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Corrosion Science 46 (2004) 12391264

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Pit to crack transition in stress corrosion


cracking of a steam turbine disc steel
A. Turnbull *, S. Zhou
Materials Centre, National Physical Laboratory, Queens Road, Teddington,
Middlesex TW11 0LW, UK
Received 16 June 2003; accepted 8 September 2003

Abstract
Long term exposure tests have been carried out on a 3 NiCrMoV steam turbine disc steel in
the form of cylindrical tensile test specimens self-loaded to 90% of r0:2 and exposed to three
environmental conditions, viz. deaerated pure water, aerated pure water, and aerated water
containing 1.5 ppm of chloride ion. Pitting occurred in all environments but the density and
depth of pits in the chloride-containing medium was markedly greater. No cracking was
observed in deaerated pure water but cracks initiated in aerated water between 13 and 19
months and in less than 7 months in aerated 1.5 ppm Cl solution. The probability of a crack
initiating from a pit of specic depth in aerated solution could be described well by a Weibull
function. Proling of pits and cracks in the disc steel tested in aerated 1.5 ppm Cl solution
showed that there while there were many cracks with a depth greater than that of the corresponding pit the depth of some cracks was smaller than that of the corresponding pit,
suggesting that cracks do not necessarily initiate from the bottom of the pits. The growth rate
of short cracks emerging from pits appeared greater than that of long cracks in fracture
mechanics specimens.
 2003 Published by Elsevier Ltd.
Keywords: A. Steel; C. Stress corrosion; Pitting corrosion

1. Introduction
Stress corrosion cracking of steam turbine steels continues to be an area of concern
for the power industry. Although failures are rare, compared with that of boiler tubes
for example, the potential consequences in terms of system damage are severe. Stress
*

Corresponding author. Tel.: +44-20-8943-7115; fax: +44-20-8614-0436.


E-mail address: alan.turnbull@npl.co.uk (A. Turnbull).

0010-938X/$ - see front matter  2003 Published by Elsevier Ltd.


doi:10.1016/j.corsci.2003.09.017

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corrosion cracking of steam turbine disc steel most commonly originates from corrosion pits, except perhaps at high stresses for which the role of pits may be less
signicant (because there is strain localisation to disrupt the surface lm and there is
no need for stress concentration). When pitting is the precursor to stress corrosion
cracking, the fundamental steps in the overall process of crack development include:
pit initiation; pit growth; transition from pit to crack; short crack growth; long crack
growth. Whilst there are considerable data for the growth rate of long cracks in
various simulated environments [1], there is comparatively little information on the
growth rate of pits and the early stages of crack growth. Key external factors aecting
pit initiation and growth include oxygen concentration, chloride concentration, nature and concentration of other anions, temperature and dynamic strain. Inclusion
density, size and distribution would be key material parameters.
As part of a larger programme designed to provide a framework for predicting the
stress corrosion cracking of turbine disc steels, long-term exposure tests have been
conducted to investigate the evolution of pits and cracks on self-loaded tensile
specimens under conditions nominally expected to represent service exposure in a
conventional coal-red power station. Typically, on-load, a thin liquid lm will form
from the steam at temperatures below about 90 C. Recent evaluation [1] suggests
that the liquid lm will contain up to about 300 ppb chloride ion under normal
operating conditions with well-controlled water chemistry, with perhaps up to 1.5
ppm chloride if the chloride in the inlet steam is not controlled tightly. On-load, the
oxygen concentration of the liquid lm will be negligible. O-load, the liquid lm on
the discs will usually be aerated, unless there is nitrogen blanketing, and at a temperature of 70 C, but the chloride ion concentration will be very low. During startup, the chemistry is less well understood but a transient combination of oxygen in
solution with some chloride is possible.

2. Experimental
2.1. Material
The material used in this work was a disc steel (3 NiCrMoV), cut from an exservice steam turbine disc supplied by PowerGen. The chemical composition is listed
in Table 1.
2.2. Specimens
Self-loaded cylindrical specimens of the disc steel were manufactured according to
ASTM E8 [2] with the longitudinal axis perpendicular to the radius of the turbine
Table 1
Chemical composition of the 3 NiCrMoV disc steel (mass %)
C
0.30

Si
0.28

Mn
0.45

P
0.017

S
0.013

Cr
0.69

Mo
0.27

Ni
2.89

V
0.091

N
0.21

Fe
bal

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Fig. 1. Photograph of the specimen and the loading frame for pitting and SCC tests.

disc. The overall length was 100.0 mm, the shoulder diameter 16.0 mm, the gauge
length 25.4 mm and the diameter 6.4 mm. The specimen and the loading frame are
shown in Fig. 1.
To avoid galvanic corrosion, the loading frames and the nuts were also made of
the disc steel. The specimen surface was dry ground using P2400 grinding paper
(1200 SiC grit nish). The surface prole [3] was measured using a laser prolometer.
Measurements were made at eighteen locations on two specimens. The length of
prole for each individual measurement was 2 mm. The arithmetical mean deviation
of the assessed prole, Ra , was 0.50 0.28 lm. The corresponding maximum height
of the prole, Rz , was 3.13 0.91 lm. The nal grinding direction, and hence any
grinding marks, were parallel to the length of the specimen.
2.3. Stress relief
To avoid an uncontrolled inuence of residual stress resulting from machining or
from grinding, all specimens, after nal grinding, were stress-relieved in vacuum for
2 h at 625 C. The mechanical properties at ambient temperature and at the test
temperature are listed in Table 2. The data were the average of three tests under each
condition.
It can be seen that the stress relief had no eect on the mechanical properties.
Since the specimens were cut from an ex-service disc, there was a concern that the
Table 2
Mechanical properties of the disc steel (mass %)
Condition

T (C)

E (GPa)

r0:2 (MPa)

UTS (MPa)

Elongation (%)

