CHAPTER 1.

EFFECT OF TENSILE HOLD ON THE FATIGUE

BEHAVIOR AND DEFORMATION MECHANISM

The current chapter illustrates the effect of temperature on fatigue properties, deformation

mechanisms, dislocation-dislocation interactions, dislocations networks, dislocation-precipitate

and fracture behavior at above service limit temperature, and ageing and above ageing

temperatures. An in-depth characterization of the deformed specimens has been carried out, and

a deformation mechanism has been analyzed.

1.1 CYCLIC DEFORMATION BEHAVIOUR AND STRESS RELAXATION

Figs. 6.1-6.2 shows the hysteresis loop for the first, half-life, and last cycles of the SU-263 alloy

tested at temperatures of 1023, 1073, 1123K, and 1173K with one minute and 5 minutes tensile

hold. The hysteresis loops exhibit type C serrations at one MTH with all testing temperatures, as

shown in Fig. 6.1. While type B serrations at 1023 K at 5 MTH, and type B+C serrations at five

MTH with 1073 K, 1123 K, and 1173 K, as illustrated in Fig. 6.2. The stress relaxation during

the tensile holding of one and five minutes at ± 0.4% and ± 0.8% strain amplitude are shown in

Fig. 6.3. It depicts that the stress relaxation rate is high initially for a few seconds and gradually

decreases for the rest of the dwell period at both one and five MTH
Figure 6.1 The hysteresis loops for the first, half-life, and last cycles of specimen fatigue tested
at ± 0.7% strain amplitude with a one-minute tensile hold at a temperature of (a)
1023K, (b) 1073, (c) 1123K, and (d) 1173K.
Figure 6.2 The hysteresis loops for the first, half-life, and last cycles of specimen fatigue tested
at ± 0.8% strain amplitude with a five-minutefive-minutes tensile hold at a
temperature of (a) 1023K, (b) 1073, (c) 1123K, and (d) 1173K.
Figure 6.3 Half-life stress relaxation curve at (a) 0.4 % strain amplitude with one-minute tensile
hold, (b) 0.4 % strain amplitude with five minutes tensile hold, (c) ± 0.8 % strain
amplitude with one-minute tensile hold, and (d) ± 0.8 % strain amplitude with five
minutes tensile hold.

1.2 CYCLIC STRESS RESPONSE AND FATIGUE PROPERTIES

The cyclic stress response for various temperatures and strain amplitudes at one- and five-minute

tensile holds is illustrated in Figs. 6.4 and 6.5, respectively. Figs. 6.4 and 6.5 show that at 1023

K, the alloy exhibits initial hardening followed by an almost steady state at low strain amplitude

and peak hardening, with no softening at high strain amplitude. At 1073 K and 1123 K, the alloy

depicted initial hardening and gradual softening at all the strain amplitudes, while at 1173 K, the

alloy exhibited limited hardening followed by softening, and the stress amplitude reached nearly

equal at all strain amplitudes. It is evident that hardening behaviour slowly reduces as a function
of increasing temperature, finally reaching a steady state at one and five minutes of tensile hold

time.

Figure 6.4 Cyclic stress response curves for various strain amplitudes with a one-minute tensile
hold at (a) 1023 K, (b) 1073 K, (c) 1123 K, and (d) 1173 K, illustrating the hardening
behavior slowly reduces as a function of increasing temperature, finally reaching a
steady state at 1173 K.
Figure 6.5 Cyclic stress response curves for various strain amplitudes with a five-minute tensile
hold were tested at temperatures of (a) 1023 K, (b) 1073 K, (c) 1123 K, and (d) 1173
K.

