metals

Article
Microstructural, Mechanical, Texture and Residual
Stress Characterizations of X52 Pipeline Steel
Olivier Lavigne 1 ID
, Andrei Kotousov 1, * ID
and Vladimir Luzin 2 ID

1 School of Mechanical Engineering, The University of Adelaide, Adelaide, SA 5005, Australia;

[email protected]
2 Australian Nuclear Science and Technology Organization, Lucas Heights, NSW 2234, Australia;
[email protected]
* Correspondence: [email protected]; Tel.: +61-8-8313-5439

Received: 13 June 2017; Accepted: 2 August 2017; Published: 9 August 2017

Abstract: In this paper, the microstructural and mechanical properties of a high-strength low-alloy
(HSLA) API 5L X52 steel, which is widely utilized in the construction of gas pipelines, were
characterized with optical microscopy, electron backscatter diffraction, and standard mechanical tests.
The outcomes of these characterizations were used to evaluate the strengthening contributions of the
solid solution, grain size, dislocations, and precipitates to the overall strength of the steel. In addition,
texture and residual stresses were determined with neutron diffraction. The residual stresses were
found to be low in comparison with the expected stresses due to the operating pressure. However,
these stresses could contribute to the initiation and propagation of stress corrosion cracking at the
outer surface of the pipe. Neutron diffraction results also suggested that the outer surface of the
pipe had a texture that is expected to have a low resistance to high pH stress corrosion cracking.
Both conclusions were found to be consistent with field observations.

Keywords: HSLA steel; API X52; gas pipeline; microstructure; neutron diffraction; strength; stress
corrosion cracking

1. Introduction

The strong environmental incentives for the use of natural gas as a source of clean energy
has boosted the mass production of high-strength low-alloy (HSLA) steels over the past decades.
These steels are now widely utilized in the construction of long-distance, high-pressure gas pipelines
and other pressure equipment worldwide. A great deal of research has also been directed to obtaining
an excellent combination of mechanical properties in HSLA through alloy design as well as optimizing
thermo-mechanical controlled processing (TMCP) parameters and corresponding microstructures.
TMCP promotes the formation of an acicular ferrite (AF)-based microstructure, which is the preferred
microstructure for pipe steels. Steels with AF microstructure normally possess higher strength and
toughness, as well as superior stress corrosion and fatigue resistance than steels with ferrite and
pearlite (P) microstructure [1,2].
API X52 steel is used widely as pipeline material in Australia and other countries. For example,
it is the most-used material in the existing European gas pipeline network. The importance of the
characterization of the material properties and susceptibility to various failure modes is progressively
increasing with the prospective plans of the EU to utilize the existing pipeline network for the
transportation of natural gas and hydrogen mixtures [3,4]. Therefore, the investigation of the
microstructure and mechanical properties of pipeline steels is an important aspect required for the
understanding of failure mechanisms including plastic collapse, fracture, and stress corrosion cracking

Metals 2017, 7, 306; doi:10.3390/met7080306 www.mdpi.com/journal/metals

Metals 2017, 7, 306 2 of 10

(SCC) [5,6]. All of these failure modes represent a significant threat to the integrity of pipelines and
pressure equipment.
In the present study, microstructural and mechanical characterizations of HSLA API 5L X52 steel
were conducted to assess its mechanical properties. Special attention was given to a theoretical model
for the prediction of yield strength (as an indication of the susceptibility of pipes to plastic collapse
failure) from the steel composition, microstructure, and measured hardness data.
The API 5L X52 pipes are normally formed by spiral welding technique, which inevitably leads
to the generation of residual stresses. Although the residual stresses do not affect the plastic collapse
conditions, their presence could significantly influence the susceptibility of the pipe to stress corrosion
or the initiation of fatigue cracks. With the help of neutron diffraction, the texture and the field
of residual stresses were determined to assess the susceptibility of the API 5L X52 to these failure
mechanisms. The outcomes of this study can contribute to the understanding of the stress corrosion
resistance, strength, and remaining life of the existing pipeline network made of X52 steel, which is
expected to be in service for the foreseeable future.

2. Materials and Methods

2.1. Material
API 5L X52M PSL2 steel was obtained from a pipe section with a wall thickness of 12.7 mm and
an outer diameter of 508 mm. Table 1 shows the chemical composition of the steel.

Table 1. Measured chemical composition (wt %) for the X52 pipeline steel.

Element C P Mn S Cu Ni Cr Mo Al Ti V Si Nb Fe
wt % 0.075 0.014 0.95 0.003 0.01 0.01 0.015 Tr. 0.021 0.014 0.0015 0.226 0.013 Bal.

