Nuclear Materials and Energy 36 (2023) 101455

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Nuclear Materials and Energy

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

Effects of thermal aging at 873 K on the impact properties of an ODS

ferritic steel
M. Oñoro *, T. Leguey , V. de Castro , M.A. Auger
Department of Physics, Universidad Carlos III de Madrid, Avda. de la Universidad 30, 28911 Leganés, Madrid, Spain

A R T I C L E I N F O A B S T R A C T

Keywords: This investigation presents the effects of long-term thermal aging on the impact properties of an ODS reduced
ODS RAF steel activation ferritic steel. The ODS ferritic steel, with composition Fe–14Cr–2W–0.4Ti–0.3Y2O3 (wt. %), was
Thermal aging manufactured by mechanical alloying, compacted by hot isostatic pressing and hot cross rolled. A 1273 K
Charpy test
annealing treatment was applied, followed by thermal aging at 873 K for 2000 h in Ar, to evaluate the thermal
DBTT
EBSD
stability of the alloy.
Charpy impact testing was performed from 77 to 473 K to investigate the mechanical response of the material
under dynamic loads. The ductile-to-brittle transition temperature (DBTT) showed a slight increase with values
of 255 ± 12 K before aging, and 270 ± 20 K after aging. The aging treatment softened the steep character of the
Charpy impact curves inducing a wider transition regime with mixed brittle and ductile fracture mechanisms.
This behavior was confirmed by the analysis of Force vs. Displacement Charpy curves and fractographic ob­
servations. Hot cross rolling induced a crack divider geometry and secondary cracks formation by delamination.
Ductile fracture was less evident after aging due to the redistribution and transformation of Cr-W-rich pre­
cipitates along grain boundaries. Electron Backscattered Diffraction highlighted the features of transgranular
brittle cracks at temperatures below the DBTT and showed misoriented and deformed regions near the fracture
surface at temperatures above the DBTT.

Introduction Oxide dispersion strengthened (ODS) reduced activation ferritic

Nuclear fusion and Generation IV fission reactors will define the
main pillars of a future green economy sustained by renewable and clean
energy generation. The development of fusion experimental devices as,
nowadays, ITER and the forthcoming DEMO are keystones for this
purpose [1,2]. Those reactors represent the convergence of the inter­
national scientific community efforts and stand for an unprecedented
agreement between politic organizations and scientific institutions.
Fusion materials science investigates state-of-the-art materials for these
reactors to obtain higher conversion efficiencies, less waste and
extended operational lifetimes that will allow for achieving economi­
cally viable commercial fusion power plants [3].
These materials will be submitted to unprecedented operational con­
ditions: extremely high temperatures, severe radiation damage, thermal
and pressure shocks, and chemically reactive environments that can lead
to compatibility issues with flowing coolants [4]. Therefore, detailed in­
vestigations are essential to assess how the harsh environment inside the
reactor will affect the properties of its structural components.
(RAF, >12 wt% Cr) and reduced activation ferritic/martensitic (RAFM,
< 12 wt% Cr) steels are being widely investigated as improved material
candidates for structural systems and components [5,6]. The develop­
ment of ODS RAF and RAFM steels aims to increase the maximum
operational temperature of the structural materials above 823 K, its
actual limit. ODS steels contain a homogeneous distribution of oxide
nanoparticles within their matrix, usually introduced by the mechanical
alloying of nanometric powders [7,8]. Ti addition enhances and refines
the nano-oxide dispersion resulting in Y-Ti-O complex nano-oxides,
thermally stable at elevated temperatures [9], which confer enhanced
high-temperature strength and adequate creep behavior to ODS RAF and
ODS RAFM steels [10]. The nanoparticles pin grain boundaries, impede
dislocation motion and act as sinks for radiation defects; they may
minimize formation of voids and H/He gas bubbles from transmutation
elements, thus, improving radiation resistance.
ODS RAF steels can increase the upper operational temperature limit
up to 970–1070 K [11], around 100 K higher than their ODS RAFM
counterparts [12], enhancing the efficiency and power outcome of the

* Corresponding author.
E-mail address: monoro@fis.uc3m.es (M. Oñoro).

