Simulated Stress-Induced Sensitization Study

for the Heat-Affected Zone of the 304LN Stainless

Steel Weld Using a Thermomechanical Simulator
NIKKI ARCHANA BARLA, PRAKRITI KUMAR GHOSH, SOURAV DAS,
and VINOD KUMAR

Stress-induced sensitization in the heat-affected zone (HAZ) of the 304LN austenitic stainless
steel weld at 923 K (650 C) was evaluated using a thermomechanical simulator (Gleeble 3800)
at different stress levels. The simulated sensitization behavior of the HAZ was studied in close
approximation of the stress and weld thermal cycle that is generally observed during pulse
current gas metal arc welding of the 25-mm-thick section of the 304LN steel. The response to the
degree of sensitization, as a function of the type and magnitude of stresses present in the matrix,
was established through observations on changes in microstructure, electrochemical properties
and hardness measurements. Transmission electron microscopy and selected area diffraction
confirm that sensitization occurred and Cr23C6 precipitates formed at grain boundaries. The
results indicate that the presence of tensile or compressive stresses, especially above the yield
stress of the steel, enhances sensitization.

https://doi.org/10.1007/s11661-018-5082-5
 The Minerals, Metals & Materials Society and ASM International 2019

I. INTRODUCTION transportation and storage of various kinds of materials

AUSTENITIC stainless steel (ASS) has a wide range
of applications in several industrial sectors, including
paper and pulp, chemical, petrochemical and nuclear
industries, where corrosion and safety play an important
role in influencing the performance of a component. In
ASS, precipitation of chromium-rich carbide and nitride
takes place at grain boundaries, when they are held at
the temperature range of 773 K to 1073 K (500 C to
800 C). The formation of carbide, known as the
sensitization of stainless steel, results in depletion of
chromium in the matrix adjacent to the grain bound-
ary.[1] Such chromium-depleted locations possess rela-
tively less resistance to corrosion and subsequently,
become prone to intergranular corrosion (IGC) attack.
Thus, the change in microstructure of the matrix that
occurs with sensitization adversely affects the corrosion
resistance and mechanical properties of ASS.[2] This is
widely recognized as a potential cause for failure in
stainless steel pipes and containers used for
NIKKI ARCHANA BARLA, PRAKRITI KUMAR GHOSH,
and SOURAV DAS are with the Department of Metallurgical and
Materials Engineering, Indian Institute of Technology Roorkee,
Roorkee 247667, India. Contact e-mail: prakgfmtiitr@gmail.com
VINOD KUMAR is with the R & D Centre for Iron & Steel, Steel
Authority of India Ltd., Ranchi 834002, India.
Manuscript submitted March 31, 2018.
in chemical, petrochemical and nuclear plants.[3] It was
further reported that the corrosion susceptibility of ASS
at a given corrosive medium is primarily influenced by
the presence of a favorable extent of (a) carbide
former,[4] (b) grain size,[5] and (c) prior deformation[6–8]
in the matrix. Introducing a stress prior to sensitization
reduces the temperature for carbide nucleation and
accelerates its precipitation at a normal sensitization
temperature compared to that observed in practically
stress-free ASS.[9] A prior deformation introduces dis-
locations adjacent to grain boundaries. The increased
dislocation density near grain boundaries facilitates
easier chromium carbide precipitation by enhancing
the diffusivity of chromium in the matrix that may also
result in IGC.[10] Carbide nucleation at the grain
boundary is favored if prior deformation is low, but
nucleation starts in the grain interior as well when the
prior deformation is high.[11] The kinetics of sensitiza-
tion in stainless steel is also accelerated by the presence
of residual stresses[12–14] in the matrix.
In the case of welding of 304 type ASS, chromium
carbide nucleates significantly in certain locations of the
weld heat-affected zone (HAZ) due to sensitization.
Once chromium carbide is nucleated, it can grow even at
relatively lower temperatures in the range of 573 K to
823 K (300 C to 550 C). Such sensitization of ASS can
readily occur during welding and subsequently proceed
at suitable service temperatures.[15] After a long service
period of about 10 to 15 years at an operating