2.2. Microstructural Analysis

2.2.1. Optical Analysis

A semi-automatic Tegramin polishing machine (Struers, Ballerup, Denmark) was used for
polishing the sample surface (cross-section of the pipe) down to 1 µm diamond paste. The samples
were then etched with 2% Nital solution, and the revealed microstructure was inspected with an Axio
Imager optical microscope (Zeiss, Oberkochen, Germany).

2.2.2. Electron Back-Scatter Diffraction (EBSD) Measurements

For EBSD measurements, final polishing was achieved using a porous neoprene disc with
a colloidal silica suspension (0.04 µm). The EBSD scans were collected using a FEI Helios Nanolab
600-SEM (Thermo Fisher Scientific, Waltham, MA, USA) equipped with an EBSD detector (EDAX
Hikari™, AMETEK, Berwyn, IL, USA). The acceleration voltage and the electron beam current of the
SEM were 20 kV and 2.7 nA, respectively. The step size was 1 µm with a hexagonal scan grid (scans
were 400 × 400 µm2 ). EDAX OIMTM Data Analysis 5.2 software (AMETEK, Berwyn, IL, USA) was
used for the data collection and analyses.

2.2.3. Hardness Measurements

The bulk hardness of the steel was determined using a Vickers indenter with a load of 10,000 gf.
The micro-Vickers hardness measurements were conducted using a LM700AT (Leco, St. Joseph, MO,
USA) at different loads from 10 gf to 1000 gf [7] in order to determine the dislocation density in the
steel, by following the method exposed in [7,8].
Metals 2017, 7, 306 3 of 10

2.2.4. Residual Stress Measurements

The residual stresses profile was measured with neutron diffraction (ND) in the pipe through
wall thickness. The measurements were performed on a strain scanning diffractometer (KOWARI,
ACNS, ANSTO, Lucas Heights, Australia) [9]. A monochromatic beam with λ = 1.67 Å from Si{400}
monochromator reflection was used in this analysis. This choice of wavelength resulted in a 3scattering
Metals 2017, 7, 306 of 10
angle of 90◦ of the sample Fe(211) reflection. A nominal gauge volume of 0.3 × 0.3 × 8 mm3 was
used scattering
to measure angletwoofprincipal
90° of the stress
sampledirections
Fe(211) reflection.
(normalAand
nominal
hoop)gauge
and volume of 0.3 × 0.3
to reconstruct the×hoop
8 mm3stress
was used to measure two principal stress directions (normal and hoop) and to reconstruct the hoop
component (under an assumption of zero normal stress). Measurement steps were 0.4 mm through
stress component (under an assumption of zero normal stress). Measurement steps were 0.4 mm
thickness and started at 0.3 mm from the outer surface. The sample was a plate of 100 × 100 mm2
through thickness and started at 0.3 mm from the outer surface. The sample was a plate of 100 × 100
dimension cut from cut
mm2 dimension thefrom
pipethe
section.
pipe section.

2.2.5.2.2.5.
Texture Measurements
Texture Measurements
The KOWARI
The KOWARI diffractometer waswas
diffractometer also also
usedused
to perform texture
to perform measurements
texture measurements in the
in pipe through
the pipe
wall thickness
through wall(at thickness
seven locations).
(at seven Samples
locations).were prepared
Samples by cutting
were prepared by acutting
slice ata slice
certain depthsdepths
at certain measured
from measured
the outer from
surface
the of the surface
outer pipes ofofabout 0.5 of
the pipes mm thick
about 0.5and
mm6thick
mm andwide. Thewide.
6 mm slice The
wasslice
thenwas
cut into
then cut into small coupons and coupons were glued together to form a cube of about
small coupons and coupons were glued together to form a cube of about 6 mm side. The orientation of 6 mm side. The
each orientation
coupon was of each couponwhen
preserved was preserved
cutting when cuttingthem
and gluing and gluing them A
together. together. A monochromatic
monochromatic beam with
beam with λ = 1.676 Å was used to measure three pole figures (110), (200), and (211) on a grid close◦
λ = 1.676 Å was used to measure three pole figures (110), (200), and (211) on a grid close to 5 × 5 , and
to 5 × 5°, and orientation distribution functions (ODF) at φ2 = 45° were plotted from these three pole
orientation distribution functions (ODF) at φ2 = 45◦ were plotted from these three pole figures [5].
figures [5].
3. Results
3. Results
3.1. Microstructural Analysis
3.1. Microstructural Analysis
3.1.1. Optical Analysis
3.1.1. Optical Analysis
Figure 1 shows
Figure thatthat
1 shows thethe
microstructure
microstructure of
of the steel consisted
the steel consistedofofferrite
ferrite
andand ~4.7%
~4.7% of pearlite
of pearlite
(determined with ImageJ analysis software (v1.48, open source)).
(determined with ImageJ analysis software (v1.48, open source)).

