Engineering Failure Analysis 45 (2014) 283–291

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Engineering Failure Analysis

journal homepage: www.elsevier.com/locate/engfailanal

Microstructural and mechanical factors influencing high pH

stress corrosion cracking susceptibility of low carbon line pipe
steel
Olivier Lavigne a,⇑, Erwin Gamboa a, Walter Costin a, Michael Law b, Vladimir Luzin b,
Valerie Linton c
a
School of Mechanical Engineering, The University of Adelaide, South Australia 5005, Australia
b
Australian Nuclear Science and Technology Organisation, Lucas Heights, NSW 2234, Australia
c
Energy Pipelines Cooperative Research Centre, Faculty of Engineering, University of Wollongong, NSW 2522, Australia

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

Article history: Several adjacent gas pipe sections were obtained from the field. These pipe sections had
Received 13 June 2014 nominally identical manufacturing, construction, coating and operational conditions. Some
Accepted 8 July 2014 sections were unaffected by stress corrosion cracking (SCC), whereas surrounding sections
Available online 16 July 2014
were affected by SCC. Slight differences in mechanical and microstructural properties were
found between the two types of section. Residual stress/strain and hardness close to the
Keywords: outer surface of the pipes and high angle boundary fraction values were lower for the
Microstructures
non-cracked pipe sections. Predominant h1 1 0i//ND texture was also found at the outer
Pipeline failures
Residual stress
surface of the non-cracked pipe sections. These characteristics lead to a lower crack growth
Stress corrosion cracking rate in laboratory SCC experiments. These features being mainly a result of the line pipe
Texture steel manufacturing operations, appropriate metallurgical processes leading to low
residual stress (6.2%YS), relatively low fraction of high angle boundaries (about 0.75) and
predominant {1 1 0}h1 1 0i texture in the material (or in the near surface) are expected to
greatly improve the stress corrosion cracking resistance of line pipe steels on the field.
Ó 2014 Elsevier Ltd. All rights reserved.

1. Introduction

The cost of management of corrosion in gas transmission pipelines has been evaluated to be approximately $5 billion
annually [1]. One form of corrosion, namely stress corrosion cracking (SCC) is particularly prejudicial for a gas pipeline’s
integrity and public safety and has caused rupture of a line in Australia and in other countries [2,3]. The constant need
for industry to manage this issue is obvious. Two types of SCC can be differentiated: near-neutral and high pH SCC
(pH > 9). To date, only high pH SCC has been observed in Australian gas pipelines. High pH SCC is characterised by an
intergranular (IG) crack path [4,5]. Crack initiation and growth occur by selective dissolution of the grain boundaries, while
a passive film forming on the pipe surface and on the crack sides that prevent general corrosion at those locations [3–7].
When high pH SCC occurs in pipelines, it first appears as colonies of parallel cracks running along the pipe main axis on
the external surface of the pipe. Over several years, cracks may coalesce to form larger cracks with a united crack front
[8] that can lead to pipe leak or rupture [3,7]. During a repair program on a gas transmission pipeline carried out in 2006,

⇑ Corresponding author.
E-mail addresses: lavigneolivier@hotmail.com, Olivier.lavigne@adelaide.edu.au (O. Lavigne).

http://dx.doi.org/10.1016/j.engfailanal.2014.07.011
1350-6307/Ó 2014 Elsevier Ltd. All rights reserved.
284 O. Lavigne et al. / Engineering Failure Analysis 45 (2014) 283–291

