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Effect of Aging on the Microstructure and Mechanical Properties of


Magnesium Alloy AZ31:

Article  in  Metal Science and Heat Treatment · July 2016


DOI: 10.1007/s11041-016-9985-8

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DOI 10.1007/s11041-016-9985-8
Metal Science and Heat Treatment, Vol. 58, Nos. 3 – 4, July, 2016 (Russian Original Nos. 3 – 4, March – April, 2016)

UDC 669.721.5:621.785.7

EFFECT OF AGING ON THE MICROSTRUCTURE


AND MECHANICAL PROPERTIES OF MAGNESIUM ALLOY AZ31

H. Kerenciler,1 S. Gündüz,2 M. Akif Erden,2 M. Türkmen,3 and H. Karabulut4

Translated from Metallovedenie i Termicheskaya Obrabotka Metallov, No. 3, pp. 54 – 59, March, 2016.

The structure and mechanical properties of magnesium alloy AZ31 are studied after conventional and defor-
mation aging under conditions corresponding to the thermal cycle of polymerization in paint coating of cars.
The aging is conducted after 3-h solution treatment at 400°C, water quenching, and aging at 180°C for from
10 min to 6 h. Some of the specimens are deformed by 0.5% right after the solution treatment and then aged by
the same regime.

Key words: magnesium alloys, aging, rupture strength, yield strength.

INTRODUCTION Elevation of the strength of an alloy is commonly ac-


companied with decrease in its formability, which means that
Magnesium alloys are promising materials for the auto- the hardening process for magnesium alloys should be deve-
motive and aerospace industries, communication and elec- loped after their plastic forming [13]. Artificial aging of
tronics due to their low weight, high specific strength, stiff-
magnesium alloys is usually performed at up to 200°C
ness, machinability and recyclability [1]. Most structural
[13 – 17]. In accordance with the binary phase diagram aging
magnesium alloys, especially in the automotive industry, be-
of Mg – Al alloys is accompanied by precipitation of a
long to the Mg – Al – Zn system (series AZ). Phase transfor-
mations in such alloys have been studied well [2 – 5]. The Mg17Al12 equilibrium b-phase (44.0 wt.% Al) with a struc-
only phase precipitated in these alloys is Mg17Al12 b-phase. ture of type a-Mn. Introduction of zinc into a Mg – Al alloy
It is always lamellar and forms in the structure by the mecha- lowers the solubility of aluminum in solid magnesium and
nism of discontinuous or continuous precipitation [6]. How- raises accordingly the content of precipitates under aging,
ever, the hexagonal close-packed lattice of magnesium alloys which is accompanied by a moderate growth in the strength
is responsible for a little number of slip systems in them. For [18]. Though the number of studies devoted to precipitation
this reason, magnesium alloys have low formability at room hardening of magnesium alloys is great, their results are am-
temperature [7 – 9] and are used in the industry primarily af- biguous.
ter pressure casting. Much effort has been devoted to the de- The aim of the present work was to study the effect of
velopment of secondary thermomechanical treatment pro- preliminary deformation, and of the temperature and dura-
cesses for refining the structure of magnesium alloys, which tion of aging on the mechanical properties of magnesium al-
should widen the range of their application [10 – 12]. loy AZ31.
1
Karabük University, Institute of Science and Technology, Depart-
METHODS OF STUDY
ment of Manufacturing Engineering, Karabük, Turkey (e-mail:
kerencihuseyin@gmail.com).
2
Karabük University, Technology Faculty, Department of Ma- We studied a sheet of alloy AZ31 with a thickness of
nufacturing Engineering, Karabük, Turkey (e-mail: 1.5 mm in the state as delivered. The chemical composition
sgunduz@karabuk.edu). of the alloy was as follows (in wt.%): 3.19 Al, 0.81 Zn,
3
Kocaeli Iniversity, Hereke Vocational School, Department of 0.334 Mn, 0.2 Si, 0.01 Be, 0.005 Cu, £ 0.005 Fe, the remain-
Metallurgy, Kocaeli-Gebze, Turkey (e-mail:
der Mg.
mustafa.turkmen@kocaeli.edu.tr).
4
Karabük University, Vocational School, Department of Occupa- The specimens for the tensile tests were fabricated ac-
tional Health and Safety, Karabük, Turkey (e-mail: cording to TS EN ISO 6892-1 [19] (Fig. 1). The solution
hasankarabulut@karabuk.edu.tr). treatment was performed in a furnace at 400 ± 2°C for 3 h
179
0026-0673/16/0304-0179 © 2016 Springer Science + Business Media New York
180 H. Kerenciler et al.

