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Stress corrosion crack initiation in Alloy 690 in high temperature water

Article  in  Current Opinion in Solid State and Materials Science · February 2018

DOI: 10.1016/j.cossms.2018.02.001

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 Current Opinion in Solid State and Materials Science xxx (2018) xxx–xxx

Contents lists available at ScienceDirect

Current Opinion in Solid State and Materials Science

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

Stress corrosion crack initiation in Alloy 690 in high temperature water

Tyler Moss, Wenjun Kuang, Gary S Was ⇑
University of Michigan, 2355 Bonisteel Blvd, Ann Arbor, MI 48109, United States

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

Article history: Initiation of stress corrosion cracks in Alloy 690 in high temperature water is a rare occurrence and
Received 25 August 2017 depends on the method by which the sample is loaded. Only in dynamic straining experiments is crack
Revised 26 November 2017 initiation consistently observed. Stress relaxation in constant deflection tests, and lack of a means of rup-
Accepted 3 February 2018
turing the oxide film in constant load tests are the principle reasons for the difficulty of initiating cracks
Available online xxxx
in these tests. These observations, combined with those from the much more susceptible Alloy 600 form
the basis for a mechanism stress corrosion crack (SCC) initiation of Alloy 690. SCC initiation is proposed to
Keywords:
occur in three stages: an oxidation stage in which a protective film of Cr2O3 is formed on the surface over
Stress corrosion cracking
Alloy 690
grain boundaries, an incubation stage in which successive cycles of oxide film rupture and repair depletes
SCC mechanism the grain boundary of chromium, and a nucleation stage in which the chromium depleted grain boundary
Oxidation is no longer able to support growth of a protective chromium oxide layer, resulting in formation and rup-
Crack incubation ture of oxides down the grain boundary. The mechanism is supported by the available literature on oxi-
Crack initiation dation and crack initiation of Alloy 690 in hydrogenated primary water conditions.
Crack nucleation Ó 2018 Elsevier Ltd. All rights reserved.

1. Introduction an ongoing program to investigate the role of cold work in SCC of

Stress corrosion cracking (SCC) of Alloy 690 in high temperature
water has been extensively studied since the 1970s as the Alloy
was introduced into pressurized water nuclear reactor (PWR)
steam generators as replacement tubing for Alloy 600 (N06600)
in 1979, and later for vessel head penetration nozzles [1]. Given
the past experience with the long incubation time to crack initia-
tion in Alloy 600, there is concern that SCC could eventually occur
in Alloy 690. There has been no evidence of primary water stress
corrosion cracking (PWSCC) of Alloy 690 in steam generators since
its introduction. Current regulations allow for a life extension of
the 40-yr operating license of a PWR for an additional 20 yr to a
total of 60 yr. With the prospect of a second life extension, operat-
ing lifetimes could approach 80 yr, emphasizing the need to under-
stand degradation modes of materials that have shown excellent
resistance to date.
Both crack initiation and crack growth are important in assess-
ing the resistance of an Alloy to stress corrosion cracking. While
crack growth rates (CGR) in pre-cracked Alloy 690 laboratory sam-
ples are generally extremely low [2,3], cold work has been
observed to increase the crack growth rate significantly (by up to
several orders of magnitude), especially in thermally treated (TT)
condition [4,5]. The Electric Power Research Institute (EPRI) has
⇑ Corresponding author.
E-mail address: gsw@umich.edu (G.S Was).
Alloy 690 in the form of an expert panel that meets annually to
review ongoing research. For crack growth to be of significance,
cracks must first nucleate. While Alloy 690 has proven to be very
resistant to crack nucleation both in service and in laboratory stud-
ies, experience with Alloy 690 has shown that it can indeed, occur.
It is the objective of this study to review what is known about crack
initiation in this Alloy and to propose a mechanism for crack
nucleation.
The difficulties associated with generating cracks in Alloy 690
have been an impediment to the study of the mechanisms of SCC
initiation. Alloys of similar composition, such as the lower chro-
mium nickel based Alloy 600, crack readily in high temperature
water, allowing researchers to study the SCC behavior in depth
and postulate mechanisms to explain the observed cracking behav-
ior. The higher chromium content of Alloy 690 is believed to be the
primary factor contributing to its resistance to IGSCC initiation.
Thus, while it is not the objective of this paper to review SCC of
Alloy 600, lessons learned in studying this Alloy will be employed
here in an effort to elucidate the mechanism by which crack initi-
ation occurs in Alloy 690. Techniques used for evaluating the SCC
initiation susceptibility can be categorized as either constant
strain, constant load, or constant extension rate tensile (CERT)
tests. As will be shown, the nucleation of IGSCC in Alloy 690 is
highly dependent on the test technique, and therefore, the follow-
ing section will review crack initiation in Alloy 690 by technique.
Results are summarized in Table 1.

https://doi.org/10.1016/j.cossms.2018.02.001
1359-0286/Ó 2018 Elsevier Ltd. All rights reserved.

Please cite this article in press as: T. Moss et al., Stress corrosion crack initiation in Alloy 690 in high temperature water, Curr. Opin. Solid State Mater. Sci.
(2018), https://doi.org/10.1016/j.cossms.2018.02.001
2 T. Moss et al. / Current Opinion in Solid State and Materials Science xxx (2018) xxx–xxx

Table 1
Summary of SCC initiation work on Alloy 690 in simulated PWR primary water.