METALLURGICAL AND MATERIALS TRANSACTIONS A

temperature as low as 573 K (300 C), the extent of
sensitization was found to increase, which causes crack-
ing due to intergranular stress corrosion (IGSC).[16]
However, the observations on corrosion-related cracking
in stainless steel pipe at a nuclear plant suggest that
seeding of sensitization may occur even at room temper-
ature.[17] Thus, the phenomenon of sensitization can
subsequently proceed by the growth of chromium
carbide nuclei at a temperature well below the normal
sensitization temperature range. Such carbide nuclei
develop under a combined effect of stress and temper-
ature in the material. This phenomenon has been referred
to as low-temperature sensitization (LTS).[17,18] Hence
there is a need for reliable prediction of time for the onset
of sensitization at low temperature.
Formation of chromium carbide nuclei and their
growth is a function of time, temperature, and stress
present in the matrix of ASS. During welding, the
temperature goes to a much higher range than the
corresponding melting temperature of the metal. Con-
sequently, the metal starts to solidify with a high cooling
rate. Hence, a significant amount of thermal stress is
developed depending upon the hot mass involved and
the difference in the coefficient of thermal expansion
between the weld and the base metal.[19–21] Due to their
differential contraction behaviors in arc welding, a
considerable amount of stresses of both tensile and
compressive nature are generated in the HAZ adjacent
to the fusion line (FL) of the arc weld deposit. The
nature of stress changes from tensile to compressive if
one moves away from the base metal within the HAZ.[22]
The presence of such stresses of different magnitude and
nature in different locations of the HAZ having varied
thermal cycle (as a function of heating rate, cooling rate,
and peak temperature) may differently influence the
phase transformation and sensitization.[19]
Sensitization of ASS as a function of time and
temperature under the stresses present in the matrix
has been extensively studied to understand the response
of different fabricated components in industrial appli-
cations. However, hardly any study has been reported so
far to understand the stress-induced phase transforma-
tion, which may be defined as the simultaneous occur-
rence of sensitization and stress development in the
matrix of ASS. This is what happens in HAZ during arc
welding of stainless steel, which influences the nucle-
ation of chromium carbide in a different manner from
the studies available in the field of sensitization due to
prior stress introduced in the matrix. It was noticed in
an earlier report, but the fact of variation in degree of
sensitization (DOS) could not be established.[23]
Thus, to understand the characteristic response of an
arc-welded ASS component to LTS under various
service conditions, it is imperative to study in detail
the phenomena of stress-induced phase transformation
Table I. Chemical Composition (Weight Percent) of 304LN ASS
C Cr Ni Mn Si
0.02 18.39 9.03 1.76 0.05
in HAZ of arc-welded stainless steel. In order to reduce
the DOS, often it is preferred to use the stainless steel
containing low carbon and nitrogen (LN) grade.[24,25]
The presence of nitrogen acts as a strong austenite
stabilizer in stainless steel. This situation provides the
matrix a higher capacity of holding carbon, and any
precipitation of carbon in the form of carbides is delayed.
Thus, significant retardation of the sensitization due to
precipitation of chromium carbide occurs in the nitro-
gen-containing stainless steel. However, in spite of all
such precautions, this type of stainless steel is also found
to be appreciably responsive to sensitization, which may
be more vulnerable under the severity of the weld thermal
cycle of arc welding.[26] During heat treatment and
welding operations, elements, such as Si, Mn, S, and P,
segregate at the grain boundaries of stainless steel. It has
been postulated that this type of segregation may result in
the formation of weak passive films at the grain bound-
aries, which can then rapidly dissolve, resulting in IGC.[27]
In view of the preceding findings, an investigation was
planned to study the stress-induced sensitization with
respect to the precipitation of Cr23C6 in the HAZ of a
pulse current gas metal arc weld of 25-mm-thickness
304LN ASS plate with the help of the thermomechanical
simulation (TMS) process. The profile of the thermal
cycle in different locations of the HAZ, recorded during
welding by employing a strain buster (i.e., a temperature
measuring module), was used as input data to operate a
thermomechanical simulator for the desired studies. The
DOS of the matrix under different combinations of type
and magnitude of stresses was studied by measuring
the change in its electrochemical behavior using the
double-loop-electrochemical potentiokinetic reactiva-
tion (DL-EPR) test. The characteristics of the precipi-
tates formed due to the sensitization were studied by
selected area diffraction (SAD) via transmission electron
microscopy (TEM). A microhardness test was carried
