materials

Article
Influence of Electropulsing Treatments on Mechanical
Properties of UNS S32750 Duplex Stainless Steel
Claudio Gennari 1, * , Luca Pezzato 1 , Gianmarco Tarabotti 1 , Andrea Zambon 2 ,
Andrea Di Schino 3 and Irene Calliari 1
1 Department of Industrial Engineering, University of Padua, Via Marzolo 9, 35131 Padua, Italy;
luca.pezzato@unipd.it (L.P.); gianmarco.tarabotti@studenti.unipd.it (G.T.); irene.calliari@unipd.it (I.C.)
2 Department of Management and Engineering, University of Padua, Stradella S. Nicola 3,
36100 Vicenza, Italy; a.zambon@unipd.it
3 Department of Engineering, University of Perugia, Via G. Duranti 93, 06125 Perugia, Italy;
andrea.dischino@unipg.it
* Correspondence: claudio.gennari@phd.unipd.it; Tel.: +39-049-8275498




Received: 9 March 2020; Accepted: 25 March 2020; Published: 1 April 2020


Abstract: Prestrained at 5% and 15% duplex stainless steel UNS S32750 specimens have been subjected
to electropulsing treatments with current density of 100 A/mm2 and 200 A/mm2 and 100 and 500 pulses
for each current density value. Corrosion tests, X-ray diffraction, microhardness and residual stresses
were collected before and after the electropulsing treatments. Tensile tests were performed after
the electropulsing treatments in order to compare the mechanical response to reference tensile tests
performed before pulsing treatments. Increase in fracture strain was observed after pulsing treatment
in comparison to the reference tensile tests. A decrease in microhardness was also observed after
electropulsing treatments for both degrees of prestrain. Electropulsing treatment almost eliminates the
work-hardened state in the 5% prestrained specimens while partially recovered the 15% prestrained
material increasing both uniform and fracture strain. Bulk temperature of the samples remained the
same for all treatments duration. The effect are to be addressed to a combined effect of increase in
atomic flux due to the electrical current and local joule heating in correspondence of crystal defects.
Electropulsing treatment applied to metallic alloys is a promising technique to reduce the work
hardening state without the need of annealing treatments in a dedicated furnace.

Keywords: electroplastic effect; pulsed current; duplex stainless steel; electropulsing treatment;
tensile test

1. Introduction
Duplex stainless steels (DSSs) are a peculiar category of stainless steels characterized by their
biphasic microstructure consisting of almost equal volume fraction of austenite and ferrite. They are
employed in different applications, such as oil and gas, paper and pulp industry, the wine industry,
etc. [1–3]. Their mechanical and corrosion properties are higher compared to austenitic stainless steels,
on the other hand they suffer from secondary phase precipitation which causes embrittlement, poor
corrosion properties and limits their working temperature to 350 ◦ C [4–12].
A balanced microstructure consisting of equal amounts of austenite and ferrite is necessary in
order to obtain the best combination of mechanical and corrosion properties. This can be achieved
with a suitable composition and a solution treatment performed at a temperature that depends on the
steel composition (however higher than 1050 ◦ C). The solution treatment is also mandatory in order
to dissolve any possible detrimental secondary phases that might have precipitated during previous
forming processes and heat cycles [13]. Secondary phases in DSSs precipitate in a temperature range

Materials 2020, 13, 1613; doi:10.3390/ma13071613 www.mdpi.com/journal/materials

Materials 2020, 13, 1613 2 of 18

between 600 ◦ C and 1000 ◦ C. Spinodal decomposition of ferrite into high chromium content ferrite and
lower chromium content ferrite could take place at lower temperature (approximately 475 ◦ C) if the
soaking time is high enough because of the slow decomposition kinetic. In high alloyed DSSs, such as
UNS S32750 and UNS S32760, secondary phase precipitation takes place in a matter of minutes; it is
therefore necessary to limit their working temperature below 475 ◦ C and perform a solution treatment
after high temperature forming processes (hot rolling, forging etc.). Most common secondary phases
found in DSSs are χ phase, σ phase and chromium nitrides (i.e., CrN and Cr2 N) and the less common
π-phase, Laves phase, R-phase and carbides. The first phase to precipitate is χ phase due to its lower
coherency strain with the cubic lattice of ferrite even though σ phase is thermodynamically more
stable [5].
The effect of electrical current during plastic deformation of materials was discovered by Machlin
in 1959 [14]. The discovery of such phenomenon led to the development of new approaches to material
forming known as electrically assisted manufacturing (EAM) in which electrical current increases the
formability of various metallic alloy exploiting the electroplastic effect (EPE). The electroplastic effect
has shown to improve the formability on a wide variety of metallic materials such as aluminum [15–17],
titanium [18–20], magnesium [21–23], stainless steels [24,25] and on a variety of forming processes
as well. Some of the authors observed a relationship of the onset of EPE on FCC materials with
respect the stacking fault energy (SFE), which drives dislocation’s motion within the material [26].
Conversely to EAM, during electropulsing treatments (EPTs), electrical current is applied prior or after
deformation. EPTs have been shown to influence mechanical and microstructure properties of different
metallic alloys [27]. Ben et al. were able to rapidly harden AISI 4340 steel due to a combined effect of
dislocations, solid solution strengthening and nano twinned martensite thanks to EPT [28]. Guan and
Tang observed an evolution of the texture in cold rolled AZ31 magnesium alloy and a grain refinement
after EPT [29]. Xiang and Zhang dramatically reduced residual stresses on the surface and inside of as
quenched samples of a pipeline steel after electropulsing treatment [30]. Luu et al. were able to perform
rapid annealing on AISI 316L with a single current pulse in between two forming processes increasing
its formability [31]. Sànchez et al. were able to reduce the force and the backspring during bottom
bending process on aluminum and stainless steel [32]. Many theories have been developed in order
to identify the mechanisms that electrical current produces on the microstructure, but a unanimous
consensus has not yet been reached.
Some of the mechanisms induced by the electrical current are: electron wind force (transfer of
momentum of conducting electron to dislocations increasing their mobility) [33], magnetoplastic effect
or magnetoplasticity (depinning of dislocations from weak obstacles thanks to the induced magnetic
field) [34], electron stagnation theory (localized change in resistivity causes an increase of electron to
atom ratio, weakening the metallic bond and easing its breaking and restoration) [15], electromigration
(increase of ions diffusivity thanks to the electrical current ) [35], reduced Gibbs free energy during
phase transformation [36,37] and localized microscale Joule heating [38].
Investigations of the effect of both EAM and EPT on DSSs are still quite limited except for the work
carried out by some of the authors [24] and a scientific report on duplex steel by Rahnama et al. [39].
The aim of the present work is to examine the effect on the mechanical properties of electropulsing
treatments on a material that possesses two phases with different crystal structure, composition,
electrical resistivity, work hardening rate etc. The opportunity to perform EPTs between forming
processes and avoid heating the material in the secondary phases’ temperature stability regime could
aid to improve processing of these steel grades.

