Accepted Manuscript

Microstructural characterizations and mechanical properties in underwater fric-

tion stir welding of aluminum and magnesium dissimilar alloys

Yong Zhao, Zhengping Lu, Keng Yan, Linzhao Huang

PII: S0261-3069(14)00748-1
DOI: http://dx.doi.org/10.1016/j.matdes.2014.09.046
Reference: JMAD 6819

To appear in: Materials and Design

Received Date: 30 July 2014

Accepted Date: 16 September 2014

Please cite this article as: Zhao, Y., Lu, Z., Yan, K., Huang, L., Microstructural characterizations and mechanical
properties in underwater friction stir welding of aluminum and magnesium dissimilar alloys, Materials and
Design (2014), doi: http://dx.doi.org/10.1016/j.matdes.2014.09.046

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Microstructural characterizations and mechanical properties in underwater

friction stir welding of aluminum and magnesium dissimilar alloys

Yong Zhao1, Zhengping Lu1, Keng Yan1,*, Linzhao Huang1

1. Provincial key Lab of Advanced Welding Technology, Jiangsu University of Science and Technology, No.2
Mengxi Road, Zhenjiang Jiangsu, China 212003

Abstract:
Formation of intermetallic compounds in the stir zone of dissimilar welds affects the
mechanical properties of the joints significantly. In order to reduce heat input and control the amount
and morphological characteristics of brittle intermetallic compounds underwater friction stir welding
of 6013 Al alloy and AZ31 Mg alloy was carried out. Microstructures, mechanical properties,
elements distribution, and the fracture surface of the joints were analyzed by optical microscopy,
scanning electron microscopy and energy dispersive X-ray spectroscopy etc. The result shows that
sound dissimilar joint with good mechanical properties can be obtained by underwater friction stir
welding. Al and Mg alloys were stirred together and undergone the process of recrystallization,
forming complex intercalated flow patterns in the stir zone. Tensile strength of the dissimilar joint
was up to 152.3MPa. Maximum hardness (142HV) appeared in the middle of the centerline of the
specimen. Intermetallic compounds layer consisting of Al3Mg2 and Mg17Al12 formed in the Al/Mg
interface and resulted in the fracture of the joint.

Keywords: Magnesium alloy, Aluminum alloy, Dissimilar alloy joint, Friction stir welding,
Microstructure, Mechanical properties

1.Introduction
As light alloys with low density, high special strength and good anti-corrosion properties
aluminum and magnesium are widely used in transportation and electronic communications
industries. In certain applications, the successful welding of dissimilar metals of aluminum and
magnesium is advantage for producing lightweight structures, pushing forward the lightweighting
technology and the project of energy-saving and emission-reduction [1]. Researchers had tried
various fusion welding methods such as gas tungsten arc welding (GTAW), gas metal arc welding
(GMAW) [2], laser welding [3] and solid state welding technology such as vacuum diffusion

*Corresponding author: Tel:(+86)013305281357,Fax:(+86)051184434793, Email:yankeng@just.edu.cn

1
bonding [4] to join Al to Mg. However, these welding methods are not widely used because of the
poor weld joint strength caused by pores, cracks and Al-Mg intermetallic compounds with high
hardness and low ductility. In addition, some specific process requirements which are difficult to
carry out cause these methods limited.
Being different from fusion welding, friction stir welding (FSW) is a solid-state welding
process. In the process of FSW, shouldered tool with a pin rotates and moves between sheets of the
pieces to be welded and friction heat which is not sufficient to melt the materials generates. In
consequence, materials to be welded reach the plastic state and are joined together under the action
of stirring and pressure [5,6]. Naturally, the obvious lower temperature helps FSW to avoid many
defects appearing in fusion welding and the nature features FSW owns make it get higher joint
strength. All these make FSW be a potential welding technique in dissimilar materials joining. More
details about the process of FSW were described in many earlier publications [7-11].
Recent years, many efforts had been focused on the application of FSW in dissimilar materials
such as dissimilar Al alloys [12-14], dissimilar Mg alloys [15], Al to steel [16,17], Al to
Mg[18-21],etc. Some researchers had tried to weld Al and Mg alloys under water using the method
of FSW and got better mechanical properties than in air [22]. While joints of Al alloys and Mg alloys
obtained by FSW under water were sound with good mechanical properties, the details of
microstructural evolution of dissimilar joints of Al and Mg alloys have not been fully understood. In
this paper, 6013 Al alloy and AZ31 Mg alloy were welded by FSW under water. The microstructure,
distribution of elements, hardness, tensile strength and fracture feature of the joints were investigated
to make a comprehensive analysis of the microstructures and mechanical properties of the FSW
joints of 6013 Al alloy and AZ31 Mg alloy.

