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Journal of Manufacturing Processes 30 (2017) 27–40

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Journal of Manufacturing Processes


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Full length article

Microstructure, mechanical properties and biocorrosion behavior of


dissimilar welds of AISI 904L and UNS S32750
K. Devendranath Ramkumar a,∗ , Akash Harendra Dagur a , Ashwin Anil Kartha a ,
Moharil Atharva Subodh a , C. Vishnu a , D. Arun a , M. Giridharan Vijay Kumar a ,
Winston Sunny Abraham a , Ankita Chatterjee b , Jayanthi Abraham b , Johann Abraham a
a
School of Mechanical Engineering, VIT University, Vellore – 632014, India
b
School of Bio-Sciences and Technology, VIT University, Vellore – 632014, India

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

Article history: This article addresses the joining of 5 mm thick plates of marine grade, super-austenitic (AISI 904L) and
Received 19 June 2017 super-duplex stainless steels (UNS S32750) by pulsed current gas tungsten arc welding using duplex
Received in revised form 29 August 2017 and austenitic stainless steel fillers. Microstructure studies revealed the segregation of Mo-rich phases
Accepted 1 September 2017
in the fusion zone while employing ERNiCrMo-10. Grain coarsening was observed at the heat affected
Available online 18 September 2017
zone (HAZ) of super-duplex stainless steel in both the cases. The study attested that all the tensile fail-
ures experienced in the parent metal, AISI 904L for both the weldments. Charpy V-notch impact studies
Keywords:
demonstrated that the weldments employing ER2553 were experienced better impact toughness than
Super-duplex stainless steel
Super-austenitic stainless steel ERNiCrMo-10 weldments. Further potentiodynamic polarization test in 3.5% NaCl environment was con-
Pulsed current gas tungsten arc welding ducted on the coupons of the weldments. The coupons of the weldments were then tested for accelerated
Microstructure corrosion in salt fog chamber for 300 h in 3.5% NaCl environment. This accelerated corrosion test con-
Microbial- induced corrosion cludes that the parent metal AISI 904L experienced better corrosion resistance than the fusion zones. The
investigation also deals with biocorrosion studies of the dissimilar welds of super-austenitic and super-
duplex stainless steels. Microbial consortium comprising of six bacterial isolates of which four were
Pseudomonas strains P. aeruginosa strain MB1, P. aeruginosa strain MB2, P. fluorescens and P. flavescens,
two belonged to Bacillus strains, B. subtilis and B. cereus, for the first time. The bacterial isolates were
inoculated in the medium with the presence of the metal coupons. The results were obtained after 15
and 30 days interval and compared with the control to determine the rate of biocorrosion which confirms
that there is an accelerated deterioration of the metal coupons by the microbial strains.
© 2017 The Society of Manufacturing Engineers. Published by Elsevier Ltd. All rights reserved.

1. Introduction on employing low heat inputs and faster cooling rates as observed
in high energy density processes such as electron beam welding
Dissimilar welding of super-duplex stainless steel (SDSS) grade (EBW) or laser beam welding (LBW), the fusion zone was enriched
UNS S32750, and super-austenitic stainless steel (SASS), grade with higher amounts of ferrite and intense precipitation of Cr2 N [2].
AISI 904L are widely employed in marine and offshore applica- Similarly higher heat inputs and slow cooling rates would cause the
tions owing to their excellent mechanical strength and corrosion precipitation of brittle intermetallic phases such as ␴ (Sigma) or ␹
resistance in the alkaline environment. As individual candidate (chi). However, this phase will emerge only when they are exposed
materials, both UNS S32750 and AISI 904L are readily weldable. to a temperature of 600–1000 ◦ C for extended periods of time
However, there are some critical issues in the welding of these met- [3–8]. The Cr2 N precipitation deteriorates the corrosion resistance
als. One of the major challenges involved in welding of UNS S32750 and the ␴ phase has profound effect in deteriorating the impact
is to obtain 50% austenite in the fusion zone and the key factor in toughness. Devendranath et al. [9] compared the microstructure,
achieving the higher austenite content without deleterious phases tensile strength and impact toughness of gas tungsten arc (GTA)
is the heat input and cooling rate [1]. Researchers connoted that welds of UNS S32750 employing ER2553 and ERNiCrMo-4. The out-
comes of the study signified that the weldments employing ER2553
imparted higher tensile strength and impact toughness compared
∗ Corresponding author. to ERNiCrMo-4 weldments and EB weldments by the same authors
E-mail addresses: deva@vit.ac.in, ramdevendranath@gmail.com (D.R. K.). [10].

http://dx.doi.org/10.1016/j.jmapro.2017.09.001
1526-6125/© 2017 The Society of Manufacturing Engineers. Published by Elsevier Ltd. All rights reserved.
28 D.R. K. et al. / Journal of Manufacturing Processes 30 (2017) 27–40