The fatigue properties at half-life obtained through the CFI tests conducted at different hold

times, strain amplitudes, and temperatures are summarized in Tables 6.1 and 6.2. The results

show that the stress required to achieve the desired strain amplitude decreases with increased

temperature. Also, the number of cycles to failure is higher at 1123 K and 1173 K compared to

1023 K and 1073.

Table 6.1 Creep-fatigue properties of SU-263 alloy at one-minute tensile hold.
Δσ
Δϵt 2 Δϵe Δϵ p
(%) T (K) (%) (%) Nf
2 2 2
(MPa)

1023 439 0.23 0.17 440

1073 374 0.25 0.15 561

0.4
1123 411 0.22 0.18 464

1173 366 0.16 0.24 445

1023 485 0.24 0.26 202

1073 439 0.20 0.30 226

0.5
1123 437 0.21 0.29 365

1173 351 0.17 0.33 374

1023 586 0.27 0.43 90

1073 490 0.25 0.45 177

0.7
1123 478 0.22 0.48 188

1173 336 0.13 0.57 201

1023 682 0.33 0.47 41

1073 514 0.23 0.57 83

0.8
1123 492 0.26 0.54 145

1173 364 0.16 0.64 181

Table 6.2 Creep-fatigue properties of SU-263 alloy at five-minute tensile hold.
Δσ
Δϵt 2 Δϵe Δϵ p
(%) T (K) (%) (%) Nf
2 2 2
(MPa)

1023 460 0.23 0.17 216

1073 399 0.22 0.18 319

0.4
1123 382 0.21 0.19 354

1173 357 0.14 0.26 356

1023 566 0.24 0.26 52

1073 432 0.20 0.30 139

0.5
1123 427 0.20 0.30 289

1173 359 0.17 0.33 201

1023 581 0.27 0.43 41

1073 486 0.13 0.57 102

0.7
1123 463 0.23 0.47 212

1173 367 0.14 0.56 160

1023 653 0.17 0.53 27

1073 492 0.19 0.61 86

0.8
1123 476 0.28 0.52 139

1173 380 0.16 0.64 109

1.3 STRAIN-LIFE BEHAVIOR

Fig. 6.6 a and b illustrate the Coffin-Manson plots, which exhibited linear behaviour at 1023 K,

1073 K, 1123 K, and 1173 K with a one-minute and five-tensile hold, respectively. It depicts that

the slope of the C-M plot is increasing with increasing temperature. TheIt is evident that the

fatigue ductility increases with temperature. Fig. 6.7 a and b illustrate the plot between stress

amplitude vs. plastic strain at one- and five-minute tensile holds. It exhibits that the slope is

decreasing with increasing temperature. TheIt is evident that the cyclic hardening behaviour

decreases with temperature. The obtained fatigue constants from the Coffin-Manson plot and

stress amplitude vsvs. plastic strain amplitude are given in Table. 6.3. It shows that the fatigue

ductility increases, and cyclic strength decreases with increasing temperatures.

Figure 6.6 The C-M plots of the SU-263 alloy tested at elevated temperatures for (a) a one-
minute tensile hold and (b) a five-minute tensile hold, illustrating the slope of the C-
M plot increases with temperature.
Figure 6.7 The plastic strain amplitude vs. the stress amplitude curve, plotted on a log-log scale
for the tests conducted at 1073 K, 1123 K, and 1173 K, for (a) one-minute tensile
hold and (b) five-minute tensile hold shows a decreasing slope with the increasing
temperature.

Table 6.3 Creep-fatigue properties of SU-263 alloy at one-minute tensile hold.

'
K
' '
Condition c ε f n
(MPa)

1023 K- 1 MTH -0.45 0.04 0.40 5370

1073 K- 1 MTH -0.70 0.23 0.24 1778

1123 K- 1 MTH -0.90 0.93 0.16 1140

1173 K- 1 MTH -1.02 2.59 0.03 295

1023 K- 5 MTH -0.53 0.04 0.27 2624

1073 K- 5 MTH -0.95 0.08 0.17 1185

1123 K- 5 MTH -1.05 2.21 0.21 1445

1173 K- 5 MTH -0.817 0.54 0.06 501

1.4 MICROSTRUCTURAL EVOLUTION DURING CREEP-FATIGUE
INTERACTION AT ELEVATED TEMPERATURES

The evolution of microstructural changes as a function of tensile hold, strain amplitude, and

temperature are shown in Figs. 6.8- 6.19. Figs. 6.8 a-f illustrates TEM bright field micrographs

of creep-fatigue tested specimens at one-minute tensile hold and temperatures of 1023 K, 1073

K, 1123 K, and 1173 K. The results show that the planar slip bands are oriented in more than one

direction at all low and high temperatures and strain amplitudes. Also, the slip bands oriented in

multiple directions in the specimen tested with a five-minute tensile hold, as shown in Fig. 6.9.

