Materials Science & Engineering A 810 (2021) 141028

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Materials Science & Engineering A

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

Microstructure evolution and mechanical behavior of a lean duplex

stainless steel aged at 475oC
Thompson Júnior Ávila Reis, Henrique Meckler Santos, Eliza Wilk Reis de Almeida,
Leonardo Barbosa Godefroid *
REDEMAT, Federal University of Ouro Preto, Ouro Preto, MG, Brazil

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

Keywords: In this research, the effects of isothermal treatments at 475 ◦ C on the microstructure and mechanical properties
Lean duplex stainless steel of a UNS S32304 lean duplex stainless steel were investigated. Samples of the alloy under as received and aged
Atomic/magnetic force microscopy conditions were analyzed by atomic force microscopy and magnetic force microscopy in order to evaluate the
Mechanical properties
ability of these techniques to identify important aspects that characterize microstructural changes caused by
aging. The mechanical behavior was evaluated by tensile tests, hardness tests, Charpy impact tests, crack
extension resistance tests, force controlled axial fatigue tests and fatigue crack growth rate tests. The fracture
surfaces of all tested specimens were analyzed by scanning electron microscopy. The results indicate that the
α-phase spinodal decomposition occurred, with a tendency to saturation for a not too long aging time. The
analysis by atomic/magnetic force microscopy allowed to identify characteristics regarding the preferential
phase dissolution of the α phase that distinguish the alloy in the as received condition from the aged alloy. As a
consequence of the formation of the α’ phase, the absorbed impact energy and the fracture toughness of the alloy
decreased substantially. On the other hand, the tensile strength and the fatigue resistance increased significantly.

1. Introduction
The duplex stainless steel (DSS) is a two-phase alloy with approxi­
mately equal volume fraction of ferrite and austenite, with high me­
chanical resistance and corrosion resistance [1,2]. Result of a perfect
union between austenitic stainless steels and ferritic stainless steels, this
grade combines the best characteristics of both alloys, such as immunity
to stress corrosion cracking and good weldability. With low percentage
of nickel in its chemical composition, these steels present tensile yield
strength much higher than the austenitic stainless steels, which enables
the design of constructions with smaller thickness maintaining a high
corrosion resistance. The addition of nitrogen to DSS increases tough­
ness and corrosion resistance of the HAZ (Heat-Affected Zone) compared
to the base metal in welded condition. DSS is an attractive option for
application on flexible pipes in the oil & gas industry, as well as on
nuclear power plants, transportation, chemical storage tanks and on
equipments for pulp and paper segments.
Despite the interesting features, all the DSS applications are limited
to temperatures below 280 ◦ C due its susceptibility to precipitation of
undesirable phases above this temperature. Between 280 and 500 ◦ C,
the ferrite decomposition generates two distinct phases, α Fe-rich and α′
Cr-rich, by a transformation called spinodal decomposition [3]. Spino­
dal decomposition refers to a reaction where two phases of the same
crystal lattice type, but different compositions and properties, form due
to the existence of a miscibility gap in the alloy system. In this reaction,
there is no barrier to nucleation. For an alloy aged inside the spinodal,
fine scale composition fluctuations develop in the ferrite phase and in­
crease very rapidly with time. An “uphill” diffusion takes place, i.e. re­
gions richer in solute than the average become richer, and poorer
become poorer until the equilibrium compositions of the α and α’ phases
are formed. This phenomenon is highlighted at 475 ◦ C due the fastest
transformation kinetics at this temperature, and is commonly termed
“475 ◦ C embrittlement”, due to the steel embrittlement. For relatively
long aging times, there is a consensus among researchers about the
possibility of formation of other processes, such as the G phase precip­
itation (an intermetallic compound rich in Ni, Si and Mo) with an in­
cubation time after the spinodal decomposition of ferrite [4], as well as
carbide and nitride precipitation in grain boundaries [5,6].
Over the past five decades, a significant amount of research has been
published on 475 ◦ C embrittlement of DSSs, showing that the plasticity

* Corresponding author.
E-mail address: leonardo@ufop.edu.br (L.B. Godefroid).

https://doi.org/10.1016/j.msea.2021.141028
Received 22 December 2020; Received in revised form 26 February 2021; Accepted 3 March 2021
Available online 5 March 2021
0921-5093/© 2021 Elsevier B.V. All rights reserved.
T.J. Ávila Reis et al. Materials Science & Engineering A 810 (2021) 141028

Table 1
Chemical composition of the UNS S32304 LDSS (wt. %).
Cr Ni Mo Mn Si N C P S Fe

22.56 3.57 0.26 1.35 0.36 0.12 0.02 0.025 <0.001 Balance

Fig. 2. SPM images of the AR-LDSS microstructure in the longitudinal section,

polished using the OP-S suspension. α = ferrite; γ = austenite.

and hardness [7–18], fracture toughness [19–38] and fatigue behavior

Fig. 1. Microstructure of the AR-LDSS in the longitudinal section, etched by
Beraha’s reagent. α = ferrite; γ = austenite.
of spinodal decomposed ferrite is reduced because of a reduction in the
number of slip systems and that deformation by twinning may also take
place in addition to deformation by dislocation glide. These micro­
structural changes can alter, among several properties, tensile strength
of the alloy [39–71]. However, some open questions still justify the in­
terest on microstructural evolution and changes in the mechanical
properties of DSSs before and after thermal aging.
The ferritic phase separation process occurs at a very fine scale (of
the order of only a few nanometers) and the presence of the α′ phase can
only be observed through a sophisticated experimental technique. Some
examples of usual procedures include: transmission electron microscopy
(TEM) [61,67–71], high-resolution transmission electron microscopy
(HRTEM) [35], field-emission gun transmission electron microscopy
(FEG-TEM) [30], atom probe field ion microscopy (APFIM) [7,22,72]

