Acta Materialia 234 (2022) 117991

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Acta Materialia
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Insights into hardening, plastically deformed zone and geometrically

necessary dislocations of two ion-irradiated FeCrAl(Zr)-ODS ferritic
steels: A combined experimental and simulation study
Peng Song a,b,∗, Kiyohiro Yabuuchi b, Philippe Spätig a
a
Department of Nuclear Energy and Safety, Paul Scherrer Institute, 5232 Villigen PSI, Switzerland
b
Institute of Advanced Energy, Kyoto University, Gokasho, Uji, Kyoto 611-0011, Japan

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

Article history: As one of promising candidate materials for fuel claddings and structural components in the Gen-IV
Received 30 August 2021 fission reactors, FeCrAl(Zr)-ODS ferritic steels were studied to well understand the radiation hardening
Revised 15 March 2022
behavior. Nanoindentation (NI) hardness and plastically deformed zone (PDZ), geometrically necessary
Accepted 1 May 2022
dislocations (GNDs) as well as microstructures were investigated for two FeCrAl(Zr)-ODS ferritic steels
Available online 6 May 2022
irradiated with 6.4 MeV Fe3+ at room temperature (RT) up to the nominal damages of 2, 10 and 50
Keywords: dpa. Irradiation-induced hardening, which was estimated by using the Nix-Gao model regardless of the
Radiation hardening damage gradient effect (DGE), increased continuously with increasing the nominal displacement dam-
Plastically deformed zone age. When taking the DGE into account, the dependence of the irradiation hardening (in MPa) on a local
Geometrically necessary dislocations damage level (dpa) obtained by finite element method (FEM) simulations was 153.65 × (dpa)0.26 and
ODS ferritic steel 158.35 × (dpa)0.25 for the non-Zr steel and the Zr-added one, respectively. The hardening caused by ion-
Nanoindentation
irradiation was discussed in terms of the loss of oxide particles, the formation of dislocation loops and
the solid solution hardening mainly by dissolved oxygen. The addition of Zr reduced the ion-irradiation
hardening of steel to some extent mainly by suppressing the formation of dislocation loops. Meantime, as
the FEM simulations revealed, the PDZ size underneath a conical indenter at the equivalent plastic strain
ε eq > 1.9% can reasonably estimate the density of GNDs. According to the strain gradient plasticity (SGP)
theory, the densities of GNDs at an indentation depth of 200 – 300 nm were slightly higher in the case
of the 50 dpa/nominal than the unirradiated, in spite of similarity for the two FeCrAl(Zr)-ODS steels.
© 2022 The Author(s). Published by Elsevier Ltd on behalf of Acta Materialia Inc.
This is an open access article under the CC BY-NC-ND license
(http://creativecommons.org/licenses/by-nc-nd/4.0/)

1. Introduction As previous studies revealed, the corrosion resistance [10], the

High-Cr oxide dispersion strengthened (ODS) ferritic steels with
Al addition have been developed in Japan to replace Zircaloy for
the accident tolerance fuel (ATF) of current light water reactors
mainly because of their good oxidation resistance arising from a
protective Al2 O3 scale especially at high temperatures in steam
[1,2], their superior structural stability and mechanical properties
(e.g. tensile, creep strength) even at elevated temperatures [1,3,4],
as well as their excellent neutron radiation tolerance [5–8]. They
are also considered as promising fuel claddings and structural
components in the future Gen-IV fast reactors [1,9], where neutron
irradiation damage is expected up to 160 dpa [9].
∗
Corresponding author at: Department of Nuclear Energy and Safety, Paul Scher-
rer Institute, 5232 Villigen, Switzerland.
E-mail address: peng.song@psi.ch (P. Song).
mechanical properties [1,3] and the radiation tolerance [5,11–13]
of ODS ferritic steels strongly depend on the dispersion morphol-
ogy of nano-sized oxide particles inside the matrix, which not only
effectively hinder the motion of dislocations and grain boundaries
(GBs) resulting in enhanced strength, but also provide point-defect
traps through particle-matrix (P-M) interfaces. Thus, they promote
the annihilation or recombination of radiation defects.
As far as the radiation hardening of ODS steels is concerned,
numerous investigations [11–14] focused on the formation of de-
fect clusters, especially the dislocation loops during ion irradia-
tions, which can be suppressed by trapping sites provided by the
initial microstructures (GBs, P-M interfaces and dislocations). In
our previous work [11], after dual-beam (Fe3+ plus He+ ) irradia-
tion at 550 °C to the nominal damage of 15 dpa (∼20 0 0 appm
He), no hardening was found in the three ODS ferritic steels, al-
though cavities (3–7 nm in mean diameter) of high number densi-
ties up to ∼1 × 1023 m−3 were formed in the irradiated steels and

https://doi.org/10.1016/j.actamat.2022.117991
1359-6454/© 2022 The Author(s). Published by Elsevier Ltd on behalf of Acta Materialia Inc. This is an open access article under the CC BY-NC-ND license
(http://creativecommons.org/licenses/by-nc-nd/4.0/)
P. Song, K. Yabuuchi and P. Spätig
approximately 80% cavities were adjacent to oxide particles. Duan
et al. [12] reported that, the Fe-ion irradiation at 300 or 500 °C up
to 10 dpa caused a significant hardness increase in a set of ODS
alloys of different grain sizes, dislocation densities and morpholo-
gies of particle dispersion, while the hardening was significantly
reduced with increasing the total sink strength (i.e. trapping sites)
of the initial microstructures. Similar dependence of hardening on
the sink strength of oxide particles was obtained by Zhang et al.
[13] for three ODS ferritic steels irradiated with high-energy Ni
ions at ∼0.8 dpa and −50 °C. In contrast, Heintze et al. [14] found
that, under Fe-ion irradiation at room temperature (RT) to 10 dpa,
the hardness increase in the two ODS ferritic steels depended only
on grain size rather than particle number density, which is ex-
plained by the fact that coherent interfaces between (Y, Ti) ox-
ide particles and matrix cannot efficiently trap self-interstitials. So
both the dispersion morphology and the interface coherency of ox-
ide particles could play a vital role in suppressing radiation hard-
ening of ODS steels.
Collision cascades produced by energetic particles (like neu-
tron, proton and heavy ions) modify the oxide particles dispersed
in the steel matrix in terms of their chemical composition [15–
18], the crystal structure [19], the particle-matrix (P-M) interface
[19,20], and the dispersion morphology [15,19–23]. Our recent
work [19] showed that, in three 15Cr-ODS ferritic steels irradiated
with Fe ions at 200 °C up to 10 dpa/nominal, the phase stability of
the dominant oxide particles was in the order of Y-Zr-O > Y-Ti-O >
Y-Al-O, according to the corresponding changes in volume fraction
and amorphization behavior. Therefore, it is necessary to investi-
gate the irradiation-induced hardening of ODS steels with different
oxide forming elements, where nano-scale oxide particles may re-
spond differently to radiation damages.
