Materials Science and Engineering A 540 (2012) 226234

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Materials Science and Engineering A

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Residual stress and deformation mechanism of friction stir welded aluminum

alloys by nanoindentation
C.A. Charitidis a, , D.A. Dragatogiannis a , E.P. Koumoulos a , I.A. Kartsonakis a,b
a
National Technical University of Athens, School of Chemical Engineering, 9 Heroon Polytechniou Str., Zografos, Athens GR-157 80, Greece
b
Sol-Gel Laboratory, IMS, NCSR DEMOKRITOS, 15310 Agia Paraskevi, Greece

a r t i c l e i n f o a b s t r a c t

Article history: Residual stress during Friction Stir Welding (FSW) of lightweight alloys is of major concern, due to their
Received 19 November 2011 functionality and applications in transport and industry elds. Several conventional techniques which
Received in revised form 30 January 2012 are used to measure and characterize welded aluminum alloys are destructive. This drawback has raised
Accepted 31 January 2012
nanoindentation as the non-destructive alternative technique with many advantages, such as easy prepa-
Available online 8 February 2012
ration 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
Keywords:
residual stress in two of most commonly used aluminum alloys in transport and industrial applications.
Nanoindentation
Aluminum alloys 2012 Elsevier B.V. All rights reserved.
Friction stir welding
Residual stress

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 prod-
uct 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 tech-
niques. This welding process was initially developed for aluminum
Corresponding author. Tel.: +30 2107724046; fax: +30 2107722339.
E-mail address: charitidis@chemeng.ntua.gr (C.A. Charitidis).
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 temper-
atures 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 dur-
ing 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 mechan-
ical 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 increas-
ing tool rotational speed and by decreasing welding speed. Low
heat input causes the intermittent material ow and improper stir-
ring 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. Fur-
ther details and analysis of the process are reported elsewhere
[3].
The frequent failure of structural components by time depen-
dent degradation in severe operating environments has recently
become a concern. In particular, pipeline operating condi-
tions are made more severe by cryogenic contents and many

0921-5093/$ see front matter 2012 Elsevier B.V. All rights reserved.
doi:10.1016/j.msea.2012.01.129
 C.A. Charitidis et al. / Materials Science and Engineering A 540 (2012) 226234 227

