metals

Article
Effect of Post Weld Heat Treatment on the
Microstructure and Mechanical Properties of a
Submerged-Arc-Welded 304 Stainless Steel
Tae-Hoon Nam 1,2 , Eunsol An 1 , Byung Jun Kim 1 , Sunmi Shin 1 , Won-Seok Ko 3 , Nokeun Park 4 ,
Namhyun Kang 2, * ID and Jong Bae Jeon 1, *
1 Functional components and Materials R&D Group, Korea Institute of Industrial Technology,
Yangsan 50635, Korea; skgnsl41@kitech.re.kr (T.-H.N.); sol@kitech.re.kr (E.A.); jun7741@kitech.re.kr (B.J.K.);
smshin@kitech.re.kr (S.S.)
2 School of Materials Science and Engineering, Pusan National University, Busan 46241, Korea
3 School of Materials Science and Engineering, University of Ulsan, Ulsan 44610, Korea; wonsko@ulsan.ac.kr
4 School of Materials Science and Engineering, Yeungnam University, Gyeongsan 38541, Korea;
nokeun_park@yu.ac.kr
* Correspondence: nhkang@pusan.ac.kr (N.K.); jbjeon@kitech.re.kr (J.B.J.); Tel.: +82-55-367-9407 (N.K.);
+82-51-510-3274 (J.B.J.)

Received: 8 November 2017; Accepted: 22 December 2017; Published: 2 January 2018

Abstract: The present study is to investigate the effect of post heat treatment on the microstructures
and mechanical properties of a submerged-arc-welded 304 stainless steel. The base material consisted
of austenite and long strips of delta-ferrite surrounded by Cr-carbide, and the welds consisted of delta
ferrite and austenite matrix. For the heat treatment at 850 ◦ C or lower, Cr-carbides were precipitated in
the weld metal resulting in the reduction of elongation. The strength, however, was slightly reduced
despite the presence of Cr-carbides and this could possibly be explained by the relaxation of internal
stress and the weakening of particle hardening. In the heat treatment at 1050 ◦ C, the dissolution
of Cr-carbide and disappearance of delta ferrite resulted in the lower yield strength and higher
elongation partially assisted from deformation-induced martensitic transformation. Consequently,
superior property in terms of fracture toughness was achieved by the heat treatment at 1050 ◦ C,
suggesting that the mechanical properties of the as-weld metal can be enhanced by controlling the
post weld heat treatment.

Keywords: austenitic 304 stainless steels; sub-merged arc welding; post-weld heat treatment

1. Introduction
Austenitic stainless steels are widely used in important parts of chemical plants such as
pressure vessels, chemical machineries, and pipes because they have excellent corrosion resistance,
acid resistance, formability, and weldability. They are also extensively applied in gas turbines,
jet propellants, and nuclear power plants because of their excellent toughness in high-temperature and
high-pressure environments [1–4].
Submerged Arc Welding (SAW) is widely used for joining ship structures and piping thick-wall
stainless steels [5,6]. In SAW, a solid filler wire is automatically inserted to pre-dispersed granular
flux and an arc generates between the base metal and the filler wire while being covered with flux.
The flux in contact with the arc melts and then the molten slag covers and protects the molten metal.
Generally high-efficiency welding is achieved by flowing a large current through a large-diameter wire.

Metals 2018, 8, 26; doi:10.3390/met8010026 www.mdpi.com/journal/metals

Metals 2018, 8, 26 2 of 13

Metals 2018, 8, 26 2 of 13
It has the advantage of improving welding productivity through high speed solidification during
welding
Dueandto improving
the heat input weldfrom
qualitythethrough welding heat
SAW welding control
process, [7].is a degradation problem of
there
Due to theand
microstructural heat input from
mechanical the SAW
properties suchwelding process, there
as inhomogeneity of theismicrostructure,
a degradationconcentration
problem of
microstructural
of residual stress,and mechanical
brittleness, andproperties suchofastoughness
deterioration inhomogeneity
in the of the microstructure,
welded concentration
material [8]. Post-weld heat
of residual stress, brittleness, and deterioration of toughness in the welded material
treatment (PWHT) is usually introduced to solve such degradation. However, if the delta ferrite [8]. Post-weld heat
in
treatment stainless
austenitic (PWHT)steel is usually introduced
is excessively to solve
present in thesuch
welddegradation.
metal duringHowever, if the delta
SAW welding, ferrite in
embrittlement
austenitic
of stainless
the welded steel occur
part may is excessively present in the weld
due to transformation metal during
into another brittle SAW
phasewelding,
such as aembrittlement
sigma phase
of the welded
during part
post heat may occur
treatment. Indue
orderto transformation into another
to solve these problems, it isbrittle phasetosuch
important as a sigma
investigate phase
post-heat
during post
treatment heat treatment.
process to control theIn order to solve
content these
of delta problems,
ferrite and theitharmful
is important to investigate
carbides [9]. Proper post-heat
treatment can
process to control
improve the contentproperties
the mechanical of delta ferrite and the harmful
by homogenizing the carbides [9]. Proper
microstructure of thepost-heat
welded
treatmentand
material cancontrolling
improve the themechanical
formation of properties
beneficialby homogenizing
and harmful phases the[10–13].
microstructure of the welded
material and controlling
Although extensive the formation
researches haveof conducted
beneficial and harmful
on the effectphases
of PWHT [10–13].
on the welded austenitic
Although extensive researches have conducted on the effect
stainless steels, industrial field still requires the comprehensive research on of PWHT on the
the resultant
welded austenitic
effect of
stainlessespecially
PWHT, steels, industrial
for thefield still requires
practical and the thecost
comprehensive research
effective process on the resultant
condition of PWHT. effect
Theofpresent
PWHT,
especially
study thusforinvestigated
the practicalthe andeffect
the cost
of effective
PWHT on process condition
the change of of PWHT. The present
microstructural study thus
and mechanical
investigated
properties of the
the effect
welded of part
PWHT on the
of AISI change
STS of microstructural
304 steel produced by SAW. and mechanical properties
The microstructural of the
changes
welded the
during partheat
of AISI STS 304
treatment steelanalyzed
were produced by the
and SAW. The microstructural
resultant changes properties
effect on mechanical during thewereheat
treatment
discussed. were analyzed and the resultant effect on mechanical properties were discussed.

