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National Technical University of Athens, School of Chemical Engineering, 9 Heroon Polytechniou Str., Zografos, Athens GR-157 80, Greece
Sol-Gel Laboratory, IMS, NCSR DEMOKRITOS, 15310 Agia Paraskevi, Greece
a r t i c l e
i n f o
Article history:
Received 19 November 2011
Received in revised form 30 January 2012
Accepted 31 January 2012
Available online 8 February 2012
Keywords:
Nanoindentation
Aluminum alloys
Friction stir welding
Residual stress
a b s t r a c t
Residual stress during Friction Stir Welding (FSW) of lightweight alloys is of major concern, due to their
functionality and applications in transport and industry elds. Several conventional techniques which
are used to measure and characterize welded aluminum alloys are destructive. This drawback has raised
nanoindentation as the non-destructive alternative technique with many advantages, such as easy preparation and high spatial resolution. In this study a methodology was brought forward to investigate the
applicability of nanoindentation method in order to overcome limitations of this technique and measure
residual stress in two of most commonly used aluminum alloys in transport and industrial applications.
2012 Elsevier B.V. All rights reserved.
1. Introduction
In transport and industrial applications the lightweight alloys
undergo signicant mechanical loads under different applied loads
and time dependent conditions. More specically, high-demanding
mechanical properties and high accuracy to strength-to-weight
ratio of such materials have led to an increased research. Aluminum
alloys offer a high potential for weight reduction in automotive
and other transportation vehicle construction. Aluminum alloy
AA6082-T6 (AA: provided by the Aluminum Association) is a
high-strength AlMgSi alloy containing manganese to increase
ductility and toughness. The T6 condition is obtained through
articial ageing at a temperature of 170200 C, mainly for
welding applications [1]. Aluminum alloy AA5083-H111 is an
AlMg alloy which can be classied as wrought alloy product with excellent corrosion resistance. The H111 condition is
obtained through both cold hardening and partial annealing. In
particular, both alloys are often applied in shipbuilding industry
[2].
The increasing relevance of aluminum alloys in transportation
requires research on more efcient and reliable joining processes.
Friction Stir Welding (FSW) is a solid-state joining process, which
emerged as an alternative technique to be used in high strength
alloys that were difcult to join with conventional joining techniques. This welding process was initially developed for aluminum
alloys, but since then FSW has also been utilized on joining a large
range of materials. In FSW the interaction of a non-consumable and
rotating tool with the work pieces being welded creates a welded
joint through frictional heating and plastic deformation at temperatures below the melting temperature of the alloys being joined.
The contacting shoulder applies frictional heat to the weld region
and prevents highly plasticized material from being expelled during the welding operation. The combined frictional heat from the
pin and the shoulder creates a plasticized condition around the
immersed pin and the contacting surface of the shouldered region
of the work piece top surface. Material ows around the tool and
coalesces behind it while relative traverse between substrate and
the rotating tool occurs. Notwithstanding the widespread interest
in the possibilities offered by FSW, data concerning the mechanical behavior of joints obtained using this process is still scarce.
The heat input (most of it generated by the friction between
tool shoulder and materials to be joined) increases by increasing tool rotational speed and by decreasing welding speed. Low
heat input causes the intermittent material ow and improper stirring action around the tool pin due to insufcient plasticization
of the materials under the tool shoulder. On the other side, high
heat input causes turbulent material ow around the tool pin due
to excess plasticization of material under the tool shoulder. Further details and analysis of the process are reported elsewhere
[3].
The frequent failure of structural components by time dependent degradation in severe operating environments has recently
become a concern. In particular, pipeline operating conditions are made more severe by cryogenic contents and many
C.A. Charitidis et al. / Materials Science and Engineering A 540 (2012) 226234
227
Fig. 1. Geometry of FSW process, also indicating the tool transverse direction and
cross section region.
2. Experimental details
2.1. Materials used and welding conditions
Single-pass friction stir square butt joint welds were produced
using a tool (Fig. 1) made from heat treated steel; the necessary
clamping arrangement of the specimens to be welded was also
designed and manufactured. The welding direction was parallel
to the rolling direction of the plates whereas no inclination angle
concerning the welding tool was used. The welding process was
performed with rotating of the tool at 375 rpm and at a feed rate of
85 mm/min. These optimum conditions were obtained from a large
number of welding procedures [11].
Table 1
Composition of both aluminum alloys in weight percent through EDAX analysis.