Fig. 6.10, attempts to analyze the effect of temperatures and tensile hold on dislocation

distribution and precipitate size. Fig. 6.10 exhibits manya huge number of dislocations arranged

as an array (slip band) and moving parallel to each other taken in [011] zone axis at 1023 K with

a strain amplitude of ± 0.8% and one MTH. The slip bands are arranged more closely with

increasing tensile hold and no change in precipitate size, as shown in Fig. 6.10 b under two-

beamtwo beam conditions ( ⃗g=0 22) along [111] zone axis. With increasing temperature and

holding time, the density of dislocations is decreased, and precipitates are coarsened, as shown in

Figs. 6.10c and d taken in [011] zone axis at 1173 K.

Fig. 6.11 illustrates the interaction between precipitate and dislocation as a function of

temperature and holding time. Fig. 6.11 showsa shows precipitate-dislocation interaction taken in

two beam conditions ( ⃗g=202) of [111] zone axis at 1073 K with ± 0.8% strain amplitude and a

one MTH. The holding time and temperature increased further, the dislocations-precipitate

interaction changed to form a loop around the precipitate due to precipitate coarsening, and the

number of dislocations reduced, as shown in Fig. 6.11b-f. Fig. 6.12a shows the presence of nano
twin inside the matrix. It is confirmed with the elected area diffraction pattern taken in the [014]

zone axis, as shown in Fig. 6.12b.

Figs. 6.13-6.19 showsshow the segregation of chromium and titanium with respect to

temperatures and holding time. Figs. 6.13a-f showsshow the STEM analysis of elemental

mapping at 1073 K with one MTH. The results exhibit that the chromium starts segregating at

the twin boundary in the matrix. Fig. 6.14 shows the elemental mapping analysis at 1123 K with

one MTH, and Fig. 6.15 depicts the elemental mapping analysis at 1173 K with one MTH. The

results show that with increasing temperature, more chromium segregated in the matrix forms a

needle shape at the twin boundary. However, no chromium segregation was observed in a

specimen tested at 1023 K, as shown in Fig. 6.16. At 1073 K with five MTH, depicted the array

of needle-shaped structures of chromium segregation within the matrix. Further, increased the

temperature above 1073 K increased, the amount of chromium segregation increased, and the

morphology changed from needle to irregular cubic shape, as shown in Figs. 6.17-6.19. The

observation indicates that the segregation of chromium depends on temperature and holding

time.
Figure 6.8 TEM bright-field low magnification micrographs of creep fatigue-tested specimens at
(a) 1023 K with ± 0.4% strain amplitude and a one MTH,(b) 1023 K with ± 0.8%
strain amplitude and a one MTH, (c) 1073 K with ± 0.8% strain amplitude and a one
MTH, (d) 1123 K with ± 0.4% strain amplitude and a one MTH, (e) 1123 K with ±
0.8% strain amplitude and a one MTH and (f) 1173 K with ± 0.8% strain amplitude
and a one MTH, showing the slip bands are oriented more than one direction at all
conditions.

Figure 6.9 TEM bright-field low magnification micrographs of creep fatigue-tested specimens at
(a) 1123 K with ± 0.8% strain amplitude and a one MTH and (b) 1123 K with ± 0.8%
 strain amplitude and a five MTH, illustrating the slip bands are arranged more
closely with increasing holding time.