an 86 meters long segment of SCC damaged pipe (approximately seven 12 meters long pipe sections) was replaced. After the
excavation of the pipe segment, it appeared that within this segment two pipe sections did not show any SCC colonies,
whereas the pipe sections at either side were heavily damaged by SCC. It was known from the construction records that
the pipe sections in question came from the same manufacturer, were manufactured at the same time and were laid at
the same time. They were both power wire brushed and coated (coal tar enamel) over the ditch by the same operating team.
Moreover it was most probable that the pipe sections experienced the same environment (soil chemistry, temperature range,
cathodic protection levels and humidity levels) as they were adjacent to each other. As these factors were then nominally
identical for these seven pipe sections (SCC affected and non-affected), the pipe segment provided an unusual and unique
opportunity to study the SCC susceptibility of the pipe steel from a comparative metallurgical point of view. This paper
presents a detailed mechanical and microstructural characterisation of these pipes with the aim of assessing and mitigating
the SCC susceptibility of pipeline steels. The mechanical properties of the SCC affected and non-affected samples taken from
the field were analysed by tangential tensile testing and hardness measurements. The residual stress within the different
pipe units were evaluated by XRD and neutron diffraction (ND) measurements. The microstructures and the macro texture
of the samples were respectively characterised by electron-back scattering diffraction (EBSD) and ND analysis. Finally the
crack growth rate of the two types of samples were assessed and compared in the laboratory by Linearly Increasing Stress
Test (LIST) in established high-pH SCC media.

2. Material and experimental details

2.1. Material

The considered pipe section (nominal wall thickness of 8.3 mm and pipe diameter of 864 mm) was made of X65 low
carbon steel. Table 1 shows the chemical composition of the steel (wt.%). The samples were taken from the field after an
operating life of 30 years and the regions of interest were cut out from the pipes (Fig. 1a) from the 2 to 5 o’clock position
of each pipe section (12 o’clock being the top of the pipe). Fig. 1b shows a typical pipe region affected by SCC where the pipe
free surface has been white painted and SCC cracks have been revealed by Magnetic Particle Inspection. All the characteri-
sations of specimens made from the SCC affected sections were carried out on areas that did not contain any stress corrosion
cracks.

2.2. Tensile test specimens

The bulk material properties of the SCC and non-SCC affected pipe units were measured by tensile testing. Six round bar
specimens of both SCC and non-SCC affected pipe were prepared in the transverse direction of the pipes (schematically
shown in Fig. 2), following the ASTM E8-2010 standard. Gauges were 25.4 mm length and 6.4 mm diameter. The tests were
performed on a Shimadzu 100 kN servo-hydraulic testing machine.

2.3. Residual stress measurements

The tangential or hoop direction residual stresses in SCC and non-SCC affected pipes were measured with X-ray and neu-
tron diffraction. The surface stresses were measured by X-ray diffraction (XRD) with a portable XRD unit (XSTRESS 3000).
Measurements below the surface were made by material removal using electro-polishing. Each depth was measured at 8
points and the results were averaged. Stresses at positions deeper than 0.5 mm were measured by neutron diffraction
[9,10]. The residual stress measurements were performed on a strain scanning instrument (Kowari-ANSTO). A monochro-
matic beam with k = 1.666 Å and diffraction from Si{4 0 0} planes were used in this analysis. This combination of wavelength
and scattering planes resulted in a scattering angle of 90°. A nominal gauge volume of 0.5  0.5  0.5 mm3 was used. Three
directions were measured, and the principal stresses were assumed to align with the sample axes.

2.4. Texture measurements

The Kowari-ANSTO strain scanning instrument was also used to perform texture measurements on the SCC and non-SCC
affected specimens. Samples were prepared by cutting a slice from the outer surface of the pipes of about 0.5 mm thick and
6 mm wide. The slice was then cut into small coupons and coupons were glued together to form a cube of about 6 mm side.
The orientation of each coupon was preserved when cutting and gluing them together. A monochromatic beam with
k = 1.666 Å was used to measure three pole figures, (1 1 0), (2 0 0) and (2 1 1) on a grid close to 5°  5°.

Table 1
Measured chemical composition (wt.%) for the X65 pipeline steel.