2. Materials and Methods

The material was supplied by the Italian division of Outokumpu S.p.A. in form of 2 mm thick
warm-rolled metal sheet. The composition of the investigated steel is reported in Table 1.
 Materials 2020, 13, 1613 3 of 18
Materials 2020, 13, x FOR PEER REVIEW 3 of 19

Steel grade C Si 1. Mn
Table ChemicalCr Ni of the
composition Moinvestigated
Cu W (wt%).
steel P S N
UNS
Steel Grade0.018 C 0.26 Si 0.84Mn 25.08
Cr 6.88
Ni 3.82
Mo 0.17
Cu - W 0.019 P 0.0010
S 0.294
N
S32750
UNS S32750 0.018 0.26 0.84 25.08 6.88 3.82 0.17 - 0.019 0.0010 0.294

Specimens for tensile tests were obtained along transverse direction with geometry according to
ASTMSpecimens
E8 standard except tests
for tensile for theweregauge length
obtained alongwhich was reduced
transverse direction towith
45 mm due toaccording
geometry the smallto
dimension of the metal
ASTM E8 standard exceptsheet.
for theSecondary
gauge length phase
whichidentification,
was reduced to phase
45 mm balance
due to quantification and
the small dimension
profile fitting sheet.
of the metal were conducted
Secondary through X-ray diffraction
phase identification, phase pattern
balance acquisition on a and
quantification Bruker D8 X-ray
profile fitting
diffractometer
were conducted (Bruker
through Corporation,
X-ray diffraction Billerica, MA,acquisition
pattern USA) equipped with Cu
on a Bruker D8 X-ray tube without
X-ray diffractometer
monochromator
(Bruker Corporation, on the detectorMA,
Billerica, side. Scanequipped
USA) steps of 0.02°
with and
Cu X-raycounting
tubetime of 5 monochromator
without s were used for X-ray
on the
diffraction
detector side. measurements.
Scan steps of 0.02 ◦
The evaluation
and counting of time
the of
volume
5 s were fraction
used forofX-ray
the constituting phases was
diffraction measurements.
performed
The evaluationthrough Rietveld
of the volume analysis
fraction on the as-received
of the material
constituting by means
phases of MAUDthrough
was performed © Software (Luca
Rietveld
Lutterotti, Trento, Italy). ©
analysis on the as-received material by means of MAUD Software (Luca Lutterotti, Trento, Italy).
Tensile
Tensiletests
testswere
were conducted
conducted at at aa strain
strain rate of 10−2 −2ss−1−1(TRIP
(TRIPeffect
effectwas
wasobserved
observedatatlower
lowerstrain
strain
rate)
rate)ononananMTS
MTS322 322tensile
tensiletest
testmachine
machine(MTS (MTSSystem
SystemCorporation,
Corporation,Eden EdenPrairie,
Prairie,MN,
MN,USA)
USA)capable
capable
ofofaamaximum
maximumforce forceofof50
50kNkNmodified
modifiedtotoperformperformelectroplasticity
electroplasticitytests.tests.Force
Forcewas
wasmeasured
measuredthrough
through
the
theload
loadcell
cellof
ofthe
theMTS
MTSwhile
whiledisplacement
displacementthrough throughthe thecrosshead
crossheadmovement.
movement.
AAself-designed
self-designedpowerpowersupplysupplycapable
capableofofdelivering
deliveringelectrical
electricalpulses
pulsesofofduration
durationofof110
110µsµsatat
maximum
maximum frequency of of5050HzHzand andup toup6 to
kA6werekA used
werefor used for the electropulsing
the electropulsing treatments.
treatments. The
The waveform
waveform of the current
of the electrical electricalis current
displayed is displayed
in Figure in 1. Figure 1. The temperature
The temperature of the specimens
of the specimens was
was collected
collected
through athrough
FLIR A40 a FLIR A40camera.
infrared infraredThe camera.
side ofThe
theside of thefacing
specimen specimen facing the
the infrared infrared
camera wascamera
painted
was
withpainted
a blackwith a black
opaque opaque
lacquer lacquer
in order in order
to obtain to obtain
a uniform a uniformdistribution.
emissivity emissivity distribution.

Figure 1. Waveform and duration of the typical electrical current pulse delivered by the power supply.
Figure 1. Waveform and duration of the typical electrical current pulse delivered by the power
Microhardness measurements were performed on a Leitz Miniload 2 (Leica Microsystem S.r.l.,
supply.
Milan, Italy) microhardness tester with 500 g load for the bulk hardness and 25 g load for the
individual phase. measurements were performed on a Leitz Miniload 2 (Leica Microsystem S.r.l.,
Microhardness
Milan,Residual stress measurements
Italy) microhardness were500
tester with performed by means
g load for the bulkof the “sin2 ψand
hardness method”. A dedicated
25 g load for the
X-ray diffractometer
individual phase. SpiderX (G.N.R. S.r.l., Agrate Conturbia, Novara, Italy), equipped with Cr tube
radiation, wasstress
Residual used measurements
to acquire the necessary X-ray pattern
were performed for both
by means the“sin
of the 2ψ method”.
ferritic and the austenitic phases
A dedicated X-
in the
ray rolling as well
diffractometer as the transverse
SpiderX direction.
(G.N.R. S.r.l., AgrateTo this end {222}
Conturbia, reflection
Novara, Italy),for ferritic phase
equipped with and {321}
Cr tube
reflection was
radiation, for austenitic phase have
used to acquire been chosen.
the necessary Thirteen
X-ray psifor
pattern angles
bothvarying between
the ferritic and the and +45◦
−45◦austenitic
phases in the rolling as well as the transverse direction. To this end {222} reflection for ferritic phase
and {321} reflection for austenitic phase have been chosen. Thirteen psi angles varying between −45°
Materials 2020, 13, 1613 4 of 18

with a counting
Materials timePEER
2020, 13, x FOR of 300 s were
REVIEW utilized. To compute the residual stresses, elastic constants values 4 of 19
for ferrite and austenite were utilized according to Johansson et al. paper [40].
and +45° with a counting
Potentiodynamic time of 300tests
polarization s werewere utilized. To compute
performed on antheAMEL residual2549stresses, elastic
potentiostat
constants values for ferrite and austenite were utilized according to
(Amel Electrochemistry, Milan, Italy) at a scanning rate of 0.5 mV/s in a 0.01 M NaCl solutionJohansson et al. paper [40].
withPotentiodynamic
a saturated calomel polarization
electrode astests wereelectrode
reference performed and on an AMEL
a platinum 2549 potentiostat
electrode (Amel
as counter electrode,
Electrochemistry, Milan, Italy) at a scanning rate of 0.5 mV/s in a
according to standard ASTM G3-14. The potentiodynamic polarization were performed in a potential 0.01 M NaCl solution with a
saturated calomel electrode as reference electrode and a platinum electrode
range between −0.8 V and 1.2 V, after stabilization of the open circuit voltage (OCP) for 30 min. Each test as counter electrode,
according
was repeatedto standard
three times ASTM G3-14.toThe
in order potentiodynamic
assure reproducibility. polarization were performed in a potential
rangeMicrostructural
between −0.8 V investigations
and 1.2 V, afterwere stabilization of the open
carried out through optical circuit microscopy
voltage (OCP) for 30
(Leica min. Each
DMRE, Leica
test was repeated
Microsystems three
S.r.l., times
Milan, in order
Italy) to assureelectron
and scanning reproducibility.
microscopy (Leica Cambridge Stereoscan LEO
440, Microstructural
Leica Microsystems investigations
S.r.l., Milan,were Italy)carried
operatingout through optical microscopy
in back scattered electron (BSE) (Leica
at 29DMRE, Leica
kV. Ordinary
Microsystems S.r.l., Milan, Italy) and scanning electron microscopy (Leica
metallographic preparation was carried out. To reveal the microstructure, electrolytic etching with Cambridge Stereoscan
LEO
NaOH 440,atLeica
3 V forMicrosystems
5 s was used.S.r.l., Milan, Italy) operating in back scattered electron (BSE) at 29 kV.
Ordinary
The specimens were preparation
metallographic divided intowas twocarried out. To reveal
main categories. Roomthe microstructure,
temperature tensileelectrolytic
tests were
etching with NaOH at 3 V for 5 s was used.
performed to obtain the reference mechanical properties, focusing on the uniform strain. Specimens
Thefirst
of the specimens
categorywere weredivided
strainedinto to two main the
5% while categories.
ones ofRoomcategorytemperature
number two tensile tests
were were
strained
performed to obtain the reference mechanical properties, focusing on
to 15%. After straining, residual stresses along the two directions and on the two phases, X-ray the uniform strain. Specimens
of the first category
diffraction were strained
measurements, corrosion to 5% while
tests, the ones of category
microhardness number
measurements andtwo were strained analysis
microstructural to 15%.
After
were straining,
conducted. residual stresses along
Three specimens per the two directions
category were thenand on theuntil
strained twofracture
phases, in X-ray
orderdiffraction
to have a
measurements, corrosion tests, microhardness measurements
reference for the specimens which were to be strained after electropulsing treatments. and microstructural analysis were
conducted. Three specimens
Each category per category
was then subdivided intowere
groups then strained on
depending until
the fracture
electricalin order to have a
parameters:
reference for the specimens which were to be strained after electropulsing treatments.
• EachGroup 1: 100 A/mm 2 100 pulses
category was then subdivided into groups depending on the electrical parameters:
2
• • 2:
Group 100 A/mm
Group 500 pulses
1: 100 A/mm 2 100 pulses

