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A R T I C L E I N F O A B S T R A C T
Keywords: Erosion-corrosion is a critical problem in marine components and has huge economic impact. In the current
Erosion-corrosion study, friction stir processing was utilized for enhancing the erosion-corrosion resistance of SS316L steel, most
Friction stir processing widely used material for marine applications. Compared to the unprocessed alloy, the friction-stir processed
Phase transformation specimen showed nearly 3.5 times and 5 times higher erosion and erosion-corrosion resistance respectively at
oblique impingement. In contrast, erosion and erosion-corrosion resistance for processed alloy was 2 times
higher at normal impingement. The unusual enhancement in erosion-corrosion resistance was attributed to
surface strengthening through grain-size refinement and martensite phase formation. In addition, higher cor-
rosion resistance due to stronger passivation also contributed towards superior performance of the processed
alloy.
⁎
Corresponding author.
E-mail address: harpreet.arora@snu.edu.in (H.S. Arora).
http://dx.doi.org/10.1016/j.wear.2017.06.009
Received 31 March 2017; Received in revised form 5 June 2017; Accepted 21 June 2017
Available online 23 June 2017
0043-1648/ © 2017 Elsevier B.V. All rights reserved.
K. Selvam et al. Wear 386–387 (2017) 129–138
Fig. 3(a) is the EBSD map for as-received SS316L showing the grain
structure and grain size distribution. The microstructure shows twin
boundaries, attributed to low stacking fault energy for austenitic steels.
Fig. 1. Schematic of friction stir processing (FSP) set-up used in the current study. A Average grain size for the as-received alloy calculated from grain size
specially designed tool-fixture was used to clamp the workpiece of variable dimensions. distribution (Fig. 3(b)) is nearly 22 µm. Microstructural details for the
The fixture has a cooling tank located above the work-piece which is connected to the processed samples are shown in Fig. 3(c) to (f). Both the processed
external chiller unit through inlet and outlet ports. The coolant used in the chiller was
samples showed significant grain refinement compared to as-received
mixture of distilled water and ethanol.
sample, with an average grain size of 0.67 µm for 388C and 0.9 µm for
1800C. Dynamic recrystallization (DRX) comprising rearrangement of
dislocations into sub-grains and grain boundary migration are believed
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Fig. 3. EBSD map for (a) as-received austenitic steel SS316L, (c) friction stir processed SS316L at 388 rpm (388C) and (e) friction stir processed SS316L at 1800 rpm (1800C); Grain size
distribution for (b) as-received SS316L, (d) 388C and (f) 1800C.
to be the primary mechanisms for grain structure refinement during FSP expressed by Zener Holloman parameter, Z = ∈̇ exp (Q/ RT ) , where ∈̀ is
[26]. A pseudo heat index for the FSP process is given as: ω2/υ, where ω the strain rate, Q is the activation energy for deformation, T is the
is the tool rotational speed υ is the transverse speed. This implies that absolute temperature and R is the gas constant. Deformation at high
heat input and strain rate are both functions of tool rotational speed strain-rates leads to significant rise in temperature which may result in
[24,25]. Higher strain rate favors finer grain structure while increasing a coarse grain structure [7,18,27]. Hence it is critical to control tem-
temperature induces grain growth. Hence temperature and strain rate perature during high strain-rate deformation process to achieve ultra-
compete to control the final grain size during dynamic recrystallization fine grain structure [13,30,31]. The finer grain structure for 388C
[27–29]. The combined influence of strain rate and temperature is sample is attributed to lesser temperature rise during processing. EBSD
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Fig. 4. EBSD phase map showing distribution of austenite and martensite phases in (a) as-received austenitic steel, SS316L; sample friction stir processed at (b) 388 rpm (388 C); (c)
1800 rpm (1800C); (d) overall fraction of austenitic and martensitic phases in all the samples. In the phase map, green color indicate austenite phase while red color indicate martensite.
