metals

Article
Fatigue Study of the Pre-Corroded 6082-T6 Aluminum
Alloy in Saline Atmosphere
Alejandro Fernández Muñoz 1 , José Luis Mier Buenhombre 2, *, Ana Isabel García-Diez 2 ,
Carolina Camba Fabal 2 and Juan José Galán Díaz 2
1 Navantia, Polígono Astilleros, S/N, 11519 Puerto Real, Spain; alfemu78@hotmail.com
2 Escuela Politécnica Superior, University of A Coruña, Mendizábal s/n, 15403 Ferrol, Spain;
ana.gdiez@udc.es (A.I.G.-D.); ccamba@udc.es (C.C.F.); juan.jose.galan@udc.es (J.J.G.D.)
* Correspondence: jose.mier@udc.es; Tel.: +34-881-013-268




Received: 24 July 2020; Accepted: 15 September 2020; Published: 18 September 2020


Abstract: This work studies the influence of the saline atmospheric corrosion on the fatigue strength
of 6061-T6 aluminum alloy. For this purpose, this alloy was subjected to tests in a salt spray
corrosion chamber at different exposure times (1, 2, and 3 months) according to ASTM B117 standard.
The morphological study of the pits was carried out by confocal microscopy. Subsequently, fatigue tests
were performed at variable stresses whose maximum stress (Smax ) was between 30% and 95% of the
yield strength (S0 ) in order to keep them within the zone of elastic behavior of the material. Data were
analyzed using the Basquin equation and the maximum likelihood function method. The results
show a similar decrease in the conventional fatigue limit (2 × 106 cycles) after one month (98 MPa)
and two months (91 MPa) of corrosion. After three months of corrosion, the material showed a very
important reduction in the fatigue limit (68 MPa) with respect to the uncorroded material (131 MPa).
The data of Se /S0 (fatigue limit/yield strength) versus the ratio Pm /Dm (pit average depth/pit diameter
at zero depth) can be fitted to a logarithmic curve.

Keywords: 6061-T6 aluminum alloy; pitting; confocal microscopy; fatigue; Basquin’s equation;
maximum likelihood method

1. Introduction
Aluminum alloys have great advantages in shipbuilding and offshore platforms applications
thanks to their lightweight, specific strength, and corrosion resistance. AlMg (series 5xxx) and AlMgSi
(series 6xxx) are the most commonly used aluminum alloys in seawater [1]. One of them is 6061alloy,
which is used for general purposes in the form of extruded profiles because the combination of
mechanical properties and adequate corrosion resistance makes it one of the most versatile aluminum
alloys in marine applications. Its good mechanical properties are due to the aging treatment, which can
be natural (T4) or artificial (T6). 6061 aluminum alloys have %Mg + %Si (wt) in amounts greater than
1.4%, which favors the increase in mechanical resistance after heat treatment compared with other alloys
such as 6063. Magnesium and silicon form Mg2 Si compound, which behaves like a semiconductor [2,3].
Additionally, it contains amounts of Cu around 0.25% to improve corrosion resistance and 0.7%
Fe, which results in the precipitation of the ternary compounds Alx Fey Siz [4,5]. All these types
of precipitates favor the appearance of localized corrosion due to the difference in electrochemical
potentials between them and the matrix [6,7]. 6061 alloy is less resistant to pitting corrosion than
non-aging AlMg alloys, especially in T6 condition, in the presence of chloride ions and poorly aerated
deep water with low pH. The study of pitting corrosion can be carried out according to the ASTM
G46 standard [8] to determine the morphology, density, size, and depth of the pits and to predict the
remaining service life of the alloy. According to this standard, the pitting factor (Fp ) can be calculated

Metals 2020, 10, 1260; doi:10.3390/met10091260 www.mdpi.com/journal/metals

Metals 2020, 10, x FOR PEER REVIEW 2 of 11
Metals 2020, 10, 1260 2 of 11

standard, the pitting factor (Fp) can be calculated by dividing the deepest metal penetration by the
average
by dividing metal
thepenetration
deepest metal when corrosion
penetration byistheuniform.
averageOne metalinstrumental
penetration whenway to parameterize
corrosion the
is uniform.
pits
Oneisinstrumental
to use confocal waymicroscopy.
to parameterize This technique
the pits isisto anuse
extension
confocalof microscopy.
conventionalThis microscopy,
technique which
is an
allows
extensionto perform the three-dimensional
of conventional microscopy, which characterization
allows to perform of the three-dimensional
materials’ surfacecharacterization
and is a very
interesting non-contact
of the materials’ surfacetechnique
and is a very for the study ofnon-contact
interesting pitting as ittechnique
is possiblefor to the
obtain
studyfinerof details
pitting ofas the
it is
morphology of a surface
possible to obtain because
finer details of oftheits higher lateral
morphology of aresolution.
surface because of its higher lateral resolution.
In
Inaddition,
addition,ititisisimportant
importantto totake
takeinto
intoaccount
accountthatthatmarine
marinestructures
structuresmay maybebesubject
subjectto tocyclical
cyclical
loads
loads of of different
different nature.
nature. TheTheformation
formationofofpits pitshas
hasaa detrimental
detrimentaleffecteffect on
on the
the fatigue
fatigue strength
strength
aluminum
aluminum alloy.alloy. Pits
Pitscan
canbebe cracking
cracking nuclei
nuclei underunder
cycliccyclic
loadsloads
that canthat can compromise
compromise structural structural
integrity
integrity
as a result asofa the
result of of
effect thestress
effectconcentration
of stress concentration
[9–11]. There [9–11]. There areinsituations
are situations which theinstructures
which the of
structures
6061-T6 alloysof 6061-T6
can be alloys
corrodedcanby bethecorroded
effect ofbythe
thesaline
effectatmosphere
of the saline atmosphere
and subsequently andbe subsequently
subjected to
be subjected
cyclic stresses to of
cyclic
low stresses
intensityofandlowhighintensity and high
frequency frequency
(vibrations) and(vibrations) and high
high intensity and low intensity and
frequency
low frequency
(waves). In the(waves).
former, In the former,
failure can occur failure
aftercan occur
a high after a of
number high number
cycles, whileofincycles, whilefracture
the latter, in the
latter,
occursfracture
at a muchoccurs
lower at a much
number lower There
of cycles. number of cycles.
are many There
studies that are
havemany studiesthethat
determined have
influence
determined
of pitting onthe theinfluence of pitting
fatigue strength of on the fatigue
aluminum strength
alloys [12–15].of However,
aluminumlittle alloys
has[12–15]. However,
been investigated
little
on the has been investigated
fatigue on the fatigue
behavior of AlMgSi alloys in behavior of AlMgSi
the presence alloys
of a high saltinconcentration.
the presence of Thea high salt
objective
concentration. The objective of this work is to provide information on the resistance
of this work is to provide information on the resistance to fatigue of this type of alloy in the extreme to fatigue of this
type of alloy inmentioned,
environments the extreme environments
given that many of mentioned, givenof
the applications that many
these of require
alloys the applications of these
good performance
alloys require
in saline good performance in saline atmospheres.
atmospheres.
The
Thepresent
presentresearch
research was
was carried
carriedout out inin two
two stages.
stages.Firstly,
Firstly,the
the pits
pits generated
generatedin inaa highly
highlysaline
saline
environment
environment were were dimensionally
dimensionally characterized
characterizedininorder orderto toevaluate
evaluatethe themain
mainpitting
pittingparameters.
parameters.
Secondly,
Secondly, the therelationship
relationshipbetween
betweenthethe severity
severityof pitting
of pittingandand
the the
decrease of fatigue
decrease strength
of fatigue was
strength
analyzed.
was analyzed.