• • 3:
Group Group
200 A/mm 2
2: 100 A/mm
100 pulses2 500 pulses

• • 4:
Group Group
200 A/mm3: 2002 A/mm
500 pulses2 100 pulses

• Group 4: 200 A/mm2 500 pulses

As for theas
As for the as supplied
suppliedreference
reference material,
material,after
aftereach
each electropulsing
electropulsingtreatment,
treatment,residual
residualstresses
stresses
along the
along the two
two directions
directions and and on on the
the two two phases,
phases, X-ray
X-ray diffraction
diffraction measurements,
measurements, microhardness
microhardness
measurements and microstructural analysis
measurements and microstructural analysis were conducted. were conducted.
Subsequentlyspecimens
Subsequently specimensof ofthethetwotwocategories
categorieswerewerestrained
straineduntil
untilfracture
fractureandandcompared
comparedto tothe
the
referencetest
reference testof
ofeach
eachcategory.
category. A A schematic
schematic of of the
the experimental
experimental procedure
procedure is is showed
showed in in Figure
Figure 2.2.

Figure 2. Schematic of the experimental procedure.

Figure 2. Schematic of the experimental procedure.

3. Results

3.1. As-Received Material

Materials 2020, 13, 1613 5 of 18

3. Results
Materials 2020, 13, x FOR PEER REVIEW 5 of 19

3.1. As-Received
Materials 2020, 13, xMaterial
FOR PEER REVIEW 5 of 19
The as-received material showed a very well-balanced microstructure free of secondary phases,
which Thewas
The confirmedmaterial
as-received
as-received both byshowed
material X-ray diffraction
showed aa very patterns examination
very well-balanced
well-balanced (onlyfree
microstructure
microstructure peaks
free of of δ-ferrite phases,
of secondary
secondary and γ-
phases,
austenite
which was were visible)
confirmed and
both to
bySEM-BSE
X-ray investigations.
diffraction patterns examination (only peaks
which was confirmed both by X-ray diffraction patterns examination (only peaks of δ-ferrite and of δ-ferrite andγ-
Phase
γ-austenite balance
were was
visible) evaluated
and to through
SEM-BSE Rietveld analysis
investigations.
austenite were visible) and to SEM-BSE investigations. performed on the X-ray diffraction
pattern
Phaseof Figure
Phase balance
balance3 was
and
was resulted
evaluated in
evaluated almost
through equal
Rietveld
through volume
analysis
Rietveld fraction of austenite
performed
analysis on theon
performed and
theferrite
X-ray X-ray(0.48
diffraction ± 0.04
pattern
diffraction
and
of 0.52 ± 0.05 respectively).
pattern of Figure 3 and resulted in almost equal volume fraction of austenite and ferrite (0.48 ± and
Figure 3 and resulted in almost equal volume fraction of austenite and ferrite (0.48 ± 0.04 0.04
0.52 ± 0.05 respectively).
and 0.52 ± 0.05 respectively).

Figure 3. X-ray diffraction pattern of the as received material along rolling direction.
Figure 3. X-ray diffraction pattern of the as received material along rolling direction.
The as received
Figure 3.material is characterized
X-ray diffraction pattern of by
theaasmicrostructure
received material consisting of fragmented
along rolling direction. austenite
The as received material is characterized by a microstructure consisting of fragmented austenite
islands (bright grains) dispersed in a ferritic matrix (dark grains) as can be seen in Figure 4a. Rolling
islands
The(bright grains)material
ashighlighted
received dispersed in a ferritic matrix (dark grains) asconsisting
can be seen fragmented
in Figure 4a.austenite
Rolling
direction is by theisblack
characterized by a microstructure
arrow. Austenite morphology was quiteof fragmented due to the
direction
islands is highlighted by the black arrow. Austenite morphology was quite fragmented due to the
last pass(bright grains)process
of the rolling dispersedwhichin awas
ferritic matrix at
conducted (dark grains)
a lower as can be seen
temperature. in Figure 4a.
Microstructure Rolling
along the
last pass
direction of the rolling
is highlighted process
by the which
black was
arrow.conducted
Austenite at a lower
morphology temperature. Microstructure along
other dimensions (transversal and normal) is shown in Figure 4b. The was quite fragmented
interphase space (spacedue to the
between
the
lastother dimensions
pass and
of the rolling(transversal
process and was
which normal) is shown ainlower
conducted Figure 4b. The interphase space (space
austenite ferrite grain centres) was smaller along theatnormal temperature.
direction Microstructure
in comparison along
to that along
between
the otheraustenite
dimensions and (transversal
ferrite grain and
centres) was smaller
normal) is shown along
in the normal
Figure 4b. direction
The in comparison
interphase space to
(space
the rolling direction.
that alongaustenite
between the rolling direction.
and ferrite grain centres) was smaller along the normal direction in comparison to
that along the rolling direction.

Figure Microstructure of
4. Microstructure
Figure 4. of the
the as
as received
received materials:
materials: (a)
(a) along
along the
the rolling
rolling direction
direction (RD)
(RD) and
and (b)
(b) along
along
the main three directions (b). Etching solution NaOH at 3 V and
the main three directions (b). Etching solution NaOH at 3 V and 5 s. 5 s.
Figure 4. Microstructure of the as received materials: (a) along the rolling direction (RD) and (b) along
the main three directions (b). Etching solution NaOH at 3 V and 5 s.
3.2. Reference Tensile Tests
3.2. Reference Tensile Tests
 Materials 2020, 13, 1613 6 of 18
Materials 2020, 13, x FOR PEER REVIEW 6 of 19
Materials 2020, 13, x FOR PEER REVIEW 6 of 19
3.2.Tensile tests
Reference on the
Tensile as received material and on the specimens prestrained at 5% and 15% were
Tests
conducted in order
Tensile tothe
tests on have a reference
as received to compare
material thespecimens
and on the tensile behaviour of at
prestrained the5%electropulsed
and 15% were
Tensile tests on the as received material and on the specimens prestrained at 5% and 15% were
specimens
conducted after
in EPTs
order(Figure
to have5). a reference to compare the tensile behaviour of the electropulsed
conducted in order to have a reference to compare the tensile behaviour of the electropulsed specimens
specimens after EPTs (Figure 5).
after EPTs (Figure 5).

Figure
Figure5. 5.
True
Truestress-strain curves
stress-strain of of
curves thethe
as as
received material
received and
material thethe
and two categories
two of of
categories specimens
specimens
prestrained
Figure 5. at 5%
True and 15%.
stress-strain
prestrained at 5% and 15%. curves of the as received material and the two categories of specimens
prestrained at 5% and 15%.
AsAsthethe
prestrain
prestrainamount
amount increased
increased lower
lower values of of
values fracture and
fracture uniform
and uniform strain were
strain wereobserved,
observed,
while yield
whileAsyieldstress (YS)
the stress
prestrainand ultimate
(YS)amount tensile
increased
and ultimate strength
lower
tensile (UTS)
values
strength increased.
of fracture
(UTS) and uniform strain were observed,
increased.
X-ray
while X-raydiffraction
yield patterns
stress (YS)
diffraction of of
thethe
and ultimate
patterns three samples
tensile
three were
strength
samples collected
(UTS)
were before
increased.
collected straining
before straininguntil fracture
until and
fracture and
FWHM
FWHM X-ray
areare diffraction
reported
reportedinin
Figure
Figure6 (6▪,( •,
patterns of the three samples
, •,Nsymbols).
symbols). were collected before straining until fracture and
FWHM are reported in Figure 6 (▪, •,  symbols).