Element
Si
Fe
Cu
Mn
Mg
Zn
Ti
Cr
Al
1.13
0.34
0.30
0.56
97.67
0.22
0.26
0.61
4.95
0.20
0.14
93.63
228
C.A. Charitidis et al. / Materials Science and Engineering A 540 (2012) 226234
1000
(a)
Al<200>
800
AA 6082-T6
base metal
2 4
23
3 5 6
5 7
Load ()
1000
750
AlFeSi
Al6Mn
50
60
70
80
3 (-3) cm (1)
-1.5 cm (2)
-1 cm
(3)
-0.8 cm (4)
0 cm
(5)
0.5 cm (6)
1.3 cm (7)
1250
500
250
0
40
2 cm
1500
-Mg2Si
-Al12(Fe,Mn)3Si
Intensity
200
2000
1750
600
400
(a)
90
100
110
2 Theta / degree
20
40
60
80
100
120
140
160
180
200
180
200
Displacement (nm)
Al<200>
1000
Al<111>
(b)
(b)
800
AlFeSi
4 5 6
23
2250
2000
20 mm
1750
Load (N)
-Mg2Si
-Al12(Fe,Mn)3Si
-15.5 mm (1)
-10 mm (2)
- 8mm (3)
0 mm
(4)
4 mm
(5)
11 mm (6)
1500
1250
1000
Al6Mn
Intensity
600
200
2500
AA 6082-T6
welding zone
400
2750
750
500
250
40
50
60
70
80
90
100
110
2 Theta / degree
20
40
60
80
100
120
140
160
Displacement (nm)
Fig. 2. XRD analysis in diffractogram form of base metal and welding zone for
AA6082-T6.
3. Analytical modeling
3.1. Nanoindentation analysis
Nanoindentation testing was performed with Hysitron TriboLab Nanomechanical Test Instrument. Details about the instrument
and the experimental setup have been presented elsewhere [2].
The surface of the samples was prepared by grinding and polishing
(with 1 and 0.1 m agglomerated -alumina suspension). Based
Compressive
stress state
Load ()
LC
Tensile
stress state
L0
S
Er =
(1)
2 Ac
where S is the unloading stiffness (initial slope of the unloading
load-displacement curve at the maximum displacement of penetration (or peak load)), Ac is the projected contact area between the
tip and the substrate and is a constant that depends on the geometry of the indenter ( = 1.167 for Berkovich tip) [3,4]. Conventional
nanoindentation hardness refers to the mean contact pressure; this
hardness, which is the contact hardness, (Hc ), is actually dependent
upon the geometry of the indenter (Eqs. (2)(4)).
Hc =
F
Ac
(2)
where
LT
1/2
+ + a1/16 hc
1/16
(3)
and
Displacement (nm)
Fig. 3. Typical nanoindentation load-displacement curves for different stress states.
hc = hm
Pm
Sm
(4)
C.A. Charitidis et al. / Materials Science and Engineering A 540 (2012) 226234
(a)
2500
2250
1 2
2000
45
1750
Load (N)
229
2 cm
-2 cm
-1 cm
0 cm
1 cm
1.2 cm
3 cm
1500
1250
1000
(1)
(2)
(3)
(4)
(5)
(6)
750
500
250
0
0
20
40
60
80
100
120
140
160
180
200
Displacement (nm)
(b)
2000
2 3 4 5 6
1750
1500
20 mm
Load ()
1250
-15.5 mm
-10.5 mm
-8.5 mm
0 mm
4.5 mm
8.5 mm
1000
750
(1)
(2)
(3)
(4)
(5)
(6)
500
250
0
0
20
40
60
80
100
120
140
160
180
200
Displacement (nm)
Fig. 5. Nanoindentation load-displacement curves at 200 nm indentation depth for (a) the AA 6082-T6 aluminum alloy and for (b) the AA 5083-H111 aluminum alloy (cross
section). Hatched area indicates the welding zone.
