Al12.

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Fig. 8. Dislocation arrangements in the AM50 alloy after 6.8% deformation. (a) Dislocations network, (b) dislocation pile-ups.

Fine b-Mg17Al12 particles have been found in the deformed AM50 alloy. They have oval or rod-like morphology with size tens of nanometers.

References
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[3] J.M. Arlhac, J. C. Chaize, Proceedings of the Third International Magnesium Conference, G. W. Lorimer (Ed.), The University Press Cambridge, UK, 1997, p. 213. [4] J. Abthoff, W. Gelse, J. Lang, Proceedings of the Third International Magnesium Conference, G. W. Lorimer (Ed.), the University Press Cambridge, UK, 1997, p. 193. [5] P.L. Bonora, M. Andrei, A. Eliezer, E. Gutman, Proceeding of the Second Israeli International Conference on Magnesium Science and Technology, E. Aghion, D. Eliezer (Eds.), Magnesium Research Institute (MRI) Ltd., Beer-Sheva 84100, Israel, 2000, p. 410. [6] M.O. Speidel, Proceeding of Conference Fundamental Aspects of Stress Corrosion Cracking, R.W. Staehle, A.J. Forty, D. Van Royen (Eds.), The Ohio State University, 1967, p. 561. [7] R.M. Wang, A. Eliezer, E.M. Gutman, Microstructure and dislocations in the stressed AZ91D magnesium alloys, Mat. Sci. Eng. A 344 (1 /2) (2003) 279 /287.