MPWT19-15278

Stress Corrosion Cracking Susceptibility of a Super Duplex Valve

Alberto Gerolin
Orion S.p.A.
Via G.S. Caboto, 8
Trieste, Friuli Venezia Giulia, 34148
Italy

ABSTRACT

This work details the failure analysis of a super duplex valve (UNS J93404) (1) ASME (2) class 1500,
operating in treated sea waters with high chloride content below 80°C. A detailed analysis of the
microstructure, fracture surfaces and mechanical properties was combined with studies of corrosion
resistance of different regions by means of immersion tests (ASTM G48) (3)33, electrochemical analysis
and polarization tests (large scale and with a micro-cell). Selection of base material was performed
according to Table A.24 of NACE MR0175/ISO 15156-3 (4).

The cast material presents a segregated microstructure containing ferritic phases with different pitting
resistance equivalent number (PREN); this strongly affects the corrosion properties of the material,
enhancing the susceptibility to localized corrosion and leading to a Stress Corrosion Cracking (SCC)
mechanism.

Keywords: Duplex, pitting corrosion, stress corrosion, polarization, SEM, AFM, NACE MR0175/ISO
15156-3.

INTRODUCTION

The super duplex stainless steels exhibit high corrosion resistance as compared to other steels, in
particular at temperatures up to 250°C1. Due to that, super duplex steels are widely used in many
applications, especially in the energy production field, where good resistance to both general corrosion
and stress corrosion is required1. These materials possess their best performances when the
microstructure is composed of austenite and ferrite obtained by means of a solution heat treatment1-2.
The solution heat treatment temperature is chosen in order to obtain an almost equal distribution of ferrite

(1)
Unified Numbering System for Metals and Alloys (UNS). UNS numbers are listed in Metals & Alloys in the Unified Numbering System, 10th ed.
(Warrendale, PA: SAE International and West Conshohocken, PA: ASTM International, 2004).
(2)
The American Society of Mechanical Engineers, Two Park Avenue, New York, NY 10016-5990
(3)
ASTM International, 100 Barr Harbor Dr., West Conshohocken, PA 19428-2959.
(4)
NACE International, 15835 Park Ten Place, Houston, Texas 77084
and austenite2-3. The duplex microstructure is ensured by the distribution of alpha and gamma stabilizing
elements in ferrite and austenite phases4, respectively. If the solution heat treatment temperature
exceeds the equalization temperature, the material possesses excess ferrite. This can induce a different
distribution of ferrite and austenite stabilizing elements in each phase, leading to local variations of the
PREN number possibly affecting the corrosion properties at the phase with lower PREN4-8. Corrosion
properties could become further degraded if sigma phase or Cr nitrides are formed during thermal
treatments2-3,9. Corrosion is strongly affected by the severity of the environment (in particular Cl- and
sulfur content)6,8-10,12-13 and the service temperature7,10-11.

The literature concerning cast super duplex stainless steels is scarce, mainly comparing the corrosion
behavior of cast and forged materials or focusing on the effect of N additions on microstructure of cast
products14-16. Stress corrosion cracking (SCC) resistance of super duplex stainless steels is well known
in different environments17-22. In particular, the ferrite represents the weakest link with regards to SCC17.
Moreover, it was shown that sour environments could enhance the risk of SCC in the temperature range
of 60-80°C19.

The valve analyzed in this work has been installed in an environment where its corrosion resistance
should not be lowered, if the microstructural requirements are fulfilled. This resulted in an unexpected
failure of the valve analyzed in this study, which was installed in the water treatment line controlling the
flow of plant. The valve underwent failure after an exposure of only 2 years at a maximum operating
temperature of 80°C in the cooling water with composition reported in Table 1. As it can be seen, the
chloride content of the cooling water is 130000 ppm and H2S is present in traces. The pH of the cooling
water was pH 5. These service conditions usually are not so critical to cause the SCC failure of the super-
duplex stainless steel with a 1500 ASME class (12 in diameter). The valve leaked and needed to be
replaced. Thus, the service time of the valve was significantly shorter than the expected service life even
though it met ASTM G48 method A at 40°C for 24h requirements of the customer (no pits and negligible
weight loss) for the specific application. To understand the failure mechanism of the valve, this work
employs high resolution surface characterization techniques and electrochemical methods to highlight
the effect of the different regions of the weld on susceptibility to localized corrosion (pitting) and stress
corrosion cracking.