As received
Stress relieved
Stress relieved

23
23
90

208 2
206 1
210 4

747 9
734 4
705 4

882 5
870 2
827 13

23 1
20 0
20 0

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Fig. 2. Microstructure of 3% NiCrMoV disc steel.

mechanical properties may vary at the dierent locations of the disc. Therefore, the
hardness of the steel was measured on ten randomly selected specimens. There was
no signicant variation in the hardness measured; the average value being 28.5
(Rockwell C), with a standard deviation of 1.5. The microstructure of the materials
after stress relief is shown in Fig. 2. The mean grain size was 26 8 lm.
2.4. Pre-pitting
Some of the cylindrical specimens were pre-pitted to produce single pits, or occasionally a few pits using the procedure developed at NPL [4]. The anticipation was
that the single pits would grow preferentially and the cracks might initiate readily at
these locations. Should this be the case then crack measurement probes could then be
located accordingly in future tests. The use of pre-pits also might be expected to give
insight as to the subsequent likely growth rate of pits should their initiation and early
development be accelerated by a water chemistry excursion.
The pre-pitting procedure established for cylindrical tensile specimens of 3%
NiCrMoV disc steel is summarised as follows. A solution of 0.02 M Na2 B4 O7 + 0.01
M NaCl (pH 9.2) was used. The test temperature was 23 1 C. A test cell with a
ushed-port seal adapted for cylindrical specimens was used to prevent crevice
corrosion at the seals between the cell and the specimen. After the specimen was
immersed in the test solution for 1 h, a constant anodic current of 10 lA was applied
to the exposed area of approximately 9.6 cm2 . This tends to lead to development of a
single dominant pit. To minimise corrosion on the periphery of the pit, the solution
was gently stirred but the stirring was applied only after the pit had just initiated as
indicated by the decrease in potential. If the applied current were increased to 20 lA,
more than one pit (usually less than 5) was produced on the specimen surface.

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2.5. Test environment


The environments used for the pitting and SCC tests are listed in Table 3.
2.6. Water supply/circulation systems
2.6.1. Deaerated high purity water at 90 C
The quality of the deaerated high purity water was maintained by using a oncethrough system, as shown schematically in Fig. 3.
The deaeration was achieved initially by continually passing nitrogen into a 20litre reservoir containing the feed-in deionised water. Further water purication and
Table 3
The environments and test temperatures for pitting and SCC testsa
Environment

Conductivity
(lS cm1 )

pH

Test temperature (C)

Simulation

Deaerated high
purity water

0.056

Assume
neutral

90

Liquid lm chemistry with


high steam wetness/high
purity

Aerated high
purity water

1.1

5.8

90

Liquid lm chemistry
during start-up/air leak

Aerated water
+ 1.5 ppm Cl

6.8

5.9

90

Liquid lm chemistry
during major system upset.

a
Prior to the detailed review and analysis of Ref. [1] there was an indication in several papers on stress
corrosion cracking that on-load conditions were best represented by laboratory tests in high purity water.
This was the basis for this environment when initiating these long-term tests. It is now realised that 300
ppb Cl is likely in the liquid lm whilst on-load.

Fig. 3. Schematic diagram showing the test cell and high purity water supply system.

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deaeration were achieved and maintained by continually circulating the feed-in deaerated deionised water in a loop containing a second deionising cartridge (purier)
and three de-gasser cylinders. The main component of the de-gasser is a membrane
that allows only the gas (oxygen) to pass through (Fig. 3). The conductivity and
oxygen level of the inlet and outlet water were monitored using on-line probes. The
low conductivity and oxygen level were achieved using a once-through water ow
system in which the water ows from the above circulation line to the test vessels and
then to drainage. The ow rate was approximately 15 ml/min and hence the water in
the 1 l test cell was replenished about once an hour. The slow rate of input of solution into the test cell allowed the temperature to be maintained within 1 C
without the need for a pre-heater.
2.6.2. Aerated high purity water at 90 C
A once-through system, similar to that shown in Fig. 3, was also used for tests in
aerated high purity water but in this case the inlet water was aerated using an air
pump. The ow rate was also approximately 15 ml/min.
2.6.3. Aerated water containing 1.5 ppm Cl at 90 C
The solution circulation loop for aerated water containing 1.5 ppm Cl was
slightly dierent from that in Fig. 3. In this case the aerated feed-in solution was recirculated from a 40-l reservoir, again at a ow rate of approximately 15 ml/min. The
solution in the 40-l reservoir was refreshed every week and the conductivity and pH
were measured before and after the solution change.
2.7. Corrosion potential measurement
The corrosion potential was measured using an external 0.01 N Ag/AgCl reference electrode designed specially with an extremely low chloride diusion rate. The
reference electrode was connected to the test cell through a glass bridge lled with the
test solution. The reference electrode chamber and the test cell were separated with a
glass valve, which was closed except when a measurement was taken. The solution
conductivity was monitored to ensure that there was no signicant chloride contamination due to the diusion of chloride from the reference electrode chamber to
the test cell during the potential measurement. For the potential measurement in
deaerated high purity water, the reference electrode chamber was sealed. The reference electrode remained at ambient temperature. All potentials quoted are with
reference to the saturated calomel electrode (SCE) at 25 C.
2.8. Test procedure
35 self-loaded cylindrical tensile specimens of disc steel were used; 16 of the
specimens were smooth (without pre-pitting), seven specimens had a single pre-pit
and 12 specimens had multiple pre-pits. The depth and the surface width of the pit
(the mouth of the pit was not always ideally circular) were measured using a travelling microscope (resolution 1 lm). In the latter case, the maximum width in one

