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Koji Fukuya
To cite this article: Koji Fukuya (2013) Current understanding of radiation-induced degradation
in light water reactor structural materials, Journal of Nuclear Science and Technology, 50:3,
213-254, DOI: 10.1080/00223131.2013.772448
Current phenomenological knowledge and understanding of mechanisms are reviewed for radiation em-
brittlement of reactor pressure vessel low alloy steels and irradiation assisted stress corrosion cracking of
core internals of stainless steels. Accumulated test data of irradiated materials in light water reactors and
microscopic analyses by using state-of-the-art techniques such as a three-dimensional atom probe and elec-
tron backscatter diffraction have significantly increased knowledge about microstructural features. Charac-
teristics of solute clusters and deformation microstructures and their contributions to macroscopic material
property changes have been clarified to a large extent, which provide keys to understand in the degradation
mechanisms. However, there are still fundamental research issues that merit study for long-term operation
of reactors that requires reliable quantitative prediction of radiation-induced degradation of component
materials in low-dose rate high-dose conditions.
Keywords: light water reactor; neutron irradiation; radiation embrittlement; IASCC; low-alloy steel;
stainless steels
∗
Email: fukuya@inss.co.jp
C 2013 Atomic Energy Society of Japan. All rights reserved.
214 K. Fukuya
Δ
from data of C–Mn steels in gas-cooled reactors over a
wide temperature range [27]. Similar linear irradiation
temperature dependence was also observed in weld met-
als and A533B steels irradiated in MTRs [25,28]. Tem-
perature dependence was clearer for higher Cu content,
while it seemed to be relatively small at temperatures
lower than 300◦ C for high-Cu steels.
Compton scattering, pair production and the photoelec- features having dominant roles in radiation embrittle-
tric effect [35]. It was confirmed that electron irradia- ment have been recognized as Cu precipitates and ex-
tion with energies of several MeV causes hardening in tended secondary defects such as microvoids in the 1980s
low-alloy steels [36–38]. For thermal neutron effects, the [47]. Odette and Lucas [1] have categorized microstruc-
contributions to displacement damage production and tural features causing hardening and embrittlement and
additional damage production through the nuclear reac- noted Cu-rich precipitates (CRPs) and matrix damage
tion of boron were discussed. It was shown that thermal (MD) as major features. The Mn–Ni precipitate (MNP)
neutrons were almost two times more effective for caus- was proposed as the late blooming phase, which was
ing radiation embrittlement than fast neutrons at the thought to be thermodynamically formed after long-
same dpa [39,40]. The contributions of thermal flux and time irradiation of low-Cu, high-Ni steels. MD is divided
gamma rays to radiation embrittlement of pressure ves- into two types: stable MD (SMD) such as interstitial
sel steels were assessed for the HFIR and LWRs consid- clusters and unstable MD (UMD) such as small vacancy
ering the neutron and gamma-ray spectrum, core struc- clusters that may redissolve at irradiation temperatures
ture and water gap between the pressure vessel and core [48], although the exact nature of MD has not been
[34,41]. The enhanced embrittlement observed in the identified. Radiation-enhanced segregation at GBs and
HFIR was attributed to additional damage induced by its influence on intergranular fracture were discussed in
high-flux gamma rays [34]. On the other hand, the con- the 1990s [49]. Further improvement of analysis tech-
tributions of thermal neutrons and gamma rays to radi- niques such as local electrode atom probe and PA with
ation embrittlement in LWRs were estimated to be neg- coincidence Doppler broadening (PA-CDB) [50] and ap-
ligible. The displacement damage induced by thermal plication of these techniques to surveillance specimens
neutrons and gamma rays was less than ∼5% in pressure have brought detailed information on microstructural
vessels in BWRs and PWRs. In advanced BWRs (AB- evolution.
WRs), a large contribution (∼50%) from gamma rays At present, it is widely believed that there are three
was expected because of the larger water gap between the major microstructural features causing embrittlement:
core and pressure vessel. However, the flux in ABWRs is solute precipitates or clusters, MD and GB segregation.
very low and would cause negligible embrittlement [41]. The first two features cause embrittlement through ma-
terial hardening. The MD is a concept including all mi-
Tensile stress. Stress during irradiation is one of the crostructural features other than CRPs. However, recent
potential factors that can cause changes in radiation em- 3DAP analyses show that solute aggregates containing
brittlement. Stress effects are an issue related to the dif- Fe, Mn, Ni, Si, Cu and P are commonly formed in com-
ference between surveillance irradiation without stress mercial and model low-alloy steels regardless of the Cu
and pressure vessels under static tensile stress during op- content. The aggregates exhibit diffused images and have
eration. Data collected in the 1960s showed that the ten- a wide range of Cu fractions, and are now often called
sile stress had no effects or a suppressing effect on the ‘clusters’, rather than ‘precipitates’, in the recent liter-
transition temperature shift [42–44] For example, no ef- ature. In this paper, thus, ‘solute cluster’ is used as a
fects for a stress of 75% yield strength were observed in general term. ‘Cu-rich cluster’ is used for clusters with
A350 (0.08%Cu) and A302 (0.15%Cu) steels irradiated high Cu fraction formed in high-Cu steels and ‘Mn–Ni–
to (2–3) × 1019 n/cm2 [42], while the transition temper- Si cluster’ for clusters containing Mn, Ni and Si atoms
ature shift was smaller for a tensile stress of 20% yield with very low Cu fraction formed in low-Cu steels. Mn–
strength in A302B steels irradiated to 5 × 1019 n/cm2 Ni–Si clusters are not included as MD described in this
[44]. In order to understand the mechanisms of stress paper, although their clusters with no or very low Cu
effects, heavy ion irradiation experiments under stress fractions are sometimes treated as MD in the literature.