Figure
Figure 1. Microstructure
1. Microstructure of of X52,typically
X52, typicallyconsisting
consisting of
offerrite
ferrite(in(inwhite)
white)and pearlite
and (in black).
pearlite (in black).

3.1.2. EBSD Measurements

3.1.2. EBSD Measurements
The EBSD measurements were performed at 0.8 mm from the pipe outer surface, and are
The EBSD in
presented measurements
Figure 2. Thewere performed
inverse at 0.8(IPF)
pole figure mmshowing
from thethe pipeorientation
outer surface, and
of the are presented
grains that
in Figure 2. Thethe
constitute inverse
steel ispole figure in
presented (IPF) showing
Figure 2a. The the orientation
average grain of the
size grains that
diameter fromconstitute the steel
this scan was
is presented in Figure
evaluated as 9.35 2a.
μm Thewithaverage grain
a standard size diameter
deviation of 3.19from
μm, this
and scan was evaluated
the average as of
grain size 9.35 µm with
ferrite
determined
a standard by the
deviation oflinear intercept
3.19 µm, method
and the withgrain
average random sizetest
of lines drawn
ferrite on the scan
determined waslinear
by the measured
intercept
as 5.53 μm. The grain boundaries character is shown in Figure 2b. The fractions
method with random test lines drawn on the scan was measured as 5.53 µm. The grain boundaries of low angle grain
boundaries (LABs, between 2° and 15°) and high angle boundaries (HABs, between 15° and 180°)
were measured as, respectively, 0.08 and 0.92. The average grain boundary misorientation angle was
measured as 39.1°.
Metals 2017, 7, 306 4 of 10

character is shown in Figure 2b. The fractions of low angle grain boundaries (LABs, between 2◦ and
15◦ ) and high angle boundaries (HABs, between 15◦ and 180◦ ) were measured as, respectively, 0.08
and 0.92.
MetalsThe
2017, average
7, 306 grain boundary misorientation angle was measured as 39.1◦ . 4 of 10

(a) (b)
Figure 2. Electron back-scatter diffraction (EBSD) scan: (a) Qualitative view of the texture (001 inverse
Figure 2. Electron back-scatter diffraction (EBSD) scan: (a) Qualitative view of the texture (001 inverse
pole figure (IPF) map); (b) grain boundary orientations.
pole figure (IPF) map); (b) grain boundary orientations.
3.2. Mechanical Properties
3.2. Mechanical Properties
3.2.1. Tensile Test Results
3.2.1. Tensile Test Results
The mechanical properties of the pipe steel provided by the manufacturer are presented in Table
2. The
The specified minimum
mechanical yield
properties strength
of the (SMYS)
pipe steel for the API
provided 5L X52M
by the PSL2 is 52are
manufacturer ksipresented
or 359 MPa.
in Table 2.
The specified minimum yield strength (SMYS) for the API 5L X52M PSL2 is 52 ksi or 359 MPa.
Table 2. Tensile tests results (provided by the manufacturer).

Orientation 2. Tensile
TableYield tests (MPa)
Strength results (provided by the manufacturer).
Tensile Strength (MPa) Elongation (%)
Longitudinal 400 500 32
Orientation
Transverse Yield Strength
395 (MPa) Tensile Strength
490 (MPa) Elongation
42 (%)
Longitudinal 400 500 32
3.2.2. Hardness Measurements and395
Transverse Determination of Dislocation
490 Density 42
The dislocation density can be estimated from indentation measurements for materials
3.2.2. Hardnessindentation
displaying size effect
Measurements (ISE) [7,8]. The hardness
and Determination value isDensity
of Dislocation related to the indentation depth
by the equation [10]:
The dislocation density can be estimated from indentation measurements for materials displaying
H
indentation size effect (ISE) [7,8]. The hardness *  1
value is related to the indentation depth by
  = 1+ h   , (1)
the equation [10]:   H0 
  h
 
H 1
where H0 is the hardness in the limitation of infinite h∗
= 1 + depth , hardness, determined in this work (1)
(bulk
H0 h
as 153 HV10), h is a characteristic length, and H is the hardness value corresponding to indentation
*

H0 ish.the
wheredepth Byhardness in the limitation
fitting Equation of infinite depth
(1) to the experimental hardness(bulk hardness,
values determined
(see the in thisinwork
regression curve
as 153Figure
HV10),3), ah*value of h* ~2086 nm length,
is a characteristic could beand
obtained. h* and
H is the the dislocation
hardness density statistically
value corresponding stored
to indentation
in the lattice, ρ, are related by the equation [7,8,10]:
depth h. By fitting Equation (1) to the experimental hardness values (see the regression curve in
Figure 3), a value of h* ~2086 nm could be obtained. h* 2and
3 1 tan θ the dislocation density statistically stored
ρ
in the lattice, ρ, are related by the equation [7,8,10]: = 3 *
, (2)
2 f bh