Table 1
Chemical composition and pH of the water inside the valve

EXPERIMENTAL PROCEDURE

Sample extraction and visual inspection

Before the samples were extracted, the valve was carefully inspected in order to identify the regions to
be analyzed. The valve was then sectioned, using a mechanical powered saw, in order to extract the part
showing leakage (Figure 1a). As it can be better seen in Figure 1b, showing the inside of the valve, the
crack runs in the cast body near and along the root of a weld bead. A forged plate of super duplex
stainless steel was welded by gas tungsten arc welding (GTAW) to the main body of the valve, obtained
by casting, in order to produce the guide for the gate. The chemical compositions of the two components
as well as of the weld bead are shown in Table 2. It is also possible to note from Figure 1b that only one
side of the welded joint was cracked.
A cross section of the welded joint containing the crack was extracted as indicated in Figure 1b.
The portion of material extracted from the valve (Figure 1c) was used to prepare the samples for various
analyses. In particular, the samples for both microstructural characterization and fracture surface
observation were collected in the region highlighted by the black square in Figure 1c. The specimens for
the corrosion testing were extracted in the regions highlighted by white circles (potentiodynamic tests)
and white squares (ASTM G48 tests) in Figure 1c.

Figure 1: a) External view of the valve at the failed area. b) Image of the internal wall of the valve
and of the macro-samples extracted. c) Image of the section of the valve used for
microstructural investigations (black square) and corrosion tests (white squares and circles).
 Table 2
Chemical composition of each component of the weld joint wt% balanced to Fe

Specimens obtained at the black square of Figure 1c have been polished on the main surface section
including cast, forged and weld areas. After surface preparation, the microstructure has been investigated
by light microscope (Olympus GX 41 microscope) after metallographic etching (Murakami reagent 10g
NaOH+10g K4(Fe(CN)6) in 100 ml deionized water heated at 90°C for 5 min). The austenite/ferrite
content has been analyzed by means of image analysis using ImageJ software, according to ASTM E562
standard32. In order to detect the phase partitioning with high resolution all the images acquired by light
microscope have been transformed in black and white. Portion of the specimens obtained at the black
square of Figure 1c was also used for scanning electron microscopy (SEM - Zeiss Evo 40+ Oxford Inca
probe) observation and energy dispersive x-ray spectroscopy (EDXS) on the internal wall of the valve.

In addition, the same specimen was also used for fracture surface analysis. This specimen was cleaned
in an ultrasound bath in order to remove the smut and contamination from fracture surface. The fracture
surface has been examined near the internal wall of the valve (probable region of crack nucleation) and
at an internal point of the fracture surface (crack propagation region).

Corrosion tests have been performed in order to evaluate the corrosion behavior of the different
components of the valve, namely cast and forged stainless steels. The immersion test according to ASTM
G48 method A standard has been performed for 24h. Samples in the shape of cubes of 20x10x20 mm
have been extracted from cast and forged material as shown in Figure 1c.

Potentiodynamic polarization curves have been carried out in a 5wt% of NaCl solution using polished
samples (up to P500 abrasive paper) cast and forged (up to P500 abrasive paper) cast and forged (see
Figure 1c). Polarization curves have been obtained at two different temperatures (25°C and 60°C). A
three-electrode electrochemical cell was employed with Ag/AgCl reference electrode and a Pt wire as
counter electrode. A potential scan rate of 0.2mV/sec was used starting at -0.15V below open circuit
potential (OCP) up to +1.4 V. The corrosion morphologies after the potentiodynamic tests have then been
analyzed by SEM+EDXS. In order to determine the Volta potential of the phases composing the cast and
forged materials the scanning kelvin probe force microscope (SKPFM) was employed on small size
samples extracted from each component of the weld joint (size 5x5x2 mm). The instrument used in this
experience is a Veeco nanoscope III multimode AFM † equipped with an extender TM electronic module.
The tests have been performed using a commercially available tip n+silicon nitride coated with PtIr5. The
scan height in the lift mode was 100nm. Topography and Volta potential were sampled with a pixel density
of 256x256 and a scan frequency of 0.1Hz. The mapped area is 100x100μm. The area of analyses has
been delimitated by 4 microidentations at a distance of 0.2mm each. On the basis of SKPFM results, the
samples were analyzed by SEM+EDXS in order to determine the semi-quantitative chemical composition
of the phases with different Volta potential. The local PREN for each phase, as well as the Creq and Nieq2,
were calculated from EDXS spectra according to the procedure employed in many scientific publications4-
5,7-8
. The N content on each phase (austenite/ferrite) that could not be precisely calculated by means of

†
Trade name
EDXS analysis, was valuated considering the ferrite phase saturated with N (max 0,05wt% N in ferrite)
and the remaining N distributed in austenite. Moreover, the phase distribution calculated by image
analysis (see previous paragraph) was taken into account for the N partition in the different phases.

