ISSN 2070-2051, Protection of Metals and Physical Chemistry of Surfaces, 2021, Vol. 57, No. 4, pp. 786–795.

© Pleiades Publishing, Ltd., 2021.

NEW SUBSTANCES,
MATERIALS AND COATINGS

Time Dependent Ambient Oxidation of AA6061-T6 Alloy

at the Temperature of 580°C
Samir Attafia, *, Sabiha Aklouche-benouaguefb, and Şükrü TALAŞc
a Laboratory
of Technology Materials, LTM, USTHB, Algeria
b Laboratory of Transport Multiphase and Porous Media, LTPMP USTHB, Algeria
c
Metallurgical and Materials Engineering, A. Kocatepe University, Afyonkarahisar, Turkey
*e-mail: attafisamir@gmail.com
Received July 26, 2019; revised January 7, 2021; accepted March 21, 2021

Abstract—The AA6061-T6 alloy is used in many industrial applications such as hydraulic pistons, aerospace
and marine vehicle fittings, including the nuclear reactors due to their excellent joining and coating proper-
ties, high strength, good formability, high resistance to aquatic corrosion and neutron transparency. This
study consists of high temperature oxidation for which the samples were oxidized using thermogravimetric
analysis, at a temperature of 580°C in an atmosphere that contains air and argon. Exposure of exposure times
at 580°C varied from 15 min to 8 h, which permitted to understand the mechanism of oxide formation mech-
anisms in this alloy and progressive formation of oxide layers on the surface. The chemistry, thickness and
the morphology of the oxide layer formed on the surface was characterized by scanning electron microscopy
(SEM-EDS), X-ray diffraction which revealed the existence of the following elements in the oxide layer, such
as Al2O3, Al9Si, SiO2, MgO and Mg3O4. Results showed that the oxide layer becomes thicker with the increas-
ing exposure time and is accompanied by a loss of weight compared to the mass formed at the beginning of
the thermogravimetric analysis.

Keywords: high-temperature oxidation, AA6061-T6 aluminium alloy, oxygen diffusion, thickness, oxide
layer, interface, degradation
DOI: 10.1134/S2070205121040067

1. INTRODUCTION melting point [8, 9]. This substantial amount of oxide

The AA6061-T6 grade of the 6xxx series of alumin-
ium alloy is widely used in the industry, in particular,
the nuclear industry for its neutron transparency, its
low warming up on gamma radiation, ductility and
toughness [1, 2]. The application of heat treatments
and the addition of other elements in small quantities,
mainly magnesium and silicon, makes it possible to
obtain maximum structural hardening by the precipi-
tation of several phases of micrometric and nanomet-
ric size, i.e. β'-Mg2Si,  β''-Mg2Si and stoichiometric
Mg5Si6 [3–7].
The different branches of metallurgy are trans-
forming aluminium oxide to aluminium product to
make parts of machine, mechanisms, instruments,
and tools that we need in different forms. However,
aluminium tends to return to its original state before
being extruded by corrosion or oxidation; in effect, the
increase in temperature makes this phenomenon
advance faster. During the first stages of production,
the temperature is very high, and the alloy develops a
thin and resistant surface oxide layer, because of the
high affinity between the aluminium and oxygen,
which thickens according to a parabolic law up to the
film present on the surface plays the role of a barrier
between the metal surface and surrounding atmo-
sphere and protects the metal from further oxidation
[8, 10–12]. The mechanism of formation and the
development of this layer between the surface of the
metal and the interfaces of metal oxide and gas oxide
during steps of growth are still complex, some dis-
agreements exist in the literature concerning the for-
mation of formed oxides and the kinetics of the reac-
tion [8, 9, 13, 14]. The increase in temperature further
promotes the diffusion of oxygen in the metal surface,
causing the phenomenon of oxidation [15].
The kinetics of oxidation at high temperatures
between 450 and 570°C was studied by Beck et al. [8]
for aluminium of high purity under dry oxygen
medium. Beck et al. observed that the complex oxida-
tion kinetics comprise two distinct and essentially
independent portions of each other. An amorphous
γ-Al2O3 film, which diffuses outside of metal ions, is
formed in a very parabolic kinetics throughout the
temperature range. At each temperature, substantially
cylindrical crystals γ-Al2O3 of constant final thickness
grow inside the metal from the amorphous oxide-