out to characterize the response of the matrix to the
precipitation process in order to correlate the changes in
its electrochemical property.
II. EXPERIMENTAL
A. Material and Processing
The material used in this work was ASS AISI 304LN,
having a chemical composition as given in Table I. The
composition of this steel was confirmed by spark
emission optical spectroscopy. The material was
received in pipe form having 300-mm inner diameter
and 25-mm wall thickness. Pulse current gas metal arc
welding (P-GMAW) was performed using pieces with
dimensions 250 9 100 9 25 mm prepared from the
pipe, when the metal was laid along the length direction.
Cu P S Mo N
0.32 0.024 0.003 0.26 0.16
METALLURGICAL AND MATERIALS TRANSACTIONS A
Conventional V-groove was prepared as per ASME
Section IX of the Boiler and Pressure Vessel Code
(Figure 1) for such plate thickness. Welding was carried
out by a multipass multiseam [denoted as (a) through
(d)] per layer deposition procedure in conventional
V-groove (Figure 2). Welding was carried out in
99.98 pct pure argon gas shielding at a flow rate of
18 L/min. The welding parameters used in P-GMAW
are given in Table II. The temperatures of different
locations of the HAZ were recorded by the suitable use
of an R-type thermocouple (platinum-13 pct rhodium)
of wire diameter 0.25 mm during the filling passes
(denoted as 1 through 9) of weld deposition. The
placement of two thermocouples (TC1 and TC2) from
Fig. 1—Schematic diagram of conventional V-groove (in mm).
Fig. 2—Schematic diagram showing the location thermocouples
placed in the HAZ of conventional V-groove weld.
Table II. Welding Parameters Used During Weld Deposition
Welding Arc Voltage Heat Input (kJ/ Welding Speed (cm/ Mean Current
Process (V) cm) min) (A)
P-GMAW 28 ± 1 13.4 ± 0.5 19.3
Table III. Locations of Thermocouples on Plate
Thermocouple Distance from FL (mm)
TC1 2 2
TC2 3 4
METALLURGICAL AND MATERIALS TRANSACTIONS A
the bottom of the plate is shown in Figure 2 and
Table III. The thermocouples were connected to a
computer through two channels of a strain buster to
record the output. The strain buster was competent to
measure the output of the thermocouples at an interval
of 10 milliseconds from both of its channels. The
thermocouple output obtained in volts was converted
to temperature and was used to plot the thermal cycle of
any location of the HAZ.
The nature of sensitization occurring in the HAZ
during P-GMAW of this pipe was studied in a Gleeble
3800 using the experimental data of the thermal cycle,
which were obtained during weld deposition.
For the HAZ simulation study in the Gleeble 3800,
a specimen of dimensions 10 9 10 9 110 mm was
machined out from the stainless steel pipe. Two types
of specimens were prepared: one with thread for
applying tensile stress (+) (Figure 3(a)) and the other
without thread for applying compressive stress ()
(Figure 3(b)). The specimens were heated to a peak
temperature of 923 K (650 C) with a heating rate of
150 C/s in the Gleeble 3800. A HAZ simulation test
was done under both tensile and compressive stresses of
50 to 200 MPa with an interval of 50 MPa, including
0 MPa stress as well. Table IV shows the designation of
the test specimens undergoing different test conditions.
In all the tests, the peak temperature, heating rate, and
cooling rate were kept constant as 923 K, 150, and 5 C/
s, respectively. With the help of thermal cycle data, the
heating rate to reach the peak temperature of 923 K and
the rate of cooling of the matrix to 773 K have been
estimated. The heating and cooling rates were used as
input to the Gleeble 3800 for the HAZ simulation test
under different stresses. The cooling rate was defined by
t8 to 5, which is the cooling time from 1073 K to 773 K
(800 C to 500 C). The peak temperature of 923 K
(650 C) was selected because it is known as the most
active temperature within the sensitization temperature
range of ASS.[28–30] The K-type thermocouple (chrome-
l-alumel) of wire diameter 0.2 mm was welded at the
midsection of the specimen for temperature measure-
ment, prior to performing the HAZ simulation test.
During the test, a built-in Gleeble 3800 hydraulic system
enabled maintenance of the desired compressive or
Pulse Parameter
Ip Ib F Tb Tp
F (A) (A) (Hz) (s) (s)
220 ± 3 0.15 332 125 107 3.97 3.66
Depth from the Bottom of the Plate (mm)
Fig. 3—Schematic diagrams of two types of test specimens used in the TMS Gleeble 3800 under different stress conditions: (a) tensile and (b)
compressive.
Table IV. Designation of the Specimens Used in the TMS
Gleeble 3800 for HAZ Simulation Tests at the Peak
Temperature of 923 K Under Varying Stresses
Specimen Designation Stress (MPa)
A 0 (no stress)
B1 + 50 (tensile)
B2 + 100 (tensile)
B3 + 150 (tensile)
B4 + 200 (tensile)
C1  50 (compressive)
C2  100 (compressive)
C3  150 (compressive)
C4  200 (compressive)
tensional stresses during heating and cooling. A precise
load cell measured the force and provided instant
feedback to the control system. A Rykalin three-dimen-
sional heat transfer model was used in the simulator that
functions according to Eq. [1]:
 
