j m a t e r r e s t e c h n o l .

2 0 2 0;9(3):5894–5911

Available online at www.sciencedirect.com

www.jmrt.com.br

Original article

The role of non-metallic Al2 O3 inclusions, heat

treatments and microstructure on the corrosion
resistance of an API 5L X42 steel

Julio Villavicencio a,∗ , Nestor Ulloa a,b,d,∗ , Luis Lozada c , Monica Moreno d , Lidia Castro d
a Facultad de Ingeniería Mecánica y Ciencias de la Producción, Escuela Superior Politécnica del Litoral, ESPOL, Campus Gustavo Galindo,
Km 30.5 Vía Perimetral, Guayaquil, Ecuador
b Facultad de Ingeniería, Universidad Nacional de Chimborazo, UNACH, Riobamba, 060102, Ecuador
c Lundin Gold, Av. Amazonas N37-29 y UNP, Quito, Ecuador
d Grupo de Investigación y Desarrollo de Nanotecnología, Materiales y Manufactura (GIDENM), Escuela Superior Politécnica de

Chimborazo, ESPOCH, Panamericana Sur Km 1½, Riobamba, Ecuador

a r t i c l e i n f o a b s t r a c t

Article history: The role of heat treatments, non-metallic aluminium oxide inclusions, and microstructure
Received 7 February 2020 on the corrosion resistance of an API 5L X42 steel was examined in a 0.1 M chloride environ-
Accepted 29 March 2020 ment (pH ∼ 7). Energy Disperse Spectrometry analysis found aluminium oxide inclusions
Available online 25 April 2020 on as-rolled, annealed, normalised, quenched, and quenched plus tempered samples. Heat
treatments changed the percentage of aluminium oxide inclusions in X42 steel. Annealed,
Keywords: normalised, quenched, and quenched plus tempered samples reached mean values of 0.15,
Carbon steel 0.15, 0.12 and 0.07 percent respectively, whereas, rolled samples reached a mean value of 0.85
Polarisation percent. It was found that the percentage of aluminium oxides did not affect the corrosion
SEM–EDS rate but promoted pitting corrosion. The average corrosion rate showed the following order
Hardening in millimetres per year: as-rolled (0.067) < annealed (0.070) < quenched (0.078) < normalised
Inclusion (0.091) < quenched and tempered (0.103). The microstructure varied depending on the heat
Pitting corrosion treatments applied to result in pearlite/ferrite phases for annealed and normalised sam-
ples, martensite/austenite for quenched samples and tempered martensite/austenite for
quenched plus tempered samples. The higher dissolution rate of manganese and copper
elements in as-rolled and annealed samples induced the hardness of ferrite grains, improv-
ing their corrosion resistance and making ferrite grains less anodic. The corrosion resistance
of quenched and quenched plus tempered microstructures did not depend on the dissolu-
tion of elements, but the distribution of phases in their microstructures. Quenched samples
showed a single-phase microstructure that reduced the formation of micro-galvanic cou-
ples, improving corrosion resistance. Quenched plus tempered samples had two-phase
microstructures that increased the number of micro-galvanic cells, therefore reducing the
corrosion resistance of the steel.
© 2020 The Authors. Published by Elsevier B.V. This is an open access article under the
CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).