https://doi.org/10.1016/j.nme.2023.101455
Received 31 March 2023; Received in revised form 13 May 2023; Accepted 26 May 2023
Available online 19 June 2023
2352-1791/© 2023 The Authors. Published by Elsevier Ltd. This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-
nc-nd/4.0/).
M. Oñoro et al. Nuclear Materials and Energy 36 (2023) 101455

Table 1
Chemical composition (wt. %) of the ODS steel powder after milling [15].
Fe Cr W Ti Y O C Al N Si S

Bal. 13.1 2.0 0.38 0.18 0.17 0.04 < 0.05 0.020 < 0.05 < 0.03

presented here, reported a decrease in ductility and a significant

Fig. 1. (a) Characteristic parameters of a Force vs. Displacement Charpy curve
(adapted from ISO 14556:2015).
embrittlement after long-term thermal aging [13]. They pointed to 14Cr
(wt. %) as a promising chromium content in ODS RAF steels performing
adequately at service temperatures [14]. The main goal of this investi­
gation is to evaluate the performance of an ODS ferritic steel, as one of
the main structural materials candidates to be used in fusion power
plants, under the expected operational temperature of these reactors.
Thus, an ODS RAF 14Cr steel was submitted to long-term thermal aging
at 873 K for 2000 h in Ar, matching the expected operational temper­
ature of DEMO and future commercial fusion power plants [1]. In a
previous work [15], the thermal stability of the grain structure and
larger secondary phases at 873 K (Cr-W-rich and Ti-rich precipitates) of
this same ODS ferritic steel was already assessed and correlated with its
tensile properties. In this investigation, the thermal stability and me­
chanical response against dynamic loads have been studied by instru­
mented Charpy impact tests before and after thermal aging.
Charpy V-notch impact tests were performed from 77 to 473 K to
obtain the ductile-to-brittle transition temperature (DBTT) value and the
characteristic parameters of instrumented Force vs. Displacement
Charpy curves. Lateral expansion and surface fractographic character­
istics were determined by optical microscopy (OM) and scanning elec­
tron microscopy (SEM) image analysis, respectively, and Electron
Backscattered Diffraction (EBSD) maps were acquired to investigate the
fracture propagation mechanisms.
Results are summarized and discussed with focus on the effects of
thermal aging on the impact resistance of the analyzed ODS ferritic steel.

Experimental

An ODS steel with nominal composition Fe–14Cr–2W–0.4Ti–0.3Y2O3

(wt. %) was manufactured by milling atomized prealloyed Fe–Cr–W–Ti
powder (Nanoval GmbH & Co. KG) and nanosized Y2O3 powder, 99.995 %
purity (SkySpring Nanomaterials, Inc.). Powders were mechanically
alloyed in a Retsch PM400 planetary ball mill under H2 atmosphere, using
austenitic steel vessels, AISI 52100 steel balls, and a 10:1 ball to powder
ratio. The chemical composition of the milled powder is summarized in
Table 1. The milled ODS powder was canned, degassed, and compacted by
HIP at 1373 K for 2 h at 175 MPa of Ar pressure; the consolidated batches
were subsequently hot cross-rolled at 1223–1423 K obtaining a ~ 70 %
thickness reduction. Details of the processing route are stated in [15,16].
Fig. 2. Ductile-to-brittle curves for ODS-R and ODS-A showing the Charpy After HCR, annealing at 1273 K for 2 h was found to optimize the
absorbed energy vs. Test temperature. mechanical properties of the ODS steel [15]. Therefore, this treatment
was applied to all the remaining batches before any further treatment.
This set of samples will be referred now on as ODS-R, taken as reference.
Table 2 Thermal aging at 873 K in Ar for 2000 h followed by air cooling was
Summary of Charpy results for ODS-R and ODS-A, and LEX fitting parameters for applied on ODS-R to assess the long-term mechanical stability of the
ODS-R. ODS steel. This batch of thermal aged samples is denoted as ODS-A.
ODS-R ODS-A Subsized Charpy KLST samples were obtained by electroerosion in
the Transversal-Short (TS) plane with dimensions 3 × 4 × 27 mm3, 60◦
DBTT (K) 255 ± 12 270 ± 20
USE (J) 3.44 ± 0.15 3.2 ± 0.4 “V” notch angle, and 1 mm notch depth, following the ISO 148:2017 and
LSE (J) 0.0 ± 0.3 0.0 ± 0.4 ISO 14556:2015 regulations. Standard grinding and polishing processes
LEX fitting curve y = (0.111 ± 0.004) × + (0.01 ± 0.01) – were used for final sample preparation before testing. Instrumented
LEX R-Square fit 0.970 –
Charpy impact tests were performed in a Zwick/Roell HIT50P instru­
ment equipped with a 25 J pendulum energy following the ISO
system. Although ODS RAF steels have been broadly investigated during 148:2017 requirements. The impact speed was 3.8 m/s (ISO 148:2017)
the last two decades [10], it is still essential to achieve a comprehensive and the test temperatures ranged from 77 to 473 K. The DBTT was
characterization of the structural material candidates’ behavior at calculated by fitting the experimental results to a sigmoidal regression.
relevant temperatures in the long term. Previous studies on ODS ferritic Load vs. Time Charpy curves were automatically recorded with the
steels, considering different thermomechanical treatments than those equipment software testXpert II. Force vs. Displacement Charpy curves
offer detailed information by allowing a comprehensive analysis of

