metals

Article
Frequency–Time Domain Analysis Based on Electrochemical
Noise of Dual-Phase (DP) and Ferrite–Bainite (FB) Steels in
Chloride Solutions for Automotive Applications
Facundo Almeraya-Calderón 1 , Marvin Montoya-Rangel 2 , Demetrio Nieves-Mendoza 3, *,
Jesús Manuel Jáquez-Muñoz 4 , Miguel Angel Baltazar-Zamora 3 , Laura Landa-Ruiz 3, * , Maria Lara-Banda 1 ,
Erick Maldonado-Bandala 3 , Francisco Estupiñan-Lopez 1, * and Citlalli Gaona-Tiburcio 1

1 Universidad Autonoma de Nuevo Leon, FIME, Centro de Investigación e Innovación en Ingeniería

Aeronáutica (CIIIA), s/n, Ciudad Universitaria, San Nicolás de los Garza 66455, Nuevo León, Mexico;
[email protected] (F.A.-C.); [email protected] (M.L.-B.);
[email protected] (C.G.-T.)
2 Unidad de Investigación y Tecnologias Aplicadas, Facultad de Química, Universidad Nacional Autónoma de
México, Apodaca 66629, Nuevo León, Mexico; [email protected]
3 Facultad de Ingeniería Civil, Universidad Veracruzana, Xalapa 91000, Veracruz, Mexico;
[email protected] (M.A.B.-Z.); [email protected] (E.M.-B.)
4 Instituto Tecnológico de Ciudad Juarez, Av. Tecnológico, 1340, Ciudad Juárez 32500, Chihuahua, Mexico;
[email protected]
* Correspondence: [email protected] (D.N.-M.); [email protected] (L.L.-R.);
[email protected] (F.E.-L.)

Abstract: The automotive industry uses high-strength (HS), low-alloy (HSLA) steels and advanced
Citation: Almeraya-Calderón, F.;
high-strength steels (AHSSs) to manufacture front and rear rails and safety posts, as well as the
Montoya-Rangel, M.; Nieves-
Mendoza, D.; Jáquez-Muñoz, J.M.;
car body, suspension, and chassis components of cars. These steels can be exposed to corrosive
Baltazar-Zamora, M.A.; Landa- environments, such as in countries where de-icing salts are used. This research aims to characterize
Ruiz, L.; Lara-Banda, M.; the corrosion behavior of AHSSs based on electrochemical noise (EN) [dual-phase (DP) and ferrite–
Maldonado-Bandala, E.; bainite (FB)]. At room temperature, the steels were immersed in NaCl, CaCl2 , and MgCl2 solutions
Estupiñan-Lopez, F.; Gaona- and were studied by frequency–time domain analysis using wavelet decomposition, Hilbert–Huang
Tiburcio, C. Frequency–Time Domain analysis, and recurrence plots (RPs) related to the corrosion process and noise impedance (Zn ). Optical
Analysis Based on Electrochemical microscopy (OM) was used to observe the microstructure of the tested samples. The results generally
Noise of Dual-Phase (DP) and indicated that the main corrosion process is related to uniform corrosion. The corrosion behavior
Ferrite–Bainite (FB) Steels in Chloride
of AHSSs exposed to a NaCl solution could be related to the morphology of the phase constituents
Solutions for Automotive
that are exposed to solutions with chlorides. The Zn results showed that DP780 presented a higher
Applications. Metals 2024, 14, 1208.
corrosion resistance with 918 Ω·cm2 ; meanwhile, FB780 presented 409 Ω·cm2 when exposed to NaCl.
https://doi.org/10.3390/
met14111208
Also, the corrosion mechanism of materials begins with a localized corrosion process spreading to all
the surfaces, generating a uniform corrosion process after some exposition time.
Academic Editor: Branimir N. Grgur

Received: 10 September 2024 Keywords: corrosion; AHSSs; electrochemical noise; wavelets; Hilbert–Huang transform (HHT);
Revised: 11 October 2024 recurrence plots (RPs)
Accepted: 16 October 2024
Published: 23 October 2024

1. Introduction
The use of advanced high-strength steels (AHSSs) continues to grow in the automotive
Copyright: © 2024 by the authors.
Licensee MDPI, Basel, Switzerland.
sector, especially for body structures, suspension, and chassis components. This is the result
This article is an open access article
of multiple characteristics, such as high formability that can be used to achieve external
distributed under the terms and designs, lightness, sufficient rigidity for vehicle handling, high mechanical strength, the
conditions of the Creative Commons possibilities of production in large quantities, and the possibility of achieving all of this
Attribution (CC BY) license (https:// under strong economic limitations [1,2].
creativecommons.org/licenses/by/ Advanced high-strength steels (AHSSs) are multi-phase metallic alloys that provide a
4.0/). higher balance of strength and ductility than conventional mild steels and high-strength,

Metals 2024, 14, 1208. https://doi.org/10.3390/met14111208 https://www.mdpi.com/journal/metals

Metals 2024, 14, x FOR PEER REVIEW 2 of 20

Metals 2024, 14, 1208 2 of 17

Advanced high-strength steels (AHSSs) are multi-phase metallic alloys that provide
a higher balance of strength and ductility than conventional mild steels and high-strength,
low-alloy
low-alloy (HSLA)
(HSLA) steels
steels [1]. Advanced steels have been used for decades in the automotive
sector; some types of steel (see Figure 1) include complex-phase (CP), transformation-
transformation-
induced
induced plasticity
plasticity(TRIP),
(TRIP),hot-formed (HF),
hot-formed ferrite–bainite
(HF), (FB),(FB),
ferrite–bainite and dual-phase (DP) steels,
and dual-phase (DP)
among others [2,3].
steels, among others [2,3].

Figure 1.
Figure 1. Classification
Classification of
of advanced
advanced high-strength
high-strength steels
steels (AHSSs).
(AHSSs).

