Journal of Manufacturing Processes 37 (2019) 305–320

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Journal of Manufacturing Processes

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Effect of weld thermal cycle on metallurgical and corrosion behavior of T

friction stir weld joint of AA2014 aluminium alloy
Sunil Sinhmar , Dheerendra Kumar Dwivedi
⁎

Mechanical & Industrial Engineering Department, Indian Institute of Technology Roorkee, Roorkee, 247667, Uttarakhand, India

ARTICLE INFO ABSTRACT

Keywords: Friction stir welding of AA2014 aluminium alloy was performed at seven different speed combinations. Weld
Aluminium thermal cycles were measured at all the speed parameters and corresponding peak temperatures were observed
Friction stir welding at higher tool rotation speed and lower welding speed. Hardness and tensile tests were performed to study the
Microstructure mechanical properties of the weld joints. Corrosion behavior was studied using immersion, Tafel and electro-
Hardness
chemical impedance spectroscopy tests. Optical microscopy, FESEM, XRD and transmission electron microscopy
Corrosion
were used to investigate the metallurgical behavior of the weld joints. Microhardness and corrosion resistance
were found higher at low rotation speed and high traverse speed. Corrosion behavior has been discussed in light
of microstructure.

1. Introduction of the FSW joint is determined by different process parameters like

Aluminium alloys have been broadly used in aviation and shipping
industries owing to the light weight and good strength. 2xxx series
aluminium alloys are heat treatable alloys, which gain strength from
precipitation hardening and contain copper as major alloying element
[1]. Duralumin was the first Al-Cu-Mg alloy that was used for airplane
design [2].
Friction stir welding (FSW) of the aluminium alloys eliminate the
defects like porosity, solidification cracking etc., generally produced
during the fusion welding [3]. Friction stir welding was developed at
‘The Welding Institute (UK)’ in the year of 1991 and become popular
over fusion welding processes for the welding of aluminium alloys [4].
FSW is a solid state welding technique which produces weld joint below
the melting temperature of the parent material. Different zones formed
after the friction stir welding are nugget zone/stir zone (NZ), hermos-
mechanically affected zone (TMAZ) and heat affected zone (HAZ) [5].
Fig. 1 is showing the different zones of a FSW joint of AA2014 alumi-
nium alloy. Nugget zone comprises the FSW tool pin affected region
where the actual joining occurs with the help of plastic deformation and
recrystallization. TMAZ includes the region under shoulder, adjacent to
the NZ which undergoes plastic deformation without recrystallization,
and next to TMAZ on base metal side, heat affected zone experiences
only microstructure change due to the thermal cycle of the welding.
This heterogeneity in the microstructure of various zones leads to the
different mechanical and electrochemical behavior [6]. Microstructure
rotational speed of the tool, traverse/welding speed, tool tilt angle,
dwell phase (the time for which rotating tool does not move for welding
even after the plunging), axial force, tool design etc. on the micro-
structure of FSW joint [7].
Effect of friction stir welding process parameters and tool pin profile
on the microstructure and mechanical properties of 2219 aluminium
alloy has been investigated along the thickness of the plate [8]. Effect of
different process parameters was also studied in underwater FSW and
found that the higher cooling rate of underwater FSW enhanced the
mechanical properties of the weld joint [9]. Residual stress and me-
chanical properties were studied as function of traverse speed in
AA5083 FSW joint and found that heat input during welding play big
role than the deformation take place by the tool [10]. Variation in the
mechanical properties and microstructure of the dissimilar FSW joint of
aluminium alloys were observed at different welding process para-
meters [11]. Fatigue and tensile properties were strongly affected by
the rotational-traverse speed ratio of the friction stir welding 2198 Al-Li
alloy [12]. Good quality weld of AA2024 was produced at high welding
speed of 355 mm/min using scroll shoulder and triflute pin [13]. High
tool revolving speed of 8000 rpm and traverse speed of 1500 mm/min
was used for the FSW of 0.8 mm thick sheet of AA6061 using different
types of backing plate and effect of heat input was investigated in term
of backing plate [14].
Gel visualization technique was used on the AA2024 to identify the
effect of different FSW parameters on the location of corrosion attack;

⁎
Corresponding author.
E-mail address: sun25.dme2014@iitr.ac.in (S. Sinhmar).