2
M. Oñoro et al.
Fig. 3. LEX parameter for ODS-R and ODS-A as a function of the Charpy absorbed energy at different test temperatures. Representative OM images (insets) of the
fracture surface of different broken specimens are included.
traditional Charpy impact tests. Force vs. Displacement curves obtained
from raw data were analyzed with the NIST Instrumented Charpy
Analysis Software (NICAS) [17]. The instrumented Charpy curves can be
classified according to ISO 14556:2015, and the force at general yield,
the maximum force, the force at initiation of unstable crack, and the
force at crack arrest, can be extracted from these curves (Fig. 1).
OM images of the fracture surface were used to calculate the Lateral
Expansion coefficient (ISO 148–1:2017). Fractographic surface obser­
vations were performed by SEM in secondary electron (SE) mode in a FE-
SEM TENEO LoVac microscope and EBSD maps were acquired on the
Longitudinal-Transverse (LT) plane with an EDAX Velocity Pro camera.
For EBSD analysis, Charpy samples were polished on the LT plane to
eliminate defects and surface tensions and, thus, to reveal the properties
of the fracture mechanisms. EBSD data processing and analysis was done
with the MTEX tool [18]. Minimum grain size was fixed to 15 px, the
Fig. 4. Force at general yield (Fgy) as a function of test temperature for ODS-R
and ODS-A.
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Nuclear Materials and Energy 36 (2023) 101455
minimum confidence index (CI) to 0.1, low-angle grain boundaries
(LAGB) were defined as those in the 5 – 10◦ interval and high-angle grain
boundaries (HAGB) as those with misorientations larger than 10◦ .
Results and discussion
Charpy impact resistance properties
The impact resistance and the mechanical response of the ODS steel
were studied in the reference material (ODS-R) and after the thermal
aging treatment (ODS-A). Due to the limited amount of material avail­
able, two or three samples were tested at each temperature. Fig. 2 dis­
plays the absorbed Charpy impact energy as a function of the test
temperature, giving rise to the characteristic ductile-to-brittle transition
curves. A sigmoidal regression (1) was used to fit the experimental
Fig. 5. Maximum force (Fm) as a function of test temperature for ODS-R and
ODS-A.
M. Oñoro et al. Nuclear Materials and Energy 36 (2023) 101455

Fig. 6. Force at initiation of unstable crack (Fiu) and force at crack arrest (Fa) as
a function of displacement for ODS-R and ODS-A.