1 tan2 θ
where θ is the angle between the surface of the3material and the surface of the indenter (22°) and f is
=
a correction factor (=1.9) for the size of theρplastic zone
3
, By introducing these values in Equation
[7,8].
∗
(2)
2 f bh
(2), ρ was approximately estimated as 6.9 × 109 cm−2.
Metals 2017, 7, 306 5 of 10

where θ is the angle between the surface of the material and the surface of the indenter (22◦ ) and
f is a correction factor (=1.9) for the size of the plastic zone [7,8]. By introducing these values in
9 −2
Equation
Metals (2), 306 approximately estimated as 6.9 × 10 cm .
2017,ρ7, was 5 of 10

Metals 2017, 7, 306 5 of 10

Figure
Figure 3. Indentationsize
3. Indentation sizeeffect
effect and fitting
fittingofofEquation
Equation(1)(1)
forfor
thethe
X52X52
steel.
steel.

3.3. Neutron Diffraction

FigureMeasurements
3. Indentation size effect and fitting of Equation (1) for the X52 steel.
3.3. Neutron Diffraction Measurements
3.3.1. Residual
3.3. Neutron Stress Measurements
Diffraction Measurements
3.3.1. Residual Stress Measurements
Figure 4a shows the profile of the residual stresses in the tangential (or hoop) direction measured
3.3.1. Residual
Figure Stress Measurements
by ND 4aforshows
the X52 the steel,
profilemainly
of the resulting
residual stresses
from theinsteelthe tangential (or hoop)
strip production. Verydirection measured
weak stress
by ND for the
FigureX52
4a steel,
shows mainly
the resulting
profile of the from
residual the steel
stresses strip
in the production.
tangential (or
distribution in the through-wall-thickness direction of the pipe was recorded, in the range of ±20 MPa Very
hoop) weak stress
direction distribution
measured
in thebythrough-wall-thickness
with ND for the X52
uncertainties ±10 MPa direction
steel,onmainly
the stress of the Although
resulting
values. pipe the
from wasstatistical
recorded,
steel in the range
striposcillations
production. are Very ±20 MPa
of weak
pronounced with with
stress
uncertainties
these error ±10
distribution in the
MPa
bars, through-wall-thickness
theonoverall
the stress
stressvalues. direction
Although
distribution of the pipe was
statistical
has features recorded,
mostoscillations in the range of
from MPa
±20
are pronounced
likely originating the with
with uncertainties
theseproduction
error bars,process:
the overall±10 MPa on
the V-shape the stress values.
in the middle
stress distribution Although
hasisfeatures
typical forstatistical
most oscillations
hotlikely
deep originating are
rolling, while pronounced
sharp
from thedrop with
to
production
these
process: theerror
compression
V-shape bars, in
close tothethe overall
surfaces
middleis stress distribution
associated
is typical with has
colder
for hot deep features
temperature
rolling, most likely
surface
while originating
treatment
sharp from An
drop(rolling). the
to compression
production process: the V-shape inbending
the middle is distribution)
typical for hot deep in rolling, while pipe
sharpthat
drop
wastostress
closeadditional
to surfaces stress component
is associated (linear
with colder stress
temperature existed
surface treatment the as-built
(rolling). An additional
compression
removed close to
by sample surfaces
cutting. is associated
In the uncut pipes, withthecolder
tensiletemperature surface treatment
stress was reconstructed (rolling).
through accurateAn
component (linear bending stress distribution) existed in the as-built pipe that was removed by sample
additional stress
measurement component
of the pipe opening(linear bending
after making stress
the distribution)
hoop cut. It was existed in the as-built
estimated to be 41pipe
MPathat was
higher
cutting. In theby
removed uncut
sample pipes, the tensile
cutting. In the stress
uncut was thereconstructed through accurate measurement of the
on the outer surface and 42 MPa lower on pipes,
the inner tensile stress
surface. Figure was
4b reconstructed
shows the total through
residual accurate
stress
pipe obtained
opening
measurementafter making
by theofcombination the
the pipe opening hoop cut.
of theafter It was
steelmaking estimated
the hoop cut.
strip production to be 41
andItbending MPa
was estimated higher on the
to be 41The
pipe process. outer
MPa surface
higher
residual
and 42onMPa
stresses lower
the outer
near theonouter
surface the
andinner
42 MPa
surfacesurface.
lower
of theon Figure
the inner
pipe 4b surface.
were shows the
Figure
thus tensile, total residual
4b shows
and had athe stress obtained
total residual
maximum value by the
stress
of
combination
obtainedof
approximatelybythethe steel
5.3% ofstrip
the YSproduction
combination of5.8%
or the steel and
of the stripbending
SMYS. production pipeandprocess.
bendingThe piperesidual
process.stresses near the
The residual
outer stresses
surface ofnear
thethe pipe outer
weresurface of the and
thus tensile, pipehad were thus tensile,
a maximum andofhad
value a maximum5.3%
approximately value of YS
of the
approximately
or 5.8% of the SMYS. 5.3% of the YS or 5.8% of the SMYS.