https://doi.org/10.1016/j.jmapro.2018.12.001
Received 25 July 2018; Received in revised form 26 October 2018; Accepted 1 December 2018
1526-6125/ © 2018 Published by Elsevier Ltd on behalf of The Society of Manufacturing Engineers.
S. Sinhmar, D.K. Dwivedi
Fig. 1. Macrostructure showing different zones formed after FSW of AA2014 at 931 rpm and 70 mm/min.
Table 1
Various rotational and traverse speeds used for FSW of AA2014.
Variation of rotational speed at constant traverse speed
Rotational speed (rpm) 508 708 931
Traverse speed (mm/min) 41 41 41
Fig. 2. Tool used for friction stir welding of AA2014.
and the role of rotational speed was found dominating [15]. Corrosion
susceptibility of the different position of the nugget zone along the
thickness was explored at various tool rotation speeds and welding
speeds and it was found that the corrosion resistance decreases with
increasing both speeds [16]. Optimum combination of the rotational
and welding speeds were established to obtain the best corrosion per-
formance of AA5052 FSW joint [17]. Increased traverse speed resulted
in the refined grains, which further improved corrosion resistance
owing to the formation of a passive film in the AA6061 FSW joint [18].
Corrosion performance of the dissimilar FSW joint was also investigated
at different welding parameters, and better corrosion resistance shown
by low heat input weld joint [19].
Furthermore, limited literature is available on the influence of weld
thermal cycle on metallurgical as well as corrosion performance of the
FSW joint. There is no literature available on the influence of weld
thermal cycle on corrosion and metallurgical behavior of the FSW joint
of AA2014 aluminium alloy to the best of knowledge of the authors.
Therefore, a systematic study of corrosion and metallurgical behavior of
AA2014 FSW joint is essential to ensure corrosion performance and
reliability during service. Present work focused on the effect of friction
stir weld thermal cycle on metallurgical and electrochemical behavior
of the AA2014 aluminium alloy weld joint using microhardness, tensile
test, immersion test, EIS (AC based test), and Tafel test (DC based test).
2. Experimental procedure
Plates of AA2014 aluminium alloy (composition wt%: Cu- 4.8, Si-
0.97, Fe- 0.7, Mn- 0.38, Mg- 0.54, Zn- 0.25) with dimensions of 70 mm
Journal of Manufacturing Processes 37 (2019) 305–320
Variation of traverse speed at constant rotational speed
1216 931 931 931 931
41 13 41 70 90
length, 27.5 mm width and 6 mm thickness were used for the FSW.
Seven combinations of different rotational and welding speeds were
used for the FSW. Four different rotational speeds were used at a con-
stant traverse speed of 41 mm/min and four different traverse speeds
were used at a constant rotational speed of 931 rpm (Table 1). A ver-
tical milling machine of 20HP, which indigenously designed was used
for the friction stir welding. FSW tool of ‘H13 steel’ with pin/probe of
Inconel material was used (Fig. 2). Details of the tool dimensions and
design are given in Table 2. Tool tilt angle used during the friction stir
welding was 1.5°. Axial force measured during the welding was 3.5 kN.
Welded plates developed using various process parameters are pre-
sented in Fig. 3. Transverse cross-sections of the weld joints are dis-
played in Fig. 4. Red circles are indicating the presence of the defect in
the weld joint. Both, low and high speeds (rotational and traverse) re-
sulted in defected weld joint. Samples welded with 708 rpm and
931 rpm at 41 mm/min produced sound weld joints.
Samples for the macro and microstructural study were cut from
transverse direction of the welds. Standard polishing procedure was
followed to obtain a mirror like surface finish for microstructure ana-
lysis and corrosion studies. Kellar’s reagent was applied for 30 s on
polished surface for etching purpose to reveal the grain boundaries.
‘Dewinter LT-23B’ optical microscope was used for the structural ana-
lysis. Matrix grain size of the weld joints was measured using line in-
tercept method. Weld thermal cycles were measured using ‘K-type’
thermocouples. Thermocouple wires could not be directly inserted in to
the nugget zone area due to the possibility of damage by rotating tool
pin, so it was kept away (5 mm) from the centerline of the weld. Second
location of thermocouple wire was kept 10 mm away to measure the
temperature of the HAZ. Thermocouples were introduced in the drilled
holes (3 mm depth and ɸ1.5 mm) from the rear side of plates. Locations
of the thermocouples are shown in schematic (Fig. 5). FE-SEM (field
emission scanning electron microscopy) was used on polished samples
before and after the corrosion testing. Phase analysis was done using
EDX (energy-dispersive X-ray spectroscopy). Existence of the secondary
phases was confirmed by ‘CuKα radiation assisted XRD (X-ray diffrac-
tion)’. Vicker’s microhardness testing instrument was used for hardness
study. Dwell phase, load and gap among two successive indentations
were 10 s, 100 g and 0.5 mm, respectively. Tensile testing was per-
formed at the transverse direction of the weld joint using universal
testing machine (Instron USA, 5980, capacity – 100 kN) at the cross
head speed of 0.5 mm/min. All the tests were executed at room tem-
perature. Dimensions used to prepare the tensile samples are shown in
Fig. 6.
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Table 2
Dimensions of the tool used for friction stir welding.
Shoulder diameter (mm) Shoulder type Pin diameter Pin type Pin length (mm) Concavity of shoulder (α)

18 Concave M6 Cylindrical (threaded) 5.7 5°

Fig. 3. Images of friction stir welded plates developed using speed parameters of (a) 508 – 41, (b) 708 – 41, (c) 931 – 41, (d) 1216 – 41, (e) 931 – 13, (f) 931 – 70, and
(g) 931 – 90.

Fig. 4. Macrostructure showing transverse cross-section of the FSW joint developed using speed parameters of (a) 508 – 41, (b) 708 – 41, (c) 931 – 41, (d) 1216 – 41,
(e) 931 – 13, (f) 931 – 70, and (g) 931 – 90.