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T.J. Ávila Reis et al.
Fig. 3. Height differences between ferrite and austenite from AFM images of
the AR-LDSS and all X-HT-LDSS samples after the OP-S polishing. (a) First
mechanical polishing; (b) Last mechanical polishing.
and atom probe tomography (APT) [17,38,73,74]. The electron
back-scattering diffraction (EBSD) technique has also been used to
monitor spinodal decomposition [56,60,62,63]. Through these tech­
niques, it is possible to verify that the spinodal decomposition of the
ferrite provides a microstructure that consists of a modulated structure
with a complex interconnected network containing the α and α’ phases,
and that the immobilization of dislocations in this modulated structure
can cause severe embrittlement. The complexity of all the techniques
mentioned above, due to the sample preparation, the restricted area of
analysis and the interpretation of the results, have stimulated the search
for more simple indirect ways of investigation of the 475 ◦ C embrittle­
ment. An alternative and indirect technique is scanning probe micro­
scopy (SPM), that uses a mechanical probe to obtain images from
interactions between the tip and the sample surface to be analyzed [75].
SPM presents high spatial resolution and can be used in various modes of
operation, among them the contact mode - atomic force microscopy
(AFM) and magnetic force microscopy (MFM). AFM reveals topographic
variations between the different phases present in the steel, according to
the chemical composition of each phase. MFM presents distinct mag­
netic patterns generated by these phases, taking advantage of the fact
that ferrite is ferromagnetic and austenite is paramagnetic. Both tech­
niques can be used to characterize the microstructural evolution of the
DSS embrittlement, from samples with very simple metallographic
preparation [76–78].
Many researchers have used relatively long aging times, even years,
to study the 475 ◦ C embrittlement [18,35,38,70]. However, some
studies show that after a relatively short time the phase transformation
is completed and some properties may become constant [30, 61, 67–69,
71]. Therefore, another current issue consists of checking the saturation
of the spinodal decomposition, and verifying the necessary aging time at
475 ◦ C to produce considerable changes in the mechanical properties of
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Materials Science & Engineering A 810 (2021) 141028
the DSSs.
The experimental results on the change in mechanical behavior of
DSSs due to their embrittlement show that some properties are reduced
(ductility, impact resistance, fracture toughness), while other properties
are increased (tensile strength, fatigue resistance) in relation to the non-
embrittlement state [17,18,30,35,38,61,67–71]. Hence, another
important issue is the knowledge of the widest possible set of steel
characteristics, in order to have an adequate materials selection that
meets the specifications required for its application.
Recently, the “lean” duplex stainless steel (LDSS) grade has received
special attention from the steel plants due to the price fluctuation of
some alloying elements such as nickel and molybdenum. For example,
the UNS S32304 LDSS [79] has lower content of these elements if
compared to the standard UNS S32205/S31803 DSS [80]. As the LDSS
still maintains good properties, it is indicated to replace the 304 and 316
austenitic stainless steels (ASS) in many applications. In principle, LDSSs
should be more resistant to the 475 ◦ C embrittlement than the standard
DSSs grades due to their lower content of alloying elements and,
consequently, due to the decreased rate of embrittlement reaction in the
ferritic phase. However, the effects of the ferrite decomposition on the
mechanical properties of the LDSSs can be as severe as in standard DSSs,
depending on the state of the ferritic phase [3]. As only the ferritic phase
is embrittled during aging treatment at 475 ◦ C the degradation in me­
chanical properties directly depends on microstructural characteristics
of the ferritic phase. The volume fraction, distribution in the matrix,
grain size and grain shape of the ferritic phase are observed to affect the
nature of precipitation and the degree of embrittlement. This fact has
recently motivated some scientific efforts to study the effects of the
475 ◦ C embrittlement on the mechanical behavior of LDSSs [81–90]. An
in-depth understanding of the microstructure-properties relationship of
this new DSS grade is another current issue.
In these contexts, this present research had three purposes related to
the 475 ◦ C embrittlement of an UNS S32304 LDSS. The first goal was the
use of the SPM technique, in the AFM and MFM modalities, to verify its
indirect ability to follow the evolution of spinodal decomposition during
the aging treatment. This objective is justified by the fact that the SPM
technique presents sample preparation and analysis of results relatively
simpler than the traditional techniques involving electron microscopy.
The second goal was to investigate the effects of the aging time at 475 ◦ C
in a broad range of mechanical properties, including fracture toughness
and fatigue resistance, giving especial attention for critical short times of
aging that can severely change the mechanical behavior of the steel. This
objective is justified by the fact that the choice of an adequate aging time
could serve as a heat treatment to benefit some properties (such as
tensile strength and hardness), without prejudice to other properties
(such as ductility and fracture toughness). The third goal was to generate
more information about an LDSS, to allow the expansion of its engi­
neering applications. This objective is justified by the fact that the
development of LDSSs is still recent, requiring more precise knowledge
about its mechanical behavior, especially with regard to fracture
toughness and resistance to fatigue cracking.
2. Material and methodology
The material used in this research was a UNS S32304 steel supplied
by Aperam South America as hot rolled sheets with 10 mm final thick­
ness. The steel was hot rolled (between 1,200 ◦ C and 1,050 ◦ C), and then
subjected to solution annealing (between 1,080 ◦ C and 1,120 ◦ C), fol­
lowed by a rapid quench, to obtain its mechanical properties and
corrosion resistance. The chemical composition of the steel, obtained by
optical emission spectrometry (OES), is shown in Table 1. The material
is an LDSS, whose chemical composition is in accordance with the
standard specifications for this DSS grade [79]. The low percentage of
nickel and molybdenum is highlighted, as well as the presence of ni­
trogen to increase the toughness and corrosion resistance of the
heat-affected zone compared to the base metal in welded condition.
T.J. Ávila Reis et al. Materials Science & Engineering A 810 (2021) 141028

Fig. 4. AFM images before electrolytic polishing from (a) AR-LDSS, (c) 6, (e) 25 and (g) 100-HT-LDSS. MFM images of the same AFM images positions from (b) AR-
LDSS, (d) 6, (f) 25 and (h) 100-HT-LDSS. Images scale in micrometers. Longitudinal section. α = ferrite; γ = austenite.

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T.J. Ávila Reis et al.
Fig. 5. AFM 3D-images after electrolytic polishing from (a) AR-LDSS, (b) 1, (c)
6, (d) 12, (e) 25, (f) 50 and (g) 100-HT-LDSS. Images scale in micrometers.
Longitudinal section. α = ferrite; γ = austenite.
Samples were annealed at 1100 ◦ C and then water quenched, to
provide a ferrite and austenite volume fraction of approximately 50% of
each phase and to avoid the precipitation of deleterious phases. Samples
were subsequently isothermally aged at 475 ◦ C for 1, 6, 12, 25, 50 and
100 h and water quenched to room temperature. The choice of these
aging times is based on references [30,61,67–69,71,83] that have
observed spinodal decomposition and the stabilization of mechanical
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Materials Science & Engineering A 810 (2021) 141028
Fig. 6. Two ways to show the microstructural evolution of the LDSS as a
function of the heat treatment time at 475 ◦ C: (a) relative heights between
ferrite and austenite; (b) dissolved ferrite layer thickness both in function of the
aging time.
properties for relatively short times. The following nomenclature was
adopted for the samples: AR-LDSS represents the as received condition
and X-HT-LDSS represents the heat-treated samples, where X indicates
the time in hours.
For the microstructural characterization, all specimens were previ­
ously submitted to usual metallographic preparation according to the
ASTM E3 standard [91]: cutting and mounting; grinding from 120#
sandpaper to 1200# sandpaper; polishing with 1 μm alumina suspension
and then 0.25 μm diamond paste. Samples were etched with Beraha’s
reagent (a solution of 1 g K2S2O5 + 3 g NH5F2 + 15 ml HCl diluted in 85
ml of distilled water) for 5s, as specified by the ASTM E407 standard
[92]. This solution provides a good distinction between the α phase that
appears in tones that vary between brown and dark green and the γ
phase that appears in light yellow tones. The steel microstructures in the
as received condition and after aging treatments were examined on a
LEICA DM2700 M light optical microscope (LOM) and a VEGA3 TESCAN
scanning electron microscope (SEM). Using digital processing in 10
optical microscopy images, with the aid of the QWIN software it was
possible to quantify the volume fraction of the two phases in the steel.
In this research, scanning probe microscopy (SPM) analyses oper­
ating in atomic force microscopy (AFM) and magnetic force microscopy
(MFM) modes were used as an indirect method to characterize the
evolution of the 475 ◦ C embrittlement. The SPM analyses were con­
ducted in the rolling longitudinal direction of the as received and aged
T.J. Ávila Reis et al. Materials Science & Engineering A 810 (2021) 141028

Fig. 7. (a) AFM image, (b) MFM image and (c) enlarged image of the white square region in (b) from the AR-LDSS. Images before electrolytic polishing. Scale in
micrometers. Longitudinal section. α = ferrite; γ = austenite.

