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Abstract
An experimental investigation has been carried out, in present paper, on microstructure and corrosion resistance of weld butt joints of
AA 2024-T3. Two different welding processes have been considered: a conventional tungsten inert gas (TIG) process and an innovative
solid state welding process known as friction stir welding (FSW). Micro-hardness measurements allow pointing out a general decay of
mechanical properties of TIG joints, mainly due to high temperatures experienced by material. In FSW joint, instead, lower temperatures
involved in process and severe plastic deformations induced by tool motion allow rising of a complex situation: by a general point of view
a slight decay of mechanical properties is recorded in nugget zone, flow arm and thermo-mechanically altered zone (TMAZ), while in
heat-affected zone (HAZ), due to starting heat treatment of alloy under investigation, a light improvement of such properties is appreciated.
In flow arm and in nugget zone, however, a light recovery of hardness, w.r.t. TMAZ zone, is recorded, due to the re-crystallisation of a
very fine grain structure. Polarisation curve tests and electrochemical impedance spectroscopy, performed in this paper, allow assessing a
generalised nobler behaviour of weld bead with respect to parent alloy. In FSW joint, however, the differences between the three examined
zone are not so evident as in TIG joint; what is more, inside FSW weld bead, retreating zone shows a behaviour nobler than advancing one.
© 2004 Elsevier B.V. All rights reserved.
Keywords: Welding; Tungsten inert gas; Friction stir; Pitting corrosion; Polarisation curve test; Electrochemical impedance spectroscopy
0924-0136/$ – see front matter © 2004 Elsevier B.V. All rights reserved.
doi:10.1016/j.jmatprotec.2004.03.022
98 A. Squillace et al. / Journal of Materials Processing Technology 152 (2004) 97–105
Focusing attention on FSW, the structure of full weld expose only a single surface to the aggressive solution. Then
zone, due to severe mechanical stresses experienced by ma- they have been electrically connected with a copper wire,
terial, shows an interesting variety of zones. The sight of set in a glass tube (it also embedded in resin), by a conduc-
weld bead, across the section, shows a region of deep defor- tive epoxy resin (Technovit 5000 KULZER HERAEUS® ).
mation that is often referred to as the nugget zone [2,7,8]: All specimens have been machined with emery papers up
this zone shows a very fine grain structure [8] and is char- to no. 1200, washed with distilled water and then polished
acterised by the presence of so-called onion rings. The thin with a degreaser to have a smooth surface.
zone subjected directly to the action of tool shoulder is re- Instrumental Vickers micro-hardness measurements have
ferred to as flow arm. Adjacent to the nugget zone is a zone been performed through the weld zone at different depths;
that, though has been not directly subjected to pin or shoul- a LEITZ WETZLER® durometer has been used with a load
der action, due to internal shear stresses, has experienced of 300 g. Impressions have been done with 0.5 mm step for
a severe thermo-mechanical alteration, this zone is referred each line.
to as TMAZ. Beyond this zone is that part of material that Two different electrochemical tests have been conducted
has been subjected only to thermal alterations, this zone is in 3.5 wt.% NaCl aqueous solution: polarisation curves (PC)
usually referred to as HAZ. The sight of the top surface of corrosion testing, performed to assess the pitting resistance
the weld bead, shows semicircular rings referred as banded by recording anodic and cathodic, and electrochemical
microstructure; the distance between such rings depends on impedance spectroscopy (EIS) testing, performed to evalu-
tool advance per revolution: band spacing will increase as ate surface’s performances. The electrochemical cell used is
this ratio grows, resulting in a less homogenous structure a 2l volume flask; solution has been stirred by air (aerated
within the weld [9]. solution) or nitrogen (deaerated solution) flow during each
Corrosion resistance of AA 2024 has been widely inves- test. The specimen represents the working electrode, while
tigated, especially its susceptibility to pitting phenomenon two platinum wires, symmetrically disposed with respect to
[10,11]; to authors knowledge, however, few data are re- specimen under investigation, served as the counter elec-
ported in literature about corrosion resistance of welded trode; a saturated calomel reference electrode (SCE) has
joints of this alloy [12]. In this research each of alterated been employed. Experiments have been conducted at room
zones above described, due to both welding processes un- temperature. After immersion, first the potential has been
der consideration, have been specifically characterised, and allowed to stabilise, and then, after 1 h immersion, the test
performances provided by the entire joints are proposed. started.