2. Materials
2. Materials and
and Methods
Methods
In this
In this study,
study, submerged-arc
submerged-arc welding
welding was was performed
performed in in austenitic
austenitic stainless
stainless steel
steel STS304
STS304 using
using
STS308L as a welding electrode. The chemical compositions of the materials used are shownshown
STS308L as a welding electrode. The chemical compositions of the materials used are in
in Table
Table
1. 1. Awith
A plate plate with
the widththeof
width
100 mm,of 100
themm, theoflength
length 1000 mm of 1000
and themmthickness
and the thickness
of 25 mm wasof 25fabricated
mm was
fabricated by the SAW. In order to evaluate the microstructure and mechanical
by the SAW. In order to evaluate the microstructure and mechanical properties, PWHT was properties, PWHT was
performed from
from 650–1050
650–1050 °C ◦ C with
with anan interval
interval of
of 200
200 °C◦ C as
as shown
shown in in Figure
performed Figure 1a. After maintaining
1a. After maintaining at at
these temperatures for 0.5–4 h, the specimens were then quenched
these temperatures for 0.5–4 h, the specimens were then quenched in water. in water.
In order
In order to toobserve
observethethemicrostructure,
microstructure, thethe
testtest pieces
pieces were were grinded
grinded usingusing sandpapers
sandpapers and
and then
then micro-polished
were were micro-polished using ausing
diamond a diamond
suspensionsuspension
with a 1 μm with a 1 µmAccording
diameter. diameter. to According
ASTM E-340, to
ASTM E-340, the polished surface was etched using a mixed solution of distilled
the polished surface was etched using a mixed solution of distilled water, hydrochloric acid and nitricwater, hydrochloric
acid with
acid and nitric
a ratioacid withThrough
of 4:3:3. a ratio of the4:3:3. Through
optical the optical
microscopy, microscopy, the
the microstructures microstructures
of the base metal, theof
the base
weld partmetal,
and thethe heatweld part zone
affected and (HAZ)
the heat affected
were zoneAccording
analyzed. (HAZ) were analyzed.
to ASTM According
E-8, subsized to
plate-
ASTM E-8, subsized plate-type tensile specimens were taken from the middle
type tensile specimens were taken from the middle of the welded plate with perpendicular to the of the welded plate with
perpendicular
welding directionto the
as welding
shown indirection
Figure 1b. as shown in Figure 1b.

Figure 1. Schematic diagrams showing (a) post-weld heat treatment schedules and (b) ASTM-E8
Figure 1. Schematic diagrams showing (a) post-weld heat treatment schedules and (b) ASTM-E8
subsized tensile specimen.
subsized tensile specimen.

The tensile tests were conducted to measure yield strength, tensile strength and elongation with
the strain rate of 10−3/s according to ASTM A370 using universal tensile machine (MTS, Eden Praire,
MN, USA). The yield strength was determined by the 0.2% offset method and the elongation was
measured by the travel distance of crosshead. Vickers hardness test was conducted with the load of
Metals 2018, 8, 26 3 of 13

The tensile tests were conducted to measure yield strength, tensile strength and elongation with
the strain rate of 10−3 /s according to ASTM A370 using universal tensile machine (MTS, Eden Praire,
MN, USA). The yield strength was determined by the 0.2% offset method and the elongation was
measured by the travel distance of crosshead. Vickers hardness test was conducted with the load
of 2.94 N for 15 s dwell time and the hardness values were measured 10 times in total, and the
average value was calculated by excluding the maximum and the minimum value. To measure
the content of delta ferrite in the weld metal, the mean value was measured 10 times per
specimen using FERITSCOPE-FMP30 (Fischer, Windsor, CT, USA). Electron backscattered diffraction
(EBSD) and Electron Probe Microanalysis (EPMA) was performed to observe the phase change
after post heat treatment using JEOL FE-SEM 7200F (JEOL, Tokyo, Japan). For thermodynamic
calculations to predict the volume fraction of equilibrium phase at given temperatures, ThermoCalc
software (Thermo-Calc Software, 2017b, Solna, Sweden) package was adopted with the latest steel
database (TCFE9).

Table 1. Chemical composition of the base metal and the filler wire (wt %).

Alloys C Mn Si Cr Ni Mo Al Co Nb Cu N
STS 304 (Base) 0.046 1.19 0.42 18.2 8.02 0.15 0.003 0.164 0.01 0.23 0.05
STS 308L (Filler) 0.02 1.98 0.41 19.7 10.79 0.03 - - - 0.13 0.05

3. Results and Discussion

Figure 2 shows the microstructure of weld metal, heat-affected zone (HAZ) and base metal
after sub-merged arc welding (SAW). The base metal consisted of austenite single phase and
hot-rolling strips. These rolling strips correspond to delta ferrite surrounded by Cr-based carbides
precipitated during hot rolling (Figure 2d–f). The weld metal was composed of austenite (white) and
delta ferrite (black). The delta ferrite is classified into lathy and vermicular type by shape (white
circle and rectangle in Figure 2c, respectively), and this shape difference is considered to be caused
by welding heat input. In the sequential order of multi-pass SAW, the welded structure initially
appeared in a lathy shape, and then the lathy shape was transformed into a twisty vermicular shape
induced by the next welding pass. From the results of the Energy Dispersive Spectroscopy (EDS)
analysis, it was confirmed that the formation of the primary Cr-carbide did not occur in the weld metal.
Scanning electron microscope (SEM) analysis revealed that pores and cracks possibly formed during
solidification were hardly found in the weld metal. Therefore, it was confirmed that the welding
conditions such as welding power and electrodes were correctly selected.
The heat affected zone of the austenitic stainless steel is generally prone to be Cr-deficient
due to the precipitation of Cr-Fe rich carbides at phase boundaries or grain boundaries causing
brittleness and welding decay [14]. From the EPMA analysis in Figure 2d, there was no remarkable
increase of Cr-carbide in HAZ, compared to the base metal where Cr-carbides initially present
around long-elongated delta ferrite. Also the shape of Cr-carbides near HAZ still remained in a long
elongated shape, which means that those carbides were likely to be formed during hot-rolling process.
It is thus considered that the formation of Cr-carbide by welding heat effect hardly occurred in
the present specimen. Figure 3a,b show Vickers hardness measured over base metal, HAZ and
welding metal. The hardness value is considered not to vary significantly over those regions despite
that the hardness increased at the regions where austenite and carbides existing together. The hardness
of the base material and the HAZ were similar with each other and the hardness of the weld metal
was slightly lower than those of the base metal and the HAZ. The hardness results provide that
microstructural changes such as grain coarsening/refining or Cr-carbides precipitation barely occurs
in the HAZ. The as-welded specimens were always fractured in the middle of the weld metal, not in
the HAZ during tensile tests. This also indicates that there is almost no formation of brittle phases in
Metals 2018, 8, 26 4 of 13

the HAZ. Therefore, the analysis of microstructural changes and mechanical properties during post
weld Metals
heat 2018,
treatment
8, 26 is focused on the weld metal, not on the HAZ. 4 of 13
Metals 2018, 8, 26 4 of 13