results across the test temperature range that includes the lower shelf
energy (LSE), the upper shelf energy (USE) and the transition region.
USE − LSE
y(T) = LSE + T− DBTT (1)
1 + e− dT
A least squares algorithm was used to minimize the deviations of the
theoretical curve from the experimental points, and the Levenberg-
Marquardt (L-M) algorithm to adjust the parameter values in the itera­
tive process. During the iterations, LSE, USE, DBTT and dT were con­
strained to positive values. A summary of the results of the fits is shown
in Table 2.
After aging, the DBTT slightly increases and the USE decreases
although both values remain within the error limits. The DBTT shifts
from 255 ± 12 K to 270 ± 20 K. Fig. 2 shows that the upper shelf energy
region of the Charpy impact curve is lower in ODS-A than in ODS-R, and
the fitted curve for ODS-A does not reach its USE in the temperature
range tested. Moreover, the Charpy impact curve for ODS-A softens at
the transition region losing the steeper transition observed in ODS-R.
Then, it is expected to find a wider transition region on ODS-A than
on ODS-R, with mixed ductile and brittle fractures. In any case, the
values obtained follow the trend of similar ODS ferritic steels [19–21]
and show the overall stability of this alloy after the thermal aging
treatment. These results also agree with the previous characterization
performed on the same ODS steels under (quasi-) static loads by tensile
testing [15]. Fig. 7. Low magnification fracture surface SE-SEM images for ODS-R and ODS-
The lateral expansion (LEX) parameter measures the change in width A at four representative test temperatures.
of the opposite face to the notch. It represents a measurement of the
ductility of the specimen under impact tests and it may help to describe
the transition regime in ferritic steels [22,23]. Fig. 3 shows the LEX
parameter as a function of the absorbed impact energy. For ODS-R, the
LEX parameter can be fitted to a linear regression (Table 2). ODS-A LEX (crystal cleavage). Final ductile fracture energy usually causes shear
values are more scattered, not allowing a good linear fit. Although the leaps formation.
impact energies in ODS-A tend to be smaller than in ODS-R, the LEX The force at general yield (Fgy) is a first approximation to the load
values do not decrease accordingly, implying some differences in the that causes initial plastic deformation across the entire sample width
fracture mechanism in the ductile regime. For both samples, lower LEX [25,26]. Fig. 4 represents Fgy as a function of the Charpy impact test
values correspond to lower test temperatures. temperature. Both samples follow a similar trend, where ODS-A values
The ductile-to-brittle transition is analyzed in greater detail by lay slightly below ODS-R results in the transition region. For both
means of the Force vs. Displacement instrumented Charpy curves samples, highest Fgy values are found at 253 K for ODS-R and 223 K for
(Fig. 1). The total absorbed energy represents the sum of three contri­ ODS-A (below this test temperature only brittle fracture takes place),
butions [24]: i) crack initiation up to the point of maximum force, ii) and lowest values occur at room temperature (RT = 298 K). Fig. 5 shows
crack propagation energy and iii) final ductile fracture energy. Crack maximum force values (Fm) as a function of the test temperature. As it
initiation energy involves elastic and plastic deformation. Crack prop­ can be seen, they behave in a very similar way before and after aging.
agation can be divided into stable plastic deformation (ductile crack Crack initiation, propagation and arrest are key concepts to describe
extension and ductile fracture), and unstable brittle crack breakthrough the appearance of brittle cracks in components or structures subjected to