PC tests have been conducted in both aerated and deaer-
ated solutions. Data have been obtained using a potentio-
2. Materials and methods stat EG&G® Princeton Applied Research Corp. Model 273
which consists of a complete hardware that measures the re-
The material under investigation is a commercial alu- sponse of an electrochemical system to dc excitation (soft-
minium alloy Al 2024-T3. Two thickness plates have been ware package Corrosion Software M352); the hardware in-
investigated: 2 and 3 mm. Simple butt weld joints have been cludes a potentiostat as electrochemical interface, a personal
realised, in room conditions, along lamination direction, ei- computer, and the electrochemical cell. Potential range in-
ther by TIG (2 mm plates) and FSW (3 mm plates). vestigated was −1000/ − 400 mV versus SCE for tests in
TIG joints have been realised autogenously, i.e. without aerated solutions and −1400/−600 mV versus SCE for tests
filler material, with a Miller 375p ac arc-welding power in deaerated solutions, both with a rate of 0.5 mV/s. Tests
source with a 380 V input and an air-cooled internal trans- have been conducted on three main zones (parent alloy, heat
former. Detailed parameters are: voltage10 V, welding cur- affected zone and weld bead) belonging to each kind of joint.
rent 157–158 A (42% of maximum amperage 375 A), argon EIS tests have been conducted in aerated solution only,
as shield gas (flow rate 20 l/min), electrode WP 1.60 mm × using a Solartron Frequency Response Analyser (FRA)
1.75 mm ISO 6848. Model 1260 and an electrochemical interface, potentiostat
About 3 mm panels have been friction stir welded using Solartron 1287, including a personal computer with a GPIB,
a DORMAC milling machine mod. FU110. The tool (car- and the electrochemical cell. Measurements have been per-
bon steel C40) shoulder diameter is 18 mm and the pin is formed starting from the 0.02 Hz up to 105 Hz, at 10 data
a truncated cone (6.5 mm base and 5.5 mm head diameter) cycles/decade, 5 mV ac amplitude and with an average si-
2.9 mm height. The tool rotational speed has been set equal nusoid curve value equal to the open circuit potential, i.e.
to 1600 rpm and translation speed equal to 80 mm/min. corrosion potential.
TIG and FSW joints have been sectioned in transverse
direction to obtain the specimens. These ones have been
cut along welding direction, to separate the weld bead and 3. Results and discussions
heat-affected zone (HAZ) from parent alloy. For electro-
chemical measurements, specimens have been embedded in It is well known that, in case of TIG welding, due to the
epoxy resin (Technovit 3040 KULZER HERAEUS® ) so to fusion of material and high temperatures experienced by
A. Squillace et al. / Journal of Materials Processing Technology 152 (2004) 97–105 99
Fig. 1. Macrography of TIG weld: (1) weld bead; (2) HAZ; (3) unaffected zone.
adjacent material a fairly wide HAZ appears (see Fig. 1), of mechanical properties, and this happens only in nugget
in which parent hardening precipitates experience a kind zone and, above all, in flow arm zone. Moving from centre
of over-ageing, causing phase transformations (θ → θ ) of weld bead toward unaffected material, after TMAZ there
[1], resulting into a general loss of mechanical proper- is the HAZ: in such a zone of FSW joints realised on an alu-
ties, as confirmed by decay in micro-hardness measures minium alloys similar to that under investigation in present
(see Fig. 2). research, i.e. in T3 condition, the low temperatures expe-
During the realisation of FSW joints, instead, two differ- rienced can induce a kind of ageing, resulting into a light
ent phenomena have to be taken into account, each of them increase of mechanical characteristics. As a matter of fact,
leading to different conclusion. By one side the tempera- by viewing micro-hardness map of FSW joint, Fig. 4, low-
tures experienced by material involved in welding process, est values regard TMAZ; values of stirred material (nugget
though lower than melting one, induce phase transforma- and flow arm zones) appear slightly higher than previous
tions leading to same considerations drawn for TIG joints ones, while values of HAZ are slightly higher than those of
and the result is still a decay of mechanical properties, this unaffected material.
situation regards nugget zone, flow arm zone and TMAZ, Results of PC tests, conducted on TIG joint are graphi-
Fig. 3; on the other hand, great shear stresses induced by cally reported in Figs. 5 and 6, while main measured data
tool motion lead to the generation of a very fine grain struc- are collected in Table 1. The highest Ecor,A value attained
ture [2], see again Fig. 3, which allows a partial recovery by parent alloy indicates that such material is the noblest
Fig. 3. Macrography of FSW weld: (1) nugget zone; (2) flow arm; (3) TMAZ; (4) HAZ; (5) unaffected zone.