E r2
T  T0 ¼ exp  ; ½1
2pkðt  t0 Þ 4k=qcðt  t0 Þ
where T is the temperature of the thermal cycle at time t,
E is the energy input, k is the thermal conductivity, q is
the material specific weight, r is the density, t0 is the time
at the end of preheating, c is the specific heat capacity,
and T0 is the preheat temperature.
B. Evaluation of Sensitization
After the HAZ simulation test, the samples were
collected from the middle part of the test specimens
where the thermocouple was welded and sectioned
through its centerline, as shown in Figure 4.
For metallographic examination, the sections of the
samples were polished with alumina suspension to
0.024 lm surface finish followed by electroetching as
recommended by the ASTM A262 Practice A in 10 pct
oxalic acid for 3 minutes at 8 V using a direct current
(DC) supply arrangement. The microstructure was
studied under optical microscope and its features were
categorized by ‘‘step,’’ ‘‘dual,’’ and ‘‘ditch’’ structures
defined as a structure with no single grain completely
surrounded by carbide, at least one grain completely
surrounded by carbide from all sides, and many grains
completely surrounded by carbides from all sides,[31]
respectively, as listed in Table V. Average attacked grain
boundary width and average attacked grain boundary
Fig. 4—Location of the thermocouple welded at the centerline of the
sample.
area, from the electroetched microstructures of all the
specimens, were measured through ImageJ analysis
software using a 100 lm scale.
Estimation of the response to sensitization of the
specimens treated at different stress levels (Table IV)
was carried out on a 78.5 mm2 exposed area using a
DL-EPR test. In this test, the specimens were polarized
anodically from open circuit potential (OCP) up to
0.7 V overvoltage at a constant scan rate. The test
provides means to numerically assess the DOS that
assists the IGC and IGSC behaviors. The tests were
performed in 0.5 N H2SO4 + 0.01 M KSCN solution at
30 ± 1 C. During the experiment, the potential was
changed from OCP to the reverse potential of 300 mV
and then came back to the initial potential with a scan
rate of 1.67 mV/s. The DL-EPR test gives DOS desig-
nated as R0 in Eq. [2]:
Ir
R0 ¼  100; ½2
Ia
where Ir is the peak current density in reverse scan and Ia
is the peak current density in forward scan. The critical
value for R0 is 1 pct. If R0 < 1 pct, the steel is not
considered as sensitized. If 1 pct < R0 < 5 pct, the steel
is considered partially sensitized, and if R0 > 5 pct, it is
assumed to be fully sensitized.[32] The DL-EPR test for
each sample was repeated three times.
C. TEM Analysis
HAZ-simulated specimens in Gleeble 3800 were
examined under TEM to study the nature of precipita-
tion of chromium carbide in the matrix. For TEM
examination, thin foils down to 40 lm were prepared,
followed by twin-jet polishing in ethanol and perchloric
acid (9:1) solution at 30 V, when the temperature was
maintained at  30 C to  35 C. The TEM studies
METALLURGICAL AND MATERIALS TRANSACTIONS A
 Table V. Types of Structures Obtained in 304LN Stainless Steel After ASTM A262 Practice A Test
Structure
Step
Dual
Ditch
Fig. 5—Typical thermal cycle of different locations of the HAZ
during multipass bead deposition in weld groove.
were carried out using a high-resolution TEM (model
JEM 3200FS) operated at 300 kV. During TEM anal-
ysis, the phases present as precipitates in the matrix were
characterized by analyzing their SAD patterns.
D. Microhardness Test
After the HAZ simulation test, microhardness tests
using Vicker’s scale were performed on all the polished
and etched specimens in order to characterize their
sensitization. The tests were performed at 500 mg load
with 15 seconds of dwell time by at least 10 indentations
on each specimen, and the average of hardness mea-
surements was reported as a characteristic of the matrix.
III. RESULTS AND DISCUSSION
A. Thermal Characteristics of Weld Deposition
Weld thermal cycle governs the diffusion of carbon
and chromium to determine the extent of sensitization in
the matrix of the HAZ of a weld joint of ASS. The
typical thermal cycle at different locations of the HAZ,
obtained during bead deposition in nine passes for filling