Although nanoindentation has been long used to study ion-
irradiation effects on the mechanical properties of nuclear ma-
terials [24–29], the interpretation of nanoindentation results is
still difficult because indentation probes a shallow irradiated layer
(commonly < 3 μm) of a steep damage gradient on a soft unirra-
diated substrate. At such small indentation depths, numerous ge-
ometrically necessary dislocations (GNDs) are produced to accom-
modate the strain gradient in the plastically deformed zone (PDZ)
underneath the indenter, whose density usually increases with de-
creasing indentation depth. This phenomenon results in a larger
hardness at a smaller indentation depth, which is known as the in-
dentation size effect (ISE) [30]. However, for an indentation depth
below ∼100 nm, dislocation activities under indentation may be-
come discrete in nature, which can limit the multiplication of
GNDs [31]. According to Johnson’s model [32], the normalized size
Znor of PDZ in elastic-perfectly plastic solids depends on the ratio
of Young’s modulus E to yield stress σ Y by the following equation:
 2 E 1 / 3
Znor = (1)
3 σY
Based on the above discussion, the normalized PDZ size and
the associated GNDs density of an ion-irradiated specimen are ex-
pected to vary with indentation depth within a damage-gradient
layer, which is the source of difficulties for assessing ion-irradiation
hardening. By using FEM simulation, Dolph et al. [24] found the
PDZs in an Fe9Cr-ODS steel produced by a conical indenter were
7.84, 7.25 and 5.49 times the indentation contact depth for the as-
received, ion-irradiated (50 dpa, 400 °C) and neutron-irradiated (3
dpa, 500 °C), respectively, without taking the damage gradient ef-
fect (DGE) into account. Hence, based upon a good understanding
of the radiation hardening in ODS steels, the PDZ size and GNDs
density can be considered.
The Zr addition into FeCrAl-ODS ferritic steels changed the crys-
tal structure of dominant oxide particles, and also improved their
2
Acta Materialia 234 (2022) 117991
coherency of particle-matrix interface and dispersion morphology
to some extent [33,34]. Therefore, this work was launched to in-
vestigate by means of nanoindentation and FEM simulation: 1)
dpa-dependence hardening behaviors of two FeCrAl(Zr)-ODS fer-
ritic steels under Fe-ion irradiation at RT; 2) the effects of ion-
irradiation on the PDZ size and the associated GNDs.
2. Materials and methods
2.1. Materials
The materials used in this study were two FeCrAl(Zr)-ODS fer-
ritic steels produced by mechanical alloy processing. The corre-
sponding chemical compositions (wt.%) were Fe-15.42Cr-1.85W-
0.1Ti-3.8Al-0.36Y2 O3 (excess oxygen: 0.084) and Fe-14.59Cr-1.84W-
0.14Ti-3.46Al-0.27Zr-0.33Y2 O3 (excess oxygen: 0.11), hereinafter,
named as (Y, Al) ODS and (Y, Zr) ODS, respectively. After hot ex-
trusion and forging at 1150 °C, the materials were finally annealed
at 1150 °C for 1 h followed by air-cooling. More details regarding
the material processing are given in Ref. [3].
Prior to ion-irradiation, the specimens were prepared so that
the specimen surfaces were perpendicular to the extrusion direc-
tion, in other words, the ion-irradiation direction is parallel to the
extrusion direction. The specimen surfaces were mechanically pol-
ished with SiC papers, and subsequently with successive grades
of diamond spray down to 0.25 μm. Finally, electrolytic polishing
was conducted in the solution of 10% (vol.) HClO4 and 90% (vol.)
CH3 COOH at room temperature to remove any residual mechanical
damage.
2.2. Irradiation conditions
For each damage level, specimens of (Y, Al) ODS and (Y, Zr) ODS
were irradiated simultaneously with 6.4 MeV Fe3+ ions by using
the DuET facility at Kyoto University [35]. The beam was raster
scanned at a frequency of 10 0 0 Hz in a horizontal direction and
300 Hz in a vertical direction under a vacuum of ∼10−6 Pa. The
flux of ion beam was measured to be approximately 2.1 × 1016
ions m−2 s−1 . The specimens during irradiation were set on a cop-
per holder cooled by flowing water inside the holder. The irradia-
tion temperature was measured by a thermocouple and controlled
to be 30 °C within the fluctuation of ±5 °C.
The displacement damages (displacements per atom, dpa) of a
Fe-15Cr alloy were obtained by SRIM [36] simulations, which used
the Kinchin-Pease method [37] and are shown in Fig. 1. The dam-
aged layer was located in the depth range of 0 – 2220 nm. The
nominal displacement damages were defined as the ones at the
ion-penetration depth of 600 nm, which were about 2, 10 and 50
dpa, and the damages were ranging roughly 1.2 – 6 dpa, 6 – 30 dpa
and 30 – 150 dpa in each damaged area, respectively (see Fig. 1).
The nominal displacement rate was around 6.4 × 10−4 dpa/s. The
injected Fe concentration for 50 dpa/nominal is shown with the
dashed profile in Fig. 1.
2.3. Transmission electron microscopy (TEM)
In order to observe depth dependent damage structures, cross
sectional TEM specimens were prepared by the lift-out technique
in a Focused Ion Beam (FIB, Hitachi, FB2200) instrument, where
the final beam used was 20 keV Ga+ . Prior to TEM observations,
flash polishing was done by using the solution consisting of 5%
(vol.) HClO4 and 95% (vol.) CH3 OH at around −35 °C to remove
the damage layer produced by FIB. About five TEM lamellas were
finally polished with 1 keV Ar+ ions instead of flash polishing. Dis-
location loops and oxide particles were observed under bright field
P. Song, K. Yabuuchi and P. Spätig
Fig. 1. The depth profiles of displacement damage (solid) and concentration of in-
jected 6.4 MeV Fe3+ ions (dash) into Fe-15Cr alloy predicted by SRIM simulation.
(BF) and weak beam dark field (WBDF) imaging conditions by us-
ing a conventional 200 kV JEOL JEM 2010 microscope equipped
with a LaB6 electron emitter. The thickness of all observation ar-
eas in TEM lamellas was measured using electron energy-loss spec-
troscopy (EELS) log-ratio technique [38].