Figure 6.10 TEM bright-field micrographs of creep fatigue-tested specimens showing (a) very
dense dislocation and dislocation interact with each other taken in [011] zone axis at
1023 K with ± 0.8% strain amplitude and a one MTH, (b) the slip bands are arranged
more closely taken in beam conditions ( ⃗g=0 22) of [111] zone axis 1023 K with ±
0.8% strain amplitude and five MTH, (c) dislocation looping around the precipitates
taken in two beam conditions ( ⃗g=111 ) of [011] zone axis 1173 K with ± 0.8% strain
amplitude and a one MTH and (d) very few dislocations and coarsened precipitates
taken in [011] zone axis 1173 K with ± 0.8% strain amplitude and five MTH. The
images illustrate that with increasing temperature and hold time decreases, the
number of dislocations decreases, and precipitates are coarsening.
Figure 6.11 TEM bright-field micrographs of creep fatigue-tested specimens showing (a)
precipitate-dislocation interaction taken in two beam conditions ( ⃗g=202) of [111]
zone axis at 1073 K with ± 0.8% strain amplitude and a one MTH, (b) the
dislocations loop around the precipitate at 1073 K with ± 0.8% strain amplitude and a
five MTH, (c) precipitate-dislocation looping and dislocation-dislocation interaction
at 1123 K with ± 0.8% strain amplitude and a one MTH, (d) precipitate-dislocation
looping and presence of nano twins inside the matrix taken in two beam conditions (
⃗g=200) of [014] zone axis at 1123 K with ± 0.8% strain amplitude and a five MTH,
(e) many precipitates looped by dislocation taken in two beam conditions ( ⃗g=111)
of [011] zone axis at 1173 K with ± 0.8% strain amplitude and a one MTH and (f)
precipitate-dislocation looping and coarsened precipitates at 1173 K with ± 0.8%
strain amplitude and a five MTH.
Figure 6.12 TEM bright-field micrographs of creep fatigue-tested specimens at 1123 K with
0.8% strain amplitude and 5 MTH showing the presence of a twin inside the matrix
and (b) selected area diffraction pattern taken in [014] zone axis captured at the
region marked in the image (a).

Figure 6.13 (a) Bright-field TEM micrograph showing dislocations and twin boundary inside the
matrix and (b-f) STEM elemental mapping showing segregation of chromium at the
 twin boundary and (Ti, Mo) carbides inside the matrix at 1073 K with ± 0.8% strain
amplitude and a one MTH.

Figure 6.14 (a-f) STEM elemental mapping showing segregation of chromium inside the matrix
at 1123 K with ± 0.8% strain amplitude and a one MTH.
Figure 6.15 (a-f) STEM elemental mapping showing segregation of chromium inside the matrix
at 1173 K with ± 0.8% strain amplitude and a one MTH.
Figure 6.16 (a-d) STEM elemental mapping shows no chromium segregationshowing no
segregation of chromium at 1023 K with 0.8% strain amplitude and a five-minute
tensile hold.
Figure 6.17 (a-d) STEM elemental mapping shows no chromium segregationshowing no
segregation of chromium at 1023 K with 0.8% strain amplitude and a five-minute
tensile hold.
Figure 6.18 (a-f) STEM elemental mapping illustratesillustrating the segregation of chromium
and (Ti, Mo) carbide segregationcarbides along the grain boundaries and within the
matrix at 1123 K with ± 0.8% strain amplitude and a five MTH.
Figure 6.19 (a-f) STEM elemental mapping shows chromium segregationshowing the
segregation of chromium and few (Ti, Mo) carbides along the grain boundaries and
within the matrix at 1173 K with ± 0.8% strain amplitude and a five MTH.

1.5 FRACTOGRAPHY

Figs. 6.20-6.23 showsshow the effect of tensile hold time and temperature on the fracture

surface. Fig. 6.20 shows the fracture of the specimen tested at one MTH with ± 0.4% strain

amplitude, exhibiting secondary intergranular cracks, dimples cleavage facets, and grain

boundary decohesion at 1023 K, as shown in Figs. 6.20 a-c. As the temperature increased to

1073 K, the alloy exhibited more cleavage facets and very few dimples and voids, as depicted in

Figs. 6.20d-f. However, in the specimen tested at 1123 K and 1173 K with low strain amplitude,

the cracks are initiated from the surface and covered with an oxidation layer. It also reveals only

dimples and very few facets on the surface, as illustrated in Figs. 6.20 g-l. Fig. 6.21 exhibits the

fracture of the specimen tested at one MTH with ± 0.8% strain amplitude. Fig. 6.21 exhibits the
fracture surface of the specimen tested at one MTH with ± 0.8% strain amplitude. As shown in