786
 TIME DEPENDENT AMBIENT OXIDATION OF AA6061-T6 ALLOY
metal interface by diffusion of inward oxygen through
the amorphous oxide layer, which covers the metal.
For high temperatures exceeding melting points, the
kinetics of oxidation of commercially pure aluminium
was studied by Bergsmark, et al. [16] between 800 and
950°C. Bergsmark et al. found that the reaction kinet-
ics are complex and cannot be described by simple rate
equations. The oxide layers formed after extended
reaction with air consist of a thin, relatively compact
layer of aluminium oxide, which is thicker and porous
layer with inclusions of unreacted aluminium particles
and oxide outgrowths on the oxide surface, some of
which consist of magnesium oxide. Cracking of the
oxide layers also contributes to yield complex kinetics.
An additional feature is that magnesium is transported
rapidly through the scale and forms the MgO-rich part
of the surface. Wang, et al. [17] simulated the tempera-
ture and stress relationships in 6061 alloy during the
temper in water. They found that the value of heat
transfer coefficient is low at the beginning of the
quenching process and the maximum cooling velocity
appears in the external edge of ribs around the profile,
while the joints of the internal surface and ribs have
the slowest cooling velocity. The temperature differ-
ence of the profile is about 100°C in the first 2s, then
decreases, apparently, and the temperature of entire
profile on the sample tends to be uniform.
One of the industrial accident scenarios is the loss
of the refrigeration of the primary circuit of the central
nuclear compound; the worst disaster of the t century
is Fukushima Daiichi, Japan. The 11 March 2011 at
the same level of gravity as the Chernobyl disaster,
Ukraine 1986 the water pool of deactivation of reactor
4 overheating, and the reactors 1, 2 and 3 melted as the
alloy AA6061-T6 is used in the heart-box of most
nuclear power stations, which makes it to be interest-
ing to study on the degradation of this alloy at high
temperature.
In this study, the experiments were dedicated to
high-temperature oxidation in air. Characterization
techniques of scanning electron microscopy (SEM),
EDS (energy dispersive X-ray spectrometry), DTA
and X-ray diffraction analysis (XRD) were used to
determine the nature of the oxides formed on the sur-
face of the alloy AA6061-T6.
2. EXPERIMENTAL
Initially, the alloy AA6061-T6 in the form of a plate
was analyzed for the chemical composition by weight
using the MetalLab GNR 7580 device. Then, samples
were sliced to obtain a sample weighing between 35 to
75 mg with a Isomet microtrononneuse device. Before
each experiment, mechanical polishing with abrasive
papers was applied until 2000G followed by finishing
with a felt paper and a diamond paste for the six faces
of each sample. The differential thermal analysis
DTA-TG coupled device of NETZSCH 404S was
operated to reach the melting temperature from room
PROTECTION OF METALS AND PHYSICAL CHEMISTRY OF SURFACES
787
temperature, with a heating rate of 20°C/min from 30
up to 800°C under Ar atmosphere.
The high-temperature oxidation with respect to
exposure time was carried out with the DTA-TG cou-
pled device of NETZSCH 404S at 580°C The sample
was placed in a silica crucible with an air flow of
50 mL/min that was introduced to the chamber so that
the phenomenon of oxidation can be activated under
the effect of oxygen in the air and argon with a purity
of 99% with a gas flow rate of 20 mL/min. Argon was
added in order to ensure the stability of the sample in
the crucible.
This test was carried out in two stages; the first step
consisted of applying the heat at a rate of 20°C/min up
to 580°C. The second step was to maintain this tem-
perature for different exposure times, which are
respectively 15, 30 min, 1, 2, 4, 6 and 8 h. The change
in the mass of the sample was followed using DTA/TG
device and the evolution of mass change as a function
of the exposure time (oxidation reaction progress
curve) was digitally recorded by a microcomputer
which was connected to the DTA/TGA device.
The oxidized samples at different exposure times
were characterized by the observation of their external
surface which was investigated by using a light micro-
scope of NIKON ÉCLIPSE MA connected to a
microcomputer to record the images.
Before proceeding with the transverse slicing of the
samples, X-ray diffraction study was carried out to
identify the nature of oxide layers formed on the exter-
nal surface. BRUKER D ADVANCE was used for the
X-ray analysis which was equipped with a copper tar-
get which produces a radiation with a wavelength (λ)
of 1.54060 Å. The results of the spectra were compared
against ICDD database using the HighScore plus soft-
ware.
The second stage of characterization involves
cross-sectional slicing of the samples to observe the
thickness of the oxide layer formed on the external sur-
face. Since the oxide layer is thin in size, the samples
were set in a hot resin and mirror polished and eventu-
ally sliced perpendicularly for the investigation under
optical microscope and scanning electron microscope
(SEM) type LEO 1430VP coupled with energy disper-
sive X-ray spectrometer (EDS).
3. RESULTS AND DISCUSSION
3.1. Preliminary Study on Melting
Point and composition
The chemical composition analysis result of the
samples by weight is shown in Table 1. It is confirmed
that the aluminium alloy is AA6061-T6, compared
with Vincent, S. et al., Maisonnette, D. et al.,
Dehnavi, V. et al. [2, 18, 19].
The result of the differential analysis of sample
(Fig. 1) shows that the chemical reaction is exother-
Vol. 57 No. 4 2021
788 SAMIR ATTAFI et al.

