Assessing the risk of under-deposit

chloride-induced stress corrosion cracking in

austenitic stainless steel nuclear waste
containers
A. B. Cook*1,2, S. B. Lyon1,2, N. P. C. Stevens1,2, M. Gunther2, G. McFiggans3,
R. C. Newman4 and D. L. Engelberg1,2,5
This paper provides a short summary of investigations that have focused on the occurrence of the
phenomenon that is commonly referred to as atmospheric chloride-induced stress corrosion
cracking (AISCC) in types 304L and 316L austenitic stainless steels; the materials from which
storage containers for the UKs intermediate level nuclear waste are currently fabricated. A brief
overview of the relationship between localised corrosion phenomena (pitting or crevice corrosion)
and stress corrosion cracking from observations derived under conditions of immersion in
chloride-containing environments is provided. The impact of environmental variables such as the
relative humidity, temperature and chloride deposition density on the development of AISCC and
potential difficulties in extrapolating data derived from laboratory investigations to an in-store
situation are also discussed. Proposals for the development of laboratory protocols that may more
accurately reflect behaviour in an actual storage situation, including the possibility of employing
accelerated testing methods, are also briefly addressed.
Keywords: Stress corrosion cracking, Stainless steel, Chloride, Low temperature, AISCC, Atmospheric, Localised corrosion

This paper is part of a special issue on Long-Term Prediction of Corrosion Damage in Nuclear Waste Systems

Introduction occur.2 Clearly knowledge of any risk that AISCC poses

Prior to emplacement in a geological disposal facility
(GDF), the UKs intermediate level radioactive waste
(ILW) will be housed in interim surface storage facilities
within containers manufactured from types 304L and
316L austenitic stainless steels.1 The construction of the
GDF is yet to begin, so this situation is likely to persist
for many decades to come. Containers in stores located
close to marine environments will almost certainly be
subject to the deposition of chloride-containing particu-
lates from sea-salt aerosol and, as such, be at risk of
developing sites of localised corrosion (pitting and/or
crevice attack). Consequently, in areas of sufficient
tensile stress there is a possibility that a transition to a
phenomenon that has become known as atmospheric
chloride-induced stress corrosion cracking (AISCC) may
1 to date and critically consider its relevance to the storage
Materials Performance Centre, School of Materials, The University of
Manchester, Manchester M13 9PL, UK
2
Corrosion and Protection Centre, School of Materials, The University of
Manchester, Manchester M13 9PL, UK
3
School of Earth, Atmospheric & Environmental Sciences, The University
of Manchester, Manchester M13 9PL, UK
4
Department of Chemical Engineering and Applied Chemistry, University
of Toronto, Toronto, Ontario M5S 3E5, Canada
5
Research Centre for Radwaste and Decommissioning, The University of
Manchester Manchester, M13 9PL, UK
*Corresponding author, email tony.cook@manchester.ac.uk
to container integrity is of great importance to the UKs
nuclear industry.
AISCC remains a relatively sparsely studied subject.314
It has, however, been clearly demonstrated in laboratory
tests that ILW container materials are susceptible to
AISCC under wetted chloride-containing deposits at,
and close to, ambient temperatures.35,713 By contrast
there have been no reports, to our knowledge at least, of
ILW containers developing AISCC in their storage
environment. This observation is probably related to the
fact that conditions employed in the laboratory are much
more aggressive, in terms of the environmental variables
that significantly impact the development of AISCC, e.g.
chloride deposition density, relative humidity (RH),
temperature and tensile stress, than those which may be
expected to be experienced in practice. In this paper, we
provide a short overview of work on AISCC reported
situation.