FigureFigure 2. Opticalmicrographs
2. Optical micrographs of ofthe
theas-weld
as-weld specimen
specimen showing (a) the(a)
showing basethemetal,
base(b)metal,
the heat-
(b) the
affected zone,
Figurezone, and (c)
2. Optical the weld
micrographsmetal (White
of the(Whitearrows and
as-weldarrows triangles
specimen are indicating the pre-existing strips
heat-affected and (c) the weld metal andshowing
triangles (a)are
theindicating
base metal,the(b)pre-existing
the heat-
andaffected
delta ferrite,
zone, andrespectively.);
(c) the weld (d) Electron
metal (White Probe and
arrows Microanalysis
triangles are(EPMA)
indicating images
the showing the
pre-existing strips
strips and delta ferrite, respectively.); (d) Electron Probe Microanalysis (EPMA) images showing the
presence of Cr-carbides
and delta in the base metal;
ferrite, respectively.); (e) Electron
(d) Electron backscattered
Probe diffraction
Microanalysis (EPMA) (EBSD) phase
images map onthe
showing
presence of Cr-carbides in the base metal; (e) Electron backscattered diffraction (EBSD) phase map on
thepresence
fusion line
of Cr-carbides in the base metal; (e) Electron backscattered diffraction (EBSD) phase cyan
including base metal (right) and heat affected zone (HAZ) (left). Red, blue, and map on
the fusion
color
line including
indicate
base metal (right)
delta-ferrite,
and6heat affected zone (HAZ) (left). Red, blue, and cyan
the fusion line includingaustenite,
base metaland Cr23Cand
(right) , respectively.
heat affected zone (HAZ) (left). Red, blue, and cyan
color indicate delta-ferrite, austenite, and Cr23 C6 , respectively.
color indicate delta-ferrite, austenite, and Cr23C6, respectively.

Figure 3. (a) Optical micrographs indicating the indenting positions; (b) Vicker hardness measured
through
Figurethe
3. base metal, micrographs
(a) Optical the HAZ, andindicating
the weld metal.
the indenting positions; (b) Vicker hardness measured
Figure 3. (a) Optical micrographs indicating the indenting positions; (b) Vicker hardness measured
through the base metal, the HAZ, and the weld metal.
through the base
Figure metal,
4 shows thethe HAZ, and theofweld
microstructure metal.
the base material and the HAZ after heat-treated at 650–
850 °C for 0.5–44 h.
Figure The size
shows the of the austenite of
microstructure grain
the boundaries of the
base material andbase material
the HAZ and
after the HAZ isat40–
heat-treated 650–
850 °C for 0.5–4 h. The size of the austenite grain boundaries of the base material and the HAZ is 40–
Metals 2018, 8, 26 5 of 13

Figure 4 shows the microstructure of the base material and the HAZ after heat-treated at
Metals 2018, 8, 26 5 of 13
650–850 ◦ C for 0.5–4 h. The size of the austenite grain boundaries of the base material and the
HAZ
60 μm is on
40–60 µm onwhich
average, average,
is notwhich is not significantly
significantly changed, compared
changed, compared to the
to the as-weld as-weld specimen.
specimen. The strips
The strips already existing in the base material still remained, without noticeable
already existing in the base material still remained, without noticeable changes in the shape changes in theand
shape
the
and the volume fraction even after the heat treatment at 650 ◦ C. In the 850 ◦ C heat treatment, however,
volume fraction even after the heat treatment at 650 °C. In the 850 °C heat treatment, however, the
the volume
volume of the
of the strips
strips decreased
decreased andand
theirtheir shapes
shapes werewere blurred
blurred as compared
as compared withwith
thethe as-weld
as-weld andand
the
the heat-treated specimens at 650 ◦ C. It can be inferred that the Cr-based carbide was decomposed into
heat-treated specimens at 650 °C. It can be inferred that the Cr-based carbide was decomposed into
an ◦ C.
anaustenite
austenitephasephaseat at850
850 °C.

Figure 4. Optical micrographs on the base metal and the HAZ of the heat-treated specimens at (a)
Figure 4. Optical micrographs on the base metal and the HAZ of the heat-treated specimens at (a) 650 ◦ C
650 °C for 0.5 h,◦ (b) 650 °C for 1 h, (c) 650 °C for 4 h, (d) 850 °C for 0.5 h, (e) 850 °C for 1 h, and (f)
for 0.5 h, (b) 650 C for 1 h, (c) 650 ◦ C for 4 h, (d) 850 ◦ C for 0.5 h, (e) 850 ◦ C for 1 h, and (f) 850 ◦ C for
850 °C for 4 h. Arrows indicating pre-existing strips of delta ferrite and Cr-carbide in the HAZ,
4 h. Arrows indicating pre-existing strips of delta ferrite and Cr-carbide in the HAZ, respectively.
respectively.