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direction was measured and the width perpendicular to this was measured also. The
average value was used later in calculating the aspect ratio. The location of the prepits was mapped out before testing so that the surface of the tested specimen could
subsequently be examined to determine the growth characteristics of the pre-pits.
All specimens were loaded to 634.5 MPa, i.e. 90% of the 0.2% proof stress (r0:2 ) at
the test temperature (90 C). In order to prevent possible stress relaxation as the
specimen and the loading frame were heated to the test temperature, all specimens
were loaded at 90 1 C with the specimen and the loading frame placed in a
temperature-controlled oven. The loaded specimens were then cooled down and
stored in a dessicator for at least 24 h before being placed in the test cell. For each
environment, the specimens were distributed in two or three dierent test cells of 1 l
capacity so that specimens could be removed and examined at dierent test intervals
without aecting the remaining specimens. After placing the specimens in the cells,
the test solution was introduced and the test temperature increased gradually to 90
C in about three hours. For deaerated high purity water, the test cells were purged
with nitrogen for 4 h before the solution was introduced.
The temperature was controlled at 90 1 C and recorded hourly.
2.9. Water chemistry control
The conductivity, oxygen level and pH were measured throughout the tests at
weekly intervals and the results are summarised in Table 4. In the case of the recirculated chloride solution, the pH and conductivity were measured immediately
after refreshment (new solution) and after testing for 7 days, just prior to refreshment (old solution).
Table 4 indicates that the conductivity of the inlet deaerated high purity water is
almost the same as the calculated value of pure water (0.055 lS/cm) [5]. The conductivity of the outlet deaerated high purity water is much higher but this is mainly
due to the fact that it is measured at 50 C (the conductivity of pure water at 50 C is
Table 4
Control of environmental conditions (all data were obtained at ambient temperature 23 1 C, unless
stated otherwise)
Environments

Deaerated
high purity
water
Aerated high
purity water
Aerated
water + 1.5
ppm Cl

Test
temperature
(C)

Solution into cell

Solution out of cell

Conductivity
(lS/cm)

O2
(ppm)

pH

Conductivity
(lS/cm)

O2
(ppm)

pH

90

0.056

<0.0001

nma

0.34b

<0.001b

nma

90

1.1

nma

5.8

1.2

4.4b

5.8

90

6.8c

nma

5.9c

8.0d

2.8b

6.3d

Note: (a) nm: not measured; (b) measured at 50 C; (c) new solution; (d) old solution.

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about 0.2 lS/cm) [5]. The oxygen content in the deaerated pure water was controlled
at less than 1 ppb, except during one excursion in one corrosion cell.
The measured conductivity of the aerated pure water of about 1 lS/cm reects the
eect of dissociation of dissolved carbon dioxide. There was only very modest
change in the pH and conductivity of the outlet aerated high purity water and
chloride-containing solution compared to that of the inlet, highlighting the eectiveness of the water chemistry control. It should be noted that the oxygen concentration of the aerated water and of the 1.5 ppm Cl solution was measured at the
outlet at a lower temperature (50 C) than the test temperature. Nevertheless, the
oxygen concentration in the test cell at 90 C can be assumed to be the equilibrium
value (1.4 ppm at 90 C), since air bubbling was continuous in the reservoir solution.
A concern for long-term tests using glass reaction vessels is the inhibiting eect on
corrosion of dissolved silica-containing species from the glass [6,7]. To minimise this,
all glassware was pre-exposed to water at 90 C for a month, as previous work [7]
had shown that using boro-silicate glass treated in this way for corrosion tests gave
equivalent results to a quartz glass vessel in terms of dissolved silica and corrosion
rate. The impact of dissolved silica is not a problem for tests in deaerated and aerated water, as the water was continuously refreshed at a rate of approximately 1 l/h.
To ensure that the accumulated silica level in the test cell was not high with the recirculated aerated 1.5 ppm Cl solution, the silica content in the new solution and
the old solution (before being refreshed after one week of testing) was analysed
using Inductively Coupled Plasma Atomic Emission Spectroscopy (ICP-AES) and
Graphite Furnace Atomic Absorption Spectroscopy (GF-AAS). The silicon content
was less than 200 ppb for the fresh solution and 700 200 ppb for the old solution.
Previous work at NPL has demonstrated that silica species at these levels do not
aect the corrosion rate of mild steel in distilled water [7].

3. Results and discussion


3.1. Eect of oxygen and chloride ion on the corrosion potential
The corrosion potential of all specimens was measured. There was little variation
for the same type of specimens in the same cell, with the spread being less than
0.05 V.
Typical corrosion potentials in each cell are shown in Fig. 4. These corrosion
potentials reect not only the specimen but also the self-loading frame, which is of
the same material.
The corrosion potential of the disc steel in deaerated high purity water stabilised
relatively quickly, at approximately )0.60 V(SCE). From other observations [8] in
which relatively low potentials (<)0.70 V(SCE)) were achieved for a short period it is
apparent that the more noble potential reects build-up of corrosion product on the
specimen surface.
In aerated pure water, the potential rose in a few days to quite noble values,
eventually uctuating in the range +0.05 V(SCE) to +0.10 V(SCE). When chloride

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Fig. 4. Variation of the corrosion potential with time for self-loaded disc specimens.

was present in the aerated solution, the corrosion potential increased more slowly
and attained a lower potential than the chloride-free environment. It was noted in a
similar test that movement of the specimen caused the potential to drop instantly.
This transient disturbance of the potential to a lower value suggest that the lm is
not a coherent passive lm but at least partially comprises a loosely adherent corrosion product, providing a transport barrier to metal dissolution.
The slow gradual increase of the corrosion potential over a long period of time in
the chloride solution has implications for testing, as the electrochemical driving force
will be changing with time. This may have an inuence on crack initiation, which is
likely to be potential dependent, and possibly also on the propagation rate in the
short crack regime.
As indicated below, all the specimens had pitted, in the case of the chloridecontaining solution, very extensively. In deaerated pure water, the pit development
process is likely to be controlled solely by internal reactions, due to the absence of a
signicant external cathodic reactant and because of the very low solution conductivity. The pits may then be growing at the free corrosion potential in the pit solution, with an internal cathodic reaction of water reduction or reduction of sulphide
species from MnS inclusion dissolution. It would be expected that the potential in
the pit would be low, with very large gradients in potential at the pit mouth, but not
reected in the measurement of potential remotely. For aerated chloride-free water,
the conductivity will be higher due to dissociation products of dissolved CO2 . Hence
some inuence of the bulk oxygen on pit growth kinetics is anticipated but with the
inuence diminishing as the pit depth increases.
3.2. Stress reduction due to specimen relaxation
On completion of the tests, the specimens were removed from the solutions approximately 1 h after the heater was switched o; when the solution temperature had