Similarly, AISI 904L receives major attention in the marine appli- 40 days. Studies showed that austenite phase was found to be more
cations owing to their excellent corrosion resistance. The presence susceptible to SRB-influenced corrosion.
of high Mo content along with the increased levels of Cr, N, and Cu It can be concluded that although both the candidate metals
causes this grade of stainless steel to have excellent resistance to offer good weldability, there are issues related to the formation of
pitting, crevice, and chloride stress corrosion cracking. The major deleterious phases and segregation of Mo. It is always desirable
problem reported during welding of AISI 904L is the segregation to have more austenite content in the fusion zone while welding
of Mo in the inter-dendritic regions of the fusion zone, owing to SDSS; however, it is difficult to obtain as it requires proper heat
its lower solubility in ␥ phase. This micro-segregation led to the inputs and moderate cooling rates. As these metallurgical phases
depletion of Mo in the dendritic cores and dramatically reduced the contribute to lowering the corrosion resistance at the fusion zone,
mechanical properties and resistance to localized corrosion attack. a study is needed to improve the fusion zone microstructure with
Studies showed that the use of Ni-Mo rich filler circumvents the higher amounts of austenite and also to reduce Mo depletion from
problem of segregation to a certain extent [11,12]. Devendranath the dendritic cores. The previous studies have reported the join-
et al. [13] investigated the pulsed current GTA welding of AISI 904L ing of austenitic/super-austenitic and super-duplex combinations,
employing four different fillers namely ERNiCrMo-4, ERNiCrMo- without having a specific emphasis on the fusion zone microstruc-
10, ERNiCrMo-14, and ERNiCu-7. The authors attested that both ture and its corrosion performance in the marine environment.
ERNiCrMo-10 and ERNiCrMo-14 weldments displayed lower seg- One of the welding approaches in lowering the segregation and
regation and improved corrosion resistance than the base metals. improving the grains is to make use of pulsation current in the GTA
Mehdi Rahmani et al. [14] investigated the gas tungsten arc welding process. This pulsation causes the periodic changes in the
welding of austenitic stainless steel (AISI304L) and super-duplex current, which allows sufficient time for melting and solidification.
stainless steel (UNS S32750) employing ER2594 and ER309L Mo Researchers have observed and reported the advantages in terms of
fillers. Devendranath et al. [15] employed filler-less, activated considerable grain refinement, minimized segregation, improved
flux tungsten inert gas (ATIG) welding for joining 5 mm thick mechanical properties and corrosion resistance.
plates of AISI 316L and UNS S32750 in a single-pass. Further, the Hence this study is attempted with the use of PCGTA weld-
authors reported the joint strength was better than the weak par- ing process to join dissimilar marine grade stainless steels namely
ent metal, AISI 316L. Although the aforementioned research works AISI 904L and UNS S32750 employing two fillers ER2553 and
have addressed the dissimilar joints of austenitic and super-duplex ERNiCrMo-10. Microstructure studies are carried out using optical
stainless steel, limited efforts have been laid to investigate the microscopy (OM) and scanning electron microscopy (SEM) tech-
microstructure, mechanical properties and corrosion studies of niques. Mechanical properties of the dissimilar weldments are
SDSS/SASS combinations, thus far. Zhiliang Zhou and Johan Löth- ascertained by conducting hardness, tensile and impact tests. Fur-
man [16] recently performed the studies on GTA welding of 12 mm ther potentiodynamic polarization test using 3.5% NaCl and salt
thick super-duplex stainless steel 2507 (UNS S32750) to super- spray corrosion studies are also carried out to assess the corro-
austenitic stainless steel (UNS S31254) using nickel alloy filler sion behavior of the weldments. This study also addressed the MIC
materials ERNiCrMo-13, ERNiCrMo-3 and super-duplex stainless studies on the dissimilar welds of SASS and SDSS by exposing it for
steel filler, ER2594. The authors observed grain coarsening as well 15 and 30 days in the medium containing Gram positive bacteria
as unmixed zones at the HAZs of 2507 and 6 Mo stainless steel sides. Bacillus cereus, Bacillus subtilis, and Gram negative bacteria Pseu-
The authors recommended the use of ERNiCrMo-13 for joining domonas flavescens, P. fluorescens, Pseudomonas aeruginosa strain
these dissimilar grades of stainless steels owing to better mechan- MB1, Pseudomonas aeruginosa strain MB2. SEM/EDAX analysis was
ical properties and pitting corrosion resistance. performed to understand the corrosion behavior of the welds. The
Microbial influenced corrosion (MIC) is one of the serious cor- outcomes of the study will be highly beneficial to the marine and
rosion problems in the marine structures which results in a huge offshore applications employing these dissimilar joints.
economic loss and accounts for 20% of the corrosion damages [17].
As reported by the above mentioned authors, MIC is not being
treated as a distinct type of corrosion form, but rather is the syn- 2. Experimental procedure
ergistic contact of microorganisms, that results in biofilms and
metabolic products that enhance corrosion processes. Little and Lee 2.1. Base metals and welding
[18] reported the types in morphology of MIC, as follows; local-
ized pitting, crevice corrosion, under deposit corrosion, cracking, The base metals employed in the study are the hot rolled,
enhanced erosion corrosion and de-alloying etc. Although duplex 5 mm thick plates of AISI 904L and UNS S32750 and the chemi-
stainless steel exhibit better-pitting corrosion resistance, the stud- cal composition of the base metals are established using optical
ies showed that DSS are vulnerable to MIC attack [19,20] in the emission spectroscopy (OES) technique. The fillers employed in the
environments containing sulphate reducing bacteria (SRB), iron current study are ER2553 and ERNiCrMo-10 of 1.6 mm diameter.
reducing bacteria (IRB), etc. It is strongly believed that these bac- These filler metals are chosen mainly to improve the fusion zone
teria cause localized pitting corrosion on surfaces under biofilm of microstructures with more austenite and to minimize Mo segre-
DSS [21,22] owing to the presence of nitrogen content. Huabing Li gation. The nominal chemical composition of the base and filler
et al. [23] investigated the corrosion behavior of super-austenitic metals are represented in Table 1.
stainless steel (S32654) caused by a corrosive marine bacterium The as-received plates were machined to rectangular plates
Pseudomonas aeruginosa. The authors reported that the corrosion of 170 mm × 55 mm × 5 mm using wire-cut electrical discharge
rate is accelerated by observing the pits after exposure for 14 days. machining (WEDM) process. The samples were acid pickled to
Although MIC studies have been conducted on the base metals make the surfaces free from organic (grease, paint, dirt) and
of the duplex, ferritic, and austenitic stainless steels by the vari- metallic residual contamination. Before welding, standard V-Butt
ous authors, the information available on the MIC performance of configurations (single V-groove with a root gap of 2 mm, size land
the welded joints is scanty. Anthony et al. [24] investigated the of 1 mm and included angle 60◦ ) were employed on the samples.
MIC corrosion behavior of 6 mm welds of 2205 duplex stainless High purity (99.9% pure) argon gas was used for shielding and back
steel using sulphate reducing bacteria, Desulfovibrio desulfuricans. purging with the flow rates of 15 and 5 lpm respectively. The diame-
Potentiodynamic polarization studies were carried out in 3.5% NaCl ter of the tungsten electrode was 1.6 mm and the tip angle was 60◦ .
at 30 ◦ C and were pre-exposed in the medium containing SRB for These dissimilar plates were mechanically clamped by providing
D.R. K. et al. / Journal of Manufacturing Processes 30 (2017) 27–40 29