phase map showing austenite and martensite phase distribution in the both the processed samples. The as-received alloy shows a strong (111)
as-received and processed samples are given in Fig. 4(a) to (d). As-re- parallel ND texture while 388C and 1800C shows strong (100) parallel
ceived alloy had austenite as the primary phase (Fig. 4(a)). It is seen ND and (211) parallel ND texture respectively. Face-centred-cubic
that there is austenite to martensite phase transformation during pro- materials show higher elastic modulus along (111) plane compared to
cessing. Martensite phase is significantly higher for 388C compared to other crystallographic plane [33]. This is likely attributed to the closest
1800C. High strain rate is known to suppress austenite to martensite atomic packing on (111) plane resulting in strong inter-atomic bonding.
transformation due to more adiabatic heating at higher strain rate [32]. Therefore, higher elastic modulus for the as-received alloy is likely due
Therefore, lower strain rate deformation accompanied by rapid cooling to strong (111) texture which changes during processing resulting in
resulted in higher fraction of martensite phase for 388C. decrease in elastic modulus.
Fig. 5(a) shows the variation in microhardness for both the pro-
cessed samples as a function of depth from the top surface. Hardness 3.2. Erosion-corrosion behavior
was maximum at the surface and decreased along the depth. 388C
showed maximum hardness of nearly 1.8 times compared to the as- The erosion and erosion-corrosion depth for the processed samples
received alloy, while it was nearly 1.5 times for 1800C sample. The was measured to be nearly 20–25 µm and 60–70 µm respectively. Since
significant rise in hardness after processing was primarily attributed to the processed depth was nearly 150 µm, the material removal was
grain boundary strengthening and austenite to martensite transforma- completely from the processed region only. Fig. 6(a) to (c) show results
tion as shown by the EBSD results. The hardness of both the processed for pure erosion test. It is seen that erosion rate was higher at 30° im-
samples decreased to the value for as-received alloy at about 150 µm, pingement compared to normal impingement for both the as-received
corresponds to the depth of the processed zone. The elastic modulus for as well as processed samples. This implies similarity of erosion beha-
all the samples was obtained using nano-indentation. The load-dis- vior/mechanism for the unprocessed and processed samples. Lower
placement curves for the as-received alloy and both the processed erosion rate at normal impingement and higher at oblique angles im-
samples are shown in Fig. 5(b). The modulus values are shown along- plies ductile mode of material removal for austenitic steel, remains the
side the load-displacement curves. Hardness increased after processing, same for processed samples as well. Further, mass loss is significantly
while elastic modulus decreased. The decrease in elastic modulus values lower for both the processed samples. At 30° impingement angle, the
after processing is likely due to texture changes during friction stir erosion resistance for 388C sample was nearly 3.5 times higher com-
processing. Fig. 5(c) shows inverse pole figures (IPF) for as-received and pared to the unprocessed alloy, while it was nearly 1.6 times higher for
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Fig. 5. (a) Hardness as function of depth for the as-received austenitic stainless steel, SS316L, friction stir processed SS316L at 388 rpm (388C) and friction stir processed SS316L at
1800 rpm (1800C); (b) load-displacement curves for the as-received austenitic stainless steel, SS316L, 388C and 1800C specimens obtained using nano-indentation; (c) Normal direction
(ND) inverse pole figure (IPF) for as-received, 388C and 1800C specimens. The color bar shows the texture intensity in each case.
1800C sample. At 90° impingement, both the processed samples corrosion and synergy are summarised in Table 1. Higher synergy for
showed nearly similar behavior with nearly two times higher erosion the as-received alloy compared to processed samples indicate its lower
resistance compared to the as-received alloy. Phenomenal increase in resistance to material loss under simultaneous influence of erosion and
erosion resistance for 388C is attributed primarily to its higher hard- corrosion. Interestingly, synergy is higher for 388C compared to 1800C.
ness, as a consequence of grain size refinement and higher fraction of This is likely due to higher fraction of martensite in 388C which has
martensite phase formed during processing (Fig. 4(b)). inferior corrosion properties compared to austenite [32,34].