Table 1. Chemical Composition of Elements by Weight of AA6061-T6 Alloy

Al % Si % Mg % Fe % Cu % Mn % Cr % Zn % Ni %
97.067 0.537 1.361 0.176 0.321 0.070 0.233 0.064 0.013
Ti % Pb % Sn % V% B% Bi % Co % Sb %
0.038 0.019 0.014 0.004 0.002 0.006 0.005 0.071

mic, and two transformation points appeared at
635.9°C (Solidus) and at 681.4°C (Liquidus).
Samples were oxidized at 100°C below the melting
point at several exposure times (min, 1, 2, 4, 6 and 8 h
using thermogravimetric analysis (TGA) in order to
simulate the estimated high temperature behavior of
this type of aluminium alloy in case the temperature
exceeds the suggested service temperature.
3.2. TGA Study of Specimens
Weight loss results are given as the weight change
against the exposure time (Figs. 2a–2c). A rapid loss
of mass was observed during the first ten minutes of
all experiments with a sharp fall that takes place after
4.66 min as with other samples behaving in the same
manner, possibly due to the volatile impurities (such as
hydroxides of aluminium) existing on the surface of
the samples. Following this drop in mass, all the sam-
ples proceed with mass gain which indicates the for-
mation of oxides between the alloying elements and
the oxygen. This stage of drop in mass is believed to be
the degradation due to the stall of the oxide layer
formed on the surface except in the case of 8h when
the mass gain is 0.005309 mg, which represents
approximately 0.01% of the total mass. This small gain
of mass is observed because the rate of formation of the
oxides is faster than the oxide dissolution rate of the
alloy. It can be seen in Fig. 2c that there is a slight fluc-
tuation at exposure times of 190.23 and 193.11 min,
which are visible in both analyzes carried out at 6 h and
8 h in DTA-TG. This fluctuation phenomenon may be
due to the microcracking of the oxide layer formed on
the surface of the samples or could be the result of the
sensitivity of the thermobalance, however, these
microcracks have also been observed by the electron
microscope (SEM) images in the following section
(Fig. 3).
3.3. XRD Study
The nature of layers formed on the external surface
of samples is characterized by X-ray diffraction under
grazing incidence. Figure 3 shows the result of high-
Score plus software processing. The absence of
α-Al 2O3 peak in two samples, 30 min and 1h, which is
due to the fact that the removal of the oxide during
metallographic process prior to TGA. A slight appear-
ance of the peak SiO2 appears in different places for
30 min, which were more apparent for 1 h. The silicon
oxide SiO2, which is not visible on the elementary
EDS mapping on the surface of the samples of 15,
30 min and 1 h, was detected by XRD due possibly to
the abrasive paper used during the mechanical polish-
ing operation. The peaks of the two phases Al9Si and
Mg 4O4 have not changed in all XRD graphs, indicat-
ing that these two phases represent the majority of
phases in this alloy.
In Fig. 4, the peaks of SiO2 change the position for
2 and 4 h samples and no change is noticed when com-
pared to other peaks of Al9Si and Mg 4O4 , which indi-
cates that the silicon is thermally activated. The Si
atoms migrate to the surface from the metal base
AA6061-T6 alloys [21] and form the silicon oxide in
the oxide layer.
The results in Fig. 5 show that no changes are
observed for the peaks of Al9Si . The appearance of
oxide peaks MgO and α-Al 2O3 , is consistent with the
shape change of the surface oxide layer of the samples
and analysis from EDS, the oxide layer is again more
compact on the surface and irregular on the metal
side. At short exposure time, there is an insufficient
time for the transformation of γ → α-Al2O3. The final
volume fraction of α-Al2O3 formed in the layer
depends on the total duration of exposure to air, the
intensity of local elemental distribution, and the
annealing effect on the already formed solid oxide lay-
ers. The γ-Al2O3 formed early in the heating process
could transform to α-Al2O3 as a result of the increasing
heat [20–22].
The peaks of SiO2 on 8 h exposure time disappear,
indicating that layer formed on the surface of the 8 h
DTA, μV/mg
681.4°C
635.9°C
0.4
0.3
0.2
0.1
0
–0.1
–0.2
–0.3
100 200 300 400 500 600 700
Temperature, °C
Fig. 1. The result of differential thermal analysis of
AA6061-T6 alloy in as received condition.