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decreased to below 50 C. The specimens with their loading frames were washed
immediately with high purity water, ethanol and acetone. Unloading was then undertaken on a mechanical test machine. The reduced stress, resulting from specimen
relaxation, was estimated from the value of the load at which the nut of the loading
frame could be readily unscrewed. For the deaerated and aerated chloride-free water
some measurements indicated a decrease to about 80% of the proof stress (from
90%) whilst others showed no reduction, despite longer exposures. This variation
could be correlated with the particular experimentalist so it is dicult to be unequivocal. However, it is likely that the decrease is relatively small. For the aerated
1.5 ppm Cl solution, it was less ambiguous; the nal stress decreased with test
duration and at the longest exposure (9187 h) the nal stress was about 71% of the
proof stress. In this case, the formation of multiple pits and cracks (see below) would
be a factor as the change in average cross-section was only 1%. However, the relaxation in the chloride-free environments, with much reduced pitting and cracking,
suggests that creep must be a factor.
3.3. Visual examination of the specimen surface
After unloading, the specimen surface was carefully examined and photographed
before and after chemical cleaning using Super Clarkes solution (10 g/l of 1,3-Din-butyl-2-thiourea (DBT) in 37.5% HCl). It had been established previously that this
cleaning solution has negligible eect on the general corrosion of the bare disc steel
and that there was no measurable change in the size of pits during the cleaning
processes (the measurement resolution of the pit dimension was 1 lm). In the deaerated pure water, a shiny black lm had formed on the specimen surface and pits
were readily visible after chemical cleaning. In aerated pure water a brownish lm
was apparent on the surface and pits were readily visible. Also, there was evidence of
crevice attack in the contact area between the specimen and the loading frame. In
aerated 1.5 ppm Cl solution, severe general corrosion was evident with a thick
reddish-brown corrosion product covering the surface. Large pits and multiple
cracks could be discerned. In some cases, the tips of cracks from adjacent pits had
turned towards each other and many cracks had coalesced, as shown in Fig. 5.
3.4. Distribution of the surface widths and depths of pits
The surface width (w) and depth (a) of pits in the gauge section were measured
using the same procedure as described earlier for pre-pits. Only pits of depth greater
than 25 lm were recorded. Measurement of the number of pits of a depth below this
value was carried out but was very uncertain and highly subjective because of the
diculty of distinguishing very shallow pits from general surface roughening. In
view of the possibility of distorting the pit density distribution, such data were neglected. The value of 25 lm was chosen based on condence in the measurement
procedure. Since the primary interest was in the evolution of pits to cracks, very
small pits depths were less relevant and their measurement added to the measurement burden unnecessarily. Nevertheless, it should be noted that the density of the

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Fig. 5. Surface appearance of a self-loaded tensile specimen tested in aerated 1.5 ppm Cl solution at
90 C for 5107 h.

shallow pits with a depth less than 25 lm was high, usually greater than 25 cm2 . It
might be expected that the density of pits with a depth greater than 25 lm would
increase signicantly with time if all these pits kept growing. This proved not to be
the case (see below), suggesting that the majority of these pits are non-propagating.
The measurement of both the width and depth of pits was made only on selected
specimens.
Examples of the results for the three environmental exposure conditions in terms
of the variation of aspect ratio with pit depth are shown in Figs. 68.

Fig. 6. Aspect ratio of pits as a function of pit depth in the self-loaded specimens in deaerated pure water
at 90 C for 8322 h (no cracks initiated from pits).

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Fig. 7. Aspect ratio of pits as a function of pit depth in the self-loaded specimens tested in aerated pure
water at 90 C for 9138 h (no cracks initiated from pits).

Fig. 8. Aspect ratio of pits as a function of pit depth on the self-loaded specimens tested in aerated 1.5
ppm Cl solution at 90 C for 9187 h.

For comparison of the three exposure conditions, the results for the longest duration only are shown here. The number of pits in these three gures does not reect
the pit density, as the number of specimens was not the same in all cases. For example, because of the very high density of pits in the chloride-containing solution,
the results for only one specimen are shown. Nevertheless, the data for other specimens are reported elsewhere [9] and these conrm the representative nature of this
particular dataset.

