Materials Science & Engineering A 708 (2017) 91103

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Materials Science & Engineering A

journal homepage: www.elsevier.com/locate/msea

Implications of dynamic strain aging under LCF-HCF interactions in a type MARK

316LN stainless steel

Aritra Sarkara, , A. Nageshaa, P. Parameswaranb, R. Sandhyaa, M. Okazakic
a
Materials Development and Technology Division, Indira Gandhi Centre for Atomic Research Kalpakkam, Tamil Nadu 603102, India
b
Physical Metallurgy Division, Indira Gandhi Centre for Atomic Research Kalpakkam, Tamil Nadu 603102, India
c
Department of Mechanical Engineering, Nagaoka University of Technology, 940-2188, Japan

A R T I C L E I N F O A B S T R A C T

Keywords: Inuence of dynamic strain aging (DSA) under sequential low cycle fatigue (LCF) and high cycle fatigue (HCF)
Dynamic strain aging loading was investigated by conducting HCF tests on specimens subjected to prior LCF cycling over a wide range
Low cycle fatigue of temperature from 573 to 973 K. DSA was found to be pronounced at 823873 K depending on the magnitude
High cycle fatigue of the stress employed under HCF cycling. DSA was seen to have contrasting implications under LCF and HCF
Low cycle fatigue-high cycle fatigue interaction
deformation resulting in an anomalous fatigue behavior in terms of remnant HCF life under LCF-HCF interaction.
316LN SS
LCF-HCF interaction was found to be pronounced at intermediate levels of prior LCF exposure, where the
remnant HCF life is dictated by competitive damage mechanism resulting from the inuence of DSA under LCF
as well as HCF. Detailed fracture surface examination revealed that extensive hardening associated with DSA
leads to an extended zone of faceted appearance with river markings (Stage-I crack) under HCF cycling (with or
without LCF exposure). This reduces the crack growth rate, delaying the transition of crack from Stage-I to Stage-
II, thereby leading to an extension of life in such cases. On the other hand, a highly striated fracture surface
indicating a quick transition in crack from Stage-I to Stage-II, was observed for loading conditions with minimal
or no inuence of DSA, thus leading to lower life compared to the previous case.

1. Introduction
Present investigations on fatigue behavior of structural materials are
limited mostly to isolated cases of low cycle fatigue (LCF) or high cycle
fatigue (HCF) even though engineering components experience a
varying load history throughout their service life. In sodium cooled fast
reactors (SFRs), components of main vessel, inner vessel and inter-
mediate heat exchanger are exposed to LCF damage during the start-
stop operation of the reactor [1,2]. Besides, they are also subjected to
HCF loading owing to thermal striping, stratication, ow induced vi-
bration etc. during the steady state reactor operation [35]. Therefore,
it is pertinent and essential to examine the material behavior under
combined cycling where strong LCF-HCF interaction is taking place, so
that adequate safety can be ensured in the design.
The mechanistic aspects of such damage evolution under high
temperature LCF-HCF interactions in type 316LN austenitic stainless
steel (the main structural material for inner vessel components in SFRs)
have been investigated through sequential application of LCF and HCF
loads [68]. DSA is a commonly observed phenomenon at high tem-
peratures, in austenitic stainless steels [9,10] which is caused by
pinning of mobile dislocations by the solute atoms [911] (Cr in the
present case [11]) during the dislocation glide motion or their tem-
porary arrest at local obstacles in their glide plane under LCF de-
formation. Even though extensive literature on the manifestations of
DSA on LCF is available [1014], the same is very limited on HCF [15]
or LCF-HCF interaction [16]. The authors have examined the inuence
of DSA under LCF and HCF cycling by undertaking a detailed study in
the temperature range, 573973 K [7]. The investigation indicated that
DSA is pronounced at 823 and 873 K under pure LCF and HCF cycling
[7]. However, the manifestations of DSA under LCF and HCF were
found to be entirely contrasting with a signicant reduction in the
cyclic life under LCF and a huge increase in life under HCF [7]. Since
HCF tests were carried out under engineering stress-control, extensive
hardening of the matrix resulting from DSA will lower the possibility of
localized plastic deformation thereby delaying the crack initiation to a
great extent, leading to an increase in life with temperature, in the
range where DSA is operative [7]. This may result in an anomalous
fatigue behavior in terms of cyclic life, under LCF-HCF interaction, as a
function of prior LCF exposure and temperature. However, even at a
temperature where DSA is highly active, the inuence of the same on

Corresponding author.
E-mail address: aritra@igcar.gov.in (A. Sarkar).

http://dx.doi.org/10.1016/j.msea.2017.09.057
Received 21 July 2017; Received in revised form 13 September 2017; Accepted 14 September 2017
Available online 18 September 2017
0921-5093/ 2017 Elsevier B.V. All rights reserved.
A. Sarkar et al. Materials Science & Engineering A 708 (2017) 91103

LCF-HCF interaction can depend strongly on the stress employed under

HCF. The present study attempts at an in-depth analysis of the above
aspects. Further, experimental studies on the nature of crack initiation
and propagation under variable amplitude loading, particularly under
LCF-HCF interaction at high temperature, are limited [1719]. In view
of this, correlation of the physical aspects of damage with the fracture
behavior will help to identify the life-controlling micro-mechanisms
responsible for damage under such loading conditions. The present
investigation focuses on the detailed characterization of the fracture
modes with a view to gaining a deeper insight into the underlying
damage mechanisms.