Immersion tests were performed on the transverse cross-section of
all the weld joints. Samples were immersed in a 3.5% NaCl solution for
30 days. Corrosion attack was investigated using optical microscopy.
Potentiodynamic polarization test (Tafel) and EIS tests were performed
at the upper surface of the weld joint and in 3.5% NaCl electrolytic
solution. Exposed area was kept 0.15 cm2 and remaining area was
masked. An open circuit delay time (OCD) of 1800s was given before
starting the corrosion tests. A ‘Gamry’ potentiostat having ‘DC105′ and
‘EIS300′ software packages was used for Tafel and EIS study, respec-
tively. All the tests were executed in triplicate and the repeatability was

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S. Sinhmar, D.K. Dwivedi
Fig. 5. Schematic showing locations of the thermocouples.
Fig. 6. Schematic of tensile specimen.
acceptable. A three electrode electrolytic cell used graphite electrode,
welded samples and SCE (saturated calomel electrode) as counter
electrode, working electrode, and reference electrode, respectively.
Potential range of −0.25 V to +0.25 V w.r.t. OCP (open circuit po-
tential) and scan rate of 1 mV/s were used for Tafel test. Frequency
range and AC voltage amplitude for EIS test were kept 10 kHz to
0.01 Hz and 10 mV, respectively. Results obtained from the EIS test
were fitted to an equivalent model circuit. All corrosion tests were
executed at room temperature.
3. Results and discussion
3.1. Microstructure
AA2014 base metal was used in as received condition for the friction
stir welding. Optical microstructure and FESEM image along with the
EDX analysis of as received base metal is shown in Fig. 7a and b, re-
spectively. Average grain size of α-Al matrix was 119 ± 49 μm. EDX
analysis of the precipitate indicated the presence of Al2Cu as the second
phase particle (Fig. 7b). FSW was done at different rotational and tra-
verse speed combination, keeping other welding parameters constant
(dwell time, tool tilt angle, axial force, plunge depth etc.). Microscopic
images of the stir zone and HAZ at different process parameters are
presented in Figs. 8 and 9, respectively. Grain refinement observed in
the NZ owing to the dynamic recrystallization and plastic deformation
experienced during the welding. Average grain size in stir zone and
HAZ are shown in Table 3. Size of the refined α-Al matrix grains ob-
served in the stir zone at various tool rotation and welding speeds was
measured using line intercept method. Change in tool rotation speed
from 508 rpm to 1216 rpm, increased average grain size of NZ from
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Journal of Manufacturing Processes 37 (2019) 305–320
9.86 μm to 19.20 μm. Change in traverse speed from 13 mm/min to
90 mm/min, decreased average grain size of stir zone from 19.46 μm to
12.86 μm.
Large size α-Al matrix grains were witnessed in the HAZ of all
parameters weld joints. Variation in the grain size of HAZ was noticed
for the different parameters, especially for the lower and higher speed
samples. Change in tool rotation speed from 508 rpm to 1216 rpm, in-
creased average grain size of the α-Al matrix of HAZ from 123 μm to
142 μm. Change in traverse speed from 13 mm/min to 90 mm/min,
decreased average grain size of the α-Al matrix of HAZ from 141 μm to
129 μm.
FESEM images of the NZ and HAZ of the weld joints developed at
various parameters are presented in Figs. 10 and 11, respectively. EDX
analysis was performed on the nugget zone and HAZ of FSW joints
produced at different speed combinations. EDX results suggested the
presence of Al2Cu precipitate and it was confirmed by the XRD analysis.
Fig. 10b is showing the EDX area analysis of NZ at 508 rpm – 41 mm/
min (area shown in Fig. 10a), which is indicating the presence of Cu as
the major alloying element along with the Al matrix. EDX study of the
precipitates present at grain boundary (point 1) and of precipitate free
zone i.e. PFZ (point 2) from inset of Fig. 11d is shown in Fig. 11e and f,
respectively. Difference in the concentration (wt%) of Cu at point 1 and
2 indicating the formation of PFZ (point 2) near the precipitate (point
1) at grain boundary of HAZ. Fig. 12 is showing the peaks obtained
from the XRD analysis of NZ and HAZ of sample welded at 931 rpm and
41 mm/min.
Difference in the precipitate size of the nugget zones can be ob-
served from the Fig. 10. Higher rotational speed (1216 rpm) and lower
welding speed (13 mm/min) samples showed coarse precipitates as
compared to the other speed parameters. Average precipitate size in the
NZ and HAZ are shown in Table 4. Change in tool rotation speed from
508 rpm to 1216 rpm, increased average precipitate size of nugget zone
and HAZ from 0.57 ± 0.16 μm to 1.4 ± 0.17 μm and from
2.25 ± 0.51 μm to 3.7 ± 0.66 μm, respectively. Change in traverse
speed from 13 mm/min to 90 mm/min, decreased average precipitate
size of nugget zone and HAZ from 1.43 ± 0.21 μm to 0.91 ± 0.20 μm
and from 3.6 ± 0.48 μm to 2.35 ± 0.60 μm, respectively. Fig. 13a and
b are showing the influence of change in rotational and welding speed
on the α-Al matrix grain size and precipitate size of nugget zone, re-
spectively. Change in the tool rotation speed from 708 rpm to 931 rpm
showed less variation in α-Al matrix grain size, whereas change in
traverse speed from 70 mm/min to 90 mm/min exhibited less variation
in α-Al matrix grain size as well as precipitate size of the nugget zone.
Fig. 14a and b are showing the influence of change in rotational and
welding speed on the α-Al matrix grain size and precipitate size of HAZ,
respectively. Change in tool rotation speed from 508 rpm to 708 rpm
exhibited less variation in the precipitate size, whereas change in tra-
verse speed from 41 mm/min to 90 mm/min exhibited less variation in
α-Al matrix grain size as well as precipitate size of the HAZ.
3.2. Weld thermal cycle
Weld thermal cycle plays a significant role to govern the micro-
structure of a weld joint. Weld thermal cycles (Fig. 15) were measured