Auto/Steel Association
The Auto/Steel Association published
published aa document
document called Advanced Applications of High
Strength Steel:
Strength Steel: Design
DesignGuidelines
Guidelinesand andStamping
StampingProcess,
Process,and andinin this
this edition,
edition, 1212 detailed
detailed cases
cases of
of using these steels were addressed [4]. Most of the steel parts
using these steels were addressed [4]. Most of the steel parts in this document were focused in this document were
focused
on on DP
DP steel. steel. are
Details Details
given areongiven on the component
the component geometry, geometry, part design,
part design, secondary
secondary metal-
metallurgical
lurgical processesprocesses
such assuchformingas forming and stamping,
and stamping, and indicators
and indicators of mechanical of mechanical
properties.
properties.
Dual-phase steels have a bainite or martensite microstructure in a ferrite matrix. The
microstructure
Dual-phase ofsteels
DP steels
havecan be improved
a bainite by an intercritical
or martensite microstructureheat treatment
in a ferriteconsisting
matrix. The of
two steps: first, intercritical
microstructure of DP steelsannealing is carriedby
can be improved out,
anand second, rapid
intercritical cooling is performed
heat treatment consisting
to
of promote
two steps: the first,
transformation
intercritical of intercritical
annealing is austenite
carriedinto out,a and
hard second,
phase (martensite) [5]. To
rapid cooling is
increase
performed the to
hardness
promote of DP
thesteel (228 to 317 HV),
transformation it is necessaryaustenite
of intercritical to perform intoa tempering
a hard phaseheat
treatment between 740 and 820the ◦ C and thus obtain a higher percentage of martensite phase [6].
(martensite) [5]. To increase hardness of DP steel (228 to 317 HV), it is necessary to
FB steels
perform have a bainite
a tempering microstructure
heat treatment betweenin a ferrite
740 and matrix,
820 °C which
and is obtained
thus obtainbya austen-
higher
itizing FB steel
percentage at a temperature
of martensite phase [6]. of 1100 ◦ C for 20–60 min, followed by air-cooling and
immersion in ahave
salt bath at temperatures of 500–800 ◦ C for a time of 1 h, and finishing the
FB steels a bainite microstructure in a ferrite matrix, which is obtained by
process in a type
austenitizing FB of rapid
steel at aquenching
temperature called
of water
1100 °C quenching
for 20–60[7–9].min, Itfollowed
has beenby reported that
air-cooling
the phase content present in AHSSs influences their mechanical properties;
and immersion in a salt bath at temperatures of 500–800 °C for a time of 1 h, and finishing the minimum
elongation
the process of in ferritic–bainitic steels is approximately
a type of rapid quenching 22%, while
called water quenching for dual-phase
[7–9]. steels, it
It has been reported
is only
that the8%phase
[10]. The mechanical
content present strength
in AHSSs of FB steels/AHSSs
influences is obtained properties;
their mechanical from the grain the
size refinement, the creation of precipitates, and the high dislocation
minimum elongation of ferritic–bainitic steels is approximately 22%, while for dual-phase density present in the
bainite
steels, itphase [11].
is only 8%Therefore, DP steels will
[10]. The mechanical enable of
strength lighter automotive production;
FB steels/AHSSs is obtained however,
from the
using
grain size refinement, the creation of precipitates, and the high dislocation density[12].
a thinner gauge strip means that corrosion resistance becomes paramount present
in theInbainite
various investigations,
phase [11]. Therefore, it hasDPbeen
steelsreported
will enable thatlighter
the heat treatmentproduction;
automotive of AHSSs
increases
however, theirusingcorrosion resistance
a thinner gauge stripwhen
means there
that is an increase
corrosion in the becomes
resistance austenitization
paramounttem-
perature,
[12]. and it will also depend on whether the heat treatment involves annealing or
quenching, due to the formation of a martensitic phase in a ferrite matrix when using
In various investigations, it has been reported that the heat treatment of AHSSs
DP steels. Abedini et al. [13] mentioned that an increase does not improve the corrosion
increases their corrosion resistance when there is an increase in the austenitization
resistance of DP steels in the martensitic phase. On the other hand, biphase steels have a
temperature, and it will also depend on whether the heat treatment involves annealing or
higher corrosion resistance than conventional steels due to the formation of galvanic pairs
quenching, due to the formation of a martensitic phase in a ferrite matrix when using DP
between martensite and ferrite or pearlite and ferrite, the latter being more susceptible. In
steels. Abedini et al. [13] mentioned that an increase does not improve the corrosion
FB steels, corrosion resistance is lower due to the creation of galvanic pairs, compared to
resistance of DP steels in the martensitic phase. On the other hand, biphase steels have a
DP steels. However, this resistance can be increased by grain size refinement in FB steel,
higher corrosion resistance than conventional steels due to the formation of galvanic pairs
which also improves its resistance to pitting and intergranular corrosion. However, the
information in the literature is limited when addressing the corrosion mechanism and
 Metals 2024, 14, x FOR PEER REVIEW 3 of 20

between martensite and ferrite or pearlite and ferrite, the latter being more susceptible. In
Metals 2024, 14, 1208 FB steels, corrosion resistance is lower due to the creation of galvanic pairs, compared to 3 of 17
DP steels. However, this resistance can be increased by grain size refinement in FB steel,
which also improves its resistance to pitting and intergranular corrosion. However, the
information in the literature is limited when addressing the corrosion mechanism and
kineticsofofAHSSs
kinetics AHSSs [14,15].
[14,15]. SomeSome chemical
chemical elements,
elements, such assuch as magnesium,
magnesium, do to
do not help not help to
improve corrosion resistance, whereas silicon
improve corrosion resistance, whereas silicon does [15]. does [15].
Figure2 2shows
Figure shows thethe banana
banana diagrams
diagrams for steel.
for steel. The presents
The AHSS AHSS presents an elongation
an elongation
lowerthan
lower than 30%,
30%, supporting
supporting tensile
tensile stressstress untilMPa,
until 1600 1600depending
MPa, depending on of
on the type the type of AHSS,
AHSS,
comparedwith
compared with conventional
conventional steelssteels
that that
only only
supportsupport
values values lower
lower than 700than
MPa 700
and MPa and
present
presentelongation
elongationuntil 65%65%
until [16].[16].

Elongation
Figure2.2.Elongation
Figure (%)(%) vs. tensile
vs. tensile strength
strength (MPa)(MPa)
bananabanana diagrams
diagrams for the types
for the different different types of steels.
of steels.