ItIthas
hasbeen
beenreported
reportedthatthatCr-based
Cr-basedcarbide
carbideisisprecipitated
precipitatedand andaadelta
deltaphase
phaseisistransformed
transformedinto into
aasigma phase in the temperature range of 600–850 ◦ C in 300-series austenitic stainless steels [11,15].
sigma phase in the temperature range of 600–850 °C in 300-series austenitic stainless steels [11,15].
The ◦ C, about 1% of the
The results
results of of the
the thermodynamic
thermodynamiccalculations
calculationsinin Figure
Figure 5 show
5 show thatthat at °C,
at 650 650about 1% of the Cr23C6
Cr 23 C 6 and 8% of the sigma phase can be precipitated in equilibrium
and 8% of the sigma phase can be precipitated in equilibrium from the base metal composition. from the base metal composition.
This
This Cr
Cr23C6 23 C 6 is
is known known to be precipitated in the austenite grain boundaries where segregated chromium
to be precipitated in the austenite grain boundaries where segregated chromium
atoms
atoms tend tendto tobe bebound
boundwithwithcarbon
carbonatoms.
atoms.Therefore,
Therefore,the theformation
formationofofCr Cr2323CC66 makes
makes chromium
chromium
concentration
concentration in the grain boundaries lowered, i.e., chromium depletion, which results in the
in the grain boundaries lowered, i.e., chromium depletion, which results in the less
less
formation
formation of the Cr-based oxides and thus provides harmful effect on corrosion properties and
of the Cr-based oxides and thus provides harmful effect on corrosion properties and
toughness
toughnessof ofgrain
grainboundaries.
boundaries. On On the
theother
otherhand,
hand,sigma
sigmaphase
phaseof ofaatetragonal
tetragonalstructure
structurecomposed
composed
of
of Fe-Cr-Ni-Mo is generally reported to be precipitated in ferrite/austenite phaseboundaries
Fe-Cr-Ni-Mo is generally reported to be precipitated in ferrite/austenite phase boundariesand andto to
be
be grown into ferrite phase [16,17]. In the present thermodynamic calculations, the sigma phasewas
grown into ferrite phase [16,17]. In the present thermodynamic calculations, the sigma phase was
expected
expectedto tohave
haveaahigh highfraction
fractionofof8%,
8%,which
whichcould couldbe beregarded
regardedas asthe
themuch
muchhigher highervalue
valuethanthanthethe
actual experimental value. The reason for this overestimation is that the
actual experimental value. The reason for this overestimation is that the thermodynamic calculation thermodynamic calculation
does ◦C
does notnot consider kineticsof
consider kinetics ofphase
phasetransformation;
transformation; alpha
alpha ferrite
ferrite waswas calculated
calculated to exist
to exist in °C
in 650 650from
from the present
the present thermodynamic
thermodynamic calculation
calculation but wasbut was not actually
not actually present
present in thein the
basebase metalmetal
wherewherethe
the
single austenite phase only existed. In the base metal, the preferred nucleation site of the sigma sigma
single austenite phase only existed. In the base metal, the preferred nucleation site of the phase,
phase, i.e., ferrite,
i.e., ferrite, is hardly is hardly existing,
existing, andthe
and thus thus the actual
actual volume volume
of the of the sigma
sigma phasephase could could
be much be much
lower
lower ◦ C,
than the calculated predictions. On the other hand, in the case of the heat treatment at 850 °C,850
than the calculated predictions. On the other hand, in the case of the heat treatment at it was
itpredicted
was predicted that 0.4% that 0.4%
of Crof Cr23 C6 phase
23C6 phase would would be precipitated
be precipitated and and
the the
sigmasigma phasephase could
could notnot be
be precipitated. The volume fraction of Cr C decreased with increasing temperature up to 900 ◦C
23 6
precipitated. The volume fraction of Cr23C6 decreased with increasing temperature up to 900 °C above
above
whichwhich the Cr-carbide
the Cr-carbide wouldwould
not benot be precipitated.
precipitated.
Metals 2018, 8, 26 6 of 13
Metals 2018, 8, 26 6 of 13

Figure 5. Predicted volume fraction of equilibrium phases at given temperatures in (a,b) the base
Figure 5. Predicted volume fraction of equilibrium phases at given temperatures in (a,b) the base metal
metal (STS 304) and (c,d) the filler metal (STS 308L).
(STS 304) and (c,d) the filler metal (STS 308L).

Figure 6 shows the microstructure of the weld metal heat-treated at 650–850 °C for 0.5 and 4 h.
Figure 6 shows themicrostructure,
microstructurethe of the weld metal heat-treated ◦ for 0.5 and 4 h.
Similar to the as-weld austenite matrix contained at 650–850
delta ferrite Cdendrites. After
Similar
heat to the as-weld
treatment at 650–850microstructure,
°C, the lathy the austenite
type matrixchanged
delta ferrite contained todelta ferrite dendrites.
vermicular type due to After heat
the heat
treatment and at 650–850 ◦ C, the
the individual
lathy type dendrite
delta ferrite changed
treatment the size of of delta ferritetoincreased
vermicular type°Cdue
at 850 to the heat
in comparison
treatment and the size of the individual dendrite of delta ferrite increased at 850 ◦ C in comparison with
with 650 °C. The phase boundary between austenite and delta ferrite is considered to migrate in favor
◦ C. The phase boundary between austenite and delta ferrite is considered to migrate in favor of
650reducing
of the interfacial energy. The initially thin dendrites of delta ferrite could thus be thicker
reducing the interfacial energy.
during heat treatment withoutThe initially
losing theirthin dendrites
total volume of delta ferrite
fraction could thus
as confirmed inbe thicker
Figure during
6e,f. The
heat treatment without losing their total volume fraction as confirmed
fraction of delta ferrite was measured to be slightly decreased during heat treatment at 650–850 °C.in Figure 6e,f. The fraction
of delta7 ferrite ◦ C. Figure 7
Figure shows was measured
the volume to be slightly
fractional changedecreased during
of delta ferrite withheat treatment and
temperature at 650–850
time obtained from
shows the volume fractional change of delta ferrite with temperature
the magnetic induction method. Because possible phases such as austenite, Cr-carbide, and sigma and time obtained from the
magnetic induction method. Because possible phases such as austenite, Cr-carbide,
phase are all paramagnetic, only ferromagnetic ferrite reacts to the magnetic induction, so that the and sigma phase
are all paramagnetic,
surface volume fraction only of ferromagnetic ferrite reacts
ferrite can be precisely to the magnetic
measured induction,
[18]. At 650–850 so that
°C, the thefraction
ferrite surface
volume fraction of ferrite can be precisely measured [18]. At 650–850 ◦ C, the ferrite fraction of the weld
of the weld metal was reduced by 1% compared to the as-weld specimen. From the thermodynamic
metal was reduced
calculation by 1% in
results shown compared
Figure 5c, toathe as-weld
small amount specimen.
of ferriteFrom the thermodynamic
has been transformed into calculation
austenite
results shown in Figure 5c, a small amount of ferrite has been transformed
because the Ae3 temperature is less than 650 °C. However, as observed from optical photographs into austenite becausein
the A temperature is less than 650 ◦ C. However, as observed from optical photographs in Figure 6,
Figuree36, the volume fraction variation of delta ferrite seems to be insignificant but rather the size of
the volumedelta
individual fraction variation
ferrite is likelyof to
delta ferrite
become seems
larger astotemperature
be insignificant but rather
increases from the 650size of individual
to 850 °C.
delta ferrite is likely to become larger as temperature increases from 650 to 850 C. ◦
Metals 2018, 8, 26 7 of 13
Metals 2018, 8, 26 7 of 13
Metals 2018, 8, 26 7 of 13