inhomogeneous welded joints, so that the welded joint is typically

the initiation point of fracture because of the microstructural and
mechanical inhomogeneities [4]. Thus safety assessment based
on precise mechanical properties of local regions is indispensable.
One of the challenges in studying the local mechanical properties
in a small volume of welded materials having microstructural
gradients is that the traditional methods, e.g. tensile test and
microhardness test, need bulky standard samples to evaluate
the mechanical behavior of materials and as a consequence are
not applicable, contrary to nanoindentation. In general conven-
tional nondestructive techniques for welding residual stress
measurement have many disadvantages in this eld because of
poor repeatability, large scatter in data, complex procedures,
Fig. 1. Geometry of FSW process, also indicating the tool transverse direction and
inaccurate results, etc. [5]. For instance, it is almost impossible
cross section region.
to use non-destructive methods to assess residual stresses in
weldments including heat-affected zones (HAZs), which have
very rapid microstructural gradients [4]. Also materials such as
2. Experimental details
high strength steel (e.g. HQ130 steel) are highly amenable to
crack formation during welding so with the normally available
2.1. Materials used and welding conditions
instrumentation and measuring facilities, it is quite difcult to nd
out the instantaneous residual stress in the weld zone [6].
Single-pass friction stir square butt joint welds were produced
OliverPharr (O&P) analysis for nanoindentation has proven to
using a tool (Fig. 1) made from heat treated steel; the necessary
be an effective and convenient method of determining the mechan-
clamping arrangement of the specimens to be welded was also
ical properties of solids, most notably elastic modulus (E) and
designed and manufactured. The welding direction was parallel
hardness (H) [7]. The method relies on the analysis of the ini-
to the rolling direction of the plates whereas no inclination angle
tial slope of the unloading load-displacement response which is
concerning the welding tool was used. The welding process was
assumed to be elastic, even if the contact is elasticplastic.
performed with rotating of the tool at 375 rpm and at a feed rate of
Recently, residual stress determination using the analytical
85 mm/min. These optimum conditions were obtained from a large
methods based on nanoindentation technique has attracted exten-
number of welding procedures [11].
sive attention. A general methodology to obtain residual stress from
nanoindentation based on the analysis of contact area difference
between a residual stress-free material and the same material with 2.2. Microstructural characterization
residual stress is proposed from Suresh and Giannakopoulos [8]. A
stress-analysis technique for sharp nanoindentation by considering The chemical composition of AA6082-T6 (high SiMg containing
the stress interaction between the residual stress and the contact aluminum alloy) and AA5083-H111 (high Mg containing aluminum
pressure from the viewpoint of the shear plasticity is explored by alloy) are listed in Table 1, determined by SEM using a PHILIPS
Lee and Kwon [9]. It is also known for various alloys, that inter- Quanta Inspect (FEI Company) microscope with W (tungsted) l-
nal uniaxial or biaxial stresses affect nanomechanical measurement ament 25 kV equipped with EDAX GENESIS (Ametex Process and
results, proved experimentally as well as by nite element simula- Analytical Instruments).
tion [10]. Qualitative analysis of the microstructure components of
Residual stress plays an important role in mechanics of materi- AA6082-T6 alloy was performed by X-ray diffraction (XRD) using
als as it is a key quantity for the mechanical behavior and lifetime a Powder diffractometer (SIEMENS D-500 equipped with a CuK
of constructions, especially for welded materials in which welded lamp with wavelength of 1.5418 A). The results of XRD analysis in
joint is related with the fatigue crack propagation (residual stress diffractogram form is shown in Fig. 2(a) and (b).
state can have a large impact on the lifetime of the weld). The For as-cast magnesium alloy, the coarse -Mg phase and -
evaluation of residual stress based on nanoindentation methods is Al12 Mg17 intermetallic compound disappeared after FSW [1214].
essential, as the instrumented indentation is widely used to probe Further, Nakata et al. [12], Lee et al. [14], and Park et al. [15] reported
mechanical properties of small scales and further mechanical char- that the grain size in the weld nugget became larger with increasing
acterization. In order to estimate the effect of residual stresses and tool rotation rate and decreasing traverse speed due to increasing
develop models for its description, to the comparison of inden- heat input, which promoted the growth of recrystallized grains.
tation depth, indentation force, unloading behavior, contact area, This observation is consistent with that in FSW aluminum alloys
pile-up or hardness with and without residual stress is essential. [1621].
For all the aforementioned reasons evaluation of residual stress on
welded structures by nanoindentation poses a complex mechanical
system.
Table 1
This work emphasizes on analysis of the precise determina- Composition of both aluminum alloys in weight percent through EDAX analysis.
tion of true contact area during nanoindentation which is crucial
Element AA6082-T6 (%, w/w) AA5083-H111 (%, w/w)
to making accurate residual stress determination. The common
used O&P method assumes that the contact periphery between Si 1.13
indenter and material sinks in, which limits its application to Fe 0.34 0.22
Cu 0.26
materials that pile-up. It is clearly shown through Scanning Probe Mn 0.30 0.61
Microscopy (SPM) that pile-up during nanoindentation of AA 5083- Mg 0.56 4.95
H111 alloy is negligible in contrast with AA6082-T6, where the Zn 0.20
resultant pile-up is signicant. The residual stresses in AA 6082- Ti
Cr 0.14
T6 and AA5083-H111 aluminum alloys were determined by the
Al 97.67 93.63
nanoindentation method.
228 C.A. Charitidis et al. / Materials Science and Engineering A 540 (2012) 226234

1000
(a) Advancing side (-) Retreating side (+)
(a)

Al<200>
Al<111>
2000
800
1 23
2 4 5 7
3 5 6 1
AA 6082-T6
1750
base metal
1500 2 cm
600
3 (-3) cm (1)
Intensity

1250 -1.5 cm (2)

Load ()
-Al12(Fe,Mn)3Si

-1 cm (3)
400 1000 -0.8 cm (4)
0 cm (5)
0.5 cm (6)
-Mg2Si

750
1.3 cm (7)
200

AlFeSi
Al6Mn
500

250
0

40 50 60 70 80 90 100 110 0
0 20 40 60 80 100 120 140 160 180 200
2 Theta / degree
Displacement (nm)
1000
(b)
Al<200>
Al<111>

Advancing side (-) Retreating side (+)

(b) 2750

800
AA 6082-T6
2500
1 23 4 5 6 1
AlFeSi

2250
welding zone
600 2000
20 mm
Intensity

1750
-Al12(Fe,Mn)3Si

-15.5 mm (1)