Figs, itIt reveals morea higher number of second cracks and cleavage facets thancompared to the

specimen tested at ± 0.4% strain amplitude, as shown in Figs. 6.21 a, b, d, e, g, and h. Figs. 6.21c

and f show the presence of creep cavities and dimples at the grain boundary. However, the

specimen tested at 1173 K exhibits quasi-cleavage-type fracture, as shown in Figs. 6.21 j-l. Fig.

6.22 illustrates the fracture surface of the specimen tested at five MTH with ± 0.4% strain

amplitude, exhibiting secondary intergranular cracks, cleavage facets, grain boundary

decohesion, and dimples in the matrix and grain boundary at 1023 K and 1073 K, as shown in

Figs. 6.22 a-f. The temperature increased to 1073 K, and the alloy exhibited many numbers of

cleavage facets compared to 1023 K. Figs. 6.22 g, h, j, and k show the crack initiation site and

crack propagation direction at 1123 K and 1173 K. The fracture surface exhibits fatigue striation

and fracture quasi-cleavage type. Figs. 6.22 i and l show oxide particles at the crack initiation

site. Fig. 6.23 shows the fracture of the specimen tested at five MTH with ± 0.8% strain

amplitude. It exhibits manya high number of cleavage facets compared to low strain amplitude,

as depicted in Fig. 6.23 a-i. At 1173 K, the crack propagates through the transgranular region,

and the fracture surface is covered with an oxide layer, as shown in Fig. 6.23 j-l.
Figure 6.20 SEM fractographs of creep fatigue-tested specimens at ± 0.4% strain amplitude with
one MTH showing, (a) intergranular crack and cleavage facets at low magnification,
(b) grain boundary decohesion, cleavage facets and dimples on a transgranular
region, (c) a magnified view of the marked area in micrograph (b) exhibiting dimples
at 1023 K, (d) grain boundary decohesion at low magnification, (e) cleavage facets,
(f) a magnified view of the marked area in micrograph (e) exhibiting dimples and
delaminated pores at 1073 K, (g) the crack initiation site and fracture surface covered
with oxide layer, (h) fully covered with elongated dimples on transgranular and
intergranular regions, (i) a magnified view of the marked area in micrograph (h)
 exhibiting dimples at 1123 K, (j) the crack initiation site, (k) fully covered with oxide
layer and elongated dimples on transgranular and intergranular regions and (l) a
magnified view of the marked area in micrograph (k) exhibiting few cleavage facets,
oxide particles at 1173 K. The observations indicate that the nature of fracture
changes with increasing temperatures.

Figure 6.21 SEM fractographs of creep fatigue-tested specimens at ± 0.8% strain amplitude with
one MTH exhibiting, (a) crack propagation direction (marked in red arrow) and grain
boundary decohesion at low magnification, (b) grain cleavage facets and dimples on
a transgranular region, (c) exhibiting dimples and fatigue striations at 1023 K, (d)
crack initiation site and crack propagation direction at low magnification, (e) grain
boundary decohesion, tornteared twins and cleavage facets, (f) a magnified view of
dimples 1073 K, (g) cleavage facets at low magnification image, (h) quasi-cleavage
facets, (i) dimples at 1123 K, (j) the crack initiation site and propagation direction,
(k) and (l) fatigue striations at 1173 K.
Figure 6.22 SEM fractographs of creep fatigue-tested specimens at ± 0.4% strain amplitude with
five MTH exhibiting, (a) intergranular crack and cleavage facets, (b) grain boundary
decohesion, (c) a magnified view of the marked area in micrograph (b) exhibiting
dimples on the transgranular region at 1023 K, (d) intergranular crack at low
magnification, (e) cleavage facets and fatigue striations, (f) a magnified view of the
marked area in micrograph (e) showing dimples at 1073 K, (g) the crack initiation
site at low magnification, (h) crack propagation direction and fatigue striations, (i) a
magnified view of the marked area in micrograph (h) exhibiting presence of oxide
 particle in crack initiation site at 1123 K, (j) the crack initiation site, (k) crack
propagation directions and (l) presence of oxide particles at 1173 K.

