Proceedings of the ASME 2012 31st International Conference on Ocean, Offshore and Arctic Engineering
OMAE2012
July 1-6, 2012, Rio de Janeiro, Brazil
ENVIRONMENT–INDUCED CRACKING IN WELD JOINTS IN SUBSEA OIL AND
GAS SYSTEMS – PART I
M. F. Dodge
Department of Engineering,
University of Leicester
Leicester, UK.
M. Milititsky R. P. Barnett
TWI Ltd. TWI Ltd.
Great Abington, Great Abington,
Cambridge, UK. Cambridge, UK.
ABSTRACT
In subsea oil and gas systems, steel linepipes (typically API
X65) have been welded to 8630M low alloy steel hubs, using a
buttering technique and nickel alloy filler materials (e.g. Alloy
625). After buttering, postweld heat treatment (PWHT) is
carried out to temper the heat-affected zone of the low alloy
steel. However, while the vast majority of subsea joints provide
successful service, a small number of in-service failures has
had significant ramifications. During PWHT of the buttered
joints, carbon migrates from the ferritic steel to the high alloy
‘austenitic’ weld metal. The resulting microstructures and
consequent localised hardening cause sensitivity to hydrogen
induced cracking.
Subsea systems employ cathodic protection (CP) using
aluminium based anodes in order to prevent corrosion.
However, while cathodic protection has proved successful as a
means of preventing corrosion of the steel components,
complications can arise due to hydrogen charging.
This paper describes the detailed characterisation of such
dissimilar interfaces from several joint types, including
examples recovered from the seabed after exposure under CP
and newly fabricated joints, using electron microscopy,
microanalysis and nanohardness testing.
1. INTRODUCTION
1.1 Background:
Gas tungsten arc (GTA) nickel alloy buttering deposits are
commonly deposited on low alloy steel forgings, facilitating in-
shop PWHT of an assembly to remove residual stress and
temper hard heat-affected zones (HAZs), formed in the as-
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OMAE2012-83402
H.B. Dong
Department of Engineering,
University of Leicester
Leicester, UK.
V. F. Marques M.F. Gittos
TWI Ltd. TWI Ltd.
Great Abington, Great Abington,
Cambridge, UK. Cambridge, UK.
welded condition. During PWHT of the buttered joints, carbon
migrates from the ferritic steel to the high alloy ‘austenitic’
weld metal [1], causing hardening by martensite formation,
carbide precipitation [2] and carbon supersaturation [3]. After
machining a beveled weld preparation in the buttered layer, a
closure weld, typically using shielded metal arc or GTA
welding with a nickel alloy consumable, is made to join the
assembly to a micro-alloyed steel pipeline. The bevel is
positioned such that the HAZ of the closure weld lies wholly
within the austenitic buttering layers, so that no further heat
treatment is required.
Subsea, the dissimilar joint is subject to CP via aluminium
based sacrificial anodes. The majority of joints of this type have
been in service without complication, however, a small number
have failed at the interface between the buttering and the low
alloy steel.
The work presented in this paper is part of an ongoing
programme being conducted by TWI Ltd and the University of
Leicester on dissimilar joints. The emphasis of part I is
characterisation of the joints using both scanning and
transmission electron microscopy, as well as nanohardness
testing. Part II of the paper will focus on slow strain rate
mechanical testing, fracture morphologies and fracture
mechanisms from samples tested in a chloride environment
under cathodic protection.
1.2 Previous work on the microstructure of low alloy
steel - 625 buttering interfaces:
As with all dissimilar welds, there are interfacial zones with
chemical gradients between the weld metal and the parent
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 metal. At the edge of the melted zone is a region, known as the
partially-mixed zone (PMZ), which has been the focus of a
number of studies in joints of this kind, [4] and [5]. A
concensus on nomenclature has not been reached between
authors on the subject, so the various regions, illustrated
schematically in Fig. 1, are described below:
1. The body centred cubic (BCC) ferritic microstructure of
the parent low alloy steel forging which contains inclusions
and carbides.
2. A mainly ferritic, decarburised, grain-coarsened heat-
affected zone (GCHAZ) immediately adjacent to the
dissimilar interface with fingers of fused weld metal that
have penetrated into prior austenite grain boundaries.
3. A martensitic region at bead overlap positions (where
‘swirls’ normally occur) that extends into the PMZ. This
zone exhibits a body centred tetragonal structure. The
formation of martensite is thought to be promoted with
lower welding arc energies [5].
4. An austenitic FCC and apparently ‘particle free’
supersaturated carbon solid solution in a region that
appears to have solidified in a planar manner. This region
has been termed the ‘Featureless zone’, the ‘White Etching
Zone’ or ‘Zone Φ’.
5. A region within the PMZ that contains higher atomic
number interdendritic particles. This region is austenitic.
6. The bulk metal further away from the fusion zone that
exhibits an FCC matrix with a less diluted chemistry.
stainless steel) and F65 (C-Mn steel). Each of these parent
steels had been TIG-welded with ERNiCrMo-3 (Alloy 625)
wire. The nominal chemical compositions of the parent steels
and welding consumable are given in Table 1. F65 is a C-Mn
steel which does not usually require PWHT; F6NM is a low
carbon martensitic stainless steel requiring PWHT to temper
hardened HAZ microstructures and the 8630 grade is a high
carbon air hardenable material, which will form high hardness
HAZs and consequently will require PWHT. Although the exact
thermal history of the retrieved subsea joints is unknown,
typical industrial heat treatments for 8630 forgings buttered
with Alloy 625 are 650°C for 5-10 hours. The F6NM steel was
supplied in the quenched and tempered condition. After
buttering using a layering weld sequence, it was given an
industry standard PWHT.
Figure 2 - A photomacrograph of a cross-section of a
commercially produced 8630-625 dissimilar weld (8630 hub
forging shown on the left).