Ref. Material condition Water chemistry Test technique Test duration Result
Constant deflection test
[6] MA and TT 316–360 °C oxygenated or deaerated Double U-bend Up to 10,080 h No cracking
water in static autoclave
[7] MA and TT 360 °C water with 3.8 ppm H2 and, Reverse U-bend Up to 16,000 h No cracking
1200 ppm B + 2 ppm Li or 200 ppm B
+ 0.5 ppm Li
[8] MA and TT 360 °C water with 30 cc H2/kg H2O Reverse U-bend 12,000 h No cracking
and 500 ppm B + 1–2 ppm Li,
[9] MA and TT, aged at 330 °C hydrogen saturated water Reverse U-bend 3000 h Max IG crack depth of 70
500 °C for 24 or 100 h with 1000 ppm B + 2 ppm Li, lm
renewed every 250 h
[10] TT 340 °C pure deaerated water C-ring test 1800 h No cracking
[11,12] MA and TT 365 °C water with 4–6 ppm H2 in Reverse U-bend Up to 33,000 h No cracking
once-through autoclaves
[13] 20% pre-strained Alloy 360 °C water with 30 cc H2/kg H2O Reverse U-bend Up to 10,015 h No cracking
690TT and 500 ppm B + 2 ppm Li, or 280
ppm B + 2 ppm Li, or1600 ppm B + 2
ppm Li, or 1600 ppm B + 3.5 ppm Li in
refreshed autoclave
[14] As received 350 °C water with 1200 ppm B + 2.2 Reverse U-bend 15,000 h No cracking
ppm Li, or 1800 ppm B + 3.5 ppm Li,
and 40 ppb Zn in once-through
autoclave
[15] MA and TT 365 °C pure water with 50 cc H2/kg Reverse U-bend Up to 33,000 h No cracking
H2O
[16] TT 360 °C PWR primary water with 23– Reverse U-bend Up to 90,000 h No cracking
35 cc H2/kg H2O in static autoclave
[17] TT 360 °C pure water with 3 bar H2, or Reverse U-bend Up to 46,000 h No cracking
PWR primary water with 0.16–0.5
bar H2 and 1000 ppm B + 2 ppm Li
[18] MA and TT 360 °C water with 1000 ppm B, 2 Reverse U-bend Up to 60,000 h No cracking
ppm Li, 167 cc H2/kg H2O in static
autoclave
[19] Hot-extruded + TT, 360 °C water with 30 cc H2/kg H2O, C-ring test Up to 3600 h No cracking
hot-rolled and 1000 ppm B + 2 ppm Li
[20] TT 380 °C hydrogenated steam, H2/H2O Reverse U-bend Up to 13,824 h One heat cracked
ratio  0.04 in static autoclave
[1] TT 400 °C hydrogenated steam, H2/H2O Reverse U-bend Up to 9720 h No cracking
ratio  0.0055
Constant load test (CLT)
[8] MA and TT 360 °C water with 30 cc H2/kg H2O, Constant load (414–621 7000 h No cracking
and 500 ppm B + 1–2 ppm Li MPa)
[13] 20% pre-strained Alloy 360 °C water with 30 cc H2/kg H2O Constant load (586 MPa) 10,000 h No cracking
690TT and 500 ppm B + 2 ppm Li, or 280
ppm B + 2 ppm Li, or1600 ppm B + 2
ppm Li, or 1600 ppm B + 3.5 ppm Li in
refreshed autoclave
[17] TT 360 °C primary water Constant load at 684 or 10,900 h at 684 MPa, No cracking
580 MPa 18,500 h 580 MPa
[21] TT 360 °C water with 30 cc H2/kg H2O From 603 to 684 MPa 11,000 h Crack depth <10 lm
and 1000 ppm B + 2 ppm Li,
[22] TT 360 °C water with 500 ppm B + 2 Constant load (300 to 123,000 h No rupture
ppm Li 550 MPa)
[23,24] TT + Cold worked 320–360 °C water with 0–45 cc H2/kg Constant load on BNT (30 Up to 34,484 h No cracking in water
H2O and 500 ppm B + 2 ppm Li in MPa
m1/2)
refreshed autoclave or 360–460 °C Constant load on Up to 26,576 h IG cracks with cavities in
air, or H2 in argon precracked CT(23–40 both water and gas
MPa
m1/2)
[25,26] TT + Cold worked 360 °C water with 1000 ppm B, 2 Constant load on tensile Up to 9950 h IG cracks with cavities
ppm Li, 25 cc H2/kg H2O bars (510 to 700 MPa)
Constant load on BNTs Up to 11,816 h IG cracks with cavities
with dynamic loading
(27.5–37 MPa
m1/2)
Constant extension rate tensile (CERT) test
[17] TT 360 °C primary water with0.16–0.5 Strain rate 5  10 8
/s Up to necking 5–65 lm deep IG cracks
bar H2 and 1000 ppm B + 2 ppm Li
[18] MA and TT 360 °C water with 25–30 cc/kg H2O Strain rate 5  10 8
/s Up to failure 20–120 lm deep IG cracks
and 1000 ppm B + 2 ppm Li in static
autoclave
8
[19] Aged, Hot-extruded + 360 °C water with 5–60 cc H2/kg H2O, Strain rate 4  10 /s 20% elongation One heat cracked with
TT, hot-rolled + cold and 1000 ppm B + 2 ppm Li depth up to 18 lm
rolled
[21] TT 360 °C water with 30 cc H2/kg H2O, Strain rate 5  10 9
-2.5  40–225 lm deep IG cracks
and 1000 ppm B + 2 ppm Li 10 7/s

Please cite this article in press as: T. Moss et al., Stress corrosion crack initiation in Alloy 690 in high temperature water, Curr. Opin. Solid State Mater. Sci.
(2018), https://doi.org/10.1016/j.cossms.2018.02.001
 T. Moss et al. / Current Opinion in Solid State and Materials Science xxx (2018) xxx–xxx 3

Table 1 (continued)