Figure 6. X-ray diffraction pattern together with full width half maximum values of the set of
three6.samples.
Figure X-ray diffraction pattern together with full width half maximum values of the set of three
samples.
Figure 6. X-ray diffraction pattern together with full width half maximum values of the set of three
Peaks broadening is affected by dislocation density, microstrain, stacking faults, crystallite size
samples.
etc.Peaks
[41–47]. It is therefore
broadening veryby
is affected difficult to separate
dislocation density,the contribution
microstrain, of eachfaults,
stacking phenomenon,
crystalliteso raw
size
FWHM
etc. values
[41–47]. is are considered. As expected, as the prestrain increased FWHMeach increased too, because of
PeaksItbroadening
thereforeisvery difficult
affected to separate
by dislocation the contribution
density, microstrain,ofstacking
phenomenon, so raw
faults, crystallite size
FWHM values are
etc. [41–47]. It isconsidered. As expected,
therefore very as separate
difficult to the prestrain increased FWHM
the contribution increased
of each too, because
phenomenon, so raw
of FWHM
the higher dislocation density, the generation of stacking fault in the austenitic phase, the
values are considered. As expected, as the prestrain increased FWHM increased too, because evolution
of the higher dislocation density, the generation of stacking fault in the austenitic phase, the evolution
Materials2020,
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2020,13, FOR PEER REVIEW 77of
of19
18

Materials 2020, 13, x FOR PEER REVIEW 7 of 19

of the crystallite size due to dislocation network, etc. The higher the prestrain the higher the
the higher dislocation density, the generation of stacking fault in the austenitic phase, the evolution of
microhardness
of as well (Figure
to 7).
thethe crystallite
crystallite sizeto
size due due dislocation
dislocation network,network, etc. The
etc. The higher the higher the
prestrain theprestrain
higher thethe higher the
microhardness
microhardness
as well (Figure as7).well (Figure 7).

Microhardnessevolution
Figure7.7.Microhardness
Figure evolutionas
asaafunction
functionof
ofprestrain
prestrainof
ofthe
thebulk
bulkmaterial
materialand
andof
ofeach
eachphase.
phase.

Figure 7. Microhardness
Microhardness ofthe evolution
thebulk
bulk as a function
material waslowerof prestrain
lower compared of thetobulk
that material and of each phase.
Microhardness of material was compared to that ofofthethe single
single phases
phases because
because it
it was measured
was measured withwitha a higher
higher load.
load. TheThe smaller
smaller the the load
load thethe more
more thethe measure
measure isis affected
affected by the
by the
Microhardness of the bulk material was lower compared to that of the single phases because it
metallographic preparation
metallographic preparationwhich
which producesaa shallowshallowwork work hardened
hardened layer layer at
at the
the surface
surface not not toto
was measured with a higher load. produces
The smaller the load the more the measure is affected by the
mentionthe
mention the indentation
indentationsize size effect.
effect. As
Asthetheprestrain
prestrainincreased,
increased, the the microhardness
microhardness of of the
the austenitic
austenitic
metallographic preparation which produces a shallow work hardened layer at the surface not to
phase
phase increased
increased due to its higher
due to itssize
higher strain
strain hardening rate because of the lower YS in comparison tothat
that
mention the indentation effect. Ashardening
the prestrainrateincreased,
because ofthe themicrohardness
lower YS in comparison to
of the austenitic
offerrite
of ferrite[48,49].
[48,49].
phase increased due to its higher strain hardening rate because of the lower YS in comparison to that
Corrosion
Corrosion propertieswere
properties werenotnotsubstantially
substantiallyaffected
affectedbyby thethe degree
degree of of prestrain
prestrain as as
cancan be seen
be seen in
of ferrite [48,49].
in Figure
Figure 8, 8,
wherewhere
the the potentiodynamic
potentiodynamic polarization
polarization plotsplots
of theofasthe as
receivedreceived
and and prestrained
prestrained at 5% atand
5%
Corrosion properties were not substantially affected by the degree of prestrain as can be seen in
and 15%
15% samplessamples
aretheare shown.
shown. The The
onlyonly observed
observed effect
effect waswas the raise in in corrosionpotential
potential ofthe the5%5%
Figure 8, where potentiodynamic polarization plots ofthe
theraise
as received corrosion
and prestrained of at 5% and
prestrained
prestrained specimen
specimen in comparison
in comparison to the others.
to the others. No
Nowas effect
effect on the corrosion current were observed.
15% samples are shown. The only observed effect theonraise
the corrosion
in corrosion current were observed.
potential of the 5%
prestrained specimen in comparison to the others. No effect on the corrosion current were observed.

Figure 8. Potentiodynamic polarization curves of tested materials.

Figure 8. Potentiodynamic polarization curves of tested materials.
Figure 8. Potentiodynamic polarization curves of tested materials.
Materials 2020, 13, 1613 8 of 18

Materials 2020, 13, x FOR PEER REVIEW 8 of 19

Compressive stresses in each phase along the two directions were measured, conversely to
whatCompressive
Johansson etstresses
al. foundin each
[40]. phase along in
A decrease thethe
two directions were
compressive stressmeasured,
values forconversely
both phases to what
were
Johansson et al. found [40]. A decrease in the compressive stress values for both
determined since the specimens were strained along the transversal direction (Figure 9b). The average phases were
determined since thewith
stress was computed specimens
the rule were strained
of mixture along to
according the[40].
transversal
Compressivedirection (Figure
stresses along 9b). The
in single
average stressrolling
phases along was computed
direction with the rule
increased of mixture
in austenite andaccording
decreased to in
[40]. Compressive
ferrite. stresses along
Average residual stress
in single phases along rolling direction increased in austenite and decreased
remained almost constant as expected since a tensile test produces the superposition of a uniaxialin ferrite. Average
residual stress remained
stress condition almost constant
on the previously existingasstresses
expected since a tensile
distribution in thetest produces the superposition
specimen.
of a uniaxial stress condition on the previously existing stresses distribution in the specimen.

Figure 9.
Figure Residualstresses
9. Residual stresses evolution
evolution on
on the
the single
single phases
phases and
and the
the average
average along
along the
the rolling
rolling direction
direction
(a) and the transversal direction (b).
(a) and the transversal direction (b).