Results for erosion-corrosion are also shown in Fig. 6(a) to (c). For To understand the superior erosion-corrosion resistance of pro-
all samples, the material loss was higher in erosion-corrosion compared cessed samples, standalone electrochemical corrosion tests were done.
to pure erosion. The increase in material loss during erosion-corrosion These include Tafel and cyclic polarization in 3.5% NaCl solution. The
may be attributed to the following factors: (i) removal of hardened cathodic and anodic polarization curves obtained using cyclic polar-
surface by corrosion, exposing relatively soft surface to further erosion; ization for all the specimens are shown in Fig. 7(a) to (d). The corrosion
(ii) corrosion attack at grain boundaries resulting in enhanced material current (Icorr) was evaluated using Tafel exploration from the polar-
removal; (iii) detachment of raised lips due to corrosion; (iv) micro- ization curves and values are shown in Table 2. Icorr is the highest for as-
pitting resulting in increase in number of stress concentration defects. received alloy followed by 1800C and lowest for 388C indicating higher
In contrast to the as-received alloy, the mass loss during erosion-cor- corrosion resistance of processed specimens. Interestingly, the grain
rosion is much smaller for the processed samples. For 30° impingement, size also follows similar order- largest for as-received, followed by
the mass loss for 1800C was nearly 3.5 times lower, while for 388C it 1800C and 388C. Higher corrosion resistance for the processed samples
was lower by nearly 5 times. At normal impingement, the performance can be attributed to their finer grain structure. Typically, the oxide
of both the processed specimens was nearly two times better compared layer formed on stainless steel has a duplex structure with Cr2O3
to the as-received alloy. The 388C sample showed unusually high ero- (having p-type semiconductor characteristics) as an inner layer and
sion-corrosion resistance, particularly at oblique angle, the first report Fe2O3 (having n-type semiconductor characteristics) as an outer layer
of its kind. The mass loss during dynamic corrosion was insignificant for [35]. The donor to acceptor ratio in the passive layer has significant
all the samples (0.25 mg/h, 0.155 mg/h and 0.215 mg/h for the as-re- influence on the oxide layer characteristics. In general, the donor to
ceived, 388C and 1800C specimens respectively). As mentioned earlier, acceptor density in passive layer decreases with the grain refinement
erosion-corrosion involves the synergy effect as expressed by the rela- [35], causing reduction in the available charge carriers and improving
tion: T = E + C + S where synergy (S) could be either positive (in- passivity. The donor to acceptor density further reduces in the chloride
crease in degradation) or negative (decrease in degradation). Fig. 6(d) environment where chloride ion tends to occupy the oxygen vacancies
shows that the synergy obtained in the current study is positive. For the in the passive film [35]. Thus, the finer grain structure of processed
as-received alloy, synergy component is the highest (~52%) followed samples contributed towards faster passivation kinetics, better passive
by 388C (~47%) and 1800C (~27%). The results for erosion, erosion- layer stability, and superior corrosion resistance.
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Fig. 6. Material removal rate (mg/h) as a function of impingement angle during pure erosion and erosion-corrosion test for (a) as-received austenitic stainless steel, SS316L, (b) friction
stir processed SS316L at 388 rpm (388C), (c) friction stir processed SS316L at 1800 rpm (1800C), (d) pie-chart showing erosion, corrosion and synergy components for as-received, 388C
and 1800C specimens.
