Journal of New Materials for Electrochemical Systems 8, 115-119 (2005)

c J. New. Mat. Electrochem. Systems

Microstructural Characteristics of Different Commercially Available API 5L X65 Steels

A. Fragiel1 , R. Schouwenaarf2 , R. Guardián3 and R.Pérez

Programa de Investigación y Desarrollo de Ductos, Instituto Mexicano del Petróleo, Eje Central Lázaro Cárdenas 152, San Bartola Atepehuacan,
07730 México D.F.
1 Facultad de Química, Circuito Exterior, Ciudad Universitaria, México D. F.
2 Depto. de Ing. Mecánica, Facultad de Ingeniería, UNAM
3 Centro de Ciencias Físicas, UNAM

( Received September 24, 2004 ; received in revised form December 10, 2004 )

Abstract: An investigation was carried out on the chemical and microstructural characteristics of commercially available API 5L X65 steels.
Parameters associated with the mechanical properties were evaluated. Some of the mechanisms involved in the mechanical performance of these
steels, such as the high density of dislocations along the grain boundaries and also the grain size refinement due to the small particle precipitation
along the grain boundaries are clearly illustrated. In spite of the microstructure differences, the different steels have similar mechanical properties.

Key words : microstructural characteristics, commercial API 5L X65 steel, chemical characteristics

1. INTRODUCTION to increase the soldability properties of the steel, however, with

High strength low alloy (HSLA) steels have been widely used
for crude oil pipeline transportation in the petroleum industry.
The API-5L X65 grade steel is one of the most common pipeline
materials in the oil industry. Many different commercial X65
brand pipeline steels are available in the market [1]. Some of
these products are obtained from different fabrication routes.
The performance characteristics of these types of alloys are com-
monly related with the grain size nature and also with the carbon-
nitride precipitation [2, 3, 4 and 5].
The nature of the precipitation and also their solubility temper-
atures are the main control factors of the HSLA steel perfor-
mance responses. Thus, for example, Nb, V and Ti are micro-
alloyed elements usually used in the grain refinement process
of the steels. These elements tend to produce small precipitates
(nm´s) which tend to enhance this phenomenon [6, 7 and 8]. Mo
is also used for this purpose and with the Nb additions they tend
to increase the steel strength [8, 9 and 10]. Mn is usually added
∗ To whom correspondence should be addressed: email: rcamposp@imp.mx
the sulphur presence; it forms MnS inclusions [11, 12]. These
inclusions give rise to ductility reductions [12, 13]. Therefore,
the nature and physical properties of the precipitation is an im-
portant factor on the mechanical properties response character-
istics of the steels [14, 15]. In this investigation, four different
commercially available API 5L-X65 steels have been studied.
A comparison between their microstructure and their precipita-
tion characteristics is carried out. The chemical compositional
nature of the precipitates and their relationships with the me-
chanical properties of these steels are explored. Some of the
common properties are withdrawn and the differences in their
physical properties are discussed.
2. EXPERIMENTAL PROCEDURE
Four different API-5L X65 steels have been used in the experi-
mental tests. These steels are commercially available and their
compositions are illustrated in table 1. The specimens were ob-
tained after a controlled lamination process with a final thick-
ness of 17.5 mm. All the specimens were allowed to reach a

115
116 A. Fragiel et al./ J. New Mat. Electrochem. Systems 8, 115-119 (2005)

ferrite-austenite transformation temperature. Mechanical prop-

erties of these materials were obtained using stress-strain tests
and micro-hardness measurements. Microstructure character-
izations were also carried out using optical, scanning (SEM)
and transmission electron microscopy (TEM). The specimens
for the optical and SEM observations were prepared using Ni-
tal (2%) etching solution on the specimen’s surface. The TEM
specimens were obtained using electrochemical techniques
where the electrolyte was based on perchloric acid and methanol
in solution.

Table 1: Chemical composition of different API 5LX65 speci-

mens.
X65 / (%) X65 - A X65 - B X65 - C X65 - D
element
C 0.1400 0.1000 0.0844 0.07
Mn 1.3100 1.2900 1.0290 1.48
Si 0.2360 0.2330 0.0322 0.25
P 0.0110 0.0160 0.0110 0.013 Figure 1: SEM micrograph showing four diffrent API 5LX65
S 0.0300 0.0050 0.0082 0.002 steel microstrutures
Al 0.0023 0.0510 0.0219 0.040
Nb 0.0380 0.0470 0.0000 0.042
Cu 0.0130 0.0070 0.0130 0.09
Cr 0.1160 0.0130 0.0360 0.02
Ni 0.0220 0.1510 0.0356 0.8
Mo 0.0000 0.0000 0.0333 –
V 0.0030 0.0580 0.0536 0.064
Ti 0.0170 0.0160 0.0132 0.017
B 0.0004 0.0005 0.0000 – Table 2: Microstructural characteristics of the steels
Ca 0.0000 0.0022 0.0000 – A B C D
Grain Size (ASTM) 12 12.3 13.7 12.3
% Ferrite/Perlite 55/45% 80/20% – 83/17%
3. EXPERIMENTAL RESULTS