Figure 6. Optical micrographs (OM) on the weld metal of the heat-treated specimens for (a) 0.5 h at
Figure 6.
Figure
650 6. Optical
°C, (b) Optical micrographs (OM)
micrographs
4 h at 650
(OM) on the
°C, (c) 0.5 h at 850on
the weld
°C, and
weld metal
metal ofof the
(d) 4 h at 850
the heat-treated
heat-treated specimens for
°C, respectively.specimens
for (a)
(a) 0.5
0.5 h
h at
To show the thickening at
650 ◦ C, (b) 4 h at 650 ◦ C, (c) 0.5 h at 850 ◦ C, and (d) 4 h at 850 ◦ C, respectively. To show the thickening
650 °C, (b) 4 h at 650 °C, (c) 0.5 h at 850 °C, and (d) 4 h at 850 °C, respectively. To show the
of delta ferrite dendrite, markers indicate the thickness of delta ferrite dendrite for the heat-treated thickening
of delta ferrite dendrite, markers indicate the thickness of delta ferrite dendrite for the heat-treated
of delta ferrite
specimens dendrite,
for (e) 4 h at 650markers
°C andindicate
(f) 4 h atthe
850thickness
°C. of delta ferrite dendrite for the heat-treated
specimens for (e) 4 h at 650 ◦ C and (f) 4 h at 850 ◦ C.
specimens for (e) 4 h at 650 °C and (f) 4 h at 850 °C.

Figure 7. Volume fraction of delta ferrite in the weld metal measured by magnetic induction method.
Figure
Figure 7.
7. Volume fraction of
Volume fraction of delta
delta ferrite
ferrite in
in the
the weld
weld metal
metal measured
measured by
by magnetic
magnetic induction
induction method.
method.
Figure 8 is the EBSD phase map that shows the presence of Cr23C6 in the weld after annealing at
650 °CFigure
Figure
8 is
for 4 h.
8 The
theCrEBSD
is the
phase map that shows the presence of Cr23C6 in the weld after annealing at
23C6, which did not exist in the as-weld specimen, was found to precipitate finely
EBSD phase map that shows the presence of Cr23 C6 in the weld after annealing
650
in °C for 4 h. The Cr 23C6, which did not exist in the as-weld specimen, was found to precipitate finely
at the
650austenite/delta-ferrite
◦ C for 4 h. The Cr C interface afternot
, which did
23 6interface
4 hexist
of heat treatment
in the as-weldatspecimen,
650 °C. Crwas
23C6 carbide is reported
found to precipitate
in
to the austenite/delta-ferrite after 4 h of heat treatment at 650 °C. Cr 23C6 carbide is reported
finely in the austenite/delta-ferrite interface after 4 h of heat treatment at 650 ◦ C. Crin
precipitate from austenite/ferrite phase boundary or austenite grain boundary 300-series
23 C300-series
6 carbide
to precipitate
austenitic fromsteels
stainless austenite/ferrite
[11,15,16]. phase
After boundary or
precipitation, it austenite
grows into grain boundary
austenite matrix in
rather than
is reported to precipitate from austenite/ferrite phase boundary or austenite grain boundary in
austenitic
ferrite stainless
matrix. steels [11,15,16].
It is known After precipitation,
that the precipitates are finelyit located
grows into austenite
in the matrix
boundaries rather
with the than
size
ferrite matrix.
distribution from It is known
several that thenm
hundred precipitates
to few μm,are finely located
depending on thein the boundaries
composition with
and the the size
formation
distribution from several hundred nm to few μm, depending on the composition
temperature [15]. As can be seen from the thermodynamic calculations shown in Figure 5, the and the formation
temperature [15]. As can be seen from the thermodynamic calculations shown in Figure 5, the
Metals 2018, 8, 26 8 of 13

300-series austenitic stainless steels [11,15,16]. After precipitation, it grows into austenite matrix
rather than ferrite matrix. It is known that the precipitates are finely located in the boundaries with
the size distribution from several hundred nm to few µm, depending on the composition and
Metals 2018, 8, 26
the
8 of 13
formation temperature [15]. As can be seen from the thermodynamic calculations shown in Figure 5,
the temperature range near ◦ C could have 0.5% volume fraction of Cr C , which is the maximum
temperature range near 650650
°C could have 0.5% volume fraction of Cr2323C6,6 which is the maximum
value in whole temperature range. Although itit is
value in whole temperature range. Although is aa small
small volume
volume fraction,
fraction, it
it is
is presumed
presumed thatthat if
if the
the
precipitates are finely distributed along the phase boundaries, it could deteriorate
precipitates are finely distributed along the phase boundaries, it could deteriorate the ductility and the ductility and
toughness of
toughness of the
the material.
material. In
In the
the thermodynamic
thermodynamic calculation,
calculation, itit was
was predicted
predicted thatthat about
about 12%
12% of
of the
the
sigma phase would be precipitated in the weld metal at 650 ◦ C. However, the EBSD results hardly
sigma phase would be precipitated in the weld metal at 650 °C. However, the EBSD results hardly
showed the
showed the presence
presence ofof sigma
sigma phase.
phase. It It is
is believed
believed thatthat the
the transformation
transformation kinetics
kinetics of of sigma
sigma phase
phase is is
relatively slow,
relatively slow, soso that sigma phase
that sigma phase could
could not not be
be transformed
transformed fromfrom ferrite
ferrite with
with the
the given
given temperature
temperature
and time. Even if sufficient time is provided, it is expected that the sigma
and time. Even if sufficient time is provided, it is expected that the sigma phase would not be phase would not be present
present
as much as the predicted value since the volume fraction of ferrite, which is
as much as the predicted value since the volume fraction of ferrite, which is the preferred nucleationthe preferred nucleation
site of
site of the
the sigma
sigma phase,
phase, is
is relatively
relatively small
small in in the
the actual
actual weld
weld metal.
metal.