(a) (b)
Figure 4. Residual stresses profiles in the hoop direction for the X52 steel: (a) Measured for the sample
(a) (b)
cut out of the pipe ring; (b) Plotted including the bending pipe linear distribution stress.
Figure 4. Residual stresses profiles in the hoop direction for the X52 steel: (a) Measured for the sample
Figure 4. Residual stresses profiles in the hoop direction for the X52 steel: (a) Measured for the sample
3.3.2. Texture
cut out ofMeasurements
the pipe ring; (b) Plotted including the bending pipe linear distribution stress.
cut out of the pipe ring; (b) Plotted including the bending pipe linear distribution stress.
The orientation distribution functions obtained from the three pole figures (110), (200), and (211)
3.3.2. Texture Measurements
allows the quantitative description of the texture of the crystalline phase. In body-centred cubic steels,
The orientation distribution functions obtained from the three pole figures (110), (200), and (211)
allows the quantitative description of the texture of the crystalline phase. In body-centred cubic steels,
Metals 2017, 7, 306 6 of 10

3.3.2. Texture Measurements

The orientation distribution functions obtained from the three pole figures (110), (200), and (211)
allows the quantitative description of the texture of the crystalline phase. In body-centred cubic steels,
ODFsMetals
at φ2017, ◦
7, 306 6 of 10
2 = 45 section displays the major texture components [5,11]. These ODFs are presented
in Figure 5 at seven locations in the pipe through-wall (Figure 5a–g) along with the color scale bar
ODFs at φ2 = 45° section displays the major texture components [5,11]. These ODFs are presented in
showing the
Figure 5 at orientations intensity
seven locations in theand
pipethe ideal locations
through-wall (Figureof5a–g)
the main
along texture
with thecomponents
color scale bar on the
ODFshowing
section (schematically shown in
the orientations intensity Figure
and 5h).locations
the ideal Although ODF
of the profiles
main texturewere smoothed
components on thebyODF
the ODF
harmonic
sectionreconstruction method,
(schematically shown in an excellent
Figure grain statistic
5h). Although was provided
ODF profiles in the by
were smoothed neutron
the ODF texture
harmonic
experiment (10reconstruction
to 100 millionmethod, an excellent for
grains considered grain
eachstatistic was provided
measurement). in the
It can neutron
be seen thattexture
the texture
of theexperiment (10 to 100
steel presents million grains considered
a layer-by-layer for each
characteristic measurement).
in the through-wall It can be seen that
direction, the texture
directly linked to
of the steel presents a layer-by-layer characteristic in the through-wall direction,
the rolling process of the slab. A relatively weak texture was found at the outer surface directly linked
of the to pipe
the rolling process of the slab. A relatively weak texture was found at the outer surface of the pipe
while a typical texture of a rolled strip was found in the central line of the pipe (i.e., along the α- and
while a typical texture of a rolled strip was found in the central line of the pipe (i.e., along the α- and
γ-fibers).
γ-fibers).

min: 0.65 max: 1.42 min: 0.41 max: 2.06 min: 0.69 max: 1.43 min: 0.16 max: 2.84
(a) OS (b) 0.8 mm from OS (c) 1.2 mm from OS (d) central line

2.5

1.5

min: 0.35 max: 2.40 min: 0.31 max: 2.51 min: 0.55 max: 1.58 0.5

(e) 1.2 mm from IS (f) 0.8 mm from IS (g) IS 0

(h)
Figure 5. ODFs at φ2 = 45° section: (a) At the outer surface (OS); (b) At 0.8 mm from OS; (c) At 1.2 mm
Figure 5. ODFs at φ2 = 45◦ section: (a) At the outer surface (OS); (b) At 0.8 mm from OS; (c) At 1.2 mm
from OS; (d) At the pipe central line; (e) At 1.2 mm from inner surface (IS); (f) At 0.8 mm from IS;
from(g)
OS;At(d)
theAtinner
the pipe central
surface; line; (e) At
(h) Schematic 1.2 mm fromofinner
representation surface
the major (IS); components
texture (f) At 0.8 mm from ND,
(where IS; (g) At
the inner surface; (h) Schematic representation of the major texture components
TD, and RD are, respectively, the normal, transverse, and rolling directions). (where ND, TD, and
RD are, respectively, the normal, transverse, and rolling directions).
Metals 2017, 7, 306 7 of 10

4. Discussion

4.1. Strengthening Mechanisms

In accordance with the structure-based strength calculation model [12,13], the yield strength, σY ,
of ferritic steels can be factorized into a number of intrinsic components:

σY = σ0 + σSS + σGS + σdis + σppt (MPa), (3)

where σ0 is the intrinsic lattice friction stress (=54 MPa for pure iron single crystal [12,14]), σSS ,
σGS , σdis , and σppt are contributions from, respectively, solid solution, grain size, dislocation, and
precipitation strengthening.