Table 1 – Nominal compositions of welding consumable (Alloy

625) and parent metals.
ERNiCrMo- ASTM
3 (Alloy A182
625) AISI 8630 F65 F6NM
Nominal Nominal Nominal Nominal
Figure 1 - Illustration of typical micro-scale regions at the Wt% Wt% Wt% Wt%
8630M-625 buttering interface (Adapted from [5]). Fe 0.8 Balance Balance Balance
Ni 65 0.85 - 4
1.3 Typical Failure modes: C 0.015 0.33 0.15 0.02
When bend specimens are notched at the fusion line (using Mn - 1 1.2 0.7
electro discharge machining) and subject to slow strain rate Cr 22 1 - 13
testing under cathodic protection, a number of fracture Si 0.1 0.25 - -
morphologies can be witnessed: S 0.005 0.01 0.005 -
1. In the planar solidification region of PMZs a ‘terraced P 0.005 0.01 0.01 -
cleavage’ morphology is found. Mo 9 0.4 - 0.55
2. Regions with a morphology which has an apparently Nb 3.5 - - -
interdendritic character are seen at bead overlap positions. V - 0.1 0.1 -
Cracking in these regions appears to correlate with the Cu - - 0.25 -
presence of martensite.

2. MATERIALS AND SAMPLE FABRICATION

Samples from buttered joints with three parent steels were
selected: 8630 low alloy steel, F6NM (13Wt%Cr 4Wt%Ni

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 Table 2 – History and origin of dissimilar weld specimens.
Joint
Combination
Sample (Parent Metal -
Reference Buttering) Origin
F6NM - Alloy Joint fabricated
Sample 1 625 for test work
Joint fabricated
Sample 2 F65 - Alloy 625 for test work
Recovered from
service (9
Sample 27 8630 - Alloy 625 months)
Recovered from
service (9
Sample 35 8630 - Alloy 625 months)
TEM Recovered from
sample 8630 - Alloy 625 service