Corrosionstudies
Corrosion studies using
using conventional
conventional electrochemical
electrochemical techniques
techniques allowallow for fordetermin-
ing the mechanism
determining the mechanismand kinetics of corrosion
and kinetics of corrosionof metallic
of metallicmaterials
materialsimmersed
immersedin in corrosive
environments.
corrosive DirectDirect
environments. or alternating current
or alternating electrochemical
current electrochemicaltechniques usually disturb
techniques usually
disturb
the systemthe system
under under
study, study,
such assuch as potentiodynamic
potentiodynamic polarization
polarization (PP),(PP),
linearlinear
polarization
polarization resistance (LPR), galvanodynamic polarization (GP), and
resistance (LPR), galvanodynamic polarization (GP), and electrochemical impedance spec- electrochemical
impedance spectroscopy
troscopy (EIS). (EIS). The
The alteration can bealteration
caused can be caused
by external by external
signals signals or
or experimentation condi-
experimentation conditions [17]. On the other hand, there is electrochemical
tions [17]. On the other hand, there is electrochemical noise (EN), whose measurements noise (EN), do
whose measurements do not disturb the system under study, and current and voltage
not disturb the system under study, and current and voltage signal fluctuations occur on
signal fluctuations occur on the electrode surface due to corrosion processes and not by
the electrode surface due to corrosion processes and not by an external signal, as in other
an external signal, as in other corrosion techniques. Oxidation and reduction reactions are
corrosion techniques. Oxidation and reduction reactions are associated with transients as a
associated with transients as a response to stochastic processes (the breakdown and re-
response to
passivation of stochastic
the passiveprocesses
layer) and (the breakdown
deterministic and re-passivation
processes (the nucleation and of the passive layer)
growth
and deterministic
of pits) [18–20] processes (the nucleation and growth of pits) [18–20]
ENENmeasurements
measurements allow
allow for for
the the obtaining
obtaining of data
of data that several
that several methodsmethods can analyze. In
can analyze.
thethe
In time
timedomain
domain (statistical
(statisticalanalysis
analysissuch
suchasaselectrochemical
electrochemical noise
noise resistance
resistance (R (Rn),), Kurtosis,
Skewness,
Kurtosis, Localization
Skewness, Index Index
Localization (L.I.));(L.I.);
in the infrequency
the frequencydomain
domain (spectral
(spectral densities),
densities),and in the
and in the time–frequency
time–frequency domaindomain
(wavelet (wavelet decomposition,
decomposition, Hilbert–Huang
Hilbert–Huang analysis,
analysis, and andrecurrence
recurrence
plots (RP))plots (RP)) [21–25].
[21–25].
Several
Severalstudies
studies have indicated that
have indicated that thethecorrosion
corrosionkinetics
kineticsobtained
obtained from frompotentiody-
potentiodynamic
namic tests in 3.5 wt. % NaCl solution at room temperature have shown that that
tests in 3.5 wt. % NaCl solution at room temperature have shown the corrosion
the corrosion rate decreases when there are ferrite–martensite phases (DP steels)
rate decreases when there are ferrite–martensite phases (DP steels) compared to when there
compared to when there are ferrite–pearlite phases (carbon steel) due to the galvanic
are ferrite–pearlite phases (carbon steel) due to the galvanic couple that is formed [13,26].
Montoyaand Nagiub found similar behavior for different dual-phase steels in an elec-
trolyte with chloride ions [2,27]. Ikpeseni et al. indicated that dual-phase steel exhibits
corrosion potentials between carbon and martensitic steel. The galvanic behavior between
the martensite and ferrite phases favors selective corrosion in the ferrite phase when it
is in a NaCl solution [28]. In AHSSs, galvanic corrosion is expected, due to each phase’s
susceptibility [29]. On the other hand, a study of the corrosion rate in DP600 and DP800
steels immersed in a 3.5% NaCl solution at room temperature indicated that the corrosion
resistance of DP800 steel was higher than DP600 steel, which could be corroborated in
Metals 2024, 14, 1208 4 of 17

the Nyquist diagrams, and the potentiodynamic curves showed similar corrosion current
densities of 12 and 17 µA/cm2 , respectively [30].
Other authors have found that DP steels with simple non-metallic inclusions, such as
manganese sulfides, exhibit low resistance to pitting corrosion in chloride solutions [31–33].
This work aimed to study the corrosion behavior of AHSSs by electrochemical noise
using a frequency–time domain analysis with noise impedance (Zn ), wavelet decomposi-
tion, Hilbert–Huang analysis, and recurrence plots (RP). The steels were tested in different
chlorides, namely MgCl2 , NaCl, and CaCl2 . Microstructural characterization was per-
formed by scanning electron microscopy. AHSSs are used in the automotive industry in
environments with a lot of snow and de-icing salts.

2. Materials and Methods

2.1. Materials
The most common AHSS grades in commercial use today are ferritic–bainitic (FB)
and dual-phase (DP) steels, which were given the designations FB780 (Yield Strength
(YS) = 780 MPa) for a ferrite–bainite microstructure and DP780 (YS = 780 MPa) for a ferrite–
martensite microstructure. The chemical compositions of the DP and FB AHSSs utilized
in this study, as determined by X-ray fluorescence (Olympus DELTA XRF, Houston, TX,
USA), are listed in Table 1.

Table 1. Chemical composition of different AHSS (wt.%).

Element DP780 FB780

Fe Balance Balance
C 0.10 0.09
Mn 2.61 1.73
Cr 0.420 0.640
Mo - 0.006
Si 0.510 0.300
Ti 0.080 0.021

2.2. Microstructural Characterization

The samples of the AHSSs were prepared using the metallography technique [34],
using different SiC grit papers until grades of 4000 were achieved. An alumina suspension
of 0.1 µm was used to obtain the microstructure. A five-weight percent Nital solution was
used to etch the samples chemically. Lastly, a secondary electron (SE) detector was used
to investigate the samples’ microstructures by scanning electron microscopy (SEM, JEOL-
JSM-5610LV, Tokyo, Japan) at a magnification of 2000×. In order to test for electrochemical
corrosion, AHSS samples were ground to 800-grit SiC paper.