2. Experimental

The chemical composition (in wt%) of 316LN stainless steel used in

the present study is Fe-0.025C-17.5Cr-12.1Ni-2.53Mo-0.07N-1.74Mn-
0.0041S-0.017P. The material was subjected to solution annealing Fig. 1. Variation of remnant HCF lives with prior LCF exposure (%) at dierent nor-
treatment at 1363 K (1090 C) /1 h followed by water quenching. The malized stresses (Temperature: 573 and 823 K).
resultant grain size was found to be ~ 80 m.
Details of baseline LCF and HCF testing at dierent temperatures
3. Results and discussion
have been illustrated in the previous investigation [6,7]. Under HCF
testing, with a view to account for the temperature-dependence of the
3.1. Inuence of DSA on LCF-HCF interaction: prior LCF cycling followed
yield stress, the maximum stress (max) employed in the present tests
by HCF
was normalized with respect to YS (max/YS), designated as N. In the
present study, testing was carried out at two temperatures, 573 and
3.1.1. Eect of stress
823 K, one in DSA (823 K) and another in non-DSA (573 K) regime.
To understand the inuence of DSA on LCF-HCF interaction beha-
Towards investigating the inuence of LCF-HCF interaction in the alloy,
vior of the alloy, the specimens were exposed to prior LCF cycling, in
specimens were initially exposed to prior LCF deformation at a t/2
the range of 2080% of LCF life and subjected to HCF at N : 1.36 and
of 0.6% for various life fractions in the range 2080%, at 573 and
1.44 (573 and 823 K). Fig. 1 shows the variation in remnant HCF life at
823 K. The pre-cycled specimens were subsequently subjected to HCF
the N value of 1.36 and 1.44 with LCF pre-exposure, at temperatures,
loading up to fracture at those temperatures at selected N values (1.36
573 and 823 K. The specimens pre-cycled in LCF showed a decrease in
and 1.44). Choice of these stress levels under HCF cycling was based on
the residual HCF life which became more prominent on increasing LCF
pure HCF tests carried out earlier [7] which showed that at 823 K, in-
exposure; both at 573 and 823 K. Earlier works [6,8] have demon-
uence of DSA under HCF cycling was pronounced at N:1.36 resulting
strated the deleterious inuence of LCF pre-exposure on the remnant
in run-out whereas the same was minimal at N:1.44 [7]. These aspects
HCF life. This has been attributed to a shortening of the crack initiation
will be dealt with further, in Section 3.1. Hence, to study the inuence
phase under HCF as a result of the prior damage inicted during the
of N under LCF-HCF interaction at 823 K, it would be relevant to
LCF phase. However, for the same N of 1.36, remnant HCF lives were
perform tests at the above mentioned stress levels. However, for a
found to be signicantly higher at 823 K compared to 573 K, which can
temperature which is outside the DSA regime (573 K), slight variation
be attributed to the strong presence of DSA at 823 K [7]. Further, it was
in N from 1.36 to 1.44 resulted in only a minor dierence in the
observed that at 573 K, remnant HCF life assumes a smooth trend
remnant HCF life [7]. Hence, tests pertaining to LCF-HCF interaction
starting from 20% prior LCF exposure contrary to that in 823 K where a
were carried out at only a single N of 1.36 at 573 K. For all the HCF
gradual decrease in remnant life was found to take place. Since 573 K is
tests carried out (virgin or pre-LCF exposed specimens), three repeti-
a temperature where there is no inuence of DSA, the HCF stress (N :
tions were performed and the average values were used. The usual
1.36) is high enough to cause signicant plastic deformation from the
range of scatter was found up to the extent of 5%. Finally, the fracture
beginning, resulting in such a trend, as opposed to that of 823 K.
surfaces of the failed specimens were studied using Philips EM 502 SEM
However, even at 823 K, remnant HCF life was found to dier sig-
to evaluate the crack initiation and propagation modes and the striation
nicantly with a small variation in N from 1.36 to 1.44. Remnant HCF
morphology. Assessment of surface morphology was made by taking
life at N : 1.44 was found to be considerably lower compared to N :
acetate replicas on the failed specimens and observing them under
1.36 (Fig. 1). Previous study carried out by the authors has shown that
optical microscope. To obtain acetate replica from the samples, the
under HCF cycling at 823 K, inuence of DSA is prominent at N: 1.36
following failure criteria was used. Specimens were never fractured
while the same becomes lesser at a slightly higher N of 1.44 [7]. On the
during cycling and the test was stopped following a 40% drop in load
other hand, at 923 K, similar change in N from 1.36 to 1.44 resulted in
under LCF or a decrease in resonance frequency to a specic level under
minor variation in HCF lives, implying that inuence of DSA at 923 K
HCF, up to which the major crack has propagated signicantly. The
may be minimal irrespective of HCF stress. Thus, the observations made
substructural changes were studied by TEM (CM 200, M/s FEI, The
in Fig. 1 that a signicant increase in remnant HCF life with a decrease
Netherlands) using samples obtained from thin slices, cut at a distance
in N from 1.44 to 1.36, can be solely attributed to the strong inuence
very near (12 mm away) to the fracture surface. The slices were rst
of DSA at N: 1.36. These eects can be brought out more clearly by
mechanically polished down to about 70 m followed by electro-
plotting the dierence in remnant HCF lives between successive levels
polishing using a solution containing 20% perchloric acid and 80%
of LCF exposure against the degree of prior LCF exposure, at two dif-
methanol at 243 K ( 30 C) using a 20 V DC supply
ferent values of N, 1.36 and 1.44, at 823 K (Fig. 2). The dierence in
reductions in the remnant HCF lives was found to reach its maximum at
40% and 50% of LCF pre-exposure at N: 1.36 and 1.44 respectively.
This indicates that the rate of damage accumulation under prior LCF
was highest at the above exposures. In other words, LCF-HCF