2. Material and experimental procedures

Commercial available base materials (BM) AA6013 aluminum alloy and AZ31 magnesium
alloy sheets (100902.5mm) were welded in the study. Their chemical compositions and
mechanical properties are listed in Table 1. The weld process was done under water at a
FSW-3LM-002 machine produced by China Friction Stir Welding Center in this experiment. The
shouldered tool which was made of H13 steel was 16mm in diameter and concave, with a 2.5mm
long and 5mm in diameter threaded cylindrical probe. During the welding process AA6013 was
placed at the advancing side (AS) and AZ31 Mg was placed at the retreating side (RS). The two
alloys were welded at a rotation speed of 1200 rpm and travel speed of 80 mm/min. The welding tool
rotated counterclockwise and the tilt angle was 2.5 from the normal surface of the workbench.

2
Oxide film was removed with steel brush and greasy was cleaned by ethanol before welding.
Following FSW, transverse cross section was observed by optical microscopy (OM). The
specimens for OM were cut perpendicular to the welding direction by using an electrical discharge
machine. After the sample was ground and polished, the Al and Mg side of the joint were swabbed
multiple times with different etching solutions (1mL HNO3+1mL CH3COOH+1g H2C2O4+150mL
distilled water for the Mg alloy; 2mL HF+5mL HNO3+95mL distilled water for the Al alloy) by
using a cotton ball until visible etching was obtained. Additionally, the samples were cleaned with
ethanol after a few seconds of the swabbing. Microstructures of the weld were observed with an
optical microscope and the fracture surface of the FSW joints after tensile tests (according to ASME
BPVC IX-2010) were examined by a JSM-6460 scanning electron microscope (SEM) equipped with
an Oxford energy dispersive X-ray spectroscope system (EDS).
The phase analysis was carried out by using a multi-functional D/max 2550VL/PC X-ray
diffractometer (XRD) to identify the intermetallic compounds in the dissimilar joints from the
fracture surface(both AZ31 side and AA6013 side). The XRD process used CuK radiation at 45 kV
and 40mA. The diffraction angle (2) at which the X-rays hit the sample varied from 20 to 110
with a speed of 6 per minute.
Vickers microhardness was measured with a MH-5D digit hardness tester across the sectioned
weld and a load of 100g and dwell time of 15s was applied.

3. Results and discussion

3.1 Appearances and microstructures

Fig.1 shows the surface appearance of the friction-stir joint of Al 6013 and Mg AZ31 performed
under water. It can be seen that sound weld without obvious defects such as cracks or tunnel type
defects was obtained when rotation speed was 1200 rpm and travel speed was 80mm/min with the
pin moving along the center. This is contrary to some other researchers result. Yan et al [23]
reported that if rotating pin traveled along the butt line between the two base materials cracks
developed.
A cross-sectional macrograph of the dissimilar joint is presented in Fig.2. In the macrograph the
left side is AA6013 and the right side is AZ31 Mg alloy. The delineation which means the boundary
between nugget zone (NZ) and the thermo-mechanical affected zone (TMAZ) on the Al side is