Chloride-induced stress corrosion
cracking in aqueous environments
Stress corrosion cracking (SCC) in non-sensitised types
304L and 316L stainless steels in chloride-containing
solution is usually found to initiate from sites of

2014 Institute of Materials, Minerals and Mining

Published by Maney on behalf of the Institute
Received 18 February 2014; accepted 7 June 2014
DOI 10.1179/1743278214Y.0000000204 Corrosion Engineering, Science and Technology 2014 VOL 49 NO 6 529
Cook et al. Atmospheric chloride-induced stress corrosion cracking in austenitic stainless steels
localised corrosion (pits or crevices).14,15 Furthermore
SCC only initiates from sites where the rate of localised
corrosion is less than the crack velocity. Hence SCC only
occurs over a very narrow potential range close to the
repassivation potential, as at higher potentials the
localised corrosion velocity will always exceed that of
crack propagation. Tsujikawa and co-workers have
investigated the relationship between SCC and localised
corrosion in some detail.1520 They found that SCC
velocity increases more rapidly with temperature than
does the localised corrosion velocity. It is this which
accounts for an apparent threshold temperature for the
development of chloride-induced SCC in these type of
stainless steels; the threshold temperature represents the
point at which SCC and localised corrosion velocity are
equal. The induction time to SCC is a function of the
chloride concentration whilst the crack growth rate is
unaffected by this quantity.15
Low temperature AISCC (,50uC)
To our knowledge, the first workers to present evidence
of under-deposit SCC at low temperature in an
austenitic stainless steel were Truman and Pirt,3 who
reported AISCC in type 302 stainless steel under
wetted zinc chloride deposits at 40uC (well below the
then almost universally accepted threshold temperature
of y60uC for chloride-induced SCC in aqueous
environments).21 It was Shoji and Ohnaka, however,
who provided the first systematic study of the AISCC
phenomenon in terms of temperature, nature of the
chloride salt and RH, and were the first to demonstrate
its occurrence in types 304L and 316L stainless steels
under ambient conditions.4
Effect of environmental variables on the
development of AISCC
Environmental RH
Shoji and Ohnaka performed tests over a two year period
at 25uC and found that AISCC developed in U-bend
specimens of both 304L and 316L stainless steels under
wetted deposits of sea-salt and Mg, Ca and Zn chlorides;
in tests at higher temperatures (50 and 70uC) performed
over a two-week period, LiCl2 was also found to promote
cracking.47 They presented data regarding the RH range
over which AISCC was observed together with measures
of crack severity including the ratio of the number of
deposits with cracks to the total number of deposits, the
mean number of cracks per deposit and the average
maximum crack length in deposits with cracks. The RH
ranges over which AISCC was observed in the case of sea-
salt and MgCl2 deposits are summarised in Table 1. In
summary, the RH range over which AISCC occurs
Table 1 RH for AISCC taken from work of Shoji and Ohnaka47
Wetted deposit
type/Cl2 deposition Temperature/test
density duration
MgCl2/2500 mg cm22 25uC/24 months
50uC/2 weeks
70uC/2 weeks
Sea-salt/2500 mg cm22 25uC/24 months
50uC/2 weeks
70uC/2 weeks
530 Corrosion Engineering, Science and Technology 2014
narrows with decreasing temperature. Given the rela-
tively short duration of the tests conducted at 50 and
70uC (two weeks) the possibility of cracks developing
over a wider RH range had experiments been conducted
over a longer timescale cannot be ruled out.6
The RH in the vicinity of chloride-containing surface
salt deposits determines the chloride concentration of
the atmospherically induced electrolyte layer and, in the
case of sea-salt, its composition too. At this juncture
it should be emphasised that chloride concentration
refers to mass per unit volume of Cl2 in the deposit and
is not to be confused with chloride deposition density
which reflects the mass of Cl2 per unit area of exposed
surface. As such the RH thresholds determined by Shoji
and Ohnaka also provide information regarding the
range of chloride concentrations that promote AISCC.