Ref. Material condition Water chemistry Test technique Test duration Result
7
[28,29] Cold worked, low C or C 360 °C water with16 cc H2/kg H2O, Strain rate 3  10 /s Up to failure A little IG cracking in low C
doped and 0.01 M H3BO3, 0.001 M LiOH, or heat, no cracking in C doped
360 °C argon heat
8
[30] Weld composite of 320 °C water with >20 cc H2/kg H2O, Strain rate 5  10 /s Up to 2394 h No cracking
Alloys 152 and 690 and 1000 ppm B + 2.2 ppm Li in
refreshed autoclave
[31] Solution anneal (SA) Deaerated pure supercritical water Strain rate 3  10 7
/s Up to failure Max IG crack depth <10 lm
and TT (385 °C: 27.6 MPa or 400 °C: 25.4
MPa)
8
[32] SA + cold work, TT + 360 °C pure water with 18 cc H2/kg Strain rate 5  10 /s and Up to failure Shallow cracks with average
cold work H2O 1  10 8/s length <10 lm
8
[33] MA 320–450 °C pure water with 6–290 cc Strain rate 5  10 /s 7% strain Shallow cracks with average
H2/kg H2O length <10 lm

Fig. 1. Cracked Alloy 690 reverse U-bend sample after 13,824 h exposure in
hydrogenated steam at 380 °C [20].
2. Review of SCC in Alloy 690
2.1. Constant deflection experiments
The constant deflection test has long been used to evaluate the
SCC susceptibility of Alloy 690 in which the strain is maintained in
samples with specific geometries, such as U-bend, reverse U-bend
and C-ring samples. U-bend samples made from plate or sheet
stock are bent into a U shape and constrained with a bolt through
the legs. The tensile strain peaks at the apex of the curve. A reverse
U-bend sample is normally made from tubing that is bent so that
the inner tube surface is in tension. C-ring samples are elastically
strained and fixed with a bolt in the shape of the letter ‘‘C”, and
can also be made from tube material with the outer surface in ten-
sion. The constant deflection technique is easy to implement but
has the drawback that stress relaxation occurs with time at high
temperature, as the typical PWR water temperature is 320 °C at a
pressure of 14.2 MPa.
Double U-bend tests on both TT and mill annealed (MA) Alloy
690 conducted by Sedricks et al. [6] showed that both conditions
were immune to cracking in both oxygenated and deaerated high
temperature water between 316 and 360 °C for up to 10,080 h,
even in the presence of a crevice, while the control material, Alloy
600, cracked under identical test conditions. Smith et al. [7] per-
formed reverse U-bend tests on three heats of Alloy 690 and a con-
trol heat of Alloy 600 in 360 °C simulated PWR primary water.
None of the Alloy 690 (TT or MA) samples cracked after 16,000 h
exposure while the Alloy 600 specimens in both conditions devel-
oped cracks. Yonezawa et al. [8] conducted reverse U-bend tests on
Alloy 690 and Alloy 600 tubing (TT and MA conditions) in 360 °C
simulated PWR primary water environment. No cracking was
found in Alloy 690 after 12,000 h exposure while Alloy 600 cracked
after 800 h. Single U-bend tests in 330 °C hydrogen saturated pure
water carried out by Nakayama et al. [9] showed that fine inter-
granular cracks initiated both in MA and TT Alloy 690 after 3000
h exposure, but much more severe cracking occurred on Alloy
600. This is the first reported incidence of SCC cracking on Alloy
690 in the laboratory.
Smith et al. [10] performed C-ring tests on TT Alloy 690 in 340
°C pure, deaerated water and observed no cracking after 1800 h
exposure. Similarly, reverse U-bend tests on 11 Alloy 690 steam
generator tubes (MA and TT conditions) in 365 °C hydrogenated
water for up to 33,000 h produced no cracking, while Alloy 600
specimens cracked with a Weibull characteristic time-to-cracking
(63.2% probability of cracking) ranging from 800 to 13,000 h, as
reported by Norring et al. [11,12]. Ogawa et al. [13] conducted
reverse U-bend tests on 20% pre-strained Alloys 690 (TT) and 600
(TT) with water chemistries of varying pH (6.61, 6.86, 7.1 and 7.3
at 285 °C). No cracks were found in Alloy 690 in 360 °C water,
while more than 60% of Alloy 600 specimens cracked in 320 °C
water after up to 10,015 h exposure at all values of pH.
Angell et al. [14] studied the effects of zinc addition on the SCC
behavior of Alloys 690 and 600 in 350 °C primary water chemistry
using the reverse U-bend test. No cracks were found in Alloy 690
specimens after 15,000 h, while Alloy 600 specimens cracked irre-
spective of zinc addition. Likewise, reverse U-bend tests conducted
by Efsing [15] produced no cracking in Alloy 690 (MA or TT) in 365
°C hydrogenated high-purity water after 33,000 h, while Alloy 600
cracked irrespective of the thermal treatment.
A report by the Electric Power Research Institute (EPRI) [1] sum-
marized the state of crack initiation studies on Alloy 690 in PWR
primary water reported by the French Atomic Energy Commission
(CEA) and Electricite de France (EDF). The CEA report by Raquet
et al. [16] showed that no SCC was found in the reverse U-bend
samples made from multiple heats of Alloy 690 (TT), nor was any
propagation detected at the surface defects created when forming
the U-bend samples after 90,000 h in 360 °C PWR primary water.
The EDF report by Vaillant [17] also indicated that the reverse U-
bend tests on Alloy 690TT did not produce any cracking in 360 °C
hydrogenated pure water or PWR primary water after 46,000 h.
Subsequent work by Vaillant et al. [18] indicated that reverse U-
bend tests with Alloy 690 (MA and TT) in 360 °C hydrogenated
water did not produce IGSCC after 60,000 h, while SCC occurred
on Alloy 600 in less than 5000 h. More recently, Tsutsumi and Cou-
vant [19] conducted C-ring tests on three heats of Alloy 690 with
different manufacturing conditions. No SCC initiation was detected
on any of the samples after 3600 h in 360 °C PWR primary water.
To accelerate the aggressiveness of the test, some reverse U-
bend tests have been conducted in steam at higher temperature.
In one study [1] on reverse U-bend tests of Alloy 690TT and Alloy
600MA tubes with and without surface grooves of depth 20–40% of
the wall thickness in 400 °C hydrogenated steam, no cracking was