Table 1
Chemical composition of the base and filler metals.

Chemical Composition (% by weight)

Base or Filler Metal C Si Mn Cr Mo Ni Cu Fe Others

UNS S32750 0.025 0.28 0.86 25.0 3.6 6.55 0.18 Rem. P – 0.037; V – 0.077; Co – 0.05; N-0.28; Nb – 0.05
AISI 904L 0.019 0.37 1.39 20.3 4.1 23.11 1.26 Rem P – 0.017; S – 0.004
ER2553 0.04 1.0 1.5 25.5 3.4 5.5 2.0 Rem P – 0.04; S – 0.03; N – 0.18
ERNiCrMo-10 0.015 0.05 0.55 22.4 14.0 Rem. 0.2 2.5 P – 0.00001; S – 0.001; Co – 0.22; V – 0.01; W – 3.34

Table 2
Process parameters employed in PCGTA welding of UNS S32750 and AISI 904L.

Filler metal Pass Peak Current Background current Voltage Frequency Duty Cycle Heat input Cumulative Heat input
(A) (A) (V) (Hz) (kJ/mm) (kJ/mm)

ER2553 Root 140 80 10.0–11.5 6 50% 0.472 2.458


Filling pass 1 140 80 9.5–11.0 6 50% 0.643
Filling pass 2 140 80 9.5–11.5 6 50% 0.577
Filling pass 3 140 80 9.6–10.6 6 50% 0.486
Cap 140 80 10.0–11.3 6 50% 0.281

ERNiCrMo-10 Root 140 80 9.7–11.3 6 50% 0.528 2.740


Filling pass 1 140 80 9.4–10.5 6 50% 0.750
Filling pass 2 140 80 9.6–10.9 6 50% 0.633
Filling pass 3 140 80 9.6–10.5 6 50% 0.488
Cap 140 80 10.2–11.2 6 50% 0.342

adequate gripping and were held in the fixture utilizing Cu back trolytically etched using 10% oxalic acid for 10 s by keeping 6 V
plates with grooves, for facilitating the flow of purging gas. DC supply and a current density of 1.6 A cm−2 . The interface and
Multi-pass PCGTA welding process was carried out to join these fusion zone microstructures of both the weldments were investi-
plates with a frequency of 6 Hz. The peak and background currents gated using OM and SEM techniques. Qualitative analysis on the
were set to 140 and 80A respectively for all the passes in both the chemical composition or characterization of the phases was done
cases. At the end of every pass, the fusion zone was cleaned using a using Energy dispersive x-ray spectroscopy analysis (EDAX).
wire brush to remove the inter-pass oxides. The process parameters
employed in the study and the heat input developed during the
2.3. Mechanical characterization of dissimilar weldments
multi-pass welding of SASS/SDSS are represented in Table 2.
The heat input of the PCGTA welding is calculated using the
Hardness measurements were carried out on the transverse
formula given below.
coupons of the weldments having dimensions similar to the ones
Im × V employed in microstructural studies. The hardness readings were
HI = ␩ × (1)
S taken across the entire width of the weldments at regular inter-
The mean current, Im can be calculated from the following vals of 0.25 mm using Vickers microhardness tester. A standard test
expression load of 500 gf was applied for a dwell time of 10 s using a square
pyramidal diamond indenter. Measurements were taken at differ-
(Ib × tb) + (Ip × tp) ent passes vis-à-vis cap, filling and root etc. to assess the precise
Im = (2)
(tb + tp) changes in the hardness values.
Where HI, heat input (kJ/mm); Im, mean current (A); V, Voltage (V); Further uniaxial tension tests were performed on the coupons
S, Welding speed (mm/min.); tb, tp are the pulse time durations for fabricated according to ASTM: E8/8 M standards. Tensile properties
background and peak current (s); Ib, Ip are background and peak were estimated by setting the cross-head velocity to 2 mm/min. so
currents respectively (A) and ␩ – arc efficiency which is considered as to induce a lower strain rate of 3.3 × 10−4 s−1 as prescribed for
to be 60% for PCGTAW. sub-sized samples by Davis et al. [25]. Tensile properties include
Followed by welding, the welded joints were subjected to 0.2% offset yield strength, ultimate tensile strength, and percent-
non-destructive testing (NDT) techniques including gamma ray age elongation were determined for the dissimilar weldments.
radiography and dye penetrant test to determine the flaws on the Room temperature, Charpy V-notch impact studies were carried
surface or sub-surface of the weldments. Further, the weldments out on the transverse coupons fabricated as recommended by ASTM
were machined to coupons of various dimensions according to the E23:12C standard. Notches were made at the center of the fusion
ASTM standards for conducting the mechanical and corrosion tests. zone (cap zone) so as to confine the impact loading to the notched
regions. The average tensile properties and impact toughness of the
dissimilar weldments were computed by performing three trials in
2.2. Metallurgical characterization of dissimilar weldments
each test to obtain the repeatability in the results.
Microstructure studies were performed on the samples of
dimensions of 28 mm × 10 mm × 5 mm, machined perpendicular to 2.4. Corrosion studies
the welding direction, using WEDM. The transverse cross-section
samples cover all the regions vis-à-vis base metals, fusion zone, 2.4.1. Potentiodynamic polarization and salt spray studies
and heat affected zones of the weldments. Standard metallographic The electrochemical test was performed on the identical sam-
procedures were adopted on the samples which include mechani- ples of base metals and the fusion zones of the dissimilar weldments
cal polishing with emery sheets of various grit sizes and followed of cross-section area 10 × 10 mm2 fabricated according to ASTM G
by disc polishing using alumina-distilled water solution to get the 59–97 standard. The coupons were polished using emery sheets
scratch-free, mirror-like surfaces. Both the weldments are elec- of various grit sizes and then disc polished to obtain a mirror-like
30 D.R. K. et al. / Journal of Manufacturing Processes 30 (2017) 27–40