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In deaerated pure water the exposure period was 8322 h rather than about 9000 h
because of a system failure near the end of the test, so comparison with the other test
conditions is not ideal.
The comparison of the variation of the aspect ratio (note a value of 0.5 would be
expected for a hemispherical pit) with pit depth shows that for the chloride-free
environments, the aspect ratio increases with pit depth much more signicantly than
for the chloride-containing pits. In the latter case, it is only when the pit depth exceeds the range 200250 lm that the mean aspect ratio exceeds 0.5. In chloride-free
environments, the corresponding depth is of the order of 75 lm. In other words, the
pits in the chloride-free water tend to be sharper for the same depth, extending in
depth relative to opening much more than for the chloride-containing environment.
The broadening of the mouth of the chloride-containing pits may reect the greater
impact of the cathodic reaction externally and the more noble potential near the
mouth, relative to the pit base, allowing enhanced corrosion. Also, the pH at the pit
mouth might be expected to be lower for aerated solution as ferrous ions emerging
from the pit are oxidised to ferric ions, which hydrolyses more eectively [10]. This
would encourage dissolution near the mouth and associated broadening. The extent
of that pH fall will depend on the corrosion rate and this may explain the distinction
between the chloride-containing and chloride-free aerated water.
There is still a basic question as to why a pit once initiated in the deaerated
chloride-free water should grow faster at the base relative to the walls. If it were
simply a case of corrosion of a lm-free surface in a neutral to alkaline local environment with internal water reduction, in other words simply corroding at a low rate
in a lm-free condition with limited connection to the outside conditions, it would
be hard to explain. However, one possible factor is dissolution of MnS inclusions. In
that context, it may be envisaged that the tighter pit is favoured because it enhances
retention of the local chemistry associated with this inclusion dissolution.
3.5. Pit densitydepth relationship
The relationship between pit density and depth for the three exposure conditions
is shown in Figs. 911. To avoid confusion, not all data sets are included, but details
of maximum pit depths and average values are given in Tables 57.
In deaerated pure water (Fig. 9), the maximum pit depth after about 22 months
was just over 200 lm with a reasonable number of pits between 100 and 200 lm. The
increase in the density of pits greater than 25 lm with the increase in exposure time
was modest, less than 20%; the pits simply got deeper. Deductions from the data for
the aerated water are more challenging because of the unusual degree of variability
at dierent exposure times; e.g. the greater pit depths at 5107 h compared with 9138
h and the low density at 15,758 h. There was nothing in the record of the tests in
terms of conductivity (monitored weekly) or any other factor that could account
for such a variation. It could be related to the material characteristics but the
specimens were prepared from the same region of the disc. Despite this variability,
there is no doubt that the combination of oxygen and an increased conductivity (due
to dissociation of dissolved CO2 ) would seem sucient to give an increased driving

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Fig. 9. Distribution of pit depths on the self-loaded specimens tested in deaerated pure water at 90 C.

10

9138 hours
13528 hours

Pit density / cm-2

15758 hours

6
4
2
0
0

50

100

150

200 250
Pit depth / m

300

350

400

Fig. 10. Distribution of pit depths on the self-loaded specimens tested in aerated pure water at 90 C.

force for pit growth. Data are shown only up to 9187 h for the aerated chloride
solution as the test was terminated because of the high level of damage to the
specimens. The pit density was at least of a factor of two higher than for the chloridefree solution.
The observation of deep pits in chloride-free water is not conned to this study.
Similar observations had been made by Gabetta and Caretta [11]. However, David
et al. [12] and Speidel et al. [1315] reported no pitting in high purity water, aerated
or deaerated. The temperatures were similar to the present test. Also, David et al.
used a 25-year old conventionally smelted steel, suggesting that steel composition
does not provide a simple resolution of these dierent results.

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Fig. 11. Distribution of pit depths in the self-loaded specimens tested in aerated 1.5 ppm Cl solution at
90 C.

3.6. Pit growth rates


The key parameters from all the test specimens have been analysed and are also
summarised in Tables 57.
The evolution of pit depth (a) with time is often described by a relationship of the
form:
a atc

where a and c are system specic constants. The variability of the data for aerated
water does not allow a detailed assessment of the pit growth rates whilst those for the
deaerated solution were limited to two exposure times. Thus analysis is meaningful
only for the 1.5 ppm Cl solution and even here the absence of data at short times is
limiting. Nevertheless, using this relationship and tting to the data for the average
of the 10 deepest pits for each specimen gives values of c 0:38 and a 1:36  106
with t expressed in seconds and a in m.
With these parameters, pit growth rates were then estimated at each of the exposure times for the 1.5 ppm chloride solution and are included in Table 7. The
values of course are smaller than the average growth rates of the ten deepest pits,
which is to be expected as the latter incorporate the faster growth rates at shorter
times. The average values were calculated only for comparison with Tables 5 and 6
for which data were limited. On this basis, the chloride-containing environment
generated pit growth rates about 46 times faster than the chloride-free water. The
pit growth rate in the aerated water was not markedly higher than for the deaerated
pure water. The presence of oxygen in pure water might be expected to enhance
the initiation of pits, and thus should give a higher pit density, but because of the
very large potential drop in such high purity water, the growth rate could proceed
independent of conditions of the bulk as the depth increased and should be

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A. Turnbull, S. Zhou / Corrosion Science 46 (2004) 12391264

Table 5
Statistics of pits in disc steels in deaerated pure water at 90 C (the specimens were loaded nominally to
90% r0:2 )
Test time
(h)

Pit densitya
(cm2 )

Maximum pit
depth (lm)

Average depth of
10 deepest pits
(lm)

Average pit
growth rateb
(1012 ms1 )

8322

14.2
16.7
15.5

163
209
186

121
139
130

4.0
4.6
4.3

9979c

16.5

211

172

4.8

15,402

18.8

218

163

2.9

Results from various specimens are shown with the average value in bold. Data from a compact tension
(CT) test is also shown.
a
Sampling area: 6.0 cm2 .
b
Average pit growth rate of 10 deepest pits assuming that the pit initiation time is negligible and
dividing by the full exposure time.
c
Compact tension specimen in parallel test set-up.

Table 6
Statistics of pits in disc steels in aerated pure water at 90 C (the specimens were loaded nominally to 90%
of YS)
Test time
(h)

Pit densitya
(cm2 )

Maximum pit
depth (lm)

Average depth of 10
deepest pits (lm)

Average pit growth


rateb (1012 ms1 )

5107

12.2
5.2
2.3
6.6

194
261
209
221

157
180
155
164

8.5
9.8
8.6
9.0

9138

35.3
13.2
32.7
33.3
28.6

117
155
177
221
168

105
135
123
133
124

3.2
4.1
3.7
4.0
3.8

13,528

24.8
32.2
28.5

274
386
330

244
323
283.5

5.0
5.7
5.4

15,758

14.8

433

249

4.4

Results from various specimens are shown with the average value in bold.
a
Sampling area: 6.0 cm2 .
b
Average pit growth rate of 10 deepest pits assuming that the pit initiation time is negligible and
dividing by the full exposure time.

comparable to that for the deaerated solution. However, comparison of such average
pit growth rates can be misleading as Fig. 10 clearly indicates pit depths in aerated
water signicantly greater than those in deaerated water.