Fig. 8. (a) AFM image, (b) MFM image and (c) enlarged image of the white square region in (b) from the 100-HT-LDSS. Images before electrolytic polishing. Scale in
micrometers. Longitudinal section. α = ferrite; γ = austenite.

Fig. 9. (a) AFM image of the AR-LDSS; (b) enlarged image of the white square region in (a); (c) enlarged image of the white square region in (b). Images after
electrolytic polishing. Scale in micrometers. Longitudinal section. α = ferrite; γ = austenite.

samples in a DIMENSION 3000 DIGITAL/BRUKER microscope operating
in tapping mode for AFM analyses and lift mode (second pass) for MFM
analyses [93]. The used probe tips were MESP Sb (n) doped Si model
with Cr/Co coating for high-sensitivity and magnetic contrast. The SPM
analyzes aimed to distinguish the α and γ phases, due to topographic
differences (AFM) and magnetic behavior (MFM), remembering that
ferrite is ferromagnetic and austenite is paramagnetic.
Special attention was given to the preparation of samples for analysis
using the SPM technique. Two different procedures were considered:
mechanical polishing using an appropriate suspension and electrolytic
polishing.
The first procedure consisted of steps of mechanical grinding and
polishing up to 0,25 μm diamond paste, followed of 15 min of polishing
using an OP-S suspension. OP-S is an active colloidal silica polishing
suspension with a pH of 9.8 and a grain size of about 40 nm [94], which
remove material through both mechanical and chemical action. The
result is a topographically suitable surface for analysis, free, for
example, of strain-induced martensite.
During the grinding/polishing of the samples, a different response
may occur between the present phases in the steel, resulting in a dif­
ference in height between these phases in the analysis plane. This dif­
ference in height is proportional to the time spent polishing the samples.
Thus, all the samples were evaluated by AFM/MFM before the electro­
lytic polishing, to guarantee that the surfaces of all samples were similar.