Fig. 1. Microstructure of the parent metal (a) AISI 904L and (b) UNS 32750.

finish. A potentiostat was employed for the electrochemical tests The corrosion studies have been repeated for three times for
including the specimen as working electrode, saturated calomel as both potentiodynamic and salt fog tests.
a reference electrode and platinum wire counter electrode. Poten-
tiodynamic polarization studies were carried out on the coupons by
2.4.2. Microbial induced corrosion studies
exposing them to a 3.5% NaCl solution at ambient temperature to
The coupons of the dissimilar weldments were cut into the
determine the corrosion potentials. Further salt spray corrosion test
dimensions of 10 mm × 2 mm, which were then polished using
was conducted on the coupons fabricated according to ASTM B117
alumina powder to obtain mirror like finish on the surfaces.
standards. The coupons were exposed to 5% aqueous NaCl environ-
Four different coupons of the weldments, such as parent metal,
ment with an air pressure of 14–18 Psi and a pH of 6.65–6.85, at a
UNSS32750 (Sample A), weld zone of ER2553 filler (Sample B), par-
temperature of 35 ◦ C for 300 h. The weight of the samples before
ent metal, AISI904L (Sample C) and weld zone of ERNiCrMo-10 filler
and after exposure in salt spray corrosion was measured.
(Sample D) were employed in this microbial influenced corrosion
The corrosion rate (weight loss measurements) is measured
studies by exposing it for 15 and 30 days. The surface sterilization of
using the formula
the polished coupons was done with 70% ethanol. Trial 1, 4 strains
  of Pseudomonas sp. and coupons in MSM broth. Trial 2, 2 strains of
CRw = 8.76 × 104 × w / (A × D × T ) (3) Bacillus sp. and coupons in MSM broth and the trial 3, Pseudomonas
sp. and Bacillus sp. and coupons in MSM broth. A control trial was
Where w = weight loss in grams; A = surface area of the specimen maintained with coupons in MSM broth devoid of microbes. All
in cm2 ; D = density of the material in g/cm3 ; T = corrosion time in the three trials were performed on the various coupons of the
hours. weldments. In the natural environment, microbial biofilms are not
D.R. K. et al. / Journal of Manufacturing Processes 30 (2017) 27–40 31

Fig. 2. Interface microstructure of PCGTA welds employing ER2553 filler at (a) AISI 904L and (b) UNS S32750 side respectively.

composed of one bacterial species, rather several microbial species were removed after each 15 days to ascertain the constitution
coexist. Hence in the present study, a consortium of microbes was of biofilm on the surface of the coupons. As recommended by
used to understand the biofilm formation and subsequent corro- Rajasekar and Ting [27], SEM-EDAX analysis was also performed
sion on the metal substrate. All the bacterial strains were procured to determine the microbial growth on the metal surface after each
from Microbial Biotechnology Lab, SBST, VIT University. interval.
The growth pattern of the microbial consortium was studied
using 6 bacterial strains which were inoculated in mineral salt
3. Results and discussion
medium (MSM) broth and incubated for 24 h. Post incubation, 1 ml
of the bacterial culture was diluted to 10−1 and inoculated in MSM
3.1. Base metals
broth to check the growth curve after regular time intervals. The
change in growth pattern was observed by estimating the optical
SE microscopy of the base metals of UNS S32750 and AISI 904L
density at 600 nm [26].
are shown in Fig. 1. Fig. 1(a) shows Ni-rich austenitic matrix with
The welded coupons and the parent metals were inoculated
the twin boundaries which are the microscopic features of base
with Pseudomonas sp. and Bacillus sp. Pseudomonas included species
metal AISI 904L. The microstructure of SDSS having the islands
such as P. aeruginosa strain MB1, P. aeruginosa strain MB2, P. fluo-
of ferrite and austenite as observed from Fig. 1(b) having the dif-
rescens and P. flavescens whereas Bacillus comprised of B. subtilis
ferences in elemental compositions and the ferrite count analysis
and B. cereus. 100 ml of sterile mineral salt medium (MSM) broth
attested that the ferrite-austenite ratio of the base metal UNS
was inoculated with 1 ml (108 cells/ml) of the bacterial consortium.
S32750 is 52:48. The ultimate tensile strength of the base metals
The metal coupons were added to the MSM broth and incubated for
was found to be 875 MPa and 655 MPa for SDSS and SASS respec-
30 days. The corrosive environmental condition was maintained by
tively; similarly, the impact toughness at room temperature was
addition of 1% sodium chloride in the medium. A set of coupons
found to be 96 and 67 J respectively.
32 D.R. K. et al. / Journal of Manufacturing Processes 30 (2017) 27–40