during FSW at all the speed parameters. Fig. 15a and b are showing the
weld thermal cycles at different rotational speeds. Fig. 15c and d are
showing the weld thermal cycles at different traverse speeds. Highest
temperature was observed in the weld joint developed at 1216 rpm
(from the weld joints developed at 508 rpm – 1216 rpm) and by the
weld joint developed at 13 mm/min (from the weld joints developed at
13 mm/min – 90 mm/min). Peak temperatures observed during the
welding at different process parameters are shown in Table 5. High
temperature retention period (from 150 °C to peak temperature) of the
weld joints increased with increase in the rotation speed, which in turn
enhanced the coarsening of precipitates along with the dissolution of
fine precipitates. On the other hand, high temperature retention period
S. Sinhmar, D.K. Dwivedi
Fig. 7. Base metal microstructure using (a) optical microscope, and (b) FESEM with EDX analysis.
Fig. 8. Optical micrographs of FSW nugget zones at speed parameters of (a) 508 – 41, (b) 708 – 41, (c) 931 – 41, (d) 1216 – 41, (e) 931 – 13, (f) 931 – 70, and (g) 931
– 90.
decreased with increase in the welding speed, which in turn reduced
the extent of coarsening and dissolution/reversion of the precipitates.
Heat input was measured for the weldments fabricated at various
rotational and traverse speeds. Tool shoulder produces utmost heat
during the FSW. Only a minor portion of the heat is generated by the
probe. Current study considered the role of shoulder as well as pin for
heat generation. Following formula was used for the calculation of heat
generation [20]:
2 F
Q= µ [(RS3 RP3 )(1 + tan ) + RP3 + 3RP2 HP ]
3 vRS2
where, Q (kJ/mm) is the total heat input during FSW, F (kN) is the axial
load, α (degree) is concavity of shoulder, RS (m) is the radius of
shoulder, RP (m) is the radius of pin, HP (m) is the height of pin, μ is the
coefficient of friction, ω (rad/s) is angular velocity of tool, and v (mm/
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Journal of Manufacturing Processes 37 (2019) 305–320
s) is the traverse speed or welding speed. Coefficient of friction (μ) was
calculated using following formula [21]:
µ= 0.5exp( RS )
where, δ is the local variation in fractional slip and can be calculated
using:
RS
= 0.31exp 0.026
1.87
Heat input experienced by the weld joints at various rotational and
welding speeds is given in the Table 6. Higher heat input was observed
at the higher rotational speed from the weld joints developed at dif-
ferent rotational speeds. Similarly, higher heat input was observed at
lower traverse speed from the weld joints developed at different tra-
verse speed. Heat input was increased with increase in the tool rotation
S. Sinhmar, D.K. Dwivedi
Fig. 9. Optical micrographs of FSW heat affected zones at speed parameters of (a) 508 – 41, (b) 708 – 41, (c) 931 – 41, (d) 1216 – 41, (e) 931 – 13, (f) 931 – 70, and
(g) 931 – 90.
Table 3
Average α-Al matrix grain size (μm) of NZ and HAZ.
Parameters At constant traverse speed
508 rpm 708 rpm 931 rpm
NZ 9.86 ± 1.39 14.03 ± 2.36 14.76 ± 2.02
HAZ 123 ± 18.22 129 ± 10.78 134 ± 16.23
speed and decreased with increase in the welding speed. Further, the
effect of change in heat input due to weld thermal cycle on various
properties of the weld joint is discussed in the following sections.
3.3. Microhardness
Microhardness across the perpendicular cross-section of the weld
joint was measured. Microhardness profile of the weld joints developed
using different rotational speeds (508 rpm–1216 rpm) and traverse
speeds (13 mm/min–90 mm/min) are shown in Fig. 16a and b, re-
spectively. Microhardness profile was of a typical ‘W’ shape, as usually
found in case of FSW joint of the heat treatable aluminium alloys.
Nugget zone of the weld joint developed using lower tool rotation speed
(508 rpm) showed higher average microhardness (134 ± 7 HV) than
those developed using higher rotational speed. Nugget zone of the weld
joint produced using higher traverse speed (90 mm/min) showed
higher average microhardness (139 ± 5 HV) than those developed
using lower traverse speed. Microhardness results were in agreement
with the Hall-Petch relationship, which suggests the increase in mi-
crohardness with decreases in the grain size [22]. High rotational speed
(1216 rpm) and low welding speed (13 mm/min) resulted in high heat
input, which in turn increased the grain size of the NZ. Increase in the
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Journal of Manufacturing Processes 37 (2019) 305–320
At constant rotational speed
1216 rpm 13 mm/min 70 mm/min 90 mm/min
19.20 ± 3.7 19.46 ± 2.02 13.13 ± 2.79 12.86 ± 2.33
142 ± 21.22 141 ± 14.54 130 ± 10.55 129 ± 10.65
welding speed reduced the heat input, which in turn caused the narrow
nugget zone (Fig. 16b). Increase in tool rotation speed or decrease in
welding speed, increased the heat input, which further accelerated the
coarsening and dissolution of the strengthening precipitates. Further,
coarsening and dissolution of the precipitates reduced the microhard-
ness [23].
3.4. Tensile properties
Tensile tests were performed on the sound weld joints produced
using 708 rpm – 41 mm/min and 931 rpm – 41 mm/min. Tensile test
samples are shown in Fig. 17. Fracture location of the tensile specimens
obtained from above mentioned parameters was heat affected zone and
hence, in agreement with microhardness profile (Fig. 16). Ultimate
tensile strength (UTS), yield strength and % elongation of the FSW joint
produced at 708 rpm and 931 rpm were 326 ± 1 MPa,
201 ± 2.6 MPa, 7.48% and 328 ± 7 MPa, 210 ± 5.5 MPa, 8.66%,
respectively. Tensile strength of both weld joint were close to each
other, whereas small difference was observed in the percentage elon-
gation. Softening caused by the high heat input at 931 rpm resulted in
more elongation in the weld joint. Fracture surface micrographs of the
weld joints are shown in Fig. 18. Low and high magnification
S. Sinhmar, D.K. Dwivedi Journal of Manufacturing Processes 37 (2019) 305–320