Load (N)
1500 -10 mm (2)
400 - 8mm (3)
1250 0 mm (4)
-Mg2Si

4 mm (5)
1000
Al6Mn

200 11 mm (6)
750

500
0
250
40 50 60 70 80 90 100 110
0
2 Theta / degree 0 20 40 60 80 100 120 140 160 180 200
Displacement (nm)
Fig. 2. XRD analysis in diffractogram form of base metal and welding zone for
AA6082-T6. Fig. 4. 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
(transverse). Hatched area indicates the welding zone.
3. Analytical modeling

3.1. Nanoindentation analysis on the half-space elastic deformation theory, H and E values can be
extracted from the experimental data (load displacement curves)
Nanoindentation testing was performed with Hysitron Tribo- using the O&P method [7], where derived expressions for calculat-
Lab Nanomechanical Test Instrument. Details about the instrument ing the elastic modulus from indentation experiments are based on
and the experimental setup have been presented elsewhere [2]. Sneddons elastic contact theory [22]:
The surface of the samples was prepared by grinding and polishing
(with 1 and 0.1 m agglomerated -alumina suspension). Based S 
Er =  (1)
2 Ac

Compressive Stress free state where S is the unloading stiffness (initial slope of the unloading
stress state load-displacement curve at the maximum displacement of pene-
LC tration (or peak load)), Ac is the projected contact area between the
tip and the substrate and is a constant that depends on the geom-
etry of the indenter ( = 1.167 for Berkovich tip) [3,4]. Conventional
nanoindentation hardness refers to the mean contact pressure; this
Tensile
Load ()

hardness, which is the contact hardness, (Hc ), is actually dependent

stress state
upon the geometry of the indenter (Eqs. (2)(4)).
L0 F
Hc = (2)
Ac

LT where
2 1/2 1/16
A(hc ) = 24.5hc + a1 hc + a1/2 hc + + a1/16 hc (3)

and
Displacement (nm)
Pm
hc = hm (4)
Fig. 3. Typical nanoindentation load-displacement curves for different stress states. Sm
 C.A. Charitidis et al. / Materials Science and Engineering A 540 (2012) 226234 229

Advancing side (-) Retreating side (+)

(a) 2500

2250

2000
1 2 3 45 6
1750
2 cm
1500 -2 cm (1)

Load (N)
-1 cm (2)
1250 0 cm (3)
1 cm (4)
1000 1.2 cm (5)
3 cm (6)
750

500

250

0
0 20 40 60 80 100 120 140 160 180 200
Displacement (nm)

Advancing side (-) Retreating side (+)

(b) 2000

1750
1 2 3 4 5 6 1
1500
20 mm
1250 -15.5 mm (1)
Load ()

-10.5 mm (2)
1000 -8.5 mm (3)
0 mm (4)
4.5 mm (5)
750
8.5 mm (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.

where hm is the total penetration displacement of the indenter at
peak load, Pm is the peak load at the indenter displacement hm ,
and is an indenter geometry constant, equal to 0.75 for Berkovich
indenter [23].
3.2. Residual stress measured by nanoindentation
A surface residual stress is assumed to be in an equibiaxial ten-
sile state and uniform in the near-surface region (taken as about
three times the indentation depth) [8,9]. If an arbitrary indentation
state (ht , L0 ) is attained in an unstressed state and if the tensile
inplane stress res is applied to the loading state at a xed pen-
etration depth ht , the indentation load L0 is reduced to a load LT
due to the decrease in surface penetration resistance (in Fig. 3 typ-
ical nanoindentation load-displacement curves for different stress
states are presented). The stress tensor is separated into mean
stress  M (hydrostatic stress) and plastic-deformation-sensitive
shear deviator stress  D . The surface-normal deviator stress in z-
direction (normal to the surface of indentation) zD is 2res /3 by
removing the hydrostatic stress 2res /3 from the surface resid-
ual 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 equibi-
axial residual stress is derived in terms of the indentation load and
contact area as:
(L0 LT )
res = 3 (5)
2ATC
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 ini-
tial 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

1000 600
(a) AA6082-T6 Welding zone (a) AA6082-T6 Welding zone
Advancing side Retreating side Advancing side Retreating side
800 400

Residual Stress (MPa)

Residual Stress (MPa)