∗
Corresponding authors.
E-mails: juliocvillavicencioc@gmail.com (J. Villavicencio), nestor.ulloa@unach.edu.ec (N. Ulloa).
https://doi.org/10.1016/j.jmrt.2020.03.116
2238-7854/© 2020 The Authors. Published by Elsevier B.V. This is an open access article under the CC BY-NC-ND license (http://
creativecommons.org/licenses/by-nc-nd/4.0/).
 j m a t e r r e s t e c h n o l . 2 0 2 0;9(3):5894–5911
1. Introduction
Low carbon steels are one of the most widely used groups
of metals and have been extensively employed for oil and
gas exploration, drilling, and production [1]. Pipeline man-
ufacturing processes add agents and other alloying and
micro-alloying elements to improve mechanical and corrosion
resistance properties. However, the addition of such elements
not only enhances certain properties but also generates non-
metallic inclusions on the metal, e.g. Al2 O3 [2].
Corrosion affects the performance of materials by slowly,
but surely, eating them away. Since inclusions are the likely
place where corrosion begins, materials in service would
gradually lose function [3]. Besides, corrosion failure costs
time and money. It could compromise serious accidents and
catastrophic environmental consequences [4]. Corrosion is
responsible for 65% of pipeline failures in Ecuador, mainly to
the lack of corrosion data gathering, poor maintenance, and
monitoring [5].
Some measures to prevent corrosion damage are corrosion-
proof materials, chemical reagents, and surface-active sub-
stances [6]. Inhibitors or surface-active substances are among
the most popular methods to protect materials from corrosion
[7]. For example, low carbon, mild, and API 5L steels use inhibi-
tion to protect the material from corrosion [8–11]. Nonetheless,
there are not that many works addressing the corrosion resis-
tance in these materials from a microstructural point of view.
Microstructure and the effect of non-metallic inclusions
on the corrosion resistance of pipeline steels have barely
been studied. Few studies related to corrosion and inclusions
have been found. One proposed by Wang et al. [12], consid-
ers inclusions, such as Al–Ca–O, Al–Mg–Ca–O, Al–Ca–O–S and
Al–Mg–Ca–O–S and their contribution to triggering pitting cor-
rosion. Another proposed by Liu et al. [13] tests the influence
of Al2 O3 inclusions on localised corrosion of Q460NH steel.
Nevertheless, these studies do not address whether the per-
centage of non-metallic inclusions in the steel influences the
corrosion rate of the metal.
Microstructural changes on pipeline steels triggered by
heat treatments and their influence on the corrosion resis-
tance in various solutions have been studied by several
academics. Unfortunately, few articles have focused on the
study of API 5L X42 steels, which are widely used in Ecuadorian
oil facilities [5,14,15].
Therefore, one aim of this paper is to expand the informa-
tion available for API 5L X42 steel regarding the percentage
of Al2 O3 inclusions, and microstructural changes in anneal-
ing, normalising, quenching, and quenching plus tempering
heat-treated samples. To measure the percentage of Al2 O3
inclusions, an image analysis approach using MATLAB is
proposed. Also, this paper includes an analysis of the rela-
tionship between the percentage of Al2 O3 inclusions and the
corrosion rate of the steel in 0.1 M KCl solution using lin-
ear sweep voltammogram measurements. Finally, this study
tests the corrosion resistance of different heat-treated API 5L
X42 microstructures to provide the reader with an alternative
method to prevent corrosion damage without using traditional
chemical techniques that would eventually reduce corrosion
failures and costs.
5895
2. Materials and methods
A six-inch internal diameter pipe from an oil company in
the Ecuadorian Amazon rainforest was used in this research.
First, the pipe was cut into thirteen small pieces, 50 mm long,
20 mm wide and 3 mm thick. Eight pieces out of thirteen
were heat-treated and utilised to analyse inclusion con-
tent, microstructure, hardness, and corrosion resistance. Two
samples were also used in this research, applying no heat
treatment. These were labelled as-rolled (AR) samples. Finally,
three samples were used to obtain their chemical composi-
tion.
2.1. Chemical composition analysis
The chemical composition of the material was obtained using
a Q2-ION BRUKER spark spectrometer with argon supply. The
specimens tested were mechanically ground using numbers
50, 80 and 120 grit abrasive papers. Once the specimens were
free from voids, one by one was placed over the spark stand
opening to seal it. Two measurements were taken from three
different samples. The chemical composition of the material
could be seen in Table 1.
2.2. Heat treatments
The heat treatments applied to the specimens include
annealed, normalised, quenched, and quenched plus tem-
pered. Giving the amount of carbon content on the API 5LX42
steel, an austenitizing temperature of 870 ◦ C is enough to con-
vert the entire structure to the austenite phase [16]. Therefore,
an austenitizing temperature of 870 ◦ C for 60 min was selected
for all samples. The first sample was annealed through fur-
nace cooling. A second sample was normalised by air cooling.
A third sample was quenched in water at 19 ◦ C. Finally, the
last sample was quenched in water at 19 ◦ C and tempered at
650 ◦ C for 60 min, followed by air cooling. A summary of the
heat treatments is displayed in Table 2. Similarly, austenitiz-
ing and tempered temperatures for API steels were used in
other studies [14,17,18].
2.3. Inclusion and microstructural analysis
The heat-treated and as-rolled (AR) specimens were ground
using grit abrasive papers grade 240, 320, 400, 600, 1000 1200,
1500, and 2000. Next, the specimens were mechanically pol-
ished using Buehler alumina with particle size 1 ␮m. When
all the specimens reached a mirror-like finishing, they were
observed to determine the percentage of inclusions, morphol-
ogy, and distribution. A scanning electron microscope (SEM)
JEOL JSM–IT100 (LA) was employed to capture micrographs for
each heat-treated and as-rolled specimens. Measurements of
370 inclusions were recorded and analysed.
A quick and easy method to analyse inclusion content on
steels is provided by the ASTM E45. This method is mainly
qualitative and gives some alternative data regarding the
length and thickness of inclusions [19]. Atkinson and Shi [20]
identify several qualitative and quantitative methods to char-
acterise inclusions in clean steels. Conversely, to the methods
5896 j m a t e r r e s t e c h n o l . 2 0 2 0;9(3):5894–5911
Table 1 – Averaged chemical composition (wt.%) of an API 5L X42 steel.
C Si Mn Cr Mo Ni
0.24 0.33 1.30 0.08 0.04 0.05
Table 2 – Heat treatments applied to an API 5L X42 steel.
Heat treatment Approach
Annealed (A) Austenitizing at 870 ◦ C for 60 min,
followed by furnace cooling.
Normalised (N) Austenitizing at 870 ◦ C for 60 min,
followed by air cooling.
Quenched (Q) Austenitizing at 870 ◦ C for 60 min and
quenched in water at 19 ◦ C.
Quenched plus Austenitizing at 870 ◦ C for 60 min and
tempered (Q&T) quenched in water at 19 ◦ C. Then
tempered at 650 ◦ C for 60 min,
followed by air cooling.
pointed out in Ref. [20] and commercial software to analyse
inclusion content like the one used in Ref. [21], we used a quan-
titative approach employing MATLAB image analysis software
to determine the area covered by inclusions.
Nowadays, MATLAB software is a powerful engineering tool
with many applications in various topics that have required
image analysis [22,23]. For this reason, MATLAB programming
was used as an image analysis tool to explore and determine