Figure 6.23 SEM fractographs of creep fatigue-tested specimens at ± 0.8% strain amplitude with
five MTH exhibiting, (a) fracture surface at low magnification, (b) cleavage and
quasi-cleavage facets, (c) grain boundary decohesion at 1023 K, (d) cleavage facets
at low magnification, (e) and (f) exhibiting grain boundary decohesion at 1073 K, (g)
the crack initiation site at low magnification, (h) quasi-cleavage facets, (i) fatigue
striations and dimples at1123 K, (j) the crack initiation site at low magnification, (k)
 and (l) magnified view of marked in (j) illustrating crack path and oxide particle at
1173 K.

1.6 EFFECT OF HOLDING TIME AND TEMPERATURE ON FATIGUE

PROPERTIES

The C-F properties of one MTH (Table. 6.1) show that with increasing temperature, the number

of cycles to failure decreased with increasing temperature, and the half-life stress amplitude

increased. At five minutes of tensile hold (Table 6.1), the C-F life increased with temperature up

to 1123 K, the temperature increased further, and the fatigue life decreased at 1173 K. Generally,

each cycle in the C-F test induced some damage to the material. The progression of this damage

is effectively described by examining the stress relaxation behavior over time, as shown in Fig.

6.3. The peak stress drops rapidly within the initial few seconds. However, a very low percentage

of the total stress relaxation occurs during the rest of the holding period. During the strain-

holding phase, the stress decreases while the total strain amplitude remains constant. This is due

to convertingthe conversion of elastic strain into inelastic strain, which leads to creep damage
(Zrnk et al. 2001)
. The interaction between cyclic and creep strainsstrain and creep strain

contributed to the shortened life observed in the CFI tests.

The C-M and cyclic stress amplitude vsvs. plastic strain amplitude plots of SU-263 alloy exhibit

a linear behavior at all the testing temperatures and holding times. This indicates that the cyclic

deformation mechanisms are similarthe same across the strain amplitudes. As the temperature

increases, the slope of the C-M plot increases and the slope of the cyclic stress amplitude vs.
plastic strain amplitude decreases; it is shown that temperature has a significant effect on C-F

properties, as shown in Figs. 6.6 and 6.7.

Table. 6.3 illustrates that as the temperature increases from 1073 K to 1123 K, the cyclic strength

coefficient increases; if the temperature increases to 1173 K, the cyclic strength coefficient

decreases. It shows that the resistance to fatigue deformation is higher at 1123 K. Additionally,

as the temperature increases, the fatigue ductility coefficient increases, while the cyclic strain

hardening exponent decreases. This indicates that the alloy's ability to undergo plastic

deformation improves with temperature, while its tendency to undergo cyclic hardening

decreases. As a function of holding time, the cyclic strain hardening exponent ( n' ) and cyclic

strength coefficient ( K ' ) decrease, while the fatigue ductility exponent ( c ¿ increases. However,

the fatigue ductility coefficient (ε 'f ) shows a temperature-dependent trend. It decreases at 1023 K

and 1073 K but conversely increases at 1123 K and 1173 K. Since the LCF tests were conducted

at the solubility limit, the precipitates weakened, resulting in the alloy exhibiting more ductile
(Anon 2004; Zhao et al. 2001)
behavior at 1123 K and 1173 K .