of a weld groove (Figure 2) by P-GMAW employing
DC electrode positive, is shown in Figure 5. The
procedure of temperature measurement was discussed
in earlier section. The time–temperature–stress profile
obtained from HAZ simulation test in the Gleeble 3800
at different stress levels is shown in Figure 6.
METALLURGICAL AND MATERIALS TRANSACTIONS A
Explanation
no single grain is completely surrounded by carbide
at least one grain is completely surrounded by carbide from all
sides
many grains are completely surrounded by carbide from all sides
Fig. 6—Time–temperature–stress profile obtained from the thermo-
mechanical simulator.
B. Characteristics of Microstructure
The microstructure of the as-received 304LN ASS is
shown in Figure 7. The figure shows the typical presence
of the twin structure in the austenite grains of the
matrix. The grain boundary is revealed to be quite thin
under the optical microscope after metallographic etch-
ing. Here, it is necessary to note this feature because it
will be referenced to compare the widening of the grain
boundary due to sensitization of the matrix.
Optical microscopic analysis of the specimens having
no stress (A), low tensile stress of + 50 MPa (B1), and
stress of + 100 MPa (B2), as can be seen in Table IV,
show relatively fewer locations of IGC attack
(Figures 8(a) through (c)) after electroetching. These
locations mostly reveal the presence of step structure
(refer to Table V), where the chromium-depleted regions
appear to be appreciably low. However, at a relatively
higher tensile stress of + 150 MPa, the B3 specimen
reveals dual microstructure (Figure 8(d)) resulting from
moderate IGC, whereas specimen B4, at an even higher
tensile stress of + 200 MPa, shows the presence of ditch
structure (refer to Table IV for details) (Figure 8(e))
arising out of maximum IGC attack among the speci-
mens tested under tensile stress. Specimen C1, under
relatively low compressive stress (refer to Table IV), also
shows almost step microstructure with negligible grain
boundary attack (Figure 8(f)), whereas C2 specimen, at
relatively higher compressive stress of – 100 MPa,
clearly shows a few locations of dual microstructure
with moderate IGC (Figure 8(g)) in the matrix. How-
ever, specimens C3 and C4 with further higher com-
pressive stresses of  150 and – 200 MPa, respectively,
show ditch microstructures with appreciably greater
IGC in the matrix, as revealed in the microstructures
presented in Figures 8(h) and (i), respectively.
As a signature of varying response to sensitization,
the average attacked grain boundary width and the
average attacked grain boundary area due to IGC in the
chromium-depleted zone adjacent to it under different
types and levels of stresses have been measured, as
Fig. 7—Microstructure observed after ASTM A262 Practice A test
on the as-received sample.
shown in Figures 9 and 10, respectively. The measure-
ments were carried out using the ImageJ analysis
software on the microstructures obtained after the
specimens were electroetched by the ASTM A262
Practice A. Figure 9 shows the change in the width of
grain boundary due to IGC under no stress (specimen
A), different magnitudes of tensile stress (specimens B1
through B4), and compressive stress (specimens C1
through C4) in the matrix. In Figure 9, specimen A
shows minimum grain boundary attack with its width
about 1 ± 0.4 m. An increase of stress to + 100,
+ 150, and + 200 MPa steadily enhances the width
of the grain boundary due to corrosion, as revealed in
specimens B2, B3, and B4, respectively. A similar trend
can also be observed for compressive samples. With an
increasing amount of compressive stress, the width of
the grain boundary steadily increases and reaches a
maximum of – 200 MPa stress level.
Similarly, Figure 10 shows the average attacked grain
boundary area in the specimens under no stress (spec-
imen A), different magnitudes of tensile stress (speci-
mens B1 through B4), and compressive stress (specimens
C1 through C4) in the matrix. In Figure 10, specimen A
shows a minimum grain boundary attack area with
about 23.57 ± 1 lm. With the increase in magnitude of
both tensile and compressive stress, the specimens
manifest the enhancement in the attacked grain bound-
ary area.