2.4. Nano-hardness measurements
Nanoindentation tests were performed on unirradiated and ir-
radiated specimens by using an instrumented nanoindenter (Agi-
lent G200) with a Berkovich tip. The continuous stiffness measure-
ment (CSM) method was selected to obtain continuous profiles of
hardness and elastic modulus as a function of indentation depth.
Before testing, the indenter tip geometry was calibrated against
the Young’s modulus of a fused silica reference sample at indenta-
tion depths larger than ∼50 nm. The testing parameters were de-
scribed as follows: the maximum indentation depth was 20 0 0 nm,
the strain rate was 0.05 s−1 , the harmonic displacement target and
frequency target were 1 nm and 45 Hz, respectively, and the Pois-
son’s ratio ν for ODS steels was 0.3. For each specimen, 24 inden-
tations (60 μm between two adjacent points) were carried out and
the averaged hardness was obtained by calculating the measured
hardness data of ∼20 tests to take into account the significant scat-
tering in the data.
2.5. Finite element method (FEM) simulation
A two-dimensional axisymmetric model was developed by us-
ing ABAQUS 6.4–1 standard code for modeling the nanoindenta-
tion process. Considering that the contact area function A ver-
sus the contact depth hc for a perfect Berkovich indenter is A(hc )
= 24.56(hc )2 , an axisymmetric rigid conical indenter with the
apex angle of 70.3° was chosen for modeling the Berkovich in-
denter, which is shown in Fig. 2. The tip radius was typically
set to be 100 nm to represent the bluntness of the indenter
in practical experiments [39]. The specimen had the dimensions
of 40 μm × 40 μm (length × width), which was meshed with
36720 8-node biquadratic axisymmetric quadrilaterals (CAX8R).
The ABAQUS code calculated the multi-axial stress/strain state by
using the von Mises stress potential and associated J2 flow law
[40]. The elastic modulus E and Poisson’s ratio ν of the two ODS
ferritic steels were 225 GPa and 0.3, respectively, which were iden-
tical with those during experimental nanoindentation testing. The
specimen was modelled as being locally isotropic. The uniaxial
3
Acta Materialia 234 (2022) 117991
true stress-true strain relationship was fitted by using the Ludwik-
Hollomon equation [40]:
σ = σYUn + K εpln (2)
where σ is von Mises stress, σYUn is the value at yield point
(ε pl = 0) for the unirradiated specimens, ε pl is equivalent plastic
strain (also PEEQ), K is known as the ‘strength coefficient’ and n as
the ‘strain-hardening exponent’. The measured yield strength val-
ues of (Y, Al) ODS and (Y, Zr) ODS were 933.6 MPa and 1041.3 MPa,
respectively (see Supplementary material S1). In the case of the ir-
radiated material, the constitutive law of the irradiated layers was
assumed to be given by:
σ = σ Irr + σYUn + K εpln (3a)
σ Irr = C × (dpa )m (3b)
where σ Irr is the increased part of flow stress produced by the
ion-irradiation, assumed as a function of the damage level (dpa) by
Eq. 3(b). Detailed discussion is present in Sections 3.2 and 3.3. The
ion-irradiated region in Fig. 2 was divided into 23 layers according
to the depth-dependent displacement damage profile (broad lay-
ers up to 1200 nm and thinner ones for the larger damage gradi-
ent), to minimize discontinuity in the calculated plastic strain be-
tween two adjacent discrete layers. The possible effects of the layer
number on the plastic strain and the load-indentation depth rela-
tionship have been investigated (see Supplementary material S2).
In the depth range of 1650 – 1950 nm, where the damage level
decreased steeply with depth, the thickness of each discrete layer
was set to be 60 nm. The constitutive laws of the unirradiated and
irradiated specimens are shown in Fig. 3(a). The contact friction of
0.2 was commonly used for the Coulomb friction between the rigid
tip and the top surface of a metal.
The discrepancy of load-depth curves between FEM simulation
and experimental tests can be quantified by the dimensionless pa-
rameter Sred, the “reduced sum of squares” [41]:
N
i=1 (Pi,
M − Pi,E )2
Sred = 2
(4)
NPav,E
where Pi,M and Pi,E are the ith load values predicted by FEM sim-
ulations and measured by experimental tesst, respectively, Pav,E is
the average value of the experimentally measured loads over the
whole indentation depth range (up to 20 0 0 nm), and N was set to
be 100 for a displacement increment of 20 nm. Generally, a model
that captures the material plasticity response reasonably has the
parameter Sred less than 10−3 [41].
3. Results and discussion
3.1. Microstructures before and after irradiations
Microstructures in the unirradiated (Y, Al) ODS and (Y, Zr) ODS
have been fully investigated in our previous work [19]. The av-
eraged grain sizes of (Y, Al) ODS and (Y, Zr) ODS were approxi-
mately 460 and 370 nm, respectively, while the dislocation den-
sities in these two ODS ferritic steels were 1.2 × 1014 m−2 [19].
Most of oxide particles in (Y, Al) ODS and (Y, Zr) ODS were Y-
Al-O particles (YAP, YAH in YAlO3 ) [33] and Y-Zr-O particles (δ -
phase Y4 Zr3 O12 , fluorite Y2 Zr2 O7 ) [19,34], respectively. The mean
diameters and number densities of oxide particles in (Y, Al) ODS
and (Y, Zr) ODS were 6.0 ± 1.5 nm/(5.2 ± 1.0) × 1022 m−3
and 6.4 ± 1.5 nm/(6.9 ± 0.4) × 1022 m−3 , respectively [19]. The
higher density of oxide particles, usually possessing a smaller
inter-particle distance, can effectively impede the dislocation climb
motion at elevated temperatures, which maintained the higher
creep strength of (Y, Zr) ODS than (Y, Al) ODS [1,4].
P. Song, K. Yabuuchi and P. Spätig
Fig. 2. Sketch of the axisymmetric cone tip-specimen model, consisting of 23 irradiated layers within the displacement damage profile.
Fig. 3. (a) scheme of the plastic properties of the unirradiated and the irradiated ODS steels, and the curves of load versus indentation depth for (b) (Y, Al) ODS and (c) (Y,
Zr) ODS, obtained by NI tests and FEM modeling.
