5/6/24, 1:05 PM Mechanical, microstructure and texture characterization of API X65 steel - ScienceDirect

Materials & Design

Volume 47, May 2013, Pages 529-538

Technical Report

Mechanical, microstructure and texture

characterization of API X65 steel
Ehab El-Danaf a , Muneer Baig b, Abdulhakim Almajid a b, Waleed Alshalfan c, Marawan Al-Mojil c,
Saeed Al-Shahrani c

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https://doi.org/10.1016/j.matdes.2012.12.031
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Abstract
American Petroleum Institute (API) grade X65 steel plate was characterized for its microstructure, texture
and mechanical properties. The microstructure was found to be mainly composed of polygonal ferrite grains
coexisting with few quasi polygonal ferrite grains. The average grain size with a critical misorientation of
15° was found to be about 3.3 μm. The average misorientation angle was about 36° with a fraction of high
angle grain boundaries of 90%. Texture was studied and revealed a high orientation density function values
around the γ-fiber. Tensile tests yielded a strength coefficient of 711 MPa, a strain hardening exponent of
0.087 and a tensile yield to ultimate stress ratio of 0.85. Constitutive modeling for the room temperature
experimental stress–strain responses in compression was also conducted and the materials constants for
the Johnson–Cook model are reported. The correlations from the model were seen to be in close proximity
with the observed experimental data. Fracture toughness was measured on a compact tension samples
along three directions, as per specifications mentioned in ASTM E399-09 standard. The KI values were not
for the plane strain condition as the thickness requirement was not met.

Highlights
► X65 steel was characterized for microstructure, texture and mechanical properties. ► Constitutive
modeling for the room temperature compression was conducted. ► Texture was studied and revealed a
high orientation density around the γ-fiber. ► Fracture toughness was measured on compact tension
samples along three directions.

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1. Introduction
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5/6/24, 1:05 PM Mechanical, microstructure and texture characterization of API X65 steel - ScienceDirect

In recent years, there have been increasing demands for high performance line pipe steels which feature not
only high strength but also good low-temperature toughness [1]. There are three basic strengthening
mechanisms for steel: (1) precipitation hardening, (2) solid solution hardening, and (3) transformation
strengthening. Transformation strengthening is the most important among them, and it is achieved by the
micro-alloying and application of thermomechanical control process (TMCP) technology. TMCP technology
has enabled the production of excellent steel plate with high-strength and good low-temperature toughness
[2]. TMCP is roughly divided into two processes; slab reheat followed by controlled cooling to
thermomechanical rolling followed by either direct quenching and tempering or water cooling followed by
air cooling [2]. Since strength and low-temperature toughness depend on various process conditions, the
processing conditions in TMCP (slab reheat temperature, cooling rate, amount of hot rolling deformation)
have to be optimized in order to obtain high-strength and low-temperature toughness of the plate [2]. It
was concluded [3] that with increasing the amount of hot deformation, many defects such as dislocations
and stacking faults within the deformed austenite grains are produced, and thus it is likely to be the most
effective means of acicular ferrite formation. However, an increase in the amount of the austenite stabilizing
elements such as Cu and Ni suppresses the formation of acicular ferrite [3].

In pipeline steels the ferrite can assume different morphologies [4]. Polygonal ferrite (PF) which is
transformed at the highest temperatures and slowest cooling rate, assumes equiaxed grains with smooth
continuous boundaries under the scale of optical microscopy; Quasi-polygonal ferrite (QF) which is
produced by transformation through short range diffusion across ferrite/austenite interface, assumes grains
with irregular and jagged boundaries containing high density of dislocations, subboundaries and
martensite/austenite (M/A) constituents; Granular bainitic ferrite (GF) which forms at the same
transformation temperature as bainite, but at slower cooling rate. Granular equiaxed retained austenite or
M/A islands dispersed in ferritic matrix; Bainitic ferrite (BF) which is characterized with many elongated
ferritic lath bundles with high density of dislocations separated with high angle grain boundaries; Acicular
ferrite (AF) which is a complex structure consisting of QF, GF, BF and few PF with dispersed islands of
second phases in the matrix it is characterized with relatively high density of dislocations and fine grained.
Kim et al. [3] have defined acicular ferrite through electron backscattered diffraction (EBSD) analyses and
showed that an acicular ferrite grain consists of several sub-units misoriented by 1–2° and that a set of
adjacent acicular ferrite grains with crystallographic misorientation below 15° makes up the
crystallographic packet. All or some of these ferrite forms can coexist but the various degree of mixture
depends on the thermomechanical processing route. The combination of these microstructures can directly
affect the strength level and consequently the susceptibility to stress corrosion cracking [5], [6], [7].