4
M. Oñoro et al.
Fig. 8. SE-SEM fracture surface images of: (a) ODS-R and (c) ODS-A tested at 77 K showing the intergranular brittle fracture by delamination; and (b) ODS-R and (d)
ODS-A tested at 473 K illustrating the differences in the microcracks distribution.
operational loadings. Steels with very high fracture initiation toughness
(high Charpy energy) can sustain very high initial driving forces.
However, these materials often lack good resistance to crack propaga­
tion (low crack arrest toughness), which may lead to ultimate structural
failure. Particularly, the crack arrest resistance of ferritic steels is heavily
temperature dependent. Fig. 6 shows the results of the force at initiation
of unstable crack (Fiu) and the force at crack arrest (Fa) that characterize
the material performance against brittle crack initiation and propaga­
tion, respectively. In Fig. 6, the Fiu for ODS-R is well grouped at the
highest displacement values but, for ODS-A, the results are broadly
distributed. This is similar to the trend observed in Fig. 3 for the LEX
parameter. The dispersion of results in the plastic regime in ODS-A
correlates with the softening of the impact energy transition curve
observed, as smaller areas of the stable plastic deformation contribution
under the Force vs. Displacement curves correspond to lower Charpy
absorbed energies. Fa values are similar for both ODS-R and ODS-A,
being the displacements for ODS-A more scattered, as it happened for
Fiu. For both samples, lower displacement values correspond to lower
test temperatures.
Fractographic analysis
To assess the fracture mechanisms operating on the samples, before
and after thermal aging, surface fractographic analyses have been car­
ried out by SEM and EBSD.
Fig. 7 shows the fracture surface for both materials at different test
temperatures. Secondary cracks are observed as a result of the delami­
nation (crack divider geometry) associated to the HCR process [27]. For
tests at 77 K, a uniform surface with brittle facets is observed for ODS-R
(Fig. 7(a)). ODS-A only differs from ODS-R by having a slightly more
irregular surface (Fig. 7(b)). None of them showed developed secondary
cracks. Brittle fracture dominates the entire surface of both samples, and
it is characterized by both transgranular and intergranular quasi-
cleavage fracture modes, being the transgranular quasi-cleavage the
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Nuclear Materials and Energy 36 (2023) 101455
dominant one (Fig. 8(a) and Fig. 8(c)). A high amount of river patterns is
also present on the surface of facets (see example in Fig. 9(a)), deter­
mining crack initiation sites and the direction of crack propagation.
Short-ranged intergranular quasi-cleavage fracture perpendicular to the
HCR direction is also visible, although in a lower extent and less evident
in ODS-A than in ODS-R.
ODS-R tested at 193 K presents a similar general view as for tests at
77 K, although ductile regions with dimples start to form surrounded by
brittle facets (Fig. 10(b)). Moreover, the observed intergranular cracks
tend to be longer, in some cases ranging all along the fracture surface
(Fig. 10(a)), with transgranular brittle fracture through their inside
walls (Fig. 10(b)).
Increasing the test temperature to 223 K represents a change in the
fractographic behavior, corresponding to the onset of the transition re­
gion of the Charpy impact curve (Fig. 2). In ODS-A, the number and
depth of the delamination cracks maximize at this test temperature
(Fig. 11). They are characterized by a step/terrace system with brittle
facets on the terraces and ductile dimples on the steps (Fig. 11(b)). The
intergranular fracture is also influenced by the Cr-W-rich secondary
phases present at grain boundaries. After thermal aging, these pre­
cipitates were observed to redistribute and transform, increasing their W
content [15]. These secondary phases could lead to crack initiation,
promoting intergranular fracture. In ODS-R tested at 253 K (Fig. 12(a)),
long deep delamination cracks perpendicular to the notch are present,
similarly to ODS-A tested at 223 K. However, the step/terrace system is
not observed. Furthermore, coalescence of ductile dimples by trans­
granular fracture mode can be seen. These ductile regions are now more
evident and abundant, and they represent the main fracture mechanism
(Fig. 12(b)). The two samples exhibit different behavior in the regions
between the delamination cracks. ODS-R has several, short and wide
brittle microcracks with elongated cleavage facets, surrounded by
ductile regions (Fig. 12(c)). ODS-A presents fewer and narrower
microcracks.
In both materials, the ductile regions enlarge with increasing
M. Oñoro et al.