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 TIME DEPENDENT AMBIENT OXIDATION OF AA6061-T6 ALLOY 789

(a) 1h
100.0
15 min
30 min
99.9

Intensity, a. u.
Al9Si 30 min
Al2O3
SiO2
99.8 Mg4O4
wt, %

Raw 6061-T6

98.7

98.6
30 60 90
Position [2θ, deg] (copper (Cu))
98.5
0 20 40 60
Time, min Fig. 3. XRD results for AA6061-T6 treated for 30 min and
1 h at high temperature. 15 min of exposure to air did not
100.0 (b) produce a different data from 30 min exposure time.
4h
99.8 2h
1h
99.6 4h
wt, %

99.4
99.2
Intensity, a. u.

2h
Al9Si
Al2O3
99.0 SiO2
Mg4O4
98.8
Raw 6061-T6

98.6
0 100 200
Time, min
(c)
30 60 90
100.00 Position [2θ, deg] (copper (Cu))
6h
8h
Fig. 4. XRD results for AA6061-T6 specimens treated for 2
and 4 h at 580°C.
99.95
wt, %

8h

99.90
Intensity, a. u.

6h
Al9Si
Al2O3
SiO2
99.85
0 200 400 600 Mg4O4
Time, min Raw 6061-T6

Fig. 2. Results of the thermogravimetric analysis, (a) 15

and 30 min, (b) 1, 2 and 4 h, (c) 6 and 8 h.

30 60 90
samples is thicker. This may impose that the silicon Position [2θ, deg] (copper (Cu))
oxide SiO2 is located below the surface, not on the sur-
face, which is in agreement with the work of Qin, Z Fig. 5. XRD results for AA6061-T6 treated for 6 and 8 h
et al [21]. When the atoms of magnesium are oxidized oxidation at 580°C.

PROTECTION OF METALS AND PHYSICAL CHEMISTRY OF SURFACES Vol. 57 No. 4 2021

790 SAMIR ATTAFI et al.

Resin

Sample

10 m (b) 20 m
(a)

Resin Resin

Sample Sample

(c) 200 m (d) 20 m

Resin
Resin

Sample
Sample
(e) 20 m (f) 20 m

Resin
Resin

Sample
Sample

20 m 200 m
(g) (h)
Fig. 6. SEM images of AA6061-T6 alloy (a) as received condition and oxidised for (b) 15, (c) 30 min, (d) 1, (e) 2, (f) 4, (g) 6
and (h) 8 h.

PROTECTION OF METALS AND PHYSICAL CHEMISTRY OF SURFACES Vol. 57 No. 4 2021

 TIME DEPENDENT AMBIENT OXIDATION OF AA6061-T6 ALLOY 791

20 m Mg
Al Mg O C Si

Al Si O

Fig. 7. The analysis results from elementary mapping of AA6061-T6 alloys oxidised for 15 min.