Conversion of the RH range for AISCC under MgCl2
deposits at 25uC to the corresponding chloride concen-
tration range using the relationship between RH and
Cl2 provided by Tsutsumi et al.22 suggests that under
ambient conditions AISCC develops under deposits
containing between 710 mol dm23 Cl2 for 304L and
8?510 mol dm23 Cl2 for 316L. The RH of maximum
cracking susceptibility in both materials under wetted
MgCl2 and sea-salt deposits, 30%, is close to the
equilibrium RH of saturated MgCl2 at 25uC, 33%.23
Hence, Shoji and Ohnaka reasonably concluded that
MgCl2 is the sea-salt constituent responsible for
promoting low temperature AISCC in types 304L and
316L stainless steels. That a highly concentrated surface
chloride solution is required for the development of
AISCC is not a universal finding, however. Fairweather
et al.12 have performed work on AISCC in type 304L
stainless steel contacted with MgCl2 at temperatures
between 30 and 60uC and at RH values between 15 and
100%.12 AISCC was observed at all temperatures and
RH values. In contrast to the work of Shoji and co-
workers the maximum AISCC susceptibility appeared to
occur at intermediate RH value, y60%, which is a value
well above that of saturated MgCl2.
Prosek and co-workers810 investigated the occurrence
of AISCC in U-bend specimens of these materials under
deposits of MgCl2 and CaCl2 using a very similar
experimental approach to that of Shoji and Ohnaka and
also found that the RH range (hence the chloride
concentration of the deposits) over which AISCC occurs
widens with increasing temperature. Prosek et al. also
found that the nature of the chloride salt had a marked
effect on AISCC behaviour, reporting that both
materials were immune to AISCC in the presence of
MgCl2 or CaCl2 deposits at 20uC and that 316L did not
develop AISCC in the presence of MgCl2 at 20, 30 or
RH of RH range over which
maximum AISCC was observed
AISCC
susceptibility 304L 316L
30% 2550% 2550%
30% 2050% 2050%
30% 2090% 2080%
30% 2550% 2540%
30% 2050% 2550%
30% 2080% 2050%
VOL 49 NO 6
 Cook et al.
40uC. The findings of Prosek et al. are summarised in
Table 2. On the basis of their observations these workers
determined temperature dependent chloride concentra-
tion thresholds for AISCC in both 304L and 316L of 14,
10 and 7 mol kg21 at 20, 30 and 40uC, respectively. It
was contended that at 20uC the Cl2 concentration
required for the initiation of AISCC exceeds the
solubility limit of both MgCl2 and CaCl2, hence the
immunity of both materials at this temperature. At 30
and 40uC the critical Cl2 concentration for AISCC in
304L is less than the solubility of both MgCl2 and
CaCl2, hence the threshold Cl2 concentration required
for the occurrence of AISCC may be exceeded in the
presence of either salt. For 316L, however, the Cl2
concentration threshold may only be exceeded if CaCl2
is present and AISCC may occur when the RH is less
than 40%.10 As the authors themselves point out these
tests were performed over a relatively short period
(10 weeks) and consequently the possibility of AISCC
occurring at lower chloride concentration in longer tests
could not be definitively ruled out.
The lower limit of a wetted deposits Cl2 concentra-
tion, as determined from the work of Shoji and Ohnaka,
for AISCC to develop in 304L contacted with MgCl2 at
25uC is relatively high, y7 mol dm23 (in good agree-
ment with the value of y8 mol dm23 that may be
inferred from work Prosek et al. at 30uC).10 If we accept
that AISCC in these materials is always associated with
some form of localised corrosion, then the observation
of the high chloride requirement for low temperature
AISCC is very likely associated with its effect on pit
stabilisation. At high chloride concentrations pit stabi-
lity can be achieved at lower anodic dissolution rates,
since a lower concentration of alloy cations are required
to maintain the critical chemistry for sustained propaga-
tion of localised corrosion.24 Hence a high chloride
concentration in the thin atmospherically induced
electrolyte layer should more easily facilitate pit growth
at the slow rate necessary to allow the transition to
AISCC from pits or crevices.