3.3. Tensile Tests

3.3. Tensile Tests
Electropulsing treatments were conducted with current density of 100 A/mm2 and 200 A/mm2 at
Electropulsing treatments were conducted with current density of 100 A/mm2 and 200 A/mm2
1 Hz for 100 s and 500 s. No increase in specimen temperature was observed during the electropulsing
at 1 Hz for 100 s and 500 s. No increase in specimen temperature was observed during the
treatments due to the small duration and low frequency of the current pulses.
electropulsing treatments due to the small duration and low frequency of the current pulses.
After electropulsing treatments, tensile tests have been conducted and compared with the reference
After electropulsing treatments, tensile tests have been conducted and compared with the
of each category (namely 5% tensile test curve of category one and 15% tensile test curve of category
reference of each category (namely 5% tensile test curve of category one and 15% tensile test curve of
two, together with the flow stress curve of the tensile test performed on the undeformed material,
category two, together with the flow stress curve of the tensile test performed on the undeformed
Figure 10). Overall improvement in mechanical properties has been observed for both categories.
material, Figure 10). Overall improvement in mechanical properties has been observed for both
In the 5% prestrained specimens, the best combination of current density and number of pulses was the
categories. In the 5% prestrained specimens, the best combination of current density and number of
lowest (100 A/mm2 and 100 pulses).2 Nevertheless, all tested conditions affected the tensile response in a
pulses was the lowest (100 A/mm and 100 pulses). Nevertheless, all tested conditions affected the
positive manner. In the case of specimens prestrained at 15% a recovery of approximately 8% in fracture
tensile response in a positive manner. In the case of specimens prestrained at 15% a recovery of
strain was observed for all tested conditions. The best combination of number of pulses and current
approximately 8% in fracture strain was observed for all tested conditions. The best combination of
density was the same observed as in the 5% prestrain case (100 A/mm2 and 100 pulses). Comparing the2
number of pulses and current density was the same observed as in the 5% prestrain case (100 A/mm
effect of the different combinations of current-number of pulses it appears that mechanical properties
and 100 pulses). Comparing the effect of the different combinations of current-number of pulses it
are more affected by the number of pulses rather than the current density. Fixing the current density,
appears that mechanical properties are more affected by the number of pulses rather than the current
as the number of pulses increased, small improvements in fracture strain were observed. The two
density. Fixing the current density, as the number of pulses increased, small improvements in fracture
current densities tested affected to a lesser extent the recovery of fracture strain in comparison to the
strain were observed. The two current densities tested affected to a lesser extent the recovery of
effect of the number of pulses.
fracture strain in comparison to the effect of the number of pulses.
Materials 2020, 13,
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18
Materials 2020, 13, x FOR PEER REVIEW 9 of 19

Figure 10. Tensile tests of electropulsed specimens after prestrain of (a) 5% and (b) 15%. The dashed
Figure10.
Figure 10.Tensile
Tensiletests
testsofofelectropulsed
electropulsedspecimens
specimensafter
afterprestrain
prestrainofof(a)
(a)5%
5%and
and(b)
(b)15%.
15%.The
Thedashed
dashed
line represents the room temperature test, while red line is the reference of each categories (5% tensile
linerepresents
line representsthe
theroom
roomtemperature
temperaturetest,
test,while
whilered
redline
lineisisthe
thereference
referenceofofeach
eachcategories
categories(5%
(5%tensile
tensile
test (a) and 15% tensile test (b)).
test(a)
test (a)and
and15%
15%tensile
tensiletest
test(b)).
(b)).

3.4. Microhardness
3.4. Microhardness
Bulk hardness of the electropulsed specimens of 5% prestrained material was slightly higher
Bulk hardness of the electropulsed specimens of 5% prestrained material was slightly higher
than that of the undeformed material (0%) while it was remarkably lower compared to the reference
than that of the undeformed material (0%) while it was remarkably lower compared to the reference
(Figure 11). Those
Those results
results were
were expected
expected on on the
the basis
basis of
of the
the true
true stress-strain
stress-strain curves
curves ofof Figure
Figure 10a.
10a.
(Figure 11). Those results were expected on the basis of the true stress-strain curves of Figure 10a.
Conversely, despite the substantial recovery of the specimens prestrained to 15% in
Conversely, despite the substantial recovery of the specimens prestrained to 15% in comparison to the comparison to
Conversely, despite the substantial recovery of the specimens prestrained to 15% in comparison to
the reference
reference tensile
tensile tests,
tests, no no appreciable
appreciable bulk hardness
bulk hardness reductionreduction was observed.
was observed. Electropulsing
Electropulsing treatments
the reference tensile tests, no appreciable bulk hardness reduction was observed. Electropulsing
treatments conducted at higher current density showed a lower bulk hardness
conducted at higher current density showed a lower bulk hardness in contrast to what could in contrast to what
be
treatments conducted at higher current density showed a lower bulk hardness in contrast to what
could be expected
expected onof
on the basis the basis
flow of flow
stress curvestress curve10b.
of Figure of Figure 10b. Microhardness
Microhardness of the singleofphases
the single phases
showed the
could be expected on the basis of flow stress curve of Figure 10b. Microhardness of the single phases
showed
same theassame
trend trend
the bulk as the bulk
hardness. hardness.
Austenite is theAustenite is thebecause
harder phase harder phase because of its higher
showed the same trend as the bulk hardness. Austenite is the harderofphase
its higher work-hardening
because of its higher
work-hardening
rate rate
compared to ferrite. compared to ferrite.
The reduction The
of hardnessreduction of
was almost hardness
the samewas almost
foralmost the same
both phases. for both
work-hardening rate compared to ferrite. The reduction of hardness was the same for both
phases.
phases.

Figure 11. Single phase hardness and bulk hardness of specimens strained and electropulsed at (a,c) 5%
Figure 11. Single phase hardness and bulk hardness of specimens strained and electropulsed at (a,c)
and (b,d)11.
Figure 15% compared
Single to the baseline
phase hardness (0%)hardness
and bulk and the related reference
of specimens tests. and electropulsed at (a,c)
strained
5% and (b,d) 15% compared to the baseline (0%) and the related reference tests.
5% and (b,d) 15% compared to the baseline (0%) and the related reference tests.
Materials 2020, 13, 1613 10 of 18
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Materials 2020, 13, x FOR PEER REVIEW 10 of 19
3.5. Ultimate
3.5. Ultimate Tensile
Tensile Strength
Strength and
and Yield
Yield Stress
Stress
3.5. Ultimate Tensile Strength and Yield Stress
Ultimate tensile
Ultimate tensile strength
strength was was affected
affected to to aa much
much lesser
lesser extent
extent by by both
both prestrain
prestrain and and byby the
the
Ultimate
electropulsing tensile strength
treatment. As was
can beaffected
seen to
from a much
Figure lesser
12a, 5%extent
prestrainby both
electropulsing treatment. As can be seen from Figure 12a, 5% prestrain had no effect on the UTS whilehad prestrain
no effect and
on theby the
UTS
electropulsing
while
the treatment.
the electropulsing
electropulsing As can
treatments
treatments be seen
caused acaused from Figure 12a,
a slight decrease
slight decrease 5% prestrain
of UTS in of had no
UTS in comparison
comparison effect on
to that of the the UTS while
toprestrained
that of the
the electropulsing
prestrained
material. Asmaterial.
opposedtreatments
As whatcaused
to opposed a slight
to what
expected, decrease
expected,
the theofelectropulsing
electropulsing UTStreatments
in comparison to that
treatments
increased of the
increased
UTS in prestrained
UTScase
the in the
of
material.
case of As
the opposed
sample to
strainedwhat
at expected,
15% (Figure the electropulsing
12b). This is treatments
because the increased
uniform
the sample strained at 15% (Figure 12b). This is because the uniform strain of the reference specimen UTS
strain of in
thethe case
referenceof
the sample
specimen
(εu = 0.184) u = 0.184)
strained
(εwas at 15% (Figure
was very
very close to theclose 12b).
valueto of This
thethe is
value because the
of the applied
prestrain uniform
prestraintoapplied strain of the reference
to the specimens
the specimens of category specimen
of category
two (ε =
(ε u = (ε =
0.184) was very close to the value of the prestrain applied to the specimens
0.15). Therefore, electropulsing treatments were able to recover a lot in terms of fracturefracture
two 0.15). Therefore, electropulsing treatments were able to recover a lot of
in category
terms of two (ε =
strain,
0.15).
strain, Therefore,
allowing electropulsing
the material to treatments
accept a higher were able
amount to
of recover
deformation,a lot in
hence
allowing the material to accept a higher amount of deformation, hence increasing its ability to work- terms of
increasing fracture
its strain,
ability to
allowing
work-harden
harden the material
whichwhich to accept
consequently
consequently a higher
led to led amount
to higher
higher UTS. UTS.of deformation, hence increasing its ability to work-
harden which consequently led to higher UTS.