the percentage of inclusions in 100× magnification micro-
graphs for each heat treatment. This paper uses the MATLAB
code proposed by Arslan [24]. This code uses K-means clus-
tering, serialises the pixels of an SEM image, and generates
an array of colours. The MATLAB programme calculates the
pixel ratio of the blackest colours that correspond to the inclu-
sions of the image. Therefore, this approach assesses the total
area of all inclusions observed in the SEM image. Similarly,
other experimental investigations have used image analysis
and MATLAB to map pixels and evaluate cracks, grain bound-
aries and defects in various steels including A36 and duplex
steel 2205 [25–27]. The reader should bear in mind that this
is an approach never used before to compute the inclusion
percentage on steels. However, accurate results are expected
thanks to the extraordinary capabilities of MATLAB software.
The composition and morphology of the non-metallic
inclusions were examined using the same scanning electron
microscope equipped with an Energy Disperse Spectroscopy
(EDS) tool. Finally, all specimens were chemically etched using
Nital 5% to observe their microstructural changes. Detailed
microstructural variations were observed utilising electron
microscopy.
2.4. Mechanical properties
Micro-indentations Vickers were performed using a Buehler
Micromet II hardness tester. Five indentations were made
on every specimen. Initially, micro-indentations were made
on the specimens without etching. After chemical etching of
the specimens, five additional indentations were applied to
the phases that presented uniformity. The applied load was
100 g for 15 s. Brinell hardness tests were applied to all spec-
imens without etching. A hardness tester ERNEST was used
Cu Al Co V Sn Fe
0.07 0.02 0.01 0.01 0.010 97.84
to determine the compound hardness of every sample. The
applied load was 187.5 kg for 10 s with a tungsten indenter of
2.5 mm diameter. The dwelling time during pre-loading was
6 s.
2.5. Corrosion tests
Five-round samples were extracted from five of the initial thir-
teen specimens described at the beginning of Section 2. The
round samples had a final diameter of 15 mm and a thick-
ness of 3 mm. A METROHMTM one-litre corrosion cell equipped
with an Ag/AgCl reference electrode, stainless steel counter
electrodes, a polypropylene sample holder that avoids any
interference with the sample, and a PGSTAT 204 potentiostat
performed electrochemical tests.
The round samples were manually grounded using a grit
abrasive paper grade 500 for 1 min before running corro-
sion tests. One square centimetre surface area of the sample
mounted on the sample holder was exposed to a 0.1 M KCl
solution without agitation and open to the environment
(dissolved oxygen naturally). Measurements of pH and tem-
perature were recorded before and after each corrosion test.
Values for the pH ranged from 6.07 to 6.64. The recorded tem-
perature of the solution in the corrosion tests ranged from 19
to 23 ◦ C.
To minimise noise and interference, the considerations
given in Ref. [28] were followed before each test. Thus, all
tests were carried out in an area with no other equipment
and power supplies. Besides, the computer that collected the
data was placed far away from the corrosion cell, and the cell
cables did not cross any other electrical cables.
NOVA 2.1.1 software run 1-h linear sweep voltammogram
measurements to determine corrosion rates through Tafel
plots. Besides, the selected scanning rate for the corrosion
tests was 5.5555e−5 V/s, and the sweeping potentials were
between −0.1 VOCP and 0.1 VOCP . Three linear polarisation tests
were conducted for each sample. Once the exposures were
completed, the round samples were removed from the sam-
ple holder and placed in the SEM specimen holder to conduct
EDS analysis. Table 3 enlists the corrosion parameters applied
to each linear sweep voltammogram test.
3. Results
3.1. Inclusion percentage and chemistry
Micrographs for the as-rolled and heat-treated samples with-
out etching are illustrated in Figs. 1 and 2. There are significant
differences regarding shape, size and the percentage of
inclusions. As-rolled samples have an elevated presence of
amorphous inclusions with irregular shapes. On the other
hand, annealed, normalised, quenched and quenched plus
 j m a t e r r e s t e c h n o l . 2 0 2 0;9(3):5894–5911
Table 3 – Linear sweep voltammogram parameters.
Parameter Value
Time to determine OCP (s) 120
Start potential (VOPC ) −0.1
Stop potential (VOPC ) 0.1
Scanning rate (V/s) 5.5555e−5
Step (V) 0.000153
Test duration (s) 3600
tempered samples showed inclusions with regular shapes
close to a rounded contour.
The maximum observed lengths or diameters for the
as-rolled, annealed, normalised, quenched and quenched
plus tempered samples were 84.9, 57.14, 24.05, 21.52 and
33.04 ␮m respectively. Some inclusion measurements seen
in Fig. 2 are presented in Table 4. Heat treatments not only
have a strong influence on inclusion shape and size but also
on the number of them spread over a specific area. MATLAB
programming showed that the as-rolled samples had the
highest amount of inclusions per area. Annealed, normalised
and quenched samples hosted a much lower amount of
inclusions compared to the as-rolled samples. Finally, the
quenched plus tempered samples held the lowest amount of
inclusions among all samples.
Fig. 3 presents the experimental data on the as-rolled and
heat-treated specimens. From the figure, it can be seen that AR
samples reported significantly more individual data variation
than the heat-treated samples. The standard deviation of the
AR samples is high compared to the other heat-treated sam-
ples. The mean value of AR samples indicates that 0.85 percent
Figure 1 – 100× micrographs without etching. a) as-rolled, b) annealed, c) normalised, d) quenched, e) quenched plus
tempered.
5897
of the total area covered by a 100× micrograph is occupied
by inclusions. Annealed, normalised, quenched and quenched
plus tempered specimens reach mean values of 0.15, 0.15, 0.12
and 0.07 percent respectively. Besides, the standard deviation
marked by the boxes is much lower than the one on AR sam-
ples. These results suggest that heat treatments significantly
contribute to reducing the area covered by inclusions in a 100×
micrograph. Likewise, heat treatments distribute inclusions in
an orderly manner and reduce the size of them, as the reader
can see in Table 4. A summary of the percentage of inclusions
in 100× micrographs is illustrated in Table 5 MATLAB image
analyses for all samples are provided from Figs. S1 to S94 (see
the supplementary information document).
EDS analysis was carried out on many inclusions for as-
rolled and heat-treated samples. These inclusions showed
high contents of aluminium and oxygen. No other elements
were found in the analysed inclusions. Fig. 4 displays several
inclusions and their chemical compositions. It is inferred that
oxygen and aluminium are combined to form Al2 O3 inclu-
sions. Furthermore, some inclusions in Fig. 4 show tertiary
inclusions growing inside secondary ones. Analysis of both
inclusions in such cases also indicated inclusions made of
aluminium and oxygen.
3.2. Microstructural changes
The heat treatments illustrated in Table 2 caused various
microstructural changes on the steel. First, Fig. 5a shows the
microstructure of an as-rolled case where one could observe
segregation of perlite in the form of bands. Fig. 5b is an
annealed microstructure. Pearlite continues forming bands in
5898 j m a t e r r e s t e c h n o l . 2 0 2 0;9(3):5894–5911