C P Mn S Si Nb Fe Ceq (C + Mn/6)
0.085 0.022 1.58 0.0045 0.33 0.054 Bal 0.417
 O. Lavigne et al. / Engineering Failure Analysis 45 (2014) 283–291 285

Fig. 1. (a) Extracted pipe section from the field showing an area where the samples were cut out (ND is the normal direction, TD is the transverse direction
and RD is the rolling direction, the rolling plane (RP) is defined by the RD and TD axis). (b) Typical SCC colony occurring on pipe surfaces (cracks decorated
by magnetic particle inspection).

Fig. 2. Schematic of the specimen orientations and location of the structural analysis.

2.5. Hardness measurements

An IBIS nanoindentation system and software (Fischer-Cripps Laboratories Pty Ltd.) was used to measure the distribution
of the near surface hardness of the samples. A Berkovich type indenter was used with a diamond tip at a 0.5 N load. The Vick-
ers hardness was calculated from the load vs. depth curves recorded and after area correction. Arrays of 11  11 indents with
50 lm spacing were made on two samples of both SCC and non-SCC affected pipes and results were averaged. Measurements
were started from 30 lm below the surface. The bulk hardness of the specimens was determined using a classical Vickers
hardness testing machine at a 30 kg load.

2.6. EBSD measurements

The grain boundary microstructures of the two types of samples were observed by electron-back scattering diffraction
technique. EBSD was measured with a FEI Helios Nanolab 600-SEM equipped with an EBSD detector and the TSL OIM data
286 O. Lavigne et al. / Engineering Failure Analysis 45 (2014) 283–291

collection 5.2 software. The collected data were analysed using OIM-Analysis software (TSL Co., Ltd.). Acceleration voltage of
SEM beam for the EBSD measurement was 20 kV and the beam current was 2.7 nA. The sample surfaces were polished using
a semi-automatic LaboForce polishing machine (Struers). Final polishing was achieved using a porous neoprene disc with a
colloidal silica suspension (0.04 lm).

2.7. SCC growth tests

Flat tensile specimens were used taken with the long axis of the tensile specimens parallel to the long axis of the pipe
segment [4,11] to avoid having to straighten the material and thereby possibly altering its SCC susceptibility (see Fig. 2). Four
specimens of both SCC and non-SCC affected pipes each were prepared with the following gauge dimensions: 5 mm
length  3 mm width  2.5 mm thickness. The pipe outer diameter surface was conserved (including original brushed mill
scale) in order to simulate as close as possible the SCC behaviour of the pipeline steel observed in the field. The other faces of
the samples were mechanically ground to a standard machine finish. Linearly Increasing Stress Test (LIST) was used in this
study. This apparatus has been widely described and used in literature for SCC initiation, propagation and crack growth rate
evaluation [4,12–15]. The threshold stress for SCC initiation is reduced by small amplitude, low frequency stress fluctuations
superimposed on the mean stress [7,11,16]. In a standard LIST test, the specimen was thus subjected to a cyclic linearly
increasing and decreasing stress below the measured yield stress value, between 480 MPa and 500 MPa, at a rate of
9  102 MPa s1 (for 10 cycles). The corresponding superimposed stress was thus ±2% of the mean stress. The specimens
were exposed to the simulated high pH SCC medium defined by Parkins [3,17] and usually used in literatures [4–7,11,17],
i.e. in a 1N carbonate +1N bicarbonate solution at 70 °C with a controlled electrochemical potential of 0.6 V/SCE. A conven-
tional three electrode set-up was used [18,19] with a platinum mesh as a counter electrode, a saturated silver/silver chloride
electrode as a reference electrode and the pipeline steel specimen as the working electrode. The constant potential was
applied through an EG&G 353 potentiostat (Princeton Applied Research). This potential corresponded to the middle of the
potential range causing SCC, and was also in the middle of the active to passive transition. The applied electro-chemical
potential was oxidising, so that metallic iron Fe was oxidised to Fe2+, and a black oxide film formed visibly on the ground
face of the specimens. After the end of the experiment, each specimen’s gauge section was ground to approximately half
of the width then polished down to 1 lm diamond paste and the maximum SCC crack length was measured with an optical
microscope [20].