3
sharper and clearer than that on the Mg side. This is related to the difference in the state of plastic
flow during welding process. In the stir zone, with the cavity effect produced by the rotating tool, the
material on the advancing side was squeezed to the back of the pin. In this case , the plastic
deformation direction of base metal is consistent with the welding direction and a relative
deformation difference formed between base metal and the plastic deformed metal. So the boundary
between the nugget zone and the thermal mechanically affected zone is obvious on the Al side.
Plasticity deformed metal on the retreating side flow to the back of the pin and the deformation
direction of base metal is contrary to the welding direction. Almost base metal on the retreating side
deform together with the plasticity deformed metal. This make no obvious boundary between NZ
and TMAZ form on the retreating side.
The joint of 6013 Al alloy and AZ31 Mg alloy got underwater in this experiment is much
smoother and less intermixed than that got in air with the same welding parameter in our earlier
experiment. This is because the heat input acting on the water welded specimen is lower than that
acting on the air welded specimen, making plastic flow be more difficult to achieve.
Fig.2a and Fig.2b show the microstructures of 6013 Al alloy and AZ31 Mg alloy respectively.
Obviously, the microstructures of base materials of AA6013 and AZ31 consist grains of unequal
sizes and distributions. Fig.2b shows a grain size of about 25m for the AZ31 Mg alloy base metal.
Fig.2f shows a typical optical image of the interface of a dissimilar Al/Mg weld and the right side
near the interface is recrystallized Mg. In the process of FSW, the stirring movement and friction
thermal cycle cause intense plastic deformation and high temperature and induce dynamic
recrystallization. This makes the recrystallized Mg grains (about 2m) be much finer than grains in
Fig.2b. Mofid et al [22] reported that, as a result of lower heat input and lower peak of temperature
of water submerged weld, the recrystallized Mg grain size in the interface and stir zone of water
welded specimen was considerably finer than that of air welded specimen.
The electron probe micro analysis (EPMA) image and distribution maps of major elements Mg
and Al in mixture structure of the stir zone corresponding to Fig.2f are presented in Fig.3. It can be
seen clearly in the image that elements of Al and Mg are stirred together in the weld zone. During
FSW the alloys in the two sides of the welding center undergo a high temperature action and
continuous deformation. In the process of plastic deformation, two different alloys are stirred up
together and mixture structure forms. In the high temperature action recrystallization occurs, causing
4
the original extrude slender Al grains and coarse primary Mg grains transform to fine equiaxed
grains.
Fig.2c,d and e show microstructures of various parts of the mixing welded zone. Being different
from FSW zones of same metal, microstructures in the dissimilar weld zone are intercalated to form
complex lamellar-like shear bands composed with either recrystallized Al alloy or Mg alloy. In this
study, AA6013 and AZ31 alloys in the stir zone are mixed with each other, forming an intercalated
structure. The results of EDS analysis show that the light white color band is 6013 Al alloy and the
dark color band is AZ31 Mg alloy. It also can be seen that the water welded intercalated structures
formed no matter at the upper part of the joint (Fig.2c and Fig.2d) or at the lower part of the joint
(Fig.2e and Fig.2f) are all sound without defects. Quite on the contrary, Mofid et al [22] found many
cracks in light-etching phase (Al) in the stir zone when the alloys were welded in air.
A typical complex lamellar-like shear band formed in the water-welded stirred zone noticed in
Fig.2d was studied by means of SEM. Fig.4a is a low magnification SEM image. During FSW, the
base materials experience both plastic deformation and frictional heating arising from the rotation of
the tool. Alternating bands consisting of Al and Mg alloys in the joints are caused by the two
processes. Cao G et al [24] suggested that diffusion between dissimilar metals in FSW will be
enhanced with a higher stain rate due to the enhanced plastic deformation. Fig.4b is a higher
magnification SEM image of the banded structure. A whole band can be divided into three parts c, d
and e as marked in the enlarged scale micrograph in Fig.4b. EDS analysis performed at the three
different locations revealed that the three parts contained different counts of Al and Mg elements, as
shown in Table 2. According to phase diagram of the aluminum-magnesium system [30] and Table 2,