mally improve hot cracking resistance. Moreover, the use of pulsed


current in the welding technique resulted in both grain detachment
and dendrite fragmentation which likely to form equiaxed grains.
SEM morphology of the fusion zone of ER2553 weldments
[Fig. 4(b)] exhibited clear distinction between the dendritic and
inter-dendritic regions of columnar grains. It is prominent from
the EDS analysis that there is not much variation in the chemi-
cal composition of the elements except Mo content. On the other
hand, SEM morphology showed the presence of intense precipi-
tates (appear as white in color) across the inter-dendritic regions
of the welds employing ERNiCrMo-10 filler [Fig. 5(b)]. It is to be
noticed that the greatest degree of micro-segregation occurs in the
columnar dendrites compared to the equiaxed dendrites. Further,
the EDS point analysis attested that the segregation observed in the
fusion zone are enriched with Mo, Cr and W. Owing to the lower
solubility of Mo in the austenitic (␥) phase, Mo segregates prefer-
entially in the liquid and thus retention of Mo in the inter-dendritic
arm spacing occurs. This is well supported by the findings of other
researchers [11,13,29]. Further, it is to be opined that the high seg-
regation tendency of the alloying elements Mo and W was due to a
large difference in the atomic radius of Ni and atomic radii of these
elements.

3.3. Mechanical characterization of the weldments

3.3.1. Hardness
Vickers microhardness studies were performed on the cross-
sectionally cut samples of the dissimilar weldments and the results
are represented in Table 3. It is observed from the hardness trend
shown in Fig. 6(a) and (b) that the hardness values are varying from
AISI 904L side to UNS S32750 side. A closer examination of the hard-
ness trend revealed that the average hardness value of the fusion
Fig. 3. Interface microstructure of PCGTA welds employing ERNiCrMo-10 filler at zone employing ER2553 exhibited almost similar value (192 HV)
(a) AISI 904L and (b) UNS S32750 side respectively. and that of the base metal, AISI 904L (182 HV) [Fig. 6(a)]. Whereas
the fusion zone employing ERNiCrMo-10 exhibited better hardness
3.2. Microstructure examination of the weldments than AISI 904L. However both the fusion zones exhibited lower
hardness than the base metal, UNS S32750. The increase in the
Interface microstructures of the dissimilar weldments employ- hardness at the fusion zone of ERNiCrMo-10 could be attributed
ing ER2553 filler are shown in Fig. 2(a) and 2(b). It is evident that to the presence of alloying elements Mo, W, Al, and Co. It is well
there is no significant grain growth observed at the HAZ of AISI 904L understood from the EDAX analysis that the concentration of Mo
for both the weldments. The presence of higher amounts of Ni in is higher both in the dendritic and inter-dendritic regions of the
AISI 904L prevents the grain growth as Ni serves as grain refiner. In fusion zone employing ERNiCrMo-10. As reported by Abdel Rahman
addition to this, the lower thermal conductivity and higher coeffi- et al. [30], Mo has a larger atomic size compared to other alloying
cient of thermal expansion of AISI904L compared to UNS S32750 elements, which increases the distortion of the matrix lattice and
facilitated for the absence of grain coarsening effect. However, increases the hardness value at the fusion zone. Further, the use of
coarser grains are observed at the interface of UNS S32750 for pulsed current GTA welding resulted in the formation of refined,
both the weldments, which is attributed to the effect of repeated intimate equiaxed grains which bolstered the hardness at the root
heating and cooling owing to multi-pass welding. The intense for- pass of both the weldments. Also, the maximum hardness experi-
mation of nitrides of Fe and Cr while employing ER2553 filler and enced in the investigated welded joint does not exceed 300 HV and
the formation of secondary austenite is observed at the HAZ of UNS is the mandatory requirement for super-duplex stainless steel as
S32750 while employing ERNiCrMo-10 filler respectively [Fig. 3(a) per NACE Standard MR0103 [31]. Similar results were reported by
and (b)]. Scare Mo, Ti-rich phases were observed at the fusion zone Zhiliang Zhou and Johan Löthman [16].
of ER2553 weldments. Fusion zones of the both the weldments
showed different grain growths such as columnar and equiaxed 3.3.2. Tensile and impact test
dendritic grains across the different passes [Figs. 4(a) and 5(a) ]. Fine Tensile test was conducted on both the base metals and the
equiaxed dendritic grains were observed at the middle and root PCGTA welds of UNS S32750 and AISI 904L employing different
pass of these weldments owing to the multi-pass, pulsed current fillers and the stress-strain plots are shown in Fig. 7(a). Tensile stud-
GTA welding technique. Similar observations are reported by same ies corroborated that all the tensile failures occurred at the weaker
authors in the earlier studies with welding of SDSS and austenitic base metal, AISI 904L [Fig. 7(b)]. The test data signifies that the ten-
stainless steel. According to Savage [28], the formation of equiaxed sile strengths of the welded joints are greater than one of the base
grains requires such an extensive constitutional supercooling and metals. The average tensile strengths reported by the weldments
if the liquid metal through inoculation contains a significant num- are 692 and 698.5 MPa for ER2553 and ERNiCrMo-10 respectively.
ber of solid particles on which the atoms in the constitutionally The results are well supported with hardness data that the frac-
supercooled liquid metal can be easily arranged in a crystalline ture was experienced in the location where the hardness values
form, it generally results in lower segregation. Further, the author are lower. Further, the microstructure also revealed the presence
reported the presence of equiaxed grains in the fusion zone nor- of fine equiaxed grains which improved the hardness and strength.
D.R. K. et al. / Journal of Manufacturing Processes 30 (2017) 27–40 33

Fig. 4. (a) Fusion zone microstructure and (b) SEM/EDAX point analysis at the fusion zone of PCGTA welds of AISI 904L and UNS S32750 employing ER2553.