92
A. Sarkar et al.
Fig. 2. Variation of dierence in remnant fatigue lives between dierent levels of prior
LCF exposure with degree of prior LCF exposure at dierent normalized stresses (823 K).
interaction was strongest for the above LCF pre-exposures. This suggests
that there is a critical damage (occurring at 40% LCF pre-exposure for
N: 1.36% and 50% LCF pre-exposure for N: 1.44) for which the LCF-
HCF interaction is the most eective. The maximum dierence in
remnant HCF life was noted at a higher LCF exposure of 50% at N: 1.36
compared to 40% observed at N: 1.44, indicating a delayed attainment
of the critical damage in the case of a lower N (Fig. 2). Similar concept
of critical damage has been brought out in the earlier investigations on
LCF-HCF interactions by the authors, at 923 K [6,8]. The dierence in
reductions in the remnant HCF lives started decreasing beyond 40%,
with a saturating trend from 60% LCF exposure onwards, at N: 1.44.
However, such saturation was not observed until 80% at a lower N of
1.36. The above observations indicate that at a N of 1.36, DSA mainly
results in a delay in attaining critical damage, under LCF-HCF interac-
tion (as seen from Fig. 2).
3.1.2. Eect of temperature
3.1.2.1. Prior LCF cycling followed by HCF at N: 1.44. Fig. 3 shows the
variation in remnant HCF life (N: 1.44) with LCF pre-exposure at
temperatures, 823923 K. The specimens pre-cycled in LCF showed a
decrease in the residual HCF life which became more prominent with
an increase in the LCF exposure. Initiation of microcracks under LCF
cycling could serve to bring down the HCF life by shortening the crack
initiation phase under HCF. The decreasing trend in remnant HCF life
Fig. 3. Variation of remnant HCF life with prior LCF exposure (%) for dierent tem-
peratures ranging from 823 to 923 K, at normalized stress of 1.44.
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Materials Science & Engineering A 708 (2017) 91103
Fig. 4. Variation of dierence in remnant fatigue life between 823 and 923 K with degree
of prior LCF exposure (%), at normalized stress of 1.44.
(Fig. 3) with LCF pre-exposure was found to be almost identical at all
temperatures. Even though the remnant HCF life is expected to decrease
with increase in temperature for the same N, in the present case, the
life variation with temperature did not follow such a trend. The
remnant HCF life seems to be very close in the temperature range
823923 K, as indicated in Fig. 3. However, careful observation reveals
that it is slightly higher at 823/873 K compared to 923 K, barring the
LCF life-fractions of 50% and 60% where the same was found to be
lower at 823/873 K compared to 923 K. To further elucidate these
observations, dierence in remnant HCF lives between 823 K and 923 K
is plotted against the prior LCF exposure in Fig. 4. It is important to note
that dierence in remnant lives between 823 and 873 K is very small and
within the range of usual scatter (5%). Hence, the dierence in the remnant
HCF lives between 823 K (Nf823K) and 923 K (Nf923K) was considered in the
plot. The plot showed that Nf823K - Nf923K decreased as the LCF pre-
exposure is increased, with a maximum dip at 50% pre-exposure
beyond which it again increases at 60% pre-exposure. Further, while
Nf823K - Nf923K is positive up to 40% of prior LCF exposure, the same
turned negative from 50% LCF life-fraction onwards (~ 3 105)
upto 60% LCF life-fraction (~ 4 104) (Fig. 7c). Beyond 60% LCF
pre-exposure, the Nf823K - Nf923K again turns positive; the dierence too
is very small and within the usual range of scatter (Fig. 4). The reverse
trend in remnant HCF life at 50% and 60% of prior LCF exposure
(change in Nf823K - Nf923K from positive to negative) may therefore be
attributed to the DSA eects from LCF. This is because, under LCF,
active presence of DSA leads to a higher stress response [7,11] resulting
in early initiation of cracks. Consequently, the eective crack length is
expected to be more at 50% and 60% of prior LCF exposure at 823 K
compared to 923 K where the DSA eects are minimal. The relatively
advanced crack formed at 823 K propagated quickly during the HCF
cycling resulting in a lower remnant life at that temperature compared
to 923 K for those prior LCF exposures. At higher levels of LCF
exposures (80%), the crack-initiation phase might be completed
irrespective of temperature and hence, no appreciable dierence in
remnant lives with respect to temperature is observed. At lower levels
of LCF pre-exposure (20/40%), the eective crack may not be large
enough to signicantly reduce the initiation phase under HCF. In such
case, the remnant life becomes more a function of the HCF cycling,
resulting in a higher value of Nf823K - Nf923K at those pre-exposures.
However, DSA eects under LCF gain signicance as the LCF pre-
exposure is increased, resulting in an increase in the eective crack
length under LCF cycling, thereby narrowing down Nf823K - Nf923K with
increase in LCF pre-exposure.
A. Sarkar et al.
Fig. 5. Variation of remnant HCF life with prior LCF exposure (%) for dierent tem-
peratures ranging from 573 to 923 K, at normalized stress of 1.36.
Fig. 6. Variation of dierence in remnant fatigue lives between 823 and 923 K with
degree of prior LCF exposure (%), at normalized stress of 1.36.
3.1.2.2. Prior LCF cycling followed by HCF at N: 1.36. The variation in
remnant HCF life with LCF pre-exposures at a lower N of 1.36 in the
temperature range 573923 K, is plotted in Fig. 5. The specimens pre-
cycled in LCF showed a decrease in the residual HCF life as the LCF pre-
exposure is increased, similar to the trend observed at N : 1.44.
However, unlike Fig. 3, in the present case, the remnant lives at 823/
873 K were found to be much higher compared to those observed at
923 K for almost all prior LCF exposures. To understand the inuence of
DSA on LCF-HCF interaction at N: 1.36, the dierence in remnant HCF
life between 823 K and 923 K (Nf823K - Nf923K) is plotted against prior
LCF exposure, in Fig. 6. It showed that Nf823K - Nf923K initially increased
upto 40% prior LCF exposure, before gradually decreasing upto 60%
prior LCF exposure, following which it became almost marginal at the
pre-exposure of 80%. The above behavior may be attributed to the
predominance of DSA under both LCF and HCF cycling at N: 1.36,
unlike the previous case (N: 1.44) where DSA eects only from LCF
were predominant. Upto 40% of prior LCF exposure, the benecial DSA
eects under HCF will be predominant resulting in an increasing trend
in Nf823K - Nf923K with LCF pre-exposure, as opposed to Fig. 4 where
Nf823K - Nf923K was found to decrease with increasing LCF pre-exposure
right from the beginning (20% LCF pre-exposure onwards). However,
following 40% LCF pre-exposure, the deleterious DSA eects under LCF
will start becoming stronger, counteracting the favorable inuence of
DSA arising from HCF cycling, thus lowering this dierence which
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Materials Science & Engineering A 708 (2017) 91103
becomes negligible at LCF pre-exposure of 80% (Fig. 6). It may be noted
from the earlier case (N: 1.44, 823 K) that the inuence of DSA arising
from prior LCF cycling was very prominent at 50% and 60% of pre-
exposure (Fig. 6). Hence, in the present case where DSA eects arising
from HCF also prevail, the competitive nature of damages between the
above eects is most pronounced at those LCF life-fractions. This is
reected in the form of a sharp drop in Nf823K - Nf923K from 2.4 107