Figure 2 – Micrographs and inclusion measurements of Table 4: a) as-rolled, b) annealed, c) normalised, d) quenched, e)
quenched plus tempered.

Table 4 – Dimensions for some inclusions in Fig.2.

Sample Inclusion measurement (␮m)

1 2 3 4 5

As received 24.13 39.05 63.56 76.10 27.39

Annealed 11.07 7.29 5.72 10.12 6.03
Normalised 11.80 17.35 15.20 8.90 15.40
Quenched 18.06 12.10 14.50 14.53 15.57
Quenched plus tempered 9.43 5.48 9.97 6.31 8.08

Table 5 – Mean inclusion percentage for different heat

treatments. Duplicate data with Fig. 3.
Heat Treatment Mean inclusion percentage (%)a

As-rolled (AR) 0.85

Annealed (A) 0.15
Normalised (N) 0.15
Figure 3 – Data showing the percentage of inclusions in
Quenched (Q) 0.12
Quenched plus tempered (Q&T) 0.07
100× micrographs determined by MATLAB image analysis.
AR-as-rolled, A-annealed, N-normalised, Q-quenched, and
a
Percentage of inclusions observed in 100× micrographs. Q&T-quenched plus tempered samples. Red lines represent
the mean value for each heat treatment also showed in
Table 5. (For interpretation of the references to color in the
a much more arranged way compared to the as-rolled sam-
text, the reader is referred to the web version of this article.)
ple. Fig. 5c shows a normalised microstructure. Air cooling
has provoked not only an even distribution of pearlite and
ferrite but also grain refinement. Fig. 5d displays a quenched
microstructure. This figure shows martensite/austenite mor- 3.3. Brinell and Vickers hardness
phologies distributed all over the micrograph. Finally, Fig. 5e
displays a tempered cementite microstructure because of a Average hardness values were obtained for heat-treated and
long permanence at 650 ◦ C. as-rolled samples. As-rolled samples had a hardness of 151
 j m a t e r r e s t e c h n o l . 2 0 2 0;9(3):5894–5911 5899

Figure 4 – EDS analysis evaluating inclusions on a) as-rolled, b) annealed, c) normalised, d) quenched, e) quenched plus
tempered.

HBW 2.5/187.5. Annealed samples exhibited a hardness of
141 HBW 2.5/187.5. The latter is the lowest value among
all heat-treated samples. Because of perlite redistribution,
the normalised samples achieved a hardness of 167 HBW
2.5/187.5. Quenched samples attained a hardness of 420 HBW
2.5/187.5. This value is the largest one among the heat-treated
samples. Besides, this value results from martensite/austenite
microstructures on the steel. Finally, tempered cementite
spheres on the steel contributed to getting a hardness value of
188 HBW 2.5/187.5 for the quenched plus tempered samples.
Fig. 6 offers averaged Vickers and Brinell hardness values for
different heat-treated samples.
Furthermore, Fig. 6 contains Vickers average hardness
from specific heat-treated phases. As expected, ferrite grains
5900 j m a t e r r e s t e c h n o l . 2 0 2 0;9(3):5894–5911

Figure 5 – The microstructure of an API 5L X42 steel a) as-rolled, b) annealed, c) normalised, d) quenched, e) quenched plus
tempered.

developed different hardness values. To start, the ferrite grains
held a hardness of 213 HV0.1 for the as-rolled samples. Like-
wise, ferrite grains had a hardness of 139 HV0.1 in the annealed
samples. Due to the spread of pearlite in the normalised
samples, hardness values of 174 HV0.1 were measured for
a mixture of ferrite and pearlite grains. Martensite/austenite
microstructures of the quenched samples were homogeneous
all over the surface, resulting in an average hardness of 451
HV0.1. Finally, quenched plus tempered samples achieved a
hardness of 215 HV0.1. This belongs to a mixture of tempered
martensite and austenite.
3.4. Electrochemical corrosion
The corrosion potentials (Ecorr ) and currents (Icorr ) were
obtained from the intersection of the anodic and cathodic
slopes for each test. The calculation of the corrosion rate
was computed using Faraday’s law. The intersection of the
anodic and cathodic slopes can be found from Fig. S95 to Fig.
S124 (see the supplementary information document). The cor-
rosion potentials and currents are presented in Table 6 for
each test, along with the average corrosion rates. Moreover,
Tafel diagrams for the values with an asterisk in Table 6 are
 j m a t e r r e s t e c h n o l . 2 0 2 0;9(3):5894–5911 5901

Figure 6 – Brinell and Vickers hardness for: AR, as-rolled; A, annealed; N, normalized; Q, quenched; Q&T, quenched plus
tempered.

Table 6 – Corrosion parameters obtained from Tafel polarisation curves.