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T.J. Ávila Reis et al.
Fig. 10. (a) AFM image of the 100-HT-LDSS; (b) enlarged image of the white square region in (a); (c) enlarged image of the white square region in (b). Images after
electrolytic polishing. Scale in micrometers. Longitudinal section. α = ferrite; γ = austenite.
Height measurements were made between ferrite and austenite, and
new samples were polished until the heights were considered to be
practically similar. In this condition, electrolytic polishing was executed
and SPM analyses were again performed.
The second procedure consisted of electrolytic polishing after the
OP-S polishing. Electrolytic polishing was performed with a 10% oxalic
acid solution diluted in distilled water, using a current density of 1 A/
cm2 and polishing time of 5s. This proposed method is based in two
facts. First, as it is known [88], the oxalic acid etches selectively the
regions with high Cr content. In this context, the increase of the fluc­
tuation of Cr in the ferritic phase due the spinodal decomposition in­
creases the sensibility of this phase to the electrolytic polishing. Second,
as the SPM techniques have high resolution in the surface normal di­
rection, it is possible to measure the differences of heights between
ferrite and austenite and distinguish heights fluctuations due the spi­
nodal decomposition. Then, to identify theses heights fluctuations be­
tween ferrite and austenite phase due the spinodal decomposition, 100
heights measures in samples of as received and in each aged condition
were made. These measures were later related with hardness and impact
toughness results.
To demonstrate the effects of the 475 ◦ C embrittlement in the me­
chanical properties of the studied LDSS, especially in shorter times of
aging, samples in the as received condition and in the aged conditions
were prepared. Mechanical tests were performed at room temperature in
atmospheric air, and included: hardness/microhardness, impact, tensile,
fracture toughness and fatigue tests. The specimens were always
removed from the sheets in such a way as to consider the mechanical
loading in the longitudinal (L) direction (rolling direction).
Vickers hardness (load of 62.5kgf) were carried out according to the
ASTM E92 standard [95] on a WOLPERT machine, taking 10 measures
in each sample, in order to obtain the general hardness of all conditions.
The microhardness of each phase was evaluated by Vickers microhard­
ness (load of 10gf), performed according to the ASTM E384 standard
[96] on an HXD 1000TM PANTEC microdurometer, taking 10 measures
in each phase (ferrite and austenite) of the samples. The applied load
was chosen according to the size of the indentation in relation to the
grain size of the material, thus ensuring that the measurement in one
phase would be minimally influenced by the adjacent grains in the other
phase.
Charpy V-notch impact tests were conducted according to the ASTM
E23 standard [97]. A JB-300AI/C Jinan Shidai Shijin Instruments ma­
chine with maximum impact absorption capacity of 300 J was used,
considering 5 notched bars of each condition (10 × 10 × 55 mm) in the
L-T plane orientation.
Tensile tests, fracture toughness tests and fatigue tests were executed
on a 100 kN MTS810 servo-hydraulic materials testing system interfaced
to a computer for machine control and data acquisition. Steel specimens
in the as received condition (AR-LDSS) and after being subjected to
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Materials Science & Engineering A 810 (2021) 141028
aging at 475 ◦ C for 25 h and 100 h (25-HT-LDSS and 100-HT-LDSS) were
considered for this mechanical characterization. These two particular
heat treatment conditions were chosen because, considering the possi­
bility of spinodal decomposition in short times, they could represent,
respectively, an intermediate and a final condition of aging.
Tensile tests were conducted according to the ASTM E8M standard
[98]. Three round specimens of each chosen condition with 6 mm of
diameter and 12 mm of gauge length were considered. The tests were
carried out under displacement control, at a rate of 2 mm/min. Engi­
neering stress-strain curves were plotted for each sample, and then an
average tensile curve was obtained for each condition using the Ori­
ginPro 9.0.0 (2013) software. The yield strength, the ultimate tensile
strength, the uniform strain, the strain after fracture and the area
reduction after fracture were evaluated.
Fracture toughness tests were performed according to the ASTM
E1820 standard [99], under displacement control, in order to elaborate
the J-R resistance curves to static cracking by the J-integral methodol­
ogy, that is, crack extension resistance J-integral as a function of stable
crack extension Δa. C(T) specimens in L-T orientation were used, with
10 mm thickness. A fatigue pre-cracking was obtained, maintaining a
relationship between the initial crack size and the width specimen (a/W)
of 0.50. Crack opening displacement measurements (COD) were used to
obtain the instantaneous crack size value using the compliance tech­
nique through a clip gage. Five specimens were tested for each one of the
chosen conditions, and then an average J-Δa curve was obtained for each
condition using the OriginPro 9.0.0 (2013) software. The thickness of the
specimens for these tests did not guarantee plane strain conditions, and
the resistance curves generated and the respective JQ values (J value
near the onset of stable crack growth, defined from the 0.2 mm offset
line) are a function of the thickness.
Force controlled constant amplitude axial fatigue tests (σ a x Nf) were
conducted according to the ASTM E466 standard [100], using specimens
with the same geometry as the tensile specimens. The specimens were
made with threaded heads, with a polished gauge length to guarantee a
constant surface quality, and with a gauge length two times its diameter
to minimize buckling. These tests were performed at six stress amplitude
levels for each chosen condition, always with a force ratio (minimum to
maximum force) R = − 1 at a frequency of 10 Hz. Maximum stresses
were applied in the elastic regime as well as in the plastic regime to give
a general idea of the behavior of the materials. The first level was 90% of
the tensile strength of the material, the other levels decreased by 10% for
each level.
Fatigue crack growth tests (da/dN x ΔK) were conducted according
to the ASTM E647 standard [101] on two C(T) compact specimens of
each chosen condition, with 10 mm thickness, in L-T orientation. These
tests were carried out in a loading range in the linear elastic regime of
the material to ensure the complete construction of the sigmoidal crack
growth curve, according to the validity of the tests by Fracture
T.J. Ávila Reis et al.
Fig. 11. (a) Effects of the aging time at 475 ◦ C in the hardness of the LDSS, (b)
increase in the depth of the dissolved ferrite together with its hardness and (c)
hardness increase in function of deep increase of ferrite dissolved, both in
function of the aging time.
Mechanics, always with a force ratio R = 0.1 at a frequency of 30 Hz and
sinusoidal wave. A fatigue pre-cracking was obtained, maintaining a
relationship between the initial crack size and the width specimen (a/W)
of 0.26. Crack opening displacement measurements (COD) were used to
obtain the instantaneous crack size value using the compliance tech­
nique through a clip gage. The fatigue threshold value ΔKTH was defined
as the stress intensity factor range at which the fatigue crack growth rate
reached 1 × 10− 7 mm/cycle. This value was estimated by a K-decreasing
procedure, limiting the normalized K-gradient to − 0.08 mm− 1. Crack
closure measurements were calculated close to the ΔKTH region, using
the compliance technique, when a change in linearity was formed in the
applied load versus COD curve. The parameter used to characterize the
crack closure was the KCL/Kmax relationship, where KCL represents the
value of the stress intensity factor relative to the crack closure load, and
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Materials Science & Engineering A 810 (2021) 141028
Kmax is the maximum stress intensity factor in the corresponding cycle.
The analysis of fracture surfaces by SEM was performed in repre­
sentative specimens after all mechanical tests to identify the fracture
mechanisms of the steel.
3. Results and discussion
3.1. Microstructural characterization
Fig. 1(a and b) illustrates the microstructure of the AR-LDSS, ob­
tained by LOM and SEM in the longitudinal section (rolling direction).
The microstructure of the steel consists of austenite islands embedded in
the ferrite matrix. Low carbon duplex steels solidify in a ferritic struc­
ture, while austenite forms in the solid state from precipitation at α/α
grain boundaries and grows with Widmanstätten morphology into the
interior of the grains. The elongated and flattened appearance of the
grains (mechanical fibering) with alternating ferrite and austenite
lamellae (banding) is a consequence of the steel manufacture process by
hot rolling. The fact that the α/γ interface energy is lower than the α/α
and γ/γ grain boundary energies induces the formation of that typical
lamellar microstructure. The lamellar structure is common among
duplex stainless steels [1,2], and will confer an anisotropic behavior to
the material.
Image analysis using the QWIN software indicated that the ferrite and
austenite volume fractions are 57% and 43%, respectively. This rela­
tively balanced distribution between the two phases is interesting
because, since ferrite is the phase where spinodal decomposition takes
place, its presence in a larger volume fraction could cause greater
embrittlement of the stainless steel. As expected, the phases volume
fraction and their geometric aspect were not altered by aging at 475 ◦ C.
Fig. 2(a and b) shows images obtained through SPM from the AR-
LDSS sample. This sample was prepared using only the OP-S suspen­
sion, without electrolytic polishing. Fig. 2(a) presents a topographic
image of the steel microstructure obtained by the AFM technique, while
Fig. 2(b) shows the same region with the respective magnetic contrast
image obtained by the MFM technique. The use of the AFM technique
confirmed the presence of the two phases in the steel and showed that
there is a difference in height between the phases, but without identi­
fying these phases. The abrasive effect of suspension particles in the OP-
S solution produces a surface with different topographic levels
depending on the phase on the surface. The MFM technique identified
the two phases through the difference in magnetism [75–77]. A precise
distinction between the phases is possible by analyzing Fig. 2(b), which
shows the variation of the magnetic domains of the surface illustrated in
Fig. 2(a). The γ phase is paramagnetic and therefore does not interact
with the probe during MFM analysis. Consequently, light regions with
no variation in tonality are visible in Fig. 2(b). The α phase is ferro­
magnetic, the result of the analysis by MFM corresponding to the regions
of this phase shows high interaction with the probe, decreasing or
increasing its original oscillation frequency. The MFM image corre­
sponding to the α phase regions shows waves with an aspect similar to
that of a “labyrinth” with variations in light and dark color tones due to
the change in the direction of the magnetic domain in this region. Once
this procedure was carried out, it was possible to verify that the ferrite
phase is topographically higher than the austenite phase.
An analysis by SPM in all aged samples subjected to mechanical
polishing (OP–S suspension) showed that the α phase was always
topographically higher compared to the γ phase, regardless of the degree
of aging. These results indicated that the α phase is more resistant to
mechanical polishing than the γ phase and that this behavior apparently
has no relation to the aging time. Thus, before completing its prepara­
tion with electrolytic polishing, all samples were mechanically polished
several times, until the difference in heights between the present phases
was considered satisfactory to guarantee topographic similarity.
The height differences between the α and γ phases after the first
sample preparation showed a significant scatter of results, as shown in
T.J. Ávila Reis et al.
Fig. 12. (a) Effects of the aging time at 475 ◦ C in the microhardness of the both phases and indentation size comparison of α and γ phases in (b) AR-LDSS and (c) 100-
HT-LDSS samples.
Fig. 3(a). The relative height between the α and γ phases varied from 60
to 110 nm. That is, in some samples the height between the α and γ
phases is almost twice as high as the same height in other samples. This
height variation could make it impossible to analyze the results after
electrolytic polishing. For this reason, the samples were again prepared,
performing individual monitoring until the relative heights between the
phases showed greater similarity. The use of this procedure allowed the
preparation of the samples for the electrolytic etching in such a way that
the maximum variation in the relative heights between the α and γ
phases was 15 nm. These results are illustrated in Fig. 3(b).
Fig. 4(a–h) shows the SPM images of the AR-LDSS sample and some
representative X-HT-LDSS samples, after adjusting the mechanical pol­
ishing time. Comparing the topographic images, all samples have a
similar visual appearance after polishing with the OP-S suspension.
The AFM 3D-images from the samples of the AR-LDSS and 1, 6, 12,
25, 50 and 100-HT-LDSS after the electrolytic polishing are showed in
Fig. 5(a–g). This sequence of figures confirms the change in chemical
behavior of the two phases (austenite always with the presence of twin
boundaries inside its grains) as a function of the heat treatment time.
Ferrite loses its resistance to etching, while austenite remains un­
changed, these facts being evidenced by the change in topography be­
tween the two phases and their color tones (ferrite is lighter in the as
received condition, becoming darker for longer aging times).
It was observed that the change of the heights between phases (depth
difference between α and γ) fit into an inverse relationship when plotted
with the aging time, as show in Fig. 6(a). After the electrolytic polishing
the relative heights between ferrite and austenite have increased in the
9
Materials Science & Engineering A 810 (2021) 141028
AR-LDSS and 1-HT-LDSS samples (α – γ > 0) if compared with the results
before the electrolytic polishing. The ferrite phase is more resistant than
austenite to dissolution by acid oxalic in the as received condition and
the height average value between these phases was 310 nm in AR-LDSS.
On the other hand, only 1 h of aging at 475 ◦ C was enough to reduce the
ferrite dissolution resistance, decreasing the height mean value between
these phases to 146 nm. With the increase of the aging time the ferrite
dissolution resistance decreased and after 6 h of heat treatment this
phase became less resistant than austenite (α – γ < 0). The decreasing of
the ferrite dissolution resistance was more pronounced until 25 h of
aging remaining almost equal after 50 h and decreasing a little more
after 100 h of aging. Considering that austenite does not undergoes
changing due the aging and its behavior will be the same during elec­
trolytic polishing, it is also possible to fit the increase of the dissolved
ferrite deep as a function of aging time. These results are show in Fig. 6
(b). A direct relationship between the depth of the dissolved ferrite layer
and the aging time can be seen in this figure.
As mentioned in section 2 of this work, the sensibility of the ferrite
phase to electrolytic polishing in oxalic acid is a function of Cr con­
centration [88]. Therefore, it is reasonable to affirm that the fluctuation
of heights measured in the images of AFM analyses, Fig. 5(a–g), is
directly related with the continuous increase of Cr concentration in the
α’ phase due the aging time [76,77]. The topographic fluctuations occur
because in the condition as received the α phase has a higher Cr con­
centration than the γ phase, being homogeneously distributed. After
aging, with spinodal decomposition, the Cr concentration in the α phase
fluctuates such that the depleted Cr regions allow greater dissolution of
T.J. Ávila Reis et al. Materials Science & Engineering A 810 (2021) 141028