(40% LCF pre-exposure) to 107 (50% LCF pre-exposure). Similar, but
slightly lower change in Nf823K - Nf923K was noted between 50% (107)
and 60% LCF pre-exposure (4 105) (Fig. 6). However, the dierence
in remnant HCF lives never turned negative in the present case (Fig. 6)
compared to that observed at N: 1.44 (Fig. 4), indicating that DSA
eects under HCF remain mostly dominant although the degree of such
eect may be curtailed to a signicant extent from the DSA eects
under prior LCF cycling for certain LCF exposures (50/60%).
3.2. Fractographic investigations
3.2.1. Fracture behavior under pure LCF or HCF conditions
Fracture surfaces of the specimens run to failure under LCF at 573
and 823 K are presented in Fig. 7. DSA occurring at 823 K resulted in
multiple crack initiation sites (Fig. 7a) along with the formation of
extensive secondary cracking (Fig. 7b) [7]. Extensive transgranular
Stage-II fatigue crack propagation was also noticed (Fig. 7b) char-
acterized by striations. Crack initiation sites were found to be com-
paratively lesser at 573 K (Fig. 7c) which is outside the DSA regime.
Further, the fracture surface consists only striations (Fig. 7d), without
any secondary cracking as observed at 823 K. Fracture surfaces of the
specimens that failed under pure HCF at a N of 1.36 were found to
contain mainly one or two crack initiation sites (Fig. 8ab), irrespective
of temperature (both 573 and 823 K). However, at 823 K, apart from
striated features, an extended faceted appearance is noted following the
initiation of crack (Fig. 8cd), which could be a manifestation of DSA
under HCF cycling.
3.2.2. Fracture behavior under LCF-HCF interaction
Fracture surfaces of specimens failed under LCF-HCF interaction
displayed characteristic features distinct from those obtained under
pure LCF or HCF. DSA was also seen to inuence the LCF-HCF inter-
action behavior which manifests itself in the fracture morphology, as
listed below. Experimental results indicated that inuence of DSA de-
pends on temperature as well as N, which also aects the fracture
morphology accordingly.
3.2.2.1. Inuence of temperature on remnant HCF lives (N:1.36)
3.2.2.1.1. Prior LCF cycling (20%) followed by HCF (573 K). The
fracture morphology pertaining to a temperature of 573 K which is
outside the zone of DSA (prior LCF exposure of 50% followed by HCF
cycling at N: 1.36, 573 K) was shown in Fig. 9. The fracture surface
showed multiple crack initiation sites as opposed to one or two
initiation sites found under pure HCF cycling (Fig. 9a). Multiple
cracks found in this case would have initiated during the LCF stage
itself. Since DSA-induced hardening is absent at 573 K, N of 1.36
implied a very high applied stress which facilitated coalescence of these
Stage-II cracks to from the major crack. The crack growth rate also
would have been accelerated under such situation leading to rapid
propagation of the major crack to failure (marked by white arrow at the
centre). This is reected from Fig. 9b showing Stage-II striations similar
to HCF failure of the virgin specimen at 573 K (Fig. 9a). As a result, very
poor residual HCF life of 1981 was obtained in the above case (Fig. 1).
3.2.2.1.2. Prior LCF cycling (20%) followed by HCF (823 K). The
fracture surface morphology at 823 K can be subdivided into ve
distinct zones when DSA gains prominence. This is presented in the
fractographs pertaining to the specimen failed under HCF (N: 1.36)
with 20% prior LCF exposure, at 823 K (Fig. 10). It may be noted that
LCF-HCF interaction is not so prominent at 20% LCF pre-exposure at 823 K,
A. Sarkar et al.
Fig. 7. Fracture surface of specimens failed under LCF (a)(b) 823 K [7] with (a) multiple crack initiation sites and (b) extensive secondary cracking and striations (c)(d) 573 K with (c)
less number of crack initiation sites (d) striations without secondary cracking.
implying that fracture manifestations at this loading conditions possibly
result from the DSA eects occurring mainly during HCF cycling . The zones
are marked in Fig. 10 as Zones 15 viz. (1) fatigue crack initiation (2)
transient crack arrest (3) faceted appearance with parallel river
markings (4) fatigue striations superimposed within the river-
markings on the facets and (5) highly striated region. Each zone
shown in Fig. 10 is represented separately in Fig. 11(ad) to reveal
the intricate features. For better understanding, a schematic illustration
of dierent zones is provided in Fig. 12(ac). Zone-1 & Zone-2 shown in
Fig. 10 are magnied in Fig. 11a. Zone-1 marks the initiation of the
crack which presumably occurred during the LCF stage (Fig. 12a). The
crack initiation was followed by a transient crack arrest regime (zone-2)
which signies a change in load from LCF to HCF (Fig. 10, also shown
in Fig. 12b). This is analogous to the crack retardation observed during
fatigue crack growth experiments due to periodic or spike overloading
(sudden application of a higher load) over a constant amplitude loading
[20,21]. Such a phenomenon is explained in literature based on crack
tip blunting [22], strain hardening [23], crack branching [24] etc.
However, the retardation eects are generally attributed to the eect of
residual plasticity that leads to compressive stresses ahead of the crack
tip and raises the crack opening load for subsequent crack growth,
eventually leading to crack arrest [21,24,25]. Borrego et al. [20] have
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Materials Science & Engineering A 708 (2017) 91103
observed that temporary crack retardation can manifest itself in the
form of a band-like region on the fracture surface, adjacent to the
overload zone containing an intense smeared area denoting premature
contact of the crack faces. Similar features were observed in zone-2 of
Fig. 11a in the form of a dark semi-circular band (width of ~ 100 m)
ahead of the crack front initiated under LCF (zone-1). This constitutes
almost 7% of the fracture area shown in Fig. 10. However, such features
were found to be absent at 573 K (Fig. 9) in spite of change in load
taking place during LCF-HCF interaction. This can be explained on the
basis that crack retardation under application of overload during
fatigue cycling is a strong function of the overload ratio (ratio of the
magnitude of overload to constant load) [20,26]. In the present case, it
is the ratio of the load corresponding to LCF cycling (higher load-
amplitude) to that corresponding to HCF cycling (lower load-
amplitude). The cyclic stress response at 823 K is much higher
compared to 573 K, owing to strong DSA in the former case [7],
which would have essentially caused a distinct LCF overload eect at
the former temperature. Once the residual compressive stress arising
out of the overload eect gets relaxed, the crack front ahead of the band
propagates further with progressive cycling under HCF. This is shown
as zone-3 in Fig. 10 (also seen from Fig. 12c). Marked portion of zone-3
(Fig. 10) is again magnied in Fig. 11b. This region basically shows a
A. Sarkar et al.
Fig. 8. Fracture surface of specimens failed under HCF (N: 1.36) (a) 573 K (b)(d) 823 K (a)(b) few crack initiation sites (c) extended faceted appearance after crack initiation (d) Stage
II cracking indicated by striations (shown through dotted arrows). Black arrow in (d) shows the direction of the major crack.
faceted appearance accompanied by river markings indicative of
crystallographic crack growth along the favorably oriented slip planes
(shown schematically in Fig. 12c). The river markings are found in