Please cite this article in press as: T. Moss et al., Stress corrosion crack initiation in Alloy 690 in high temperature water, Curr. Opin. Solid State Mater. Sci.
(2018), https://doi.org/10.1016/j.cossms.2018.02.001
4 T. Moss et al. / Current Opinion in Solid State and Materials Science xxx (2018) xxx–xxx
observed in any of the Alloy 690 specimens after 9720 h while all
the Alloy 600 specimens cracked after 336 h. Sui et al. [20] per-
formed reverse U-bend tests on Alloy 600 and Alloy 690TT in
380 °C hydrogenated steam and observed cracking in two speci-
mens from an Alloy 690 heat that was annealed at low tempera-
ture, while specimens annealed at higher temperature did not
crack after 13,824 h exposure, and most Alloy 600 specimens
cracked within 2578 h. Fig. 1 shows one of the cracked U-bend
samples. Thus, in all reported experiments conducted in constant
strain mode to date, only two reported the occurrence of IGSCC
in Alloy 690 and both were in U-bend samples that underwent
extensive plastic deformation.
2.2. Constant load experiments
Constant load tests have also been performed to assess the SCC
initiation susceptibility of Alloy 690. Yonezawa et al. [8] reported
that no SCC was observed in constant load tests (414–621 MPa)
of Alloy 690 tubing after 7000 h in 360 °C primary water, while
Alloy 600MA specimens cracked after 1100 h. Ogawa et al. [13]
found that none of the Alloy 690TT specimens loaded at 586 MPa
developed cracks in 360 °C primary water, while all Alloy 600 spec-
imens cracked in 340 °C primary water after 10,000 h. Vaillant [17]
showed that constant load tests of a pre-production Alloy 690TT at
684 MPa for 10,900 h and control rod drive mechanism nozzles at
580 MPa for 18,500 h produced no IGSCC in 360 °C PWR primary
water. Boursier et al. [21] conducted constant load tests on an
experimental Alloy 690 with two heat treatments and an industrial
Alloy 690 at 90% of the ultimate tensile strength (UTS) (603–684
MPa) in 360 °C PWR primary water and observed very small cracks
(depth < 10 lm) after approximately 11,000 h. Meaguchi et al. [22]
reported that none of the Alloy 690TT specimens constantly loaded
at various stress levels (300 to 550 MPa) failed after as long as
123,000 h in 360 °C PWR primary water while Alloy 600MA spec-
imens cracked after less than 20,000 h.
To study the effect of notches on SCC initiation, Arioka et al. [23]
conducted constant load tests on blunt notched compact tensile
(BNT) samples made from cold worked Alloy 690TT in PWR pri-
mary water at both 320 °C and 360 °C. These tests produced a
stress intensity factor of 30 MPa
m1/2 at the notch root but yielded
no clear evidence of SCC initiation after over 30,000 h. They [23,24]
also performed similar tests on precracked compact tensile (CT)
Fig. 2. Intergranular cavities found in front of cracks from BNTs. (a) a precursor crack after 5352 h, (b) a shallow crack after 10,049 h and (c) a mature crack after 11,709 h
[26].
Please cite this article in press as: T. Moss et al., Stress corrosion crack initiation in Alloy 690 in high temperature water, Curr. Opin. Solid State Mater. Sci.
(2018), https://doi.org/10.1016/j.cossms.2018.02.001
samples (23–40 MPa
m1/2) and found that the cracks propagated
intergranularly with the formation of grain boundary cavities in
both PWR primary water and inert environment. More recently,
Bruemmer et al. [25,26] studied the SCC initiation behavior of cold
worked Alloy 690TT in 360 °C PWR primary water using round ten-
sile samples and BNTs. Constant load was applied to the tensile
samples (510–700 MPa) and the BNTs were underwent several
cycles of slow loading and rapid unloading (37–27.5 MPa
m1/2). It
was found after approximately 9000 h exposure that the tensile
samples developed extensive intergranular cavities in the interior
of the sample, and some of the cavities were linked to the surface.
The BNTs showed concentrated cavities near the blunt notches and
the cracks are also connected to cavities, as shown in Fig. 2. The
work of Arioka et al. [23,24] and Bruemmer et al. [25,26] suggest
that cavity formation at grain boundaries during constant load
testing occurs at the carbide-matrix interface and may play an
important role in IG crack initiation of Alloy 690. Cold work has
been shown to produce cavities as well, but they are located
between intergranular carbides and were shown to have little
effect on crack propagation [27]. However, the formation of cavi-
ties is only reported to occur in highly cold worked Alloy 690 with
intergranular carbides. It also occurs in an inert environment,
bringing into question whether the process is SCC or creep crack
growth. In particular, it cannot explain the occurrence of cracking
in relatively short term CERT tests as described next.
2.3. Constant extension rate tensile (CERT) experiments
By virtue of dynamic loading, the CERT test is an accelerated test
technique for evaluating the SCC susceptibility of resistant materi-
als like Alloy 690. Angeliu et al. [28,29] studied the creep and IGSCC
susceptibility of several high purity nickel base alloys in both 360 °C
argon and PWR primary water and reported that a laboratory grade
Alloy 690 with ultra-low carbon showed a small amount of IG
cracking in both environments, while Alloys 600 and 690 contain-
ing approximately 0.03% carbon were resistant to IG cracking at a
strain rate of 3  10 7/s. Psaila-Dombrowski et al. [30] studied
the SCC susceptibility of weld composites made from Alloys 152
and 690 in 320 °C simulated primary water at a strain rate of 5 
10 8/s and did not observe any SCC cracks in Alloy 690 after strain-
ing for 2394 h. Vaillant [17] observed that CERT tests at 5  10 8/s
in 360 °C primary water induced intergranular cracks (20–120 lm
 T. Moss et al. / Current Opinion in Solid State and Materials Science xxx (2018) xxx–xxx
Fig. 3. A IGSCC crack on a 20% cold rolled SA Alloy 690 after straining to failure at
1  10 8 s 1 in 360 °C water containing 18 cm3 (STP) H2/kg H2O [32].
deep) on all 17 Alloy 690 heats while no cracking was observed in
reverse U-bend test in the same environment or in CERT tests in
argon. In CERT tests conducted at 5  10 8/s on several heats of
Alloy 690 (MA and TT) in 360 °C primary water, Vaillant [18] also
observed significant intergranular cracking on three Alloy 690
tubes but not in the reverse U-bend tests and demonstrated that