2.3. Electrochemical Technique

In order to assess the corrosion behavior of various AHSSs in 3.5 weight percent NaCl,
2 weight percent CaCl2 , and 2 weight percent MgCl2 solutions, the EN measurements were
conducted at room temperature using a standard three-electrode cell, as shown in Figure 3
[two nominally identical specimens were used as the working electrodes (WE1 and WE2)
and a saturated calomel electrode as the reference electrode (RE), respectively]. The EN
measurements were conducted following ASTM G199-09 [35–38]. A scanning rate of one
data point per second was used to measure 1024 data points in each trial. A Gill-AC poten-
tiostat/galvanostat/ZRA (Zero Resistance Ammeter) from ACM Instruments (Manchester,
UK) was used to record the EN measurements simultaneously. The measurements were
carried out twice.
A program developed in MATLAB 2018a software (Math Works, Natick, MA, USA)
was used to handle data analysis obtained from EN measurements. Energy dispersion plots
(EDPs) were used in the frequency–time domain analysis, where the original signal (with
DC) was subjected to the orthogonal wavelet transform. In order to obtain the intrinsic
 scanning rate of one NaCl, 2 weight
data point percentwas
per second CaCl 2, and 2 weight percent MgCl2 solutions, the EN
used to measure 1024 data points in each
measurements were conducted at room temperature using a standard three-electrode cell,
trial. A Gill-AC potentiostat/galvanostat/ZRA (Zero Resistance Ammeter) from ACM In-
as shown in Figure 3 [two nominally identical specimens were used as the working
struments (Manchester, UK) was used to record the EN measurements simultaneously.
electrodes (WE1 and WE2) and a saturated calomel electrode as the reference electrode
The measurements were(RE), carried out twice.
respectively]. The EN measurements were conducted following ASTM G199-09 [35–
Metals 2024, 14, 1208 A program developed in MATLAB
38]. A scanning 2018a
rate of one software
data point per(Math
secondWorks,
was usedNatick, MA,1024
to measure USA)data points in
5 of 17
was used to handle each
datatrial.
analysis obtained
A Gill-AC from EN measurements.
potentiostat/galvanostat/ZRA (Zero Energy dispersion
Resistance Ammeter) from ACM
Instruments
plots (EDPs) were used (Manchester, UK)domain
in the frequency–time was used to recordwhere
analysis, the ENthe
measurements simultaneously.
original signal
The measurements
(with DC) was subjected were carried
to the orthogonal outtransform.
wavelet twice. In order to obtain the in-
functions (IMF) of the EN signal by aninempirical decomposition method (EMD), EN
trinsic functions (IMF) ofAtheprogram developed
EN signal MATLAB 2018a
by an empirical software (Math
decomposition Works,
method Natick,
(EMD), MA, USA)
analysis with the Hilbert–Huang
was used to handle transform (HHT)
data analysis was from
obtained required. Afterward,Energy
EN measurements. instantaneous
dispersion
EN analysis with the Hilbert–Huang transform (HHT) was required. Afterward, instanta-
frequencies plots (EDPs)
werewere
shown usingwere used in the
a Hilbert frequency–time domain analysis, where the original signal
spectrum.
neous frequencies shown using a Hilbert spectrum.
(with DC) was subjected to the orthogonal wavelet transform. In order to obtain the
intrinsic functions (IMF) of the EN signal by an empirical decomposition method (EMD),
EN analysis with the Hilbert–Huang transform (HHT) was required. Afterward,
instantaneous frequencies were shown using a Hilbert spectrum.

Three-electrode
Figure3.3.Three-electrode
Figure cellcell
for for electrochemical
electrochemical noise noise (EN) measurements.
(EN) measurements.

3. Results
3. Resultsand
andDiscussion
Discussion
Figure 3. Three-electrode cell for electrochemical noise (EN) measurements.
3.1. Microstructure
3.1. Microstructure
3. Results and Discussion
Asshown
As shown in in Figure
Figure
3.1. 4a, hard
4a, hard islands
Microstructure islands martensite,
martensite, or bulk martensite,
or bulk martensite, and a soft fer-
and a soft ferrite
rite phase, or black
phase, or black grains, makegrains, make up the
up theinmicrostructure
As shown microstructure
of DP780
Figure 4a, hard islands of
steel. The
martensite, DP780
average
or bulk steel.
size ofThe
martensite, thea average
and soft ferrite
size of theislands
martensite martensite
ranges islands
phase,from ranges
5 tograins,
or black andfrom
55%, make their
up the 5relative
to 55%, andoftheir
volumes
microstructure vary
DP780 relative
steel. The volumes
accordingly [38– sizevary
average of the
41]. The microstructure
accordingly [38–41].martensite
The islands
of FB780 ranges
steel,
microstructure from
as shown 5 in
to 55%,
of FB780 Figure and4b,
steel, their relativeup
asisshown
made volumes
in of vary
30 and
Figure 4b,accordingly
is made [38–
45% up
41]. The microstructure of FB780(darksteel, grains),
as shownwith
fine
of 30bainite (bright
and 45% grains)
fine bainiteand soft ferrite
(bright matrix
grains) and soft ferriteinmatrix
Figure 4b, is made
an average
(darkgrain up of 30 and 45%
size
grains), with an
fine bainite (bright grains) and soft ferrite matrix (dark grains), with an average grain size
of approximately
average grain size4 and 2 µm, respectively
ofapproximately
approximately [42–45].
of 4 and4 2and
µm, 2 µm, respectively
respectively [42–45]. [42–45].

Figure 4. Microstructures of (a) DP780 and (b) FB780 steels by scanning electron microscopy (SEM).

3.1.1. Noise Impedance

The following formula expresses the noise impedance (Zn ), also known as spectral
noise resistance [46,47]: s
ψV ( f )
Zn = (1)
ψI ( f )
The PSD division of potential and current square root calculates Zn . The electrochemi-
cal noise impedance zero (Zn 0) is related to the corrosion resistance [47].
Figure 5 shows the noise impedance graphic (Zn ) of an DP780 alloy exposed in the dif-
ferent electrolytes. The alloy shows similar behavior in the three electrolytes. However, the
alloy exposed to NaCl exhibited higher corrosion resistance with a Zn 0 value of 918 Ω·cm2
(see Table 2). On the other hand, the alloy exposed to MgCl2 presented the lowest Zn 0
value, with 441 Ω·cm2 , indicating that the alloy presents faster corrosion degradation in
this medium. The DP780 obtained a value of 825 Ω·cm2 exposed to CaCl2 , indicating that
its corrosion resistance is like that of NaCl.
 ical noise impedance zero (Zn0) is related to the corrosion resistance [47].
Figure 5 shows the noise impedance graphic (Zn) of an DP780 alloy exposed in the
different electrolytes. The alloy shows similar behavior in the three electrolytes. However,
the alloy exposed to NaCl exhibited higher corrosion resistance with a Zn0 value of 918
Ω·cm2 (see Table 2). On the other hand, the alloy exposed to MgCl2 presented the lowest
Metals 2024, 14, 1208 Zn0 value, with 441 Ω·cm2, indicating that the alloy presents faster corrosion degradation
6 of 17
in this medium. The DP780 obtained a value of 825 Ω·cm2 exposed to CaCl2, indicating
that its corrosion resistance is like that of NaCl.