Fig. 10. FESEM images of FSW nugget zones at speed parameters of (a) 508 – 41, (b) EDX analysis of NZ showed in ‘a’, (c) 708 – 41, (d) 931 – 41, (e) 1216 – 41, (f)
931 – 13, (g) 931 – 70, and (h) 931 – 90.

Fig. 11. FESEM images of FSW heat affected zones at speed parameters of (a) 508 – 41 and inset showing higher magnification grain boundary, (b) 708 – 41, (c) 931
– 41, (d) 1216 – 41 and inset showing higher magnification grain boundary, (e) EDX analysis of point 1 in inset of image ‘d’, (f) EDX analysis of point 2 in inset of
image ‘d’, (g) 931 – 13 and inset showing higher magnification grain boundary, (h) 931 – 70, and (i) 931 – 90.

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fractographs of the weld joint produced at 708 rpm are shown in

Fig. 18a and b, respectively. Low and high magnification fractographs
of the weld joint produced at 931 rpm are shown in Fig. 18c and d,
respectively. Factors affecting the tensile properties of FSW joint are
degree of plastic flow, mixing of material in nugget zone, presence of
defect, degree of dissolution and overaging of precipitates and grain
size in HAZ [24]. Presence of the dimples in fractographs (Fig. 18b and
d) indicating the ductile fracture of both weld joints and is in agreement
with the percentage elongation.

3.5. Corrosion testing

Three different type of corrosion tests were performed in 3.5% NaCl

solution. Corroded surface of the NZ and HAZ after immersion test of
the weld joint developed at 508 rpm, 708 rpm, 931 rpm, 1216 rpm,
13 mm/min and 90 mm/min are shown in Figs. 19 and 20, respectively.
Fig. 12. XRD patterns of NZ and HAZ of sample welded at 931 rpm and 41 mm/ Corroded surface of the weld produced at 70 mm/min is not shown due
min. to almost same corrosion attack as of weld joint produced at 90 mm/
min. Severity of corrosion in nugget zone and HAZ was increased with
increase in the tool rotation speed. At low rotational speed (508 rpm)

Table 4
Average precipitate size (μm) of nugget zone and HAZ.
Parameters At constant traverse speed At constant rotational speed

508 708 931 1216 rpm 13 mm/min 70 mm/min 90 mm/min

rpm rpm rpm

NZ 0.57 ± 0.87 ± 1.12 ± 1.4 ± 1.43 ± 0.98 ± 0.91 ±

0.16 0.18 0.18 0.17 0.21 0.13 0.20
HAZ 2.25 ± 2.33 ± 2.79 ± 3.7 ± 3.6 ± 2.71 ± 2.35 ±
0.51 0.76 0.82 0.66 0.48 0.57 0.60

Fig. 13. α-Al matrix grains and precipitate size variation in nugget zone with change in (a) rotational speed, and (b) traverse speed.

Fig. 14. α-Al matrix grains and precipitate size variation in heat affected zone with change in (a) rotational speed, and (b) traverse speed.

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Fig. 15. Temperature profiles of the weld joints produced at different rotational speeds at (a) 5 mm, (b) 10 mm distance; and weld joints produced at different
traverse speeds at (c) 5 mm, (d) 10 mm distance.

Table 5
Peak temperature in the FSW joint at different speed combination at 5 mm and 10 mm distance away from the center of the weld.
Parameters At constant traverse speed At constant rotational speed

508 rpm 708 rpm 931 rpm 1216 rpm 13 mm/min 70 mm/min 90 mm/min

Temperature at 5 mm (°C) 328 362 374 406 385 366 362

Temperature at 10 mm (°C) 280 333 355 377 361 334 329

Table 6
Heat input in the weld joint at various tool rotation speeds and welding/traverse speeds.
Speed parameters At constant traverse speed At constant rotational speed