A. Turnbull, S. Zhou / Corrosion Science 46 (2004) 12391264

1255

Table 7
Statistics of pits in disc steels in aerated 1.5 ppm Cl at 90 C (the specimens were loaded nominally to 90%
of YS)
Test time
(h)

Pit densitya
(cm2 )

5107

47.1
46.7
54.0
65.4
53.3

7173

9187

Average depth
of 10 deepest
pits (lm)

Average pit
growth rateb
(1011 ms1 )

Pit growth
ratec
(1011 ms1 )

825
999
792
829
861

668
814
744
761
747

3.63
4.43
4.05
4.14
4.06

1.5

42.8
42.5
42.7

925
939
932

813
813
813

3.15
3.15
3.15

1.2

69.3
43.5
56.4

1024
1209
1117

902
970
936

2.73
2.93
2.83

1.0

Maximum pit
depth (lm)

Results from various specimens are shown with the average value in bold.
a
Sampling surface area: 6.0 cm2 .
b
Average pit growth rate of 10 deepest pits assuming that the pit initiation time is negligible and dividing by the full exposure time.
c
Pit growth rate calculated using Eq. (1) and based on average depth of 10 deepest pits for each
specimen.

3.7. Extension of pre-pits


Since multiple pits developed readily from the smooth specimens in all environments pre-pitting to achieve reasonable depths turned out not to be a necessary
requirement. Nevertheless, the nal depth of the pits that had evolved from pre-pits
was measured, and the maximum depths are shown in Table 8. Comparing Table 8
with Tables 57, it would appear that the growth rate of the pre-pits is lower than
those of the pits developed from a smooth surface, especially in aerated 1.5 ppm Cl
solution. However, the comparison is valid only with respect to the same range of pit
depths (i.e. between the initial pre-pit depth and the nal depth from the pre-pit), as

Table 8
Depths of pre-pits on the disc steel before and after testing at 90 C (initial stress: 90% r0:2 )
Environment

Deaerated high
purity water
Aerated high
purity water
Aerated 1.5 ppm Cl
solution

Test duration
(h)

Specimen
no.

8322

13

9138
7173
9187

Pit depth (lm)


After

Pit growth
rate
(1012 ms1 )

89

182

3.1

41

103

140

1.1

47
1

72
102

133
193

2.4
2.8

Before

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A. Turnbull, S. Zhou / Corrosion Science 46 (2004) 12391264

the pit growth rate is known to decrease with time. In that context, the dierence in
growth rate for the deaerated solution does not seem signicant. Also, when account
is taken for the distribution of pit depths in Fig. 11, rather than considering just the
maximum value, it really is not possible to suggest any special features associated
with the pre-pit.
In pursuing this pre-pitting approach, the hope was that the pre-pits would grow
preferentially and cracks might initiate more readily at these locations because of the
greater depth. Crack measurement probes could then be located accordingly in future tests. However, not only did the pre-pits have a modest growth rate in aerated
1.5 ppm Cl solutions but cracks did not develop from these sites. For this environment, about 40% of pits had cracks at the depth corresponding to the extended
pre-pit depths. It is feasible that with less than one or two pre-pits on these specimens, the statistics were just not favourable enough.
3.8. Pit-to-crack transition
In aerated water, cracks were observed on specimens removed at 13,528 h (about
19 months) and at 15,758 h (22 months) but not on specimens removed at 9138 h
(about 13 months). By contrast, no cracking was observed in deaerated pure water
even after 22 months, although long crack growth is reported in such an environment [1,13,14]. Cracking was most extensive in the aerated chloride-containing
water.
The generally accepted phenomenological criteria for a pit to crack transition are
that the threshold stress intensity factor has to be exceeded (the pit has to exceed a
minimum depth) and the growth rate of the crack must exceed that of the pit [16].
For the tests with chloride, analysis of the data from all the tests is summarised in
Table 9 and for aerated water, the results are shown in Table 10.
In the case of very long cracks, the curvature of the specimen made reliable estimation of the crack length problematic using the normal optical methods of focusing on the specimen and adjusting the position laterally to measure the length.
Thus, in Table 9, the true value will be greater than the quoted value.
The extent of cracking in the aerated water and in the 1.5 ppm Cl solution is
represented in Fig. 12. A key feature of Fig. 12 is the remarkable similarity in the
percentage of pits with cracks at specic pit depths despite changes in exposure time
and the presence or absence of chloride. Of course, the density of deep pits is greater
in the 1.5 ppm solution. Thus, overall, cracking will be more extensive and the cracks
larger in the 1.5 ppm solution. Crack coalescence will also be more signicant.
The likelihood of cracking from a pit was described reasonably by a Weibull
distribution function:
F a 1  expfa  a0 =g  a0 b g

where a0 is the threshold pit size, g is the scale parameter (equal to the value of a at
which F a is 0.632) and b is the shape parameter, the value of which reects the
extent to which the probability of crack initiation increases or decreases with time. In
the case of pits, the probability of the transition to a crack increases with pit depth

A. Turnbull, S. Zhou / Corrosion Science 46 (2004) 12391264

1257

Table 9
Crack density in disc steels in aerated 1.5 ppm Cl at 90 C (the specimens were loaded to 90% of YS)
Test time
(h)

Crack densitya
(cm2 )

5107

11.5
21.3
28.7
21.0
20.6

1157
1085
985
1075
1076

7173

27.7
22.7
25.2

9187

38.3
28.2
33.3

Average crack
length (lm)

Average
surface crack
growth rate
(1010 ms1 )

Maximum
crack length
(lm)

Maximum
surface crack
growth rate
(1010 ms1 )

0.6

2397
2230
2591
3421
2660

1.4

>1479
>1792

>0.5
>0.7

>3662
>4528

>1.4
>1.7

>1684
>2110

>0.5
>0.6

>4363
>5240

>1.3
>1.6

Results from various specimens are shown with the average value in bold.
a
Sampling surface area: 6.0 cm2 .