were recently conducted on A533B steels [45,46]. The
results showed that the tensile stress reduced radiation
hardening and produced smaller solute clusters. 3.2.1. Solute clusters
Recent observations in surveillance materials. Re-
cent 3DAP observations of surveillance materials have
3.2. Microstructural evolution and embrittlement provided key data for understanding microstructural
mechanisms evolution in actual vessel materials under operating con-
Understanding of radiation embrittlement mech- ditions. In surveillance specimens (16MND5 steels with
anisms is directly connected with understanding mi- 0.09 and 0.044%Cu) irradiated in French PWRs at 2
crostructural features formed under irradiation and × 1011 n/cm2 /s, fine clusters (3–4 nm in diameter) were
their role in hardening and the transition temperature detected and the cluster density increased with fluence
shift. Application of advanced microanalysis techniques up to 1.7 × 1020 n/cm2 [51,52]. The averaged compo-
such as small-angle neutron scattering (SANS), 3DAP, sition in the 0.044%Cu steel was Fe–6Mn–10Ni–8Si in
positron annihilation (PA) and transmission electron at% and did not change with fluence up to 7.6 × 1019
microscopy (TEM) has provided significant improve- n/cm2 . The clusters were uniformly formed in the ma-
ment for mechanistic understanding [3]. Microstructural terial although some clusters were present along line
218 K. Fukuya
loops, mostly the interstitial type, are formed as a stable (1) P segregation occurs both during post-weld heat
microstructural feature in commercial steels regardless treatment of the fabrication process and dur-
of the material composition and irradiation conditions. ing service at operation temperatures and under
The dislocation loops have a definite but smaller contri- neutron irradiation. P segregation at GBs dur-
bution to radiation hardening than solute clusters. The ing thermal ageing is treated as thermal equilib-
detailed nature of vacancy-type MD is still unknown in rium segregation. Model estimation shows that
commercial steels. From current data by PA measure- the P concentration at GBs remains almost un-
ments, it is reasonable to conclude that vacancy clus- changed due to thermal aging alone for 60 years
ters containing more than one or two vacancies are not at around 300◦ C in commercial low-alloy steels
formed, which make a definite contribution to harden- [49,115].
ing. However, it is necessary to carefully consider inter- (2) Neutron irradiation significantly enhances P seg-
actions between point defects and solute atoms. It is ev- regation at GBs. This was confirmed by a sample
ident that Cu-rich clusters in high-Cu model alloys are of data in irradiated commercial steels [113,116–
formed in a manner that Cu atoms cover the inner sur- 121] and model alloys [122,123]. The enhance-
face of microvoids [84,105]. Some fraction of vacancies ment is thought to be caused by accelerating
must be assumed for explaining SANS data (mass den- thermal segregation due to radiation-enhanced
sity of the clusters) of the clusters formed in commer- diffusion (vacancy dragging) and also radiation-
cial steels [3]. These facts suggest that vacancies are con- induced diffusion (mobile P-interstitial dumb-
tained in the clusters and involved in cluster formation bells) [114,124–126]. P segregation at GBs be-
processes. comes higher for higher P content. In com-
Dislocation loops can be sinks for point defects. mercial Mn–Mo–Ni steels, P segregation seems
Thus, dislocation loops are expected to be decorated to saturate at high fluences and the saturation
with segregated solute atoms such as Ni, Si and Mn level seems to be about 0.2 monolayer coverage
and therefore can act as nucleation sites of clusters. En- at 1 × 1020 n/cm2 in steels containing P less
hanced formation of both dislocation loops and solute than <0.02%. P segregation in C–Mn steels and
clusters was observed along pre-existing line disloca- VVER-type vessel steels is found to be higher
tions. Unfortunately, no analytical methods are available than that in Mn–Mo–Ni steels [114] although
which can directly identify the state and distribution of the reason is unclear.
point defects and solute atoms at the same time. Detailed (3) Segregation of other elements, C, Ni, Mn, Si, Mo
correspondence of solute clusters with dislocation loops and Cu, is also known to exist at GBs both be-
or vacancy clusters is still unknown. Vacancy clusters, if fore and after irradiation in commercial steels
they exist as UMD, might act as point defect sinks and [57,121]. Irradiation enhances segregation of Ni,
change the concentration of point defects, resulting in a Mn and Si at GBs [52,57,121]. C desegregation
change in the diffusion coefficient of solute atoms and during irradiation has been discussed since P and
nucleation of solute clusters. Furthermore, the interre- C are competitive segregants in steels and C en-
lationship between MD and solute clusters might relate hances the GB cohesion [57,121–123]. The in-
with hardening processes. In the case that enhanced for- crease in P coverage is expected to cause a de-
mation of dislocation loops and solute clusters near pre- crease in C coverage. However, in commercial
existing line dislocations is dominant, source hardening A533B steels which typically contains less than
might be a dominant hardening process. Continuing re- 0.03% P, changes in C concentration at GBs due
search efforts to identify MD and its relation to solute to irradiation are so small that the trend is not
cluster evolution and hardening are essential to under- clear [121]. The influence of segregation of other
stand embrittlement mechanisms. elements on the irradiated mechanical behavior
has not been well examined.