3. EXPERIMENTAL APPROACH
3.1 Metallurgy across the Dissimilar Interfaces:
Transmission electron microscopy (TEM) specimen
creation: An 8630 joint buttered with Alloy 625 was selected
for in-depth characterisation by TEM. An FEI quanta 3D dual
beam focussed ion beam-scanning electron microscope (FIB-
SEM) with Omniprobe micromanipulator was used in-situ to
create TEM samples approximately 60nm thick. The key steps
in TEM specimen preparation using a dual beam system are
described briefly below:
The ion beam is used to mill either side of a deposited
protective platinum strip. The trenches created allow
the wafer face to be seen when tilted about eucentric
height.
The ion beam cuts through the thickness of the wafer
leaving the side opposite the micromanipulator needle
attached (Figure 3a).
The needle is placed in contact with the wafer and
secured by a small platinum deposit. The wafer is then
cut free from the bulk sample (Figure 3b).
The sample is secured to a copper grid using deposited
platinum tabs. It is then detached from the needle.
An electron transparent window is created by thinning
front and back faces using a small ion beam current.
The sample is measured to ensure transparency and
uniformity.
Figure 3 - a) Milled trenches allow the wafer to be released on
three sides; b) extraction of the wafer using a micromanipulator
and tungsten needle; c) ion beam image showing wafer
thickness; d) SEM image of finished wafer.
TEM sample analysis: Jeol JEM 2010 and Jeol 2100
microscopes coupled with Oxford Instruments energy-
dispersive X-ray (EDX) microanalysis equipment were used to
image and perform phase identification from the samples
created in the dual beam system. When appropriate, elemental
mapping was used.
Microstructure and Chemistry: Sections from each joint
combination cut transverse to the weld and the buttering
interface were prepared using standard polishing techniques
and examined using light and scanning electron microscopy.
Semi-quantitative analyses were conducted using EDX in order
to determine profiles for Fe, Ni, Cr, Mo and Nb.
Nanohardness Indentation: Due to the fine scale of the
various microstructures near the fusion line, nanohardness
testing was selected to measure the variation in hardness across
the steel-buttering interface. A Micromaterials Nanotester,
equipped with a Berkovich tip, was used at room temperature to
determine nanohardness. For the F65 and F6NM samples, 5 x
20 arrays were used with an indent spacing of 5μm. For the
8630 buttered with 625, angled arrays of 10 x 10 indents were
used, providing a higher point-to-point resolution.
Measurements extended up to 15 and 60μm into the steel and
nickel alloy, respectively. Indentations were performed at a
maximum load of 1.5mN using load/unload rates of 0.05mN/s
and hardness and elastic modulus were calculated by Oliver and
Pharr analysis [6].

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 4. RESULTS
4.1 Metallurgy across the welding interface:
SEM Microstructure and Chemistry: All joints examined
exhibited typical microstructures as described in Figure 1.
However, joint 27 was also found to contain localised cracks
along the interface, Fig. 4. These cracks appeared to have
formed during the seabed exposure of the sample and were
typical of cracks produced by testing under CP to simulate
subsea interfacial failures. It was notable that these cracks were
all subsurface.

Typically, the width of the PMZ in 8630-625 welded samples

was 40μm. The planar solidification region (‘featureless zone’)
was approximately 20μm wide and was identified as being the
distance between the dissimilar interface and the regions where
interdendritic niobium-molybdenum based carbide occurs, as
seen in TEM sample 2 (Fig. 5). Figure 5 - TEM brightfield image of niobium carbide in an
8630M-625 dissimilar joint.

Figure 4 - SEM backscatter image of retrieved subsea 8630-

625 joint (8630 alloy is shown on the right).

TEM Microstructure and Chemistry: An approximately mid- Figure 6 - Positioning of TEM samples with respect to the
wall thickness position in a continuous (i.e. mid-weld bead dissimilar interface in an 8630-625 joint and b) FEG-SEM
position) PMZ was selected for TEM analysis. Three brightfield STEM images of TEM samples 1-3.
extractions were made, two across the interface and one
towards the outer edge of the planar solidification region, (Fig.
6). TEM sample 1 was extracted from a region towards the
edge of a weld bead, i.e. close to a discontinuous PMZ (bead
overlap swirl). Sample 3 was selected from a mid-bead
position.