Fig. 13. (a) Effects of the aging time at 475 ◦ C in the impact absorbed energy of
the LDSS, (b) relative heights between ferrite and austenite together with
toughness and (c) impact absorbed energy in function of relative heights, both
in function of the aging time.

this phase by the electrolytic polishing compared to the γ phase. The

measured heights are an indirect way to follow separately the two
phenomena that occur during the spinodal decomposition, that are the
increase in the magnitude of Cr concentration and the coarsening of the
modulated structure. This fact explains the fast change in the heights
Fig. 14. (a) Macrofractographies of all impact specimens (codes according to
between ferrite and austenite during the first hours of aging until
the standard adopted in section 2) and SEM microfractographies of represen­
approximately 25 h. There was no significant change in the heights with
tative impact specimens: (b) AR-LDSS. (c) 100-HT-LDSS. The white arrow in­
aging times greater than 25 h because the fluctuation of Cr content
dicates the direction of the fracture.
achieved its maximum value and the coarsening of the modulated
structure do not affect the ferrite phase sensibility to the electrolytic
behavior of the α phase in duplex stainless steels. According to Gheno
polishing.
et al. [77], this change is related to changes in both the size and shape of
In the same way that a change in the mechanical properties of the α
the magnetic domains structure of the α phase, and can be identified by
phase is expected with the occurrence of spinodal decomposition, the
MFM analysis. Fig. 7(a–c) and Fig. 8(a–c) illustrate images by AFM and
precipitation of the α′ phase may imply a change in the magnetic

10
T.J. Ávila Reis et al.
Table 2
Mechanical properties at room temperature.
HVα HVγ HV YS (MPa) UTS (MPa) UE (%)
AR-LDSS 237 265 250 533 708 32
25-HT-LDSS 330 265 323 677 903 16
100-HT-LDSS 350 265 346 702 955 15
Hardness tests – HV: Vickers hardness; HVα and HVγ: Vickers microhardness of α and γ phases.
Tensile tests - YS: Yield strength; UTS: Tensile strength; UE: uniform elongation; FE: Elongation after fracture.
Toughness tests – AE: impact absorbed energy; JQ: critical J-integral.
Fatigue tests - σf: fatigue endurance; ΔKTH: fatigue threshold; KCL/Kmax: crack closure ratio.
Fig. 15. Engineering stress-strain curves (average of three tensile tests for
each condition).
MFM of the AR-LDSS and the 100-HT-LDSS, respectively, and confirms
this statement. Magnifications of the magnetic domains illustrated in
Figs. 7(c) and 8(c) were made in regions where their undulations were
very clear. The direction of the magnetic domains is perpendicular to the
sample surface in these directions. When the magnetic domains are
oriented in this way, abrupt changes are observed in the interaction
between the probe and the sample, producing images with enough
definition of the change in direction of the magnetic domains. It was
observed that the undulations of the magnetic domains in the sample
aged at 475 ◦ C are thinner than the same undulations in the regions
analyzed in the AR-LDSS sample. This morphology change indicates the
precipitation of α’ phase in α phase of duplex stainless steels [77].
A final application of the SPM technique can be seen in Fig. 9(a–c)
and Fig. 10(a–c) for the AR-LDSS and 100-HT-LDSS samples, respec­
tively, after electrolytic polishing and with different levels of magnifi­
cation. Here it should be remembered that ferrite is more resistant to
etching in the AR-LDSS sample, while austenite is more resistant to
etching in the 100-HT-LDSS sample. Figs. 9(c) and 10(c) characterize the
ferrite with a relatively high magnification (approximately 32,000X). In
the case of the AR-LDSS sample, the surface has little topographic
variation: although some black corrosion spots are observed, there is no
significant variation in the color tones of the image, so it can be said that
this surface is practically flat. In the 100-HT-LDSS sample, on the other
hand, a surface with a very irregular topography is observed. The sharp
fluctuation in the color tones from one region to another in this image
indicates its topographical irregularity. This topographic variation is
related to the distribution of the α′ precipitates. It can be considered then
that the topographically higher regions would be those in which the
concentration of α′ precipitates is greater. The topographically lower
regions, on the other hand, would be those in which the concentration of
α’ precipitates is lower and, for this reason, is more sensitive to disso­
lution in the electrolytic etching. All these results are interesting because
they show the versatility of the SPM technique to confirm the presence
11
Materials Science & Engineering A 810 (2021) 141028
FE (%) AE (J) JQ (kJ/m2) σf (MPa) ΔKTH (MPa.m1/2) KCL/Kmax
57 174 1178 284 5.0 0.31
45 94 494 356 7.2 0,70
41 64 278 383 8.7 0.74
of spinodal decomposition in duplex stainless steels, with sample prep­
aration and image interpretation simpler than traditional transmission
electron microscopy techniques.
3.2. Relationship between microstructure and hardness-impact tests
The relationship between microstructural evolution and the respec­
tive change in mechanical properties of the duplex stainless steel during
the aging treatment can be easily demonstrated by means of Vickers
hardness and Charpy impact tests. In this analysis, the measurement of
the topographic variation between the two phases using the SPM tech­
nique and the results obtained in the hardness and impact tests are
considered for all aged samples. The dependence of hardness and
absorbed energy by impact with the aging time of the steel and the
respective relationships with the microstructural observations verified
by means of the SPM technique are strong evidence that the LDSS ferrite
studied underwent a two-phase decomposition, Fe-rich ferrite (α) and
Cr-rich ferrite (α’), and that the transformation mechanism was spinodal
decomposition.
Fig. 11(a–c) illustrates the variation in Vickers hardness (load =
62.5kgf) of the studied stainless steel with the aging treatment. In Fig. 11
(a) it is possible to observe a significant increase in hardness in the first
hours of the heat treatment, with a tendency to saturation after about 50
h. Similar results are reported by several researchers [3,7,14,15,18,30,
31,35,38,72,83–85,88], who indicate spinodal decomposition as
responsible for this behavior. Using the depth variation of the dissolved
ferrite grains (see Fig. 6(b)) as a parameter for analyzing the evolution of
spinodal decomposition, Fig. 11(b and c) show the effect of the micro­
structure on the hardness (hardness variation in relation to the AR-LDSS
sample) of the heat treated steel. The direct relationship between these
quantities is evident, with well-adjust trend curves. These results are
showing the dependence on the mechanical behavior of the LDSS with
the evolution of spinodal decomposition. In addition, in the specific case
of Fig. 11(c), the successful use of the SPM technique is confirmed for
monitoring spinodal decomposition.
When the microhardness (load of 10gf) of each phase is evaluated
separately, it can be seen that ferrite behaves with an identical tendency
to the global behavior of the steel, and that the austenite is not affected
by the heat treatment. Fig. 12(a) presents these results. Fig. 12(b and c)
illustrates the indentations performed in the α and γ phases of the AR-
LDSS and 100-HT-LDSS samples. While for the sample in the as
received condition the difference in indentation is small (11%), in the
case of the aged sample this difference is easily noted (32%). Similar
behavior has also been observed by other researchers [14,18,30,38,87]
and represents further evidence of the evolution of spinodal decompo­
sition that occurred in ferrite.
Fig. 13(a–c) illustrates the variation of the impact absorbed energy of
the studied steel as a function of the aging treatment. In Fig. 13(a) it is
possible to observe, contrary to the variation in the hardness of the
material, a significant decrease in the impact toughness with the aging
time. In this case, it can also be seen that the effect of aging occurs in the
first hours of the heat treatment, with a tendency to saturation after
about 50 h. Similar results are also reported by several researchers [14,
15,19,21,30,34–38,64,69,72,85,87,88], who reinforce spinodal
T.J. Ávila Reis et al. Materials Science & Engineering A 810 (2021) 141028