2.2.Materials
Materialsand
andMethods
Methods
Sheets of 6082-T6
Sheets 6082-T6alloy
alloywith
with2 mm
2 mmof thickness werewere
of thickness used.used.
The composition (%wt) of
The composition this material
(%wt) of this
is as follows:
material is as 0.7–1.2%
follows: Si, 0.6–1.2%
0.7–1.2% Si,Mg, 0.4–1.0%
0.6–1.2% Mg,Mn, 0.50% Fe,
0.4–1.0% Mn,0.10%
0.50%Cu,
Fe,0.25% Cr,Cu,
0.10% 0.20% Zn,Cr,
0.25% and0.20%
0.10%
other elements, Al balance. Before any test, the material was machined according
Zn, and 0.10% other elements, Al balance. Before any test, the material was machined according to the ASTM E-8/E
to
8M-08
the ASTMstandard
E-8/E[16] to obtain
8M-08 the samples
standard [16] toused throughout
obtain this work.
the samples used Its dimensions
throughout arework.
this shownIts in
Figure 1. The
dimensions areorientation of the samples
shown in Figure was chosenofso
1. The orientation that
the the main
samples wasaxis of the
chosen sospecimen was parallel
that the main axis of
to the
the direction
specimen wasofparallel
rolling. to the direction of rolling.

1. (a)
Figure 1.
Figure (a) Dimensions
Dimensionsofof
thethe
specimens
specimens(in mm) used in
(in mm) the in
used tensile
the test and test
tensile fatigue
andtest, (b) orientation
fatigue test, (b)
of the specimens
orientation with respect
of the specimens to the
with rolling
respect to direction ofdirection
the rolling the metalofsheets.
the metal sheets.

The corrosion
The corrosiontests were
tests werecarried out inout
carried a saltinspray chamber
a salt sprayDYCOMETAL SSC 400 (DYCOMETAL
chamber DYCOMETAL SSC 400
EQUIPOS CONTROL DE CALIDAD, S.L., Barcelona, Spain)
(DYCOMETAL EQUIPOS CONTROL DE CALIDAD, S.L., Barcelona, Spain) according according to ASTM B117 standard
to ASTM[17].
According
B117 standardto this
[17].standard,
According thetosalt
thissolution
standard,was theprepared by dissolving
salt solution 5 parts
was prepared byby mass of sodium
dissolving 5 parts
chloride (Merck, Darmstadt, Germany) in 95 parts of water. The
by mass of sodium chloride (Merck, Darmstadt, Germany) in 95 parts of water. The salt salt used contained, as set
usedby
the standard, less than 0.3% by mass of total impurities. The pH of the saline
contained, as set by the standard, less than 0.3% by mass of total impurities. The pH of the saline solution was 6.5,
the saline
solution wasconcentration
6.5, the saline was 15%, and thewas
concentration pressure wasthe
15%, and between 0.9 was
pressure and 1.0 bar. The
between temperature
0.9 and 1.0 bar.
inside the chamber was 35 ◦ C. The samples were corroded for 1 month (C1), 2 months (C2), and 3
The temperature inside the chamber was 35 °C. The samples were corroded for 1 month (C1), 2
months(C2),
months (C3).andThe loss of mass
3 months (C3). due to corrosion
The loss of mass due wastodetermined with
corrosion was a SCALTEC
determined precision
with a SCALTECscale
model SBC
precision 22 (SCALTEC
scale model SBCInstruments
22 (SCALTEC GmbH, Goettingen,
Instruments Germany)
GmbH, with an accuracy
Goettingen, Germany)ofwith
0.01 mg.
an
accuracy of 0.01 mg. Weight measurements were made before and after the corrosive attack and
 Metals 2020, 10, x FOR PEER REVIEW 3 of 11
Metals 2020, 10, 1260 3 of 11