Figure 1 shows the SEM images of the microstructures obtained

from the four different X65 steels. The grain sizes are similar in
all the specimens with a maximum size of approximately 10 µm.
However, there are pronounced differences in the ratio between
the ferrite (%) and the pearlite (%). The values are illustrated in
table 2. Some of the mechanical parameters obtained from the
stress-strain measurements are illustrated in table 3. It is inter- Table 3: Mechanical characteristics parameters of the API
esting to point out that in spite of the microstructure differences steels.
of the specimens (ferrite (%)/pearlite (%)); the mechanical pa-
API 5LX65 YS(MPa) UTS(MPa) E(Gpa) HV
rameters are quite similar in values. The magnitude similarities
A 428 563 151 175.374
of the associated parameters of the mechanical properties could
B 423 541 142 182.365
perhaps be related with the similar controlled lamination pro-
C 431 530 182 209.574
cess used to obtain these steels [6].
D 520 570 175 190.0
The presence of inclusions or precipitates in these steels has a
strong influence on their mechanical properties [17, 18]. Thus
for example, the high strength of the micro-alloyed steels is re-
lated with the grain refinement induced by small metallic par-
 Microstructural Characteristics of Different Commercially Available API 5L X65 Steels / J. New Mat. Electrochem. Systems 8, 115-119 (2005) 117

ticles. Thus for example, the precipitation of small carbon ni-

trides particles has a strong influence on the grain refinement
and also in the obtained high strength values [19].

Large particles precipitation (in the µm´s range) has been as-
sessed in the four different X65 steels. This is illustrated in
figure 2, where the optical micrographs clearly show the nature
of the precipitation in some of the steel types. The precipitated
particles show different morphologies. Spheroidal shapes can
frequently be found, however, most of the precipitated parti-
cles do not present defined shapes. They usually have elongated
shapes. These results are illustrated in the attached histograms
(figure 3). In this figure the number of spheroidal and elongated
shapes are illustrated. The chemical spectra obtained from the
elongated particles and spheroidal particles show a composition
rich in Mn and S. This result is illustrated in figure 4. Therefore,
the elongated particles are MnS compounds.

Figure 2: Inclusion distribution form different API 5L X65

steels (Optical Microscopy) Figure 3: Inclusion distribution histograms. a) Distribution for
A,B steels, b) Distribution for C steel, c) Distribution for D
steel.
Transmission electron microscopy observations of specimens
from the four different steels have also been carried out. These
specimens show similar microstructural characteristics. Thus,
for example, figure 5 shows bright and dark field images from
two different steel specimens. Both specimens show high den-
sity of dislocations close to the grain boundaries. It is widely
known that this dislocations accumulation has strong influence
on the mechanical properties. The grain boundaries act as bar-
rier to the dislocation movements and therefore an effect on
the steel ductility properties is always expected. Another in-
teresting structural feature commonly obtained in these steels
is related with the strong small particles precipitation along the
grain boundaries. This result clearly illustrates the grain size re-
finement mechanism through the precipitation of small particles
along the grain boundaries. This is showed in figure 6.

Titanium sulphide particles of different morphological charac- Figure 4: Typical chemical composition of the API steels ob-
teristics have also commonly found in the steel specimens. Fig- tained by EDX analysis.
ure 7 shows the bright and dark field images of two different
118 A. Fragiel et al./ J. New Mat. Electrochem. Systems 8, 115-119 (2005)
Figure 5: Dark field TEM image of C(a), D(b) steels types
Figure 6: TEM micrograph showing small particles precipita-
tion along the grain boundaries
Ti2 S particles. The images show two crystalline specimens of
Ti2 S particles along different crystalline orientation. This is par-
ticularly clear from the dark field image (figure 7a) where both
particles display different image contrast with different extinc-
tion distances. It is interesting to point out that small particles
precipitation, similar to the precipitation along the grain bound-
aries, is also obtained in these Ti2 S particles. The small particle
precipitation can clearly be seen along the boundary between
the two crystals and also along the edge of both crystallites.
However, it is also important to mention that some Ti2 S parti-
cles do not show any precipitation. This is illustrated in figure 8.
4. CONCLUSIONS
The mechanical properties obtained from the different steels are
similar in their magnitudes; therefore there is not appreciable
Figure 7: Dark (a) and bright (b) field TEM images showing
two different TiS2 precipitated particles
Figure 8: TEM bright field image of a TiS2 precipitated
dependence on the microstructures characteristics. These steels
have spheroidal inclusions ( ∼ 80%) and also inclusions with
undefined shapes ( ∼ 20%). The inclusions chemical composi-
tion shows Ca, S, and Mn and also minor amounts of Mg and C.
High dislocation density and also high small particles precipi-
tation are obtained along the grain boundaries. Different Ti2 S
particles morphology has been found.
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