Figure 5.5.Noise
Noiseimpedance (Zn) for(Z
impedance DP780 in different electrolytes.
Figure n ) for DP780 in different electrolytes.

TableFigure 6 shows
2. Noise the noiseparameters.
impedance impedance of the FB780 alloy in different electrolytes. In
this graphic, the FB780 exposed to MgCl2 presented a different behavior; at high frequen-
cies, the Zn values did not change; however, when
Alloy exposed to NaCl and CaCl2, theZZ
Electrolyte 2
n 0 (Ω ·cm )
n

values increased at high frequencies. That behavior can be related to a more uniform cor-
NaCl
rosion process that occurs on the surface. Furthermore, the FB780 exposed to MgCl2 pre- 918 ± 24
DP780 MgCl
sented the highest Zn0 values of FB780 samples with 502 Ω·cm
2 2. In contrast, when FB780 ± 16
441
was exposed to NaCl, the Zn0 value was 409 Ω·cm2. CaCl2 825 ± 28
NaCl 409 ± 21
FB780 MgCl2 502 ± 14
CaCl2 432 ± 17

Figure 6 shows the noise impedance of the FB780 alloy in different electrolytes. In this
graphic, the FB780 exposed to MgCl2 presented a different behavior; at high frequencies,
the Zn values did not change; however, when exposed to NaCl and CaCl2, the Zn values
increased at high frequencies. That behavior can be related to a more uniform corrosion
process that occurs on the surface. Furthermore, the FB780 exposed to MgCl2 presented
Metals 2024, 14, x FOR PEER REVIEWthe highest Zn 0 values of FB780 samples with 502 Ω ·cm2 . In contrast,
7 of 20 when FB780 was

exposed to NaCl, the Zn 0 value was 409 Ω·cm2 .

Figure
Figure6. 6.
Noise impedance
Noise (Zn) for(Z
impedance FB780 in different electrolytes.
n ) for FB780 in different electrolytes.
Table 2. Noise impedance parameters.

Alloy Electrolyte Zn0 (Ω·cm2)

NaCl 918 ± 24
DP780 MgCl2 441 ± 16
CaCl2 825 ± 28
Metals 2024, 14, 1208 7 of 17

3.1.2. Time-Domain Analysis

Wavelets
A high–low filter is used with wavelets to separate a signal; high frequencies are
called details and low frequencies are approximations [45]. An N number of the data’s total
energy can be found using Equation (2) [47].

N
E= ∑ xn2 (2)
n −1

Additionally, Equation (3) provides the energy fractions of the details and approximations:

1 N 2 1 N
ED dj = ∑
E n =1
d j,n ED sj = ∑ s2j,n
E n =1
(3)

The total energy evaluated is equal to the energy of each wavelet transform component,
according to Equation (4):
j
Metals 2024, 14, x FOR PEER REVIEW E = ED sj ∑ ED dj 8 of 20 (4)
j =1

The authors linked the initial crystal energy, D1 to D3, to metastable pitting. While D7
andTheD8 authors linked the
are connected to initial crystal
diffusion energy, D1processes
or regulated to D3, to metastable pitting. While
(uniform corrosion), the crystals
D7 and D8 are connected to diffusion or regulated processes (uniform corrosion), the crys-
D4 through D6 are linked to localized corrosion [48,49].
tals D4 through D6 are linked to localized corrosion [48,49].
Figure 7 shows the energy dispersion plot for the DP780 alloy in the different elec-
Figure 7 shows the energy dispersion plot for the DP780 alloy in the different elec-
trolytes. DP780 showed energy accumulation from the D5 crystal, indicating that localized
trolytes. DP780 showed energy accumulation from the D5 crystal, indicating that localized
attacks
attacks were
were beginning.
beginning. Moreover,
Moreover, the major
the major amount amount of energy
of energy is accumulated
is accumulated in crystalsin crystals
D7 and D8, indicating that a uniform corrosion process is presented.
D7 and D8, indicating that a uniform corrosion process is presented. This behavior This behavior is
is as-
associated
sociated withwith a uniform
a uniform pittingpitting attack
attack on on the
the alloy alloy surface.
surface.

Figure
Figure7. 7.
Energy dispersion
Energy plot plot
dispersion of DP780 alloy. alloy.
of DP780

Figure 8 shows
Figure the the
8 shows energy dispersion
energy plot for
dispersion the for
plot FB780
thealloy
FB780in different
alloy in electrolytes.
different electrolytes.
FB780
FB780 exposed
exposedto NaCl and CaCl
to NaCl presented
and 2CaCl a similarabehavior
presented similar to DP780 alloys,
behavior to with en-
DP780 alloys, with
2
ergy accumulation at the D5 and D6 crystals, indicating that localized processes were
energy accumulation at the D5 and D6 crystals, indicating that localized processes were oc-
curring on metal surfaces. In addition, the energy accumulation at the D7 and D8 crystals
is associated with uniform corrosion provoked by a uniform pitting distribution.
Metals 2024, 14, 1208 8 of 17

Metals 2024, 14, x FOR PEER REVIEW 9 of 20

occurring on metal surfaces. In addition, the energy accumulation at the D7 and D8 crystals
is associated with uniform corrosion provoked by a uniform pitting distribution.

Figure
Figure8.8.Energy
Energydispersion plotplot
dispersion of FB780 alloy.alloy.
of FB780

Recurrence
Recurrence Plots and
Plots Hilbert–Huang
and Transform
Hilbert–Huang Transform
Recurrence
Recurrence plots are are
plots a useful tool for
a useful non-linear
tool system analysis.
for non-linear Various methodol-
system analysis. Various method-
ogies
ologies must be used to assess the type and progress of corrosionsurface
must be used to assess the type and progress of corrosion on the on thebecause
surface because
corrosion is a chaotic and non-linear system. An effective method for obtaining that anal-
corrosion is a chaotic and non-linear system. An effective method for obtaining that analysis
ysis is RPs.
is RPs.
Recurrence plots are time-function-realized, two-dimensional graphs. The path of xi
in Rm, Recurrence
where m is the plots aredimension,
spatial time-function-realized,
is given to I andtwo-dimensional
j at a time interval ofgraphs. The path of xi
ε. The times
in R , where m is the spatial dimension, is given to I and j at a time interval
ti andmtj from two dimensions are displayed as a two-dimensional square matrix by the RP. of ε. The times
t
The and t
i matrix from two dimensions are displayed
j is displayed in Equation (5) [50–53]: as a two-dimensional square matrix by the RP.
The matrix is displayed in Equation (5) [50–53]:
𝑅 𝜀 Θ 𝜀 − 𝑥⃗ − 𝑥⃗ , 𝑖, 𝑗 1, … , 𝑁 (5)
→ →
 
