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Corrosion Science
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A study on corrosion behavior of friction stir welded and tungsten inert gas
welded AA2014 aluminium alloy
⁎
Sunil Sinhmar , Dheerendra Kumar Dwivedi
Mechanical & Industrial Engineering Department, Indian Institute of Technology Roorkee, Roorkee 247667, Uttarakhand, India
A R T I C L E I N F O A B S T R A C T
Keywords: The present study comprises the comparison of the electrochemical behavior of friction stir weld (FSW) joint and
Aluminium tungsten inert gas (TIG) weld joint of AA2014 using immersion test, potentiodynamic polarization test and
Welding electrochemical impedance spectroscopy (EIS). Weld thermal cycles and microhardness were correlated with
Pitting corrosion corrosion behavior of the weld joints. TIG weld joint showed lower corrosion resistance than FSW joint. Heat
Polarization
affected zone was the most corrosion susceptible region in both type of weld joints. Optical microscopy, FESEM,
EIS
TEM and XRD analysis were performed to discuss the corrosion behavior in light of the microstructure.
⁎
Corresponding author.
E-mail address: sun25.dme2014@iitr.ac.in (S. Sinhmar).
https://doi.org/10.1016/j.corsci.2018.01.012
Received 22 August 2017; Received in revised form 9 January 2018; Accepted 18 January 2018
0010-938X/ © 2018 Elsevier Ltd. All rights reserved.
Please cite this article as: Sinhmar, S., Corrosion Science (2018), https://doi.org/10.1016/j.corsci.2018.01.012
S. Sinhmar, D.K. Dwivedi Corrosion Science xxx (xxxx) xxx–xxx
Table 1 Table 2
Chemical composition (wt%) of AA2014. Tool dimensions and FSW process parameters.
AA2014 4.8 0.97 0.7 0.38 0.54 0.25 Balance Shoulder Pin shape Pin Pin Rotational Traverse Tool
diameter diameter length speed speed tilt
(mm) (mm) (mm) (rpm) (mm/ angle
performed on AA2024 and AA6061 aluminium alloys and it was found min) (°)
that phase transformation caused by the high heat input during the TIG 18 Cylindrical M6 5.7 931 41 1.5
welding lead to the more corrosion [11,12]. Metal inert gas weld joint (threaded)
of AA6xxx also showed lower corrosion resistance compared to the FSW
joint [13]. HAZ was the most corrosion susceptible region in the TIG
weld joint of AA2219. It was attributed to the segregation and reversion Table 3
of second phase (Al2Cu) along the grain boundary [14]. TIG welding process parameters.
As the AA2014 is a very important aluminium alloy from the
Welding Voltage (V) Welding speed Shielding gas Gas flow rate
commercial point of view, so it is essential to study the corrosion be- current (A) (mm/min) (l/min)
havior of this alloy. FSW and TIG welding are the two major joining
techniques uses for this alloy. Corrosion behavior of the FSW joint of 150 12 150 Ar 15
AA2014 was studied in the literature but same for TIG welding alone
and comparative study of FSW and TIG weld joint of AA2014 is not
welding along with schematic of the position of thermocouples. Sam-
available to the author’s knowledge. Although heat input during the
ples from transverse cross-section were polished on SiC papers up to
welding is a very important factor, but comparative weld thermal cycles
2000 grit and then followed by rough and fine cloth polishing using
for both welding techniques in correlation with corrosion behavior has
heavy magnesium oxide powder slurry. Keller’s etchant (2.5 ml of
not been reported. The present study investigates the corrosion beha-
HNO3, 1.5 ml HCl, 1.0 ml of HF and 95 ml of distilled water) was ap-
vior of AA2014 correlating with microstructure (including precipitate
plied on the polished samples for 25 s to reveal the grain boundaries.
reversion and coarsening) and weld thermal cycle history.