IG cracking correlated well with grain boundary sliding. Boursier
et al. [21] also reported that CERT tests in 360 °C primary water pro-
duced extensive cracking on Alloy 690TT with different surface
states and concluded that high strain rate and strain localization
accelerated the crack growth rate in the slow crack propagation
phase. Was and Teysseyre [31] reported that CERT tests at a nomi-
nal rate of 3  10 7/s in pure, deaerated supercritical water pro-
duced only shallow cracks on Alloy 690 while Alloy 600 showed
more significant intergranular cracking. Tsutsumi and Couvant
[19] evaluated the SCC initiation susceptibility of several heats of
Alloy 690 in 360 °C primary water by CERT tests at 4  10 8/s and
found that only an experimental heat cracked after straining to
20%, and the degree of cracking was affected by the surface condi-
tion. Kuang and Was [32] investigated the SCC initiation behavior
of cold rolled Alloy 690 (solution annealed (SA) and TT conditions)
in 360 °C hydrogenated water CERT tests at 5  10 8/s and 1 
10 8/s, and found that the susceptibility to cracking was highly
dependent on the intergranular carbide density and strain rate.
The shallow IG cracks generated were normally within one grain
domain with an average length <10 lm, as shown in Fig. 3.
Moss and Was [33] studied the oxidation and SCC initiation of
Alloys 600 and 690 (MA) in hydrogenated subcritical and supercrit-
ical water from 320 to 450 °C. Following CERT tests they observed
shallow surface cracks after 7% strain at 5  10 8/s that propagated
along the grain boundary. Recent observations have revealed that
grain boundary cracking occurs within the grain boundary migra-
tion zone that is depleted of Cr and enriched in Ni. Cr2O3 is observed
in the grain boundary ahead of crack tips, and intergranular crack
growth is hindered by chromium carbides. They found that the
stress corrosion crack initiation morphology of pre-strained Alloy
690 tested in CERT was essentially the same in both subcritical
and supercritical water, and that crack depth increased smoothly
with temperature, suggesting that the mechanism does not change
across the transition. From the SCC initiation work on Alloy 690 that
has been conducted thus far, only the CERT test, which dynamically
strains the sample, can consistently initiate cracks on Alloy 690
regardless of the heat or the processing condition.
3. Mechanism of SCC initiation in Alloy 690
The difficulty associated with generating cracks in Alloy 690 has
been an impediment to the study of the mechanisms of SCC initi-
ation. Alloys of similar composition, such as the lower chromium
Please cite this article in press as: T. Moss et al., Stress corrosion crack initiation in Alloy 690 in high temperature water, Curr. Opin. Solid State Mater. Sci.
(2018), https://doi.org/10.1016/j.cossms.2018.02.001
5
nickel based Alloy 600, crack readily in high temperature water,
allowing researchers to study the SCC behavior in depth and postu-
late mechanisms to explain the observed cracking behavior. Thus, a
mechanistic origin for IGSCC crack initiation in Alloy 600 is further
along, as briefly reviewed in the following section.
The most promising model for IGSCC initiation in Alloy 600 is
selective internal oxidation (SIO) [34]. Selective internal oxidation
was first proposed as a mechanism for SCC of Alloy 600 in PWR pri-
mary water by Scott and Le Calvar [35], and was shown to occur by
Newman et al. [36] and Capell and Was. [37]. The internal oxida-
tion mechanism in essence involves weakening of grain boundaries
by selective oxidation on the surface or ahead of crack tips. Selec-
tive intergranular oxidation in Alloy 600 has also been reported to
occur in high temperature steam [38,39]. The oxide embrittles the
grain boundary and allows a crack to propagate upon application of
stress [36,37]. The observed morphology of Alloy 600 SCC is largely
consistent with what would be expected from SIO [40–42]. Four-
nier et al. [41] observed a maximum in the depth of grain boundary
oxidation at a potential that is close proximity to the Ni/NiO
boundary, where a local maximum in SCC growth rate is observed
[43]. Couvant et al. [44] have developed a quantitative model to
predict SCC initiation of Alloy 600 in primary water for the French
nuclear industry based on collected observations of grain boundary
oxidation.
However, SIO cannot be directly applied to Alloy 690. Moss et al.
[45] found that oxidation of Alloy 690 and Alloy 600 in hydro-
genated subcritical and supercritical water resulted in a multi-
layer oxide structure composed of particles of NiO and NiFe2O4
formed by precipitation on the outer surface, and a chromium-
rich inner oxide layer formed by diffusion of oxygen to the
metal-oxide interface. The continuous oxide on Alloy 690 is more
chromium rich than that observed on Alloy 600 and is composed
of an oxide with chromium and iron content similar to that in
the metal matrix but the structure of NiO, hereafter referred to
as MO. The inner oxide on Alloy 690 initially forms by internal oxi-
dation before a protective layer of chromium-rich MO is formed
with Cr2O3 at the metal-oxide interface. Similar penetrative oxides
forms in Alloy 690 grain matrix in simulated PWR primary water
have also been reported by Olszta et al. [46] and Kuang et al.
[47]. Grain boundaries in Alloy 690 act as fast diffusion paths for
chromium to form a protective Cr2O3 layer at the surface, prevent-
ing intergranular oxidation from occurring not only in high tem-
perature water [45,46], but also in hydrogenated steam [48]. A
Cr-depleted grain boundary migration zone normally forms
beneath the surface due to the outward diffusion of Cr along the
grain boundary, as shown in Fig. 4. Without forming an intergran-
ular oxide, which is a prerequisite for SIO, Alloy 690 is highly resis-
tant to cracking. Interestingly, Kuang et al. [49] recently reported
that twin boundaries in Alloy 690 are susceptible to intergranular
oxidation but resistant to Cr diffusion and grain boundary migra-
tion after exposure in simulated PWR primary water, which seems
Fig. 4. Scanning electron microscopy (SEM) micrograph illustrating the cross-
section surface and near-surface grain boundary of Alloy 690MA + 20%CR material
exposed to 360 °C simulated PWR primary water for 1000 h [46].
6 T. Moss et al. / Current Opinion in Solid State and Materials Science xxx (2018) xxx–xxx