shear deviator stress D . The surface-normal deviator stress in zdirection (normal to the surface of indentation) zD is 2res /3 by
removing the hydrostatic stress 2res /3 from the surface residual stress res and is added to the contact pressure [9]. LT L0 is
dened as a product of the selected deviator stress component and
its corresponding contact area ATC . Thus, an equation for the equibiaxial residual stress is derived in terms of the indentation load and
contact area as:
res = 3
(L0 LT )
2ATC
(5)
Here, ATC in the tensile stress state is calculated from LT A0C /L0
because the contact hardness Hc or L0 /A0C = LT /ATC is independent
of the elastic residual stress. This measurement is based on the initial elastic unloading part of the load-displacement curve which is
unaffected by the residual stresses for materials with isotropic or
230
C.A. Charitidis et al. / Materials Science and Engineering A 540 (2012) 226234
(a)
1000
(a)
Welding zone
AA6082-T6
Welding zone
AA6082-T6
Retreating side
Advancing side
Retreating side
Advancing side
800
400
600
600
400
200
200
-200
0
-400
-6
-5
-4
-3
-2
-1
-4
-3
-2
3000
AA5083-H111
2500
(b)
Welding zone
AA5083-H111
Welding zone
Retreating side
Advancing side
2000
1000
Retreating side
Advancing side
(b)
-1
1500
1000
500
500
-500
0
-500
-1000
-8
-4
12
16
20
24
-24
(6)
3(L0 LT )
(1 + p)ATC
-16
-12
-8
-4
12
16
20
24
Fig. 6. Residual stress distribution for (a) the AA 6082-T6 aluminum alloy and for (b)
the AA 5083-H111 aluminum alloy (transverse). Hatched area indicates the welding
zone.
zD =
-20
(7)
Lee and Kwon [25] showed the validity of (5) by empirical indentation tests on biaxially strained specimens. The stress ratio became
Fig. 7. Residual stress distribution for (a) the AA 6082-T6 aluminum alloy and for
(b) the AA 5083-H111 aluminum alloy (cross section). Hatched area indicates the
welding zone.
C.A. Charitidis et al. / Materials Science and Engineering A 540 (2012) 226234
120
Welding zone
AA6082-T6
100
80
90
60
40
2.0
Hnano (GPa)
AA5083-H111
AA6082-T6
y=55.25x-6.71
110
100
Hmicro (HV0.3)
Hmicro (HV0.3)
(a)
231
1.8
80
70
1.6
60
1.4
1.2
50
1.0
-5
-4
-3
-2
-1
Hnano (GPa)
Hmicro (HV0.3)
(b)
90
1.0
1.2
1.4
1.6
1.8
2.0
2.2
Hnano (GPa)
Welding zone
AA5083-H111
80
70
60
1.8
1.6
1.4
1.2
1.0
0.8
0.6
0.4
0.2
0.0
-16 -14 -12 -10 -8
-6
-4
-2
10 12 14 16
propagate downward and toward the surface as the loading continues and then the crack becomes unstable [32].
In the measured residual stresses shown in Fig. 6(a) for AA6082T6 the stresses appear to rise to a tensile stress of 800 MPa at
1 cm from the center, before reversing in trend to form a tensile region near the weld line of about 600 MPa. It can be seen
that this tensile region peaks at around 1 cm from the weld line,
a distance corresponding to the edge of the tool shoulder, before
dropping slightly at the weld centre as it is shown in Fig. 6(a). Also,
in the measured residual stresses shown in Fig. 6(b) for AA5083H111 the stresses from the parent material to the welding zone
appear to decrease linearly to a compressive stress steady state of
Fig. 10. Pile-up of aluminum (a) AA 6082-T6 [3] and (b) AA 5083 alloys through
SPM imaging.
232
C.A. Charitidis et al. / Materials Science and Engineering A 540 (2012) 226234
(a)
hc/hm
AA6082-T6
AA5083-H111
100
10
1000
(b)
10
hc/hm
Displacement, hm (nm)
AA6082-T6
AA5083-H111
0.1
0.015
0.02
0.025
0.03
0.035
H/E*
Fig. 11. Normalized pile-up/sink-in height for both alloys.
about 500 MPa near the weld line. This form of prole has been
observed previously for aluminum AA5083-H111 by Peel et al. [29].
The dip around the pin position may be attributed to the high
temperatures associated with this region, which would limit the
capacity of the material to support the generated load. Alternatively, it could be a consequence of stress relief that occurred when
the plate was cut up. For both alloys, a small plateau region appears
near the welding line; yet, the peak stresses are much higher in the
case of AA5083-H111.
In the measured residual stresses shown in Fig. 7(a) for AA6082T6 the stresses appear to rise to a tensile stress of 250 MPa at 1 cm
from the center, before reversing in trend to form a compressive
region near the weld line. It can be seen that this tensile region
peaks at around 1 cm from the weld line, a distance corresponding to the edge of the tool shoulder, before dropping slightly at
the weld centre. Also, in the measured residual stresses shown in
Fig. 7(b) for AA5083-H111 the stresses appear to decrease linearly
to a compressive stress steady state of about 500 MPa near the
weld line.
(8)
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