Sample Test Ecorr (V vs. Ag/AgCl) Icorr (␮A) Average corrosion rate (mm/year)

1 −0.55 7.23
As received 2 −0.58a 4.56a 0.067
3 −0.61 5.48
1 −0.53 7.7
Quenching 2 −0.53 6.51 0.078
3 −0.60a 5.74a
1 −0.56 7.82
Annealing 2 −0.61a 3.47a 0.07
3 −0.57 6.84
1 −0.57 8.13
Normalised 2 −0.56a 7.41a 0.091
3 −0.59 7.88
1 −0.53 10
Quenched and
2 −0.56a 7.52a 0.103
tempered
3 −0.58 8.94

a
Data of the Tafel diagrams from Fig. 7.

displayed in Fig. 7. Likewise, other Tafel diagrams grouped by
heat treatment and immersion time are provided from Fig.
S125 to Fig. S134 (see the supplementary information docu-
ment).
To obtain corrosion rates for each sample, the results
of each set of three measurements were averaged. Cor-
rosion rates for the samples evaluated after 1-h tests
showed the following order: as-rolled < annealed < quenched
< normalised < quenched and tempered. These results sug-
gested that the annealed and quenched samples responded
effectively to corrosion attack in the chloride environment.
3.5. SEM and EDS analysis of corrosion products
SEM images and EDS chemical analysis of corrosion products
after 1-h immersion tests are shown from Fig. 8 to Fig. 10. It
is important to highlight that all samples were affected by
pitting corrosion. Fig. 8 shows an as-rolled sample in which
the metal around a spherical inclusion has dissolved. Also,
circular corrosion pits and micro-cracks can be seen in this
figure.
Fig. 9a shows a quenched sample after conducting a corro-
sion test. Fig. 9a-1 illustrates circular corrosion pits. The centre
5902 j m a t e r r e s t e c h n o l . 2 0 2 0;9(3):5894–5911
Figure 7 – Polarisation curves for 1-h immersion in 0.1 M
KCl.
of each pit displays micro-holes. Fig. 9a-2 zooms in one pit.
Additionally, Fig. 9a-3 indicates the formation of micro-cracks
around another corrosion pit. EDS chemical analysis indicates
that the elements found in region A of Fig. 9a-2, are practically
the same as the ones got in region B of Fig. 9a-4.
Fig. 9b illustrates an annealed sample. Large amounts of
corrosion pits are observed in this image. EDS chemical anal-
yses A and B in Fig. 9b confirmed that the layer covering the
surface of the two circular pits in Fig. 9b-4 corresponds to
corrosion products.
Images of normalised and quenched plus tempered sam-
ples are observed in Fig. 10a and b, respectively. Fig. 10a-3
Figure 8 – Morphology of stings after 1 h immersion of an as-rolled API 5L X42 steel in 0.1 M KCl solution, and EDS chemical
composition of regions A and B.
displays the dissolution of metal near corrosion pits. This
heat-treated sample also has micro-cracks around a corrosion
pit, as seen in Fig. 10a-2.
Fig. 10b-1 shows a young corrosion pit with a spherical
shape. A micro-hole has formed inside this pit. The pit sur-
roundings are covered in a layer of corrosion products. In
Fig. 10b-2, it is possible to spot smaller circular corrosion-
pits neighbouring the young corrosion pit. In Fig. 10b-3 the
rounded shape of the inclusion is no longer distinguished.
The corrosion products in this sample seem to be evenly dis-
tributed over almost the entire region previously covered by
an Al2 O3 inclusion in Fig. 10b-4.
To sum up, the dissolution of Al2 O3 inclusion is constantly
repeated after running corrosion tests in as-rolled, annealed,
normalised, quenched, and quenched plus tempered samples.
EDS chemical analysis in all samples revealed that aluminium
has practically vanished, leaving behind elements such as iron
and oxygen likely bond as iron oxides.
4. Discussion
4.1. Micro-cracks and pitting corrosion mechanism
Micro-cracks were observed in as-rolled and heat-treated
samples (Figs. S140–S145 in the supplementary information
document) before conducting corrosion tests. These cracks
result from heating and cooling regimes during pipeline
manufacturing for as-rolled samples and the other control
temperature regimes of Table 2 for heat-treated samples.
The formation of micro-cracks around inclusions depends
on an important physical property, which is the coefficient of
thermal expansion. This property determines the morphol-
ogy and stress on the inclusion/metal interface. Differences in
 j m a t e r r e s t e c h n o l . 2 0 2 0;9(3):5894–5911 5903

Figure 9 – Morphology of stings after 1 h immersion of an API 5L X42 steel in 0.1 M KCl solution, and EDS chemical analysis
of the areas marked on the image. a) Quenched and b) annealed.

the coefficients of thermal expansion between inclusions and
metal contribute to the formation of micro-cracks or internal
tensions around inclusions as pointed out by Wang [12] and
Chan [29].
Therefore, micro-crack formation or textured stresses
(stress fields) during cooling are generated in the metal next
to Al2 O3 inclusions because of a variation in the coefficients
of thermal expansion of steel (10.8 × 10−6 /◦ C) and aluminium
oxide (8.2 × 10−6 /◦ C) [12,30,31].
The samples analysed after corrosion tests suggested the
occurrence of pitting corrosion. This type of corrosion has
been observed particularly in chloride solutions surrounding
spherical inclusions [12,13,32,33]. The chemical dissolution of
Al2 O3 is thermodynamically unstable in aqueous solution at
5904 j m a t e r r e s t e c h n o l . 2 0 2 0;9(3):5894–5911

Figure 10 – Morphology of stings after 1 h immersion of an API 5L X42 steel in 0.1 M KCl solution, and EDS chemical analysis
of the points marked on the images. a) Normalised and b) quenched plus tempered.