Fig. 5. (a) Fusion zone microstructure and (b) SEM/EDAX point analysis at the fusion zone of PCGTA welds of AISI 904L and UNS S32750 employing ERNiCrMo-10.

Table 3
Hardness measurement on the PCGTA welds of UNS S32750 and AISI 904L.

Parent Metal – UNS S32750 Parent Metal – AISI 904L Average Hardness value in the fusion zone (HV)

ER2553 ERNiCrMo-10

Cap Middle Root Avg. Cap Middle Root Avg.

280 ± 3 178 ± 3 175 ± 2 197 ± 2 203 ± 3 192 ± 2 227 ± 3 227 ± 3 240 ± 2 231 ± 3

It is to be noticed that plastic strain is induced in the fusion zones dimensions, which coalesced as the weldments failed by ductile
upon tensile loading. SEM fractographic features of the tensile stud- mode [Fig. 8(a) and (b)].
ied samples showed the presence of dimples and voids in various Room temperature Charpy V-notch impact test results showed
that the weldments employing ER2553 exhibited higher impact
34 D.R. K. et al. / Journal of Manufacturing Processes 30 (2017) 27–40

Fig. 6. Hardness profiles of the PCGTA welds involving AISI 904L and UNS S32750 employing (a) ER2553 and (b) ERNiCrMo-10 fillers.

Table 4
Mechanical properties of the PCGTA weldments of UNS S32750 and AISI 904L.

Mechanical Property Unit Base Metal – UNS S32750 Base Metal – AISI 904L ER2553 ERNiCrMo-10

0.2% Yield Strength MPa 492 ± 4 335 ± 3 382.5 ± 3.2 396.5 ± 3.1
Ultimate Tensile Strength MPa 875 ± 3 655 ± 2.5 692 ± 3.5 698.5 ± 3.2
% Elongation % 39.8 ± 0.8 56.8 ± 1.2 36.2 ± 2.1 33.1 ± 1.8
Fracture Location – – – Parent metal of AISI 904L Parent metal of AISI 904L
Impact toughness J 96 ± 2.0 67 ± 1.2 76 ± 2.4 38 ± 1.8
Physical observation of impact tested sample – – – Broken into two halves V-notch deformation

toughness (76 J) than the ones employing ERNiCrMo-10 (38 J). 3.4. Corrosion studies
However, the impact toughness of the welds is lower than the base
metal, UNS S32750. Upon impact loading, the weldments employ- 3.4.1. Potentiodynamic polarization
ing ER2553 had shown notch deformation, which, in turn, indicated The open circuit potential test was conducted for stabilizing
that the maximum energy has been absorbed by the weldments. the voltage or potential before the potentiodynamic polarization
On the other hand, ERNiCrMo-10 weldments broke into two halves studies and the test was running for 1 h. The open circuit potential
which indicated lesser energy absorption [Fig. 9(a) and (b)]. It is evi- values (OCP) recorded was 0.43 V for both the parent metals, AISI
dent that the impact toughness of ERNiCrMo-10 weldments was 904L and UNS S32750. Similarly the OCP values were found to be
greatly reduced owing to the effect of micro-segregation as wit- 0.14 V and 0.17 V for the fusion zones of ER2553 and ERNiCrMo-
nessed in the SEM/EDAX analysis [Fig. 5]. The fractographic features 10 fillers. Potentiodynamic polarization curves of various coupons
of the impact tested samples indicated the presence of infrequent of the dissimilar weldments exposed in 3.5% NaCl environment is
voids in the ER2553 weldment [Fig. 10(a)]. The presence of Mo-rich shown in Fig. 11. It is inferred from the studies that the base metal
segregates in the fusion zone of ERNiCrMo-10 would serve as crack AISI 904L exhibited better corrosion resistance than other zones
nucleating sites and exhibited fracture. This is well understood by of the weldment [Table 5]. It is opined that the material exhibits
the presence of tearing boundaries with discontinuous cracks as higher corrosion potential exhibits better corrosion resistance. AISI
the fractographic traits which concluded brittle mode of fracture 904L has almost equal amounts of Ni and Cr with alloying ele-
[Fig. 10(b)]. Table 4 shows the average mechanical properties of ments such as Cu, Mo etc. In turn, these elements will form the
the dissimilar weldments. oxides of Ni and Cr, and exhibit a passivation layer which pre-
D.R. K. et al. / Journal of Manufacturing Processes 30 (2017) 27–40 35

Fig. 7. (a) Stress-strain plots of tensile tested base metals and PGTA welded joints of UNS S32750 and AISI 904L. (b) Photographs showing the tensile tested samples of PCGTA
weldments experienced fracture at the parent metal of AISI 904L for both the weldments.

Table 5
Electrochemical data for the base and weld metals in 3.5% NaCl environment at room temperature.

Specimen ECorr (mV) ICorr (A/cm2 ) Corrosion rate (mpy)

Base Metal – AISI 904L −130 ± 1.2 2.122 × 10−8 0.022 ± 0.002
Base Metal – UNS S32750 −426 ± 1.0 2.875 × 10−6 4.469 ± 0.011
Fusion Zone – ER2553 −423 ± 1.4 3.321 × 10−5 51.42 ± 0.022
Fusion Zone – ERNiCrMo-10 −170 ± 1.2 3.628 × 10−8 0.056 ± 0.017