1.7 EFFECT OF HOLDING TIME AND TEMPERATURE ON CYCLIC STRESS

RESPONSE AND DEFORMATION MECHANISMS

Hysteresis loops typically reveal insights into cyclic hardening or softening behavior during each

cycle. The hysteresis loops exhibit various types of serration in the plastic portion of the

hysteresis loops, which is a manifestation of Dynamic strain aging (DSA). DSA is a high-

temperature deformation mechanism commonly observed in nickel-based superalloys

(Jadav et al. 2019; Shankar and Kumar 2022)
. The DSA effect is characterized by serrations, which show

up in the plastic region of the hysteresis loop during cyclic deformation owing to the interaction
between moving dislocation and the diffusing solute atoms (Prasad Reddy et al. 2014a) . In

nickel-based superalloys, interstitial atoms (C and N) at intermediate temperatures and

substitutional solute atoms (Cr and Mo) at higher temperatures are usually responsible for jerky
(Hörnqvist et al. 2014; Rao et al. 2019)
flow or serrations in the stress-strain curves . In SU-263

alloy, type C serrations were observed at one MTH with all temperatures (Fig.6.1). Type B

serrations were at 1023 K at five MTH, and type B+C serrations were at five MTH with

temperatures of 1073 K, 1123 K, and 1173 K (Fig.6.2). Type C serrations could be associated

with a reduction in yield strength occurring below the typical level of the flow curve, attributing

their occurrence to dislocation locking and unlocking, type A serrations represent repeated

deformation bands originating from one end of the specimen and extending uniformly along the

gauge length in the same direction (Portevin-Le-Chatelier effect), while type B serrations result
(Li et al. 2022; Rodriguez 1984)
from slip bands propagation from different directions .

The CSR curves of the SU-263 alloy show initial hardening followed by stable response at low

strain amplitude and peak hardening until failure at high strain amplitude of the alloy tested at

1023 K with both holding times (Figs. 6.4 and 6.5). However, as the temperature increased,

hardening behavior slowly reduced and almost reached equal stress amplitude at 1173 K with all

the strain amplitude. These variations in CSR curves result from microstructural changes that
(Valsan et al. 1994)
occur during cyclic loading . The cyclic hardening or softening behavior is

predominantly influenced by changes in dislocation distribution, precipitate morphology, and

dislocation-precipitate interactions, which are significantly affected by temperature and time,

leading to notable differences in stress response

(Valsan et al. 1994; Wang et al. 2023b; Ye et al. 2004; Zhang et al. 2019)
. The TEM studies of CFI specimens revealed the planar slip bands

oriented in more than one direction at all conditions (Figs. 6.8 and 6.9). This observation
indicates the multiple slip system is activated at all conditions. However, the slip bands are

arranged more closely with increasing hold time temperatures, as depicted in Figs. 6.8 and 6.9.

Fig. 6.10 shows that the dislocation density is higher at 1023 K thancompared to other

conditions. As the temperature and hold time increase, the number of dislocations decreases, as

shown in Figs. 6.10 and 6.11. This indicates that higher temperatures and longer hold times

accelerate the recovery process (dislocation annihilation), reducingleading to a reduction in

cyclic hardening with increasing temperature. Wang et al. conducted an interrupted fatigue study

in the IN750H alloy. They reported and reported that, during the initial stage of cyclic

deformation, dislocation density increases, and with further deformation, the precipitates act as
(Wang et al. 2021)
obstacles for dislocation movement, which leads to initial hardening . As

stress reaches a certain threshold, dislocations bypass or cut through obstacles. Additionally,

dislocations move and eventually annihilate. The softening rate increases whenWhen the

dislocation annihilation rate surpasses the dislocation formation rate, the softening rate increases.

Consequently, dislocation density decreases as the number of cycles increases

(Wang et al. 2021)
. Fig. 6.11 illustrates the effect of temperature on precipitate size. At 1023 K, there is no

change in precipitate size. However, at 1073 K with one MTH, the precipitate size increased to

35 nm, and at 1173 K with one MTH, the γ′ precipitate size grew to 51 nm, which is double the

initial size, as shown in Figs. 6.10 and 6.11. This indicates that as the temperature increased, the

size of the γ′ precipitates increased, while the overall volume fraction decreased due to the
(Anon 2004; Zhao et al. 2001)
testing temperature approaching the solubility limit .

Consequently, the precipitate-dislocation looping increased with temperature and holding time.