508 rpm 708 rpm 931 rpm 1216 rpm 13 mm/min 70 mm/min 90 mm/min

Total heat input (kJ/mm) 0.86 1.12 1.28 1.37 3.95 0.75 0.58

corrosion attack was localized and discrete (Figs. 19a and 20 a), but at
higher rotational speed (1216 rpm) it was almost as ‘uniform corrosion’
(Figs. 19d and 20 d). Uniform corrosion attack is an electrochemical
reaction that ensues uniformly over a large exposed area [25]. On the
other hand, severity of corrosion in nugget zone and HAZ was reduced
with increase in the welding speed. Corrosion attack was localized
(Figs. 19f and 20 f) at higher traverse speed (90 mm/min), but it was
almost ‘uniform corrosion’ (Figs. 19e and 20 e) at lower welding speed
(13 mm/min). It was noticed that the severity of the corrosion attack
was more in HAZ than the nugget zone.
Potentiodynamic polarization test (Tafel) was carried out on the
weld joint produced at various tool rotation speeds and different
welding speeds. Tafel curves obtained from the NZ and HAZ of the FSW
joint developed using different rotational speeds are shown in Fig. 21a.
Tafel curves obtained from the NZ and HAZ of the FSW joint developed
using different traverse speeds are shown in Fig. 21b. Tafel curves

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S. Sinhmar, D.K. Dwivedi
Fig. 16. Microhardness profile of friction stir weld joint developed at (a) various tool rotation speeds, and (b) various traverse speeds.
Fig. 17. Tensile specimens of the weld joint developed at a tool rotation speed of 708 rpm (a) before tensile test, (b) after tensile test; and weld joint produced at
931 rpm (c) before tensile test, (d) after tensile test.
indicate that the corrosion potential (Ecorr) of nugget zone is less ne-
gative than the HAZ. It suggests that the corrosion resistance of the NZ
is more than the HAZ. Corrosion potential obtained from the Tafel tests
of NZ and HAZ are shown in the Table 7.
Corrosion resistance was found to decrease (Ecorr became more ne-
gative) with increasing the rotational speed. Lower corrosion potential
(more negative) observed from NZ and HAZ of weld joint produced at
1216 rpm was −662 mV and −682 mV, respectively. On the other
hand, corrosion resistance was improved with increase in the welding
speed. Lower corrosion potential observed from NZ and HAZ of weld
joint produced at 13 mm/min traverse speed was -661 mV and
−677 mV, respectively. Sample welded at 70 mm/min showed slightly
higher corrosion potential than the 90 mm/min.
Corrosion potentials of the NZ and HAZ suggested that the variation
in rotational speed (508 rpm – 1216 rpm) affected the corrosion re-
sistance more than the variation in the traverse speed (13 mm/min –
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Journal of Manufacturing Processes 37 (2019) 305–320
90 mm/min) as evident from Table 7. Corroded surface after po-
tentiodynamic polarization test of NZ and heat affected zone of the FSW
joints developed at 508 rpm, 708 rpm, 931 rpm, 1216 rpm, 13 mm/min
and 90 mm/min are shown in Figs. 22 and 23, respectively. Pitting
corrosion was witnessed in stir zone and heat affected zone of the weld
joints produced at various rotational and traverse speeds. Pitting was
observed within the grain (Fig. 22c) and along the grain boundary
(Fig. 22d). Severe pitting corrosion attack was observed in NZ and HAZ
of the weld joint developed at high rotation speed (1216 rpm) as shown
in Figs. 22d and 23 d, respectively. NZ and HAZ of the FSW joint de-
veloped at low traverse speed (13 mm/min) also showed severe pitting
corrosion as shown in Figs. 22e and 23 e, respectively. Findings of the
Tafel test are in agreement with the immersion test. Furthermore, the
Tafel test was performed on the cross-section of the weld joints to
compare the corrosion behavior with the upper surface of the weld
joints. Cross-section of the weld joints showed same trend of the
S. Sinhmar, D.K. Dwivedi Journal of Manufacturing Processes 37 (2019) 305–320

Fig. 18. Fractographs of friction stir welded tensile specimens at speed parameters of (a) 708 – 41 at lower magnification, (b) 708 – 41 at higher magnification, (c)
931 – 41 at lower magnification, and (d) 931 – 41 at higher magnification.

Fig. 19. Immersion test corroded surface of NZ welded at speed parameters of (a) 508 – 41, (b) 708 – 41, (c) 931 – 41, (d) 1216 – 41, (e) 931 – 13, and (f) 931 – 90.

corrosion behavior as the upper surface. Corrosion potentials of the
cross-section of the weld joints at lower and higher speeds are shown in
Table 8.
Electrochemical impedance spectroscopy was performed on the NZ
and HAZ of the weld joints produced at various rotational speeds and
welding speeds. Nyquist plots of the EIS tested weld joints developed at
various tool rotation speeds and different traverse speeds are shown in
Fig. 24a and b, respectively. Nyquist plot comprises real impedance
(Zre) at x-axis and imaginary impedance (Zim) at y-axis. Single time
constant and high frequency capacitive loop/semi-circle was observed
in the Nyquist plot (Fig. 24). Diameter of the semi-circle shows the
corrosion resistance in term of polarization resistance (Rp) at x-axis
[26]. Larger size of the semi-circle indicates the more corrosion
resistance compared to the small size semi-circle. The weld joint pro-
duced at lower rotational speed (508 rpm) showed larger diameter
(Fig. 24a), which offered more corrosion resistance than the higher
rotational speed (1216 rpm). Nugget zone of the weld joints produced
at different parameters showed larger diameter than the HAZ. On the
other hand, weld joint developed at lower welding speed (13 mm/min)
showed lower polarization resistance compared to the higher traverse
speed (Fig. 24b). An equivalent circuit (Fig. 24c) called constant phase
element (CPE) was used to fit the data obtained from the EIS test. CPE
gives results in term of solution resistance (Rs), polarization resistance
(Rp), admittance (Y0) and n (value shows deviation of capacitor from
ideal capacitor). Admittance (Y0) behave as inductor at n = -1, resistor
at n = 0 and capacitor at n = 1. Extracted data (NZ and HAZ) using