Fig. 9. SE-SEM fracture surface images for ODS-A at different test tempera­
tures: (a) Brittle facets with river patterns at 77 K, (b) ductile dimples at 276 K
and (c) ductile dimples at 323 K.
temperature. However, a fracture surface like the one observed in ODS-R
is not visible in the ODS-A samples until the temperature increases in ~
100 K respect to the reference material. Fig. 9(b) and Fig. 9(c) show the
details of ductile dimples in ODS-A, which tend to coalesce with
increasing test temperature. Precipitates (secondary phases) are
frequently observed inside them, probably acting as nucleation sites for
microvoids.
As it can be seen in Fig. 7, delamination occurs for both samples up to
the maximum test temperature of 473 K, even if the ductile fracture
mechanism predominates at those temperatures. Fig. 8(c) and Fig. 8(d)
show that at the highest test temperature the microcracks are less
evident in ODS-R than in ODS-A.
The fracture mechanisms originated during the Charpy tests propa­
gate from the fracture surface through the LT planes of the sample.
Therefore, EBSD maps were acquired on the ODS-A sample before and
after impact tests on the LT plane, from the surface and along the notch
depth direction. Three different test temperatures were selected to
perform EBSD measurements: 77, 223, and 473 K. These temperatures
were selected to highlight the characteristic features of the brittle, the
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Nuclear Materials and Energy 36 (2023) 101455
Fig. 10. SE-SEM fracture surface images of ODS-R tested at 193 K showing: (a)
Intergranular brittle fracture by delamination and (b) the dominating trans­
granular brittle fracture.
transition and the ductile fracture regimes observed in Fig. 2, respec­
tively. EBSD maps from untested specimens are additionally presented
for comparison.
Fig. 13 presents the pole figures for ODS-A on the 〈0 0 1〉, 〈0 1 1〉, and
〈1 1 1〉 directions. The aged ODS steel mostly shows a recrystallized
matrix with a 〈0 0 1〉 preferential orientation and a 〈1 1 1〉 second pref­
erential orientation. Fig. 14 shows the crystallographic orientation maps
with estimated grain boundaries outlining ferritic grains, and Fig. 15
shows the Kernel Average Misorientation (KAM) maps.
The EBSD map shown in Fig. 14(b), which corresponds to a specimen
tested at 77 K, shows an abrupt fracture surface, characteristic of a
brittle fracture. The presence of two secondary cracks can be observed in
the squared areas of the figure. Neither of these two cracks follow any
specific grain boundary, being clearly transgranular. Furthermore, it
does not appear to be any modification of the crystallographic orienta­
tion from the fracture surface to the interior of the sample. At 223 K
(Fig. 14(c)), the fracture surface is now characterized by a rougher edge
and does not exhibit the features of the brittle fracture, previously
observed at 77 K, showing the transition from the brittle regime to the
mixed (brittle and ductile) one. Crystal orientations 〈0 1 1〉 and 〈1 1 2〉
are present near to the surface, not corresponding to any preferential
orientation previously observed in the pole figures. Thus, fracture dur­
ing the Charpy test caused the crystallographic bending of this region
from the 〈1 0 0〉 preferential orientation, which is still present at the
interior of the material. At this temperature there is no visible secondary
crack formation, neither transgranular nor intergranular, neither at the
surface nor inside. The crystallographic orientation change confirms the
ductile behavior of the sample in this region. Fig. 14(d) shows the EBSD
map at 473 K, the highest test temperature. The edge of the sample is
rough, and no secondary cracks are observed, as it happened at 223 K.
M. Oñoro et al.
Fig. 11. SE-SEM fracture surface images of delamination for ODS-A tested at
223 K: (a) General view, (b) terrace-step system and (c) brittle facets and cracks
of different sizes surrounded by the increasing ductile regions.
KAM maps were based on a threshold angle of 2.5◦ to effectively
remove the subgrain boundaries and reveal local dislocation structures
of the deformed material. Untested ODS-A exhibits a similar general
behavior to ODS-A tested at 77 K (Fig. 15(a) and Fig. 15(b), respec­
tively). The area near the fracture surface shows the same average
misorientations as the bulk material, which confirms brittle fracture
without deformation. This trend changes considerably for the samples
tested at 223 and 473 K. The samples tested at 223 K reach higher
misorientation values near the fracture surface, while lower misorien­
tation values can be found at longer distances from the surface. The
samples tested at 473 K show high misorientation values along the entire