carefully removing impurities on the surface. The analysis of the corrosion products was done with a
WeightD5000 SIEMENS were
measurements X-raymadediffractometer
before and (SIEMENS,
after the Munich,
corrosiveGermany).
attack andThe Diffractplus
carefully removingV.8.0 (8.0,
Bruker
impurities on AXS Advanced
the surface. TheX-ray Solutions
analysis GmbH, Karlsruhe,
of the corrosion products Germany)
was done with and Bruker-AXS
a D5000 SIEMENS (Bruker AXS
Advanced X-ray
X-ray diffractometer Solutions
(SIEMENS, GmbH,
Munich, Karlsruhe,
Germany). TheGermany)
Diffractplus software programs
V.8.0 (8.0, Bruker AXS were used for data
Advanced
acquisition
X-ray Solutions and processing.
GmbH, Karlsruhe, Germany) and Bruker-AXS (Bruker AXS Advanced X-ray Solutions
Morphological
GmbH, Karlsruhe, Germany) studies of the
software pits werewere
programs performed
used for bydata
confocal microscopy
acquisition using a Sensofar PLμ
and processing.
Morphological studies of the pits were performed by confocal microscopy using awas
2300 dual microscope (SENSOFAR, Terrassa, Spain). The acquisition of data donePLµ
Sensofar using the
Gwyddion
2300 dual microscope (Czech MetrologyTerrassa,
(SENSOFAR, Institute, Brno, The
Spain). Czech Republic)
acquisition and was
of data SensoMAP
done using (SENSOFAR,
the
Gwyddion (Czech Metrology Institute, Brno, Czech Republic) and SensoMAP (SENSOFAR, Terrassa, by a
Terrassa, Spain) computer packages. Scanning electron microscopy (SEM) image was obtained
Spain) JEOL JSM 6400
computer microscope
packages. Scanning (JEOL, Tokio,
electron Japan). (SEM) image was obtained by a JEOL JSM
microscopy
The equipment
6400 microscope (JEOL, Tokio, used for the tensile and fatigue tests was a servo-hydraulic universal testing
Japan).
machine Instron 8800
The equipment used for the tensile with Fast Track controller
and fatigue tests(Instron, Norwood, Massachusetts,
was a servo-hydraulic universal testingMA, USA).
machine Axial stresses
Instron 8800 were
with applied in the controller
Fast Track direction of(Instron,
alloy rolling. The software
Norwood, used for MA,
Massachusetts, the tests design is
USA).
WaveMaker
Axial stresses were (WaveMaker,
applied in the Inc.,Mountain
direction of alloy View, California,
rolling. CA, USA).
The software used The
for the100tests
kN design
load cellis has a
force relative error over the entire measurement range of
WaveMaker (WaveMaker, Inc.,Mountain View, California, CA, USA). The 100 kN load cell has a force 0.22%. The temperature and humidity
relativeconditions
error overwere environmental.
the entire measurement Therange
oxideoflayer 0.22%. of the
Thetest samples was
temperature and not removed
humidity in both kinds
conditions
of tests in order to obtain similar conditions to those of service
were environmental. The oxide layer of the test samples was not removed in both kinds of tests of the material. Therefore, theintests are
carried out with the surface in the same conditions that are presented
order to obtain similar conditions to those of service of the material. Therefore, the tests are carried out in service, without previously
with thetreating
surfacethem.
in theThesame fatigue tests were
conditions that arecarried out byinapplying
presented a periodic
service, without axial load
previously of constant
treating them. stress
amplitude with a stress ratio (R = S /S ) of 0.1 and a frequency
The fatigue tests were carried out by applying a periodic axial load of constant stress amplitude with
min max of 15 Hz. As a criterion for athe end
of these
stress ratio (R =tests,
Smin /Sthe
max )fracture
of 0.1 and of athe samplesofor15conventional
frequency Hz. As a criterion fatigueforlimit
the endat 2of×these
10 cycles
6
tests, were
the fracture of the samples or conventional fatigue limit at 2 × 10 cycles were considered [18–20] previously
considered [18–20] (the end of the test is set to this value for
6 those samples that were not (the
end of broken).
the test isThe
setmaximum
to this value stress valuessamples
for those (Smax) were thatbetween
were not30% and 95%broken).
previously of the elastic limit, in order to
The maximum
keep them
stress values (Smaxwithin the zone 30%
) were between of elastic
and 95% behavior
of theof the material.
elastic A minimum
limit, in order to keep of themfourwithin
Smax values
the and
three samples in each S
zone of elastic behavior of the material. A minimum of four Smax values and three samples in each Sinto
m level were tested for each corrosion time. The results were divided m
two
groups in order to evaluate separately the slope of the S–N curve
level were tested for each corrosion time. The results were divided into two groups in order to evaluate between 10 3 and 106 cycles by the

Basquin
separately method
the slope [21–23]
of the and the
S–N curve fatigue10
between limit
3 and (Se10
) by the maximum
6 cycles likelihood
by the Basquin method function
[21–23] method
and [24–
the fatigue limit (Se ) by the maximum likelihood function method [24–27]. Starting from a data sample, with
27]. Starting from a data sample, the objective of the likelihood method is to find the population
the highest
the objective of the probability
likelihood methodof having is togenerated this sample.
find the population A the
with detailed
highest explanation
probabilityof of this statistical
having
method, widely used in parameter estimation, has been published
generated this sample. A detailed explanation of this statistical method, widely used in parameter by Myung in 2003 [28].
estimation, has been published by Myung in 2003 [28].
3. Results and Discussion
3. Results and Discussion
Figure 2a shows the three-dimensional representation of the uncorroded material obtained by
confocal
Figure microscopy
2a shows where rolling grooves
the three-dimensional in the x direction
representation can be seen.material
of the uncorroded Furthermore, microcracks
obtained by
canmicroscopy
confocal also be perceived by grooves
where rolling scanningin electron microscope
the x direction (Figure
can be seen. 2b). They microcracks
Furthermore, have a depth of
approximately
can also be perceived by10scanning
μm and electron
their formation may(Figure
microscope be due2b).
to the
Theyrolling
have process.
a depth ofThese microcracks are
approximately
10 µm not
andevenly distributedmay
their formation overbethe
duesurface, but appear
to the rolling very These
process. localized. These defects
microcracks may
are not constitute
evenly
anodic
distributed zones
over the where
surface,pitting corrosion
but appear very can be intense,
localized. Theseand thus may
defects reduce the fatigue
constitute strength
anodic zones of the
where material.
pitting corrosion can be intense, and thus reduce the fatigue strength of the material.