600
200

400
0

200
-200

0
-400
-6 -5 -4 -3 -2 -1 0 1 2 3 4 5 6 -4 -3 -2 -1 0 1 2 3 4

Distance from weld center (cm) Distance from weld center (cm)

3000
(b) AA5083-H111 Welding zone (b) 1000
AA5083-H111 Welding zone
Advancing side Retreating side Advancing side Retreating side
2500

500

Residual Stress (MPa)

2000
Residual Stress (MPa)

1500
0
1000

500
-500

-500 -1000
-24 -20 -16 -12 -8 -4 0 4 8 12 16 20 24 -24 -20 -16 -12 -8 -4 0 4 8 12 16 20 24
Distance from weld center (mm) Distance from weld center (mm)

Fig. 6. Residual stress distribution for (a) the AA 6082-T6 aluminum alloy and for (b) Fig. 7. Residual stress distribution for (a) the AA 6082-T6 aluminum alloy and for
the AA 5083-H111 aluminum alloy (transverse). Hatched area indicates the welding (b) the AA 5083-H111 aluminum alloy (cross section). Hatched area indicates the
zone. welding zone.

no strain hardening [8]. In order to measure the actual contact area

A0C with pile-up or sink-in information from an O&P curve analysis,
prior to indentation, an empirical calibration for instrumental stiff-
ness and the area function of the indenter tip was performed by
making preliminary indentation tests on a fused silica, a standard
material for this purpose [3].
This model presented below is applicable in the specic stress
state of equibiaxial tensile or compressive state. This impedes wide
application of the instrumented indentation technique to complex
biaxial stress states in actual structures [24]. In order to analyze
general stress states this model needs modication. If we denote
one major stress component of the biaxial residual stress as res,x
and the other as a minor stress component res,y then res,y can
be expressed as pres,x using the stress ratio p or res,y /res,x . The
inuence of biaxial stress on the indentation plasticity also can
be analyzed through a similar hydrostatic-stress-removal method.
The deformation -sensitive deviator stress component is given as
(1 + p)res,x
zD =
3 to the weld zone. As a result, residual stresses measurements are
in this case. Thus, if information on p is given, individual principal
stresses can be calculated from the instrumented indentation test
using (7).
3(L0 LT )
res,x =
(1 + p)ATC
Lee and Kwon [25] showed the validity of (5) by empirical inden-
tation tests on biaxially strained specimens. The stress ratio became
an important issue in stress characterization, and Underwoods
observation of a nonsymmetrical contact deformation in uniaxial
stress [26] supplied a clue to extracting the surface stress direction-
ality. Lee et al. [27] tried to estimate the stress ratio by analyzing
the pile-up heights along the two principal biaxial stress axes. The
ratio of stress-induced pile-up shifts was linearly proportional to
the stress ratio. Several preliminary observations on the welded
joints yielded a stress ratio of about 0.33, and this value was used
in subsequent biaxial stress analyses [28].
4. Results and discussion
4.1. Residual stress distribution across the friction stir-welded
joint
According to the geometry of the welding process, the largest
(6) stresses are expected parallel to the welding direction and close
focused on this region [29]. The instrumented nanoindentation
curves of AA 6082-T6 and AA 5083-H111 for the different regions
across the friction stir welded joint including the HAZ, the thermo
mechanical affected zone (TMAZ), the base metal (BM) and the
(7) reference curve far away from the welded joint is presented in
Figs. 4 and 5, for transverse and cross section respectively. The load
decreased due to surface stress at given indentation depth means
that the residual stress has positive sign (tensile). On the other hand,
 C.A. Charitidis et al. / Materials Science and Engineering A 540 (2012) 226234 231

120
(a) AA6082-T6 Welding zone 110
AA5083-H111
AA6082-T6
100
y=55.25x-6.71
Hmicro (HV0.3)

100
80

60 90

Hmicro (HV0.3)
40 80
2.0

1.8 70
Hnano (GPa)

1.6
60
1.4

1.2
50
1.0
-5 -4 -3 -2 -1 0 1 2 3 4 5
1.0 1.2 1.4 1.6 1.8 2.0 2.2
Distance from weld center (cm)
Hnano (GPa)
(b) AA5083-H111 Welding zone
90
Fig. 9. Distribution of micro- and nano-hardness for both alloys [43].
Hmicro (HV0.3)