Fig. 17. (a) J-R curves (average of five fracture toughness tests for each con­
dition). (b) Fracture toughness JC versus impact absorbed energy AE. (c)
Fracture toughness Jc versus tensile strength UTS.

decomposition as responsible for this behavior. In this way, the hard­

Fig. 16. SEM microfractographies of the central area of representative tensile
specimens: (a) AR-LDSS; (b) 25-HT-LDSS; (c) 100-HT-LDSS.
ening of ferrite grains by the α’ phase precipitation and the consequent
tendency for these grains to present cleavage fracture in weak {100}
type planes are the mechanisms responsible for the pronounced drop in
fracture toughness of the aged steel. Using the relative heights between
ferrite and austenite grains (see Fig. 6(a)) as a parameter for analyzing
the evolution of spinodal decomposition, Fig. 13(b and c) show the
relationship between microstructure evolution and impact toughness of
the heat treated steel. The correlation between these quantities is again
evident, with well-adjust trend curves. These results are again showing

12
T.J. Ávila Reis et al. Materials Science & Engineering A 810 (2021) 141028

Fig. 18. SEM microfractographies of representative fracture toughness specimens: (a, b) AR-LDSS; (c, d) 25-HT-LDSS; (e, f) 100-HT-LDSS. (b), (d) and (f) are
magnifications of the regions marked with a dashed circle in (a), (c) and (e). The dashed lines indicate the separation between the fatigue precrack and tensile tear
regions. The white arrows indicate the direction of crack growth.

the dependence on the mechanical behavior of the LDSS with the evo­
lution of spinodal decomposition. Once again, in the specific case of
Fig. 13(c), the successful use of the SPM technique is confirmed for
monitoring spinodal decomposition.
It is interesting to comment that researchers [14,15,30,64,69] found
an impact absorbed energy for some DSS grades much lower than the
values found in the present work, under the same aging conditions
performed here (sometimes less than 10 J). The lower concentration of
alloying elements of the studied LDSS here decreases the decomposition
kinetics of the α phase, leading to less aggressive results. This is an
advantage of LDSS over conventional DSS.
Fig. 14(a) shows the macrofratography of all impact samples. In this
Figure, the codes are in accordance with the standard described in
section 2: AR = as received condition; X-HT indicating the aging time (X
in hours). There is a decrease in the lateral expansion of the specimens
and an increase in the number of separations with an increase in the