dierent orientations indicating that several Stage-I cracks are present,
many of which are arrested at microstructural barriers such as grain
boundary (marked in the gure). Most of the surface area of the
fractograph shown in Fig. 10 comprises of zone-3 (~ 1000 m which
amounts to almost 70% of the fracture area shown in the gure) which
can be attributed to the eect of DSA under HCF cycling. This is further
substantiated by the fact that similar features were observed also under
pure HCF cycling at 823 K (Fig. 8c). It was reported by Ritchie et al.
[27] that when the local plasticity ahead of the crack tip approaches
microstructural size-scales, crystallographic crack growth in the form of
faceted appearance is facilitated. A similar situation arises in the
present case due to DSA-induced hardening under HCF cycling which
reduces the plastic zone size associated with the crack, thus promoting
the above fractograhic features. Marked portion of Zone-4 shown in
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Materials Science & Engineering A 708 (2017) 91103
Fig. 10 (~ 15% of the fracture area) is presented in Fig. 11c where a
transition from crystallographic facets to striations is found to take
place. The width of the river markings gradually increases in this zone
with striations starting to appear inside the region between these
parallel markings, presenting a uted appearance (referred in
Fig. 12d). This is indicative of the transition in crack from Stage-I to
Stage-II where deformation through slip becomes more homogeneous
with activation of multiple slip systems. The river patterns ultimately
make way for a highly striated appearance which is indicated as Zone-5
in Fig. 10 (~ 8% of the fracture area). This highly striated region is also
shown in detail in Fig. 11d (referred in Fig. 12e). In this case, the crack
propagates along dierent slip-planes as a result of multiple slip. In
absence of DSA at 573 K, the transition of Stage-I (zone-1) to Stage-II
(zone-5) crack takes place very fast, evading zones 24. This has
resulted in a fracture surface fully dominated by striations, at the
above temperature (Fig. 9b). Consequently, a wide dierence in
remnant lives was found between the temperatures 573 and 823 K,
A. Sarkar et al.
Fig. 9. Fracture surface pertaining to loading condition: HCF cycling (N: 1.36) with prior
LCF exposure of 50%, 573 K (a) overall fracture surface showing initiation of multiple
cracks (marked by white arrows) (b) Stage-II crack propagation (white arrow indicates
direction of crack propagation).
Fig. 10. Zonewise representation of fracture surface of specimens failed under HCF cy-
cling (maxN: 1.36) with prior LCF exposure of 20% at t/2: 0.6%, 823 K. Thick white
arrow (dotted) indicates the direction of crack propagation.
for the same N (Fig. 1).
3.2.2.2. Inuence of N on remnant HCF lives (823 K)
3.2.2.2.1. Prior LCF cycling (20%) followed by HCF (N: 1.44). This
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Materials Science & Engineering A 708 (2017) 91103
section mainly pertains to the eect of N on fracture morphologies, at
823 K where strong presence of DSA is noted. However, inuence of
DSA becomes lower when the N is increased from 1.36 to 1.44 (Fig. 1).
Distinct zones appear in the fracture surface (Fig. 13) under HCF
cycling at N: 1.44 with 20% LCF pre-exposure, similar to that observed
for a lower N of 1.36 (Fig. 10). No signicant dierence was observed
with respect to zones 12 (~ 7%) between the two loading conditions of
N: 1.44 and 1.36 (Figs. 10 and 13). Zones 35 on the fracture surface
under the above loading condition are shown in Fig. 14(a-d). The extent
of zone-3 is greatly reduced in comparison with the previous case of N:
1.36, as can be observed by comparing Figs. 10 and 14. The width of
zone-3 was found to be ~ 700 m (50% of the fracture area) (Fig. 14a)
compared to ~ 1000 m in the earlier case (70% of the fracture area)
(Fig. 10). This indicates an early transition of zone-3 to zone-4 (shown
through Fig. 14b, magnied image of the marked portion A in Fig. 14a).
This is further corroborated from the fact that the image in Fig. 14b (N:
1.44) containing large number of river markings without any trace of
facet, is taken at a distance of ~ 300 m from initiation at the surface
(can be clearly observed from Fig. 14a). In contrast, the image
pertaining to zone-3 for the loading condition with N: 1.36 (40%
LCF pre-exposure, 823 K) showing well-dened facets, is being taken at
a distance of ~ 550 m from the surface initiation (Fig. 10). Magnied
image of the marked portion B of Fig. 14a (Fig. 14c) showed that wide
river markings gradually fade away to make way for zone-5,
characterized by Stage-II striations. Features pertaining to zone-5
remain similar irrespective of the applied stress in HCF (N: 1.36 and
1.44), wherein striations appear throughout the fracture surface
(Fig. 14d and Fig. 11d). The above observations suggest that the
major dierence between the two loading conditions (N : 1.36 and
1.44) was related to the area of zone-3 which was seen to be more for
the lower N of 1.36. As indicated earlier, this was caused mainly by the
extensive hardening occurring under DSA during HCF cycling which in
turn restrict the size of the plastic zone at the crack tip, resulting in a
slow crack propagation rate in the above zone. Similar observations
were also made by earlier researchers for fatigue crack propagation in
Alloy 718 wherein faceted appearance with parallel fracture markings
were identied as manifestations of very low fatigue crack-propagation
rates (105 mm/cycle) [28]. Hence, the inuence of DSA is manifested
mostly in way of extending zone-3 (N : 1.36) under HCF cycling. For a
loading condition where the inuence of DSA is less marked (N : 1.44),
the local plastic deformation in the vicinity of the crack was higher
from the beginning of the HCF cycling, since the DSA-induced
hardening is less pronounced. This allowed a relatively smooth
transition from zone-3 to zone-4 with the extent of zone-3
signicantly reduced (Fig. 14a). As a result, river markings started
widening in zone-3 itself with no trace of facets (Fig. 14b). This led to a
lower residual life at N: 1.44 compared to the case of N of 1.36
corresponding to 20% LCF pre-exposure (Fig. 1). Zone-4 marks an
increase in the plastic deformation at the crack tip irrespective of DSA
(both N : 1.36 and 1.44). Even if DSA is active (N: 1.36), the eect of
hardening caused by DSA has been outweighed over the course of
cycling, when zone-4 is reached. Hence, the crack propagation rate in
zone-4 will start increasing wherein striated features corresponding to
Stage-II crack appear (Figs. 11c and 14c, also referred in Fig. 12d). Such
striated features will eventually become more prominent at zone-5
(Fig. 8d and Fig. 14d, also referred in Fig. 12e). Similar concept was put
forth by earlier researchers during crack growth studies in Alloy 718, by
observing that the transition from heterogeneous to homogeneous slip
(characterized by well-dened striations) took place as the plastic zone
size grows bigger to contain dierent grains [28]. Under such cases, the
crack propagation rate was reported to increase from the earlier
105 mm/cycle to 102 mm/cycle.
3.2.2.3. Inuence of DSA in the active zone of LCF-HCF interaction
3.2.2.3.1. Prior LCF cycling (50)% followed by HCF (N:1.36,
823 K). When the prior LCF exposure is further increased to 50% and
A. Sarkar et al. Materials Science & Engineering A 708 (2017) 91103