map, even at long distances from the surface (Fig. 15(c)). These maps
confirm the change in the deformation mechanisms observed at these
temperatures by OM, SEM and crystallographic EBSD maps.
Conclusions
In this study, the thermal stability and performance under dynamic
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Nuclear Materials and Energy 36 (2023) 101455
Fig. 12. SE-SEM fracture surface images at different magnifications for ODS-R
tested at 253 K: (a) General view, (b) region between delamination cracks and
(c) microcracks surrounded by ductile dimples.
loads of an ODS RAF steel before and after thermal aging at 873 K for
2000 h have been investigated. The mechanical response has been
studied by instrumented Charpy impact tests, and the principal fracture
mechanisms that operate in this alloy have been described using frac­
tographic analyses. The following conclusions can be stated:
• The thermal aging treatment performed on the ODS ferritic steel
softens the Charpy impact energy transition curves inducing a wider
transition region with mixed ductile and brittle fracture mechanisms.
The USE decreases after thermal aging and the DBTT value slightly
increases from 255 ± 12 K to 270 ± 20 K.
• After aging, initiation of unstable crack starts at lower displacement
values, limiting the energy absorbed by the material. The force at
general yield, Fgy, and the maximum force under dynamic loads, Fm,
are not significantly altered after aging.
• SEM analysis shows a mixed fracture mechanism behavior in both
materials, with elongated brittle cracks of different sizes, and ductile
regions that enlarge as the test temperature increases. While a fully
M. Oñoro et al.
Fig. 13. Pole figures for ODS-A: (a)-(c) Untested specimen and specimens tested at (d)-(f) 77 K, (g)-(i) 223 K and (j)-(l) 473 K.
brittle behavior is observed at the lowest test temperature, the
ductile regime is not fully achieved at the highest test temperature.
Aging decreases the extent of the ductile regions over the tested
temperature range.
• Brittle fracture is characterized by a dominating transgranular frac­
ture mode, accompanied by a moderate intergranular fracture mode
related with delamination in both materials, associated to the HCR
process. The redistribution and transformation of Cr-W-rich pre­
cipitates along grain boundaries after thermal aging may contribute
to the mixed fracture behavior observed at the transition regime.
Above 253 K, coalescence of ductile dimples is observed with
transgranular fracture mode that becomes dominant.
• In ODS-A, the EBSD analysis supports the OM and SEM observations
of the fracture modes. Secondary transgranular brittle cracks appear
at 77 K and KAM maps highlight the absence of deformation, char­
acteristic of brittle fractures, at this test temperature. At test tem­
peratures near and above the DBBT, highly misoriented and
deformed regions are observed; preferential orientations change
from 〈0 0 1〉 and 〈1 1 1〉 to 〈0 1 1〉 and 〈1 1 2〉 directions.
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Nuclear Materials and Energy 36 (2023) 101455
• To summarize, thermal aging under the present conditions does not
alter notably the impact resistance of the investigated ODS ferritic
steel, but a small decrease in the ductile behavior with enhanced
intergranular fracture is evidenced.
CRediT authorship contribution statement
M. Oñoro: Investigation, Writing – original draft, Writing – review &
editing, Visualization. T. Leguey: Investigation, Writing – original draft,
Writing – review & editing, Supervision, Funding acquisition. V. de
Castro: Investigation, Writing – original draft, Writing – review &
editing, Supervision, Funding acquisition. M.A. Auger: Investigation,
Writing – original draft, Writing – review & editing, Supervision,
Funding acquisition.
Declaration of Competing Interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
M. Oñoro et al. Nuclear Materials and Energy 36 (2023) 101455

Fig. 14. EBSD crystallographic orientation maps for ODS-A: (a) Untested
specimen and specimens tested at (b) 77 K, (c) 223 K, and (d) 473 K. Fig. 15. KAM maps for ODS-A: (a) Untested specimen and specimens tested at
(b) 77 K, (c) 223 K, and (d) 473 K.

9
M. Oñoro et al.
Data availability
Data will be made available on request.
Acknowledgements
Funding from Agencia Estatal de Investigación (PID2019-105325RB-
C33/AEI/10.13039/501100011033), and Comunidad de Madrid
through the programs Talento-CAM (2017-T1/IND-5439 and 2021-5A/
IND-20954), the V PRICIT (EPUC3M14), and TECHNOFUSIÓN(III)CM
(S2018/EMT-4437) is gratefully acknowledged. M.A. Monge is also
acknowledged for providing technical advice and support with the EBSD
measurements.
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