3. Results

3.1. Mechanical properties

Table 2 gathers the mechanical tests results for the SCC and non-SCC affected pipe obtained through the tensile round bar
specimens testing. The presented values are an average of 6 measurements on two different SCC and non-SCC affected pipe
sections respectively. TS is the tensile strength, YS/TS is the yield strength to tensile strength ratio, TE is the total elongation
of the sample at failure and Am is the sample cross sectional reduction in area. The results show that the two types of spec-
imen present very close mechanical properties.

3.2. Residual stress measurements

Fig. 3 shows the values of the residual stresses in the tangential (or hoop) direction measured by XRD and ND for the two
types of specimens. At a glance the SCC affected specimen displays higher values of tensile residual stress than the non-SCC
affected one in the first 1.5 mm from the outer surface, up to 25 MPa. An additional stress component (linear bending stress
distribution) exists in the as-built pipe that is removed by sample cutting. In the uncut pipes the tensile stress was measured
to be 18 MPa higher on the outer surface and 18 MPa lower on the inner surface. The maximum values of the measured ten-
sile residual stresses at the outer surface of the pipes are thus respectively around 9.9% and 6.2% of YS for the SCC affected
specimen and the non-SCC specimen.
Plastic strain can be evaluated by measuring the full width values at half the maximum intensity (FWHM) of the XRD
peak [21,22] as shown in Fig. 4. FWHM of the SCC affected specimen shows higher values between 20 lm and 400 lm below
the outer surface than the non-affected SCC specimen.

Table 2
Mechanical properties for the SCC and non-SCC affected pipe (average of 6 measurements on 2 different SCC and non-SCC affected pipe sections).

Pipe wall thickness (mm) YS (MPa) TS (MPa) YS/TS Am TE (%)

SCC affected 8.3 ± 0.1 525 ± 34 598 ± 13 0.877 ± 0.039 65.5 ± 9.2 23.5 ± 1.8
Non-SCC affected 8.3 ± 0.1 539 ± 32 618 ± 4 0.873 ± 0.05 68.3 ± 2.9 24.5 ± 2.6
 O. Lavigne et al. / Engineering Failure Analysis 45 (2014) 283–291 287

Fig. 3. Values of the residual stresses in the tangential (or hoop) direction measured by XRD and ND for the two types of specimen.

Fig. 4. Full width values at half maximum intensity (FWHM) of the XRD peaks for the SCC affected sample and the non-SCC affected one.

3.3. Vickers hardness measurements

The values of the bulk hardness for the SCC and non-SCC affected pipe units have been found to be similar, i.e. 212 ± 4
HV30 for both types of specimens. However microhardness measurements conducted near the outer surface have shown
more marked differences. Fig. 5 shows a detailed microhardness mapping from 30 lm below the outer surface of the pipes
on a 500  500 lm2 area region. The SCC affected pipe units display higher microhardness values range (between 200 and
220 HV0.05, Fig. 5a) than the non-SCC affected pipe units (microhardness values between 180 and 200 HV0.05, Fig. 5b).

3.4. Grain boundary character distribution

The fraction of high angle boundaries (HAB), low angle boundaries (LAB) and coincidence site lattice (CSL) at different
depth from the outer surface for the two types of specimens are shown in Fig. 6. CSL boundaries beyond R13b type are
not expected to provide strong resistance to intergranular crack propagation [23], therefore the fraction of CSL plotted in
Fig. 6 includes the CSL boundaries types from R3 to R13b. Each point on this graph represents a fraction of a grain boundary
type on a scanned area of 200  50 lm2 (0.5 lm step). The SCC affected sample shows a higher HAB fraction than the non-
SCC affected specimen.