After the ion irradiations to 2 and 10 dpa/nominal, TEM obser-
vations have been done for the local microstructures in the depth
range of ∼400 – 1300 nm from the specimen surface to avoid the
effects of surface sink and injected Fe interstitials (see Fig. 1). The
dpa dependence of microstructures can be obtained from each lo-
cal depth corresponding to a well-defined local damage level (local
dpa). Fig. 4 shows the averaged diameter and number density of
oxide particles as a function of local dpa. It is obvious that, both di-
ameters and number densities of oxide particles in (Y, Al) ODS and
(Y, Zr) ODS decreased continuously with increasing damage level,
and the number densities at ∼30 dpa/local were closely one order
of magnitude lower than those at 0 dpa. Importantly, it is difficult
to find significant differences between the dispersion morpholo-
gies of oxide particles in the two FeCrAl(Zr)-ODS steels under RT
irradiations, whereas oxide particles in (Y, Zr) ODS remained little
bigger volume fractions than (Y, Al) ODS after the Fe-ion irradia-
tions at 200 °C [19]. The oxide particles in (Y, Ti) ODS had much
higher number densities than those of (Y, Al) ODS and (Y, Zr) ODS
below ∼20 dpa/local, but it became inverse above ∼20 dpa/local,
which is shown in Fig. 4(b).
According to the vacancy mechanism, the radiation enhanced
diffusion coefficient of Y atom, DY at RT was estimated to be
5.3 × 10−9 nm2 /s and the corresponding diffusion distance was
around 0.02 nm during the irradiation period (∼5 h for 10
4
Acta Materialia 234 (2022) 117991
dpa/nominal) [22]. This short diffusion distance indicated the neg-
ligible particle recovery through the recoiled solutes (particularly
Y) diffusing to the nanoparticles and the re-precipitation. Oxygen
as an interstitial atom in bcc Fe has an exceptional high affinity for
vacancies [42] and the diffusion coefficient of oxygen in vacancy-
included bcc Fe at RT was estimated to be around 9.53 × 10−7
nm2 /s based on Arrhenius equation [42]. Furthermore, the diffu-
sion of oxygen can be further reduced because both oxygen and
vacancy structures would form strong chemical bonds with the
solute Ti and Y atoms [43]. So in this work, the dissolved oxide
forming atoms were expected to be at the vicinity of the parent
oxide particles, which was confirmed by the satellite precipitates
produced in the two ion-irradiated FeCrAl(Zr)-ODS steels at 200 °C
[19]. The evolution rate of the particle radius r can be solely con-
trolled by the ballistic dissolution and depicted by the following
equation [44]:
dr/dt = −ζ K  (5)
where ζ K represents the flux of atoms from the particle surface, K
is the displacement rate (in dpa/s) in the matrix,  is the atomic
volume of ejected atoms. Supposing close fluxes of ejected atoms
from Y-X-O (X = Ti, Al, Zr) particles for a given displacement rate,
small oxide particles tended to be invisible during TEM observa-
tions after a critical period of ion irradiation, which explained the
P. Song, K. Yabuuchi and P. Spätig
Fig. 4. (a) Averaged diameter and (b) number density of oxide particles as a function of local dpa in (Y, Ti) ODS [22], (Y, Al) ODS and (Y, Zr) ODS irradiated to nominal
displacement damages of 2 and 10 dpa. Each local damage corresponds to the calculated value based on SRIM simulations at the corresponding depth.
lower number densities of oxide particles in (Y, Ti) ODS than those
of (Y, Al) ODS and (Y, Zr) ODS above ∼20 dpa/local. However, the
threshold displacement energies of oxide forming atoms like Y, Ti,
Al, Zr in nano-sized particles require to be known for well un-
derstanding the distinct fluxes ζ K of ejected atoms produced by
knock-on atoms. Monnet et al. [45] investigated the particle-size
evolution of different oxides Y2 O3 , MgAl2 O4 , MgO and Al2 O3 inside
ferritic matrix by using 1 MeV electrons at 400 °C. It is found that
Y2 O3 showed the negligible diameter shrinkage compared with the
other oxides because of the high threshold displacement energy of
Y [45].
In the previous studies [46–48], nearly complete dissolution of
oxide particles without the formation of new clusters or precipi-
tates was observed by atom probe tomography (APT) after heavy
ion irradiations at RT [46], at 100 °C and -75 °C [47] where the
damage level ranged from about 50 to 150 dpa. This phenomenon
was also confirmed by glancing-incident angle X-ray diffraction
(GIXRD) for the ion-irradiation (-123 °C, ∼50 – 100 dpa) [48].
Moreover, the dissolved oxide forming atoms like Y and O were
present as solute atoms in ferrite confirmed by APT [46,47]. After
the irradiation up to 50 dpa/nominal (around 30 – 150 dpa/local),
the particle density would be lower than 4.6 × 1021 m−3 (see ∼30
5
Acta Materialia 234 (2022) 117991
dpa/local in Fig. 4(b)), indicating that most of oxide particles in (Y,
Al) ODS and (Y, Zr) ODS were dissolved into ferrite matrix.
Previous studies [49,50] demonstrated that, after ion irradia-
tions at RT, the primary dislocation loops formed in Fe-Cr al-
loys consisted of the 1/2<111> and 100 interstitial types but no
1/2<110> type. According to the g•b = 0 invisibility criteria, a half
of the 1/2<111> loops and two thirds of the 100 loops are visi-
ble with g = [11̄0], while all of the 1/2<111> loops and one third
of the 100 loops are visible with g = [002]. Fig. 5 shows the
microstructures of (Y, Al) ODS (Figs. 5(a), 5(b)) and (Y, Zr) ODS
(Figs. 5(d), 5(e)) in an identical grain for each ODS steel after the
irradiation to ∼72 dpa/local at the depth of about 900 nm, which
were observed by using g = [11̄0] and g = [002] under weak
beam dark field (WBDF, g3g) conditions. In Figs. 5(a), 5(b), 5(d)
and 5(e), there are many tiny “white dots”, marked with dashed
circles. For each ODS steel, the density of “white dots” imaged by
g = [002] was evidently bigger than that imaged by g = [11̄0],
whereas the visibility of oxide particles via strain contrast does
not depend on the chosen g vector. So the “white dots” circled can
be considered as dislocation loops and the other weak contrasts
without being circled might be some surface contaminations. Ox-
ide particles in the unirradiated grains of (Y, Al) ODS and (Y, Zr)
P. Song, K. Yabuuchi and P. Spätig
Fig. 5. Microstructures in the irradiated grains of (Y, Al) ODS (a, b) and (Y, Zr) ODS (d, e) observed under weak beam dark field (WBDF, g3g) imaging conditions by using g =
[11̄0] and g = [002] close to pole [110] in an identical region at ∼900 nm (∼72 dpa/local) at a nominal damage of 50 dpa. High density of oxide particles in the unirradiated
(Y, Al) ODS (c) and (Y, Zr) ODS (f) imaged by using g = [11̄0] shown here for comparison with dislocation loops. Dislocation loops circled were counted for estimating
number density.