Figure
Figure 8.
8. (a)(a)EBSD
EBSD map
mapshowing
showingpresence of Cr
presence C6 atCphase
of23Cr boundary; (b) OM image after color-
23 6 at phase boundary; (b) OM image after
etching showing the presence of Cr 23C6 (dark).
color-etching showing the presence of Cr23 C6 (dark).

Figure 9a–d show the microstructures of the base material and HAZ of the specimens annealed
Figure 9a–d show the microstructures of the base material and HAZ of the specimens annealed
at 1050 °C for 0.5–4 h. The grain size of the base metal after PWHT in 1050 °C for 4 h became larger
at 1050 ◦ C for 0.5–4 h. The grain size of the base metal after PWHT in 1050 ◦ C for 4 h became
(72 μm) than the as-weld specimen (52 μm), which shows the grain growth of austenite with
larger (72 µm) than the as-weld specimen (52 µm), which shows the grain growth of austenite with
increasing time and temperature. This grain growth is believed to occur because of the acceleration
increasing time and temperature. This grain growth is believed to occur because of the acceleration of
of thermally-assisted migration of the austenite grain boundary. The strip already existing in the base
thermally-assisted migration of the austenite grain boundary. The strip already existing in the base
metal was observed to disappear as the heat treatment time became longer. As can be seen from the
metal was observed to disappear as the heat treatment time became longer. As can be seen from the
thermodynamic calculation in Figure 5, the Cr-based carbide was considered to transform into the
thermodynamic calculation in Figure 5, the Cr-based carbide was considered to transform into the
austenite phase at 1050 °C since the dissolution temperature of the Cr-based carbide is about 900 °C.
austenite phase at 1050 ◦ C since the dissolution temperature of the Cr-based carbide is about 900 ◦ C.
Figure 9e–h shows the microstructure of welded specimens after heat treatment at 1050 °C for
Figure 9e–h shows the microstructure of welded specimens after heat treatment at 1050 ◦ C
0.5–4 h. The delta ferrite, which existed as lathy or vermicular shape in the as-weld specimen, lost its
for 0.5–4 h. The delta ferrite, which existed as lathy or vermicular shape in the as-weld specimen,
shape into the elliptical or the spheroidized after the heat treatment of 1050 °C. This is due to the
lost its shape into the elliptical or the spheroidized after the heat treatment of 1050 ◦ C. This is due to
migration of austenite/delta-ferrite interface for decreasing the interfacial energy, similar to the
the migration of austenite/delta-ferrite interface for decreasing the interfacial energy, similar to the
mechanism of the shape change from the lathy to the vermicular type observed in the heat treatment
mechanism of the shape change from the lathy to the vermicular type observed in the heat treatment
at 650–850 °C. The volume fraction of delta ferrite at 1050 °C decreased by heat treatment time as
at 650–850 ◦ C. The volume fraction of delta ferrite at 1050 ◦ C decreased by heat treatment time as
confirmed in Figure 7 where delta-ferrite, which was 8% of volume fraction in the as-weld specimen
confirmed in Figure 7 where delta-ferrite, which was 8% of volume fraction in the as-weld specimen
decreased down to 1.2% after heat treatment at 1050 °C for 4h. From the thermodynamic point of
decreased down to 1.2% after heat treatment at 1050 ◦ C for 4h. From the thermodynamic point
view, the transformation of delta ferrite to austenite was believed to be promoted at 1050 °C, well
of view, the transformation of delta ferrite to austenite was believed to be promoted at 1050 ◦ C,
above the Ae3 temperature. From the thermodynamic calculations, austenite single phase exists at
well above the Ae3 temperature. From the thermodynamic calculations, austenite single phase exists at
1050 °C, without Cr-carbide or delta-ferrite phase, and well agree with the experimental observations.
1050 ◦ C, without Cr-carbide or delta-ferrite phase, and well agree with the experimental observations.
The residual delta-ferrite, which was not transformed into austenite by the rapid cooling after the
The residual delta-ferrite, which was not transformed into austenite by the rapid cooling after
welding, was gradually austenized by heat treatment at 1050 °C. In addition, at that temperature,
the welding, was gradually austenized by heat treatment at 1050 ◦ C. In addition, at that temperature,
residual stress due to welding could be released and carbides could dissolve sufficiently, which could
possibly lead to noticeable changes in the mechanical properties.
Metals 2018, 8, 26 9 of 13

residual stress due to welding could be released and carbides could dissolve sufficiently, which could
possibly
Metals 2018,lead
8, 26to noticeable changes in the mechanical properties. 9 of 13

Figure 9. Optical micrographs on the base metal and the HAZ of the heat-treated specimens at 1050 °C
Figure 9. Optical micrographs on the base metal and the HAZ of the heat-treated specimens at
for (a) 0.5 h, (b) 1 h, (c) 2 h, and (d) 4 h, respectively. Optical micrographs on the weld metal of the
1050 ◦ C for (a) 0.5 h, (b) 1 h, (c) 2 h, and (d) 4 h, respectively. Optical micrographs on the weld
heat-treated specimens at 1050 °C for (e) 0.5 ◦h, (f) 1 h, (g) 2 h, and (h) 4 h, respectively. Arrows and
metal of the heat-treated specimens at 1050 C for (e) 0.5 h, (f) 1 h, (g) 2 h, and (h) 4 h, respectively.
triangles indicate the pre-existing strips in the base/HAZ and delta ferrite in the weld metal,
Arrows and triangles indicate the pre-existing strips in the base/HAZ and delta ferrite in the
respectively.
weld metal, respectively.