Optical microscopy was performed on Dewinter LT-23B microscope
and ‘Image J’ software was used to calculate the average grain size of
2. Experimental procedure each zone of the weld joints. Field emission scanning electron micro-
scopy (FESEM) and energy dispersive X-ray spectroscopy (EDS) were
As received AA2014-T651 aluminium alloy plates were used for the used for micro analysis of elements present in the different phases. X-
FSW and TIG welding. Plate dimensions were ray diffraction (XRD) with CuKα radiation was used to analyze the
70 mm × 27.5 mm × 6 mm and 100 mm × 27.5 mm × 6 mm for FSW phases of the joints. Transmission electron microscopy (TEM) was used
and TIG welding, respectively. Abutting surfaces were properly cleaned on the electron transparent foils of the joints for profound study.
using acetone before the welding. An indigenous modified vertical Microhardness study of the both weld joints was performed using
milling machine (15 HP) was used for the FSW. Plates were properly Vicker’s microhardness tester. Load, dwell time and distance between
clamped in the fixture before starting of the welding. The non con- two consecutive indentations were 100 g, 10 s and 0.5 mm, respec-
sumable tool of ‘H13 steel’ having a cylindrical threaded pin of Inconel tively. The temperature was measured during welding using K-type
was used for the FSW. Rotational and traverse speeds were 931 rpm and thermocouples. Thermocouple wires were inserted into the drilled holes
41 mm/min, respectively. Tool dimensions and friction stir welding of 1.5 mm diameter and 3 mm depth at the bottom side of the plates to
parameters are given in Table 2. Axial force (F) during FSW was 3.5 kN be welded. A special backing plate with slots was prepared to accom-
and concavity (α) at the shoulder of FSW tool was 5°. modate the thermocouple wires. The locations of the holes were kept at
Double sided TIG welding was carried out on ‘EWM Triton 180 AC/ 5 mm and 10 mm distance from the weld center line in both the welding
DC hightec welding’ machine without using any filler material. Process techniques. Thermocouple wire was not kept in the center of the weld
parameters used for the TIG welding are given in Table 3. Samples were because the moving pin of the FSW tool and melting in TIG welding
extracted for various testing and characterization after performing both could have destroyed the wire.
types of welding. Fig. 2 is showing the plates welded using FSW and TIG Corrosion behavior of the upper surface of weld joints obtained
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S. Sinhmar, D.K. Dwivedi Corrosion Science xxx (xxxx) xxx–xxx
through both welding techniques was studied via immersion test, po- affected zone (Fig. 3b). Average grain size of α-matrix in nugget zone
tentiodynamic polarization (Tafel) test and electrochemical impedance and heat affected zone of FSW joint was 14.7 ± 2.02 μm and
spectroscopy. Samples for each corrosion test were polished up to the 134.35 ± 16.23 μm, respectively. Plastic deformation and dynamic
mirror finish. All the corrosion tests were performed in aerated 3.5% recrystallization produced by the FSW tool pin in nugget zone resulted
NaCl solution and at room temperature. Samples were immersed for in refined grain structure. Average grain size of α-matrix in fusion zone
30 days during the immersion test and the solution was changed on (Fig. 4a) and heat affected zone (Fig. 4b) of TIG weld joint was
alternate days. The extent of attack of the corrosion on the surface of 99.7 ± 13.84 μm and 185.5 ± 35.55 μm, respectively. The equiaxed
immersed samples was analyzed using optical microscopy. Gamry’s dendritic microstructure was observed in fusion zone after the solidi-
‘1000 interface’ potentiostat was used for the electrochemical study. fication of the material (Fig. 4a). The large difference in the grain sizes
Software used for the Tafel polarization and EIS testing were DC105 of respective regions was observed in the both welding techniques.
and EIS300, respectively. Exposed area for the electrochemical tests These microstructure variations are expected to alter the various
was kept 0.15 cm2 and remaining portion of the samples was masked. A properties of the joints and will be discussed in the below given sec-
horizontal electrolytic cell of glass with three electrode setup was used tions.