It is important that the increase in the yield strength is not accompanied by a decrease in fracture toughness
and formability because a decrease in toughness will encourage stress induced cracking, and reduced
formability will cause difficulties in forming (e.g. pipe-bowing). Thus, the important requirement for the
pipeline manufacturing industry is to select the material that has high strength in association with high
toughness and formability. The American Petroleum Institute (API) specifications for line pipe steels
generally require a low YS/UTS ratio which is equivalent to a high work hardening rate. API specifies a
YS/UTS ratio generally not greater than 0.93 for an application involving pipelines. This ratio is affected by
the microstructure of the steel and is achieved by carefully controlling the hot rolling, cooling and coiling
schedules. It is important that the microstructure of the pipeline steel provides combination of
aforementioned properties. Therefore, judicious selection of alloying elements is necessary to obtain
beneficial effect on mechanical properties with reduced alloy cost. For instance, the numbers of alloying
elements are reduced to achieve lower carbon equivalent (CE) to ensure good field weldability.

Standard K1C fracture toughness testing procedures essentially dictates a size requirement for valid K1C
testing (thickness, B ⩾ 2.5 ( ) which almost prohibits routine measurement of K1C for a number of

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5/6/24, 1:05 PM Mechanical, microstructure and texture characterization of API X65 steel - ScienceDirect

steel products due to limited thickness [8]. This is the reason behind the good proportional relationships
between the Charpy absorbed energy and the K1C values which have been established for a wide variety of
steels [9]. Several empirical formulae have been proposed that predict K1C from the upper shelf Charpy
energy, CVN [10]. Numerous studies have been performed in this area to characterize the fracture and
fracture toughness of steels. Of these studies only very few studies has been dedicated to determination of
plane strain fracture toughness. This is due to the stringent requirements on the geometry of the specimens
(ASTM E399-09 standard test method) for obtaining a valid K1C test. In a previous study [4], comparison
studies on mechanical properties were made on a commercial X70 grade polygonal ferrite (PF) dominated
pipeline steel and a laboratory developed X90 grade acicular ferrite (AF) dominated pipeline steel obtained
by optimum thermo-mechanical controlled processing (TMCP). The Charpy impact test results indicated
that, the upper shelf energy (USE) of the AF pipeline steel was a little bit higher, but its energy transition
temperature (ETT) was extremely low, about −162 °C, much lower than that of the PF pipeline steel of about
−121 °C.

The present work focuses on the characterization of microstructure, texture and mechanical properties of
X65 API steel plates. The room temperature compression stress–strain behavior is modeled using Johnson
Cook model. The fracture toughness was evaluated in T-L (crack propagation is in the rolling (longitudinal)
direction), L-T (crack propagation is in the transverse direction) and at 45° to T-L orientation using the
compact tension sample which was fatigue pre cracked using the ASTM E399-09 standard procedure.

2. Experimental procedures

2.1. Material composition

The API grade X65steel plates was supplied by SABIC Research and Development Center, Jubail, Saudi Arabia
in the form of rolled plates of 15 mm thickness. The chemical composition can be seen in Table 1.

Table 1. Chemical composition of X65.

API grade C Si Mn P S Fe

X65 0.1 0.3 1.45 0.02 0.003 Bal.

2.2. Microstructure
The microstructure on the transverse section was studied by optical microscopy (OM) and by electron
backscattered diffraction (EBSD) using Oxford HKL system incorporated on a field emission scanning
electron microscope (FESEM) 7600 JEOL. The specimens were prepared according to the standard
procedures for specimen preparation including grinding, polishing and etching. Nital etchant was used to
reveal the specimen’s microstructure; grain size, by immersion for 5 s. For EBSD, the samples were taken
through the same procedure for OM, and further polished using colloidal silica on a vibratory polisher.

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