Fig. 5. Schematic of the proposed SCC initiation mechanism of Alloy 690 subjected to dynamic stress; surface oxidation accompanied by grain boundary chromium depletion
and grain boundary migration, and internal oxidation away from the grain boundary (a–c), rupture and repair of oxide by dynamic straining (d–f), and crack initiation along
the boundary when a Cr2O3 is no longer able to form (g–i).

inconsistent with their higher SCC resistance compared to random
high angle boundaries. The effects of grain boundary structure on
the intergranular degradation behavior will be addressed in
another work as this paper focuses on random high angle bound-
aries. The following details the proposed SCC initiation mechanism
of random high angle boundaries in Alloy 690 and how each stage
of the mechanism is supported by the oxidation and crack initia-
tion morphology observed in the literature.
Intergranular stress corrosion crack initiation in Alloy 690 is
proposed to occur in three stages: an oxidation stage in which a
protective film of Cr2O3 is formed on the surface over the grain
boundaries, an incubation stage in which successive cycles of oxide
film rupture and repair depletes the grain boundary of chromium,
and a nucleation stage in which the chromium depleted grain
boundary is no longer able to support formation of a protective
chromium oxide layer, exposing the grain boundary to the water
environment and subsequent formation and rupture of oxides
down the grain boundary.
Fig. 5a shows a schematic of a high angle grain boundary in
Alloy 690 prior to exposure in water. Oxidation proceeds first by
formation of a protective Cr2O3 layer on the surface above the grain
boundary as shown in Fig. 5b. Chromium is supplied by diffusion
along the grain boundary causing chromium depletion in the
matrix adjacent to the boundary. Grain boundary migration
accompanies chromium depletion. Away from the grain boundary
region, the surface is unable to form a protective oxide layer, lead-
ing to internal oxidation as shown schematically in Fig. 5c. This
internal oxidation region is much thinner at the grain boundary
since the boundary is able to supply Cr to form a compact oxide
above it.

Fig. 6. Schematic of oxidation behavior observed on Alloy 690 in hydrogenated subcritical and supercritical water [45].