Figure 12. Evolution of UTS with respect the different electropulsing treatments and references (a) 5%
prestrainedEvolution
Figure 12. Evolution
specimensofand
of UTS(b)
UTS with
with respect
respect
15% the different
the
prestraineddifferent electropulsing treatments and references (a) 5%
electropulsing
specimens.
prestrained specimens and (b) 15% prestrained specimens.
prestrained specimens and (b) 15% prestrained specimens.
The yield stress, in the case of 5% prestrain, was higher in comparison both to that of the
The
The yield stress,
yieldthe
stress,inin
thethe
case of 5%
case of prestrain, was higher
5% prestrain, in comparison
wasA higher both to both
in comparison that oftothe reference
that of the
the
reference and electropulsed specimens, as expected. substantial reduction was observed for
and the
referenceelectropulsed
and the specimens,
electropulsed as expected.
specimens, as A substantial
expected. A reduction
substantial was observed
reduction was for the
observedspecimens
for the
specimens electropulsed with lower current density, while a very low or even no reduction was
electropulsed
specimenswith with lower
electropulsed current density,
withdensity
lower currentwhile a very
density, low or even
while a very no reduction
low or even was measured
no reduction with
was
measured higher current (Figure 13a). Unexpectedly yield stress increased in the case of
higher
measuredcurrent
with density
higher (Figuredensity
current 13a). Unexpectedly
(Figure 13a). yield stress increased
Unexpectedly yield in the
stress case ofin
increased the samples
the case of
the samples prestrained at 15% and electropulsed, even in comparison to the reference value (Figure
prestrained
the samples at 15% and electropulsed,
prestrained at 15% and even in comparison
electropulsed, even in to the reference
comparison to value
the (Figurevalue
reference 13b). (Figure
13b).
13b).

Figure 13.
Figure Evolution of
13. Evolution of YS
YS with
with respect
respect the
the different
different electropulsing
electropulsing treatments
treatments and
and references
references (a)
(a) 5%
5%
prestrained
Figure 13. specimensofand
Evolution YS (b) 15%
with prestrained
respect the specimens.
different electropulsing treatments and references (a) 5%
prestrained specimens and (b) 15% prestrained specimens.
prestrained specimens and (b) 15% prestrained specimens.
3.6. Uniform and Fracture Strain
3.6. Uniform and Fracture Strain
The effect
3.6. Uniform andofFracture
the electropulsing
Strain treatments are much more evident considering the uniform and
Thestrain
fracture effectrather
of the than
electropulsing
UTS and YS treatments
(Figures 14areand
much
15).more
In theevident
case ofconsidering theprestrained
the specimens uniform andat
The
fracture effect of
strainstrain the
ratherwaselectropulsing
than UTS and treatments
YS (Figure are much more evident considering the uniform and
5%, uniform almost the same of the14 and 15).specimen
reference In the caseforofthe
theelectropulsing
specimens prestrained at
treatments
fracture
5%, strain
uniform rather than UTS andsameYS (Figure
the 14 and 15).specimen
In the case ofthethe specimens prestrained at
conducted atstrain was
the lower almost
currentthe
density. of reference
Nevertheless, even at 200 for A/mm2electropulsing treatments
a substantial increase in
5%, uniform strain was almost the same of the reference specimen for the electropulsing
conducted at the lower current density. Nevertheless, even at 200 A/mm2 a substantial increase in treatments
conducted
uniform at the
strain waslower current
observed density. Nevertheless,
in comparison even atmaterial.
to the untreated 200 A/mm 2 a substantial increase in
Much more evident was the
uniform strain was observed in comparison to the untreated material. Much more evident was the
Materials 2020,
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13, 1613
x FOR PEER REVIEW 11 of
11 of 18
19

effect of2020,
Materials the 13,
electropulsing treatments on the specimens prestrained at 15%. The relative recovery
x FOR PEER REVIEW 11 of in
19
uniform strain was higher
observed in comparison
in this to the
case compared to untreated material.
the previous Muchconstant
one; a slight more evident was
increase of the
the
effect
uniformof the electropulsing
strain
the treatments
increasing the
electropulsing on
on the
the specimens
current density prestrained
and the number
specimens at 15%.
of pulses
prestrained The relative
was observed
15%. recovery
(Figure 14b).in
uniform strain was higher in this case compared to the previous one; a slight constant increase of the
uniform strain increasing
increasing the
the current
current density
density and
and the
the number
number ofof pulses
pulses was
was observed
observed(Figure
(Figure14b).
14b).

Figure 14. Evolution of uniform strain with respect the different electropulsing treatments and
Figure Evolution
14. (a)
reference of uniform
5% prestrained strain with
specimens andrespect theprestrained
(b) 15% different electropulsing
specimens. treatments and reference
(a) 5% prestrained specimens and (b) 15% prestrained specimens.
Figure 14. Evolution of uniform strain with respect the different electropulsing treatments and
reference (a) 5% prestrained specimens and (b) 15% prestrained specimens.

Figure 15. Evolution of fracture strain with respect the different electropulsing treatments and reference
(a) 5% prestrained
Figure specimens
15. Evolution and (b)
of fracture 15% with
strain prestrained
respectspecimens.
the different electropulsing treatments and
reference (a) 5% prestrained specimens and (b) 15% prestrained specimens.
In the case of the specimen prestrained at 5% fracture strain did not show any trend (Figure 15a).
Figure 15. Evolution of fracture strain with respect the different electropulsing treatments and
As said before,
In the case thethetreatment at lower current density and lower number of pulses showed a fracture
reference (a)of specimen
5% prestrained prestrained
specimens andat (b)5%15%fracture strainspecimens.
prestrained did not show any trend (Figure 15a).
strain comparable to that of the reference specimen. The fracture strain
As said before, the treatment at lower current density and lower number of pulses showed a fracture of the specimens treated at
200 A/mm 2 , even if to it was higher comparedspecimen.
to the prestrained material, was
strain Incomparable
the case of the that of theprestrained
specimen reference at 5% fractureThe strain
fracture didstrain
not showof slightly
the inferiortreated
specimens
any trend (Figure
to that ofat
15a).
the 100 A/mm 2 treatment,
200 A/mm 2, even if it was higher compared to the prestrained material, was slightly inferiorthe
regardless of the number of pulses. It is clear from Figure 15b that, in to case
that
As said before, the treatment at lower current density and lower number of pulses showed a fracture
of
of 15% prestrained
the comparable
100 specimens,regardless
A/mm2 treatment, the number of
thepulses
ofspecimen.
number affected in more
of fracture
pulses. It isextent
clear the
fromfracture
Figurestrain
15b rather
that, in
strain to that of the reference The strain of the specimens treated at
than
the the
case current
of 15% density.
prestrained EPTs conducted
specimens, with
the lower
number number
of pulses of pulses
affected showed
in more the same
extent increase
the in
fracture
200 A/mm , even if it was higher compared to the prestrained material,
2
2 500 was slightly inferior to that
fracture
strain strain. The most severe electropulsing treatment (200 A/mm pulses) increased fracture
of the rather
100 A/mm than 2the current
treatment, density.
regardlessEPTs conducted
of the numberwith lower
of pulses. number
It is clear of pulses
from showed
Figure 15bthe same
that, in
strain
increase in comparison
in 15%
fracture to the prestrained
strain. The most material
severe but was the worst
electropulsing in terms
treatment of absolute increase in
the case of prestrained specimens, the number of pulses affected in (200
moreA/mm 500
extent2 the pulses)
fracture
fracture
increased strain. It is strain
fracture worth noting the generally
in comparison high
toconducted
the scatteringmaterial
prestrained of the data butregarding
was the the testin
worst conducted
terms of
strain rather than the current density. EPTs with lower number of pulses showed the same
on the specimens
absolute in increase prestrained
in strain.
fractureThe at 15%.
strain. It severe
is worthelectropulsing
noting the generally
increase fracture most treatmenthigh (200scattering
A/mm 500 2 of the data
pulses)
regarding fracture
increased the test conducted
strain in on the specimens
comparison to the prestrained
prestrained atmaterial
15%. but was the worst in terms of
3.7. Residual Stresses
absolute increase in fracture strain. It is worth noting the generally high scattering of the data
The average
3.7. Residual
regarding testtransverse
theStresses conductedresidual stresses for
on the specimens both degrees
prestrained of prestrain showed almost the same
at 15%.
values (Figure 16). Since tensile test introduces uniaxial stress configuration in the specimen, no
The average transverse residual stresses for both degrees of prestrain showed almost the same
variation
3.7. Residual in the average residual internal stresses was expected. On the other hand, electropulsing
Stresses
values (Figure 16). Since tensile test introduces uniaxial stress configuration in the specimen, no
treatments have shown to induce changes in the grain orientation within the materials not to mention
variation in the average
The average transverse residual internal
residual stresses
stresses for bothwasdegrees
expected. On the other
of prestrain hand,
showed electropulsing
almost the same
the change in morphology of secondary low conductivity phases (i.e., cementite particles in perlite)
treatments have shown to induce changes in the grain orientation within
values (Figure 16). Since tensile test introduces uniaxial stress configuration in the specimen, the materials not to mention no
hence, a change in the residual stresses of the single phase was expected [30,50–53]. An increase in
the change
variation inin themorphology
average residualof secondary
internallow conductivity
stresses phases On
was expected. (i.e.,the
cementite
other hand,particles in perlite)
electropulsing
treatments have shown to induce changes in the grain orientation within the materials not to mention
the change in morphology of secondary low conductivity phases (i.e., cementite particles in perlite)
Materials 2020, 13, 1613 12 of 18
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hence, a change in the residual stresses of the single phase was expected [30,50–53]. An increase in
compression stress amounts in ferrite after the first electropulsing treatment was determined and this
compression stress amounts in ferrite after the first electropulsing treatment was determined and this
did not change even after the electropulsing treatment at higher current density and higher number
did not change even after the electropulsing treatment at higher current density and higher number
of pulses (Figure 16a). In the case of the specimens prestrained at 15%, again an increase of the
of pulses (Figure 16a). In the case of the specimens prestrained at 15%, again an increase of the
compressive state in ferrite (approximately from −50 MPa to −400 MPa) was determined for the lower
compressive state in ferrite (approximately from −50 MPa to −400 MPa) was determined for the lower
current density treated samples. The higher current density treatment produced a decrease of the
current density treated samples. The higher current density treatment produced a decrease of the
compressive stresses in ferrite from −400 MPa to almost the same value as the prestrained material
compressive stresses in ferrite from −400 MPa to almost the same value as the prestrained material
(Figure 16b). The compressive state in austenite was much severe in comparison to that in ferrite
(Figure 16b). The compressive state in austenite was much severe in comparison to that in ferrite
(Figure 16a) but no significant trend have been observed. Same considerations can be made in the case
(Figure 16a) but no significant trend have been observed. Same considerations can be made in the
of the material prestrained at 15% (Figure 16b). On the other hand, the average residual stresses in
case of the material prestrained at 15% (Figure 16b). On the other hand, the average residual stresses
both cases remained almost constant.
in both cases remained almost constant.