Figure 2. (a) Image

Figure 2. (a) of the surface
Image texturetexture
of the surface of the uncorroded
of the uncorroded alloy, xwhere
alloy, where axis represents the rolling
x axis represents the rolling
direction, (b) scanning electron microscopy (SEM) image showing the rolling microcracks.
direction, (b) scanning electron microscopy (SEM) image showing the rolling microcracks.
Metals 2020,
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As an example of calculating the pitting parameters, see Figure 3 obtained by confocal

As an example of calculating the pitting parameters, see Figure 3 obtained by confocal microscopy
microscopy from a sample corroded for two months. The maximum depth (P) is 20.5 μm and the
from a sample corroded for two months. The maximum depth (P) is 20.5 µm and the mean diameter
mean diameter (D) at zero level is 40 μm. If it is considered that the pit can approach an elliptical
(D) at zero level is 40 µm. If it is considered that the pit can approach an elliptical geometry in depth,
geometry in depth, the P/D ratio gives information on the concentration of stresses at the bottom of
the P/D ratio gives information on the concentration of stresses at the bottom of the notch and the
the notch and the severity of the defect. In this way, P represents the major axis of the ellipse and D is
severity of the defect. In this way, P represents the major axis of the ellipse and D is the minor. If the
the minor. If the value of D approaches zero, the stress value at the bottom of the pit becomes infinite
value of D approaches zero, the stress value at the bottom of the pit becomes infinite (ideal crack).
(ideal crack).

Figure 3. Two-dimensional
Two-dimensional digital
digital image
image of
of aa pit
pit of the sample corroded
corroded during
during two
two months
months (C2)
(C2)
obtained by
byconfocal
confocal microscopy.
microscopy. Pit depth
Pit depth and mean
and mean diameter
diameter were determined
were determined by Sensomap
by Sensomap software.
software.
The average parameters were determined by confocal microscopy for a total area of the confocal
image The(Aaverage of 33 mm2 . were
imla_conf ) parameters Thesedetermined
parametersbycan be seen
confocal in Table 1,for
microscopy where ρp area
a total is pitofdensity, Fp is
the confocal
the pitting
image (Aimla_conf ) ofP33
factor, m is
mmthe. average
2 pit depth, D
These parameters canm is
bethe average
seen pit1,
in Table diameter
where ρmeasured at theFsurface,
p is pit density, p is the

and Pmax
pitting is thePmdeepest
factor, pit value
is the average pitdetected.
depth, DmPits with
is the a depth
average pitsuperior
diameterto 10 µm were
measured chosen
at the forand
surface, the
calculation
P of the values,
max is the deepest pit valueas itdetected.
was intended to conduct
Pits with a depththe study without
superior to 10 μm taking
wereinto account
chosen for the
lamination defects.
calculation In Figure
of the values, as 4,
it the
wasnormal distribution
intended to conduct of the depth
study (a) and diameter
without (b) ofaccount
taking into the pit can
the
be observed.defects.
lamination It can beIn seen
Figurehow 4, both the diameter
the normal and the
distribution ofdepth of the(a)
the depth pitand
are diameter
greater for(b) samples C1
of the pit
and C2
can be than for C3,Italthough
observed. can be seen the difference
how bothisthegreater in theand
diameter case the
of depth.
depth Itofcanthealso
pitbeareseen how the
greater for
depth of C1
samples the and
pit increases
C2 than forsignificantly
C3, althoughthe longer the exposure
the difference time.inThis
is greater the trend
case ofis depth.
also observed in the
It can also be
case of diameter, but again in a less pronounced way.
seen how the depth of the pit increases significantly the longer the exposure time. This trend is also
observed in the case of diameter, but again in a less pronounced way.
Table 1. Parameters determined by confocal microscopy for a total area (Aimla_conf ) of 33 mm2 where ρp
is pit density,
Table Pmax isdetermined
1. Parameters the deepestbypitconfocal
value detected, Pm isfor
microscopy the average
a total areapit
(Adepth, σPm
imla_conf) of 33ismm
the2 standard
where ρp
deviation
is of PmP,max
pit density, Dmisisthe
thedeepest
averagepit
pitvalue
diameter measured
detected, Pm is at surface,
the averageσDmpitisdepth,
the standard deviation
σPm is the of
standard
D , and
deviation
m F is the pitting factor.
pof Pm, Dm is the average pit diameter measured at surface, σDm is the standard deviation of
Dm, and Fp is the pitting factor.
Parameter C1 C2 C3
ρp (pic/mmParameter
2) C1
0.12 C2 C3
0.44 1.25
ρp (pic/mm2)
Pmax (µm) 0.12
39 0.44 1.25
57 130
Pm (µm)Pmax (μm) 19.5
39 57 26.0
130 50.0
σPm 13.2 14.1 33.0
Pm (μm) 19.5 26.0 50.0
Dm (µm) 11.5 10.9 14.1
σDm σPm 13.2
4.5 14.1 33.0
5.5 6.8
(P/D)m Dm (μm) 11.5
1.61 10.9 14.1
2.35 3.27
Fp σDm 4.5
2.00 5.5 6.8
2.19 2.60
(P/D)m 1.61 2.35 3.27
Fp 2.00 2.19 2.60
Metals 2020, 10, x FOR PEER REVIEW 5 of 11
Metals 2020, 10, 1260 5 of 11