3.5. Texture measurements

The orientation distribution functions (ODF) were plotted from the three pole figures obtained from the ND measure-
ments at the specimens’ outer surface (Fig. 7). The ODF allows to quantitatively describe the texture of a crystalline phase.
In bcc steels, ODF at u2 = 45° section displays the major texture components [23–25]. The ideal locations of the main texture
components on the ODF section are schematically shown in Fig. 7a. Although ODF profiles were smoothed by the ODF har-
monic reconstruction method, an excellent grain statistic was provided in the neutron texture experiment (10–100 million
288 O. Lavigne et al. / Engineering Failure Analysis 45 (2014) 283–291

Fig. 5. Mapping of the Vickers microhardness values below the surface for (a) the SCC affected specimen and (b) the non-SCC affected sample.

Fig. 6. Fraction of grain boundary types for the two types of specimen.

grains considered for each measurement). The non-SCC affected sample (Fig. 7c) shows a high density of h1 1 0i//ND orien-
tations with a maximum density at the {1 1 0}h1 1 0i components compared to the SCC affected specimen (Fig. 7b).

3.6. Crack growth rate (CGR) evaluation in simulated high-pH SCC environment

The crack velocity for both types of specimens was evaluated by dividing the longest crack size by the time of the exper-
iment. The CGR was obtained on an average on four samples for each specimen. For the SCC and non-SCC affected samples
the CGR measured was respectively 7.2  107 mm s1 ± 2.9  107 mm s1 and 6.1  107 mm s1 ± 1.7  107 mm s1. These
 O. Lavigne et al. / Engineering Failure Analysis 45 (2014) 283–291 289

(a)

(b)

2.5

(c) 1.5

0.5

Fig. 7. ODFs in u2 = 45° section: (a) schematic representation of the major texture components, (b) at the outer surface for the SCC affected sample and (c)
at the outer surface for the non-SCC affected specimen.

values are in good agreement with the values found in the literature in the simulated high pH SCC conditions (between 107
and 106 mm s1) [11,17,26]. As the original pipe surface was conserved (which was only power brushed over the ditch), the
specimen surface was quite rough, leading to the initiation of many stress corrosion cracks (between 50 and 200 per sample).
Crack initiation and propagation has been also observed from the machined surface of the specimens. A point to note is it
was not possible to dissociate the crack initiation time from the propagation time with this method, however the comparison
between the obtained values for both specimens are still full of information.
290 O. Lavigne et al. / Engineering Failure Analysis 45 (2014) 283–291

4. Discussion

4.1. Mechanical factors

It has been found that the residual stress of the SCC affected sample was higher than the residual stress of the non-SCC
affected specimen in the first 1.5 mm from the outer surface of the specimens (Fig. 3). This induces higher strain concentra-
tion (Fig. 4) and strain hardening of the regions below the free surface of the pipes (Hardness measurements, Fig. 5). Residual
stresses are primarily induced during pipe manufacturing (rolling process, bending and welding) and line construction
(welding) but can be enhanced by other factors as surface loading from heavily loaded trucks for example, or longitudinal
stress from ground movement or slope instability. It is also recognised that pipeline load cycling during operation may alter
the residual stresses formed during fabrication [27,28]. For high pH SCC to occur, the stress or the stress intensity factor must
be above a threshold level [7,27]. The minimum level of residual stress to cause dislocation movement (strain or yielding) at
localised (defect) region and hence to cause high pH SCC in pipeline steel has been estimated to be on the order of 60–100%
of the YS [27]. However this range of values has been determined through laboratory tests and the correlation of laboratory
determined threshold stress with the actual stress in service is quite challenging. Examining the results from this study, it is
possible that low residual stress levels (9.9% of the YS) associated with local high stress raisers as pits or dents [29] together
with tensile stresses resulting from the pipeline operation may be sufficient to initiate SCC. However, a lowest residual stress
of 6.2% of the YS might be not enough to make the steel susceptible to SCC by itself. Others synergic parameters must of
course be taken into account and some of them are discussed below.