5 mm
1.5 mm

Æ1
15 mm

2m
m

25 mm
76 mm

Fig. 1. Specimen for tensile tests.


20 mm
à
and followed by water quenching at room temperature. To
prevent natural aging, the specimens after the quenching
were placed into a freezer.
After the quenching the specimens were subjected to ag-
ing at 180°C for from 10 min to 6 h and then cooled in air. A
part of the specimens before the aging were deformed by
0.5% by tension.
The tensile tests were performed at room temperature in
a Schimadzu machine at a speed of 3.33 ´ 10 – 4 sec – 1. We
determined the average values of mechanical characteristics
after testing three specimens per point.
The metallographic specimens were prepared by a stan- 20 mm
b
dard method with final polishing with diamond powder with
particle size 1.5 mm. Then the specimens were etched in a so- Fig. 2. Microstructure of alloy AZ31 in the state as delivered (a)
lution containing 6 g picric acid, 5 ml acetic acid, 10 ml and after a treatment for solid solution (b ). Light microscopy.
water and 100 ml ethanol for 5 – 20 sec. The microstructure
was studied under an optical microscope. The grain size d
was determined by the method of secants drawn at an angle under the action of plastic deformation; the twins became
of 45° to the rolling direction. At least 500 grains were mea- places of nucleation for precipitates.
sured for each specimen. The precipitated Mg17Al12 phase in the specimens sub-
Scanning electron microscopy was used to study the pre- jected to preliminary deformation prior to the aging are pre-
cipitated particles and the fracture surfaces of the specimens. sented in Fig. 4. By the data of a local chemical analysis the
particles contain aluminum and magnesium, which proves
RESULTS AND DISCUSSION that this is a Mg17Al12 phase indeed. Similar results can be
found in [23, 24] for magnesium alloy AZ63 after pressure
Figure 2 presents the single-phase structure of magne- casting.
sium alloy AZ31 in the state as delivered and after the solu- Table 1 presents the results of mechanical tests of the al-
tion treatment. It can be seen that the grain size after the solu- loy in different states. It can be seen that in the state as deli-
tion treatment is about twice larger than in the state as deli- vered AZ63 with a single-phase fine-grained structure has a
higher strength but lower ductility than in the alloy with
vered (12 and 6 mm respectively). After a short aging with
coarse-grain structure after the solution treatment. Figure 5
preliminary deformation (Fig. 3a and b ) the structure con-
presents the mechanical properties of the alloy after aging.
tains a Mg17Al12 intermetallic compound over grain bound-
With increase in the aging time the strength characteristics
aries and in grain bodies [20, 21], which is accompanied by
twins. When the duration of the aging is increased, the twins pass through a maximum at tag = 45 – 60 min. The absolute
become coarser simultaneously with grain growth value of the maximum is higher in the case of the use of pre-
(Fig. 3c – e). liminary deformation. The elongation also has a maximum at
The microstructure changes with aging in the same man-
ner both with and without preliminary deformation (0.5%).
The only difference is the finer structure of the specimens TABLE 1. Mechanical Properties and Grain Size of Magnesium
subjected to preliminary deformation. The preliminary defor- Alloy AZ31
mation accelerates the kinetics of the precipitation of parti- State s0.2 , MPa sr , MPa d, % d, mm
cles of Mg17Al12, and the precipitates hinder the grain growth
As delivered 83 157 13 6
as it has been suggested in [22]. The authors of [22] have ob-
After solution treatment 77 130 14 12
served formation of twins in the matrix of a magnesium alloy
Effect of Aging on the Microstructure and Mechanical Properties of Magnesium Alloy AZ31 181