RESULTS

Visual Inspection

The valve, as shown in Figure 1a, suffered leakage of the cooling water with very high Cl- content from
a vertical crack that appeared after one year of service life. The internal view of the valve (Figure 1b)
showed that the crack propagated along a forged plate welded to the cast valve body. This plate was
installed in order to produce a guide for the gate used to reduce the flow in the water treatment line. The
crack developed only in the cast material and not in the weld or in the forged plate, although both have
similar chemical composition as shown in Table 2. Examining the crack morphology (Figure 1c), it is
possible to notice that the crack is almost not branched. Moreover, it seems to be more opened at the
internal wall of the valve suggesting that crack nucleation occurred at this side.

The weld joint microstructures are shown in Figure 2, together with the delta ferrite volumetric content
acquired by image analyses. All the analyzed areas present a typical duplex microstructure composed
by austenite (white) and ferrite (dark). No deleterious phases (sigma, chi, carbides or nitrides) were
detected in each component of the weld joint, as well as in the HAZ. The cast material has coarser grains
than the forged one while in the weld bead phases have an acicular shape. In particular, in the weld bead
it is possible to observe the presence of columnar grains of ferrite surrounded by Widmanstaetten
austenite. The austenite is present also inside the ferritic columns as small clusters. The delta ferrite
content acquired by means of image analysis according to ASTM E562 standard is in both weld bead
and cast material about 60 vol% and 50% in the forged material. The heat affected zone (HAZ) is
composed by a thin ferritic strip (0.1- 0.2mm) where some austenite clusters are present. The observed
microstructure is fully in agreement with literature data24,28.
 Figure 2: Microstructures of the weld joint components. The presented HAZ is only the one at
the cast side.

As shown in Figure 3 some pits very close to the only affecting the cast material were found. The area
surrounding the pits has been also corroded. As shown in the literature19,34 duplex stainless steels can
be more susceptible to localized attack when sulphide together with chlorides are present in the
aggressive media. As shown in Table 1 sulphates are certainly present in the technical water and
sulphides may also be possible. Therefore, it is likely that the presence of small amounts of sulphides
could favor the attack of the passive layer already thinned by the high amount of chlorides.

Figure 3: Top view of the valve internal wall close to the fracture initiation: a) specimen used for
the analysis, b) on surface. The white arrows indicate some of the pits. The EDXS area indicates
the area analyzed by EDXS.

The microstructural analysis of the cross section of a pit near the fracture surface of the sample used for
microstructural characterization (Figure 2) is shown in Figure 4. The ferritic phase was preferentially
dissolved with respect to the austenitic phase (Figure 4a). This is in agreement to literature data, where
the austenite behaves as cathode with respect to ferrite in not strongly acidic environments17,31,36,37.
Therefore, it is likely that the localized attack has nucleated and propagated mainly at the ferritic phase.
The pit morphology acquired by SEM (Figure 4b) showed the presence of a vermicular microstructure
composed by residuals of the austenitic phase not dissolved by the corrosive process.
 Figure 4: pits found very close to analyzed by light microscope a) and SEM b). The red arrows
indicate preferential dissolution of ferrite phase.