Fig. 8—Microstructure observed after ASTM A262 Practice A test on specimens (Table IV) under different stresses: (a) A—showing step
structure; (b) B1—showing step structure; (c) B2—showing dual type structure; (d) B3—showing dual microstructure, with moderate grain
boundary attacks; (e) B4—showing ditch microstructure; (f) C1—showing almost step microstructure, with negligible grain boundary attacks; (g)
C2—showing few dual microstructures; (h) C3—ditch microstructure; and (i) C4—ditch microstructure.

METALLURGICAL AND MATERIALS TRANSACTIONS A


Fig. 9—Average attacked grain boundary width in specimens under
no applied stress and different magnitudes of tensile and compressive
stresses.
Fig. 10—Average attacked grain boundary area in specimens under
no applied stress and different magnitudes of tensile and compressive
stresses.
C. Electrochemical Characteristics
The sensitivity of matrix to corrosion attack, based on
its DOS as a function of type and magnitude of stresses
present in it, is further confirmed by the DL-EPR test.
The observations shown in Figure 11 reveal the extent
of sensitization through precipitation of chromium
carbide adjacent to the grain boundary. Under the
stresses of different types and magnitude, the chemical
characteristics of the matrix to passivation and repas-
sivation responding to IGC as a function of its poten-
tial–current density relationship are shown in this figure.
Figure 11(a) shows the DL-EPR curve for the specimen
with no stress and the specimens with tensile stresses of
different magnitude. In this figure, the specimen with no
stress shows the lowest peak reactivation current density
and the specimens with different magnitudes of tensile
stress show the increase in peak reactivation current
density as stress increases. Similarly, a significant change
METALLURGICAL AND MATERIALS TRANSACTIONS A
is observed in the peak current density during the
reverse scan in higher compressive stress specimens in
Figure 11(b). The peak reactivation current density
is increased with increasing compressive stress.
Figures 11(a) and (b) clearly reveal that the type and
magnitude of stresses distinctly influence the magnitude
and spread of the hysteresis loop of the potential–cur-
rent density curves, indicating variation in the response
of the matrix to IGC. These figures exhibit the occur-
rence of a relatively higher extent of pitting and IGC
attributed to larger hysteresis during the measurements
with considerably lower repassivation potentials, espe-
cially in case of specimens B3, B4, C3, and C4 having
relatively higher stresses in the range of 150 to 200 MPa.
Figure 12 shows the variation of R0 as a measure of
DOS (Eq. [2]) with the change in type and magnitude of
stresses present in the matrix of different specimens, as
designated in Table IV. This figure reveals that, per
general norms of considering R0 to realize the sensitivity
of the matrix to partial or full sensitization, as described
in Section II–B, specimens A, B1, B2, B3, C1, and C2
(refer to Table IV) show the value of R0< 5 depicting
their sensitivity to partial sensitization. The figure further
reveals that specimens B4, C3, and C4 (refer to Table IV)
have a clear response to full sensitization, with the value
of R0 lying in the range of 6.37 to 8.29. Although sample
B3 shows partial sensitization, the value of R0 is close
(4.79) to that for full sensitization (5). All these results
practically corroborate the observations discussed pre-
viously relevant to the effect of type and magnitude of
stresses affecting the DOS of the matrix at the given
nitrogen content of the 304LN stainless steel. However,
in this context, the role of nitrogen content on DOS
under stress-induced transformation of chromium car-