room temperature. This instability is attributed to a deficient
conductivity (standard Gibbs energy of r G = +15.86 ◦ KJ/mol) in
which the assumption of a coexistence galvanic pair between
Al2 O3 inclusions and metal could not be considered.
The pitting corrosion mechanism could be explained using
Fig. 11. Micro-crevices were created around Al2 O3 inclusions
during the heating and cooling schemes of as-rolled, annealed,
normalised, quenched, and quenched plus tempered treat-
ments. The difference in the coefficients of thermal expansion
between inclusions and metal created the crevices in Fig. 11a.
During the corrosion test, chloride ions accumulated into
these micro-crevices and got in contact with the inclusion
and metal boundaries. Similar observations have been argued
by Liu et al. [13] and Szummer et al. [34]. Likewise, several
 j m a t e r r e s t e c h n o l . 2 0 2 0;9(3):5894–5911
Figure 11 – Al2 O3 dissolution and pit formation.
researchers linked this conduct to localised corrosion because
it promotes an anodic reaction that causes the dissolution of
the metal surface around inclusions [12,13,32,35–39].
The figures available in Section 3.5 show pits in the inclu-
sion/metal interface. An illustration of pit formation can be
seen in Fig. 11b. The catalytic accumulation of chloride ions
that migrated into the pits and the concentration of oxygen
inside them caused an accelerated dissolution of the metal
that resulted in bigger pits. Bigger pits made it easier to detach
and dissolve an Al2 O3 inclusion in Fig. 11c. Indeed, high size
pits have been associated with a reduction of the pH inside
the pit [40], resulting in the dissolution of Al2 O3 inclusions.
4.2. Corrosion rate and its relation to inclusion
percentage and microstructure
The nature of inclusions found in the analysed steel showed
alumina compounds in all samples. Depending on the heat
treatment, these inclusions change their form. Globular and
irregular particles, clusters and even tertiary inclusions grow-
ing inside secondary ones were shown in Fig. 4. These
morphologies usually belong to alumina inclusions that are
linked to oxygen activity and aluminium concentration [41].
Localised corrosion was observed around alumina inclu-
sions in all samples after corrosion tests. Aluminium oxides
are hard non-deformable solids [42], but the experiments of
this work have shown that aluminium oxides dissolved after
1-h corrosion tests, leaving behind pits. As a result, high quan-
tities of inclusions would promote localised corrosion.
Fig. 12a shows the percentage of inclusions and corro-
sion rates for each sample. Even though the as-rolled samples
got the highest percentage of inclusions among all samples,
the measured corrosion rates were the lowest. Quenched and
5905
annealed samples achieved low corrosion rates, but they dis-
played a low percentage of inclusions in the metal. Though
the percentage of inclusions for the normalised and annealed
samples was the same, these two samples got different corro-
sion rates. Surprisingly, the quenched plus tempered samples
whose percentage of inclusions was the lowest got the worst
corrosion rate among all samples.
Under laboratory conditions, aluminium oxide inclusions
do not play a significant role in corrosion rates in a chloride
environment with an almost neutral pH. Nevertheless, the
dissolution of aluminium inclusions encourages the forma-
tion of pits. The greater the number of inclusions, the higher
the number of pits that would be observed. Hence, there is
no clear evidence to acknowledge a relationship between the
percentage of aluminium oxide inclusions and the detriment
or enhancement of corrosion rates. This finding agrees with
Reformatskaya et al. [43] research in which it is argued that
the corrosion rate of carbon pipe steels is influenced by phase-
structure composition rather than non-metallic inclusions.
Having rejected the hypothesis that the percentage of Al2 O3
inclusions influences corrosion rates, the next parameters to
be analysed are the hardness and microstructure of each sam-
ple. Hardness and microstructure changed after applying the
four heat treatments of Table 2.
Fig. 12b shows that the highest Brinell and Vickers
hardnesses were achieved by quenched and quenched
plus tempered samples. The former presented a marten-
site/austenite microstructure, while the latter was composed
of tempered martensite and austenite. The corrosion rates
observed in quenched samples are among the lowest recorded
for this study. Following the present results, Bhagavathi et al.
[44] suggest that improvement of corrosion rates is because of
the formation of martensite in a ferrite matrix phase which
5906 j m a t e r r e s t e c h n o l . 2 0 2 0;9(3):5894–5911
Figure 12 – a) Percentage of inclusions and corrosion rates, b) Vickers, Brinell Hardness and Corrosion rate. AR, as-rolled; A,
annealed; N, normalised; Q, quenched; Q&T, quenched plus tempered.
forms a weak galvanic couple. This galvanic couple is even
weaker between austenite and martensite, which is the case
for quenched specimens in the present study.
Conversely, quenched plus tempered specimens reached
the highest corrosion rates. This finding corroborates the ideas
of Kelestemur and Yildiz [45], who suggest that martensite