The observation of the surface fracture was then performed on the sample (Figure 5a) extracted in the
black square zone of Figure 1c. In Figure 5b, it is possible to observe the crack nucleation region located
at the internal wall of the valve. This region is characterized by a vermicular morphology quite similar to
the one observed in Figure 4b at pit nucleation. Also, in this case is evident that one phase has been
mainly dissolved, the observed fibers being the residuals of the austenitic phase. This fibrous part of the
fracture surface has a total depth of about 1-1.5 mm. From these observations it is possible to state that
the fracture cracks a pit.
The crack propagation region is composed of a quasi-cleavage fracture, probably produced by high strain
rates at which the material has been subjected during the crack propagation and suggesting the
mechanical component of the fracture. Some areas showing a differential dissolution of the two stainless
steel phases are also evident (white arrows in Figure 5c). Moreover, the fracture surface, in the
propagation region, is strongly oxidized and shows some deposits rich in Cl and S. These findings clearly
suggest that cracking occurred by combination of mechanical stress and corrosion attack. Some other
cracks developed perpendicular to the main fracture surface have been probably generated by hydrogen
assisted cracking (black arrows in Figure 5c).
 Figure 5: Surface fracture analysis: a) specimen used for the analysis, b) SEM analysis of the
crack nucleation region and c) SEM analysis of crack propagation region.

Summarizing, the origin of the failure derives from pitting attack due to the presence of an aggressive
environment (see Table 1). Nucleated pits acted as a local stress raiser for the cast material thus favoring
a stress corrosion cracking phenomenon. When the local stresses at the pit tip are higher strain rates
(cleavage); this mechanism is assisted by the corrosive process. The origin of the stresses could be
related to the complex shape of the cast material and to its thermal history. If fact it was heat treated and
quenched with high cooling rates in water. It is likely that this has produced thermal internal stresses
more than transformational one38. Because of the wall thickness and a low thermal conductivity that
enhanced the presence of residual stresses because of a differential thermal expansion between surface
and the core of the wall. It is likely that the crack nucleation site is the region of the cast material where
it has been reached the maximum internal stresses. These stresses are the addition of internal stresses
caused by the heat treatment and internal stresses caused by the welding process. The last stresses are
probably negligible compared to the heat treatment stresses.
In order to understand why the localized corrosion attack affected only the cast material and not the
forged one some more analyses were performed.
Corrosion tests and microstructural investigation

A preliminary corrosion test was conducted according to ASTM G48 standards. This test is widely used
to check the corrosion resistance of quality inspection after industrial production. The presence of pits
and the weight loss on small cubes of 1 cm3 immersed in 6wt% FeCl for 24 hours at room temperature,
40°C and 60°C. The images of sample surface after the immersion test according to ASTM G48 are
shown in Figure 6.

Figure 6: Stereoscope images of the surface of the samples after the immersion test for 24 h
according to ASTM G-48 A. The black arrow indicates the presence of a pit.

It is possible to observe that the forged material does not show any pits for all the tested temperatures
and the weight loss is almost negligible. A similar behavior is also shown by the cast material up to 40°C.
On the other hand, at 60°C the cast material presents a considerable weight loss together with the
presence of a high number of pits some of them with dimensions in the range of mm. These results
confirm the in-service behavior of the valve, namely the forged component has better corrosion resistance
with respect to the cast one, quite evident at temperatures in the range of 60°C. To confirm the previous
results potentiodynamic polarization were performed in 5wt% NaCl solution on both cast and forged
samples at room temperature and at 60°C, using the Avesta cell to prevent crevice corrosion during the
test. The results of these tests are shown in Figure 7.
 Figure 7: potentiodynamic polarization curves of cast and forged sample at room temperature
and 60°C.

The potentiodynamic tests at room temperature show that both a stable passive behavior with similar
passivity currents in the range of 10-7 A/cm2 for a wide potential range. At 60°C the two materials still
show a passive behavior although with higher passive currents (10-6 A/cm2) compared to room
temperature. Nevertheless, the cast stainless steel presents break down around +0.5V vs Ag/AgCl. For
this sample after the break down potential the current does not increase rapidly but step by step
highlighting good corrosion resistance as expected for a super duplex stainless steel. SEM analysis of
the corrosion morphology after potentiodynamic testing was then performed (Figure 8).
 Figure 8: corrosion morphologies after potentiodynamic at both room temperature and 60°C.
The arrows indicate the regions of deep localized corrosion of ferrite.

The SEM micrographs of the corroded area of the forged sample show homogeneous dissolution of ferrite
at room temperature becoming more intense at 60°C. The morphology of the cast shows a very small
preferential dissolution of the ferritic phase, but it is also clear that the dissolution of ferrite is not fully
homogenous at room temperature. As indicated by white arrows in Figure 8, the ferrite is locally corroded
preferentially close to the austenite boundary, with the formation of morphologies similar to ditches
surrounding most of the austenite grains. This phenomenon become even more intense at 60°C. These
features can be considered sites for preferential pitting nucleation and propagation as actually occurred
for this component in service life.