13
T.J. Ávila Reis et al.
Fig. 19. (a) Force controlled fatigue σmax x Nf plot. Three specimens were used
for each load level. The points corresponding to Nf = 107 cycles are run-outs (no
fracture). (b) Fatigue endurance limit σf (Nf = 107 cycles) versus tensile
strength UTS.
aging time. The fracture mechanism is altered, as can be seen in Fig. 14
(b, c) for AR-LDSS and 100-HT-LDSS samples, respectively. While the as-
received sample shows a ductile behavior, with the traditional presence
of dimples, the aged sample changes its behavior to brittle, with almost
the entire fracture showing cleavage facets. These characteristics are
directly related to the decrease in the impact toughness of the aged
material, and were also found in the references cited above.
The existence of separations (also known as split-out or delamination)
on fracture surfaces of impact samples, Fig. 14(a), refers to a sudden
instability which takes place near the crack tip and the appearance of
additional cracks in the remaining ligament, perpendicular to the pri­
mary fracture plane. This phenomenon is related to stress triaxiality in
the front of the crack tip when the structure is under plane strain con­
ditions, plus the existence of weak interfaces oriented normal to the
thickness direction. In rolled steels, the mechanisms of cracks initiation
depend on the chemical composition, microstructure and, mainly, on the
conditions of hot rolling. The possible causes (isolated or combined) that
induce this type of cracks are [102–115]: presence of elongated in­
clusions, intergranular failure due to segregation of impurities at grain
boundaries or the central position of the rolled plate, banded micro­
structure along the rolling direction, existence of a crystallographic
texture. In the present work, the existence of separations in front of the
notch of all impact samples is due to the lamellar austenite/ferrite
microstructure in the rolling direction of the studied LDSS (mechanical
fibering, banded structure) and also due to the difference in mechanical
behavior of the present phases. It is important to highlight that the direct
dependence between the number of separations with the aging time is
due to the evolution of the spinodal decomposition in the ferrite grains,
the increase in the mechanical resistance of the ferritic phase and the
14
Materials Science & Engineering A 810 (2021) 141028
Fig. 20. SEM microfractographies of representative force controlled fatigue
specimens of the AR-LDSS condition, (a) low cycle fatigue, σmax ≅ 640 MPa; (b)
high cycle fatigue, σmax ≅ 350 MPa. The white arrows indicate the fatigue crack
nucleation and its growth direction. The dashed line indicates the separation
between the fatigue and tensile tear regions.
increase in the difference in mechanical resistance between the present
phases.
3.3. Mechanical properties of selected conditions
The main properties obtained in the mechanical tests performed in
this work are summarized in Table 2 for the AR-LDSS, 25-HT-LDSS and
100-HT-LDSS samples. The two particular heat treatment conditions
were chosen for the mechanical characterization of steel considering
that, as can be seen in the results presented in Figs. 11 and 13, the
sample aged for 25 h and the sample aged for 100 h represent, respec­
tively, an intermediate situation and the saturation for spinodal
decomposition. The following text deals with results obtained in the
tensile, fracture toughness and fatigue tests. In these analyzes, only the
formation of the α’ phase with the aging time is being considered,
without considering the possibility of precipitation of the G phase in the
LDSS, due to its chemical composition and the aging times [36,81,84,
85].
Fig. 15 shows the engineering stress-strain curves (averages of three
tests for each situation) obtained in the tensile tests. It is possible to see
that the evolution of LDSS aging causes a decrease in its ductility (28%
T.J. Ávila Reis et al.
Fig. 21. (a) Fatigue crack growth da/dN x ΔK plot. Two specimens were used
for each condition. The points corresponding to the region near da/dN =
10− 7mm/cycle were used to estimate the threshold ΔKTH. (b) Fatigue threshold
ΔKTH versus tensile strength UTS.
reduction between AR and 100-HT conditions) and an increase in its
mechanical strength (35% gain between AR and 100-HT conditions).
This behavior is due to the manifestation of spinodal decomposition, as
also found in other researches [3,15,17,18,30,31,38,72,83]. According
to Chandra et alli [15] and Weng et alli [30], as aging time increases,
dislocations are increasingly pinned in the complex interconnected and
modulated structure between the α and α’ phases, thereby lowering the
mobility of the dislocations. This dislocation pinning behavior results in
an increase in mechanical strength and a decrease in ductility of the
material. Another interesting result that can be seen in Fig. 15 is the
behavior similarity between the 25-HT-LDSS and 100-HT-LDSS samples,
confirming the tendency for saturation of spinodal decomposition after a
certain aging time. As suggested by Schwarm et alli [38], the fluctua­
tions of Cr and Fe initially create a very fine structure, and the me­
chanical properties change rapidly in the first hours of aging. However,
this complex structure grows over time, reducing barriers to the dislo­
cations movement and decelerating the change in mechanical
properties.
The fracture mechanism in all tensile samples was ductile, with
nucleation, growth and coalescence of microcavities and formation of
dimples, as can be seen in Fig. 16(a–c). These samples showed some
separations in the central part of the fracture surfaces, the explanation
being the same as that already presented in the discussion of the impact
15
Materials Science & Engineering A 810 (2021) 141028
tests, section 3.2. It is also possible to observe that the dimples decrease
in size when the as received sample is compared with the aged samples,
a characteristic that shows the decrease in the ductility of the material
with the heat treatment. The microcavities are nucleated heteroge­
neously at sites where compatibility of deformation is difficult, for
example: dislocation pile-ups, holes and particles, grain boundaries,
distribution of different phases. The size of the dimples on a fracture
surface is governed by the number and distribution of microcavities that
are nucleated. When the nucleation sites are few and widely spaced, the
microcavities grow to a large size before coalescing and the result is a
fracture surface that contains large dimples. Small dimples are formed
when numerous nucleating sites are activated and adjacent micro­
cavities join (coalesce) before they have an opportunity to grow to a
larger size [116–121]. In the specific case of this work, aging causes an
increase in the formation of microcavities in the ferrite grains, either by
dislocations pile-ups in the complex structure between the α and α’
phases, but also by the difference in mechanical behavior between the
ferrite and austenite grains. As previously mentioned, the increase in the
amount of microcavities nucleating sites in the ferrite grains resulted in
a decrease in the size of the dimples in the fracture surface of the aged
samples. The propensity for coalescence of microcavities at the expense
of their growth implied a rapid formation and propagation of the central
crack (that is, the crack that induces fracture) of the tensile samples,
with a consequent decrease in the ductility of the material.
Fig. 17(a–c) presents the results of fracture toughness (J-integral
methodology) obtained in this research. Fig. 17(a) shows the J-R resis­
tance curves, where dashed curves are adjustments in the form of a
power law (J = C(Δa)n). The curves are averages of five fracture
toughness tests for each condition. The JQ fracture toughness value (the
critical value of the J-integral for the beginning of stable crack growth) is
shown in Table 2 for the three analyzed conditions, and its variations
with the impact absorbed energy and with the tensile mechanical
strength are shown in Fig. 17(b and c), respectively. In the same way
already found by impact tests, fracture toughness decreases as the aging
time increases. There is a 76% JQ reduction between AR and 100-HT
conditions. There are few studies in the literature [5,19,21,25–28]
characterizing the fracture toughness of DSS by fracture mechanics
(research focuses on evaluating toughness by impact tests), and none of
them deals with LDSS. These authors also credit the loss of fracture
toughness in aging with spinodal decomposition. However, it should be
noted that the JQ values in the present study are still higher than those
reported in the literature for other DSS grades (with higher Cr, Ni and
Mo additions). This conclusion is interesting, because it shows again an
advantage of using LDSS. The direct relationship between JQ and the
impact absorbed energy is found in the works of Chopra and Chung [5,
19,21] on aged DSS for application in the nuclear sector. The inverse
relationship between fracture toughness and tensile strength is not
surprising, as it is a trend seen by all metal alloys, related to the mate­
rial’s inability to develop a plastic zone that shields the crack tip
[122–134]. The proximity of JQ values between the 25-HT-LDSS and
100-HT-LDSS samples should also be highlighted, reinforcing the trend
of the steel aging saturation.
Fig. 18(a–f) shows the surface of fracture toughness specimens.
These regions represent approximately the moment when the crack
changes from a blunted tip to the beginning of its stable growth. The
fracture mechanism is similar to the impact test samples, confirming the