Fig. 11. (a): Magnied image of the marked portion in zone-1 & 2 from Fig. 10. (b): Magnied image of the marked portion in zone-3 from Fig. 10 showing faceted appearance with river
markings.(c): Magnied image of the selected portion in zone-4 from Fig. 10 showing uted appearance marked by white arrows. Thick white arrow indicates the direction of crack
propagation. (d): Fracture surface of zone-5 depicted in Fig. 10 showing typical Stage-II striations. Thick white arrow indicates the direction of crack propagation.

subjected to HCF cycling at a N of 1.36 (823 K), both zones 3 and 4 was
seen to coexist, with no well-dened boundary between them
(Fig. 15a). This was further corroborated from the magnied image
of the marked portion of Fig. 15a (Fig. 15b) showing characteristics of
both zone-3 and zone-4 i.e. sharp facets with river markings as well as
ill-dened facets with striations superimposed on the river-markings. A
higher prior LCF cycling to 50% would have allowed most of the
initiated cracks (zone-1) to advance signicantly to zone-4, wherein
striations started appearing. However, for the same LCF exposure, there
may be some minute cracks which are still in zone-1. Occurrence of
DSA under HCF cycling will hinder fast advancement of these cracks
and they will propagate to zone-3 through crystallographic crack-
growth. Hence, characteristic features of both zones 3 and 4 were
observed together in the same region of the fracture surface for the
above loading condition. Nonetheless, this phenomenon is very local
since majority of the cracks have grown to Stage-II (zone-4) under LCF
cycling, limiting such features only to a small area of the fracture
surface, close to the initiation zone. As cycling proceeds under HCF,
transition of zone-4 to zone-5 will gain prominence rather than zone-1
to zone-3. However, only the biggest of the Stage-II crack in zone-4 will
further advance to zone-5 at the expense of other minor zone-4 cracks,
ultimately causing failure. This is shown in Fig. 15c (taken from a
region close to the overload failure in the fracture surface) where apart
from the major Stage-II crack (zone-5, marked by white arrow), several
other minor zone-4 cracks (indicated by ute-like appearance with
dierent orientations and striation spacings) are found (marked by
dotted white arrows). Since zone 4 is reached in the LCF stage itself.
Hence, signicant LCF-HCF interaction occurred at this pre-exposure
resulting in a large drop in residual HCF life (Fig. 1). This is also
reected as attainment of the critical damage at 50% LCF pre-exposure
(Fig. 2).
3.2.2.3.2. Prior LCF cycling (50)% followed by HCF (N: 1.44,
823 K). The fracture morphology pertaining to a higher N with
minimal inuence from DSA (N: 1.44, 823 K, 50% LCF pre-exposure)
was shown in Fig. 16. In this case, zone-3 ceased to appear. The image
which was taken at the same distance from the initiation zone as in
Fig. 15, represent mostly zone-5 of the fracture surface. This indicates
that transition from zone-4 to zone-5 is faster in this case, compared to a
lower N of 1.36. Even though the major crack (zone-5) (marked by
white arrow) was found to propagate further to failure, several other
smaller cracks (marked by black arrows) were present as indicated by
dierent orientations and sizes of striations. The striation spacing was
found to be continually increasing for the major crack (marked by white
arrow) leading to failure while the other Stage-II cracks (marked by
black arrows) gradually became non-propagating which is clear from
the decreasing size of striation spacing in the direction of their growth.
These cracks thus manifest themselves as isolated pockets of striations
on the fracture surface. Similar features were also reported by the