(4) It is well established that high-level P segre-
3.2.3. Grain boundary segregation gation at GBs enhances intergranular fracture
GB embrittlement due to P segregation was initially and transition temperature shift in thermally
examined for understating effects of long-term thermal aged steels. In such cases, the transition tem-
ageing on embrittlement of weld HAZ [112]. Since in- perature shift is proportional to the P segrega-
tergranular fracture was found in an irradiated high-P tion level [112,116]. Recent studies carefully ex-
C–Mn weld [112], the influence of irradiation on P segre- amined the correlation between transition tem-
gation and GB embrittlement has been studied. Knowl- perature shift, radiation-induced hardening and
edge on the segregation behavior and its influence on P segregation in A533B-type steels containing
embrittlement, obtained until the early 2000s, has been a wide range of P contents (0.008–0.57%P),
summarized in the literature [49,114], and new studies and found that P segregation affects the tran-
have increased understanding of the critical condition sition temperature shift only when the P con-
for embrittlement due to P segregation. Major points are centration at GBs exceeds approximately 0.3
summarized below. monolayer coverage [120,121]. Figure 12 shows
224 K. Fukuya
(2) Influence of specimen size has long been one induced by cooling rates [165]. However, frac-
of the essential issues for determining fracture ture toughness distribution in pressure vessels of
toughness. For the master curve application, a decommissioned VVER, which had been an-
IAEA coordinated programs extensively exam- nealed after 13 years in operation, showed no
ined influences of specimen type and size (CT vs. clear trend with large scatter, although the rea-
pre-cracked Charpy V-notch), pre-crack depth son for the observed large scatter was unclear
and strain rate [155,156]. These factors affect the [166].
master curve reference temperature T0 and bring (5) Effects of warm pre-stress (WPS) on fracture
a bias to T0 determination compared to data toughness have been extensively studied in Eu-
from large CT specimens. Considering actual ropean countries. This is to establish a reason-
practice for determining fracture toughness from able margin for PTS evaluation since WPS is
surveillance specimens, applicability of 10 mm expected to increase fracture toughness at low
CT and 3.3 mm precracked Charpy V-notch temperatures. A sample of fracture toughness
specimens was examined [157–159]. The fracture data have been reported after various stress–
toughness obtained with 10 mm CT specimens temperature procedures, for example, load, cool-
was almost comparable to those with full-sized ing and fracture, and load, unload, cooling and
pre-cracked Charpy V-notch specimens in A508 fracture [167,168]. It was confirmed that WPS
surveillance material irradiated up to 3.8 × 1019 effects appear in unirradiated pressure vessel
n/cm2 [157]. steels. The WPS effect was also confirmed in irra-
(3) Some determination methods of fracture tough- diated steels. The increase
√ of fracture toughness
√
ness master curves from surveillance Charpy at 90◦ C from 100 MPa m to 238 MPa m af-
data have been proposed. One method calculates ter WPS (160◦ C) was observed in high-Cu weld
the temperature dependence of fracture tough- (0.22%Cu) irradiated to 1.1 × 1019 n/cm2 [169].
ness from Charpy absorbed energy data using The increase of fracture toughness after WPS
material properties such as work hardening co- was also reported in 1/2TCT surveillance spec-
efficient and tensile strength [160]. Another de- imens irradiated to 4.6 × 1019 n/cm2 [170].
termines the reference temperature of the mas-
ter curve of Charpy absorbed energy. Although
this method does not determine the tempera- 3.3.4. Multiscale modeling
ture dependence of fracture toughness, the ref- A large number of computer simulation works on
erence temperature of Charpy absorbed energy radiation embrittlement have been conducted and have
is almost of the same value as T0 obtained contributed to understanding the mechanisms of em-
from fracture toughness tests [161,162]. Further brittlement and fracture mechanics. Multiscale model-
studies are needed to assess the applicability of ing is a combination of physical and mechanical mod-
these methods to fracture toughness evaluation eling in various time and space scales. It consists of
of RPVs. modeling, for example, damage production processes
(4) The scatter of the fracture toughness value is by molecular dynamics calculations, diffusion processes
one of the key issues for both probabilistic and by ab initio calculations, clustering processes by kinetic
deterministic evaluation of structural integrity. Monte Carlo calculations, dislocation interactions by
The scatter initiates from microscopic variation dislocation dynamics calculations, and macroscopic de-
such as carbide distribution even in a homoge- formation and fracture processes by crystalline plastic-
neous material, and also from macroscopic vari- ity calculations. In European countries, a multiscale ap-
ation of microstructure and material properties proach was organized as the PERFECT project and has
within the volume of a pressure vessel. Influence been followed by the PERFORM60 project [171–173].
of macroscopic variation was recently reported The major results of the PERFECT project were sum-
using full size vessel products and trepans from marized in a special publication [174].