Rij (ε) = Θmaximum,
where ||.|| is the norm (Euclidean, ε − xi −or xManhattan),
j , i, j = µ1,is. .the distance umbral,
., N (5)
Θ(x) is the Heaviside function, and N is the number of data or points xi. Equation (4) illus-
trates
where the||.||
recurrence
is therate,
norm which determines
(Euclidean, the recurrence
maximum, density:
or Manhattan), µ is the distance umbral,
Θ(x) is the Heaviside function, and N is1 the number of data or points xi . Equation (4)
𝑅𝑅 𝜀 determines
illustrates the recurrence rate, which 𝑅 ,the recurrence density: (6)
𝑁
,
N
1
In an umbral zone, the recurrence rate (RR) indicates the likelihood of reconstructing
RR(ε) = 2 ∑ Ri, j (6)
a single track. N i, j=1
The diagonal lines of the RP show the system’s determinism and how the trajectory
has changed over time
In an umbral in the
zone, phase
the space. The
recurrence determinism
rate (DET)
(RR) indicates is computed
the likelihoodusing the
of reconstructing
following equation:
a single track.
The diagonal lines of the RP show∑the system’s 𝑙𝑝 𝑙 determinism and how the trajectory
𝐷𝐸𝑇 (7)
has changed over time in the phase space. ∑ The𝑙 𝑝 determinism
𝑙 (DET) is computed using the
following equation:
Long diagonal lines on the RP are necessary for periodicity, and DET approaches
N
unity; stochastic signals result in solitary dots, ∑
which l p(l ) DET to values near zero.
l =lminrestricts
DET = (7)
N
∑ l p(l )
l =1
Metals 2024, 14, 1208 9 of 17

Long diagonal lines on the RP are necessary for periodicity, and DET approaches
unity; stochastic signals result in solitary dots, which restricts DET to values near zero. The
average diagonal line length (L), another RQA metric associated with diagonal lines, is
depicted as follows in Equation (8):

∑lN=lmax l p(l )
L= (8)
∑lN=lmin p(l )

TT gives the average length of the vertical structures and indicates the average time
the system spends in a given condition (as indicated by the number of recurrence points);
see Equation (9).
∑vN=vmin v P(v)
TT = (9)
∑vN=vmin P(v)
The electrochemical phenomenon that takes place throughout the corrosion process is
described by the electrochemical noise (EN) technique. The Hilbert–Huang analysis is one
methodology used to describe the EN method. This technique facilitates the frequency and
timing of energy exchanges; the energy, known as instantaneous energy, is derived from the
signal’s inherent function and is retrieved by signal decomposition [54–56]. Equation (10)
explains the empirical method of decomposition (EMD):

N
x (t) = ∑ h (i ) ( t ) + d ( t ) (10)
i =1

where d(t) is the average of the trend at a low frequency of the time series x(t) and cannot be
decomposed; h(i) (t) is the i-th term of IMF that is generated; these numbers must satisfy the
conditions that the extreme and cross numbers are equal or differ by a maximum of 1 and
that each point using the local maximum and minimum must be 0. The HHT is represented
by Equation (11):
Z ∞
1 h j (τ )
y j (t) = p dτ (11)
π −∞ t − τ
where p is connected to the Cauchy principle and is associated with an average of IMF; yj (t)
is the Hilbert transform, and IMF is represented by hj .
Figure 6 shows the signal analysis results by RPs and HHT, comparing the results
with optical microscopy. Figure 9a shows the graphics of DP780 exposed to NaCl, where
the RP showed a high determinist behavior with a value of 0.9769 (see Table 3) and RR
of 0.0562. The RP presents some blue points in the graphics, indicating that a process
occurs at that time. It can be related to the energy presented at middle frequencies in the
Hilbert specter. That behavior is associated with localized corrosion; however, the high
DET value (indicating a uniform process) can be related to the corrosion process in the
material; a galvanic couple occurs in the superficies of dual-phase alloy. The dominance of
uniform process that occurs in a surface is related to the corrosion process that consists of
the diffusion of ions on the metal surface, that attacks in specific zones (the more susceptible
phase), generating localized attacks (energy at middle frequencies and blue zones in RP)
that generate a uniform pitting attack. Finally, the localized attack occurs in the ferrite
phase. All the DP780 samples from Figure 9a–c show this behavior. Figure 9c shows a
similar behavior with a high DET value (0.9844). It can be related to oxygen diffusion, so
the microscopy shows a highly corroded area; however, when zoomed in to a microscopic
level, it can be observed how the corrosion is occurring in preference zones (ferrite), being
governed by the process described previously.
Figure 10 shows the results of FB780 alloy exposed to the different electrolytes.
Figure 10a,c show similar behavior in DP780, indicating that a uniform process occurs on
the surface. However, the uniform process from the surface will attack preferent zones,
principally ferrite zones. For that reason, in the Hilbert specter, energy is accumulated
 Metals 2024, 14, x FOR PEER REVIEW 11 of 20

However, after some exposure time, energy begins to appear at middle frequencies, indi-
Metals 2024, 14, 1208 cating that localized processes are occurring, and due to the galvanic couple in ferrite 10 of 17
zones, the attacks will be uniform after some time.
In contrast, Figure 10b shows a localized process; in this case, the value of RR in-
creases to 0.0823 (in comparison with the other values between 0.05 and 0.06). Also, L and
at the beginning of the time period at low frequencies due to ion diffusion in the metal
Tʹs values are higher than those obtained in the other samples (10.07 and 13.92); those
surface. However, after some exposure time, energy begins to appear at middle frequencies,
values are related to the time of recurrence point occurrence. The recurrence points are
indicating that
related to thelocalized processes
localized process, andare occurring,
a high value ofand due
these twotoparameters
the galvanic couple
indicates thein ferrite
zones, the attacks will
localization process. be uniform after some time.