ODS imaged by g = [11̄0] are shown in Figs. 5(c) and 5(f), re-
spectively, in contrast with the distinct dispersion morphologies
of dislocation loops. As a result, the total number densities of
both 1/2<111> and 100 loops in (Y, Al) ODS and (Y, Zr) ODS
at ∼72 dpa/local were (1.3 ± 0.2) × 1022 and (6.7 ± 0.7) × 1021
m−3 , respectively, with the corresponding averaged loop sizes of
(3.9 ± 0.9) and (4.2 ± 1.0) nm. Moreover, the fractions of 1/2<111>
loop were 79.9 % and 92.5 % for (Y, Al) ODS and (Y, Zr) ODS, re-
spectively. In the (Y, Ti) ODS at the same irradiation condition (RT,
∼72 dpa/local), the averaged number density and size of disloca-
tion loops were (4.1 ± 0.7) × 1022 m−3 and 2.8 ± 0.7 nm, respec-
tively [22]. Because of the similar sizes of dislocation loops, the
higher density of dislocation loops demonstrated more interstitial
defects formed in the ion-irradiated ODS steels.
3.2. Experimental measurements of nanoindentation (NI) hardness
Figs. 6(a) and 6(d) show the depth profiles of the averaged
nanoindentation hardness (HNI ) of (Y, Al) ODS and (Y Zr) ODS,
respectively, before and after irradiations, where all averaged HNI
continuously decrease with increasing the indentation depth (h)
to 20 0 0 nm, due to the indentation size effect (ISE). The relative
hardening (HIrr /HUnirr - 1) was plotted in Figs. 6(b) and 6(e), where
HIrr and HUnirr are the average hardness values at the indentation
depth of the unirradiated and the irradiated specimens, respec-
tively. The measured hardness at the indentation depth less than
150 nm, which is strongly affected by the specimen surface condi-
tions such as oxidation, roughness [51], was not considered. From
150 to approximately 330 nm the relative hardening increased fast,
and then decreased slowly from approximately 330 to 20 0 0 nm.
The increasing relative hardening (150 – 330 nm) is mainly as-
cribed to the increasing displacement damage with depth. Beyond
6
Acta Materialia 234 (2022) 117991
about 330 nm, the PDZ expanded to the unirradiated substrate to
cause the decrease of the relative hardening. It was found by the
FEM simulations that the PDZ at the indentation depth less than
330 nm was limited within the irradiated region (0 – 2220 nm).
In Nix-Gao model [30] based upon strain gradient plasticity
(SGP) theory, the ISE is modelled by using the concept of GNDs for
a crystalline material, as shown schematically in Fig. 7. All GNDs
are assumed to be circular loops within a hemispherical volume V
given by the contact radius ac , where ac = h/tanθ , (90°-θ ) is the
apex angle of a conical indenter (see Fig. 7). The depth-dependent
density ρ G of GNDs is defined as the total line length λ of disloca-
tion loops divided by the hemispherical volume V [30]:
π hac
λ 3 tan2 θ
ρG = = b
= (6)
V 2
3
π a3c 2 bh
where b is the Burgers vector (0.248 nm for 1/2<111> dislocations
in ferrite). Moreover, the nanoindentation (NI) hardness H at a cer-
tain indentation depth h is given by the following formula [30]:
 
H ρG h∗
= 1+ = 1+ (7)
H0 ρS h
where H0 is the depth-independent bulk equivalent hardness only
related to the density ρ S of the statistically stored dislocations
(SSDs); h∗ represents a characteristic length that depends on the
indenter geometry (tanθ ), ρ S , and the shear modulus μ of a given
material. In spite of the damage gradient effect (DGE), Nix-Gao
model is still widely adopted to evaluate a bulk equivalent hard-
ness for a thin ion-irradiated layer [25,27,39,52].
Figs. 6(c) and 6(f) show the part plots of the square of the
measured hardness (HNI )2 against the reciprocal of the indenta-
tion depth 1/h, where the linear fitting in the indentation depth
P. Song, K. Yabuuchi and P. Spätig Acta Materialia 234 (2022) 117991

Fig. 6. The average hardness profiles of (a) (Y, Al) ODS and (d) (Y, Zr) ODS, the corresponding profiles of relative hardening (HIrr /HUnirr −1) (b, e), and each plot of (HNI )2
versus inverse depth 1/h for (c) (Y, Al) ODS and (f) (Y, Zr) ODS, and (g) equivalent bulk hardness H0 measured for the indentation depth (150 nm < h <330 nm) of the ODS
ferritic steels including (Y, Ti) ODS [22] estimated by using Nix-Gao model, as well as (f) the corresponding hardening H0 as a function of nominal dpa.

range of 150 – 330 nm was used to evaluate the bulk equiva-
lent hardness of the surface thin layers for the unirradiated and
the irradiated specimen (see the dashed lines), and thus the aver-
aged H0 values were deduced. Although the CSM during the ex-
perimental nanoindentation testing should cause the fluctuation of
the measured hardness, all the values of R-squared factor (R2 ) (se-
lectively shown in Figs. 6(c) and 6(f)) were larger than 0.88, which
means the good linear fitting of H2 versus 1/h. The applicability of
Eq. (7) in the case of irradiated specimen is further discussed in
the Section 3.3. For the unirradiated ODS specimens, each plot of
(HNI )2 versus 1/h yielded a nearly straight line rather than a bi-
linear curve (see black lines in Figs. 6(c) and 6(f)). In other words,
the initial dislocations barriers (e.g. oxide particles) in ODS steels
ensured a continuous dislocation activity even at a small indenta-
tion depth (∼150 nm). The averaged H0 values of the unirradiated
(Y, Al) ODS and (Y, Zr) ODS were (4.42 ± 0.21) and (4.82 ± 0.20)
GPa, respectively, which can be converted to the corresponding
yield strength σ Y values of 933.6 and 1041.3 MPa of each ODS ma-
terial with the relationship:
 
σY (MPa ) ≈ 214 H0 × 103 MPa (8)
Large scatter in the measured H0 in Fig. 6(g) may be due to inho-
mogeneous microstructures or/and variable crystal orientations of
indented grains of ODS ferritic steels [28]. The amount of irradi-
ation hardening, H0 were obtained by subtracting the averaged
H0 of the unirradiated from the irradiated counterpart. As shown
in Fig. 6(h), it is apparent that the amount of hardening increased
considerably with dpa. Despite large scatters, (Y, Zr) ODS exhibited

7
P. Song, K. Yabuuchi and P. Spätig
Fig. 7. Geometrically necessary dislocations produced by a rigid conical indentation,
which are idealized as a circular dislocation loops in Nix-Gao model [30].
the lowest hardening at all nominal damage levels compared with
(Y, Al) ODS and (Y, Ti) ODS in our previous study [22]. The hard-
enings H0 (in GPa) of (Y, Al) ODS and (Y, Zr) ODS were fitted to
be H0 = 0.62 × (dpa)0.26 and H0 = 0.44 × (dpa)0.25 , respec-
tively. The exponents of those two ODS ferritic steels (also the m
in Eq. 3(b)) are in a good agreement with 0.25 – 0.3 of the Fe-(9
– 10)Cr alloys irradiated with Fe ions at RT [26,52], although the
exponent of (Y, Ti) ODS is 0.16 much smaller than the other ODS
ferritic steels. The possible reason of this difference among the ODS
steels will be discussed in the Section 3.4.