pressure vessels of decommissioned plants. In- The multiscale approaches provide both basic
fluence of macro-segregation in ingots on frac- knowledge of microstructural evolution and microme-
ture toughness was examined in French A508 chanics of fracture, although current modeling has not
forged rings and the scatter of surveillance tran- yet provided a prediction of fracture toughness changes
sition temperature shifts and some high shifts which is applicable to actual reactor evaluation. Some
data were explained by C macro-segregation in examples of knowledge that has come from using the
ingots [163,164]. Other studies showed that the approaches are: the interaction and diffusion energies
master curve reference temperature at the sur- of point defects and various solutes [175] and the dis-
face of unirradiated actual VVER440 pressure location pinning strength of various clusters [176]. For
vessel steels was 35–70◦ C lower than those of micromechanics, several models for crack initiation at
the mid-thickness region and that this differ- carbides and cleavage propagation were proposed to
ence came from the microstructural difference explain the shape and shift of the fracture toughness
Journal of Nuclear Science and Technology, Volume 50, No. 3, March 2013 227
curve [177–181]. These efforts are still of essential im- The fundamental cause of IASCC has been con-
portance to establish the physical basis of embrittlement sidered to be irradiation-induced changes in materi-
prediction. als. Neutron irradiation causes displacement damage
in materials, which consequently causes changes in mi-
crostructure, microchemistry and macroscopic proper-
ties. Neutron irradiation also causes changes in stress–
3.4. Summary of radiation embrittlement strain states through irradiation creep and stress relax-
Knowledge of microstructural features and under- ation. These changes are accumulated as the fluence in-
standing of mechanisms on radiation embrittlement creases. Furthermore, neutron irradiation together with
have been significantly improved by recent development gamma-ray irradiation causes radiolysis in water. The
of nano-scale analytical techniques such as 3DAP and radiolysis produces various active chemical products
PA. The formation of solute clusters of Cu, Mn, Ni causing ECP change in water containing DO, while
and Si, and dislocation loops has been confirmed in the products disappear through reactions with hydro-
low-alloy steels irrespective of the material composition gen causing no ECP change in water containing DH.
and irradiation condition. These features are now be- IASCC behavior has long been studied for two differ-
lieved to be dominant for radiation hardening and em- ent water conditions. In this paper, the following terms
brittlement, and are incorporated into recently devel- are used for water conditions: BWR water conditions
oped mechanism-guided embrittlement predictions used [288◦ C pure water containing DO, known as normal
in some countries, which give much better correlation water chemistry (NWC), and hydrogen water chemistry
with surveillance data than previous empirical correla- (HWC) adding hydrogen to NWC]; and PWR water con-
tions. However, there are still unresolved issues to ob- ditions [290–360◦ C water containing 500–1500 ppm B
tain a sound understanding of radiation embrittlement as H2 BO3 , ∼2 ppm Li as LiOH and ∼30 cc H2 /kgH2 O
at higher fluences in long-term operations. The issues in- (∼2.7 ppmDH)]
clude identifying microstructural features that are dom- IASCC data are obtained by conducting reactor
inant at high fluences for various material compositions irradiation in LWRs and MTRs followed by post-
and neutron fluxes, and formation and development irradiation examinations (PIEs) using hot cell facility
processes of the features. As a physical basis, studies on and involve large costs and long times; thus, system-
the interaction between point defects and solute atoms, atic databases are still scarce. However, in the past two
the interrelationship between MD and solute clusters, decades, initiation and growth data at high fluences have
and the contribution of each microstructural feature become available. In this section, current phenomeno-
to embrittlement are essential. Especially, the relation- logical knowledge on IASCC behavior is briefly summa-
ship between dislocation loops and Mn–Ni–Si clusters is rized. In Sections 4.2, 4.3 and 4.4, radiation effects on
important to understand the nucleation process and materials, water and stress–strain, and mechanisms are
high-dose behavior of solute clusters. The acquired discussed.
knowledge will be properly modeled and incorporated
into embrittlement prediction or correlation.
4.1.1. Susceptibility
IASCC susceptibility of LWR-irradiated materials
has been examined mostly using slow strain rate ten-
4. IASCC of core structural materials
sile (SSRT) tests. This method has provided knowledge
4.1. Radiation effects on SCC on influences of various parameters although the sus-
IASCC is an intergranular-type SCC (IGSCC) that ceptibility means only the qualitative relative easiness
occurs under the radiation environment in the core of of IASCC occurrence. Major points have been summa-
LWRs. The susceptibility, initiation and propagation rized in the literature [4–7]. IASCC susceptibility ap-
of IGSCC are enhanced by neutron irradiation. Fail- pears at ∼1 dpa in both oxygenated BWR water and hy-
ures of core structural SS components were found in drogenated PWR water conditions. This dose has been
both BWRs and PWRs [6]. The IASCC susceptibil- often recognized as the threshold dose for IASCC oc-
ity is mostly determined by the following primary fac- currence, but it does not mean substantial immunity to
tors: neutron fluence of materials, electrochemical cor- IASCC at doses lower than 1 dpa. The factors that en-
rosion potential (ECP) in water and applied tensile stress hance IASCC susceptibility are: higher DO, higher ECP,
level. Many secondary factors are also known to affect and lower strain rate in BWR water conditions [182];
IASCC: material conditions including alloy type, com- and lower DH, higher water temperature and lower
position and cold work (CW); irradiation conditions strain rate in PWR water conditions [183–185]. With re-
such as temperature, flux and spectrum; environmental spect to material factors, many elements have been ex-
conditions such as temperature, water purity and dis- amined by using SSRT tests and swelling tube tests. In
solved oxygen (DO) and dissolved hydrogen (DH) con- BWR water conditions, IASCC susceptibility was sup-
centrations; and stress–strain conditions such as strain pressed by the addition of Mo, Cr, C, N, Hf and Ti, and
rate. enhanced by the addition of Si, P, Nb and Ti [186–190].