4.1.1. Solid Solution Strengthening

The solid solution strengthening can be obtained by considering the effect of only Si and Mn
atoms, using the equation proposed by Pickering [14]:

σSS = 83.2 × (mass% Si) + 32.3 × (mass% Mn) (MPa) (4)

Using the values presented in Table 1, σSS was thus determined as approximately 49 MPa.
The effect of carbon was not considered, since its solubility in ferrite is negligible [15]. Carbon is
expected to be found essentially in the pearlite phase (Figure 1) and as NbC precipitates [16]. However,
the fraction of pearlite measured here (Section 3.1.1) is not expected to have any effect on the yield
strength [13,17], and the effect of the NbC precipitates on the yield strength is exposed hereafter.

4.1.2. Grain Size Strengthening

The grain size strengthening in ferrite can be expressed from the Hall-Petch equation as [13,16]:

σGS = 15.1d−1/2 (MPa), (5)

where d is the average grain size of ferrite (in mm) determined by the linear intercept method with
random test lines in the EBSD analysis (≈5.53 × 10−3 mm, see Section 3.1.2). Consequently, the value
of σGS was estimated as approximately 203 MPa.

4.1.3. Dislocation Strengthening

The strengthening contribution due to dislocations can be calculated using the following
relation [13,18]:
σdis = 0.38Gbρ−1/2 (MPa), (6)

where G is the shear modulus of the ferrite (81.6 GPa [12]), b is the Burgers vector of the dislocations
(0.248 nm [12]), and ρ = 6.9 × 109 cm−2 (see Section 3.2.2). σdis was therefore determined as
approximately 64 MPa.

4.1.4. Precipitation Strengthening

The degree of strengthening due to the precipitates is dependent on both their fraction and size in
the microstructure, and can be expressed by the following simplified relation [13]:

σppt = B (%solute) (MPa), (7)

where the values of B are presented in Table 3 [13].

Metals 2017, 7, 306 8 of 10

Table 3. Coefficient (B) of precipitation strengthening, from [13].

Solute and Precipitate Bmax (MPa/wt %) Bave (MPa/wt %) Solute Concentration (wt %)
V as V4 C3 1000 500 0–0.15
V as VN 3000 1500 0–0.06
Nb as Nb(CN) 3000 1500 0–0.05
Ti as TiC 3000 1500 0.03–0.18

The concentration of Ti and V being negligible in this X52 steel (Table 1), σppt was determined as
approximately 19 MPa by considering the average value of B for Nb as NbC precipitates.
Adding up all the intrinsic contributions in the analytical expression of the yield strength
(Equation (3)) results in an overall calculated strength of approximately 389 MPa, which correlates
well with the experimental value from the tensile tests (395 MPa).
Similarly, the hardness depends on the average ferrite grain size. This dependence has been
shown to follow a Hall-Petch relation for a ferrite/cementite steel [19], and has been determined by
regression analysis as:
HV = 56.55 + 214.19d−1/2 , (8)

where d is expressed in µm. With d = 5.53 µm, HV is analytically determined as 148, which is also in
good agreement with the measured bulk hardness value of 153 HV10.
It can be noted that the yield and the tensile strengths are empirically related to the hardness by
the following equations (derived for an X65 steel) [20]:

σY = 2HV + 105, (9a)

TS = 1.3HV + 344. (9b)

With HV = 153, σY and TS are estimated as 411 and 543 MPa, respectively, which slightly
overestimates the measured values (Table 2) of 4% and 11%, respectively.