Figure 4. Normal distribution of the depth (a) and diameter (b) of the pit.
Figure 4. Normal distribution of the depth (a) and diameter (b) of the pit.
Table 1 shows that the pitting parameters increase with corrosion time, especially in C3
Table 1 The
specimens. showspitthat the pitting
density parameters
(ρp) is tripled eachincrease
month or, with
whatcorrosion time, there
is the same, especially in C3 specimens.
is a constant speed of
The
pits pit density (ρ
appearance onp )the
is surface
tripled ofeachthemonth or, what
alloy. Taking intois account
the same, thatthere
the Fis a constant
p factor is 1.00speed of pitsis
when there
appearance on the surface of the alloy. Taking into account
uniform corrosion, there is a high degree of localized attack from the first that the F factor is 1.00 when there
p month of testing (Fp = 2.00); is
uniform corrosion,
in particular, there is
the pitting a high increases
severity degree of considerably
localized attack from from
thethe first
third month
month ofof (Fp =is2.00);
testingThere
testing. also
in
an particular,
increase inthe thepitting
(P/D)m severity
ratio with increases considerably
the corrosion from thethe
time, although third monthpitofdiameter
average testing. There
(Dm) has is
also an increase
hardly changedinduring
the (P/D) ratiotwo
themfirst with the corrosion
months in sample time,C2. although
On the the otheraverage
hand, pit thediameter
values of(Dthem)
has hardly changed
maximum depth of during
pitting the(Pmaxfirst
) havetwotomonths
be takenin sample C2. On
into account forthe
theother hand, the
estimation values
of the of the
maximum
maximum
net sectiondepth
stressof
that pitting (Pmaxthe
supports ) have to be taken
material, that is,into account for
considering onlythetheestimation
uncracked of cross
the maximum
section of
net
thesection
sample.stress that supports the material, that is, considering only the uncracked cross section of
the sample.
The results of the X-ray diffraction (XRD) analyses were similar in all samples. Figure 5 shows
The results of the
the diffractograms X-ray
of the diffraction
samples (XRD)
C1 (black analyses
line), C2 (red were similar
line), and C3 in all
(bluesamples. Figure 5 shows
line), respectively. The
the diffractograms
oxidation product of theconsists
layer samplesmainly C1 (black line), C2
of bayerite (red line),
[β-Al(OH) and
3. 3H C3In(blue
2O]. line),ofrespectively.
the case sample C3,
The
more oxidation product peaks
intense bayerite layer consists
were obtainedmainly thanof bayerite
in the [β-Al(OH)
other samples, 3 . 3Hindicating
2 O]. In thea case
higherof sample
level of
C3, more intense
corrosion. bayerite
Bayerite peaks were compound
is a metastable obtained than that in constitutes
the other samples, indicating stage
an intermediate a higher level
between
of corrosion.aluminum
amorphous Bayerite ishydroxide
a metastable and compound
gibbsite [29]. thatThe constitutes
last one an is aintermediate
common compound stage between
in the
amorphous
atmosphericaluminum
corrosion of hydroxide
aluminum and gibbsite
alloys, [29]. The
especially when lastthere
one areis a alkaline
commonions compound in the
in the medium
atmospheric
[30]. corrosion of aluminum alloys, especially when there are alkaline ions in the medium [30].

Figure5.5.X-ray
Figure X-raydiffraction
diffractionanalysis
analysisofofcorrosion
corrosionproducts
productswhere
whereaabayerite
bayerite[β-Al(OH)
[β-Al(OH)j .j. 3H2O]
3H2O] peak
peak
can be seen in the sample corroded for 3 months.
can be seen in the sample corroded for 3 months.

The tensile tests are shown in Figure 6. The data obtained for the tensile strength (Su ) and yield
The tensile tests are shown in Figure 6. The data obtained for the tensile strength (Su) and yield
strength (S0 ) of the uncorroded material (R) match the values found in the literature (see Table 2):
strength (S0) of the uncorroded material (R) match the values found in the literature (see Table 2): 311
1
Metals 2020, 10, 1260 6 of 11
Metals 2020, 10, x FOR PEER REVIEW 6 of 11

311
MPaMPa for for Su and
Su and 275275 MPaMPaforforS0.SIn
0 . In
thethe corroded
corroded samplesC1
samples C1and
andC2,C2,SSuuand
andSS00dodonot not change
change with
respect
respect to the uncorroded material.
uncorroded material. By last, there is a decrease in the tensile strength for the corroded
samples
samples during
during33months
months(C3).
(C3).InIn this case,
this Su Sfalls
case, to 286
u falls MPa,
to 286 8% lower
MPa, thanthan
8% lower the Rthe
value, and its
R value, yield
and its
strength decreases
yield strength to 255 to
decreases MPa,2557% MPa,less7%than in R.
less Defining
than the valuethe
in R. Defining of Svalue
0 for each
of S 0type
for of sample
each type is
of
very important because it will be used as a reference stress in the subsequent
sample is very important because it will be used as a reference stress in the subsequent fatigue testsfatigue tests of this work.
The elongation
of this work. The (εf )elongation
is the parameter mostparameter
(εf) is the sensitive to mostthe sensitive
corrosionto process, as can be
the corrosion seen inas
process, Figure
can be 6.
It is around
seen in Figure17% foris the
6. It uncorroded
around 17% for material, 15.5% for
the uncorroded C1, and
material, approximately
15.5% for C1, and 11% for C2 and11%
approximately C3.
According
for C2 and to C3.these results,toitthese
According can be deduced
results, that,
it can be from
deducedthe that,
first month
from the of first
corrosion,
month the ductility
of corrosion,
decreases
the ductilitysignificantly.
decreases significantly.