Table 10
Statistics for cracks in disc steels in aerated pure water at 90 C (the specimens were loaded to 90% of YS)
Test time
(h)

Crack densitya
(cm2 )

Average crack
length (lm)

Average
surface crack
growth rate
(1011 ms1 )

Maximum
crack length
(lm)

Maximum
surface crack
growth rate
(1010 ms1 )

5107
9138
13,528

No crack
No crack
No crack
5.33
1.33

N/A
N/A
N/A
789
556

N/A
N/A
N/A
4.99b
2.33b

N/A
N/A
N/A
1619
1169

N/A
N/A
N/A
1.02b
0.49b

15,758
a
b

Sampling surface area: 6.0 cm2 .


Assuming crack initiation time is 91,388 h.

and this is consistent with the calculated value of 1.5 for b. For g, a value of 295 lm
was determined. The value of g would be expected to be stress-dependent and
conceptually would be expected to depend on the nature of the environment. In that
context, the overlap of the data for the chloride-free and chloride containing solution
was surprising. Nevertheless, recent measurements [8] of the potential at the tip of a
crack indicated no distinction between an aerated solution containing chloride and a
chloride-free solution, although there was a distinct eect of oxygen concentration.
This may be a possible explanation for the similarity of the results of Fig. 12, although some caution is necessary in extrapolating data from deep (6 mm) cracks to
relatively shallow pits. However, if the Weibull relationship is combined with the pit
density distribution to predict the likely number of cracks on the two specimens in
aerated water removed at 9138 h, a value of 17 is obtained. In practice, no supercial

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A. Turnbull, S. Zhou / Corrosion Science 46 (2004) 12391264

Fig. 12. Likelihood of cracks developing from pits as a function of depth.

cracking was observed but more detailed evaluation is being conducted to check for
sub-surface cracks perhaps initiating from the base of pits but yet to break surface.
However, since some deep pits were observed at 5000 h with no cracking also, it
perhaps suggests that there is some other factor that is inuencing the transition that
can be related to exposure time.
The same predictive approach for the likelihood of cracking can be used for the
results in the deaerated solution, for which no cracks were observed, since it could be
argued that the pits were simply not deep enough in this case to make the transition
to a crack. In this case, the probable number of cracks to be expected in the specimens tested in the deaerated solution was 22, assuming the same Weibull function
parameters. It could be argued that the behaviour for the deaerated solution is
distinct from that of the aerated solution, particularly in the light of the crack-tip
potential measurements [8]. However, in view of the absence of cracks in the shortterm aerated chloride-free tests, too strong a conclusion would not be merited.
Longer-term tests in the deaerated pure water would be required to resolve this but
would be dicult to justify since this environmental combination of pure water and
deaeration is now recognised to be not so practically relevant.
3.9. Crack growth rates
As indicated, the pit to crack transition beyond the threshold value has been associated with the condition that the growth rate of the crack should be greater than
that of the pit [16]. The crack growth rate can be estimated approximately from
measurement of the crack depth by sectioning of the specimen and by assuming
initiation on initial exposure. Work on this aspect is in progress. Table 11 shows
preliminary estimates for the maximum crack depth derived from four longitudinal
slices on specimens tested in aerated 1.5 ppm Cl solutions for 5107, 7173 and 9187 h.
The maximum crack growth rate was calculated by dividing the maximum depth by

A. Turnbull, S. Zhou / Corrosion Science 46 (2004) 12391264

1259

Table 11
The depth and growth rate of cracks initiated from pits in the disc steel tested in aerated 1.5 ppm Cl
solution at 90 C
Test time (h)

Maximum crack depth (lm)

Maximum growth rate (1011 ms1 )

5107
7173
9187

820
960
1030

4.5
3.7
3.1

the total exposure time, ignoring any initiation period, and is also shown. (Of course,
from a practical viewpoint, the concern over initiation time may be academic since
it is the growth rate of the aw (pit plus crack) that is important). The estimated
crack growth rates are about a factor of 3 less than the surface crack growth rates
(Table 9). They are consistent with the average pit growth rates for the deepest pits
(Table 7).
For this steel, the stress corrosion growth rates of long cracks were determined
previously [17] using FM specimens with a 6 mm pre-fatigue crack immersed in the
same aerated 1.5 ppm solution. The test period was 7176 h. The extension in crack
depth was measured by fracturing the specimen at the end of the exposure period
rather than by in-situ crack depth monitoring. The crack grows only about 250 lm
over this extended period and the stability in the crack depth measuring system was
not adequate, although this has now been overcome with a new system capable of
stable 1 lm resolution. Assuming the cracks initiated on initial exposure, the crack
growth rates were estimated to be 8.9 1012 and 1.0 1011 ms1 for static loads of
40 and 50 MPa m1=2 respectively.
The uncertainty in the time to initiate a crack and some dierences in the rate of
change of corrosion potential with time for the two types of specimen means that
comparison of growth rates from the tests on plain specimens and from the fracture
mechanics specimens should be treated with caution. With that caveat, the indications are that the growth rate of the short crack initiated from pits is about four
times faster than that of the long crack.
3.10. Crack morphology
A typical etched cross-section of the specimens tested in aerated 1.5 ppm Cl
solution is shown in Fig. 15. Examination of a number of such sections indicated
that the crack was predominantly transgranular, although there was some evidence
of intergranular cracking (Fig. 13).
3.11. Pit and crack proles
A detailed study has been conducted on the proling of pits and cracks using a
layer removal technique and an image analyser. For the self-loaded specimen exposed to 1.5 ppm solution for 5107 h, longitudinal slices were removed along the
gauge length in controlled intervals of approximately 50 lm.