region c and e correspond to Al and Mg solid solution, respectively. Region dwhich consists

of 68.62 wt.% Al and 31.38 wt.% Mg, contains the intermetallic compound Al3Mg2 and Al solid
solution. Earlier papers [25,26] stated that besides Al3Mg2, Al12Mg17 was also found in the stir zone
of air welded specimen and the brittle compounds are the main reasons for the formation of the crack
in the stir zone.
A local SEM image of the interface (region f in Fig.2f) is shown in Fig.5a. It can be seen that
the interface is marked by a distinguishable white interlayer varied in thickness between the Mg
alloy (at the right side in Fig.5) and the Al alloy (at the left side in Fig.5). Analyze the chemical

5
compositions of the white interlayer by EDS. The results of EDS line analysis show that the amounts
of aluminum (Fig.5b) and magnesium (Fig.5c) are all slow changes rather than sudden changes at the
Al/Mg interface, revealing that there is an intermetallic (IMC) layer formed at the interface of 6013
Al alloy and AZ31 Mg alloy. According to the EDS quantitative analysis, the composition of the
white intermetallic layer is defined to the Al3Mg2 or phase ((Al=67.4 at.%),(Mg)=32.6 at.% ).
The presence of intermetallic layer in the welded specimen is related to the solidification of the
liquated material in the interface. It should be emphasized that the thickest layer in the interface of
water welded specimen is only about 10um, which is much thinner than the layer in the Al/Mg
interface of air welded specimen in our earlier experiment, revealing that lower heat input can reduce
the amount of intermetallic compounds in the stir zone.

3.2 Distribution of microhardness

The Vickers microhardness values of the dissimilar joint were measured along the dashed lines
marked in Fig.2, which are 0.5 mm (Crown), 1.25 mm (Middle) and 2mm (Bottom) to the top
surface, and the results are shown in Fig.6. The microhardness presents an uneven distribution. The
average hardness values of base materials of 6013 Al alloy and AZ31 Mg alloys are 125HV and
65HV, respectively. Micro hardness values of the stir zone depend on the phase constituents and the
extent of local recrystallization. The high, maximum hardness values of the stir zone are due to the
presence of hard, brittle intermetallic compounds. In Fig.6, the hardness distribution at the middle
line of the cross section shows a maximum hardness (142HV) at the centerline, but not much higher
than that of base material 6013 Al alloy. Mofid M A et al [22] reported that maximum hardness
values were much greater than base materials when welded in air because more intermetallic
compounds formed in the stir zone of air welded specimen. Then, microhardness falls below the
value of base material AA6013 and then rises slowly with the approach to the base material on the Al
side while it falls to and keeps at the average level of base material AZ31 on the Mg side. The sharp
variation of hardness in the weld zone is related to the online ring structure and the intercalated
microstructure.
In spite of the fact that grains at the nugget zone are recrystallized and being much smaller than
the base material, the microhardness falls immediately in other locations except the area where
intermetallic layer presents. This is because the nugget hardness in the precipitation hardenable

6
aluminum alloys greatly depends on the strengthening precipitates rather than the grain size. There is
no report about the detailed research of the precipitate distribution across the Al/Mg weld joint. But
studies[27,28] on the FSW of age hardenable Al-Mg-Si alloys indicated that the dissolution of the
fine needle shaped precipitates leaded to lower hardness at the stir zone.
The hardness traverse at the 0.5mm (Crown) and 2mm (Bottom) line are generally lower than
that of the 1.25mm (Middle) line. This is because there is only a little intermixing occurred between
6013 Al alloy and AZ31 Mg alloy in the top and the bottom region according to the EDS analysis
listed in Table 2.