Figure 6. Tensile curves of the uncorroded and corroded samples.

Figure 6. Tensile curves of the uncorroded and corroded samples.
Table 2. Yield stress, tensile strength, and elongation values obtained from Figure 6.
Table 2. Yield stress, tensile strength, and elongation values obtained from Figure 6.
Material S0 (MPa) Su (MPa) εf
Material S0 (MPa) Su (MPa) εf
Uncorroded (R) 275 311 17.0
Uncorroded
C1 (R) 271275 311311 17.0
15.5
C2 C1 276271 309311 15.5
11.6
C3 C2 255276 286309 11.6
11.2
C3 255 286 11.2
The adjustment of the S/N curves by the Basquin method was performed using the maximum
Theofadjustment
95% S0 , 90%ofSthe S/N curves by the Basquin method was performed using the maximum
stresses 0 , 80% S0 , and 70% S0 in the case of the uncorroded material (R) and 95% S0 ,
stresses
70% S0 , of 95%
55% S0 ,Sand
0, 90% S0, 80% S0, and 70% S0 in the case of the uncorroded material (R) and 95% S0,
45% S0 in the corroded samples. This adjustment is equivalent to expressing
70% S 0, 55% S0, and 45% S0 in the corroded samples. This adjustment is equivalent to expressing
fatigue strength as a straight line of slope b in an S/N diagram in double logarithmic scale.
fatigue strength as a straight line of slope b in an S/N diagram in double logarithmic scale.
b
∆SΔ𝑆= KN
𝐾𝑁 (1)
(1)
K represents
represents the
the stress
stressrequired
requiredtotoproduce
producefracture
fracturewhen
whenonlyonlyone
one stress
stress cycle
cycle is is applied
applied and
and b isb
is the
the Basquin
Basquin exponent,
exponent, which
which characterizes
characterizes howhow muchmuch the number
the number of cycles
of cycles variesvaries
until until fracture
fracture with
with
the the change
change of alternating
of alternating tension.tension. b is range
b is in the in the of
range
−0.05ofto−0.05
−0.12tofor
−0.12
mostforuncorroded
most uncorroded metals
metals [31,32].
Figure 7 shows the ∆S versus N graph that collects the average experimental data shown in
[31,32].
TableFigure
3, with7 ashows the ∆S scale
logarithmic versus forNthegraph
x andthat collects
y axes, the average
together with the experimental
adjustments data shownfor
obtained in
Table 3, with a logarithmic scale for the x and y axes, together with the adjustments
each sample. There is a significant decrease in fatigue strength when corrosion is only one month. obtained for each
sample. There
Meanwhile, is a significant
the changes are moredecrease
appreciable in for
fatigue
a highstrength
numberwhen corrosion
of cycles betweenisthe only
stateone month.
C1 and C2.
Meanwhile,
In the case ofthe
C3,changes
the curve arebegins
more at appreciable for alevel
a lower stress highbecause
numberitsofelastic
cycleslimit
between the than
is lower state the
C1 and
rest
C2.the
of Inmaterials,
the case ofand
C3,testing
the curveat a begins
higher at a lower
level couldstress
have level
masked because its elastic
the fatigue limit
crack is lower
growth thanwith
process the
arest of the
process of materials,
high plastic and testing at a higher level could have masked the fatigue crack growth
deformation.
process with a process of high plastic deformation.
Metals 2020,10,
Metals2020, 10,1260
x FOR PEER REVIEW 77 ofof1111

Figure7.7.Stress
Figure Stressrange
range(∆S)
(ΔS)vs.
vs.average
averagenumber
numberofofcycles
cyclesatatfailure
failure(N)
(N)curve.
curve.
Table 3. Data of stress range (∆S) and average number of cycles at failure (N) for Smax /S0 ratios tested.
Table 3. Data of stress range (∆S) and average number of cycles at failure (N) for Smax/S0 ratios tested.
σ is the standard deviation of N data and (%σ) standard deviation expressed as percentage.
σ is the standard deviation of N data and (%σ) standard deviation expressed as percentage.
Sample Smax /S0 ∆S (MPa) N (cycles) σ σ (%)
Sample Smax/S0ΔS (MPa) N (cycles) σ σ (%)
0.95 235 52,432 20,813
0.95 235 52,432 20,813 4040
0.90 223 68,404 29,931 44
R
R 0.800.90 223
198 68,404
147,233 29,931
7945 445
0.700.80 198
174 147,233 191,183
348,293 7945 555
0.950.70 174
235 348,293
20,248 191,183
4129 55 20
0.700.95 235
174 20,248
78,343 4129
18,991 2024
C1
0.550.70 174
136 78,343
175,615 18,991
35,238 2420
C1 0.450.55 112 376,934
136 175,615 134,688
35,238 2036
0.950.45 112
235 376,934
21,944 134,688
2789 3613
0.700.95 174
235 79,986
21,944 7991
2789 1310
C2
0.55 136 138,925 14,744 11
0.70 174 79,986 7991 10
C2 0.45 112 264,567 23,102 9
0.55 136 138,925 14,744 11
0.95 218 28,266 5367 19
0.45 112 264,567 23,102 9
0.70 160 66,757 15,519 23
C3
0.550.95 218
126 28,266
148,015 5367
50,770 1934
0.450.70 160
103 66,757
236,728 15,519
89,123 2338
C3
0.55 126 148,015 50,770 34
0.45 103 236,728 89,123 38
Table 4 includes the fatigue strength coefficient (K), the Basquin exponent (b), and the coefficient
of determination (R2 ). The coefficient of determination is 0.98 for sample C2, while it is higher than
Table 4 includes the fatigue strength coefficient (K), the Basquin exponent (b), and the
0.99 for C1 and C3, which is indicative that the number of stress values used is sufficient for a high
coefficient of determination (R2). The coefficient of determination is 0.98 for sample C2, while it is
approximation of the Basquin equation. In relation to the coefficient K, an increase is obtained with
higher than 0.99 for C1 and C3, which is indicative that the number of stress values used is sufficient
the severity of the pits, given by the P/D ratio, especially between R and C1. Similarly, the Basquin
for a high approximation of the Basquin equation. In relation to the coefficient K, an increase is
exponent (b) shows a significant decrease from the first month of corrosion.
obtained with the severity of the pits, given by the P/D ratio, especially between R and C1. Similarly,
the Basquin exponent (b) shows a significant
Table 4. decrease
Fitting constants of thefrom the equation.
Basquin first month of corrosion.