200 m
Al Mg O C Si Mg

Al Si O

Fig. 8. The analysis results from elemental mapping of AA6061-T6 alloy oxidised for 30 min.

on the surface, the atoms of silicon are left behind and
form an enriched region at the metal/oxide layer inter-
face. This region is poor in free magnesium in reason
of the sluggish diffusion and the atoms of Si precipitate
in the form of Mg2Si [25].
3.4. Microscopy and EDS Analysis
An SEM image of reference sample is provided in
Fig. 6a without chemical etching. The first observa-
tion on the microstructure of the alloy AA6061-T6
revealed that the matrix is gray, with black dots in the
form of dispersoids, which are found to block the
recrystallization [20]. They are dispersed in the similar
manner, having a micrometric size. The SEM charac-
terization of a sample in as received form (Fig. 6a) was
carried out by using Secondary Electron Detector
(SE). SEM images showed that dark coloured and
white precipitations are dispersed homogeneously in
the matrix [3, 7]. The second phase particles are in the
order of micrometer in size and in the form of spheroi-
dal shape for both dark coloured and white particles,
some grains of different size are also observed. It is
considered that dark or black precipitates being Mg2Si
[24] and white regions being pure aluminium in the
matrix during the production stage [2].
The SEM observations of samples that have under-
gone 15 and 30 min of oxidation treatment (Figs. 6b, 6c)
show no visible change on the outer surface of the
sample. The observation of samples that are oxidized
during 1, 2, 4, 6 and 8 h (Figs. 6d–6h) at 580°C revealed
a colour change from light gray to the dark gray, indi-
cating that the oxygen has reacted with the substrate,

PROTECTION OF METALS AND PHYSICAL CHEMISTRY OF SURFACES Vol. 57 No. 4 2021

792 SAMIR ATTAFI et al.

20 m Al Mg O C Si Mg

Al Si O

Fig. 9. Elementary EDS mapping of AA6061-T6 alloy oxidised for 1 h.

20 m Mg
Al Mg O C Si

Al Si O

Fig. 10. Elementary EDS mapping of AA6061-T6 alloy oxidised for 2 h.

an oxide layer is formed on the surface. It is loose,
porous and has microcracks which can be observed in
Figs. 6d–6h [21–23]. These microcracks are believed
to be the result of the difference in the coefficient of
thermal expansion between the substrate alloy and the
thickness of the oxide layer formed on the surface [13].
Several white spots of different size and shape were
also observed. These may be the pure aluminum that
did not react with Oxygen or has not been dissolved in
the matrix during the manufacturing [2]. The dark
coloured patches are always present, which indicate
that this phase does not react with oxygen at high tem-
perature.
In Figs. 7 and 8, elemental mapping is given to
show the concentration of chemical elements on the
cross-sectional view of the surface after oxidation
treatment. The concentration of all elements, and
magnesium, in particular, is more at the interface
(resin/sample) than inside of the sample. These
results confirm the interaction between oxygen and
one or more elements in the AA6061-T6 alloy and a
thin oxide layer on the outer surface of the samples
during the high-temperature oxidation treatment.

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 TIME DEPENDENT AMBIENT OXIDATION OF AA6061-T6 ALLOY 793

20 m
Al Mg O C Si Mg

Al Si O

Fig. 11. Elementary EDS mapping of AA6061-T6 alloys oxidised for 4 h.

20 m Mg
Al Mg O C Si

Al Si O

Fig. 12. EDS elementary mapping of AA6061-T6 alloys oxidised for 6 h.

High concentration of all elements and magnesium at
the interface of coating/sample, by against a con-
sumption of aluminum on the right and left side is
clearly visible.
In Figs. 10 and 11, the samples which have been
oxidation treated for 2 and 4 h have a radical change in
the shape of the surface microstructure; some studies
show that this layer is porous and fissured transversely
in many places [21–23] and its thickness increases
with the oxidation time. The result of the analysis by
elementary mapping of the sample 2 h given in figure
10 shows that the concentration of all chemical ele-
ments decreased at the interface (coating/sample), the
concentration of magnesium also decreased except in
the right side, where the oxide layer is thicker than the
left side.
The result of the analysis by elementary EDS map-
ping of the sample treated for 4 h oxidation, is shown
in Fig. 11. The observations are identical to the sample
of 2 h, a decrease in the concentration of all the chem-
ical elements at the interface (coating/sample), the
aluminium is always involved and the magnesium in
this instance is present at the centre of the layer
formed.
Figures 12 and 13 show the EDS mapping analysis
of AA6061-T6 alloy after 6 and 8 h of oxidation treat-
ment. It can also be noticed in Figs. 12 and 13 that the