for the electrochemical corrosion testing. Saturated calomel electrode Field emission scanning electron microscope (FESEM) images of
(SCE), graphite electrode and weld joint sample (to be corrosion tested) both types of weld joints are given in Fig. 5. EDS analysis of the pre-
were the reference electrode, counter electrode and working electrode, cipitates present on the surface of nugget zone and fusion zone sug-
respectively. Open circuit delay (OCD) time was kept 1800s. Process gested the presence of Al2Cu (Fig. 5a and b). Presence of the Al2Cu
parameters for the Tafel polarization test were: potential range precipitates was confirmed by the XRD analysis of FSW and TIG weld
−0.25 V to +0.25 V with respect to open circuit voltage (OCV) and a joints in Fig. 6. Fine Al2Cu precipitates (average size 1.12 ± 0.18 μm)
scan rate of 1 mV/s. EIS study was performed at a frequency range of and coarse precipitates (average size 3.51 ± 0.40 μm) were observed
10 kHz to 0.01 Hz at open circuit potential with AC amplitude of 10 mV. in the nugget zone and fusion zone, respectively (Fig. 5a and b). The
average size of the coarse precipitates distributed within the grains of
3. Results and discussion HAZ of FSW and TIG weld joints were 3.51 ± 0.40 μm (Fig. 5c) and
3.80 ± 0.69 μm (Fig. 5e), respectively. Magnified view of precipitates
3.1. Microstructure present at the grain boundary of the heat affected zone of FSW (Fig. 5c)
and TIG (Fig. 5e) weld joints are shown in Fig. 5d and f, respectively.
The optical microstructure of the FSW and TIG weld joints are
shown in Figs. 3 and 4, respectively. The microstructure of the weld 3.2. Weld thermal cycle and heat generation
joints mainly comprises α-Al matrix grains and Al2Cu precipitates.
Nugget zone (Fig. 3a) is showing the finer grains compared to the heat The microstructure of the weld joint is significantly affected by the
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S. Sinhmar, D.K. Dwivedi Corrosion Science xxx (xxxx) xxx–xxx
weld thermal cycle during the welding [15]. Maximum temperature slightly lower than the FSW joint.
observed near the nugget zone (5 mm away from the center of the weld)
and HAZ (10 mm away from the center of the weld) of FSW joint
3.3. Microhardness
(Fig. 7a) was 374 °C and 355 °C, respectively. Similarly, maximum
temperature observed near the fusion boundary (5 mm away from the
Microhardness testing results of the FSW and TIG weld joints are
center of the weld) and HAZ (10 mm away from the center of the weld)
shown in Fig. 8. Maximum microhardness observed in FSW and TIG
of TIG weld joint (Fig. 7b) was 703 °C and 544 °C, respectively. Thus,
weld joints were 128 HV and 113 HV, respectively. Friction stir weld
temperature observed in the TIG welding was higher than the friction
joint showed higher hardness compared to the TIG weld joint. Both
stir welding.
weld joints showed higher hardness in nugget (FSW) and fusion zone
Major heat generation occurs mainly due to the friction between
(TIG) compared to the heat affected zone. The small grain size of the α-
shoulder-workpiece interfaces and plastic deformation during friction
Al matrix of the nugget zone (Fig. 5a) contributed to higher hardness
stir welding. FSW tool pin also participates in the heat generation but to
(Hall-Petch relationship) of the joint [7]. Weld thermal cycle indicates
less extent as compared to the shoulder. Many studies have been per-
that HAZ of TIG weld joint (Fig. 7b) was experienced higher peak
formed to investigate the heat generation in FSW [16–18]. Some re-
temperature than HAZ of FSW joint (Fig. 7a). Generally, Guinier-Pre-
searchers considered only role of the shoulder in heat generation, while
ston (GP) zone precipitates dissolve above 200 °C. Therefore, as the
others considered the effect of both shoulder and tool pin. The present
temperature increases, the fine Al2Cu precipitates also get dissolve and
study considers the role of the pin along with the shoulder for heat
segregate at grain boundaries, which in turn reduces the hardness of
generation during FSW. The formula used for heat generation in friction
HAZ [14].