Chloride deposition density
A means of mitigating AISCC based on limiting the
surface chloride deposition density has been proposed
by Albores-Silva et al.13 These workers demonstrated
the existence of thresholds in this quantity below which
AISCC does not develop in 316L U-bend specimens,
taken from the body of an ILW container, contacted
with wetted MgCl2 deposits. Threshold values of 10
and 25 mg cm22 were found at 50 and 30uC, respectively,
at the equilibrium RH of MgCl2. At 60% RH a
higher threshold value of somewhere between 50 and
100 mg cm22 was found.13 In tests at ambient tempe-
rature even higher threshold values have been
Table 2 RH ranges for AISCC taken from work of Prosek et al.10
Wetted deposit type/Cl2 deposition density Temperature/test duration
MgCl2/26 000 mg cm22 20uC/10 weeks
30uC/10 weeks
40uC/10 weeks
CaCl2/29 000 mg cm22 20uC/10 weeks
30uC/10 weeks
40uC/10 weeks
Corrosion Engineering, Science and Technology
Atmospheric chloride-induced stress corrosion cracking in austenitic stainless steels
determined.25 We have previously briefly discussed the
need for caution when employing threshold values in
deposition density determined over such a short-time-
scale in a laboratory situation to predict AISCC
susceptibility elsewhere, but we will revisit our concerns
in the remainder of this section.26,27
The thresholds mentioned above were determined
from a 12 week test, a relatively short duration given
that the induction time (the time required for a stable pit
to reach the slow state of localised corrosion from which
the pit to crack transition can take place) associated with
AISCC can be longer and will very likely increase as the
amount of surface chloride is decreased. The induction
time will also display large scatter at constant deposition
density as the initiation of localised corrosion is a
random event (a large scatter is typically observed in
induction times associated with pitting the time for a
stable pit to develop after conditions conducive to
pitting are developed). For example, induction times for
AISCC of between 48 weeks and 812 weeks, respec-
tively, may be inferred from the work of Shoji and
Ohnaka for AISCC produced at room temperature at
30% RH in U-bends of 304L and 316L contacted with
wetted MgCl2 deposits, at a Cl2 deposition density of
y1300 mg cm22.4 For U-bends contacted with sea-salt
deposits induction times were between 4 weeks and two
years for 304L and between 6 months and two years for
316L; in the case of 316L not all deposits had developed
cracks at the end of the two year test period.4 Cook et al.
observed an average induction time at 40uC and 30%
RH, of y13 weeks for 304L and y20 weeks in 316L,
with tensile specimens loaded to their respective
yield stresses at a chloride loading of 340 mg cm22
(450 mg cm22 MgCl2).11,28 The latter induction time
exceeds the ,12 week period that may be predicted
from the tests of Albores-Silva et al.,13 but may simply
be related to the lower applied stress employed in
experiments conducted by Cook et al.11,28 During their
investigations Cook et al.28 also obtained some evidence
that the chloride deposition density affects the induction
time but not crack growth rate.
As such careful consideration should be given to
whether the use of thresholds based on the chloride
deposition density determined from experiments con-
ducted under conditions of constant RH and tempera-
ture, with relatively large deposits (several mm2 in area)
in a laboratory situation is an entirely suitable means of
predicting the tendency towards AISCC in the storage
situation.411,13 The deposition density is related to the
average amount of salt deposited per unit area, it does
not provide an accurate measure of the dimensions of
any salt contaminated regions (unless of course salt
contamination is uniform), the size of the individual
RH range over which AISCC was observed
304L 316L
No AISCC No AISCC
2744% No AISCC
2567% No AISCC
No AISCC No AISCC
1749% 1740%
1269% 1239%
2014 VOL 49 NO 6 531
Cook et al. Atmospheric chloride-induced stress corrosion cracking in austenitic stainless steels
salt-deposits and hence the dimensions and/or continuity
of any atmospherically produced electrolyte layer.