Figure 16. Evolution of transverse residual stresses in austenite (red circles), ferrite (black squares) and
Figure 16. Evolution of transverse residual stresses in austenite (red circles), ferrite (black squares)
their average (blue thick line) for specimens prestrained and electropulsed at (a) 5% and (b) 15%.
and their average (blue thick line) for specimens prestrained and electropulsed at (a) 5% and (b) 15%.

Different evolution of the average residual stresses along the longitudinal direction can be seen in
Different evolution of the average residual stresses along the longitudinal direction can be seen
Figure 17. A gradual increase in the compression state in the case of the specimen prestrained at 5%
in Figure 17. A gradual increase in the compression state in the case of the specimen prestrained at
was evident (Figure 17a) with a slight decrease for the specimens treated with 100 pulses at 200 A/mm2 .
5% was evident (Figure 17a) with a slight decrease for the specimens treated with 100 pulses at
The same trend was observed for the material prestrained at 15% under electropulsing treatment at
200 A/mm2. The same trend was observed for the material prestrained at 15% under electropulsing
100 A/mm2 , while substantial decrease in the compressive stress state for the treatments conducted at
treatment 2at 100 A/mm2, while substantial decrease in the compressive stress state for the2treatments
200 A/mm were induced. Electropulsing treatments consisting of 500 pulses at 200 A/mm presented
conducted at 200 A/mm2 were induced. Electropulsing treatments consisting of 500 pulses at
stress values and distributions comparable to that of the prestrained material. Residual stresses of the
200 A/mm2 presented stress values and distributions comparable to that of the prestrained material.
single phase followed the same trend of the average residual stress both for the specimens prestrained
Residual stresses of the single phase followed the same trend of the average residual stress both for
at 5% and 15% as can be seen in Figure 17. The only exception was the material prestrained at 15%
the specimens prestrained at 5% and 15% as can be seen in Figure 17. The only exception was the
treated with 100 pulses at 100 A/mm2 in which ferrite abruptly changed from a tensile stress value of
material prestrained at 15% treated with 100 pulses at 100 A/mm2 in which ferrite abruptly changed
approximately 150 MPa to a compressive value of 300 MPa when increasing the number of pulses.
from a tensile stress value of approximately 150 MPa to a compressive value of 300 MPa when
increasing the number of pulses.
Materials 2020, 13, 1613 13 of 18
Materials 2020, 13, x FOR PEER REVIEW 13 of 19

Figure 17. Evolution of longitudinal residual stresses in austenite (red circles), ferrite (black squares)
Figure 17. Evolution of longitudinal residual stresses in austenite (red circles), ferrite (black squares)
and their average (blue thick line) for specimens prestrained and electropulsed at (a) 5% and (b) 15%.
and their average (blue thick line) for specimens prestrained and electropulsed at (a) 5% and (b) 15%.
3.8. X-ray Diffraction
3.8. X-Ray Diffraction
X-ray diffraction measurements were conducted in order to evaluate the evolution of the peak’s
X-ray diffraction
broadening measurements
as a function of the specimen wereconditions.
conducted in order to evaluate the evolution of the peak’s
broadening as a function of the specimen conditions.
An overview of the evolution of the FWHM of the peaks related to the different treatment
An overview
conditions of the
is reported evolution
in Figure of thethe
18. Being FWHM
FWHM ofinfluenced
the peaks by related to the density,
dislocation different treatment
microstrain,
conditions
stacking is reported
fault in Figure
density, etc., 18. Being
it is obvious the
that FWHM
the higherinfluenced
value of thebyFWHM
dislocation density,
is found in themicrostrain,
specimens
stacking fault density, etc., it is obvious that the higher value of the FWHM is
prestrained at 5% and 15% (black squares in Figure 18). In order to enhance the differencesfound in the specimens
in FWHM
prestrained at 5% and 15% (black squares in Figure 18).
of each phase, a separate diagram was built (Figures 19 and 20). In order to enhance the differences in FWHM
of each phase, a separate diagram was built (Figure 19 and 20).

Figure 18. FWHM of the electropulsed specimens prestrained at (a) 5% and (b) 15%.
Figure 18. FWHM of the electropulsed specimens prestrained at (a) 5% and (b) 15%.

As expected from the tensile test curves, the most significant decrease in FWHM of the 5%
As expected from the tensile test curves, the most significant decrease in FWHM of the 5%
prestrained samples, was observed in the case of the treatments that showed the highest recovery in
prestrained samples, was observed in the case of the treatments that showed the highest recovery in
fracture strain (100 pulses at 100 A/mm2 in2 Figure 19). A slight increase in FWHM was observed with
fracture strain (100 pulses at 100 A/mm in Figure 19). A slight increase in FWHM was observed
the other electropulsed treatment, with a subsequent reduction for the electropulsing treatment at
with the other electropulsed treatment, with a subsequent reduction for the electropulsing treatment
higher current density and number of pulses. It is interesting to note the higher reduction in terms of
at higher current density and number of pulses. It is interesting to note the higher reduction in terms
absolute values for the FWHM relative to the austenitic phase, due to its higher dislocation density in
of absolute values for the FWHM relative to the austenitic phase, due to its higher dislocation density
in the as strained condition because of the low yield point and higher work hardening rate compared
to ferrite.
Materials 2020, 13, 1613 14 of 18

the as strained condition because of the low yield point and higher work hardening rate compared
Materials
Materials 2020,
2020, 13,
13, xx FOR
FOR PEER
PEER REVIEW
REVIEW 14
14 of
of 19
19
to ferrite.