228 K. Fukuya
Ni–Si clusters [232] and carbides [234] were observed in Tensile property changes originate from the elastic
irradiated SSs. However, the generality of these features interaction of moving dislocations and microstructural
is unclear. features such as dislocation loops. The increase in yield
strength (σ y ) has a good correlation with the evolu-
tion of microstructural featurespredicted by the barrier
4.2.2. Mechanical properties hardening model [235]: σ y ∝ (Ni × di )2 , where Ni
Tensile properties. The formation of radiation- and di are the number density and diameter of the ith
induced microstructural features consequently causes microstructural feature, respectively. This relation was
changes in stress–strain response under tensile loading. confirmed in LWR-irradiated SSs assuming the proper
These include: hardening, increase in yield strength and hardening coefficient for each feature [218–220,223,
tensile strength, and decrease in ductility (uniform elon- 224].
gation and total elongation). Radiation-induced tensile Factors that affect microstructural evolution conse-
property changes in SSs have been well studied in wide quently cause variation of tensile property changes. Ma-
temperature ranges [235]. Tensile property data in LWR terial composition and CW, and irradiation temperature
irradiation conditions have been accumulated in the and flux are known as such factors. Variations in these
last two decades. Figure 18 shows the change in yield factors are probably the main reason for the observed
strength and total elongation of LWR-irradiated SSs variations in yield strength at low doses in Figure 18.
[194,196,236–239]. The yield strength increases rapidly Since the dominant microstructural feature is disloca-
with increasing dose and saturates to 800–1000 MPa at tion loops in LWR irradiation conditions, a faster in-
doses of 1–10 dpa. The increase in yield strength accom- crease and saturation in yield strength are caused by
panies the decrease in ductility and work hardening co- factors that enhance dislocation loop formation: for ex-
efficient. At an yield strength of 600–700 MPa, the uni- ample, higher flux, lower irradiation temperature, and
form elongation becomes very low and plastic instability addition of C, Si, P and Nb [196,224,238,239]. How-
appears. As the yield strength saturates, the elongation ever, effects of these factors on a saturation level of yield
saturates to ∼5%. Hardness is often used as a measure of strength have not been clearly identified.
mechanical properties. The increase in hardness (DHv)
is almost linear with the increase in yield strength (Dsy), Deformation mode and microstructure. Radiation-
and a correlation of σ y (MPa) = 3.03Hv (kg/mm2 ) induced microstructural changes cause significant
was derived based on data of LWR-irradiated SSs [240]. changes in deformation mode as well as hardening.
The deformation mechanisms in austenitic SSs are
slip formation at higher temperature and twinning
at lower temperature. Slip formation is dominant at
around 300◦ C. The deformation mode in irradiated SSs
becomes heterogeneous and planar from the homo-
geneous one in unirradiated conditions. This change
occurs due to the formation of dislocation channels in
which moving line dislocations clear away dislocation
loops, forming a path for subsequent slips. In such a
deformation mode, plastic strain is localized within
channels. In the last decade, channel formation and flow
localization in irradiated materials have been extensively
studied [241–244] and their influences on intergranular
fracture and IASCC have also been examined [245–249].
A detailed observation of deformation microstruc-
ture in LWR-irradiated SSs was reported in several ref-
erences [242,245,246,249]. The channel formation was
commonly observed in LWR-irradiated SSs after defor-
mation at around 300◦ C. Figure 19 shows an example
of dislocation channels observed near the surface region
in PWR-irradiated type 316 SSs after being slowly de-
formed to 3% at 300◦ C [245]. The width of the chan-
nels was found to be 20–100 nm and the estimated strain
within a channel might exceed 100%. It was confirmed
from crystalline plasticity calculations that the disloca-
tion channels were formed by the local shear compo-
Figure 18. Change in (a) yield strength and (b) fracture elon- nent of tensile stress [250]. The twin formation was ob-
gation in LWR-irradiated SSs. served and seemed to be pronounced after deformation
232 K. Fukuya
image and solute distributions near crack tips in CW Recent studies for IASCC mechanisms have placed the
type 316 SSs PWR-irradiated to 38 dpa after a constant focus on clarifying the role of deformation and oxidation
load test at stress of 750 MPa in PWR water conditions processes.
[304]. The oxygen concentration near the crack tip is
very low and the crack has steps on the wall. Such steps 4.4.2. Role of deformation
were also found in PWR-irradiated type 316 SSs [301] As described in Section 4.2.2, dislocation channeling
and corresponded to the intersection with slip bands is a distinguishing characteristic of the deformation mi-
or deformation twins. Although crack tip observations crostructure in irradiated SSs. The interactions between
of growing IASCC cracks are still scarce, the available dislocation channels and GBs cause high local strain–
observations have indicated that crack tip oxidation or stress near GBs. When dislocation pileups occur, micro-
oxygen penetration occurs within very narrow cracks, cracks can be initiated as Zener–Stroh type cracks by
typically less than 5 nm, in both BWR and PWR wa- coalescing dislocations piled up along a slip plane. GB
ter conditions, and that the crack propagation relates to separation also can occur if the local stress exceeds GB
deformation microstructure such as slip bands or twins cohesion strength. Such IG fracture can occur without
near GBs. any environmental factors and have been found in LWR-
To date it is widely accepted that IASCC occurrence irradiated SSs. IG fracture in an argon gas atmosphere
cannot be attributed to a single static material prop- was found in type 304 and 316 SSs LWR-irradiated to
erty and is the result of combined effects of multiple 7–73 dpa after tensile tests at low strain rates (<10−6 /s)
dynamic processes. The important factors are likely to and temperatures of 300–340◦ C [184,194,197,305,306].