PROTECTION OF METALS AND PHYSICAL CHEMISTRY OF SURFACES Vol. 57 No. 4 2021

794
200 m
Al
Fig. 13. EDS elementary mapping of AA6061-T6 alloys oxidised for 8 h.
bi-layers formed on the surface of the samples oxi-
dized for 6 and 8 h. The layer in Fig. 13 is cracked in
the longitudinal direction. It is also noticeable that the
shape of the oxide layer has changed such that it is
always porous and irregular on the base metal side and
more compact and firm on the layer [21–23].
The oxide layers formed after reaction with air will
consist of a thin, relatively compact layer of alumin-
ium oxide, usually thicker and porous containing
unreacted aluminium particles. The porosity at the
interface of oxide and aluminium surface will depend
on many factors such as the atomic exchange of ions
through the same interface. The initial formation of
amorphous alumina on the surface wears off when it is
in contact with the moisture in air. It can be derived
that the aluminium surface is slightly reacted with
moisture in the air forming hiydroxides of aluminium
120
Layer thickness, μm
100
80 y = –0.002x2 + 0.471x
60
40
20
0 100 200 300
Exposure time, min
Fig. 14. Layer thickness variation with respect to exposure
time.
PROTECTION OF METALS AND PHYSICAL CHEMISTRY OF SURFACES
SAMIR ATTAFI et al.
Al Mg O C Si Mg
Si O
which transforms at around 70°C from Al2O3⋅3H2O
(Bayerite) to Al2O3⋅H2O (Boehmite) [26], which also
explains the initial minute weight loss as observed in
section 3.2. For the plain surface, lower heat flux
regime, which is similar to TGA study, allows the
weight loss occur since the number of the active nucle-
ation site density increases which is also indication of
homogeneous corrosion [27]. However the formation
of porous structure is more complex and involves the
film evaporation or moisture evaporation and hence
shaping the oxide film. The elevated temperature
results in the boiling of water vapour and the transfor-
mation from Bayerite to Boehmite when the tempera-
ture is sufficiently high the moisture is warded off and
additional oxide layer is firm in the absence of mois-
ture. The concentration of all the chemical elements is
high in the layer formed on the surface of the samples
except for the magnesium which forms compound(s)
with Al and Si. For 8 h treated specimens, aluminum
and magnesium produce low concentrations but high
concentrations of oxides are clearly visible in the layer
formed. This is reflected in the thickness of layers as
shown in Fig. 14. The thickness of oxide layer
increases with the increase of exposure time in all
specimens. The trend of increase in oxide thickness
layer is shown in Fig. 14. It is noted that the increase
in thickness accelerated after 6h of exposure to air and
ramps up at 8 h of exposure time during which the
amount of ions and diffused atoms increases and
hence does the thickness of the layer.
400 500
CONCLUSIONS
This experimental work concentrated to oxidation
at a high temperature of the AA6061-T6 alloy. This
Vol. 57 No. 4 2021
 TIME DEPENDENT AMBIENT OXIDATION OF AA6061-T6 ALLOY
alloy interacts with oxygen at high temperature, an
oxide layer covers the surface, which is porous and
contain microcracks in longitudinal and transverse
directions. The oxide layer changes its shape after 4h
of oxidation treatment in TGA device. It becomes
more compact on the outer surface and porous in the
metal oxide interface; the thickness of this layer
increases with the exposure time.
The use of the XRD has shown that the silicon is
the principal cause of porosity in the oxide layer,
which was revealed that it oxidizes below the specimen
surface, forming the silicon oxide SiO2 and the mag-
nesium remains oxidized on the outer surface in the
form of MgO.
EDS mapping and XRD analysis showed a
decrease in aluminium concentration and an increase
in magnesium at the surface. The presence of the dif-
ferent oxide which is detected by EDS, XRD and SEM
allows us to conclude that the aluminum oxidized at
high temperature and formed SiO2, MgO and Al2O3
on outer surface.
The microcracks on the outer surface of the oxide
layer were observed by microscopy and below the sur-
face by SEM, which concludes that this oxide layer
does not cling to the alloy at prolonged oxidative envi-
ronment conditions.
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