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 Figure 8 - TEM brightfield photomicrograph of the region at
the top of TEM sample 1.

Figure 7 - TEM brightfield photomicrograph montage of TEM

specimen 1.

Along the interface of sample 1, lath-like martensitic grains

were seen running vertically through the wafer. Immediately
adjacent to this is a transition zone, typified as the white,
carbide free region near to the protective platinum cap. The
nickel alloy, seen on the right hand side of Fig. 7, appeared
featureless in the SEM but, at this magnification,
nanoprecipitates were visible as dappled specks surrounded by
an FCC matrix. Point electron diffraction analysis was
inconclusive but it is suggested they were M7C3 carbides, as
they were consistent in size and shape with the precipitates
documented in [7] and [8].

At higher magnification, tilted images (Fig. 8) revealed the lath

structure more clearly and also a narrow band of particles
which are shown in the EDX elemental maps of sample 3,
given in Fig. 9b, to be rich in chromium. These particles are
potentially M23C6 carbides where M is principally Cr. Dark
globular particles, approximately 200nm x 50nm located on a
grain boundary obliquely crossing the so-called ‘featureless
zone’ in Figs. 7 and 8 are also thought to be carbides, although
point electron diffraction did not confirm this. Sample 3, further
away from the discontinuous PMZ at the bead overlap position,
had a considerably narrower lath martensite zone but displayed
a more pronounced carbide free region in the Alloy 625 next to Figure 9 – a) TEM brightfield image and b) Lower
the interface (Fig. 9a). magnification EDX elemental maps across the dissimilar
interface in TEM specimen 3.

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 an SEM-EDX linescan from the interface towards the bulk
4.2 Nano-indentation Testing: weld metal, between the middle columns of indents.
By setting the nano-indentation array at a shallow angle to the
fusion line, indent spacing limitations were overcome. An
effective spacing of less than 0.5μm perpendicular to the
interface was created without interference from the plastic
zones of neighbouring tests, Fig. 10. A calibrated FEGSEM was
used to measure the perpendicular (±1º) distance from the
centre of each indent to the fusion line. A typical array of
indentations is shown in Fig. 11.

The results from the F65 and F6NM nanohardness tests have
been discussed at length in [9]. Discounting the high
nanohardness values that appear to follow the dendrites away
from the interface, the F65 to Alloy 625 joint (no PWHT)
showed no hardness peak on the Alloy 625 side. Occasionally,
near-interface peaks in hardness were seen in the F65 parent.
Figure 10c shows nanohardness of the F6NM to Alloy 625
interface. Higher values were seen in the Alloy 625 side, with
lower hardness in the F6NM. Nanohardness measurements
showed a slight decrease in hardness immediately adjacent to
the interface on the Alloy 625 side. It should be noted that Figure 11 - A typical nano-indentation array across an 8630M-
indentation spacing may have not been fine enough to 625 interface is shown (array B on sample 35).
characterise some near-interface features.

Figure 10 – a) Light micrograph of cross-section and

indentation locations of F65-625 interface; b) Nanohardness
map for F65-625 interface is indicated; c) Nanohardness map
of F6NM-625 interface.

In an attempt to maximise resolution, for the 8630 parent Figure 12 - Nanohardness profile data for sample 27 (8630-
material joints (specimen numbers 27 and 35) the indents were Alloy 625) together with EDX data. In each graph, the interface
aligned at an acute angle of between 5° and 15° to the interface is represented by the vertical axis.
(Fig. 11). Perpendicular measurements to the interface allowed
hardness profile results to be plotted as a function of distance
from the apparent fusion line. Each array was accompanied by