be oxidation and deformation. The oxidation and corro- The IG cracking initiated from the specimen surface and
sion kinetics near GBs in a water environment are con- the sensitivity to IG fracture decreased with increasing
trolled by GB chemistry and water conditions, and also tensile strain rate [305]. Similar IG cracks in an argon
determine the fracture strength of oxidized or corroded atmosphere were not found at 288◦ C in type 304 SSs
GBs. GB chemistry includes not only RIS, but also the irradiated to 18 dpa [307] and in type 316 SSs irradi-
existence of other elements such as He generated un- ated in a FBR to 50 dpa [212], suggesting that the IG
der irradiation and H generated by corrosion processes. fracture is easier at higher temperatures (300–340◦ C vs.
He and H are likely to have influences on GB cohe- 288◦ C). The IG fracture without an environmental fac-
sion or strength. The deformation controls local stress– tor might be a common phenomenon in highly irradi-
strain exerted on GBs and GB fracture processes. Ma- ated SSs at high temperatures and a low strain rate [308].
terial variables and irradiation conditions affect defor- In such conditions, the dominant deformation mode is
mation and oxidation processes through microstructural slip/channeling in irradiated SSs.
evolution and RIS. Figure 25 shows a schematic illus- Characteristics of IG cracking have been exam-
tration depicting various processes related to IASCC. ined by surface observations after tensile tests were
Figure 27. Contribution of localized deformation as measured by the weighted average channel height to cracking in SSs irradiated
with protons to 1–5 dpa and SCC-tested in BWR water conditions [247].
238 K. Fukuya
evidence is needed to firmly correlate IASCC initiation data are needed for conclusive understanding, GB ox-
with dislocation pileups in channels, these findings sup- idation might be enhanced by RIS at GBs, possibly as
port the idea that the dislocation pileup in dislocation Cr depletion and Si enrichment. It was confirmed that
channels might be one of the key triggers for the IASCC as the Cr content in material decreased, the inner ox-
initiation site. Since there are incalculable variations in ide layer became thicker with lower Cr fraction and then
channel–GB interactions in a specimen due to varia- became less protective as a diffusion barrier [316]. A Si-
tions in the spatial configuration of grains and GBs, a enriched area might be easily oxidized and more soluble
probabilistic approach might be useful for a quantita- and then would enhance GB oxidation and GB fracture
tive understanding of the role of localized deformation [323,324]. This might be one of the reasons for enhance-
on IASCC initiation. ment of IASCC susceptibility by Si addition reported
Channel transfer to the neighboring grain and dis- in BWR-irradiated and proton-irradiated SSs [188,325].
location absorption can cause GB steps and GB slid- Preferential and accelerated oxidation at GBs may be a
ing, respectively, as described in Section 4.2.2. Such steps key factor for IASCC. However, detailed knowledge of
and sliding may break surface oxides if applied strain GB oxidation in irradiated SSs is still limited, especially
is sufficiently larger than the ductility of oxides. When considered in combination with water radiolysis effects.
this process continues in a channel and a GB, acceler-
ated oxidation is expected to occur at the intersection
and along the GB, and might result in triggering IASCC 4.4.4. Other contributors
initiation. However, these type of interactions might not Hydrogen effects. Hydrogen is known to affect
be dominant since IASCC cracks were more frequently cracking processes through various metallurgical fac-
found for GBs without slip continuity in BWR water tors. There are a number of studies concerning hy-
conditions [308]. drogen effects on cracking, mechanical properties, and
microstructure in various non-irradiated materials.
However, knowledge on hydrogen effects on irradiated
4.4.3. Role of oxidation
materials and IACC is limited. Several measurement re-
Oxidation kinetics and the nature of oxides are key sults of hydrogen concentration were reported for LWR-
information for the understanding of mechanisms of irradiated SSs [213,218,220,326,327]. The measured
IASCC as well as IGSCC in non-irradiated SSs. The values ranged from 10 to 200 wtppm with very large scat-
oxidation rate and structure of non-irradiated SSs in ter and showed no clear trend against dose. Since the
LWR water conditions have been well examined [315–
317]. The surface oxide is a double-layer structure: an
inner Cr-rich spinel layer and an outer Fe- and Ni-rich
spinel layer in PWR water conditions, and an inner Fe–
Cr–Ni spinel layer and an outer hematite layer in BWR
water conditions. There are proposed IGSCC mecha-
nisms of austenitic SSs in LWR water conditions such
as slip dissolution or slip oxidation [207,318], creep and
GB sliding [319], and hydrogen embrittlement [320]. In
these mechanisms, oxidation plays essential roles for not
only the oxidation itself, but also as a source of vacancies
and hydrogen atoms. Enhancement of oxidation results
in enhanced sensitivity to cracking in any mechanism.
While a similar role of oxidation is expected for IASCC
occurrence, experimental studies on the role of oxidation
in IASCC of irradiated SSs are scarce.