bide precipitation in the matrix requires further study to
acquire better competence of handling LN grade ASS in
a fabrication process such as welding.
The preceding observations clearly indicate that the
presence of stress in the matrix of 304LN ASS signif-
icantly affects its sensitization behavior and the severity
of attack is intensified with the increase of magnitude of
the stresses. It is noted that a given level of compressive
stress makes the matrix almost similar or relatively more
prone to IGC attack, as it occurs in the presence of a
similar level of tensile stress due to its high sensitivity to
sensitization. However, it appears that the presence of
stress about ± 150 MPa makes the matrix relatively
more prone to sensitization. These findings are signif-
icantly relevant to characterize the HAZ of the arc weld
of this steel, where the matrix remains under an
appreciable amount of residual stress that is developed
during cooling of the molten weld pool. Here, the
sensitization may occur in the HAZ simultaneously
during development of the stresses. At this juncture, it
may be noted that the compressive or tensile is a concept
of direction. Further, in the microlevel, the matrix of the
planer component of any type of stress is susceptible to
sensitization by carbide precipitation due to its relatively
higher free energy.[33–35] Hence, the knowledge gathered
from these studies manifests the critical requirement of
the control of residual stresses in the arc weld of this
steel, primarily from the point of view of its magnitude
Fig. 11—DL-EPR curves for the specimens (a) under no applied stress and different magnitudes of tensile stress and (b) under different
magnitudes of compressive stress.
Fig. 12—DOS of specimens under no applied stress and different
magnitudes of tensile and compressive stresses.
and distribution with reference to its direction in the
matrix of the HAZ. For more precise control of
stress-induced sensitization, the mechanism of carbon
diffusion leading to the formation of chromium carbide
precipitates in the matrix, which is simultaneously
generating tensile or compressive stress, must be thor-
oughly understood. However, this is beyond the scope
of the current study.
D. TEM Analysis
Sensitization of the matrix is ultimately confirmed by
the detection of carbide precipitation through TEM
studies carried out on all the tensile and compressive
stress-induced specimens simulated in the HAZ test in
the Gleeble 3800. Dark-field TEM images clearly reveal
Fig. 13—TEM micrograph showing chromium carbide precipitates
on the grain boundary.
the formation of carbide precipitates within dislocation
networks at the grain boundary, as shown in Figures 13
and 14(a). The precipitates are found to be present in
both the irregular and well-defined geometric shapes, as
shown in Figures 13, 14(a), and 15(a). The SAD
patterns of the precipitates shown in Figures 14(b) and
15(b), along with spot indexing of the SAD patterns
presented in Figures 14(c) and 15(c), confirm the pre-
cipitates as chromium carbide Cr23C6 having fcc struc-
ture. It is also noted that the observed chromium
carbide has a coplanar relationship with the austenite
matrix. From the SAD pattern, the orientation rela-
tionship between the austenite and Cr23C6 carbide is
determined as ½110Cr23 C6 ==½111c : The TEM images
confirm that the carbide formation is favored by the
grain boundary as well as by the dislocation present
along with it.
METALLURGICAL AND MATERIALS TRANSACTIONS A
Fig. 14—TEM micrographs showing (a) chromium carbide precipitate on the grain boundary surrounded by dislocation tangles, (b) SAD
pattern of the precipitate, and (c) spot indexing of the SAD pattern.