3.3 Tensile properties and fracture feature of joints

The tensile strength of the friction stir welded joints of 6013/AZ31 is up to 152.3MPa,
equivalent to 63.3% of AZ31 Mg alloy strength. The elongation of the underwater dissimilar joint is
1.3% which is much lower than that of the AZ31 Mg alloy. The lower plasticity is attributed to the
high hardness and low toughness phase formed at the weld interface as discussed in the following
part. Fig.7a shows the fracture location of the tensile specimen. It is seen that the tensile specimen
failed at the joint center where the hardness gradient is the sharpest according to Fig.6. Fig.7b shows
a low magnification image of the fracture surface of the Al side of a tensile specimen. It can be seen
that the fracture appearance is not all the same and can be divided into three layers across the whole
surface. The crown layer, middle layer and the bottom layer are about one-sixth, three-sixth and
two-sixth of the whole fracture surface, respectively. Large area of the cross section especially the
middle (Fig.7e and Fig.7f) and the bottom (Fig.7d) show brittle fracture with evidence of
cleavage-like feature, indicating that the dissimilar weld failed through brittle fracture. The fracture
surface near the crown shows some swirl like pattern (Fig.7c), which is different from other areas of
the fracture surface. Element analysis shows that counts of composition of the three areas are
different. The bottom area contains 91.19 at.% Al and 8.81 at.% Mg, the middle area contains 85.83
at.% Al and 12.73 at.% Mg, while the crown area contains 78.65at.% Al and 21.35at.% Mg. In the
process of FSW, with the effect of shoulder and pin of the welding tool, the crown zone of the cross
section is stirred more strongly than the middle and the bottom zone, leading to more Mg was stirred
into Al alloy.
Fig.8 and Fig.9 show the X-ray diffraction patterns of the matching fracture surface of the

7
AA6013 side and AZ31 Mg alloy side respectively. Qualitative analysis shows that intermetallic
compounds Al3Mg2 and Mg17Al12 were detected on both Mg and Al side. The amount of intermetallic
compounds on the fracture surface is very small, leading to the intensity of the intermetallic
compounds peaks lower than the reference peaks. This result is similar to the discovery of S.H. Et al
[29]. They found Mg, Al3Mg2 and Al12Mg17 on the Mg side while Al and Al3Mg2 on the Al side. The

eutectic temperature of -Mg and Al12Mg17 is about 437 and there is a wide range of chemical

compositions that can develop inhomogeneous interfacial layer at a low melting temperature
according to the Al-Mg phase diagram [30]. The temperature in the stir zone is sure to drop to a
lower value though the maximum temperature in the stir zone may be higher than the eutectic
temperature. So under such wide ranges of temperature and chemical compositions, it is difficult to
avoid intermetallic compounds in the process of FSW. But the amount and thickness of the
intermetallic compounds can be reduced by decreasing heat input in this investigation, as states in

4. Conclusions
6013 Al alloy and AZ31 Mg alloy were FS-welded under water in this study and from the above

investigations, the main conclusions can be summarized

(1). Sound welding with good mechanical properties was produced between 6013 Al alloy and
AZ31 Mg alloy through FSW under water with the welding speed of 80mm/min and rotation speed
of 1200 rpm.
(2). EPMA images show that elements of Al and Mg are stirred together and mixture structure
form in the stir zone. The EDS analysis indicates that the mixture structures are formed with
lamellar-like shear bands which are composed with either recrystallized Al alloy or Mg alloy.
(3). An intermetallic layer is observed at the interface of 6013 Al alloy and AZ31 Mg alloy and the
IMC layer is much thinner than the layer observed in air welded specimen.
(4). The results of Vicker microhardness show that the maximum hardness(142HV) appears in the
middle of the centerline of the water welded specimen and is not much higher than the micro
hardness value of base material 6013 Al alloy.
(5).The tensile strength of the underwater friction stir welded joint is up to 152.3MPa, equivalent
to 63.3% of AZ31 Mg alloy strength, but attribute to the intermetallic compounds the ductility of the
joint is low.
(6). The tensile specimen failed at the joint center where the hardness gradient is the sharpest and