stir welding is [19]:
2 F
Qfsw = μω 2 [(RS3 − RP3)(1 + tan α ) + RP3 + 3RP2 HP ] 3.4. Corrosion testing
3 vRS
where, Qfsw is the heat input (kJ/mm) during friction stir welding, μ is Corrosion behavior of the friction stir weld and TIG weld joint was
the friction of coefficient, ω is the angular velocity (rad/s), F is axial investigated using immersion test, Tafel test (direct current based test)
load (kN), RS is radius of shoulder (m), RP is radius of tool pin (m), HP is and electrochemical impedance spectroscopy (alternate current based
the height of tool pin (m), v is the traverse speed (mm/s) and α is the test). Optical images of the corroded surface of both weld joints after
concavity of the shoulder (degree). 30 days immersion in 3.5% NaCl solution are shown in Fig. 9. Corrosion
The formula for the heat input during the TIG welding is: attack sites were fewer in nugget zone (Fig. 9a) compared to the HAZ of
FSW joint (Fig. 9b) as well as both zones of TIG joint (Fig. 9c and d).
V×I
Qtig = η × Severe corrosion attack was observed in TIG weld joint, especially in
vs
heat affected zone (Fig. 9d). Black circles in Fig. 9d are indicating se-
where, Qtig is the heat input (kJ/mm) during TIG welding, η is the arc vere corrosion sites in the heat affected zone of TIG weld joint.
efficiency, V is the voltage (volt), vs is the welding speed (mm/s) and I Potentiodynamic polarization corrosion test was performed on FSW
is the current (ampere). Different values of arc efficiency were calcu- and TIG weld joint and Tafel curve (Fig. 10) was obtained. Corrosion
lated in literature [20,21]. The value of arc efficiency used in this work potential of each zone of FSW and TIG weld joint observed from the
was 0.78 [22]. Different parameters used for heat input calculation are Tafel curve is shown in Table 5. More negative value of corrosion po-
shown in Table 4. Total heat input calculated during TIG welding was tential shows less corrosion resistance. In the present study, the
4
S. Sinhmar, D.K. Dwivedi Corrosion Science xxx (xxxx) xxx–xxx
corrosion potential of the nugget zone of FSW joint showed lower ne- Electrochemical impedance spectroscopy (EIS) is a most reliable
gative value compared to the other zones in case of both weld joints. non-destructive electrochemical technique [23]. Information revealed
Hence, the corrosion resistance of the nugget zone and HAZ of FSW by EIS technique are more than the potentiodynamic polarization test.
joint was higher than the TIG weld joint. This technique provides an average electrochemical response across the
5
S. Sinhmar, D.K. Dwivedi Corrosion Science xxx (xxxx) xxx–xxx
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S. Sinhmar, D.K. Dwivedi Corrosion Science xxx (xxxx) xxx–xxx
Table 4
Process parameters used for heat input calculation.
FSW TIG
compared to the fusion zone (Fig. 4a) and HAZ (Fig. 4b) of TIG weld
joint. Small grain size provided the large grain boundary area and fa-
cilitated more passivation which in turn reduced the corrosion current.
Thus, nugget zone showed more passivation than the fusion zone of TIG
weld joint. These results are in agreement with Ralston et al. [30] who
showed that the small grain size of aluminium led to more passivation
which in turn improved the corrosion resistance of the material. Pas-
sivation due to the grain refinement and its effect on corrosion were
reported elsewhere and described schematically [31]. The finer grain
size of the nugget zone of FSW joint corresponded to higher corrosion
resistance, whereas largest grain size of the heat affected zone of TIG
weld joint among all the zones corresponded to the lower corrosion
resistance. Hence, corrosion resistance can be related with the refine-
ment of microstructure, which in turn reduces the corrosion reactivity
by improving the passivation.