80
propagate downward and toward the surface as the loading con-
70 tinues and then the crack becomes unstable [32].
In the measured residual stresses shown in Fig. 6(a) for AA6082-
60 T6 the stresses appear to rise to a tensile stress of 800 MPa at
1.8 1 cm from the center, before reversing in trend to form a ten-
1.6
1.4
sile 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,
Hnano (GPa)

1.2
1.0 a distance corresponding to the edge of the tool shoulder, before
0.8
dropping slightly at the weld centre as it is shown in Fig. 6(a). Also,
0.6
0.4 in the measured residual stresses shown in Fig. 6(b) for AA5083-
0.2 H111 the stresses from the parent material to the welding zone
0.0 appear to decrease linearly to a compressive stress steady state of
-16 -14 -12 -10 -8 -6 -4 -2 0 2 4 6 8 10 12 14 16
Distance from weld center (mm)

Fig. 8. Transverse distribution (comparison) of Hmicro and Hnano for both alloys (a)
AA 6082-T6 and (b) AA 5083-H111. Hatched area indicates the welding zone [43].

the load increased due to surface stress at given indentation depth

means that the residual stress has negative sign (compressive).
Fig. 6 shows the transverse stresses within the weld as a func-
tion of distance from the weld line. The distribution of residual
stresses measured by nanoindentation is in agreement with the
distribution measured by other researchers [29] based on X-ray
method. The weld zone is under tension and the parent mate-
rial far away from the weld zone is under compression. The strain
elds associated with individual dislocations result in broadening
as can short range stresses caused by the dislocation arrays and
sub-grain boundaries of the type commonly found in the parent
material. Both of these factors affect peak width due to the dif-
ferent grain sizes, the number of subgrains and their size and the
differences in dislocation densities in the parent material and the
weld zone.
Fig. 7 shows the residual stresses in a plane perpendicular
to welding direction which is dened as cross section; the peak
stresses are somewhat lower than in the transverse direction for
both alloys.
The loaddisplacement curves for all applied loads exhibit many
discontinuities (Figs. 5 and 6), especially for the case of AA5083-
H111 cross section (Fig. 6b), where a sudden increase in the
displacement is revealed in the loading part without any appre-
ciable change in the load. This phenomenon is called pop-in
behavior, noticed in many brittle thin lms due to the cracking and
chipping events [30,31]. The pop-in phenomenon in the loaddepth
curves generated by Berkovich indenter suggests that a crack Fig. 10. Pile-up of aluminum (a) AA 6082-T6 [3] and (b) AA 5083 alloys through
begins growing at the very early stage of the loading, continues to SPM imaging.
232 C.A. Charitidis et al. / Materials Science and Engineering A 540 (2012) 226234

(a)

hc/hm

AA6082-T6
AA5083-H111

10 100 1000
Displacement, hm (nm)