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A. Turnbull, S. Zhou / Corrosion Science 46 (2004) 12391264

Fig. 13. The etched cross-section surface of specimens tested in aerated 1.5 ppm Cl solution at 90 C,
showing predominantly transgranular cracking.

The individual images of each exposed new section are shown in Fig. 14. For a
tensile specimen, the width of the slice will increase progressively from the top
surface. As described above, the transition from a pit to a crack is a probabilistic
process with the likelihood increasing with pit depth. Hence, there will be some deep
pits from which no crack develops (e.g. Pit A). It is also interesting to note that the
depth of some cracks is smaller than that of the corresponding pit (e.g. Pit B),
suggesting that cracks do not necessarily initiate from the bottom of the pits. The
alternative explanation that the pit subsequently grew faster seems less likely because
corrosion blunting might have been anticipated. On the other hand, there were many
cracks with a depth greater than that of the corresponding pit (e.g. Pit C), but it is
dicult intrinsically to ascertain whether the cracks initiated at the bottom of the
pits or the initiated crack progressed beyond the depth of the pits. The possibility
that the crack does not initiate from the base of the pit has implications for the
prediction of the pit to crack transition using fracture mechanics concepts, as the
stress intensity factor is usually based on treating the pit as an equivalent crack of
the same depth. An added complication is the probabilistic nature of the transition
as evidenced by Fig. 12. There is also clear evidence that some pits and cracks
coalesced (e.g. Area D).
3.12. MnS inclusions
It is evident that anionic species in solution are not required to cause pitting attack in this steel. Inclusions are likely to be involved, of which the most aggressive
and plentiful is MnS. The MnS inclusion distribution in the disc steel was analysed
by sectioning a cylindrical specimen longitudinally. This was then mounted in phe-

A. Turnbull, S. Zhou / Corrosion Science 46 (2004) 12391264

1261

Fig. 14. Microphotograph of the cross-section surface using the layer removal technique, constructed with
an image analyser.

nolic resin such that the curved surface of the gauge length was visible. The surface
was then ground and polished such that a plane surface was obtained in which the
MnS inclusions could be clearly seen using optical microscopy.
For analysis of the MnS size and size distribution, 56 digital images were obtained
using a camera attached to an optical microscope. Each image covered an area
of 0.021 mm2 . The area of each inclusion was measured and the diameter of the

1262

A. Turnbull, S. Zhou / Corrosion Science 46 (2004) 12391264

Fig. 15. The distribution of the equivalent circle diameter of MnS inclusions in 3% NiCrMnV disc steel.
Table 12
Statistics of MnS inclusions in the 3% NiCrMnV disc steel
Diameter of the equivalent circle (lm)
Maximum

Minimum

Average

Density
(cm2 )

15.3

0.37

1.72 1.94

2.24 104

inclusion was estimated by tting it to a circle (the diameter of the equivalent circle).
The size distribution obtained from these images is shown in Fig. 15 and Table 12.
The density for this rather old steel is very high indeed and would provide plentiful
sites for initiation of pitting and indeed for perhaps continuing to inuence the
propagation rate and shape for the reasons articulated above.

4. Conclusions
Pitting was observed under all exposure conditions with the pit density and
growth rates increasing generally in the order: deaerated pure water; aerated pure
water, and aerated 1.5 ppm chloride-containing water.
Pits formed in the pure water tended to be tighter with a higher depth to mouth
opening ratio than for the chloride-containing water. This is rationalised on the
basis of retention of local pit solution chemistry inuenced by MnS inclusions
for the pure water bulk solution and a combination of mildly acidic pit environments and potential drop considerations in the chloride-containing solution.

A. Turnbull, S. Zhou / Corrosion Science 46 (2004) 12391264

1263

Extensive stress corrosion cracking from pits had initiated in the chloride-containing solution at exposure time less than 7 months. In aerated water, cracking was
observed at 19 months but not at 13 months. A minimum pit size of 50 lm for
initiation of cracks was identied. However, no cracking was observed in deaerated pure water after 22 months despite pit depths of up to 200 lm. There was
no evidence of cracking in the absence of pits.
The probability of a crack initiating from a pit of specic depth in aerated solution was surprisingly similar for the 1.5 ppm chloride solution and the chloridefree water at long exposure times. The transition from a pit to a crack was well
described by a Weibull cumulative distribution function. Of course, the density
of deep pits is greater in the 1.5 ppm solution. Thus, overall, cracking will be more
extensive and the cracks deeper in the 1.5 ppm solution.
The growth rate of short cracks initiated from pits in aerated 1.5 ppm Cl solution was about four times greater than that of long cracks determined using FM
specimens with a 6 mm pre-crack but in both cases there was uncertainty in the
time to initiate the crack.
The cracking mode in aerated 1.5 ppm Cl solution was identied as predominantly transgranular.
Proling of the pits and cracks by progressive layer removal and imaging indicated that whilst the crack depth usually exceeded the pit depth there were examples where the pit depth extended signicantly beyond the crack; i.e. the crack
may not have initiated from the base of the pit. In that circumstance, simple application of fracture mechanics principles based on the pit acting as an eective
crack of the same depth would not be pertinent.
It should be emphasised that these measurements of pit and crack growth rates
are based on continuous exposure and in the case of the 1.5 ppm chloride under
very severe conditions. More work is required to translate these measurements
into likely growth rates in service, for which the exposure conditions will be transient and in the case of the severe conditions, short-lived.

Acknowledgements
This work was conducted as part of the Life Performance of Materials programme, a joint venture between the United Kingdom Department of Trade and
Industry and an Industrial Group comprising Alstom, BNFL Magnox, British Energy, Innogy, Powergen, and Siemens. The authors are grateful to Angela Mensah,
Linda Orkney and Gareth Hinds for assistance with the experimental work.

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