3.3. FEM simulation for hardening, plastically deformed zone and
GNDs
Based on the elastic-plastic properties of the unirradiated spec-
imens for (Y, Al) ODS and (Y, Zr) ODS, the curves of load versus
indentation depth were obtained through FEM simulations, which
are plotted in red dashes in Figs. 3(b) and 3(c). For the unirradi-
ated cases, the parameter Sred values of (Y, Al) ODS and (Y, Zr) ODS
were (6.0 ± 1.5) × 10−4 and (8.0 ± 1.8) × 10−4 , respectively. These
discrepancies were possibly caused by the harmonic displacement
oscillation of the CSM or the residual surface roughness [53].
Previous works [6,54–58] revealed that, the neutron irradia-
tions modified the elastoplastic and plastic instability behaviors
of bcc and hcp metals or alloys to some extent, which depended
much on the neutron fluence, irradiation temperature and initial
microstructures (e.g. grain size). Furthermore, the true stress-true
strain curves after the yield point showed nearly same continu-
ous strain hardening tendency with those of the unirradiated steels
[54,56]. Maloy et al. [54] ascribed this phenomena to the fine grain
size on the order of 1 μm or less, which can produce high strain
hardening rates and limit the length and propagation of nascent
localized shear bands. In this work, the two FeCrAl(Zr)-ODS fer-
ritic steels have ultrafine grain sizes less than 1 μm [19]. Thus
it was assumed that the strain hardening behavior of the stud-
ied ODS ferritic steels was the same before and after irradiation,
which is shown in Fig. 3(a). This assumption is further supported
by the analysis of various metals (bcc, fcc, hcp) in terms of true
stress-true strain curves, where all strain-hardening rates were
nearly not affected by the neutron irradiations at low temperatures
(< 200 °C), even in the case of localized deformation through dis-
location channeling induced by irradiation [58]. After taking the
depth dependence of displacement damage into account, the load-
depth curves for the 50 dpa/nominal could be obtained through
the FEM simulations (see Fig. 2) for a given C in Eq. (3b). With
the parameter C adjusted to be 153.6 and 158.4 for (Y, Al) ODS
and (Y, Zr) ODS, respectively, the corresponding values of the pa-
rameter Sred were (6.2 ± 2.4) × 10−4 and (5.3 ± 1.5) × 10−4 ,
which explained good consistency between FEM simulation and
8
Acta Materialia 234 (2022) 117991
Table 1
Maximum depth Z of plastically deformed zone (PDZ) at the indentation depth of
330 nm for equivalent plastic strain ε eq of 0.002 and 0.019.
FeCrAl(Zr)-ODS steels Y-Al-ODS Y-Zr-ODS
ε eq > 0.002 > 0.019 > 0.002 > 0.019
Z, nm of the unirradiated 2732.0 1936.8 2646.9 1904.0
Z, nm of the 50 dpa/nominal 2974.1 2119.8 2815.3 1990.0
nanoindentation experiments. The corresponding FEM load-depth
curves are also shown in Figs. 3(b) and 3(c) for the case of the 50
dpa/nominal. We recognized here that if the strain hardening rate
n would be affected by irradiation, then that the fitted parameter
C with Eqs. (3a) and (3b) would be in turn affected.
Another important issue is the relation between the PDZ size
and the density of GNDs. Figs. 8(a) and 8(b) show the contour plots
of equivalent plastic strain (PEEQ) larger than 0.2 % for (Y, Al) ODS
before and after the ion-irradiation at 50 dpa/nominal at the in-
dentation depth h of 330 nm, which corresponds to the measured
relative hardness peak (see Figs. 6(b) and 6(e)). The PDZ shown
in Figs. 8(a) and 8(b), expanded much deeper than the indenta-
tion depth and also along the specimen surface beyond the con-
tact radius, which was much larger than the PDZ defined in Nix-
Gao model (see Fig. 7) for which the contact radius corresponds to
the plastic zone radius. For the equivalent plastic strain ε eq > 0.2
% or 1.9 %, the values of the maximum depth Z below indenter are
displayed in Table 1. The PDZ size (ε eq > 0.2%) turned out to be
8 – 9 times the indentation depth, irrespective of ion irradiations.
In fact, we can regard Z as the radius of a hemispherical plastically
deformation zone and the scaling factor f was defined as the ratio
of Z to the contact radius ac :
f = Z / ac (9)
In the case of 50 dpa/nominal at h = 330 nm, the PDZ radius Z for
εeq > 0.2 % and > 1.9 % were 2815.3 – 2974.1 nm and 1990.0 –
2119.8 nm, respectively. The latter is similar with the depth range
(0 – 2220 nm) of the ion-irradiated layer. However, the larger PDZ
(for ε eq > 0.2 %) clearly extends into the soft unirradiated sub-
strate. So the PDZ size at ε eq > 1.9 % was considered to estimate
the density of GNDs. Durst et al. [59] found that, compared with
the strain limit ε eq of 0.2 %, the PDZ at ε eq > 1.5% gave rise to a
reasonable estimation of the density of GNDs and the NI hardness
for various metallic materials. Thus, after replacing the contact ra-
dius ac with Z, the density of GNDs in Eq. (6) is rewritten as:
π hZ
λ 3 h 3 tan2 θ
ρG = = b
= = (10)
V 2
3
π z3 2 b( f ac )2 2 f 2 bh
Accordingly, the relationship of H versus h in the Nix-Gao model
becomes
 
H ρG h∗
= 1+ = 1+ (11)
H0 ρS f 2h
For ε eq > 1.9%, the ratio f and the density of GNDs are shown
Fig. 9 as a function of indentation depth. In the unirradiated cases,
the ratio f was almost depth-independent and around 1.95, which
means that the constant value of the slope h∗ /f2 ensured the va-
lidity of the linear fitting on the experimental plots of H2 versus
1/h. However, in the cases of 50 dpa/nominal, the ratio f decreased
from 1.95 to 1.8 at the indentation depth h < 330 nm, and then
went up quickly to approximately 2.2 at h > 330 nm. Although
it is recommended to consider the depth dependence of homoge-
nously distributed microstructures (e.g. radiation defects or clus-
ters) when using the Nix-Gao model to obtain a bulk equivalent
nano-hardness, the Nix-Gao model could be valid in the case of
P. Song, K. Yabuuchi and P. Spätig
Fig. 8. Contour plots of different equivalent plastic strains in (Y, Al) ODS before irradiation (a) and after the irradiation up to 50 dpa/nominal.