10
(b)
hc/hm

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. Alterna-
tively, 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 AA6082-
T6 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 correspond-
ing 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.
4.2. Nano- and micro-hardness distribution across the weld for
both alloys
Transverse distribution of Hmicro and Hnano presented the same
shape [3,33] and the same decrease of values between base metal
and welding zone (20% for AA5083 and 33% for AA6082), as
shown in Fig. 8.
In Fig. 9 the distribution of micro- and nano-hardness for both
alloys is presented. The linear regression equation for this relation-
ship is:
Hmicro (HV ) = 55.26 Hnano (GPa) 7.28 (8)
where Hmicro represents the microhardness and Hnano represents
the nanohardness.
The square of the correlation coefcient R2 for (8) is 90, indi-
cating that approximately 90% of the total variation is explained by
this linear regression equation. The Vickers and Berkovich inden-
ters have similar geometric effects on indentation geometry, so it
is reasonable that Vickers testing and nanoindentation Hc values
 C.A. Charitidis et al. / Materials Science and Engineering A 540 (2012) 226234
exhibit reasonable statistical relationship. The indentation shape
produced by the Berkovich indenter (used for the Hnano tests in this
study), is designed to be similar to the indentation created by the
Vickers indenter. The experimental results show that Hnano results
from a nanomechanical test instrument with a Berkovich indenter
can be reliably compared with Hmicro (Vickers) test results. Thus,
the selection of an appropriate H test should be based on the prob-
lem being investigated. The results of this investigation show that
Hnano test results from a nanomechanical test instrument with a
Berkovich indenter can be used to reliably analyze Hnano distribu-
tion on a friction stir welded alloy. The enhancement of elasticity
for weaker loads may be a real physical effect of superelastic behav-
ior of materials under mN scale forces [34], due to the inactivation
of dislocations. It may also be an artefact due to the piling-up of the
surface during indentation.
4.3. Pile-up/sink-in deformation
The contact area is inuenced by the formation of pile-ups
and sink-ins during the indentation process. To accurately mea-
sure the indentation contact area, pile-ups/sinks-ins should be
appropriately accounted for. The presence of creep during nanoin-
dentation has an effect on pile-up, which results in incorrect
measurement of the material properties. FischerCripps observed
this behaviour in aluminum where the measured elastic modu-
lus was much less than expected [35]. Rar et al. [36] observed
that the same material when allowed to creep for a long dura-
tion produced a higher value of pile-up/sink-in indicating a switch
from an initial elastic sink-in to a plastic pile-up [36]. Creep-
ing time is reported to have no impact on the pile-up/sink-in of
rate sensitive aluminum alloy [37]. In Fig. 10, SPM imaging of AA
6082-T6 [3] and AA 5083 alloys for 5000 N of applied load is pre-
sented; AA 6082-T6 exhibits signicant pile-up compared to AA
5083.
In Fig. 11, the normalised pile-up/sink-in height hc /hm is plot-
ted vs. displacement hm and the normalized hardness H/E*. Higher
stresses are expected in high H/E*, hard materials, and high stress
concentrations develop towards the indenter tip, whereas in case
of low H/E*, soft materials, the stresses are lower and are dis-
tributed more evenly across the cross section of the material [35].
Rate sensitive materials experience less pile-up compared to rate
insensitive materials due strain hardening. Cheng and Cheng [38]
reported a 22% pile-up for a work hardening exponent. This is
consistent with the fact that when hc /hm approaches 1 for small
H/E*, deformation is intimately dominated by pile-up [39,40]. On
the other hand when hc /hm approaches 0 for large H/E* it corre-
sponds to purely elastic deformation and is apparently dominated
by sink-in in a manner prescribed by Hertzian contact mechanics
[41].
An advantage of extracting residual stress by nanoindentation
is that there is no prerequisite of the knowledge of the stress state
of a reference sample or any particular mechanical properties of
the test materials; nanoindentation gives the opportunity of con-
tinuous measurement of residual stress and strain based on the
continuous measurement of stiffness [42]. However, as the method
relies on an accurate determination of the hc /hm ratio and as a
consequence of the contact area, experimental factors such as sur-
face roughness, creep and pile-up may result in large error in the
experimental determination of the hc /hm ratio from the unload-
ing curve of indentation. In nanoindentation measured areas that
exhibit pile-up the contact area calculated by the O&P method will
be overestimated, which leads to an underestimation of hardness
of both free and residual stress state region. Also, many uncertain-
ties are connected with creep, since O&P method is unable to take it
into account time dependent deformation. These drawbacks pose
233
a both interesting and complicated problem for the estimation of
residual stress by nanoindentation.
5. Conclusions
Friction stir welding, contrary to classical welding techniques,
has the advantage that most of the welding parameters can be
controlled in a precise manner, thus controlling the energy input
into the system. However, the effect of different welding param-
eters on the weld properties remains an area of uncertainty. In
this work, the results of microstructural, mechanical integrity and
residual stress investigations of two friction stir welds (AA6082-T6
and AA5083-H111 aluminum alloys (in both the longitudinal (par-
allel to tool travel) and transverse (perpendicular to tool travel)
directions) produced under varying conditions), are reported. It
was found that the weld properties were dominated by the ther-
mal input rather than the mechanical deformation by the tool.
It is clearly from this work that nanoindentation could arise
like an alternative technique to estimate and describe residual
stresses distribution. It is found that residual stress distribution
in the longitudinal direction of AA5083-H111 is in agreement
in trend with classical methods such as synchrotron residual
stress analysis. Increasing the traverse speed (and hence reduc-
ing the heat input) narrows this weld zone. Further investigation
includes extended pile-up investigation and synchrotron residual
stress analysis, which is reported to indicate whether the weld
zone is in tension in both the longitudinal and transverse direc-
tions.
Acknowledgements
Authors would like to thank D.I. Pantelis and N.M. Daniolos for
providing the FSW aluminum alloys.
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