4.2. Microstructure and Stresses Implications in Stress Corrosion Cracking Susceptibility

HSLA X65 steels were found to have an increased resistance to high pH SCC when a high intensity
of texture along the <110>//ND was measured [5,11]. At the outer surface of the considered X52 steel,
the measured texture is weak and does not present these orientations, suggesting that this steel is
normally susceptible to high pH SCC. Moreover, a high fraction of HABs is also measured, which can
promote high pH SCC to initiate and propagate [5]. The microstructure of this steel is thus typically
susceptible to high pH SCC [5,11,21,22].
Pipelines are operated to a maximum pressure level that is a percentage of the specified minimum
yield strength. For Class 1 locations, for example (offshore, or location unit that has 10 or fewer
buildings intended for human occupancy), the maximum allowable operating pressure (MAOP) is
80% of SMYS [22]. However, the areas of pipelines presenting greatest risk of high pH SCC have been
defined for MAOP >60% of SMYS [23]. For high pH SCC to occur, the stress or the stress intensity
factor must be above a threshold stress, which is reduced by small amplitude and low frequency stress
fluctuations superimposed on the mean stress [22]. It has been shown that the threshold stress for an
X52 steel decreased to 40% of the SMYS when stress fluctuations of 15% of the mean stress were applied
every 12 days [24]. Overall, this study determined the threshold stress values to comprise between
40% and 110% of the SMYS, depending on the amplitude and frequency of the stress fluctuations.
Pitting and rougher surfaces can also contribute to the decrease of the threshold stress values [25].
It can therefore be understood that the pipeline considered in this study presenting a susceptible
microstructure, operating as level of stress as low as 35% of the SMYS, and presenting additional levels
of residual stress at the outer surface (~6% of SMYS) is theoretically susceptible to the development
Metals 2017, 7, 306 9 of 10

of high pH SCC. This is consistent with observed on-site high pH SCC failure of pipeline made of
X52 steel [21].

5. Conclusions
This paper presents the outcomes of micro- and macro-characterizations of API X52 steel, which
is one of the most common structural materials of the existing pipeline network in Europe and
globally. As outlined in the previous section, the structure-based strength calculation model provides
a simple way to effectively evaluate the yield strength of X52 steels through the evaluation of
individual strengthening contributions. It is demonstrated that this model can adequately predict the
yield strength of steels with ferritic/pearlitic microstructure. However, the theoretical calculations
would probably require some adjustment in order to apply to higher strength steels such as X70,
the microstructure of which usually incorporates smaller grain sizes and different grain shapes
corresponding to acicular ferrite/bainite micro-constituents.
The present characterizations also indicated the potential contribution of the microstructure,
relatively weak texture, and residual stresses due to manufacturing to high pH stress corrosion
cracking susceptibility. This suggestion is consistent with field observations of failed X52 pipes, and
more generally with failed pipes made of higher strength API steels such as X65 [5]. Therefore, the
evaluation of the remaining life of the existing X52 pipeline network and its utilization for alternative
gas mixture transportation or storage should consider the possible damage accumulation due to stress
corrosion cracking as a result of the past operation.

Acknowledgments: This work was funded by the Energy Pipelines CRC, supported through the Australian
Government’s Cooperative Research Centres Program. The funding and in-kind support from the APIA RSC is
gratefully acknowledged. The authors acknowledge the facilities, and the scientific and technical assistance of the
Australian Microscopy & Microanalysis Research Facility at the University of Adelaide as well as Michael Law
(ANSTO) for the sample preparation for the texture measurements. The authors would also like to thank
Geoff Callar (APA Group) and Erwin Gamboa (The University of Adelaide) for discussion.
Author Contributions: Olivier Lavigne performed the OM, EBSD, and indentations experiments; Vladimir Luzin
performed the ND experiments; Olivier Lavigne, Vladimir Luzin and Andrei Kotousov analyzed the data;
Olivier Lavigne and Andrei Kotousov wrote the paper.
Conflicts of Interest: The authors declare no conflict of interest.

References
1. Costin, W.L.; Lavigne, O.; Kotousov, A. A study on the relationship between microstructure and mechanical
properties of acicular ferrite and upper bainite. Mater. Sci. Eng. A 2016, 663, 193–203. [CrossRef]
2. Costin, W.L.; Lavigne, O.; Kotousov, A.; Ghomashchi, R.; Linton, V. Investigation of hydrogen assisted
cracking in acicular ferrite using site-specific micro-fracture tests. Mater. Sci. Eng. A 2016, 651, 859–868.
[CrossRef]
3. Fernandes, T.R.C.; Chen, F.; Da Graça Carvalho, M. “HySociety” in support of European hydrogen projects
and EC policy. Int. J. Hydrog. Energy 2005, 30, 239–245. [CrossRef]
4. Mulder, G.; Hetland, J.; Lenaers, G. Towards a sustainable hydrogen economy: Hydrogen pathways and
infrastructure. Int. J. Hydrogen Energy 2007, 32, 1324–1331. [CrossRef]
5. Lavigne, O.; Gamboa, E.; Costin, W.; Law, M.; Luzin, V.; Linton, V. Microstructural and mechanical factors
influencing high pH stress corrosion cracking susceptibility of low carbon line pipe steel. Eng. Fail. Anal.
2014, 45, 283–291. [CrossRef]
6. Carretero Olalla, V.; Bliznuk, V.; Sanchez, N.; Thibaux, P.; Kestens, L.A.I.; Petrov, R.H. Analysis of the
strengthening mechanisms in pipeline steels as a function of the hot rolling parameters. Mater. Sci. Eng. A
2014, 604, 46–56. [CrossRef]
7. Faraji, G.; Mashhadi, M.M.; Bushroa, A.R.; Babaei, A. TEM analysis and determination of dislocation
densities in nanostructured copper tube produced via parallel tubular channel angular pressing process.
Mater. Sci. Eng. A 2013, 563, 193–198. [CrossRef]
Metals 2017, 7, 306 10 of 10