à 20 mm b 20 mm c 20 mm

Mg17Al12

d 20 mm e 20 mm f 20 mm

Fig. 3. Microstructure of magnesium alloy AZ31 after solution treatment, 0.5% deformation and aging at 180°C for different times (light
microscopy): a) 30 min; b) 45 min; c) 1 h; d ) 1.5 h; e) 4 h; f ) 5.5 h.

tag = 45 – 60 min; the height of the maximums is about equal level than without deformation. In [13] the optimum me-
for both aging variants. However, in the case of preliminary chanical properties of magnesium alloys have been obtained
deformation the elongation at tag > 1 h remains at a higher after aging at 170°C for 6 h; the aging increased the Vickers

Mg17Al12 Mg17Al12

à 10 mm b 5 mm

I
Mg
c

Al

0 1 2 3 4
E, keV

Fig. 4. Microstructure of magnesium alloy AZ31 after aging at 180°C for 5.5 h (a, b ) and energy
dispersive spectrum analysis of particles of Mg17Al12 intermetallic (c). Scanning electron microscopy.
182 H. Kerenciler et al.

sr ; s0.2 , ÌPà d, % s, ÌPà


200 50 200 10%
à 45 min
180 30 min
sr 160 1h
160 ST
40 SD 2h 3h
140 120 4h
5h 6h
120 80
100 30
40
80 s0.2
60 0
20 e, %
40 d
s, ÌPà
20 à
200 b 1h 10%
10 45 min
0 2 4 6 tag , h 30 min
160 SD 2h
ST 3h 4h
sr ; s0.2 , ÌPà d, % 120 5h
220 50 6h
200 80
180 40
sr 40
160
140 0
e, %
120
100 s0.2 30 Fig. 6. Stress – strain curves for magnesium alloy AZ31 after aging
80 at 180°C for different times (given at the curves): a) without prelimi-
60 nary deformation; b ) before aging with 0.5% deformation; SD) state
d 20 as delivered; ST) after solution treatment.
40
20 b
10
0 2 4 6 tag , h tion and the presence of particles of precipitated Mg17Al12
phase in grain bodies and on grain boundaries. The particles
Fig. 5. Dependence of mechanical properties of magnesium alloy limit the growth of microvoids at high degrees of deforma-
AZ51 on the duration of aging at 180°C: a) without preliminary de- tion. It has been reported [28, 29] that the geometry of the
formation; b ) 0.5% preliminary deformation.
dimples is related to the mechanical properties, and the size
of the dimples depends primarily on the deformation rate.
However, in our case the deformation rate is constant, and
hardness, the tensile strength and the elongation. In [13] so- the size of the dimples should be dependent of the micro-
lution treatment of alloy AZ80 was conducted at 400°C for structure and on the texture. The observed difference in the
3 h with subsequent water quenching. dimples may be caused by difference in the ductility in dif-
Prolongation of aging above the optimum time should ferent states (initial, quenched and aged), because tension ac-
cause coalescence of the precipitates, and this explains the tivates different slip systems.
lowering of the strength characteristics in this case [25].
The stress-strain curves of the specimens aged in diffe- CONCLUSIONS
rent modes are presented in Fig. 6. It can be seen that the
specimens deformed prior to the aging have higher strength 1. Aging at 180°C for 45 – 60 min produces an optimum
characteristics than the not deformed specimens. A similar combination of the characteristics of strength and ductility
effect of preliminary deformation in aging has been observed
in magnesium alloy AZ31, i.e., the rupture strength
in aluminum [26] and magnesium [27] alloys.
sr = 190 MPa, the yield strength s0.2 = 130 MPa, and the
Figure 7 presents fracture surfaces of the alloys in differ-
ent structural states. In the initial condition and after the solu- elongation d ~ 20%.
tion treatment the fracture surfaces (Fig. 7a and b ) exhibit 2. Deformation of degree 0.5% before aging raises sr to
large dimples and many flat regions typical for brittle frac- 210 MPa and s0.2 to 150 MPa without changing the level of
ture. The flat regions in Fig. 7b indicate that the fracture has the elongation.
developed either over twin boundaries or over shear bands. 3. The hardening in the aging process is connected with
However, after conventional aging for 45 min (Fig. 7c ) and precipitation of particles of b-phase (Mg17Al12 ) in the bodies
1-h aging with preliminary deformation (Fig. 7d ) we observe and on the boundaries of grains.
small dimples and cleavage facets. These aging modes corre- 4. Analysis of fracture surfaces shows partially brittle
spond to elongation maximums (Fig. 5). These phenomena fracture behavior of the alloy in the state as delivered and af-
are explainable by the smaller grain size in the aged condi- ter solution treatment. After the aging by the optimum re-
Effect of Aging on the Microstructure and Mechanical Properties of Magnesium Alloy AZ31 183