Previous researchers have reported that dislocation annihilation and dissolution or precipitate
(Dinesh et al. 2025; Zhang et al. 2019)
coarsening are responsible for cyclic softening . The
specimens tested at 1123 K with five MTH displayed few nano twins, as shown in Fig. 6.12.

TheIn nickel-based superalloys, the twins will be created in nickel-based superalloys when
(Murr et al. 1995)
dislocations are hindered in the glide plane . These nano twins act as barriers to

further dislocation motion. This could be whythe reason for the specimen tested at 1123 K

exhibitedexhibiting reasonably high stresshigh stress amplitude with high numbers of cycles.

However, the alloy tested at 1173 K exhibited more number cycles, but the half-life stress

amplitude decreased drastically. Chromium began to segregate within the matrix in specimens C-

F tested at above 1023 K (Figs. 6.13-6.19). The extent of segregation increased with increasing

temperatures and prolonged holding times. Additionally, the morphology of the chromium

segregation evolved from a needle-like shape to an irregular cubic form, eventually forming

M23C6 carbides within the matrix. However, no chromium segregation was detected in the alloy

tested at 1023 K with one and five MTH where there is no change in γ′ precipitates. The

redistribution of elements near the interface between the precipitate and the matrix during the γ′

coarsening process can result in the segregation of chromium.

1.8 EFFECT OF HOLDING TIME AND TEMPERATURE ON FRACTURE

BEHAVIOUR

The fractography studies of C-F tested specimens exhibited that, generally, the crack initiated

from the surface of the specimens and the crack growth exhibited mixed mode of failure, with a

predominance of either transgranular or intergranular fracture, depending on the holding time

and testing temperature. The alloy tested at 1023 K and 1073 K with one- and five-minute tensile

hold exhibited a mixed failure modemode of failure, predominantly intergranular across all strain

amplitudes (Figs. 6.20-6.23). As the strain amplitude increased, the number of grain boundary

decohesions, cleavage facets, and secondary cracks also increased. The intergranular fracture is
due to the nucleation and growth of grain boundary cavities (dimples), which develop and
(Goyal et al. 2018)
connect to form cracks that ultimately lead to fracture . The C-F tested above

1073 K predominantly displayed transgranular fracture characterized by dimples, ridges, fatigue

striations, and quasi-cleavage facets. This is due to the weakening of the γ′ phase at approaching

solubility temperature, which increasesleads to an increase in ductile behavior. The specimens

tested at five MTHsMTH exhibit more number of ridges or crack initiation sites than

thosecompared to the specimens tested at one MTH (Figs. 6.22 and6.22and 6.23). The previous

researchers also observed the same behavior and reported that more crack initiation sites were
(Ding et al. 2018; Shi et al. 2013)
exhibited due to the high inelastic strain . The specimen tested

at five MTH exhibited more ductile behavior than one MTH due to a higher recovery rate

(dislocation annihilation). However, the number of cycles to failure at five MTH is less than one

MTH due to the combined effects of creep and oxidation.

1.9 SUMMARY

a) The SU-263 alloy exhibited higher creep-fatigue life at 1123 K and 1173 K compared to

1023 and 1073 K.

b) The interplay between the precipitation of fine carbides within the grains and this

selective dissolution of γ′ precipitates is primarily responsible for the cyclic stress

responses at each corresponding temperature and can be summarized as:

[i.] 1023 K (below ageing temperature)- No carbide formation; no precipitate dissolution;

depicted peak hardening due toon account of precipitate dislocation interactions.

i.[ii.] 1073 (ageing temperature)- Cr and Mo segregation initiation; particle coarsening

resulting in shearing+ looping and drop in peak stress observed.

[iii.] At 1123 K and 1173K (above aging temperature), Fine metallic carbide precipitation

(Cr, Mo, Ti) dispersed within the grains, undergoing precipitate dissolution and a

significant drop in dislocation density (dislocation annihilation), resulting in a

declinedrop in peak stress and delayed the strain accumulation for failure. This

improved the fatigue life and resulted in transgranular failure, usually associated

with a ductile response in contrast to intergranular failure.

[iv.] The failure modemode of failure changed from intergranular to transgranular with

temperature and holding time.