Please cite this article in press as: T. Moss et al., Stress corrosion crack initiation in Alloy 690 in high temperature water, Curr. Opin. Solid State Mater. Sci.
(2018), https://doi.org/10.1016/j.cossms.2018.02.001
 T. Moss et al. / Current Opinion in Solid State and Materials Science xxx (2018) xxx–xxx
Due to its brittle nature, the Cr2O3 layer ruptures when strain is
applied and the surface re-passivates by further diffusion of chro-
mium along the grain boundary, Fig. 5d and e. Successive incre-
ments of strain further rupture the oxide layer, which then
passivates by more chromium diffusion to the surface as shown
in Fig. 5f. The introduction of strain is important and it distinguishes
CERT tests from constant deflection or constant load. However,
creep can also introduce significant amounts of dynamic strain.
After repeated cycles of oxide fracture followed by repair, the
grain boundary becomes further depleted in chromium and
migrates further from its original position. At some point the grain
boundary region is no longer able to supply enough chromium to
form a protective surface film, exposing the grain boundary to
the water environment, resulting in grain boundary oxidation
and subsequent crack nucleation by fracture along the oxidized
boundary, shown schematically in Fig. 5g–i. The following sections
provide additional observations to support the key features of the
proposed mechanism.
3.1. Oxidation
Electropolished coupons exposed in hydrogenated 360 °C and
400 °C supercritical water were used to study the oxidation behav-
ior of Alloy 690 [45]; a schematic of the oxidation observed is
shown in Fig. 6. Internal oxidation occurred in the matrix and
consisted of Cr2O3 platelets and NiO structured chromium-rich
oxide penetrating into the metal. There was no internal oxide
observed near the grain boundary, instead a thin layer of Cr2O3
formed on the surface. Grain boundary migration was also
observed in the sub-surface grain boundary as shown in Fig. 7. It
is directly induced by Cr diffusion and always accompanied by a
Cr depleted zone. Scanning auger electron microscopy (SAM)
measurement [45] shows that chromium was depleted from the
Fig. 7. Grain boundary migration and chromium depletion observed in SEM at 5
keV in cross section of Alloy 690 exposed at 400 °C for 250 h. A lighter contrast
indicated chromium depletion which was confirmed by scanning auger microscopy
and the grain boundary location was revealed by sputtering with 2 keV argon at a
current of 1 lA [45].
Please cite this article in press as: T. Moss et al., Stress corrosion crack initiation in Alloy 690 in high temperature water, Curr. Opin. Solid State Mater. Sci.
(2018), https://doi.org/10.1016/j.cossms.2018.02.001
7
matrix composition of 31 at.% to a value of 20 at.% in the migrated
region at a distance of 200 nm below the surface. The Cr concentra-
tion of the migration zone was depleted to 10 at.% according to
the measurement of Olszta et al. by atom probe tomography
(APT) [46]. Energy dispersive spectroscopy (EDS) measurement
by Kuang et al. [50] also showed that the Cr content in the migra-
tion zone dropped to 13–17 at.%. Grain boundary migration has
been reported to occur in alloy 600 after exposure in high temper-
ature hydrogenated steam [38,39]. Carbide precipitation may also
induce grain boundary migration in alloy 690 when the intergran-
ular carbide density is high [51]. However, the Cr depletion and
grain boundary migration presented in this work were not due to
carbide precipitation as either the carbide density was low
[45,46] or no carbides were formed [50]. These morphologies sug-
gest that chromium is preferentially diffusing to the surface along
the grain boundary to form a protective layer of Cr2O3.
These oxide structures have been observed by several other
researchers on highly polished Alloy 690 and in the initial stages
of Alloy 600 oxidation. Olszta et al. [46] used a combination of
TEM and atom probe tomography to show that the surface grain
boundary oxide was composed of Cr2O3 on coupons of Alloy 690
exposed to PWR primary water. Olszta et al. [52] also observed
internal oxidation in the matrix and in the wake of the crack. They
characterized the internal oxide layer as consisting of discrete
Cr2O3 platelets surrounded by nanocrystalline NiO structured
chromium rich oxide. More detailed work by Kuang et al. [47]
revealed that the internal oxide is composed of penetrative Cr2O3
along the widely-spaced lattice planes of matrix and chromium
rich spinel. Bertali et al. [53] observed grain boundary migration
and chromium depletion in Alloy 600 exposed to 480 °C
hydrogenated steam for 120 h. This morphology suggests that ini-
tially the oxidation of Alloy 690 and Alloy 600 are governed by
similar processes. However, the similarity breaks down upon fur-
ther exposure where grain boundary oxidation is observed in Alloy
600 while none is observed in Alloy 690. Bertali et al. [53] sug-
gested that grain boundary migration is a precursor to the fracture
of the oxide formed above Alloy 600 grain boundaries, as it leaves a
chromium depleted grain boundary that is susceptible to oxida-
tion. This morphology was not observed in Alloy 690, possibly
because there is enough chromium to passivate the surface above
the grain boundary with a more protective layer of Cr2O3.
3.2. Crack incubation
As described earlier, laboratory tests to study crack initiation
have shown that Alloy 690 is very resistant to cracking in constant
strain and constant load modes [1,6–8,10–19,22]. If a constant load
or deflection is applied after an oxide layer is formed, it can cause
rupture of the oxide layer, which is then passivated with an oxide
grown on the already elastically strained metal and does not fur-
ther stress the oxide. So there is no driving force for subsequent
crack initiation, which explains the paucity of observations of
cracking in these types of tests. Only experiments in which the
samples were dynamically strained [17–19,21,31–33] consistently
show IG crack initiation. Dynamic straining is necessary to repeat-
edly fracture the protective Cr2O3 oxide above grain boundaries,
further depleting the grain boundary of chromium. In fact, the
absence of crack initiation in samples subjected to a constant load
is evidence of the incubation behavior proposed schematically in
Fig. 5d–f.
The role of grain boundary migration on surface passivation by
Cr2O3 is not well understood. If grain boundary migration is the
source for chromium diffusion from the bulk to reach the surface
by way of the grain boundary, there should be no breakdown in
the passivation of the surface as long as there is room for the grain
boundary to migrate. However, the grain boundary migration may
8 T. Moss et al. / Current Opinion in Solid State and Materials Science xxx (2018) xxx–xxx
Fig. 8. Scanning transmission electron microscope dark field image of an oxidized
grain boundary in solution annealed Alloy 690 strained to 1.78% at 1  10 8 s 1 in
360 °C pure water containing 18 cc H2/kg H2O.
Fig. 9. SEM-FIB (5 keV) cross section of a crack in 20% pre-strained Alloy 690
strained to 7% at 5  10 8 s 1 in 360 °C hydrogenated water. Dark contrast
(chromium rich) oxide and chromium depletion was observed beyond the crack