8
the specimen failed through brittle fracture. XRD analysis shows both Al3Mg2 and Mg17Al12 on both
Al and Mg side of the fracture surface.
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11
TABLE LIST

Table 1. Chemical compositions and mechanical properties of experimental materials

Table 2. EDS analysis of Al and Mg elements at different locations in the weld zone (wt,%)

12
FIGURE CAPTIONS

Fig.1 Appearance of the plates friction-stir-welded under water

Fig.2 Weld map of non-porous FSW of 6013 to AZ31 performed under water
Fig.3 EPMA image and distribution maps of major elements Mg and Al of mixture structure:(a)
EPMA image; (b) the distribution map of Mg; (c) the distribution map of Al
Fig.4 Detail of the band of the mixing structure of the weld zone:(a)low magnification, (b)enlarged
scale
Fig.5 Cross-sectional SEM images and EDS line analysis of Al/Mg interface

Fig.6 Microhardness profiles of microstructure from Mg to Al with different locations

Fig.7 Fracture location in tensile specimen and SEM images of fracture surface
(a) Fracture location of the specimen
(b) Low magnification image of the fracture surface of the Al side
(c) High magnification image of the crown section
(d) High magnification image of the bottom section
(e) High magnification image of the middle section
(f) High magnification image of the crown section
Fig.8 X-ray diffraction patterns of the fracture surface of 6013 alloy side
Fig.9 X-ray diffraction patterns of the fracture surface of AZ31 Mg alloy side

13
Highlights:
Aluminum and magnesium alloys were joined by underwater friction stir welding.

Underwater FSW was conducted to improve properties of joint with lower heat input.

Microstructures and mechanical properties of dissimilar joint were investigated.

Intermetallic compounds developed in the fracture interface were analyzed.

Fracture features of the tensile samples were analyzed.

14
 Table 1 Chemical compositions and mechanical properties of experimental materials

Metal Chemical composition (wt,%) UTS/MPa

Al Mg Mn Cu Si Zn
Al 6013 Bal. 0.90 0.21 0.90 0.73 - 385
Mg AZ31 3.74 Bal. 0.29 - 0.02 0.75 241

15
 Table 2. EDS analysis of Al and Mg elements at different locations in the weld zone(wt,%)

Locations Al Mg
c 92.24 7.76

d 68.62 31.38
e 8.47 91.53

16
Fig.1

Fig.1 Appearance of the plates friction-stir-welded under water

Fig.2

Fig.2 Weld map of non-porous FSW of 6013 to AZ31 performed under water
Fig.3

Fig.3 EPMA image and distribution maps of major elements Mg and Al of mixture
structure:(a) EPMA image; (b) the distribution map of Mg; (c) the distribution map of
Al
Fig.4

Fig.4 Detail of the band of the mixing structure of the weld zone:
(a)low magnification, (b)enlarged scale
Fig.5

Fig.5 Cross-sectional SEM images and EDS line analysis of Al/Mg interface
Fig.6

Fig.6 Microhardness profiles of microstructure from Mg to Al with different

locations
Fig.7

Fig.7 Fracture location in tensile specimen and SEM images of fracture surface
(a) Fracture location of the specimen
(b) Low magnification image of the fracture surface of the Al side
(c) High magnification image of the crown section
(d) High magnification image of the bottom section
(e) High magnification image of the middle section
(f) High magnification image of the crown section
Fig.8

Fig.8 X-ray diffraction patterns of the fracture surface of 6013 alloy side
Fig.9

Fig.9 X-ray diffraction patterns of the fracture surface of AZ31 Mg alloy side