vents corrosion. Similarly the base metal, UNS S32750 has almost 3.4.2. Salt spray test
equal amounts of ferrite and austenite. The ferrite phase contains Salt spray corrosion studies were performed on the coupons of
a higher amount of Cr and austenitic phase has Ni. Similar findings the dissimilar weldments involving UNS S32750 and AISI 904L for
are reported by Loto [32]. Similarly both the fusion zones con- 300 h. No appreciable physical and morphological changes were
tains substantial amounts of Cr, Ni, and Mo which is well indicated observed on the any of these coupons after an exposure of 300 h.
from the SEM/EDAX analysis. A slight reduction in the corrosion To be more precise, there is no red rust formation on any of
resistance of fusion zone of ERNiCrMo-10 over the parent metals these samples exposed for 300 h. However, slight weight changes
can be reasoned out to the segregation of secondary phases in the were noticed on the samples before and after the corrosion study.
interdendritic spacing. The impoverishment in the corrosion resis- The studies attested that the parent metal, AISI 904L exhibited
tance of fusion zone of ER2553 weldment could be attributed to the better resistance to corrosion by showing the corrosion rate of
galvanic coupling established between the discontinuous zones, 0.0122 mm/year; whereas the corrosion rates of parent metal UNS
which form small anodes where metal dissolution occurs, and the S32750, fusion zone of ERNiCrMo-10 and fusion zone of ER2553
remainder of the surface where the cathodic reaction takes place are found to be 0.0140, 0.0147 and 0.0197 and mm/year respec-
as reported by Sedricks [33]. However in the present study, there tively. It is well understood that the higher amounts of Cr and Mo
was no current pits observed for any of these samples on increas- along with Ni and Cu in AISI 904L improved the corrosion resistance.
ing the current density. The studies attested that potentiodynamic The enriched Cr content in the ferrite phase and Ni in the austenite
polarization test confirmed the reproducibility of the results. phase improved the pitting and crevice corrosion resistance of UNS
S32750. Similarly, the higher amounts of Ni, Mo, and Cr in the fusion
zone of ERNiCrMo-10 showed better corrosion resistance than the
36 D.R. K. et al. / Journal of Manufacturing Processes 30 (2017) 27–40

Fig. 8. SEM fractographs of tensile tested dissimilar welds of AISI 904L and UNS Fig. 10. SEM fractographs of impact tested dissimilar welds of AISI 904L and UNS
S32750 employing (a) ER2553 and (b) ERNiCrMo-10 fillers respectively. S32750 employing (a) ER2553 and (b) ERNiCrMo-10 fillers respectively.

fusion zone employing ER2553. Similar observations are reported


by other researchers [34–36]. It is evident from salt fog test that tion of the microbes, the OD value was 0.297. This was followed by
there were not much differences observed in the weight loss on stationary phase where the OD was found to be stable for 8–10 h.
repeating the studies. In the stationary phase, no net growth of the bacterial cells was
observed because during this phase the number of cells increased
3.4.3. Microbial corrosion studies became equal to the number of cells died. The consortium of bac-
The growth of bacterial cells was studied where the initial opti- terial cells reached stationary growth after 8 h and beyond this
cal density (OD) at zeroth h was nil. The increase in growth was point the growth was constant till 10 h and there was a negligi-
calculated by measuring the optical densities at regular intervals of ble decrease in growth of the cells during the post incubation for
time. The inoculation size was 106 CFU/ml. After 15 min, the OD was 10 h as depicted in the Fig. 12. The decrease in bacterial cells occurs
found to be 0.09. The rate of microbial growth from 0 h to 1 h was due to the depletion of the nutrients present in the medium. Thus,
considered as the lag phase in the study. After 1 h of incubation, during the experiment, medium was added in the flasks at regular
there was initiation of exponential phase with rapid multiplica- intervals of time.

Fig. 9. Photographs showing the impact tested samples of PCGTA weldments employing (a) ER2553 and (b) ERNiCrMo-3 filler.
D.R. K. et al. / Journal of Manufacturing Processes 30 (2017) 27–40 37

rod shaped bacteria is well depicted in the SEM image shown in


Fig. 13. After 15 days of exposure, the bacterial isolates have formed
biofilm and the corrosion is evident with the presence of cavities
and pits on the surface. It can be inferred that in the consortium, the
combination of both Bacillus and Pseudomonas species have caused
extensive damage to the stainless steel substrates by causing pitting
corrosion and entering the cavities and widening the pits when the
exposure time was extended to 30 days [Fig. 14]. Similar reports of
pitting corrosion were observed upon incubating carbon steel with
sulphate reducing bacteria by other researchers [37,38].
The fusion zones of both the weldments were also investigated
for biological induced corrosion behavior. The surface of the fusion
zone employing ER2553 (Sample C) is prone to corrosion attack
by the bacterial strains which are prominent in the SEM images.
The conversion of smooth surface to rough is prominent after a
15 day exposure and cavities are formed within 30 days of expo-
sure. The SEM image shows the presence of clusters of microbes
Fig. 11. Potentiodynamic polarization plots of dissimilar welds of UNS S32750 and forming a line along the surface of the fusion zone of ER2553 weld-
AISI 904L in 3.5% NaCl environment. ment [Fig. 15]. Similarly, the fusion zone employing ERNiCrMo-10
(Sample D) shows the surface corrosion by the individual bacte-
rial isolates, which is more prominent after 15 days of exposure
[Fig. 16]. However, post 30 days of incubation, the microbes have
further colonized the surface with the formation of biofilm leading
to corrosion as noticed in the previous trials of our study. Several
cracks are visible on the surface which shows that the bacterial
isolates are able to corrode the metal and utilize the surface for
growth.
Energy Dispersive X-ray Spectroscopy (EDAX) analysis was also
performed to investigate the elemental changes on the samples
exposed to MIC for 15 and 30 days. EDAX spectroscopy was carried
out before and after the MIC experiments on the same coupons.
It is inferred that the parent metals UNS S32750, AISI 904L and
the fusion zone of ER2553 contained Fe as their major component
along with Cr, Ni, and Mo; whereas the fusion zone employing
Fig. 12. Growth curve of the bacterial consortium. ERNiCrMo-10 was found to have more amount of Ni as seen in
Fig. 16. It is well inferred that there is a change in the percent-
SEM is used to infer the morphological changes on the exposed age of the elements present before and after the experiment. The
surfaces before and after the bacterial attack. As observed in the concentration of Fe and Cr in the parent metal of UNS S32750 was
control image of the parent metal UNS S32750 (A), the surface impoverished after exposure to bacterial attack. The Fe content of
was smooth and without any corrosion. However, after 15 days of the parent metal UNS S32750 was around 65% by weight before
incubation of the coupons with the bacteria, the surfaces of all the the corrosion trial, which was then reduced to 61% by weight after
specimens had turned rough and colonies of bacteria formed. Clus- the biocorrosion study with microbial consortium. The Cr content
ters of rod shaped identical bacterial cells were found to grow on was also decreased from around 24%–21% by weight after 15 and
the metal surface in all the trials. The morphological trait of the 30 days interval. This clearly indicates that the bacterial isolates