Figure 10 summarized the yield and tensile strength, uniform and total elongation, and fracture
Figureof10specimens
toughness summarized thePWHT.
after yield and
Thetensile
yield strength,
and tensileuniform andin
strengths total
all elongation,
range of heatand fracture
treatment
toughness of specimens
temperatures and times were afterlower
PWHT.thanThe yield
those ofand tensile strengths
the as-weld specimen.inThe
all yield
rangestrength
of heat treatment
gradually
decreased as the temperature increased while there was no significant change depending ongradually
temperatures and times were lower than those of the as-weld specimen. The yield strength the time.
decreased as the temperature increased while there was no significant change depending
The tensile strength of the specimens heat-treated at 650–850 °C was 570–580 MPa and a noticeable on the time.
The tensilewas
strength of found
the specimens heat-treated at 650–850 ◦
difference hardly depending on the heat treatmentCtime.
was 570–580 MPa
In the case of and a noticeable
the heat treated
difference was hardly found depending on the heat treatment time. In the case
specimen at 1050 °C, the tensile strength was markedly lower and continuously decreasing with of the heat treated
the
specimen at 1050 ◦ C, the tensile strength was markedly lower and continuously decreasing with
time. As shown in Figure 10b, the uniform and total elongation decreased with increasing
the time. Asupshown
temperature to 850 in°C,Figure 10b, with
compared the uniform andspecimen.
the as-weld total elongation decreased
On the other hand, with increasing
the specimen at
temperature up to 850 ◦ C, compared with the as-weld specimen. On the other hand, the specimen at
1050 °C showed higher elongation than the as-weld specimen, and prolonged its elongation as the
heat treatment time increased.
Metals 2018, 8, 26 10 of 13

1050 ◦ C showed higher elongation than the as-weld specimen, and prolonged its elongation as the
heat
Metalstreatment
2018, 8, 26 time increased. 10 of 13

10. (a)
Figure 10. (a) Yield
Yieldand
andtensile
tensilestrength
strength
ofof
thethe as-weld
as-weld andand
thethe heat-treated
heat-treated specimens;
specimens; (b) uniform
(b) uniform and
and total elongation of the as-weld and the heat-treated specimens; (c) fracture toughness of
total elongation of the as-weld and the heat-treated specimens; (c) fracture toughness of the as-weld the as-
weldthe
and and the heat-treated
heat-treated specimens;
specimens; (d)hardness
(d) Vickers Vickers of
hardness of the
the as-weld andas-weld and the specimens.
the heat-treated heat-treated
specimens.
These changes of mechanical properties can be understood based on the microstructural evolution
duringThese
heatchanges
treatment.of mechanical
In the case properties
of reduction caninbe understood
strength based on
and ductility the microstructural
shown at 650–850 ◦ C,
evolution of
relaxation during heat
internal treatment.
stress, decreased In the case fraction
volume of reduction
of deltain ferrite
strength andand ductility
increased sizeshown at 650–
of individual
850 °C, relaxation of internal stress, decreased volume fraction of delta
delta ferrite dendrite could be responsible for such degradation. As shown in Figure 8, the carbides ferrite and increased size of
individual delta ferrite dendrite could be responsible for such degradation.
were found to form in the austenite/ferrite phase boundaries. It is expected that material strength As shown in Figure 8, the
carbides
would were found
increase to form in the
by compromising austenite/ferrite
ductility phase boundaries.
with the formation of Cr-carbide, It but
is expected
inverselythatthe material
strength
strength would increase by compromising ductility with the formation
decreased at the corresponding temperature. This reduction in strength, first of all, could probably of Cr-carbide, but inversely
theexplained
be strength decreased
by the stressat the corresponding
relaxation due to temperature.
the recovery of This
thereduction
hot-rolledinmicrostructure
strength, first of inall,
thecould
base
probably be explained by the stress relaxation due to the recovery of the hot-rolled
metal and by the relaxation of the internal stress in the base and the weld metal initially caused by the microstructure in
the base metal and by the relaxation of the internal stress in the base and
welding process [19]. Second, as shown in Figure 7, the slight decrease in volume fraction of the delta the weld metal initially
causedinby
ferrite thethe welding
weld metal process [19]. Second,
could possibly cause the as shown
strengthinreduction
Figure 7,inthe slight
terms decrease hardening.
of modulus in volume
fraction of the delta ferrite in the weld metal could possibly cause the
Third, as can be seen in Figure 6, when the individual size of the delta ferrite increased without strength reduction in terms
losingof
modulus hardening. Third, as can be seen in Figure 6, when the individual
its volume fraction substantially, the strength can be reduced owing to the weakening of dispersion size of the delta ferrite
increased without
strengthening losing its volume
or precipitation fraction substantially,
strengthening the strength
[20]. Stochastically, can be reduced
the probability of theowing
existence to the
of
weakening of dispersion strengthening or precipitation strengthening
dislocation sources is higher in the austenite matrix whose volume fraction and size is much higher [20]. Stochastically, the
probability
than of theGiven
delta ferrite. existence
that of dislocation
austenite sources is
has generally higher
lower in strength
yield the austenite matrixthe
than ferrite, whose volume
operation of
fraction and size is much higher than delta ferrite. Given that austenite
dislocation is likely to initiate in the austenite matrix. The dislocation movement in the austenite couldhas generally lower yield
strength
then than ferrite,
be impeded the delta
by stiff operation
ferriteofarrays
dislocation
and if theis likely to initiate
individual in the
size of the delta
austenite
ferrite matrix. The
increased,
dislocation
particle movementcould
strengthening in thebe austenite
degraded. could then be impeded by stiff delta ferrite arrays and if the
individual size of the delta ferrite increased,
On the other hand, in the case of heat treatment particle strengthening
above 1050 ◦ C, could be degraded.
the yield and tensile strengths
On the other hand, in the case of heat treatment
were lower but elongations were higher than the as-weld specimen. As above 1050 °C, the yield and tensile
shown in Figure strengths
8, the
were lower
decrease butvolume
in the elongations
fraction were higher
of delta than
ferrite at the
1050as-weld specimen.toAs
◦ C is considered shown
be the cause inofFigure 8, the
the strength
decrease in the volume fraction of delta ferrite at 1050 °C is considered
reduction. Since the thickness of delta ferrite was small as about 1–2 µm, it is believed that the to be the cause of the strength
reduction. Since the thickness of delta ferrite was small as about 1–2 μm, it is believed that the delta
ferrite is strengthening the weld metal in terms of modulus hardening and particle hardening.
Therefore, decreasing the fraction of delta ferrite may have affected the decrease of strength and
increase of elongation inversely. In addition, as shown in Figure 9, the austenite grain size of the base
and welds increased during the heat treatment at 1050 °C, and thus Hall-Petch effect due to the
Metals 2018, 8, 26 11 of 13