à 10 mm b 10 mm

Fig. 7. Fracture surfaces of magnesium


alloy AZ31 in different states: a) as deli-
vered; b ) after solution treatment; c) after
aging at 180°C for 45 min without pre-
liminary deformation; d ) after aging at
180°C for 1 h after preliminary deforma- 10 mm 10 mm
c d
tion.

gime the fracture surfaces exhibit finer dimples and cleavage 12. S. W. Xu, N. Matsumoto, S. Kamado, T. Honma, and Y. Kojima,
facets. “Dynamic microstructural changes in Mg – 9Al – 1Zn alloy
during hot compression,” Scr. Mater., 61, 249 – 252 (2009).
13. S. Ming-hong, S. Guo-dong, W. Yu, and Q. Jun, “Paint-bake re-
REFERENCES sponse of AZ80 and AZ31 Mg alloys,” Trans. Nonferrous Met.
Soc. China, 20, 571 – 575 (2010).
1. R. Zhu, W. Li, Y. Wub, X. Cai, and Y. Yu, “Effect of aging treat- 14. R. Gonzales-Martinez, J. Göken, D. Letzig, K. Steinhoff, and
ment on low-cycle fatigue behavior of extruded Mg – 8Al – K. U. Kainer, “Influence of aging on damping of the magne-
0.5Zn alloys,” Mater. Des., 4, 203 – 207 (2012). sium-aluminum-zinc series,” J. Alloys Comp., 437, 127 – 132
2. J. F. Nie, X. L. Xiao, C. P. Luo, and B. C. Muddle, “Characteri- (2007).
sation of precipitate phases in magnesium alloys using electron
15. S. M. Hirth, G. J. Marshall, S. A. Court, and D. J. Lloyd, “Ef-
microdiffraction,” Micron, 32, 857 – 863 (2001).
fects of Si on the aging behavior and formability of aluminum
3. S. Celotto, “TEM study of continuous precipitation in Mg –
alloys based on AA6016,” Mater. Sci. Eng. A, 319, 452 – 456
9 wt.% Al – 1 wt.% Zn alloy,” Acta Mater., 48, 1775 – 1787
(2001).
(2000).
16. N. E. Bekheet, R. M. Gadelrap, M. F. Salah, and A. N. Abdel
4. A. F. Crawley and K. S. Milleken, “Precipitate morphology and
Azum, “The effects of aging on the hardness and fatigue behav-
orientation relations in an aged Mg – 9% Al – 1% Zn – 0.3% Mn
ior of 2024 Al alloy/SiC composites,” Mater. Des., 23,
alloy,” Acta Metall., 22, 557 – 562 (1974).
153 – 159 (2002).
5. J. B. Clark, “Age hardening in a Mg – 9 wt.% Al alloy,” Acta
Metall., 16, 141 – 152 (1968). 17. J. P. Zhou, D. S. Zhao, R. H. Wang, Z. F. Sun, J. B. Wang,
6. M. X. Zhang and P. M. Kelly, “Crystallography of Mg17Al12 J. N. Gui, and O. Zheng, “In situ observation of ageing process
precipitates in AZ91D alloy,” Scr. Mater., 48, 647 – 652 (2002). and new morphologies of continuous precipitates in AZ91 mag-
7. R. E. Reedhill and W. D. Robertson, “Deformation of magne- nesium alloy,” Mater. Lett., 61, 4707 – 4710 (2007).
sium single crystals by nonbasal slip,” Trans. Amer. Inst. Min. 18. S. W. Xu, N. Matsumoto, S. Kamado, T. Honma, and Y. Kojima.
Metall. Eng., 209, 496 – 502 (1957). “Effect of Mg17Al12 precipitates on the microstructural changes
8. F. E. Hauser, P. R. Landon, and J. E. Dorn, “Fracture of magne- and mechanical properties of hot compressed AZ91 magnesium
sium alloys at low temperature,” Trans. Amer. Inst. Min. Metall. alloy,” Mater. Sci. Eng. A, 523, 47 – 52 (2009).
Eng., 206, 589 – 593 (1956). 19. Turkish Standard TS EN ISO 6892-1, Metallic Materials – Ten-
9. A. R. Chaudhuri, H. C. Chang, and N. J. Grant, “Creep deforma- sile Testing, Part 1: Method of Test at Room Temperature, Turk-
tion of magnesium at elevated temperatures by nonbasal slip,” ish Standards Institution, March 2011.
Trans. Amer. Inst. Min. Metall. Eng., 203, 682 – 688 (1955). 20. Y. Uematsu, K. Tokaji, and M. Matsumoto, “Effect of aging
10. N. V. Ravi Kumar, J. J. Blandin, C. Desrayaud, F. Montheillet, treatment on fatigue behavior in extruded AZ61 and AZ80 mag-
and M. Suery, “Grain refinement in AZ91 magnesium alloy nesium alloys,” Mater. Sci. Eng. A, 517, 138 – 145 (2009).
during thermomechanical processing,” Mater. Sci. Eng. A, 359, 21. R. Zhu, W. Ji, Y. Wu, X. Cai, and Y. Yu, “Effect of aging treat-
150 – 157 (2003). ment on low-cycle fatigue behavior of extruded Mg – 8Al –
11. R. S. Chen, J. J. Blandin, M. Suery, Q. D. Wang, and E. H. Han, 0.5Zn alloys,” Mater. Des., 41, 203 – 207 (2012).
“Thermomechanical processing and superplasticity of AZ91 22. N. V. Ravi Kumar, J. J. Blandin, and M. Suery, “Effect of
magnesium alloy,” J. Mater. Sci. Technol., 20, 295 – 297 thermomechanical treatments on the microstructure of AZ91 al-
(2004). loy,” in: K. U. Kainer (ed.), Magnesium Alloys and their Appli-
184 H. Kerenciler et al.