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A. Sarkar et al. Materials Science & Engineering A 708 (2017) 91103

Fig. 12. Zone wise depiction of the fracture surface

of a specimen failed under HCF cycling with prior
LCF exposure where DSA is highly active. With
progressive cycling (marked by black arrows) as
each zone is formed (marked as (a)(e)), a new
characteristic feature is added in the fracture sur-
face. The newly added features are presented in
mentioned in the captions for each zone. Dierent
fracture marks presented in the schematic are also
listed in a tabular format below. Note: The crack lo-
cated on the left is assumed to be the dominant crack
leading to failure.

Fracture mark Connotation

Crack Initiation

Crack Arrest

Faceted appearance

Fluted appearance

Striations with overload

can quickly advance to zone-5. Moreover, this process is faster for a

loading condition where the DSA eects are not very prominent (N:
1.44, 823 K) compared to a loading condition dominated by DSA (N:
1.36, 823 K). Presumably, this resulted in a much lower residual life at
N: 1.44 compared to N: 1.36, corresponding to 50% LCF pre-exposure
(Fig. 1). In other words, LCF-HCF interaction gains predominance early
at a higher N of 1.44 compared to N: 1.36. This is also reected from
the shift in critical damage to a lower LCF exposure of 40% at a higher N
of 1.44, as opposed to 50% at N: 1.36 (Fig. 2).

3.2.2.4. Inuence of DSA outside the zone of eective LCF-HCF interaction

Fig. 13. Depiction of zone 13 in the fracture surface of specimens failed under HCF
cycling (N: 1.44) with prior LCF exposure of 20%, 823 K.
authors at 923 K in an earlier investigation, as an important
manifestation of LCF-HCF interaction [8]. It is clear from the above
observations that, for a higher LCF exposure (50%), reaching zone-4 in
the LCF stage itself has curtailed the residual HCF life, since the same
3.2.2.4.1. Prior LCF cycling (80)% followed by HCF (N: 1.36 and
1.44, 823 K). Increase in LCF exposure to 80% almost nullied the
eect of the DSA irrespective of the applied stress under HCF (as seen
from Figs. 1 and 2), since the major Stage-II crack relevant to failure
might have formed during the LCF cycling itself, which will propagate
very quickly to failure under HCF. This was also reected from Fig. 17
showing mostly Stage-II crack propagation (zone-5) without any traits
of striation pockets. With progressive cycling, as the crack propagates,
the striation spacing of the major crack increased rapidly typical of
fatigue failure (marked by the black arrow). This is because, unlike
previous cases, the major crack is formed in the LCF stage itself by
coalescence of small Stage-II cracks, since the prior exposure to LCF is
very high (80%). As a result, fracture surface appearance for this
loading condition was found to be similar for a specimen failed under