Fig. 15—TEM micrographs showing (a) chromium carbide precipitate, (b) SAD pattern of the precipitate, and (c) spot indexing of the SAD
pattern.

METALLURGICAL AND MATERIALS TRANSACTIONS A


Fig. 16—Matrix hardness of the specimens under no applied stress,
tensile stresses, and compressive stresses of different magnitudes.
E. Hardness
It is generally known that the hardness of the matrix
increases with the enhancement of sensitization of ASS.
In this case, the hardness of the specimen is observed to
increase with the increase of both the tensile and
compressive stress in the matrix, as shown in
Figure 16, which is predominantly attributed to the
relatively favored chromium carbide precipitation in the
matrix. Although it can be seen that, at a given stress,
especially in the range of 150 to 200 MPa, the hardness
of specimens C3 and C4 is relatively higher than that
observed in the corresponding specimens under tensile
stress (B3 and B4), it is emphasized here that the
difference in hardness from this limited set of experi-
mental observations between two comparable specimens
(B3 with C3 and B4 with C4) is too narrow to draw any
final conclusion. However, the observation is in agree-
ment with a work reported earlier.[32] It is, thus, no
wonder that specimen A with no applied stress shows
the lowest matrix hardness. The observed behavior of
the change in hardness as a function of stress-induced
chromium carbide precipitation under the tensile and
compressive stresses is much in line with the observation
on the DOS of the matrix.
IV. CONCLUSIONS
In the present study, stress-induced sensitization
behavior of 304LN was simulated for different levels
of tensile and compressive stresses (± 50 to 200 MPa) at
a temperature (650 C) that normally can be experi-
enced in the HAZ region. The study was conducted
primarily with the changes in microstructural features
and as a function of DOS responding to the electro-
chemical behavior of the matrix. The observations
provide some unique knowledge of the characteristics
of sensitization under simultaneous development of
tensile or compressive stresses (stress-induced transfor-
mation) at a given nitrogen content of a 304LN stainless
steel.
It was found that the presence of tensile stress gives
step and dual microstructure, whereas the presence of
compressive stress gives rise to dual and ditch
microstructure with appreciable average attacked grain
boundary width and average attacked grain boundary
area. On the contrary, the matrix, free from applied
stresses, shows step microstructure only.
However, the most important observation may be
that the DOS behavior responds similarly irrespective of
the orientation of stress. The sensitization was marked
by the formation of Cr23C6 precipitate at the grain
boundary, the enhancement of matrix hardness, and the
electrochemical behavior. Thus, it can be concluded
from the current set of results that a stress level above
the yield stress at the corresponding temperature may
lead to high DOS irrespective of the direction of stress,
as can be seen from the DOS results as well as the
microstructural changes. This understanding may be
useful to control the development of stress during arc
welding of 304LN stainless steel in order to produce a
more durable and safer weld joint in service.
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