phases become more resistant to corrosion than tempered
martensite microstructures observed in steels with 0.176% of
carbon and 0.557% of manganese. This effect is attributed to
the spread distribution of tempered martensite creating many
corrosion cells where tempered martensite acts like an anode
that hastened corrosion.
Also, quenched crystalline structures differ from tempered
crystalline structures in several respects. Steel water-
quenching produces a body-centred tetragonal (BCT) marten-
site phase rich in point and line crystalline defects also known
as dislocations whereas tempering of water-quenching phases
annihilated dislocations, decompose retained face-centred
cubic (fcc) austenite and precipitate carbides [46]. Dwivedi
et al. [47] emphasise that high dislocation density is related
to the weakening of crystallographic orientation, resulting
in high corrosion rates in sites where dislocations and the
surface intersect. Escrivà et al. [48] found distinct corrosion
resistance differences between quenched and quenched plus
tempered steels. To illustrate, quenched ASTM A182 (F22) and
Ni–Cr–V–Mo (HT10) low-alloy steels had a higher corrosion rate
than the same quenched plus tempered steels. On one hand,
the study claims that atoms allocated in edge dislocations
have higher free energy resulting in preferential corrosion that
promotes iron dissolution in quenched steels. On the other
hand, tempered microstructures achieve low corrosion rates
attributed to lattice strain relief and decreasing dislocation
density.
Therefore, the quenched heat treatment should not
improve corrosion resistance as observed in the X42 steel.
However, F22 and HT10 steels have significant quantities of
chromium (2.20–2.47 wt%), molybdenum (0.93–1.52 wt%) and
nickel (3.20 wt% for HT steels) that differs from the chemi-
cal composition of the X42 steel. In fact, the elements of F22
and HT10 steels nucleated (Mo, V, Cr) 1,2 C carbides. Tempering
contributed to the distribution of these carbides enhancing
corrosion resistance. Unfortunately, the precipitation of car-
bides is not occurring in the X42 steel, which despite forming
lattice structures stressed by the severity of quenching only
relies upon the effect of chemical elements like manganese to
enhance corrosion resistance.
The lowest corrosion rates among the heat treatments
were observed for microstructures made of ferrite and pearlite
 j m a t e r r e s t e c h n o l . 2 0 2 0;9(3):5894–5911
Figure 13 – Linear EDS analysis for a) as-rolled sample crossing ferrite-pearlite grains. b) Quenched sample crossing
martensite–austenite grains.
combinations in the as-rolled and annealed samples. How-
ever, the findings of the current study do not support previous
research by Bhagavathi et al. [44] in which ferrite and pearlite
combinations form a stronger galvanic couple where ferrite
act as anode reducing the corrosion resistance of dual-phase
steels with 0.04 wt.% of carbon and 0.6 wt.% of manganese.
To explain this, an evaluation of Vickers hardness of ferrite
grains in Fig. 12b showed that hardness values of as-rolled
samples are higher than the ones measured in ferrite grains
for annealed and normalised samples. We hypothesise that
improvement of ferrite hardness in microstructures composed
by ferrite and pearlite is a key partner to enhance corrosion
rates. There are similarities between the arguments expressed
in this study and those described by Khalfallah et al. [49] where
an increase in surface hardness improves corrosion resistance
in austenitic stainless steels.
Annealed, normalised and as-rolled samples present com-
binations of body-centred cubic (bcc) ferrite and pearlite,
which is a lamellar structure, composed of bcc ferrite and
orthorhombic cementite. The dislocation density of annealed
and normalised structures is not as severe as the dislo-
cation density of the quenched structures. An example of
this is the study carried out by Kadkhodapour et al. [50] in
5907
which hardness and dislocations in a ferrite matrix with dis-
persed martensite were evaluated. Using a kernel average
misorientation approach, the study demonstrated that inner
areas of ferrite grains have lower dislocation densities than
those areas close to the boundary of ferrite/martensite and
martensite phases. Hardness also showed higher values in
regions close to the boundaries between ferrite and marten-
site.
Accordingly, lower dislocation densities are expected on
annealed than normalised heat treatments because: first, the
cooling rate for the annealed heat treatment is not as egre-
gious as the cooling rate applied in normalised or as-rolled
samples. Therefore, lower dislocation density is expected
in ferrite grains produced by annealing. Second, ferrite has
a lower solubility for carbon than austenite [46]. A steady
cooling rate applied to the annealed heat treatment allows car-
bon to diffuse from ferrite into austenite grains. As a result,
ferrite grains reach lower hardness values, as observed in
Fig. 12b. Conversely, the normalised heat treatment, which
has a higher cooling rate than the annealed heat treatment,
produces ferrite grains with trapped carbon atoms and higher
dislocation densities. These two aspects increase the hardness
of the normalised structures.
5908 j m a t e r r e s t e c h n o l . 2 0 2 0;9(3):5894–5911