99
A. Sarkar et al.
Fig. 14. (a): Depiction of zone 35 in the fracture surface of specimens failed under HCF cycling (N: 1.44) with prior LCF exposure of 20%, 823 K. (b): Magnied image of the Marked
portion A from Fig. 9(a) showing the transition from zone-3 to zone-4. (c): Magnied image of the Marked portion B from Fig. 9(a) showing the transition from zone-4 to zone-5. (d):
Fracture surface of zone-5 showing typical Stage-II striations. Loading condition: HCF cycling (N: 1.44) with prior LCF exposure of 20%, 823 K. Thick white arrow indicates the direction
of crack propagation.
LCF (evident from Fig. 7b). Hence, there is almost no dierence in
residual HCF lives post LCF exposure of 80% between the two dierent
N at this LCF pre-exposure, as depicted from Figs. 1 and 2 (N: 1.36 and
N: 1.44) indicating that no signicant LCF-HCF interaction is taking
place. The above observations also explain the absence of the
aforementioned striation pockets in this case, which originate in the
HCF stage due to lack of coalescence among the smaller Stage-II cracks
developed during LCF cycling. It may be noted that crack coalescence
will be lacking even under LCF cycling when the prior LCF exposure is
50%. Hence, under such cases, when the specimen is subjected to
HCF loading, distinct appearance of zone-3 and zone-4/striation
pockets will be found, leading to a delay in the onset of zone-5 crack.
3.3. Microstructural investigations in terms of surface replica and TEM
3.3.1. Surface replica
Surface features pertaining to the specimen failed under pure LCF at
823 K is presented in Fig. 18(a, b). Apart from the major crack
(Fig. 18a) [7], extensive secondary cracking is observed (Fig. 18b).
Fig. 19 shows the surface feature of a specimen which went for run-out
at 823 K (N: 1.36) [7]. Although the stress is well above the YS, the
surface damage in terms of slip activity is seen to be negligible as in-
dicated by the absence of any slip lines or bands. Further, no evidence
of surface crack initiation was found. Some small oxide scales were
observed on the surface which however, did not contribute to crack
100
Materials Science & Engineering A 708 (2017) 91103
initiation. This reinforces the statements made in Section 3.1 implying
that DSA strongly prohibits localized plastic deformation under HCF,
leading to suppression of crack initiation. Fig. 20(ac) denotes the
surface features of the specimens failed under HCF cycling (N: 1.44 and
1.36) with prior LCF exposure of 50%. Signicant surface relief was
observed adjacent to the primary crack front for N: 1.44 (Fig. 20a).
Marked-up portion from Fig. 20(a) showed formation of ne slip lines
and slip-bands along with formation of small secondary cracks around
the primary crack (Fig. 20b). It may be recalled that DSA eects under
HCF cycling are negligible at N: 1.44 (823 K). Under such situations, at
a high N > 1, slip activities near the major crack formed during LCF
exposure will be highly accentuated during the course of HCF cycling.
Fig. 20(c) shows the surface features for the specimen failed under HCF
cycling at N: 1.36 with LCF pre-exposure of 50%. In this case, no de-
tectable surface relief was observed, even in the vicinity of the major
crack. This suggests that the plastic deformation in terms of slip activity
is minimized for N: 1.36. This correlates well with the arguments made
previously that under HCF cycling, DSA suppresses the localized plastic
deformation near the crack, thereby delaying its propagation.
3.3.2. TEM investigations
TEM images for specimens failed under pure LCF and HCF as well as
under LCF-HCF interaction are shown in Fig. 21. The specimen that
went for run-out under HCF at N: 1.36 shows minimal dislocation
activity (Fig. 21a). Some isolated dislocations were found spread
A. Sarkar et al.
Fig. 15. Fracture surface pertaining to loading condition: HCF cycling (N: 1.36) with
prior LCF exposure of 50%, 823 K. (a) Co-existence of zone-3 and zone-4 (b) magnied
image of marked portion of (a) showing facets with river-markings (zone-3) and uted
appearance (zone-4) together (c) Stage-II crack propagation with major crack (zone-5,
marked by white arrow) propagating at the cost of other minor Stage-II non-propagating
cracks of uted appearance (zone-4, marked by dotted white arrows).
randomly in the substructure which well-correlate with the replica
image of the run-out sample under HCF cycling shown in Fig. 19. In
contrast, the specimen undergoes gross plastic deformation resulting in
the formation of specic dislocation substructure under LCF at 823 K
(Fig. 21b). However, cross-slip does not seem to be predominant due to
presence of strong DSA present at 823 K, resulting in a highly non-
uniform cell structure. This was further corroborated by Reddy et al.
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Materials Science & Engineering A 708 (2017) 91103
Fig. 16. Fracture surface pertaining to loading condition: HCF cycling (N: 1.44) with
prior LCF exposure of 50%, 823 K showing Stage-II crack propagation in zone-5. Major
crack in zone-5 (marked by white arrow) is propagating at the expense of minor cracks
(marked by black arrows) which too are in zone-5.
Fig. 17. Fracture surface pertaining to loading condition: HCF cycling (N: 1.36) with
prior LCF exposure of 80%, 823 K showing Stage-II crack propagation (propagation of the
major crack is marked by black arrow) with continually increasing striation spacing.
[11] showing traces of planar and mixed slip mode at 823 K, depending
on the strain amplitude applied. TEM image of the specimen failed
under HCF cycling (N: 1.36) with prior LCF exposure of 50% (Fig. 21c)
also does not show any major development in substructure. Only some
planar arrays of dislocations were noticed interspersed with small dis-
location loops indicating a strong inuence of DSA. It is important to
note that development of substructure under LCF-HCF interaction is
entirely dierent at 923 K where inuence of DSA is minimal [8]. Ex-
tensive formation of microtwins was noticed at that temperature on
attaining the critical damage. [8]
4. Summary
DSA was found to be operative in the temperature range of
823923 K with a peak in the range 823873 K. Remnant HCF life was
found to decrease with increase in LCF pre-exposure irrespective of
A. Sarkar et al. Materials Science & Engineering A 708 (2017) 91103

Fig. 18. Replica image of specimen failed under LCF at t/2: 0.6% showing (a) plastic
deformation in terms of slip bands (marked by white arrows) in the vicinity of primary
crack [7] (b) secondary cracking.

Fig. 19. Replica image showing the surface feature of the specimen went for run-out at Fig. 20. Replica image of specimens failed under HCF cycling (N: 1.44) at 823 K with
N: 1.36 showing negligible slip activity [7]. prior LCF exposure of 50% with (a)-(b) N: 1.44 and (c) N: 1.36 showing (a) primary
crack (marked by black arrow) and short secondary cracks (marked by white arrows) (b)
temperature (823923 K). Inuence of DSA was found to be weaker at a magnied view of the surface relief developed in the vicinity of primary crack; dotted
white arrow indicates a short secondary crack and white arrows denote ne slip bands (c)
higher applied stress in HCF, wherein the DSA eects from LCF were
primary crack with no detectable surface damage.
predominant, resulting in lower remnant HCF lives at 823 K compared
to 923 K. At a lower value of the HCF stress, the DSA eects from HCF
were more pronounced leading to a strong competitive damage be-
tween DSA eects from both LCF and HCF. The remnant HCF lives were

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A. Sarkar et al. Materials Science & Engineering A 708 (2017) 91103

ultimately pushed up since the DSA eects from HCF proved more
decisive compared to that of LCF at lower stress. The above eects were
more prominent at intermediate levels of prior LCF exposure. At a
temperature in the range of DSA (823 K), fracture surface of a specimen
under HCF cycling (with or without LCF pre-exposure) was found to
contain an extended zone of facets with parallel river markings before
the transition to striated appearance. In contrast, at a temperature
outside the DSA regime (573 K), the transition from Stage-I to Stage-II
crack took place very fast, resulting in a vast dierence in lives between
the above temperatures. In the LCF exposures where strong LCF-HCF
interaction is taking place or critical damage is reached, the inuence of
DSA is neutralized to some extent on the account of Stage-II crack
formation in the LCF stage itself. The Stage-II cracking gets delayed at
an applied stress where the inuence of DSA is very high (N: 1.36),
resulting in a delayed attainment of the critical damage or a rightward
shift in the zone of eective LCF-HCF interaction.

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Fig. 21. Substructures of specimens (a) run-out under pure HCF cycling (N: 1.36)
showing isolated dislocations (b) failed under LCF showing non-uniform cell structure
and (c) failed under HCF (N: 1.36) with prior LCF exposure of 50% planar arrays of
dislocations (marked by black arrows) along with dislocation loops (marked by red
arrow), at 823 K.

103