100 A. Squillace et al. / Journal of Materials Processing Technology 152 (2004) 97–105
Fig. 5. Anodic and cathodic PC of parent alloy, HAZ and weld bead of TIG welded specimen in 3.5% NaCl aerated solution.
one. For all zones under investigation, an Epit,D value lower other two zones pits would tend to be generated, but a shield
than Ecor,A value has been found, this means that all zones action, provided by corrosion products themselves, prevents
are subjected, in equilibrium conditions, to pitting corro- this occurrence.
sion. Turning, then, attention on last column of above men- Focusing attention in Fig. 6, weld bead show an higher
tioned table, the value of difference between two potentials ipit,D value than HAZ and parent alloy: this means that just in
increases moving from weld bead to parent alloy. Such re- this zone a greater number of pits would tend to be generated
sults indicate that, in equilibrium condition, the general ten- than in other two zones.
dency of entire joint is towards pitting corrosion, but while Turning attention on FSW joint, Table 2 shows, one more
in parent alloy pits are generated and then they increase, in time, a parent alloy Ecor,A value greater than the others. It
A. Squillace et al. / Journal of Materials Processing Technology 152 (2004) 97–105 101
Fig. 6. Anodic and cathodic PC of parent alloy, HAZ and weld bead of TIG welded specimen in 3.5% NaCl deaerated solution.
Table 1 as confirmed by Fig. 7; but, this time, both HAZ and weld
Measured main potentials, during PC test, for TIG joint bead show an Ecor,A value lower than Epit,D value: this means
Ecor,A (mV) Epit,D (mV) Ecor,A −Epit,D (mV) that, in equilibrium conditions, both HAZ and weld bead
Parent alloy −690 −714 24
show a passive behaviour, while parent alloy shows again a
HAZ −701 −709 8 well developed pitting phenomenon. What is more, in FSW
Weld bead −701 −705 4 joint, the HAZ shows the greatest ipit,D value, Fig. 8, then
Table 2
Measured main potentials, during PC test, for FSW joint
Ecor,A (mV) Epit,D (mV) Ecor,A −Epit,D (mV)
Fig. 7. Anodic and cathodic PC of parent alloy, HAZ and weld bead of FSW Fig.
welded specimen
8. Anodic andincathodic
3.5% NaCl aerated
PC of parentsolution.
alloy, HAZ and weld bead of FSW welded specimen in 3.5% NaCl deaerated solution.
102 A. Squillace et al. / Journal of Materials Processing Technology 152 (2004) 97–105
the oxide layer of this zone is characterised by the greatest side, as well as weld bead, shows a passive behaviour, while
number of defects. advancing side, shows a slight pitting phenomenon. To con-
To take into account the asymmetric nature of FSW pro- clude, the advancing side shows also the greatest ipit,D value,
cess, a further series of tests has been carried out on speci- so same considerations above mentioned can be drawn.
mens cut respectively from advancing and retreating part of Results of EIS tests, carried out on TIG welded specimens,
weld bead. Results are reported in Figs. 9 and 10 and data are graphically reported in Fig. 11. The value of Eoc of these
are collected in Table 3. In equilibrium conditions retreating tests has been set equal to −716 mV, with an oscillation
Fig. 9. Anodic and cathodic PC of total weld bead, retreating side and advancing side of FSW welded specimen in 3.5% NaCl aerated solution.
Fig. 10. Anodic and cathodic PC of total weld bead, retreating side and advancing side of FSW welded specimen in 3.5% NaCl deaerated solution.
Fig. 11. Bode plots of impedance vs. frequency for parent alloy, HAZ and weld bead of TIG welded specimen in 3.5% NaCl aerated solution.
A. Squillace et al. / Journal of Materials Processing Technology 152 (2004) 97–105 103
Table 3
Measured potentials for advancing and retreating side and total weld bead
of FSW joint
Ecor,A (mV) Epit,D (mV) Ecor,A −Epit,D (mV)
Fig. 14. Bode plots of impedance vs. frequency for parent alloy, HAZ and weld bead of FSW welded specimen in 3.5% NaCl aerated solution.
104 A. Squillace et al. / Journal of Materials Processing Technology 152 (2004) 97–105
Table 4
Values of main electrical components belonging to equivalent circuits of TIG joint
Rsol () Rox () Rct () L (H) CPEox (F/cm2 )·Hz1−α α CPEAl (F/cm2 )·Hz1−α α
Fig. 15. Bode plots of impedance vs. frequency for total weld bead, retreating side and advancing side of FSW welded specimen in 3.5% NaCl aerated
solution.
Fig. 16. (a) Equivalent circuit for retreating side and (b) for both global weld bead and advancing side of FSW joint.
Table 5
Values of main electrical components belonging to equivalent circuits of FSW joint
Rsol () Rox () Rct () L (H) CPEox (F/cm2 )·Hz1−α α CPEAl (F/cm2 )·Hz1−α α
Acknowledgements [5] W.M. Thomas, et al., Friction stir butt welding, International Patent
Application No. PCT/GB92/02203, December 1991.
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The authors want to thank Alenia Aeronautica for provid- Neutron and synchrotron measurements of residual strain in TIG
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167.
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