Indeed the use of large salt deposits is very unlikely to
be at all representative of the conditions encountered
during interim storage. The size of the aerosol particles
and the rate of change in coverage will depend on the
proximity of the storage facility to the sea. The larger
aerosol particles, those that form part of the coarse
aerosol size mode (i.e. .1 mm radius) will fall to ground
within 10 km. A typical marine aerosol size distribution
can extend to sub-micrometre sizes, with two distinct
subsets; the accumulation (ry0?10?2 mm) and nuclea-
tion modes (ry0?020?03 mm).29 Consequently, owing
to the rapid loss of coarse aerosol, the majority of
individual aerosol particles depositing on the surface of
ILW containers situated more than 10 km from the surf
zone will be sub-micrometre in diameter and hence sub
mm2 in area.29 As such, levels of coverage similar to
those at which AISCC may initiate and subsequently
propagate relatively rapidly in a laboratory situation
may take many years to develop in service, if they ever
develop at all. The size and distribution of salt-crystal-
lites prior to wetting and any changes in their spatial
distribution that occur during wet/dry cycles will be
important in terms of the development of localised
corrosion and AISCC in a storage situation, as it is these
quantities that will determine the fraction of surface in
contact with electrolyte at any given RH and tempera-
ture, and consequently the probability of localised
corrosion initiating.
Perhaps a more appropriate means of predicting
AISCC in ILW container material would be to
determine if there exists a critical deposit size below
which AISCC can no longer be supported. Some
preliminary work regarding the effect of deposit size
and distribution on induction time and extent of
cracking has been conducted using arrays of deposits
produced via a spray technique, albeit at a temperature
well above that which will be encountered during ILW
storage: 80uC and 30% RH.30 In the case of wetted sea-
salt deposits, the parameters correlate with changes in
the average deposit size and spacing prior to environ-
mental exposure, i.e. induction times increased and the
extent of cracking was seen to decrease with decreasing
deposit size and increasing deposit spacing. As the
chloride concentration in the vicinity of individual
deposits is independent of the deposit size and/or
deposition density, changes in induction time must be
related to a decrease in the probability of the initiation
of localised corrosion brought about by changes in
surface coverage by the chloride-containing electrolyte.
In the case of MgCl2 the deposit sizes were below the
resolution of the optical microscope employed and
therefore no conclusive evidence of their effects was
determined.30
Aerosol composition
Laboratory studies are often performed under deposits
of a single salt, such as MgCl2 or CaCl2, rather than
sea-salt.411,13 It is by no means clear that such an
approach is actually applicable to the in-store environ-
ment. Sea-water contains a complex mixture of salts
which wet at various RH, e.g. at 25uC NaCl wets to form
a saturated solution at around 75% RH, KMgCl3.6H2O
at 59% RH and MgCl2 at 33% RH.23,31 KMgCl3.6H2O is
a sea-water evaporite commonly referred to as carnallite.
532 Corrosion Engineering, Science and Technology 2014
It is likely, therefore, that in areas of aerosol deposition
the surface of ILW containers will remain wet to some
degree, and hence at risk of developing localised
corrosion over a very wide RH range.
Marine aerosols also contain organic species that may
affect both the wetting characteristics of the aerosol
particles and the surface salt loading. As discussed in the
section on Environmental RH, organic materials are
ubiquitous components of fine atmospheric aerosol
particles and arise from both primary and secondary
processes.32,33 Sea-salts and organic content are com-
monly ejected simultaneously from oceanic waters via
breaking waves or whitecap production, with particu-
lates dispersed into the atmosphere via bubble-bursting.