Fig. 8. Showing microhardness variation along the cross-section of FSW joint and TIG Presence of intermetallic particles/precipitates in the micro-
weld joint. structure of aluminium alloys affects the mechanical as well as corro-
sion behavior. Copper deleteriously affects the corrosion performance
of the alloy by forming a galvanic cell of copper rich zone and copper
the electrochemical potential of the aluminium matrix is more active
depleted zone [32]. In AA2014 aluminium alloy, Al2Cu forms a gal-
(anode) compared to the Al2Cu precipitate (cathode), which in turn
vanic cell with the Al- matrix due to the large potential difference. So,
leads to the dissolution of the aluminium matrix [29]. The proposed
this is the preferential site for corrosion reaction to occur. The positive
mechanism of pitting is schematically shown in Fig. 14. The potential
potential of the Al2Cu precipitate compared to the Al-matrix favors the
difference between the aluminium matrix and Al2Cu precipitate is large
reduction reaction to occur. Welding process changes the micro-
which led to the corrosion of α-Al matrix adjacent to the Al2Cu pre-
structure in the nugget zone/fusion zone of the weld joint. Most of the
cipitate and resulted in pit formation. The grain size of the α-Al matrix
time grain coarsening occurs in the heat affected zone (Figs. Figure 3b
of nugget zone (Fig. 3a) and HAZ (Fig. 3b) of FSW joint was finer as
and Figure 4b) along with the reversion of precipitates due to thermal
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S. Sinhmar, D.K. Dwivedi Corrosion Science xxx (xxxx) xxx–xxx
Fig. 10. Potentiodynamic polarization curves of different zones of (a) FSW joint, and (b) TIG weld joint.
Table 5 Table 6
Results obtained from Potentiodynamic polarization test of FSW and TIG weld joints. EIS data of FSW and TIG weld joint extracted from the equivalent circuit.
FSW NZ FSW HAZ TIG FZ TIG HAZ Rs (Ω) Rp (Ω cm2) Yo (Ω−1 cm−2 sn) n
Ecorr (mV) −659 −675 −692 −741 FSW NZ 14.76 3270 1.16 × 10−5 0.92
FSW HAZ 15.30 2152 2.126 × 10−5 0.84
TIG FZ 15.71 1920 6.76 × 10−5 0.89
cycles of the welding. Size of the precipitates in nugget zone of FSW TIG HAZ 15.65 1579 6.78 × 10−5 0.89
joint (Fig. 5a) was finer as compared to the fusion zone of TIG weld
joint (Fig. 5b) due to the plastic deformation and dynamic re-
of coarse precipitates and precipitate free zone (PFZ) with the corrosion
crystallization occurred during the friction stir welding. This size dif-
susceptibility of the material [33]. In both types of welding, heat af-
ference in precipitates is evident from Fig. 15. The TEM micrographs of
fected zone experienced dissolution and coarsening of the precipitates.
nugget and fusion zone along with the selected area diffraction (SAD)
However, the peak temperature experienced was more in case of the
pattern (Fig. 15b) taken from nugget zone of FSW joint are shown in
TIG weld joint, which resulted into the more coarsening of precipitates
Fig. 15a and c, respectively. Plane (310) observed from the SAD pattern
within grains and at the grain boundary of the heat affected zone
ring was corresponding to the Al2Cu precipitates and it is in agreement
(Fig. 5e and f).
with the XRD analysis (Fig. 6). Previous studies correlated the presence
Microhardness profile of the both weld joints is showing that the
Fig. 11. EIS test results of FSW and TIG weld joint as (a) Nyquist plot, (b) bode plot, and (c) equivalent circuit for fitting the EIS data.
8
S. Sinhmar, D.K. Dwivedi Corrosion Science xxx (xxxx) xxx–xxx
weld joint (Fig. 7b) caused reversion and coarsening of precipitates and
α-Al matrix (Fig. 5b and e). Furthermore, the higher temperature ex-
perienced during TIG welding compared to the friction stir welding led
to the sensitization of microstructure and the presence of Cu was in-
creased at grain boundary in form of coarse Al2Cu precipitates (Fig. 5f).
Hence, the corrosion resistance of the FSW joint was higher as com-
pared to the TIG weld joint of AA2014.
4. Conclusions
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S. Sinhmar, D.K. Dwivedi Corrosion Science xxx (xxxx) xxx–xxx
Fig. 14. Schematic of different stages of pitting process in a material having matrix as anode and precipitates as cathode.
Fig. 15. Showing (a) TEM micrograph of nugget zone of FSW joint, (b) SAD pattern of nugget zone shown in ‘a’, and (c) TEM micrograph of fusion zone of TIG weld joint.
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S. Sinhmar, D.K. Dwivedi Corrosion Science xxx (xxxx) xxx–xxx
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