delta ferrite is strengthening the weld metal in terms of modulus hardening and particle hardening.
Therefore, decreasing the fraction of delta ferrite may have affected the decrease of strength and
increase of elongation inversely. In addition, as shown in Figure 9, the austenite grain size of the
base and welds increased during the heat treatment at 1050 ◦ C, and thus Hall-Petch effect due to the
increase of grain size also has an effect on the reduction in yield and tensile strengths. Furthermore, the
stress relaxation due to the heat treatment at 1050 ◦ C could make the base and weld metal softer.
Figure 10c shows the fracture toughness obtained by integrating stress-strain curves. When heat
treatment temperature was in the range of 650–850 ◦ C, the fracture toughness was lower than that
of the as-weld specimen. When the heat treatment temperature was more than 1050 ◦ C, the fracture
toughness was in overall similar or higher than the as-weld specimen. In the temperature range
studied in the present work, the strengths were reduced as compared with the as-weld specimen,
but ductility significantly increased at 1050 ◦ C. This ductility increase is reflected in the increase of the
fracture toughness, and the PWHT at a temperature of 1050 ◦ C was found to provide positive effect on
improving the toughness of the as-weld material.
Figure 10d shows the hardness variation of the welds with the PWHT temperature and time.
After 10 times of indentations, the values were averaged by excluding the maximum and the minimum.
Hardness is determined by the magnitude of strengthening under compression, and thus it can be
interpreted similarly to the strength. Vickers hardness showed a monotonic decrease with increasing
the heat treatment temperature. The hardness change with the heat treatment time was negligible
for 1 to 4 h, and temperature was more of an influential factor on the hardness. As described above,
reduction of hardness with increasing temperature is also able to be explained by the relaxation of the
residual stress, the decrease of delta-ferrite volume fraction and the increase of the individual delta
ferrite thickness.
Figure 11 contained the true stress-strain curves together with work hardening rate for analyzing
the difference in work hardening behaviors after PWHT. In the as-weld specimen, the work hardening
rate decreased rapidly after passing yield point and maintained in the steady state. On the other hand,
the work hardening rate of the specimen at 650 ◦ C for 2 h was generally higher than that of the
as-weld specimen, and decreased continuously with further straining after having a short steady-state
flow regime. The work hardening rate of PWHT 850 ◦ C increased continuously with deformation
after reaching the steady state. This is presumably due to the deformation-induced martensitic
transformation (DIMT) occurring in both of 304 base metal and 308 weld metal. When the DIMT occurs,
the martensite phase is produced with the deformation, and the volume fraction of martensite increases
steadily as the deformation continues, leading to the gradual increase of the work hardening rate [18].
The inflection shown in true stress-strain curve is related to the initiation of DIMT. A number of
researches reported that the DIMT indeed occurs in 300-series austenitic stainless steels and results
in the continuous increase of the work hardening rate during deformation [18,21,22]. At 1050 ◦ C,
the work hardening rate gradually increased and an inflection was observed in true stress-strain curve.
In this temperature, the initially present Cr-carbide arrays would dissolve and thus make austenite
matrix denser with carbon atoms. The austenite is thus more stabilized and the DIMT kinetics could
be slower, leading to the increase of elongation. Since the delta ferrite already existing in the weld
metal was mostly transformed into austenite and also the grain size of austenite increased at 1050 ◦ C,
the yield strength became lower than the as-weld specimen.
[18,21,22]. At 1050 °C, the work hardening rate gradually increased and an inflection was observed
in true stress-strain curve. In this temperature, the initially present Cr-carbide arrays would dissolve
and thus make austenite matrix denser with carbon atoms. The austenite is thus more stabilized and
the DIMT kinetics could be slower, leading to the increase of elongation. Since the delta ferrite already
existing in the
Metals 2018, 8, 26weld metal was mostly transformed into austenite and also the grain size of austenite
12 of 13
increased at 1050 °C, the yield strength became lower than the as-weld specimen.

Figure
Figure11.
11.True
Truestress-strain
stress-straincurves
curvesand
andwork
workhardening
hardeningrates
ratesin
interms
termsof
of(a)
(a)PWHT
PWHTtemperature
temperatureand
and
(b) PWHT time.
(b) PWHT time.

4. Conclusions
The effect of PWHT on the microstructure and mechanical properties of submerged-arc-welded
304 austenitic stainless steel was investigated. The results are summarized as follows:

(1) The base metal initially had a microstructure consisting of austenite matrix and strips of
delta-ferrite surround by Cr23 C6 . The weld metal consisted of lathy and vermicular type of
delta ferrite and austenite matrix. There was insignificant variation of microstructures and
mechanical properties between HAZ and the base metal, implying that heat affection by welding
was negligible.
(2) Cr-carbides were precipitated at the delta-ferrite/austenite interface in the weld metal after the
heat treatment at 650–850 ◦ C. Despite of the presence of Cr-carbide, the yield strength was lower
than the as-weld specimen, which could be possibly explained by the relaxation of internal stress
accumulated during the hot-rolling and the welding.
(3) After heat-treatment at 1050 ◦ C, the pre-existing strips in the base metal was dissolved into
austenite and the delta-ferrite of the weld metal was transformed into austenite, leading to
the microstructure close to the austenite single phase. Although the yield strength was lower
than that of the as-weld specimen due to the disappearance of hard phases and the relaxation
of residual stress, the elongation became higher than that of the as-weld metal due to the
compromising effect of strength and partially to the DIMT occurring during deformation. In terms
of fracture toughness, the heat treatment at 1050 ◦ C were suggested to provide superior property
than as-weld material due to the trade-off between strength and ductility.

Acknowledgments: This study has been conducted with the support of the Korea Institute of Industrial
Technology as “Development of metal powder large-area DED process including pre- and post- processes
based on simulations (KITECH EO-17-0041)” and “Development of Manufacturing Technology of Cryogenic
Stainless Steel Welded Steel Pipe (KITECH JG-17-0006)”.
Author Contributions: Tae-Hoon Nam and Jong Bae Jeon conceived and designed the experiments;
Tae-Hoon Nam and Eunsol An performed the experiments; Byung Jun Kim, Sunmi Shin, Nokeun Park,
Won-Seok Ko, Namhyun Kang and Jong Bae Jeon analyzed and discussed the data; Tae-Hoon Nam and
Jong Bae Jeon wrote the paper.
Conflicts of Interest: The authors declare no conflict of interest.

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