The speciation produced via these physical processes is
commonly referred to as primary marine aerosol. The
organic content so produced has been found to consist
mainly of colloids or aggregates formed from oceanic
phytoplankton.34 Although marine organics contribute
only a small amount to the overall organic aerosol
budget, it has been shown that the organic component
arising from marine processes will contribute signifi-
cantly to the primary marine aerosol speciation budget
during periods of high biological activity; accounting for
up to 63% of the sub-micrometre aerosol dry mass.35
The close proximity of most of the UKs nuclear
infrastructure to coastlines further increases the sig-
nificance of primary marine derived aerosols to corro-
sion in this industry, as the transit distances and times
from production to deposition may be very short
compared to sites further inland. Clearly any laboratory
protocol designed to assess the likelihood of AISCC in
ILW containers must consider the effects of organic
species present in marine aerosol. Some preliminary
work on the effect of organic content has been presented
elsewhere.27 The limited data produced so far suggests
that the presence of primary organic aerosol compo-
nents such as the exudate derived from Phaeocystis
Globosa may decrease induction times associated with
AISCC.27
Extrapolation of laboratory data to the in-store situation
As implied in this and the previous sections, extrapolat-
ing laboratory data regarding AISCC in ILW container
materials to the in-store condition will be challenging,
largely as a result of difficulties in replicating coverage
via aerosol deposition and time-dependent changes in
RH and temperature. To our knowledge the only work
to date that addresses prediction of damage accumula-
tion resulting from AISCC in ILW containers during
storage is the atmospheric corrosion of stainless steel
in stores (ACSIS) model of King and co-workers.36
This model uses information regarding in-store time
evolution of the environmental RH and temperature
together with information regarding the chloride
deposition density to determine whether pitting and/or
AISCC will initiate during times of wetness. In ins-
tances where localised corrosion or AISCC is predicted
to initiate, the extent of damage in terms of pit, crevice
or crack depth is also calculated. The model assumes
AISCC will only occur above a certain threshold value
of the chloride deposition density and over a defined
range of RH. Threshold values for the chloride
deposition density are taken from the work of
Albores-Silva et al.13
VOL 49 NO 6
 Cook et al.
Accelerated testing
As discussed in the section on Environmental RH,
induction times associated with AISCC can be long and
show large variability. As such it may be prudent to
consider the development of accelerated testing meth-
ods; that is, to work at temperatures well above those
expected in-store to complement and guide work
performed under conditions more relevant to the storage
condition. By working at a range of higher tempera-
tures, trends in the induction time and crack growth rate
as a function of various critical experimental quantities,
such as deposit size and distribution, salt composition
and time of wetness, etc., may be obtained over
relatively short timescales and then extrapolated to
conditions more representative of the in-store environ-
ment. The accuracy of any predictions may then be
examined by performing a range of more representative
experiments at lower temperature to compare predicted
and experimentally measured values. Such an approach
is being adopted as part of the strategy at The University
of Manchester to map the parameter space over which
AISCC can develop in types 304L and 316L stainless
steels.
Summary
AISCC is a complex, sparsely studied phenomenon that
may prove a risk to the integrity of ILW containers
during both interim storage and the operational phase of
geological disposal. Very little data regarding para-
meters such as induction times and crack growth rates
and their dependence on various environmental vari-
ables are available. Here we have sought to provide a
short but balanced review/assessment of the work
performed to date and in doing so to provide some
food for thought with regards to the development of
future experimental protocols to provide data that
accurately reflects corrosion in the storage situation.
Much more systematic work will be required to
determine the parameter space in terms of aerosol
composition, particulate size and distribution (or
chloride deposition density if correlation can be made
between the size and distribution of aerosol deposits). In
summary, the experimental evidence suggests that at low
temperature AISCC can only develop in highly con-
centrated chloride solutions and is controlled largely by
factors related to pit initiation and stability.
Acknowledgements
Financial support for D. Engelberg (EPSRC grant
no. EP/I036397/1 and NDA contract no. NPO004411A-
EPS02) and M. Gunther (EPSRC funded Nuclear FIRST
CDT) is gratefully acknowledged.
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