Fig. 9. (a) the ratio f of Z to contact radius ac and (b) the density of geometrically
necessary dislocations (GNDs) as a function of indentation depth h.
ion-irradiated damages based on the good linear fitting on H2 ver-
sus 1/h in this work and also in others [27,39,52]. The reason can
be that, the slope h∗ /f2 is balanced by the decreased ratio f and the
increased ρ S with increasing depth. The densities of GNDs shown
9
Acta Materialia 234 (2022) 117991
in Fig. 9(b), which display close tendencies for the two FeCrAl(Zr)-
ODS ferritic steels, decreased from ∼1.1 × 1015 m−2 to ∼7.0 × 1014
m−2 for the 50 dpa/nominal when the indentation depth increased
from 200 nm to 300 nm, slightly higher than those of the unir-
radiated (ranging from ∼9.8 × 1014 m−2 to ∼6.7 × 1014 m−2 ).
For comparison we mention that, in the pure Ni irradiated with
6 MeV protons to 0.1 dpa at 120 °C, at the indentation depth of
∼200 – 300 nm, the density of GNDs varied from ∼2.0 × 1016
m−2 to ∼1.5 × 1016 m−2 , much higher than those of the unirra-
diated (∼7.0 × 1015 m−2 ) [60]. Such discrepancy can be associated
with the high density of statistically stored dislocations (SSDs) in-
side the as-received ODS steels, the motion and multiplication of
which can contribute much to the primary plastic deformation un-
derneath nanoindenter. Therefore, it is better to account for the
density of GNDs when estimating the irradiation-induced harden-
ing at a shallow reference depth.
The FEM method in this work, consisting of divided layers of
the irradiation region having a dose dependent hardening, could
certainly be considered for other materials (e.g. Fe-Cr alloy [26])
besides ODS steels. A sufficient number of discrete layers have to
be used so that the numerical solution does not depend on the
number of layers. Additionally, a large number of layers can reduce
the discontinuity in the deformation between adjacent layers.
3.4. Hardening mechanism
According to the results of FEM simulations, where the
dpa-dependence of yield strength σ Y is σ Y (MPa) = 933.6 +
153.6 × (dpa)0.26 and σ Y (MPa) = 1041.3 + 158.4 × (dpa)0.25 for
(Y, Al) ODS and (Y, Zr) ODS, respectively, the depth dependence
of yield strength is shown in Fig. 10. The stress increment σ
for (Y, Al) ODS and (Y, Zr) ODS at ∼72 dpa/local (50 dpa/nominal,
∼900 nm towards surface) was 467.1 and 461.3 MPa, respectively,
which are just larger than the counterparts of (353.1 ± 84.5) and
(240.3 ± 89.4) MPa, obtained by the Nix-Gao model on the basis
of Eq. (8). Accompanied by the dissolution of oxide particles, the
dissolved solute atoms (e.g. Y, O, Al, Zr) and radiation-induced
dislocation loops can act as short-range obstacles for dislocation
motion, hence, causing changes in the flow stress of ODS steels.
Actually, the square superposition law was valid just when obsta-
cle strengths are weak and nearly the same [61], the combined
P. Song, K. Yabuuchi and P. Spätig
Table 2
Hardness changes of two ODS steels contributed by oxide particles, dislocation loops and dissolved O interstitials.
Oxide particles at 0 dpa
Do , nm No , × 1021 m−2 σ o , MPa
(Y, Al) ODS 6.0 52 428.9
(Y, Zr) ODS 6.4 69 510.3
1) Strength factor of oxide particles α o : 0.4; 2) Strength factor of dislocation loops α l : 0.75.
Fig. 10. Depth dependence of yield strength of (Y, Al) ODS and (Y, Zr) ODS before
and after the ion-irradiation at 50 dpa/nominal.
change in the flow stress in this work was calculated by the
linear-superposition model:
σf = σl + σso − σo
where σ l , σ so and σ o represent the strengthening contribu-
tors by dislocation loops, solid atoms and oxide particles, respec-
tively. Furthermore, σ l and σ o can be expressed by the follow-
ing equation based on Orowan type bypassing mechanism [44]:
σ = Mαμb(Nd )0.5
where M is the Taylor factor (3.06); α is the barrier strength factor
of the contributor, being 0 – 1; μ is the shear modulus (80 GPa
for alpha iron); N and d are the number density and mean diam-
eter of the contributor, respectively. The strengthening produced
by dissolved solute atoms could be formulated linearly on the
concentration of solute atom CatX in bcc alloys. Oxygen atoms as
interstitials in bcc ferrite, having the strengthening coefficient of
around 10 0 0 MPa per at.% [62], contributed to 561.6 and 630.3 MPa
for (Y, Al) ODS and (Y, Zr) ODS MPa, respectively, which are shown
in Table 2. However, the strengthening coefficients of substitu-
tional solute atoms like Y (20 MPa per at.%) [62] and Al (9 MPa
per at.%) [63] are far smaller than that of O, so the corresponding
strengthening components (∼5 MPa for Y or Al) can be negligible.
The stress increments by O interstitials compensated the lost parts
of oxide particles for the corresponding obstacle strength factor
α o of 0.4 (see Table 2). As the strength factor of dislocation loops
α l to be 0.75, the final calculated stress increments of (Y, Al) ODS
and (Y, Zr) ODS were 456.9 and 361.5 MPa, respectively, which are
close to those obtained by the FEM simulation (at ∼72 dpa/local).