K (MPa)
MaterialTable 4. Fitting B
constants of the Basquin equation. R2
R 1.287
Material K (MPa) −0.1570B R2 0.999
C1 3.008 −0.2557 0.996
C2 R 4.846 1.287 −0.1570
−0.3002 0.999 0.983
C3 C1 7.495 3.008 −0.2557
−0.3453 0.996 0.997
C2 4.846 −0.3002 0.983
C3 7.495 −0.3453 0.997
Applying Basquin’s equation for the value of 200 MPa, it is calculated that the life (N) for the
uncorroded material (R) is 141,251 cycles, while for C1 and C2, it decreases to approximately 42,000
Applying Basquin’s equation for the value of 200 MPa, it is calculated that the life (N) for the
cycles, which represents a decrease with respect to R of almost 72% (Figure 8). In the case of C3, N is
uncorroded material (R) is 141,251 cycles, while for C1 and C2, it decreases to approximately 42,000
cycles, which represents a decrease with respect to R of almost 72% (Figure 8). In the case of C3, N is
Metals 2020, 10, 1260 8 of 11
Metals 2020, 10, x FOR PEER REVIEW 8 of 11

36,108 cycles,
36,108 cycles, which
which isis aa 74%
74% decrease
decrease with
with respect
respect to R. Thus,
to R. Thus, there
there is
is aa clear
clear decrease
decrease in in fatigue
fatigue
strength with corrosion time and the highest difference is between the uncorroded material
strength with corrosion time and the highest difference is between the uncorroded material (R) and (R) and the
corroded
the material
corroded during
material during one month
one month(C1). When∆S
(C1).When ΔSisis150
150MPa,
MPa,the
thenumber
number of of cycles to failure
cycles to failure is
is
882,630 for R,
882,630 for R, while it is 123,775 and 106,567 cycles for C1 and C2, respectively, which represents aa
while it is 123,775 and 106,567 cycles for C1 and C2, respectively, which represents
decrease in
decrease in relation
relation to
to RR of
of approximately
approximately 86%
86% for
for C1
C1 and
and 88%
88% for
for C2.
C2. The
The material
material in
in state
state C3
C3 has
has aa
decrease of
decrease Nff of
of N of91%
91%compared
compared with R.
with R.

Figure 8. Number of cycles to failure (N) vs. corrosion time (t). Data were calculated from the Basquin
Figure 8. Number of cycles to failure (N) vs. corrosion time (t). Data were calculated from the
equation for ∆S = 200 MPa (dark) and ∆S = 100 MPa (light).
Basquin equation for ∆S = 200 MPa (dark) and ∆S = 100 MPa (light).

The adjustment of the S/N curves by the maximum likelihood method was performed for the
The adjustment of the S/N curves by the maximum likelihood method was performed for the
maximum stress levels 65% σ0 and 55% σ0 in the case of R, 40% σ0 and 35% σ0 in C1 and C2, and 40%
maximum stress levels 65% σ0 and 55% σ0 in the case of R, 40% σ0 and 35% σ0 in C1 and C2, and 40%
σ0 and 35% σ0 in C3. This method assumes that the runouts test stress is distributed normally for a
σ0 and 35% σ0 in C3. This method assumes that the runouts test stress is distributed normally for a
certain number of cycles [33]. The probability of experimental data is given by
certain number of cycles [33]. The probability of experimental data is given by
Yn