Figure 19. FWHM evolution of ferrite (a) and austenite (b) for the specimens prestrained at 5%
Figure 19. FWHM evolution of ferrite (a) and austenite (b) for the specimens prestrained at 5% and
and electropulsed.
electropulsed.
The reduction of FWHM in the case of the 15% prestrained samples was lower in comparison
The reduction of FWHM in the case of the 15% prestrained samples was lower in comparison to
to that of the samples prestrained at 5%. Same trend both for the ferritic and austenitic phase was
that of the samples prestrained at 5%. Same trend both for the ferritic and austenitic phase was
observed (Figure 20). FWHM remained almost constant regardless the current density and number of
observed (Figure 20). FWHM remained almost constant regardless the current density and number
pulses, except for a slight increase after 500 pulses at 100 A/mm2 (more evident in Figure 20a).
of pulses, except for a slight increase after 500 pulses at 100 A/mm22 (more evident in Figure 20a).

Figure 20. FWHM evolution of ferrite (a) and austenite (b) for the specimens prestrained at 15%
Figure 20. FWHM evolution of ferrite (a) and austenite (b) for the specimens prestrained at 15% and
and electropulsed.
electropulsed.
4. Discussion
4. Discussion
It is mandatory to know how duplex stainless steels behave during tensile test to understand the
It is mandatory
microscopic changes to
inknow how duplex
dislocation stainless
network, strain steels behave
and stress during tensile
distribution testaffect
that can to understand the
current flow.
microscopic changes in dislocation network, strain and stress distribution that can affect current flow.
Due to the lower yield stress, austenite is the phase in which most of the strain is localized at the
beginning of deformation. It absorbs much of the early stage deformation because it possesses 12 low-
shear strength preferred slip systems and allows easy dislocation mobility in almost all
crystallographic directions while ferrite is characterized by relatively higher-shear strength slip
systems, which typically possess higher critically resolved shear stresses for their activation [54].
Materials 2020, 13, 1613 15 of 18

Due to the lower yield stress, austenite is the phase in which most of the strain is localized at
the beginning of deformation. It absorbs much of the early stage deformation because it possesses
12 low-shear strength preferred slip systems and allows easy dislocation mobility in almost all
crystallographic directions while ferrite is characterized by relatively higher-shear strength slip
systems, which typically possess higher critically resolved shear stresses for their activation [54].
Even though ferrite has more slip system, its Peierls stress is higher compared to the yield stress of
austenite, justifying the fact that austenite is more ductile than ferrite. Ferrite starts to accommodate
plastic deformation after austenite has work-hardened enough to increase its yield stress above
that necessary to overcome the Peierls barriers in ferrite. After that, ferrite starts to accommodate
higher plastic strain than austenite, while some austenitic grains experience a more pronounced
increase in the hardening effect depending on the orientation relationship between austenite and
ferrite (Kurdjumov–Sachs orientation is the most favourable for the transfer of strain field between
austenite and ferrite [10,55–57]). Direct dislocation transfer between austenite and ferrite is obviously
impossible due to the phase boundary, but dislocations on the austenitic phase that keep piling up on
the phase boundary could generate dislocation sources in the adjacent ferritic phase. It is therefore
clear, that phase boundaries play an important role in governing the deformation mechanism of duplex
stainless steels.
They are also inhomogeneities, filled with dislocations and stacking faults which increase the
local resistivity. When electrical current passes through the material, macro and microscopic effect
occur. Bulk joule heating is a macroscopic effect, while at microscopic level electrons from electrical
current interacts with the inhomogeneities in the microstructure. As modelled by Zhao et al. [38],
electrical current does not flow homogeneously throughout the microstructure: if secondary phases
are not present, it is influenced by the grain boundary network. The grain boundary network acts
on the electrical current, forcing it to flow across an “easy path”, such as the triple junctions. As a
consequence, the current flow is affected by the angle between the macro current flow and the grain
boundaries [38]. This uneven distribution of electrical current could cause local increase in current
density which can enhance plastic deformation thanks to localized Joule heating and to the effect of a
stronger electron wind force on dislocations.
In this specific case, on top of grain boundary network, another phase with different crystal
structure, dislocation density and composition is present. It is therefore legitimate to hypothesize an
uneven distribution of the current within the material. In correspondence of regions with different
electrical resistivity (grain and phase boundary, dislocation tangles, dislocation sub cell walls etc.)
there could be stagnation of electrons as proposed by Ruszkiewicz et al. [15]. Electron stagnation could
cause local increase in electron to atom ratio, leading to lowering the bonding energy between the
ions of the crystal structure therefore easing dislocation motion in the case of current applied during
deformation [58]. In this case the effect of electric current facilitates the recovery of the work-hardened
state thanks to localized Joule heating effect, the reduction in bonding energy and the increase in atomic
flux due to electromigration [35,59,60]. Electrical current will be unevenly distributed at multiscale
levels: at microscopic level dislocation tangles, sub cell walls, grain boundaries etc., affect the current
distribution while at an intermediate scale the different resistivity, composition and work hardening
state of the two phases could lead to partial redistribution of the current within one phase or the other.
All the above mentioned phenomena are concurrent and caused the recovery of the work-hardened
state observed in the specimens. On top of that, possible room temperature grain rotation could
have been taken place as observed by Rahnama et al. [39]. In order to investigate grain orientation,
further electron backscattered diffraction (EBSD) analysis have to be performed and kernel average
misorientation (KAM) measurements within single grains must be acquired.

5. Conclusions
The influence of electropulsing treatment has been investigated on prestrained UNS S32750 duplex
stainless steel. It has been found that electropulsing treatments conducted on 5% and 15% prestrained
Materials 2020, 13, 1613 16 of 18

specimens almost eliminate the work-hardening state in the first case, while partially recover the
work-hardened state in the second. Interesting to note is the increase in yield stress and ultimate tensile
strength in the case of electropulsed specimens prestrained to 15% coupled with the increase both in
uniform and fracture strain.
Residual stresses did not show any particular trend: average transverse residual stress remained
almost constant even though variations within the single phase was observed. Longitudinal compressive
stresses values increased in the case of the specimens prestrained at 5% and electropulsed, while in
the case of the 15% prestrained samples the highest compressive state was found for the material
electropulsed with 500 pulses at 100 A/mm2 .
The effect of electropulsing treatment was observed in terms of peak’s FWHM reduction of X-ray
patterns. An effect in terms of recovering the work-hardened state thanks to uneven distribution and
increased atomic flux due to the electrical current was hypothesized, based on the data acquired and
the literature.
These results are promising in terms of replacing furnace annealing treatments with
electropulsing treatments.

Author Contributions: Conceptualization: C.G.; methodology: C.G. and L.P.; software: C.G.; validation:
A.D.S.; formal analysis: C.G.; investigation: C.G., L.P. and G.T.; resources: I.C.; data curation: C.G. and G.T.;
writing—original draft preparation: C.G.; writing—review and editing: C.G., A.Z, I.C. and A.D.S.; visualization:
C.G.; supervision: I.C.; project administration: I.C.; funding acquisition: I.C. All authors have read and agreed to
the published version of the manuscript.
Funding: This research was funded by PuCEAF project, Progetti SID 2019, Università degli Studi di Padova.
Acknowledgments: We would like to acknowledge Marco Frigo from Outokumpu S.p.A. who kindly supplied
the investigated material.
Conflicts of Interest: The authors declare no conflict of interest.

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