Figure 14 – Linear EDS analysis for a) annealed sample crossing ferrite-pearlite grains, b) normalised sample crossing
ferrite–pearlite grains, c) quenched plus tempered sample crossing austenite grains and iron carbides colonies.

Dwivedi et al. [47] hold the view that heat treatments influ-
ence corrosion resistance, especially when dislocations get in
contact with surfaces. It is a fact that ferrite grains in annealed
and normalised structures develop crystallographic defects
triggered by cooling rates. More research on this topic needs
to be undertaken before the association between dislocation
densities and corrosion resistance of ferrite grains in annealed
and normalised structures is more clearly understood. By
contrast, as Guo et al. [51] observed: the effect of the com-
position of allowing elements in duplex stainless steels can
explain the corrosion behaviour occurring in the ferrite phase.
It can thus be suggested that ferrite grains in annealed and
 j m a t e r r e s t e c h n o l . 2 0 2 0;9(3):5894–5911
normalised microstructures of the X42 low-alloy steel rely
upon the hardness improvement thanks to the dissolution of
elements within ferrite grains rather than dislocation density.
An explanation for the improvement of corrosion resis-
tance is the dissolution of various elements into ferrite grains.
It is well known that elements, such as manganese, copper,
and nickel strengthen ferrite and improve the hardenability
of low carbon steels [52,53]. Technically, there is a signifi-
cant probability of dissolution in ferrite of elements in the
following order: manganese, chromium, tungsten, molybde-
num, and vanadium where manganese possesses a higher
tendency to dissolve in ferrite than vanadium. Solution hard-
ening indicates that any element dissolved in ferrite increases
its hardness and strength. In particular, enhancement of
hardness follows as silicon, manganese, nickel, molybde-
num, vanadium, tungsten and chromium where silicon has a
greater effect on hardness improvement than chromium [54].
Therefore, linear EDS analysis revealed chemical composition
changes in neighbour grains made of different microstruc-
tures (see the supplementary information document).
To start, Fig. 13a shows the average mass percentage of
the elements found in 20 different points crossing two ferrite
and one pearlite grains in an as-rolled sample. Data sug-
gests high quantities of copper and considerable quantities
of manganese in ferrite grains. These two elements augment
ferrite hardness, which improves the corrosion rate. In fact,
Fig. 13a shows that manganese dissolved in ferrite grains
almost equals the amount of manganese measured in the
pearlite grain. High dissolution of manganese and copper in
ferrite grains has contributed to increasing their hardness, as
observed in Fig. 12b for Vickers data.
Fig. 13b contains information for a quenched sample
where EDS analysis showed manganese, molybdenum, and
chromium distributed in martensite and austenite regions.
Particularly, manganese is interesting because its average
mass percentage is similar in austenite and martensite areas.
Additionally, quenched samples showed molybdenum con-
tents that were not observed in any other EDS linear analysis.
In particular, quenching achieves the highest hardness, as
seen in Fig. 12b. Though the martensite phase is mainly
observed in this heat treatment, the corrosion resistance is
not as good as the one seen in the as-rolled specimens.
In a similar tendency, Fig. 14a displays information for an
annealed sample. EDS analysis shows copper, manganese, and
chromium within ferrite grains whose mass percentage val-
ues are like those observed in the as-rolled sample. Lower
manganese and copper dissolution in ferrite grains decreased
their hardness compared to as-rolled specimens, as observed
in Fig. 12b. Nevertheless, these two elements contributed to
the increase of ferrite hardness enhancing the corrosion rate.
Moreover, normalised samples reached one of the highest
corrosion rates. In the case of normalised samples, it could
be attributed to the fact that copper is no longer part of fer-
rite grains, as exemplified in Fig. 14b. This element has been
replaced by nickel, which also increases ferrite hardness if it is
compared to the annealed sample. This makes sense consid-
ering that nickel attains a greater hardness improvement than
copper when it dissolves in ferrite grains. Nonetheless, corro-
sion resistance for the normalised samples is lower compared
to the annealed and as-rolled specimens. Hence, it could be
5909
conceivable hypothesised that heat treatments that provoke
the dissolution of nickel instead of copper in ferrite grains may
make them more anodic. As a result, ferrite grains become less
protected to the surrounding environment.
Finally, quenched plus tempered samples reached the
highest corrosion rates. Previously, it was suggested that this
effect occurs because tempered martensite is more anodic
than martensite itself [45]. Hardness enhancing of quenched
plus tempered microstructures does not seem to improve cor-
rosion resistance. In fact, the measurements of Brinell and
Vickers hardness in Fig. 12b are combinations of austenite and
iron carbides. The content of elements is around the same
whether the EDS analysis is performed on austenite grains
or the whole microstructure, as seen in Fig. 13c. The reason
why this heat treatment does not improve corrosion resis-
tance compared to quenched specimens is that martensite in
Fig. 12b is mainly a hard brittle single-phase microstructure
where no important galvanic couples are formed.
To summarise, there is no relationship between the per-
centage of inclusions and corrosion rate for an API 5L X42
steel immerse in a chloride environment with a pH close to
a neutral value. In contrast, ferrite hardness improvement
in as-rolled and annealed samples because of the dissolu-
tion of elements like copper and manganese in ferrite/pearlite
microstructures enhanced corrosion resistance and made fer-
rite grains less anodic. Although quenched and quenched
plus tempered samples achieved the highest hardness values,
their microstructure does not necessarily improve corrosion
resistance compared to as-rolled and annealed specimens.
The corrosion resistance of quenched and quenched plus
tempered heat treatments do not seem to depend upon
the chemical composition of the phases observed, but they
depend on the distribution of phases in the microstruc-
ture. A mainly single-phase martensite microstructure in
quenched samples reduces the formation of galvanic cou-
ples, which increases corrosion resistance. Conversely, iron
carbides colonies distributed along a tempered microstructure
make tempered martensite more anodic, resulting in higher
corrosion rates compared to quenched microstructures.
5. Conclusions
Aluminium oxides, their shape, and distribution in API 5L X42
steel samples do not influence the corrosion rate. The findings
of this study suggest that aluminium oxides disintegrate in
an oxygen dissolved environment in the presence of chloride
ions and lab conditions. A steel microstructure with a high
number of inclusions would cause a greater number of pits or
holes after corrosion tests. Nevertheless, this is not a cause to
worsen the corrosion resistance of the metal. Taken together,
these results suggest that other aspects like phase-structured
composition and hardening have a more profound effect on
corrosion resistance.
The data reported here support the assumption that heat
treatments and microstructures play an important role in the
corrosion resistance of API 5L X42 steels. In ferrite/pearlite
microstructures, heat treatments that improve ferrite hard-
ness and dissolve more manganese and copper in ferrite
grains are fundamental in promoting corrosion resistance.
5910 j m a t e r r e s t e c h n o l . 2 0 2 0;9(3):5894–5911
Indeed, as-rolled and annealed samples were demonstrated to
have the best corrosion resistance among all heat treatments
thanks to significant quantities of manganese and copper in
ferrite phases. Further work needs to be done to establish
whether copper and manganese dissolution in ferrite grains
make them less anodic, resulting in lower corrosion rates.
Finally, it seems possible that corrosion resistance of
quenched samples is enhanced thanks to a hard/brittle and
mostly single-phase martensite microstructure where the
formation of galvanic couples is reduced to the minimum.
Conversely, a quenched plus tempered heat treatment poses
a two-phase microstructure that significantly increases the
number of galvanic cells made of iron carbide (acting as the
anode) and austenite. As a result, higher corrosion rates were
observed for these microstructures compared to the quenched
microstructures.
Funding
This research did not receive any specific grant from funding
agencies in the public, commercial, or not-for-profit sectors.
Conflicts of interest
The authors declare no conflicts of interest.
Acknowledgments
The authors would like to express their gratitude to Professor
Haci Baykara for his contribution to the review of this research
paper, and Petroamazonas EP Empresa Hidrocarburífera del
Ecuador for providing the pipelines to perform this study.
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