Fig. 13. SEM/EDAX analysis on (a) Control before prone to Biological induced corrosion; (b) and (c) Biological induced corrosion of UNS S32750 showing the corrosion attack
of bacterial consortium after 15 days and 30 days respectively.
38 D.R. K. et al. / Journal of Manufacturing Processes 30 (2017) 27–40

Fig. 14. SEM/EDAX analysis on (a) Control before prone to Biological induced corrosion; (b) and (c) Biological induced corrosion of AISI 904L showing the corrosion attack
of bacterial consortium after 15 days and 30 days respectively.

Fig. 15. SEM/EDAX analysis on (a) Control before prone to Biological induced corrosion; (b) and (c) Biological induced corrosion of fusion zone employing ER2553 showing
the corrosion attack of bacterial consortium after 15 days and 30 days respectively.

Fig. 16. SEM/EDAX analysis on (a) Control before prone to Biological induced corrosion; (b) and (c) Biological induced corrosion of fusion zone employing ERNiCrMo-10
showing the corrosion attack of bacterial consortium after 15 days and 30 days respectively.
D.R. K. et al. / Journal of Manufacturing Processes 30 (2017) 27–40 39

are capable of utilizing the metal content as their nutrients to form (1) Microsegregation of Mo, Cr, and W-rich phases are observed in
colonies which further results in corrosion of the metal coupons the fusion zone of the weldment employing ERNiCrMo-10
[39]. Microbes require prolonged duration for complete consump- (2) Tensile studies corroborated that the joint strength of both the
tion of the metallic coupons and thus, the changes observed in Fe weldments is greater than the weaker parent metal, AISI 904L.
and Cr concentrations before and after the investigation can be con- Tensile failures were observed at the parent metal, AISI 904L
sidered significant. The other parent metal, B, and the fillers were for both the cases.
also observed to have decreased content of the elements in certain (3) Impact toughness was impaired for the weldments employing
cases. In all the scenarios, Pseudomonas sp. was able to utilize Fe ERNiCrMo-10 owing to the effect of micro-segregation.
and decrease its concentration in the metal coupons. Thus, it can (4) Both the potentiodynamic polarization and salt spray corrosion
be confirmed that Pseudomonas and Bacillus sp. are capable of caus- studies attested that the base metal, AISI 904L exhibited better
ing corrosion of the metal coupons due to the presence of Fe, Cr and corrosion resistance compared to other coupons.
Ni which they are able to use in nutrient depleted conditions [40]. (5) All the coupons in both the weldments are vulnerable to micro-
The term, microbiologically induced corrosion refers to the col- bial influenced corrosion attack.
onization of microbes on metal surfaces which finally results in (6) Consortium of Pseudomonas sp. and Bacillus sp. were found to
corrosion of the metal. The rapid growth of microbes on the metal induce biological corrosion aggressively on the coupons. This
surface is a natural phenomenon where the microbes adhere to is a first report on microbial corrosion by Pseudomonas sp. and
the surface of the metals and form biofilms. Microbial adhesion Bacillus sp. on weldments involving UNS S32750 and AISI 904L.
and the consequent biofilm formation are the determining steps in (7) The synergetic effect of the isolates producing acids and exo-
microbiologically influenced metal deterioration [41]. During the enzymes could be attributed to the initial constitution of biofilm
early stage of the experiment, it was observed that single bacte- and progressive damage to the metal substrate by corrosion.
rial cells attach to the metal surface and then starts to multiply to (8) Based on the outcomes of the present studies, PCGTA weld-
form colonies. After a certain stage, the metal surface does not act ing of AISI 904L and UNS S32750 employing ERNiCrMo-10 and
as the adhering surface but the bacterial cell attaches to the biofilm ER2553 are recommended.
itself and increases their growth [42]. Microbes influence corrosion
by altering the electrochemical conditions at the media and metal Acknowledgements
interface due to the chloride ions present in the media. Both the iso-
lates Pseudomonas sp. and Bacillus sp. have the ability to produce The authors wish to thank Mr. Natarajan, Managing Director,
organic/inorganic acids, extracellular metabolites, and enzymes to M/s. Delta Wear Tech Engineers, Pvt. Ltd. Chennai for providing the
facilitate corrosion. The surface of metals as observed in the control welding facilities. The authors are also thankful to acknowledge VIT
SEM images shows grooves present after polishing which helps the University for providing the research ambience and all the facilities
bacterial cells to attach to the metal and thus begin to corrode the required to accomplish the work. The authors wish to convey their
metal. Hence, it can be confirmed that the surface roughness plays deepest gratitude to Mr. Arul Maximus Rabel, Scientist, Sathyabama
an important role in biofilm formation of bacteria on metals. Bac- University, Chennai for extending their support.
teria are capable of producing exopolysaccharide which have been
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