effect of aging. In the case of the AR-LDSS, sample stable crack extension
takes place by a typical microvoid nucleation, growth, and coalescence
mechanism, and also some separations. The aged samples had a change
in the fracture mechanism to predominantly cleavage, with an increase
in the number of separations. These changes in the fracture mechanism
reflect the evolution of spinodal decomposition. The explanation for
these separations is the same as that already presented in the discussion
of impact tests, section 3.2.
Fig. 19(a and b) presents the fatigue results under force control ob­
tained in this work. Fig. 19(a) shows the graph of the maximum stress
T.J. Ávila Reis et al.
Fig. 22. SEM microfractographies of representative fatigue crack growth specimens near the threshold region, da/dN = 10− 7mm/cycle: (a) AR-LDSS; (b) 25-HT-
LDSS; (c) 100-HT-LDSS. The white arrows indicate the direction of crack growth.
σ max as a function of the number of cycles to fracture Nf, both in loga­
rithmic scale to linearize this relationship, while Fig. 19(b) shows the
relationship between the fatigue limit σf and the tensile strength σ UTS of
the stainless steel. For this type of fatigue test, it is very interesting to
note that the evolution of the spinodal decomposition provides greater
resistance to initiation and growth of fatigue crack (35% gain between
AR and 100-HT conditions at the high cycle fatigue region). This result
may seem surprising, since it is indicating that the α’ phase present in the
ferrite would not be a deleterious phase for the fatigue resistance.
However, several authors [3,43–47,58–64,66–69,71] have demon­
strated that the aged DSS may, in fact, have a greater resistance to
nucleation and crack propagation than the unaged material, especially
in the high cycle fatigue region. The ferrite and austenite phases behave
in a similar way when the steel is unaged, and crack nucleation occurs
from slip bands in both phases. When the steel is aged, fatigue cracks
develop preferentially in austenite (softer phase), but are blocked at the
α/γ interfaces due to the difficulty they experience when trying to
advance to the hardened ferrite. In addition, the deformation mecha­
nism changes in the hardened ferrite, when twinning starts to operate
and also serves as an obstruction to the crack propagation. The prox­
imity of σ max versus Nf lines and the σ f values between the 25-HT-LDSS
and 100-HT-LDSS samples should also be highlighted, again reinforcing
the trend of the steel aging saturation.
16
Materials Science & Engineering A 810 (2021) 141028
Fig. 20(a and b) illustrates the fracture surface of two samples of AR-
LDSS, fatigued at loading levels to have a representation of the low cycle
(σmax ≅ 640 MPa) and high cycle (σmax ≅ 350 MPa) regions, respec­
tively. It is possible to observe the crack nucleation on the surface of the
samples in both conditions, with the only difference that loading in the
plastic region (low cycle) induced a smaller area of fatigue crack growth,
while loading in the elastic region (high cycle) showed a larger area. The
aged and fatigued samples in the low cycle region had a fracture surface
similar to that shown in Fig. 20(a). The fatigued samples chosen in the
high cycle region did not present fatigue fracture.
Fig. 21(a and b) presents the results of fatigue crack growth obtained
in this research by the methodology of fracture mechanics. Fig. 21(a)
shows the graph of the crack growth rate da/dN as a function of the
cyclic stress intensity factor ΔK, both in logarithmic scale to generate the
traditional sigmoidal curves with the three distinct regions of fatigue
behavior, while Fig. 21(b) shows the relationship between the threshold
ΔKTH and the tensile strength of the stainless steel. Considering only the
crack growth from pre-cracked specimens, the evolution of the spinodal
decomposition made the LDSS more resistant to fatigue. This result,
together with the direct dependence between the ΔKTH threshold and the
tensile strength, are surprising conclusions, as apparently a material
with less ability to plastic deformation should present a lesser crack
propagation shield. However, as commented by some researchers [42,
T.J. Ávila Reis et al.
45,47–49,57,65,70,89,90], this apparently unusual behavior is also
related to the difference in the mechanism of crack growth in the ferrite
and austenite phases. The more ductile austenite and the hardened
α′ phase create a more pronounced roughness/tortuosity in front of the
crack, intensifying the crack closure phenomenon and guaranteeing a
better performance for the aged steel. The difference in rough­
ness/tortuosity can be seen on the fracture surfaces corresponding to the
ΔKTH threshold region, as shown in Fig. 22(a–c). The consequent vari­
ation in crack closure with the aging of steel is shown in Table 2 through
the KCL/Kmax ratio: an increase of 138% is verified between the condi­
tions AR and 100-HT. The same effect of roughness-induced crack
closure on fatigue crack growth and its dependence on microstructural
parameters in region I have been verified for several other steel grades
[132–140].
4. Conclusions
In this research, the effects of an isothermal treatment at 475 ◦ C for
times between 1 h and 100 h on the microstructure and mechanical
properties of a UNS S32304 lean duplex stainless steel (ferrite +
austenite) were investigated. The main conclusions are listed below.
1. The aging treatment caused the evolution of spinodal decomposition
in the studied steel, with the precipitation of the α′ phase in the α
phase, as with other duplex stainless steel grades. This phase trans­
formation was effectively monitored by the Scanning Probe Micro­
scopy (SPM) technique, in the Atomic Force Microscopy (AFM) and
Magnetic Force Microscopy (MFM) modalities, through relatively
simple sample preparation and topographic analysis of chemically
etched surfaces. Through this microscopic technique, it was possible
to observe that spinodal decomposition occurs intensely in the first
hours of aging, and tends to saturate after approximately 25 h. The
verified effectiveness in the application of the SPM technique re­
inforces its practical use for determining the embrittlement degree of
stainless steels subjected to aging.
2. Through the microhardness test, it was possible to verify that the
presence of the α′ phase caused significant hardening of the ferrite,
keeping unchanged the austenite behavior. The hardening curve of
the ferrite also indicated a marked variation for the first aging hours,
with a tendency to saturation after 25 h.
3. The mechanical tensile strength and hardness of steel increased with
the evolution of aging, while ductility and impact resistance
decreased. These properties also indicated a tendency to saturation
after 25 h of aging. The tensile fracture mechanism was ductile in all
tested samples, but with a decrease in the size of the dimples as a
function of aging time. On the other hand, in the impact test, there
was a change in the fracture mechanism, from predominantly ductile
in the as-received condition to predominantly brittle after 100 h of
aging, with increased separations.
4. The fracture toughness, measured by the J-integral and by the
resistance curve, was lower for aged steel, compared to the as-
received condition, decreasing with increasing aging time and with
increasing mechanical tensile strength. A direct relationship was
verified between fracture toughness and impact absorbed energy,
and the same type of fracture mechanism already observed in impact
tests. Again, the tendency to saturation of the mechanical behavior
was noticed after 25 h of aging.
5. The resistance to fatigue cracking, as verified by load-controlled fa­
tigue tests and crack growth tests, was higher for aged steel
compared to the as-received condition, increasing with increasing
aging time and increasing of mechanical tensile strength. The crack
closure mechanism was detected in all tested samples, being more
pronounced for longer aging times. Once again, the tendency to
saturation was verified after 25 h of aging.
6. Thinking of a heat treatment at 475 ◦ C for the studied LDSS or some
application at this temperature, the crucial problem is its loss of
17
Materials Science & Engineering A 810 (2021) 141028
ductility (tensile tests) and fracture toughness (Charpy impact and J-
integral tests). Anyway, it should be noted that the reduction in these
properties was less than values found in the literature for other DSS
grades. Besides that, heat treatment around 25 h can already provide
interesting values of tensile and fatigue resistance for the LDSS.
CRediT authorship contribution statement
Thompson Júnior Ávila Reis: Conceptualization, Methodology,
Experimental procedures, Validation, Writing - original draft. Henrique
Meckler Santos: and Eliza Wilk Reis de Almeida: Investigation, Re­
sources, Formal analysis, Experimental procedures. Leonardo Barbosa
Godefroid: Conceptualization, Methodology, Data curation, Writing -
review & editing, Supervision, Funding acquisition.
Data availability
The data of the used material of this research can be checked from
Refs. [79,80]. The used methodology to reproduce the results can be
obtained from Refs. [91–101]. We don’t have a repository where the
data and results are stored.
Declaration of competing interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
Acknowledgements
The authors would like to thank APERAM South America Company
for supplying sheets of the lean duplex stainless steel employed in this
research, and CAPES (Coordenação de Aperfeiçoamento de Pessoal de
Nível Superior) for its financial support.
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