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Fig. 7. Cyclic polarization curves for (a) as-received austenitic stainless steel, SS316L, (b) friction stir processed SS316L at 388 rpm (388 C), (c) friction stir processed SS316L at 1800 rpm
(1800C), (d) pit initiation resistance (Epit - Ecorr) for as-received, 388 C and 1800C specimens.
sample again showed two times higher resistance, similar to pure ero-
Table 2
sion, which can be attributed to brittle fracture of the passive oxide
Results of electrochemical corrosion test for all the samples. layer during normal impingement. Thus, the passive oxide layer could
not contribute to further enhance the erosion-corrosion resistance of
Sample Icorr (µA) Ecorr (mV) Epit (mV) Epp (mV) Epit Area processed specimens. Further, comparison of Figs. 8 and 9 indicates
–Ecorr under
that platelet formation for pure erosion is more severe compared to
(mV) the loop
(mV.A/ erosion-corrosion. Slurry impingement results in material extrusion
cm2) which is weakened by the corrosive media present in the slurry. This
leads to rapid loss of material as debris, instead of pile up as in the case
As-received 19.3 −319 168.4 −18.66 487.4 7.035
of pure erosion and likely explains increased material loss in erosion-
388-C 5.23 −368 303.4 −41.06 671.4 6.35
1800-C 9.49 −326 387.1 −26.57 713.1 4.245 corrosion.
4. Conclusions
impingement, material hardness as well as passive layer stability are the Surface properties of SS316L stainless steel were tailored using
controlling factors. 388C specimen has the highest hardness as well as submerged friction stir processing and their erosion and erosion-cor-
better passive layer stability than the as-received alloy which enhanced rosion behavior was evaluated. Major findings of the current study are:
its erosion-corrosion resistance by five times. In contrast, the material
removal at normal impingement is dominated by plastic deformation 1. Submerged friction stir processing refined the grain structure from
and indentation. Therefore, material plasticity plays a more dominant 22 µm for the as-received alloy to as low as 0.67 −0.89 µm for the
role at normal impingement. Greenwood and Williamson [38] proposed processed specimen.
that plasticity index for the material is inversely proportional to hard- 2. The processed samples showed significant increase in hardness.
ness to modulus (H/E) ratio. H/E ratio for the processed materials was Compared to as-received alloy (220 HV), the hardness of the pro-
calculated to be 0.022 and 0.02 for 388C and 1800C specimens re- cessed samples was around 420 HV for 388C processing condition
spectively. These values are close enough which explains similar ero- and 350 HV for 1800C processing condition. Increase in hardness is
sion behavior for both the processed samples at normal impingement. attributed to grain refinement and austenite to martensite trans-
During erosion-corrosion at normal impingement, both processed formation.
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Fig. 8. Scanning electron images for as-received SS316L subjected to pure erosion at (a) 30° impingement and (b) at 90° impingement; SS316L friction stir processed at 388 rpm (388C)
and subjected to pure erosion at (c) 30° impingement and (d) at 90° impingement; SS316L friction stir processed at 1800 rpm (1800C) and subjected to pure erosion at (e) 30°
impingement and (f) at 90° impingement.
3. The processed samples demonstrated significantly higher erosion 4. The processed samples also showed superior corrosion properties
and erosion-corrosion resistance. At oblique impingement, 388C which is due to higher stability of the passive layer as a result of
shows around 3.5 times higher erosion resistance and about 5 times pegging of the oxide layer and faster passivation kinetics.
higher erosion-corrosion resistance. At normal impingement, pro- 5. Erosion-corrosion process was found to be erosion dominant, how-
cessed samples showed two times higher erosion as well as erosion- ever, synergy with corrosion was also observed to be contributing
corrosion resistance. significantly.
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Fig. 9. Scanning electron images for as-received SS316L subjected to erosion-corrosion at (a) 30° impingement and (b) at 90° impingement; SS316L friction stir processed at 388 rpm
(388C) and subjected to erosion-corrosion at (c) 30° impingement and (d) at 90° impingement; SS316L friction stir processed at 1800 rpm (1800C) and subjected to erosion-corrosion at
(e) 30° impingement and (f) at 90° impingement.
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