Morphology of oxides formed on irradiated SSs has
been examined in only a few papers. In type 316 SSs ir-
radiated to 5 dpa with protons and exposed to BWR
NWC water for 70 h, neither enhancement of oxidation
nor a difference in oxide structure was found compared
to unirradiated SSs [321]. In CW type 316 SSs irradi-
ated up to 73 dpa and exposed to PWR water condi-
tions for 1000 h, slight enhancement of the inner oxide
layer thickness was found [322]. Preferential oxidation
and Ni enrichment ahead of the oxides were also found
Figure 28. Distribution of Fe, Ni, Cr and O in the cross sec-
along several GBs, as shown in Figure 28 [322]. This in- tion of the surface oxide layer in type 316 SSs PWR-irradiated
dicated that the oxidation of both the matrix and GBs to 20 dpa after immersion in PWR water conditions for 1000 h
might be enhanced in irradiated SSs. Although more [322].
Journal of Nuclear Science and Technology, Volume 50, No. 3, March 2013 239
measured values were generally inconsistent with calcu- damaged area containing dense dislocation loops. High-
lated generation amounts from nuclear reactions [220], concentration hydrogen is expected to enhance deforma-
hydrogen in LWR-irradiated SSs is likely to originate tion localization and might have an enhancement effect
from the water environment probably through corrosion on IASCC initiation and growth.
reactions.
The relationship between hydrogen and IG crack- GB cohesion or strength. Among various mi-
ing in irradiated SSs has been discussed in a limited crostructural and microchemical changes, some changes
number of papers. The hydrogen measurements in type result in the decrease in cohesion or strength of GBs.
316 SSs irradiated to 6 and 53 dpa after SSRT tests This might not be a direct cause of IASCC but might
in PWR water conditions revealed that the hydrogen have an important role in crack initiation and propa-
concentration near the IG fracture surface was slightly gation. Possible factors are hydrogen, helium, RIS and
higher than that away from the fracture surface [184]. oxygen. As for hydrogen, it causes GB decohesion which
This provided evidence that hydrogen is associated with is one of the causes of hydrogen embrittlement.
cracking processes in irradiated SSs. Hydrogen charg- As described in the previous sections, He is gen-
ing effects on mechanical properties were examined in erated under LWR irradiation and helium bubbles are
type 304 SSs BWR-irradiated up to 20 dpa [328]. Af- formed on GBs in PWR-irradiated SSs to high doses
ter hydrogen charging and discharging at 100◦ C, IG [219]. The high generation rate of He in PWR irra-
fracture was found after tensile tests at room temper- diation compared to FBR irradiation was considered
ature and its fraction increased with increasing dose. as one of the reasons that PWR-irradiated SSs exhib-
The cause of IG fracture was attributed to combined ited higher IASCC susceptibility than FBR-irradiated
effects of hydrogen-induced martensite formation and SSs [213]. It is well known that He induces IG fracture
radiation-induced GB Cr depletion, based on the sim- and significantly reduces ductility in slow tensile and
ilarity to hydrogen-induced IG cracking in sensitized creep conditions at high temperatures (typically higher
type 304 SSs. Hydrogen charging effects were also exam- than 400–450◦ C) [235]. At LWR-relevant temperatures,
ined in type 304 SSs BWR-irradiated to 2–3 dpa [329]. high-temperature He embrittlement is not believed to be
IG cracking was found by bending at 23◦ C after hy- important. However, dense fine bubbles on GBs might
drogen charging, indicating that hydrogen caused IG reduce stresses that would lead to GB fracture. The cri-
cracking. Similar IG cracking was found by bending at teria for IG cracking in He-implanted SSs were reported
23◦ C after SSRT tests in BWR water conditions. How- to be ∼30 nm for cavity spacing and ∼4 nm for the
ever, steels that exhibited higher IASCC susceptibility cavity diameter at temperatures lower than 500◦ C [333].
by SSRT tests in BWR water conditions showed lower He bubbles observed in PWR-irradiated SSs seem to
sensitivity to IG cracking at 23◦ C after SSRT tests and satisfy these conditions. In recent micro-tensile tests on
hydrogen charging. Thus, these results seem to suggest helium-implanted type 316 SSs, preferential fracture on
that processes related to hydrogen might not be involved GBs was found [334]. Fine bubbles on GBs might pro-
in IASCC in BWR water conditions. Hydrogen embrit- vide a preferential path of fracture with probably lower
tlement or hydrogen-induced cracking might be a pos- strength than the matrix, but the exact role of helium
sible effect of hydrogen on IASCC. High yield strength and bubbles is not yet understood.
and well-developed RIS in highly irradiated SSs might GB segregation of solute elements is a potential fac-
provide more preferable conditions for hydrogen embrit- tor enhancing GB fracture. GB embrittlement due to
tlement. However, based on current irradiated data, it is segregation of impurities such as P has been extensively
still uncertain whether hydrogen is the cause or the result studied for body centered cubic (BCC) alloys and steels.
of the cracking. Recent ab initio calculations of GB cohesive energy
Another possible effect of hydrogen is the interac- showed GB decohesion by some elements in face cen-
tion of hydrogen with the deformation microstructure tered cubic (FCC) systems [335–337]. For Ni 5 (012)
[330,331]. It is known that hydrogen, if the concentra- symmetrical tilt GBs, most of the solute elements includ-
tion is sufficiently high, can relax elastic interactions ing helium have embrittling potency, while B, C and Si
between moving dislocations and obstacles enhancing can enhance the GB cohesion [335]. Other recent ab ini-
dislocation gliding and it can reduce SFE and cross-slip tio calculations showed that significant GB decohesion
enhancing the planar dislocation microstructure. These occurs for segregation of S and O atoms in Ni [336,337].