However, the strength factor of dislocation loops (0.75) in this
work is obviously larger than 0.17 – 0.34 for 1/2 111 loops
(7.6 ± 3.8 nm) in the 12Cr-6Al-ODS ferritic steel after neutron irra-
diation at 300 °C to 2.6 dpa [64]. This fact was possibly caused by
the underestimation of the loop density in this work, because tiny
Acta Materialia 234 (2022) 117991
Dislocation loops at 50 dpa/nominal O interstitials at 50 dpa/nominal Final stress
1)
Dl , nm Nl , × 1021 m−2 σ l , MPa 2)
CatO , at. % σ so , MPa σ f , MPa
3.9 13 324.2 0.56 561.6 456.9
4.2 6.7 241.5 0.63 630.3 361.5
dislocation loops cannot be fully imaged even under WBDF due to
their weak strain contrast. Another possibility might be an extra
contributor like oxygen-vacancy complexes. As numerous vacancies
were caused by ion irradiation at RT, oxygen-vacancy complexes
were expected to be formed because of the high affinity between
oxygen and vacancy in bcc Fe [42,43]. These oxygen-vacancy com-
plexes may trap screw dislocations via attractive interactions and
induce a considerate hardening in bcc alloys [65]. It was reported
that high density oxygen-vacancy complexes in bcc vanadium (V)
alloy caused the fracture modes from dimple to a fully transgraular
cleavage as the oxygen concentration increasing from 0.1 to 1.6 at.%
[65].
In the irradiated ODS ferritic steels, both oxide particles and ra-
diation defects impeded the motion of dislocation lines. The num-
ber density of the former was continuously decreased by irradia-
tion (see Fig. 4(b)), which is much more significant in (Y, Ti) ODS
than the other two steels. This result indicates that in (Y, Ti) ODS
dose dependence of hardening, namely the exponent, can be lower
(see Fig. 6(h)). Actually, accompanied by the particle dissolution,
more radiation defects particularly interstitial loops would be ac-
cumulated in (Y, Ti) ODS due to the weakened trapping capacity of
P-M interfaces. In (Y, Al) ODS and (Y, Zr) ODS, the dispersion mor-
phology of oxide particles responded similarly and less sensitive
to ion irradiations at RT. So the exponent of ∼0.25 in Fig. 6(h) has
been considered to be adequate to describe fluence dependence re-
(12) flecting the accumulation of radiation defects.
The simulation work based on density functional theory re-
vealed that four distinct Y2 O3 -Fe interfaces can trap strongly both
interstitial and vacancy defects via long-range attraction [66]. The
trapping effect of particle-matrix (P-M) interfaces on point defects
can be measured by the sink strength of oxide particles Zo , be-
(13) ing commonly expressed by 4π No do , where No and do are num-
ber density and diameter of oxide particles, respectively [5]. Prior
to irradiation, the initial sink strengths of oxide particles for (Y,
Ti) ODS, (Y, Al) ODS and (Y, Zr) ODS were 20.7 × 1014 , 7.5 × 1014
and 13.6 × 1014 m−2 , respectively [11]. This is consistent with the
lower hardening of (Y, Zr) ODS compared to (Y, Al) ODS, which was
mainly ascribed to the dislocation loops formed in the latter (see
Table 2). It is expected that, at a low displacement damage, the
minimum amount of radiation defects would be produced inside
(Y, Ti) ODS. However, this is in contrast with the fact that the hard-
ening was slightly higher in (Y, Ti) ODS than the other two at 2
dpa/nominal (see Fig. 6(h)). The reason is possibly that, tiny oxide
particles in (Y, Ti) ODS cannot trap self-interstitials in an efficient
way because of their coherent particle-matrix (P-M) interfaces of
a low interfacial energy [20,33]. Likewise, the response of grain
boundaries (GBs) to point defects depended much on GB crystal-
lographic parameters such as coherency and misorientation angle
[67–70], while low energy GBs presented weaker capacity of trap-
ping point defects than high energy GBs [68,70].
4. Conclusions
Two FeCrAl(Zr)-ODS ferritic steels, named by (Y, Al) ODS and (Y,
Zr) ODS, were irradiated with 6.4 MeV Fe ions up to nominal dis-
placement damages of 2, 10 and 50 dpa at RT. Irradiation-induced
10
P. Song, K. Yabuuchi and P. Spätig
hardening, plastically deformed zone (PDZ), geometrically neces-
sary dislocations (GNDs) and post-irradiation microstructures were
investigated by experimental nanoindentation (NI) measurements,
FEM simulation and TEM observations. Main results are as follow-
ings:
1) Experimental NI measurements revealed that, the radiation
hardening of the two FeCrAl(Zr)-ODS steels increased contin-
uously with elevating the nominal displacement damage. Af-
ter taking the damage gradient effect (DGE) into account, the
dependence of the irradiation hardening (in MPa) on local
dpa through the FEM simulations was demonstrated to be
153.65 × (dpa)0.26 and 158.35 × (dpa)0.25 for (Y, Al) ODS and
(Y, Zr) ODS, respectively.
2) The similar hardening behaviors of both steels were related
to the close dispersion morphologies of oxide particles at a
given dpa, which affected the accumulation of radiation defects
particularly interstitial dislocation loops in specimens. More-
over, the irradiation-induced stress increments were mainly
contributed by the dissolved oxygen and the dislocation loops
formed.
3) The PDZ sizes at the equivalent plastic strain ε eq > 0.2 % for
the ODS steels before and after irradiations were ∼8 – 9 times
of the indentation depth. However, the PDZ sizes at the strain
limit ε eq > 1.9 % agreed well with the depth dependence of the
relative hardening and were adopted to estimate the density of
GNDs.
4) According to the strain gradient plasticity (SGP) theory, the es-
timated densities of GNDs in the two FeCrAl(Zr)-ODS under in-
dentation were close: they decreased from ∼1.1 × 1015 m−2 to
∼7.0 × 1014 m−2 for the 50 dpa/nominal when the indenta-
tion depth increased from 200 nm to 300 nm, slightly higher
than those of the unirradiated (ranging from ∼9.8 × 1014 m−2
to ∼6.7 × 1014 m−2 ).
Declaration of Competing Interest
The authors declare that they have no known competing finan-
cial interests or personal relationships that could have appeared to
influence the work reported in this paper.
Acknowledgments
The authors are also grateful to the technical support by mem-
bers of Application of Duet and Muster for Industrial Research and
Engineering (ADMIRE), Kyoto University. The first author wishes
to thank Prof. em. Akihiko Kimura at Kyoto University for fruit-
ful discussion on hardening mechanisms of the ion-irradiated ODS
ferritic steels. The financial support of the Swiss National Science
Foundation (Grant No. 20 0 021_184695) is gratefully acknowledged.
Supplementary materials
Supplementary material associated with this article can be
found, in the online version, at doi:10.1016/j.actamat.2022.117991.
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