cations, Wiley-VCH Verlag GmbH & Co, KgaA, Weinheim 26. S. Gündüz and R. Kaçar, “Strengthening of 6063 aluminum al-
(2006), pp. 161 – 167. loy by strain ageing,” Kovove Mater., 46, 345 – 350 (2008).
23. M. Marya, L. G. Hector, R. Verma, and W. Tong, “Microstruc- 27. K. Zheng, J. Dong, X. Zeng, and W. Ding, “Effect of pre-defor-
tural effects of AZ31 magnesium alloy on its tensile deforma- mation on aging characteristics and mechanical properties of
tion and failure behaviors,” Mater. Sci. Eng. A, 418, 341 – 356 Mg – Gd – Nd – Zr alloy,” Trans. Nonferrous Met. Soc. China,
(2006). 17, 1164 – 1168 (2007).
24. C. L. Liu, Y. C. Xin, G. Y. Tang, and K. C. Paul., “Influence of
28. A. Das and S. Tarafder, “Geometry of dimples and its correla-
heat treatment on degradation behavior of bio-degradable
die-cast AZ63 magnesium alloy in simulated body fluid,” Ma- tion with mechanical properties of austenitic stainless steel,”
ter. Sci. Eng. A, 456, 350 – 357 (2007). Scr. Mater., 59, 1014 – 1017 (2008).
25. L. Yan, Z. Zhi-min, and X. Yong, “Influence of aging on micro- 29. F. Lv, F. Yang, Q. Q. Duan, Y. S. Yang, S. D. Wu, S. X. Li, and
structure and mechanical properties of AZ80 and ZK60 magne- Z. F. Zhang, “Fatigue properties of rolled magnesium alloy
sium alloys,” Trans. Nonferrous Met. Soc. China, 21, 739 – 744 (AZ31) sheet: influence of specimen orientation,” Int. J. Fa-
(2011). tigue, 33, 672 – 682 (2011).

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