Metals 2024, 14, x FOR PEER REVIEW 12 of 20

Figure 9. Recurrence
Figure 9. Recurrenceplots,
plots, Hilbert specter,
Hilbert specter, and
and microscopy
microscopy analysis
analysis for DP780
for DP780 exposedexposed to (a) NaCl,
to (a) NaCl,
(b) MgCl 2, and (c) CaCl2.
(b) MgCl2 , and (c) CaCl2 .
Metals 2024, 14, 1208 11 of 17

Table 3. Recurrence plots parameters.

Alloy Electrolyte RR DET L TT

NaCl 0.0562 ± 0.0002 0.9769 ± 0.001 5.06 ± 0.02 6.51 ± 0.05
DP780 MgCl2 0.0592 ± 0.0001 0.9831 ± 0.0002 6.28 ± 0.09 8.16 ± 0.09
CaCl2 0.0589 ± 0.0004 0.9844 ± 0.0004 5.04 ± 0.005 6.48 ± 0.07
NaCl 0.0593 ± 0.0002 0.987 ± 0.0008 6.26 ± 0.008 8.12 ± 0.05
FB780 MgCl2 0.0823 ±plots,
Figure 9. Recurrence 0.0001 0.9391
Hilbert specter, and±microscopy
0.0001 analysis10.07 ± 0.03
for DP780 13.92 ± 0.2
exposed to (a) NaCl,
CaCl2 (b) MgCl2, and0.06 ± 0.004
(c) CaCl 2. 0.9142 ± 0.0001 4.17 ± 0.08 5.45 ± 0.03

Metals 2024, 14, x FOR PEER REVIEW 13 of 20

Figure
Figure 10. Recurrenceplots,
10. Recurrence plots, Hilbert
Hilbert specter,
specter,andand
microscopy analysis
microscopy for FB780for
analysis exposed
FB780to exposed
(a) NaCl, to (a) NaCl,
(b) MgCl2, and (c) CaCl2.
(b) MgCl2 , and (c) CaCl2 .
Table 3. Recurrence plots parameters.

Alloy Electrolyte RR DET L TT

NaCl 0.0562 ± 0.0002 0.9769 ± 0.001 5.06 ± 0.02 6.51 ± 0.05
DP780 MgCl2 0.0592 ± 0.0001 0.9831 ± 0.0002 6.28 ± 0.09 8.16 ± 0.09
CaCl2 0.0589 ± 0.0004 0.9844 ± 0.0004 5.04 ± 0.005 6.48 ± 0.07
Metals 2024, 14, 1208 12 of 17

In contrast, Figure 10b shows a localized process; in this case, the value of RR in-
creases to 0.0823 (in comparison with the other values between 0.05 and 0.06). Also, L
and T’s values are higher than those obtained in the other samples (10.07 and 13.92); those
values are related to the time of recurrence point occurrence. The recurrence points are
related to the localized process, and a high value of these two parameters indicates the
localization process.

4. Discussion
Two basic reactions dominate the corrosion process:

Fe → Fe2+ + 2e− (12)

O2 + 2H2 O + 4e− → 4OH− (13)

Those reactions generate an active oxidation; when oxygen is diffused on the surface,
the corrosion products generated are porous and do not give passivation to the surface.
That facilitates the attack of Cl− ions on the ferrite phase, generating a localized attack
and avoiding the passivation of surface-generating pitting in the ferrite zone [57,58]. The
following reactions govern the chemical reaction:

Fe2+ + Cl− → FeCl2 (14)

FeCl2 + H2 O → Fe(OH)2 + 2Cl− (15)

This alloy type’s corrosion process depends on the metal matrix’s metallurgical het-
erogeneities and the passive layer’s absence [58,59]. The presence of cathodic and anodic
zones due to the difference in phases, grain variations, and impurities, and the lack of ho-
mogeneity is conducive to localized attacks. For these alloys, the phase difference generates
galvanic corrosion [60].
The cathode role of bainite and martensite, due to the oxygen reception, made ferrite
act as an anode due to the low presence of O2 , making it susceptible to OH− and Cl−
attacks [61].
The dissolution process was generated in uniform form in ferrite, so the results of RPs
and HHT presented high activity at low frequencies, which was conducive to initiating
some localized attacks. Also, some authors consider that the corrosion process in this class
of alloys is not only for the galvanic couple; it can be generated by an auto-corrosion of the
only phase in double-phase steels [62–64].
The corrosion mechanism of DP780 and FB780 presented previously can be com-
plemented with a uniform dissolution of the area when exposed to CaCl2 . This occurs
due to the effect of the solution in ferrite, martensite, and bainite, generating a galvanic
couple through an auto-corrosion process. The ferrite dissolution provoked active zones,
and the uniformly distributed pitting was connected, generating a uniform dissolution of
material, as shown in Figure 11 [64,65]. Therefore, the RPs and HHT showed high energy
accumulation at middle and high frequencies due to localized processes (at middle and
high frequencies) that provoke uniform attacks (at high frequencies).
The corrosion behavior of FB780 steel with a ferrite–bainite microstructure in CaCl2
and MgCl2 solutions presents localized corrosion, where the bainite phase dissolved faster
than the ferrite phase because it acted as an anode. The iron carbides (green dots) acted as
cathodes, as Figure 10a indicated. The disintegration process of ferrite–martensite DP780
steel in test solutions is depicted in Figure 10b. Because it functions as a cathode, martensite
acts as a barrier to corrosion, and the continuous ferrite-phase matrix restricts the spread
of corrosion.
In the case of ferrite–bainite DP, the microstructure influences the corrosion initiation
of the Cr-Mo alloyed steel. Zones with low Cr-Mo content generates more crystal defects,
decreasing the potential and increasing the susceptibility of microgalvanic corrosion. The
Metals 2024, 14, 1208 13 of 17

Metals 2024, 14, x FOR PEER REVIEW

ferrite phase works as a cathode for a higher Cr-Mo concentration, and the bainite15isof 20

dissolved [65–68].

Figure 11. Schematic representation

Figure 11. of corrosion
Schematic representation in (a) ferrite–bainite
of corrosion FB780
in (a) ferrite–bainite steel/CaCl
FB780 2 -MgCl
steel/CaCl 2-MgCl22, (b)

dual-phase
(b) dual-phase DP780 DP780solutions.
steel/test steel/test solutions.