8. Graça, S.; Colaço, R.; Carvalho, P.A.; Vilar, R. Determination of dislocation density from hardness
measurements in metals. Mater. Lett. 2008, 62, 3812–3814. [CrossRef]
9. Alipooramirabad, H.; Paradowska, A.M.; Ghomashchi, R.; Kotousov, A.; Hoye, N. Prediction of welding
stresses in WIC test and its application in pipelines. Mater. Sci. Technol. 2016, 32, 1462–1470. [CrossRef]
10. Nix, W.D.; Gao, H. Indentation size effects in crystalline materials: A law for strain gradient plasticity.
J. Mech. Phys. Solids 1998, 46, 411–425. [CrossRef]
11. Arafin, M.A.; Szpunar, J.A. A new understanding of intergranular stress corrosion cracking resistance of
pipeline steel through grain boundary character and crystallographic texture studies. Corros. Sci. 2009, 51,
119–128. [CrossRef]
12. Kamikawa, N.; Sato, K.; Miyamoto, G.; Murayama, M.; Sekido, N.; Tsuzaki, K.; Furuhara, T. Stress-strain
behavior of ferrite and bainite with nano-precipitation in low carbon steels. Acta Mater. 2015, 83, 383–396.
[CrossRef]
13. Liu, G. Designing with Carbon-, Low-, and Medium-alloy Steels. In Handbook of Mechanical Alloy Design;
Totten, G.E., Xie, L., Funatani, K., Eds.; Taylor & Francis Inc., Marcel Dekker Inc.: New York, NY, USA, 2004;
pp. 73–89.
14. Pickering, F.B. Physical Metallurgy and the Design of Steels; Applied Science Publishers: London, UK, 1978; p. 63.
15. Bhadeshia, H.K.D.H. Models for the Elementary Mechanical Properties of Steel Welds; Institute of Materials:
London, UK, 1997; pp. 229–284.
16. Altuna, M.A.; Iza-Mendia, A.; Gutierrez, I. Precipitation strengthening produced by the formation in ferrite
of Nb carbides. In Proceedings of the 3rd International Conference on Thermomechanical Processing of
Steels, Padova, Italia, 10–12 September 2008.
17. Gladshtein, L.I.; Larionova, N.P.; Belyaev, B.F. Effect of ferrite-pearlite microstructure on structural steel
properties. Metallurgist 2012, 56, 579–590. [CrossRef]
18. Yang, J.R.; Bhadeshia, H.K.D.H. The dislocation density of acicular ferrite in steel welds. Weld. Res. Suppl.
1990, 69, 305s–307s.
19. Zhao, M.C.; Hanamura, T.; Qiu, H.; Nagai, K.; Yang, K. Grain growth and Hall-Petch relation in dual-sized
ferrite/cementite steel with nano-sized cementite particles in a heterogeneous and dense distribution.
Scr. Mater. 2006, 54, 1193–1197. [CrossRef]
20. Hashemi, S.H. Strength–hardness statistical correlation in API X65 steel. Mater. Sci. Eng. A 2011, 528,
1648–1655. [CrossRef]
21. Saleem, B.; Ahmed, F.; Rafiq, M.A.; Ajmal, M.; Ali, L. Stress corrosion failure of an X52 grade gas pipeline.
Eng. Fail. Anal. 2014, 46, 157–165. [CrossRef]
22. Zheng, W.; Elboujdaini, M.; Revie, R.W. Stress corrosion cracking in pipelines. In Stress Corrosion Cracking;
Raja, V.S., Shoji, T., Eds.; Woodhead Publishing Ltd.: Cambridge, UK, 2011; pp. 749–771.
23. Standard Practice. Stress Corrosion Cracking (SCC) Direct Assessment Methodology; NACE International:
Houston, TX, USA, 2008; ISBN 1-57590-191-9.
24. Fessler, R.R. Combination of conditions causes stress-corrosion cracking. Oil Gas J. 1976, 74, 81–83.
25. Wells, D.B. SCC threshold stress in line pipe steels. In Proceedings of the 8th Symposium on Line Pipe
Research, Houston, TX, USA, 26–29 September 1993.

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