𝑉=
V [11− F𝐹(S𝑆i , ,x,𝑥̅ , σ𝜎)]ri [11− F𝐹 , 𝑥̅σ, )]
(Si𝑆, x, 𝜎
fi
(2)
(2)
i=1

where 𝑥̅x is
where is the mean, σσ is
the mean, is the standard deviation, rii represents
the standard represents the
the number
number of of “run-outs”
“run-outs” at at the
the ith
ith
stress
stress level (Si),
level (S i ),ff
i iis
isthe
thenumber
number of
offailures
failuresobserved
observed atatthe
the same
same stress
stress level,
level, and
and F
F is
is the
the cumulative
cumulative
probability
probability of of failure.
failure. This
This equation
equation can
can be
be written
written as
as
1 S
 1 𝑥̅ 𝑥!2 
𝐹 𝑆, 𝑥̅ , 𝜎 1 𝑒𝑥𝑝  1 x − x  𝑑𝑥
Z
(3)
F(S, x, σ) = √ exp− 2
𝜎√2𝜋 𝜎 dx (3)
−∞ σ 2π 2 σ
Equation (2) in the form of napierian logarithms is expressed as
Equation (2) in the form of napierian logarithms is expressed as
𝑙𝑛𝑉 X n 𝑟 𝑙𝑛 1 𝐹 𝑓 𝑙𝑛𝐹 (4)
lnV = ri ln(1 − Fi ) + fi lnFi (4)
where Fi is F(Si,𝑥̅ ,σ). It is necessary to obtaini=the
1 partial derivatives with respect to 𝑥̅ y σ and equate
them to zero to calculate the maximum of Equation (4). Thus, a system of two non-linear equations
where Fi is F(Si ,x,σ). It is necessary to obtain the partial derivatives with respect to x y σ and equate
with two unknowns 𝑥̅ y σ is obtained. The resolution of the system makes it possible to calculate the
them to zero to calculate the maximum of Equation (4). Thus, a system of two non-linear equations
fatigue limit and the associated deviation.
with two unknowns x y σ is obtained. The resolution of the system makes it possible to calculate the
Table 5 shows the results of the fatigue limit Se and the percentage deviation (σ%) calculated
fatigue limit and the associated deviation.
considering a technological life level of 2 × 106 cycles. The value obtained for the fatigue limit of
Table 5 shows the results of the fatigue limit Se and the percentage deviation (σ%) calculated
sample R is 161 MPa. In the case of C1, the limit6 is 98 MPa, which implies a reduction in the fatigue
considering a technological life level of 2 × 10 cycles. The value obtained for the fatigue limit of
limit of 39%. In the same way as in the analysis of fatigue strength, it is in this first stage of corrosion
sample R is 161 MPa. In the case of C1, the limit is 98 MPa, which implies a reduction in the fatigue
that the most pronounced reduction in fatigue response occurs. The decrease in fatigue limit is not so
limit of 39%. In the same way as in the analysis of fatigue strength, it is in this first stage of corrosion
marked between C1 and C2 (94 MPa). However, the C3 samples corroded for three months show a
that the most pronounced reduction in fatigue response occurs. The decrease in fatigue limit is not so
large decrease of Se (68 MPa) with respect to the previous stage samples (C2). The total decrease of Se
between material R and C3 was 57.4%. The drastic decrease in fatigue resistance during the first
month of saline corrosion is in accordance with studies carried out by other authors [12], in which it
Metals 2020, 10, 1260 9 of 11

marked between C1 and C2 (94 MPa). However, the C3 samples corroded for three months show a
large decrease of Se (68 MPa) with respect to the previous stage samples (C2). The total decrease of
Se between material R and C3 was 57.4%. The drastic decrease in fatigue resistance during the first
month of saline corrosion is in accordance with studies carried out by other authors [12], in which it
was observed that the corrosive effect has a more pronounced effect on aged aluminum alloys, such as
alloy 6061-T6, than non-heat treatable aluminum alloys (2xxx, 5xxx groups).

Table 5. Fatigue limit (Se ), and the percentage deviation (σ%) calculated considering a technological
life level of 2 × 106 cycles.

Material %S0 Smax (MPa) F r Se (MPa) σ (%)

65 161 6 3
R 161 1.55
55 151 0 3
40 99 2 1
C1 98 1.47
35 86 0 3
40 99 4 0
C2 94 0.21
35 86 0 3
35 68 2 1
C3 68 0.76
27 62 0 3

Figure 9 shows the fatigue parameter Se /S0 versus (P/D)m ratio for R, C1, C2, and C3 samples.
The point corresponding to the reference material (uncorroded sample) does not start from Pm /Dm = 0,
but from 8.6 µm/74 µm = 0.11. This is explained by the presence of microcracks resulting from the
lamination process. The maximum depth observed in these microcracks was 10 µm. This graph
shows that all data can be correlated by a logarithmic curve. The determination coefficient (R2 ) is
0.985, which indicates a good fit. This demonstrates that a correlation can be established between
a dimensional ratio of the pits (P/D)m and the normalized fatigue limit (Se /S0 ), allowing even to
integrate the uncorroded material data into the fit. This result makes sense considering that the ratio
(P/D)m is indicative of the concentration of stresses at the edge of the pit, reducing the fatigue strength
of the material. According to various authors [34,35], the significant decrease in fatigue strength
in precorroded aluminum alloys is related to the progressive appearance of pits, which are stress
concentration points where cracks begin.

Figure 9. Fatigue Se /So ratio vs. (P/D)m ratio for R, C1, C2, and C3 samples.

4. Conclusions
Corrosion parameters show a large increase after 3 months in a salt spray chamber. Pitting factor
(Fp ) values indicate that corrosion is highly localized from the first month. X-ray diffraction analysis
shows the formation of aluminum hydroxides: bayerite. The appearance of intense bayerite peaks at
the third month of corrosion (C3) is related to a higher level of corrosion.
Metals 2020, 10, 1260 10 of 11

The samples corroded for three months (C3) are the most affected in the tensile test. In this case,
tensile strength (Su ) falls to 286 MPa, 8% lower than the uncorroded material value, and its yield
strength (S0 ) decreases to 255 MPa, 7% less than in R. On the other hand, the results show a significant
decrease in ductility from the first months of corrosion.
The application of the Basquin equation and the maximum likelihood model shows a significant
decrease in the number of cycles until failure during the first month of corrosion (around 72% for C1
when ∆S is 200 MPa, and 86% when ∆S is 150 MPa). This decrease continues for the next two months
(C2 and C3), but without the variations being so marked with respect to C1.
Finally, the fatigue data were treated with the maximum likelihood model. The conventional
fatigue limit suffers an important decrease between R (161 MPa) and C1 (98 MPa) and between C2
(94 MPa) and C3 (68 MPa). The representation of the fatigue parameter Se /S0 versus ratio Pm /Dm ratio
shows that data can be correlated by a logarithmic curve. The determination coefficient (R2 ) is 0.985,
which indicates a good fit.

Author Contributions: The main investigation was performed by A.F.M. and J.L.M.B.; data curation, software,
and formal analysis were performed by A.F.M.; the methodology was conducted by all the authors; the tasks
were supervised by A.F.M. and J.L.M.B.; the visualization and validation were done by J.L.M.B. and A.I.G.-D.;
the writing, review, and editing of the document were done by J.L.M.B., A.I.G.-D., C.C.F., and J.J.G.D. All authors
have read and agreed to the published version of the manuscript.
Funding: This research received no external funding.
Conflicts of Interest: The authors declare no conflict of interest.

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