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Fig. 20. Immersion test corroded surface of HAZ welded at speed parameters of (a) 508 – 41, (b) 708 – 41, (c) 931 – 41, (d) 1216 – 41, (e) 931 – 13, and (f) 931 – 90.

Fig. 21. Tafel curves of NZ and HAZ at (a) various tool rotation speeds at constant welding speed of 41 mm/min, and (b) various welding speeds at constant tool
rotation speed of 931 rpm.

Table 7
Corrosion potentials (Ecorr in mV) at upper surface of the sample welded at various rotational and welding speeds.
Parameters 508 rpm 708 rpm 931 rpm 1216 rpm 13 mm/min 70 mm/min 90 mm/min

NZ −604 −632 −659 −662 −661 −635 −642

HAZ −625 −669 −675 −682 −677 −670 −669

equivalent circuit after the EIS test is shown in Table 9. Solution re-
sistance (Rs) obtained from the EIS test was almost similar for all the
weld joints, and having very small value than the polarization re-
sistance (Rp). Higher polarization resistance indicates the higher cor-
rosion resistance. Polarization resistance was reduced with increase in
the rotation speed (508 rpm – 1216 rpm) at constant traverse speed
(Table 9). Polarization resistance increased with increase in the welding
speed (13 mm/min – 90 mm/min) at constant tool rotation speed
(Table 9). Polarization resistance of NZ was more as compared to the
HAZ in all the cases. So, the EIS test findings are also in agreement with
the Tafel test and immersion test results.
Microstructure of AA2014 aluminium alloy mainly contains matrix
grains along with majority of Al2Cu precipitates as second phase
particles of white color as shown in Figs. 10 and 11. Earlier, the mi-
crostructure was uniform before FSW become disintegrated after the
welding. As discussed in ‘section 1’, it is divided into different zones.
Second phase particles are considerably sensitive to the thermal cycle of
the welding and the precipitates present in different zone is affected up
to a different level. Increase in the tool rotation speed and decrease in
the welding speed resulted into the more frictional heat, which in turn
increased the heat input to the weld joint. Increase in heat input causes
longer high temperature retention period, facilitating coarsening of the
precipitates as well as α-Al grains (Fig. 10). Reverse trend was observed
with increase of traverse speed. Low heat input reduced the extent of
grain coarsening. Dissolution and coarsening of the precipitates was
witnessed in the HAZ of the weld joints. Temperature in the NZ was

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Fig. 22. Corroded surface observed after Tafel test of NZ welded at speed parameters of (a) 508 – 41, (b) 708 – 41, (c) 931 – 41, (d) 1216 – 41, (e) 931 – 13, and (f)
931 – 90.

Fig. 23. Corroded surface observed after Tafel test of HAZ welded at speed parameters of (a) 508 – 41, (b) 708 – 41, (c) 931 – 41, (d) 1216 – 41, (e) 931 – 13, and (f)
931 – 90.

Table 8 (Fig. 26) [27]. Large potential difference among the Al2Cu particle and
Corrosion potentials (Ecorr in mV) at cross-section of the sample welded at lower PFZ led to the more corrosion. Precipitates having different types of
and higher rotational and welding speeds. shape and size in various zones affect the numerous properties of weld
Parameters 508 rpm 1216 rpm 13 mm/min 90 mm/min joint accordingly. Small precipitates also help to improve the tensile
properties of the weld joint. These produce pinning effect on the grain
NZ −613 −665 −658 −652 boundary during the tensile testing, which in turn resist movement of
HAZ −629 −669 −671 −657
the grains and hence, improve the strength of the weld joint.
Microhardness and corrosion resistance showed similar trend with
change in rotational and traverse speed. Bar diagram (Fig. 27) is
showing the change in corrosion potential and microhardness of the
sufficient to dissolve (partial/full) precipitates. Chance of full dissolu- nugget zone of friction stir weld joints developed at various rotational
tion was increased with increase in rotational speed or reducing the (508 rpm – 1216 rpm) and traverse speeds (13 mm/min – 90 mm/min).
traverse speed. Generally, this type of microstructural change results in Formation of the coarse precipitate at high rotation speed or low tra-
deterioration of mechanical properties. Finer precipitates in the nugget verse speed results in the PFZ. Precipitate free zone is comparatively
zone (931 rpm – 41 mm/min) compared to the HAZ were evident in the soft and high pitting susceptible region [28]. Fine grains observed at
TEM analysis (Fig. 25a and b). Precipitate free zone (PFZ) was wit- low tool rotation speed or high welding speed, were more susceptible to
nessed in the HAZ of the weld joints developed at higher rotation speed the oxide film formation as compared to the large grains. Large grain
(inset of Fig. 11d) and lower traverse speed (inset of Fig. 11g). Coarse boundary area of fine grains provide more active region to form the
Al2Cu precipitates act as cathode (due to less negative or noble po- oxide film. Presence of oxide film enhances the corrosion resistance of
tential than Al matrix) and PFZ in the Al- matrix is act as anode the aluminium alloys [29]. Hence, the fine grains are beneficial from

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Fig. 24. Nyquist plots of NZ and HAZ at (a) various tool rotation speeds at constant welding speed of 41 mm/min, (b) various welding speeds at constant tool rotation
speed of 931 rpm, and (c) showing the equivalent circuit used for fitting of the curves obtained from EIS test.