effects are expected to enhance dislocation channel for- It is known that S enhanced IASCC susceptibility in
mation in irradiated materials. This effect was confirmed BWR water [188,329]. S-induced decohesion might as-
by slow tensile tests on type 316 SSs irradiated to 5 dpa sist IG cracking in an argon atmosphere and also assist
with Fe ions [332]. The average spacing between sur- IASCC susceptibility, while Ni–S film formation at GBs
face slips after slow tensile tests at 300◦ C was larger in due to S and Ni segregation has been proposed [329]. In
an hydrogen atmosphere than in an argon atmosphere. LWR water conditions, O atoms are preferentially con-
TEM observations on the specimen cross sections con- sumed by forming oxides rather than being segregated
firmed that the surface slips were formed by disloca- at GBs. However, in the observations of rapidly grow-
tion channels which could penetrate the near-surface ing IASCC crack tips, O atoms penetrated into the GBs
240 K. Fukuya
condition data are needed based on theoretical modeling To establish a realistic prediction of IASCC in LWR
and data acquisition. conditions from available databases, relationships be-
tween PIE data and in-reactor data, and between LWR-
Fracture toughness. It is well known that irradiation irradiated data and FBR-irradiated data, must be clar-
causes reduced fracture toughness and that the reduc- ified. To overcome limitations of databases on irradi-
tion is related to loss of ductility [235]. Fracture tough- ated materials, mechanistic understanding is believed to
ness data of LWR-irradiated SSs have been accumu- be essential. Understanding of IASCC mechanisms has
lated in the last decade [223,236,349–352]. Data analy- been improved in this decade, although exact causes of
sis and assessment of failure analysis have been reported IASCC are yet uncertain. It has been confirmed that
[353,354]. Figure 30 shows the data of fracture toughness IASCC susceptibility can correlate with material prop-
in LWR-irradiated SSs. Fracture toughness generally de- erty changes such as RIS, dislocation microstructure
creased rapidly to 5–10 dpa and the lower bound of the and hardening but it cannot be explained by a single
data seems to saturate to ∼50 kJ/m2 . Current databases static material property change. Current consensus is
have large data scatters, probably due to large variation that IASCC is likely to be caused by combined effects of
of irradiation and material conditions, and also due to multiple dynamic processes. Recent studies focused on
test methods, and specimen size and shapes. Fracture the role of deformation and oxidation behaviors as es-
toughness depends on material and irradiation condi- sential processes for IASCC. Characteristics of disloca-
tions as well as test methods and conditions, while influ- tion channels and their interactions with GBs continue
ences of these parameters in LWR irradiation conditions to be examined, and the importance of localized defor-
are not well understood. Fracture toughness has a close mation on IG cracking has been confirmed. However,
link to tensile properties and correlations have been pro- changes in GB properties by oxidation and other pro-
posed [235,355,356]. Development of mechanistic un- cesses in irradiated SSs and changes under irradiation
derstanding and database improvement are needed for are not well understood. Degradation of GB cohesion
reliable prediction. or strength due to irradiation and oxidation needs to
be clarified considering effects of RIS and other factors
such as hydrogen and helium.
4.6. Summary of IASCC The evaluation of structural integrity of core inter-
Databases on IASCC initiation and CGR in LWR- nals requires prediction methods of stress relaxation,
irradiated SSs have been significantly expanded in the swelling and fracture toughness as well as IASCC ini-
last decade and they now provide phenomenological tiation and CGR. While empirical prediction curves for
knowledge on the general response of IASCC initiation these properties have been proposed, further improve-
and CGR to fluence, stress and water conditions. How- ment is needed not only by accumulation of irradiated
ever, the knowledge is still insufficient for a full descrip- data, but also by mechanistic modeling.
tion of effects of such parameters on IASCC. While initi-
ation stress and CGR tend to saturate at certain doses, it
is unclear where complete saturation occurs and at what 5. Conclusions
saturation level: these might depend on material and In this paper, current phenomenological knowledge
water conditions. Based on current databases, empirical and understanding of mechanisms on radiation embrit-
trend curves of IASCC initiation and CGR have been tlement and IASCC in PWRs and BWRs were reviewed,
developed but are applicable to only limited conditions. placing emphasis on microscopic material changes and
their role in degradation processes. Knowledge of mi-
crostructural evolution in LWR irradiation conditions
has been significantly improved by recent development
of nano-scale analytical techniques such as 3DAP and
by applying such techniques to LWR-irradiated mate-
rials. In RPV low-alloy steels, solute clusters of Cu,
Mn, Ni and Si and dislocation loops were identi-
fied as features causing hardening and embrittlement.
Mechanism-guided correlations of transition tempera-
ture shift have been developed based on improved un-
derstanding. In SSs for core internals, deformation and
oxidation have been recognized as potential processes
causing IASCC initiation and growth. However, full un-
derstanding of the mechanisms has not been achieved
yet and there are still many issues for improving the un-
derstanding of phenomenology and mechanisms of ra-
Figure 30. Fracture toughness data in LWR-irradiated SSs diation embrittlement and IASCC. Several important is-
tested at ∼300ºC. sues were pointed out in the review.
242 K. Fukuya
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