tip [33].
be simply a consequence of chromium diffusion in the grain bound-
ary. If this is the case, passivation could break down after the grain
boundary is depleted to a critical depth at which Cr2O3 can no
longer be formed quickly enough to prevent grain boundary
oxidation.
3.3. Crack nucleation
After the grain boundary is sufficiently depleted of chromium, a
protective oxide layer is no longer able to reform upon cracking,
and grain boundary oxidation occurs. Fig. 8 shows an example of
an uncracked, but oxidized grain boundary in solution annealed
Alloy 690 that has been strained to 1.78 at.% 1  10 8 s 1 in 360
°C hydrogenated water. Fujii et al. [54] performed micro tensile
tests on individual oxidized grain boundaries of Alloy 600 and
found that the stress required to cause fracture of the grain bound-
ary was as low as 180 MPa, whereas unoxidized grain boundaries
did not fracture at 1000 MPa. Similarly, the grain boundary
strength of Alloy 690 would decrease as the intergranular oxida-
tion occurs and a crack nucleates when the oxide develops to a cer-
tain depth.
Formation of Cr2O3 in grain boundaries ahead of the crack tip,
and intergranular oxidation of what appeared to be intact grain
boundaries from CERT testing provide further support for this pro-
cess. Fig. 9 shows grain boundary oxidation ahead of a crack that
Please cite this article in press as: T. Moss et al., Stress corrosion crack initiation in Alloy 690 in high temperature water, Curr. Opin. Solid State Mater. Sci.
(2018), https://doi.org/10.1016/j.cossms.2018.02.001
nucleated in 20% cold worked Alloy 690 after CERT testing in
hydrogenated water at 360 °C. Characterization of the crack [33]
showed that oxidation extended beyond the crack tip, similar to
observations in Alloy 600. The crack is filled with NiO and
chromium-rich oxide on the crack walls. Because NiO fills open
cracks, the location of the crack tip is defined by the depth of pen-
etration of NiO. Cr2O3 is observed beyond the crack tip with evi-
dence of chromium depletion extending deeper along the grain
boundary. These combined observations show that grain boundary
oxidation of Alloy 690 is possible and could weaken grain bound-
aries sufficiently such that initiation occurs.
3.4. Other factors affecting IGSCC initiation
Creep damage has been observed in Alloy 690 and is always a
factor to consider when evaluating SCC of components exposed
to high temperature for long times. As reviewed earlier, Arioka
et al. [23,24] observed extensive intergranular cavities in the inte-
rior of compact tension samples made from cold worked Alloy
690TT which had been constantly loaded in both PWR primary
water and an inert environment for over 30,000 h. Similarly,
Bruemmer et al. [25,26] examined blunt notch compact tension
specimens of 31% cold rolled Alloy 690 exposed to low frequency
cyclic loading and observed numerous cracks ahead of the notch
with fracture surfaces suggesting void nucleation. Additionally,
there was no oxide present on the crack walls, suggesting that they
were isolated to the bulk and did not connect to the surface. These
works provide evidence that significant creep rates and creep dam-
age are possible in Alloy 690 if the stresses are high enough and the
material is sufficiently abused.
The mechanism for SCC initiation of Alloy 690 proposed herein
suggests that a dynamic strain is required for crack initiation to
occur. Moss and Was [33] used CERT to achieve a dynamic strain
but creep strain can also serve this purpose. The amount of strain
needed to fracture the protective Cr2O3 layer is not known, but it
should vary with the oxide thickness and therefore the strain rate
(via creep or CERT). This would suggest that the creep deformation
during constant load experiments could eventually cause initiation
if exposed for enough time. Moss and Was [55] determined factors
of improvement for Alloy 690 over Alloy 600 by comparing the
densities of cracks from CERT experiments on each alloy. At 360
°C the factor of improvement in the nucleation of SCC in Alloy
690 over Alloy 600 was approximately 195X. Richey et al. [56]
observed SCC initiation of 25% cold worked Alloy 600 after 1000
h of exposure. These combined results would suggest that 25% cold
worked Alloy 690 would initiate after 195,000 h (22 years) of
exposure at constant load. This would be difficult to achieve in a
laboratory, but is within the time scale for reactor conditions. Nev-
ertheless, the load on a component could not be sustained over
that timespan due to stress relaxation from creep.
Carbides on grain boundaries can have complex interactions
with deformation and oxidation to influence SCC initiation behav-
ior. Moss and Was [57], through cross section examination,
showed that carbides can promote formation of a protective oxide
layer that prevents internal oxidation of the Alloy 690 matrix. Con-
sistently, Bertali et al. [53] showed that chromium carbides can be
consumed or oxidized to promote a thick external chromium rich
oxide layer in Alloy 600 exposed to 480 °C steam. The work from
Langelier et al. [58] also suggested that Cr carbides slow oxide
growth down the boundary. The oxidation results, according to
the proposed SCC initiation mechanism, suggest that the thicker
chromium rich layer above grain boundaries and larger supply of
chromium would inhibit initiation of SCC. Support for this mecha-
nism comes from the observation by Moss and Was [33] that sur-
face cracks in Alloy 690 arrested at chromium carbides and that
cracks were shallower when carbides were present.
 T. Moss et al. / Current Opinion in Solid State and Materials Science xxx (2018) xxx–xxx
4. Conclusions
While the database on crack initiation of Alloy 690 is sparse,
only dynamic straining experiments consistently generate SCC
cracks in pressurized water reactor primary water. Stress relax-
ation in constant deflection tests and lack of a means of rupturing
the oxide film in constant load tests are the principle reasons for
the difficulty of initiating cracks in these tests. Analysis of the data
in conjunction with that of the much more susceptible Alloy 600
supports the following mechanism of SCC initiation in hydro-
genated water. The crack initiation process is composed of three
stages; an oxidation stage in which a protective film of Cr2O3 is
formed on the surface over the grain boundaries, an incubation
stage in which successive cycles of oxide film rupture and repair
depletes the grain boundary of chromium, and a nucleation stage
in which the chromium depleted grain boundary is no longer able
to support formation of a protective chromium oxide layer, expos-
ing the grain boundary to the water environment and subsequent
formation and rupture of oxides down the grain boundary. Each
stage of the initiation process is well substantiated by the experi-
mentally observed oxidation and crack initiation behavior of Alloy
690.
Acknowledgements
The authors would like to acknowledge support provided by the
Electric Power Research Institute under contract EP-P35621.
Appendix A. Supplementary material
Supplementary data associated with this article can be found, in
the online version, at https://doi.org/10.1016/j.cossms.2018.02.
001.
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