Table 9
EIS data of the NZ and HAZ of different speed parameters weld joint extracted from the equivalent circuit.
Parameter 508 rpm 708 rpm 931 rpm 1216 rpm 13 mm/min 70 mm/min 90 mm/min

NZ
Rs (Ω) 15.80 18.91 14.76 18.41 15.23 17.32 19.70
Rp (Ω. cm2) 4575 3972 3270 3135 3229 3630 3621
Y0 (Ω−1 cm-2sn) ×10-5 1.024 1.066 1.163 1.547 1.533 1.133 1.090
n 0.924 0.897 0.922 0.931 0.880 0.900 0.890

HAZ
Rs (Ω) 17.80 20.20 15.30 18.71 15.00 20.00 20.05
Rp (Ω. cm2) 4110 2286 2152 1221 1900 2236 2352
Y0 (Ω−1 cm-2sn) ×10-5 1.434 1.636 2.126 2.536 2.152 1.941 1.835
n 0.889 0.888 0.840 0.823 0.904 0.848 0.902

Fig. 25. Transmission electron microscopy images of (a) stir zone, and (b) HAZ of weld joint at 931 rpm – 41 mm/min.

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Fig. 26. Schematic showing the formation of precipitate free zone in vicinity of coarse precipitate.

4. Conclusions

Friction stir welding of AA2014 aluminium alloy was performed at

various rotational and traverse speed. Optimum speed combination is
necessary for a sound weld joint. Therefore, this investigation is rea-
sonably significant for metallurgical and corrosion behavior study of
the FSW joint. Major conclusions drawn are:

1 Increase in rotational speed (508 rpm – 1216 rpm) and decrease in

Fig. 27. Bar diagram showing corrosion potential and microhardness of sam-
ples welded at various rotational and traverse speeds.
corrosion as well as microhardness point of view.
Role of weld pitch is also important to produce a sound weld joint.
Weld pitch (rev/mm) is the ratio of rotational speed to the traverse
speed. It gives the number of revolution taking place during one mm
traverse of the tool. Generally, weld pitch governs specific heat input in
to the weld zone during the welding. Weld pitch calculated for the
different combination of rotation and traverse speeds are given in
Table 10. Sound joints were produced at weld pitch of 17.26 rev/mm
and 22.70 rev/mm, which were obtained using speed parameters of
708 rpm – 41 mm/min and 931 rpm – 41 mm/min, respectively. This
indicates that there is a range of weld pitch which results in a sound
weld joint. Weld pitch beyond this range (17.26 rev/mm – 22.70 rev/
mm), does not plasticize the material properly. So, weld pitch can be
helpful to evaluate the weld property behavior in early stage. Friction
stir weld joint needs a proper combination of heat input and mixing of
the material in the stir zone (nugget zone). Therefore, parameters
providing either less heat input (low tool rotation or high welding
speed) or the high heat input (high tool rotation or low welding speed)
decrease the tendency to produce sound FSW joints [30].
traverse speed (90 mm/min – 13 mm/min) resulted in to the large α-
Al matrix grain as well as coarse precipitates in the nugget zone and
heat affected zone.
2 Lower rotational i.e. 508 rpm (from rotation speed variation) and
higher traverse speed i.e. 90 mm/min (from traverse speed varia-
tion) resulted in to the higher microhardness. Both parameters re-
sulted in to the relatively small α-Al matrix grain size which affected
the microhardness of the joint.
3 Inappropriate speed combination resulted in to the defects in the
weld joint which further reduced the tensile strength of the weld
joint. Rotation speed of 708 rpm and 931 rpm at 41 mm/min tra-
verse speed produced sound weld joint and shown higher tensile
properties.
4 Three different type of corrosion test showed that the weld joints
developed at higher tool rotation speed and lower welding speed
were more susceptible to the corrosion. Peak temperature reached in
the weld joint was more at these parameters, which resulted in to
the coarse precipitates and precipitate free zone.
5 Precipitate free zone is neither good for mechanical properties nor
for corrosion resistance. It produced non uniformity in the micro-
structure which was a weakening factor for the weld joint.
6 Optimum speed parameters for friction stir welding of AA2014
(6 mm thickness) plate based on present investigation are 708 rpm
and 931 rpm at 41 mm/min.
7 Majority of the precipitates observed in the weld joints were Al2Cu,
and their presence affected the corrosion performance significantly.

Table 10
Weld pitch (rev/mm) value obtained from different speed combinations.
Parameters 508 rpm 708 rpm 931 rpm 1216 rpm 13 mm/min 70 mm/min 90 mm/min

Weld pitch (rev/mm) 12.39 17.26 22.70 29.65 71.61 13.3 10.34

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