In order to try to better understand the causes for localized corrosion as observed in the cast material,
scanning kelvin probe force microscopy (SKPFM) has been used together with EDXS. The analysis area
has been marked by 4 microindentations in order to easily detect the area to be analyzed and observed.
The results obtained by SKPFM and EDXS on the same area are shown in Figure 11.

The austenite and the ferrite behave as cathode and anode respectively (Figure 9c and e). The
electrochemical potential is quite homogenous inside each phase and the potential difference ranges
around 0.2V. This result is perfectly in agreement with the corrosion morphologies observed in Figure 8
for the forged material showing the preferential dissolution of ferrite.

The presence of the two phases is also clear in the SEM micrograph of Figure 9b for the cast material
and also in this case the austenite and the ferrite seem to behave as cathode and anode respectively
(Figure 9d and f). Nevertheless, a gradient of the electrochemical potential which, in its bulk, is similar to
the one of the austenitic phase becoming more anodic close to the austenite boundary. Therefore, only
the ferritic phase that closes the border is the potential anode of a galvanic couple with austenite. Also,
this finding is perfectly in agreement with the corrosion morphologies shown in Figure 8 for the cast
material showing an almost homogeneous corrosion of both phases apart from the ferritic area close to
the austenite suffering a deep localized attack. The EDXS analyses on forged material (Figure 9 a) and
Table 5) show the enrichment of alpha stabilizers in the ferritic phase (Cr, Mo) and austenite stabilizers
in the gamma phase (Ni, Mn and N). This is in agreement with several works that showed a very similar
PREN in the case of a balanced distribution of the two phases5,7. Moreover, a decrease of corrosion
resistance is observed if the PREN is not uniform. The more anodic ferrite in the cast material (Figure
9b) and Table 5) exhibits a reduction of Cr and, mostly, Mo content as compared to the less anodic ferrite.
This was associated to a higher PREN for the phase presenting less anodic behaviour. This behavior
could be linked to the segregation of ferrite stabilizing elements during the solidification of the material,
that has not been modified by the solution heat treatment. These results suggest that the corrosion
resistance of each phase is strongly influenced by the elemental distribution determining the PREN. The
localized corrosion has also been enhanced by the area distribution of these ferrites with lower PREN
since these present a small anodic area compared to both the less anodic ferrite and the austenite
(cathode). In this case, the cathodic/anodic area ratio is very high and stimulates the localized corrosion
process.

Figure 9: SEM+SKPFM analysis on forged and cast material. a) SEM+EDXS analyses on forged
material, b) SEM+EDXS analyses on cast material, c) SKPFM map of forged material, d) SKPFM
map of cast material, e) line section of Figure 9 b), f) line section of Figure 7d).
 CONCLUSIONS

A super duplex valve used in a water treatment line in an oil and gas power plant failed after a few months
of service life because of SCC in the cast main body of the valve. The stress corrosion crack nucleated
at the base of pits acting as a local stress riser. The stresses responsible of the failure are mainly linked
to the heat treatment of the valve.

The high chloride concentration together with the presence of sulphur compounds and a relatively high
temperature (up to 80°C) were responsible for pit nucleation but only in the cast stainless steel. Corrosion
as well as electrochemical tests showed that the cast stainless steel valve is much more prone to pitting
corrosion at 60°C.

SKPFM showed that the austenite and the ferrite phases present in the super duplex microstructure
behave as cathode and anode respectively. Nevertheless, the ferritic phase of the cast sample shows a
gradient in the electrochemical potential which, in its bulk, is similar to the one of the austenitic phase
becoming more anodic close to the austenite boundary. Therefore, only the ferritic phase close to the
border is the potential anode of a galvanic couple with austenite, thus suffering intense localized attack
favoring pit nucleation.

The ferritic phase in the cast material showed variable electrochemical behavior because of elemental
segregation during solidification. The segregation was caused by a non-uniform distribution of Cr and Mo
inside the ferritic phase leading to the formation of regions close to the austenite boundary with lower
PREN compared to the rest of the material.

ACKNOWLEDGEMENTS

The authors are grateful to Friuli Innovazione, in particular to Eng A. Lanzutti, for the technical support.

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