4.2. Susceptible microstructure

A detailed study on the effect of the texture on the IGSCC of X65 pipeline steel has been reported earlier [23]. Authors
have shown that the boundaries of {1 1 0}//RP and to some extent {1 1 1}//RP textured grains respectively associated with
h1 1 0i and h1 1 1i rotations axes, provided high resistance to IGSCC, while the boundaries of {1 0 0}//RP textured grains were
the most susceptible. In the present study, the texture found at the outer surface of the non-SCC affected specimen (Fig. 7c)
displays indeed a high density of {1 1 0}h1 1 0i orientations compared to the SCC affected sample (Fig. 7b). This feature could
also explain the resistance to IGSCC observed for the non-SCC affected sample. Moreover, the grain boundaries’ character in
terms of orientation angles has been found to be different between the two specimens. The SCC affected specimen shows
indeed a higher fraction of HAB than the non-SCC affected sample. It is well accepted that random HAB have higher energy
than LAB or CSL boundaries and provide relatively easy path for crack propagation [30–32]. Moreover Wang and Atrens [4]
have shown that IGSCC could only propagate into the steel when an oxide crack corresponded to a GB. For a lowest HAB
fraction there is thus less probabilities for a crack coming through the oxide layer formed onto the surface to find a suscep-
tible GB on the matrix surface. Moreover during the propagation step the crack would encounter more LAB or CSL that may
retard its growth. The lowest fraction of HAB for the non-SCC affected sample along the wall pipe thickness would thus play a
role on the retardation of SCC initiation and propagation steps.

4.3. Environmental factors

IG high pH SCC takes many years to develop on the field. In laboratory simulated media, cracks develop in few days. In a
typical LIST experiment conducted in this study, cracks initiate and propagate in about a week. This accelerated stress cor-
rosion cracking test would expect to smooth the small differences in the mechanical and microstructural properties found
between the two types of specimen, however the CGR measured could still be discerned. The CGR of the non-SCC affected
samples were found to be lower than the CGR of the SCC affected specimens. As mentioned in the Section 3.6, these crack
growth rates include a crack initiation time. For the non-SCC affected sample the initiation time would be delayed due to the
lower residual stress/strain found below the surface and the GB character (less HAB and higher fraction of {1 1 0}h1 1 0i grain
orientation on surface than the SCC affected specimen). The crack propagation step would be lowered due also to the GB
character (more LAB and CSL than the SCC affected sample). These features, when taken together, lead to a lower overall
CGR for the non-SCC sample. This result implies that the subtle mechanical and microstructural differences mainly due to
the metallurgical processes found between the two types of specimen may play major roles on the SCC susceptibility of
the steel pipe on the field.

5. Conclusions

The SCC susceptibility of the X65 pipeline steel regarding its mechanical properties and microstructure was assessed in
this study by comparing two nominally identical adjacent pipe units, with nominally identical environment and field coating
procedure, some showing SCC and other adjacent sections not showing SCC. Small differences in the values of residual stress/
strain and hardness were found close to the outer surface of the pipes. Some relevant differences in the grain boundaries
character were also highlighted. It appeared that the specimen showing the lowest residual stress/strain and a predominant
h1 1 0i//ND texture close to the surface and the lowest HAB fraction, displayed the lowest crack growth rate in laboratory
 O. Lavigne et al. / Engineering Failure Analysis 45 (2014) 283–291 291

accelerated stress corrosion cracking test. Pipe sections with these features were found to not suffer SCC on the field over
30 years. These features being mainly a result of the line pipe steel manufacturing operations, appropriate manufacturing
processes leading to low residual stress (6.2%YS), relatively high fraction of LAB and CSL boundaries (about 0.25) and pre-
dominant {1 1 0}h1 1 0i grain orientations in the material (or in the near surface) would expected to greatly improve the stress
corrosion cracking resistance of line pipe steels.

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 would like to thank Geoff Callar for his expertise and help, as well as the workshop of the School of Mechan-
ical Engineering.
The authors acknowledge the facilities, and the scientific and technical assistance, of the Australian Microscopy & Micro-
analysis Research Facility at the University of Adelaide.

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