It is importantIt is
toimportant
mentiontothe mention of Cl− ofions;
the aggression Cl ions; in several research studies,
studies, dif-
−
aggression in several research
ferent alloys have been exposed to this medium, demonstrating that Cl − − will attack the
different alloys have been exposed to this medium, demonstrating that Cl will attack
more susceptible zones, provoking localized corrosion in this part and generating a more
the more susceptible zones, provoking localized corrosion in this part and generating
aggressive attack. It can be observed with energy at the middle crystals in a wavelets anal-
a more aggressive
ysis orattack.
at middle It frequencies
can be observed
in the HHT with energy
studies at the
[69–73]. For middle crystals
these alloys, in a be-
the attacks
wavelets analysis or at middle frequencies in the HHT studies [69–73]. For
gan at the ferrite-phase or inclusion zones; authors such as Macdonald [73–76] describethese alloys, the
attacks began at
thisthe ferrite-phase
phenomenon withor
theinclusion
point defectzones;
model, authors
indicatingsuchthatasthe
Macdonald
passive layer [73–76]
generated
describe this phenomenon with the
on a material surface pointdefects
presents defectofmodel,
cation andindicating that the generating
oxygen vacancies passive layerand an-
generated on anihilating
material the metal/film
surface and film/solution
presents defects of cationinterfaces, being a similar
and oxygen process
vacancies to high-tem-
generating
perature
and annihilating oxidation. FBand
the metal/film steelfilm/solution
shows a higherinterfaces,
corrosion kineticbeing due to the ferritic
a similar processphasetoma-
trix; as it is more present in the material, the anode is higher, and corrosion resistance
high-temperature oxidation. FB steel shows a higher corrosion kinetic due to the ferritic
decreases.
phase matrix; as it is more present in the material, the anode is higher, and corrosion
Due to the non-linear signal characteristics, the analysis by methods such as wavelets,
resistance decreases.
HHT, and RPs are crucial in these complex systems. This research showed that a non-
Due to theconventional
non-linear EN signal characteristics,
analysis the analysis
is helpful to determine the by methods
attacks suchcouples,
in galvanic as wavelets,
support-
HHT, and RPsing arewavelets
crucialwithin these
HHT andcomplex systems.
RPs methods. It is This research
possible showed
to analyze that ainnon-
the changes the cor-
conventional EN analysis
rosion is helpful
process to time,
within the determine
and nottheonlyattacks
with ain galvanic
scalar aspect,couples, supporting
as in conventional meth-
ods. With
wavelets with HHT andtheRPsHHT and RPsItmethods,
methods. is possibleit was possible to
to analyze thedetermine
changesthe in moment of pitting
the corrosion
process withinattack and nucleations.
the time, and not only Also,with
whenaonlyscalarlocalized
aspect, corrosion was present, it could
as in conventional be iden-
methods.
tified with these methods [77–89].
With the HHT and RPs methods, it was possible to determine the moment of pitting attack
However, with wavelets, HHT, and RPs, it is not possible to determine the corrosion
and nucleations. Also, when only localized corrosion was present, it could be identified
resistance of a material; for that reason, it is important to complement with a noise imped-
with these methods [77–89].(Zn) due to the certainty of this analysis in determining the corrosion re-
ance analysis
However,sistance.
with wavelets, HHT, and
With this analysis, RPs,
it was it is not
possible possiblethe
to determine to high
determine
corrosion the corro- of
resistance
sion resistanceDP780
of a material; for that
in comparison reason,
to FB780 it different
in the is important to complement with a noise
electrolytes.
impedance analysis (Zn ) due to the certainty of this analysis in determining the corrosion
5. this
resistance. With Conclusions
analysis, it was possible to determine the high corrosion resistance of
DP780 in comparison DP780 and FB780
to FB780 presented
in the differenta galvanic couple with an auto-corrosion process on the
electrolytes.
surface. The corrosion process is generated by an ion diffusion in the surface (a uniform
5. Conclusionsprocess) that attacks specific zones such as ferrite, inclusions, or some defects (localized
process) and mitigates the attack of Cl− that dissolves the ferrite phase uniformly, connect-
DP780 and FB780 presented a galvanic couple with an auto-corrosion process on
ing the pitting distributed in a uniform way and dissolving the surface.
the surface. The corrosion process
Wavelets, RPs, is generated
and HHT bythe
help identify ancorrosion
ion diffusion
process in
thatthe surface
occurs on the(asur-
uniform process) that attacks specific zones such as ferrite, inclusions, or some defects
face. The RPs help to find the recurrence zones where some localized attacks (galvanic
(localized process) and mitigates the attack of Cl− that dissolves the ferrite phase uniformly,
connecting the pitting distributed in a uniform way and dissolving the surface.
Wavelets, RPs, and HHT help identify the corrosion process that occurs on the surface.
The RPs help to find the recurrence zones where some localized attacks (galvanic coupling)
Metals 2024, 14, 1208 14 of 17

occur; in this case, the blue zones of the RPs indicate the uniform attacks generated by the
dissolution of the material.
The presence of inclusions influences the beginning of localized attacks.
The Zn parameter showed that DP780 presented a higher corrosion resistance
(918 Ω·cm2 and 825 Ω·cm2 ) than FB780 exposed to NaCl and CaCl2 . However, DP780
presented a lower noise impedance when exposed to MgCl2 (441 Ω·cm2 ).
Parameters such as L (diagonal line) and TT (the average length of the vertical struc-
tures) help determine the corrosion type on the material’s surface. A high value of these
parameters is related in this research to localized corrosion, indicating the time associated
with the change in one process, as presented with FB780 exposed to MgCl2 (10.07 and 13.92).
As the uniform process occurs constantly, the TT value is going to be lower (4.17–6.2).

Author Contributions: Conceptualization, F.A.-C., M.M.-R. and C.G.-T., methodology, M.M.-R.,

F.E.-L., E.M.-B., M.L.-B., J.M.J.-M. and L.L.-R. data curation, F.A.-C., L.L.-R., D.N.-M., F.A.-C. M.A.B.-
Z. and F.E.-L.; formal analysis, F.A.-C., C.G.-T., M.M.-R., E.M.-B., M.A.B.-Z., L.L.-R., D.N.-M., M.L.-B.
and C.G.-T.; writing—review and editing, F.A.-C., J.M.J.-M. and C.G.-T. All authors have read and
agreed to the published version of the manuscript.
Funding: This research received no external funding.
Data Availability Statement: The raw data supporting the conclusions of this article will be made
available by the authors on request.
Acknowledgments: The authors would like to thank the UANL-CA-316 working group and Univer-
sidad Autónoma de Nuevo León (UANL) for the facilities given to developing this investigation.
Conflicts of Interest: The authors declare no conflicts of interest.

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