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Figure 13 - Nanohardness profile data for sample 35 (8630-
Alloy 625) together with EDX data. In each graph, the interface
is represented by the vertical axis.
The plots in Fig. 12 and Fig. 13 for 8630/625 interfaces are
largely consistent with the earlier hardness maps for F65/625
and F6NM/625 in that the highest hardness was measured
deeper into the buttering, rather than immediately at the
interface. The EDX traces showed an apparent difference in the
chemical gradients at the interfaces of the two different 8630
samples, despite the fact that the bulk dilution of the beads
seemed to be leveling out at a similar composition. Unlike the
F65 and F6NM interfaces, however, three out of four plots for
8630 did show a hardness peak just inside the melted zone. One
of the arrays from the sample which contained cracks, 27B,
gave the clearest indication of a hardness peak close to the
fusion line.
5. DISCUSSION
5.1 Nanohardness Testing:
Nanohardness testing indicated a different material response for
the 8630-Alloy 625 interface when compared to the F65 and
F6NM joints buttered with the same filler. In the Alloy 8630
joints, significant hardening was found close to the fusion line.
This is an important finding and may be consistent with the
failures observed in the 8630-nickel alloy combinations in the
field ([1]and [10]). The 8630-625 dissimilar interface is known
to have inferior fracture toughness values, compared to other
interfaces tested [11]. In previous work, it has been suggested
that, if nanohardness profiles could be correlated with fracture
toughness of dissimilar interfaces measured under CP, the
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technique might be used to qualify welds of this type in the
future [9].
However, some refinement of the nanohardness testing
technique may be necessary before definitive conclusions can
be made. Consideration must be given to the unknown service
conditions of each individual joint. There is also significant
point-to-point variability in the nanohardness tests shown in
this paper, despite the arrays being positioned in very similar
regions and similar weld procedures being used throughout.
TEM work has demonstrated that there can be very large
microstructural variations experienced in distances much less
than the hardness indentation spacing: this is likely to create
nanohardness profile fluctuations. Large disparities in hardness
may arise from either grain misorientation between successive
indents or different phases, e.g. carbides, being sampled.
The cracks found in sample 27, which had been retrieved from
the seabed after being subjected to CP for 9 months, are
significant because they yield important clues about the
development of interfacial cracking in service. Thus, the
indications are that cracks develop progressively, rather than
being generated in a single large event, and are capable of
initiating below the surfaces of components. Similar cracking to
that seen in sample 27 has been observed at low alloy steel-625
interfaces tested at slow strain rates in chloride solution with
CP. Cracks have been observed forming ahead of the main
crack front, away from the area of maximum bending stress.
Fracture toughness data for joints of this kind will be presented
in part II of this paper.
6. CONCLUSIONS
The following conclusions can be drawn from this work:
1. The planar solidification region in 8630/625 buttering
interfaces is decorated by fine precipitates that are
potentially M7C3, the formation of which is likely
attributable to carbon diffusion during PWHT.
2. Hardness peaks at the interface between 8630 steel and
Alloy 625 weld metal may arise from either martensite
or carbide particles, or a combination of both. Peaks in
nanohardness at the 8630/625 interfaces were not
replicated at those with F65 and F6NM.
3. Characterisation of dissimilar joints by nanohardness
arrays requires an effective indentation spacing
perpendicular to the interface of much less than
0.5μm. Parallel to the interface, indentations should be
spaced as close together as possible, within the
limitations imposed by the plastic zones of
surrounding indentations. The described FIB-SEM lift-
out procedure has great potential for analysing
individual indents by TEM. Combined with the nano-
indentation material response, TEM analysis would
describe unequivocally the microstructures responsible
for peak hardness near the interface.
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 4. Cracks found in an 8630-625 joint, retrieved from the
seabed, indicate a progressive cracking mechanism for
interface cracking which can initiate subsurface.
ACKNOWLEDGMENTS
This work was joint funded by TWI Ltd., Cambridge, and
Mintweld, a European Commission Seventh Framework
Programme (FP7) sponsored project. The authors acknowledge
the University of Loughborough and Oxford Materials for use
of dual beam and TEM systems, respectively. Hiroto Kitaguchi,
Ashley Spencer and Geoff West are thanked for their
contributions.
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