Nuclear Instruments and Methods in Physics Research B 267 (2009) 1505–1508

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Nuclear Instruments and Methods in Physics Research B

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

Ion-irradiation-induced damage of steels characterized by means

of nanoindentation
C. Heintze a,*, C. Recknagel a, F. Bergner a, M. Hernández-Mayoral b, A. Kolitsch a
a
Forschungszentrum Dresden-Rossendorf, P.O.B. 510119, 01314 Dresden, Germany
b
CIEMAT, Avenida Complutense 22, 28040 Madrid, Spain

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

Article history: Self-ion irradiation was used to simulate the damage caused by fast neutrons in the austenitic stainless
Available online 3 February 2009 steel SS 304 SA, the ferritic/martensitic steel Eurofer’97 and a Fe–9 at.%Cr model alloy. The irradiation-
induced hardness change in the damage layer was evaluated by means of nanoindentation. Three-step
PACS: irradiations were performed at room temperature and 300 °C up to 1 and 10 dpa. An irradiation-induced
61.80.Jh hardness change was shown for all materials. No influence of irradiation temperature could be resolved.
61.82.Bg Irradiation-induced hardening exhibits different fluence dependencies in Eurofer’97 and Fe–9 at.%Cr.
While the data indicate a saturation-like behaviour for Fe–9 at.%Cr, an increase of hardness with fluence
Keywords:
Self-ion irradiation
up to 10 dpa was found for Eurofer’97.
Nanoindentation Ó 2009 Elsevier B.V. All rights reserved.
Irradiation hardening
Iron base alloys

1. Introduction binary Fe–9 at.%Cr model alloy were investigated with two irradi-
ation fluences and two irradiation temperatures involved.
Austenitic stainless steels and ferritic/martensitic Cr-steels are
candidate materials for future nuclear applications such as Gener-
2. Experiments
ation-IV fission or fusion reactors. In these applications structural
materials of some components are exposed to intense irradiation
Composition, origin and heat treatment of the materials are
fields, high temperatures and mechanical loading. These conditions
summarized in Tables 1 and 2. Slices of 10  10  1 mm3 were
cause degradation of the mechanical properties. To ensure the
cut. All specimens were prepared by automatic grinding with
integrity and safety of these components the degradation mecha-
SiC-paper (up to 2500 grit) and polishing with diamond suspen-
nisms and their impact on the mechanical properties have to be
sion (particle size 3 and 1 lm). Single beam ion irradiations with
understood.
Fe-ions were performed with the 3 MV-Tandetron accelerator at
The investigation is devoted to the effect of irradiation on the
Forschungszentrum Dresden-Rossendorf, Institute of Ion Beam
mechanical properties. Self-ion irradiation was chosen to simulate
Physics and Materials Research. Irradiations were carried out at
the damage induced by fast neutrons for several reasons including
300 °C up to damage levels of 1 and 10 dpa and at room temper-
avoidance of activated material due to neutron irradiation, reduc-
ature (1 dpa only). The resulting damage profiles have been calcu-
tion of irradiation times and improved capabilities to vary irradia-
lated by means of the SRIM code version 2006.02 assuming an
tion conditions. However, due to the limited penetration depth of
average displacement energy of 40 eV [1]. A three-step irradiation
the ions special methods are needed to characterize the ion-in-
with different ion energies was applied to obtain a roughly rect-
duced damage.
angular damage profile (Fig. 1). The thickness of the damage layer
This investigation is focussed on the application of nanoinden-
is about 1.4 lm. The damage profile resulting from a one-step
tation. The aim is to verify the suitability of nanoindentation test-
irradiation with an energy of 5 MeV is presented for comparison.
ing for the purpose of damage characterization and to contribute to
It is important to note that the hardness results for the present
the understanding of irradiation hardening. An austenitic stainless
rectangular damage profile are more reliable than results for
steel, SS 304 SA, a reduced activation Cr-steel, Eurofer’97, and a
one-step irradiations [2] causing a non-monotonously graded
profile.
* Corresponding author. Tel.: +49 351 260 2127; fax: +49 351 260 2205. The depth-sensing nanoindentation measurements were car-
E-mail address: c.heintze@fzd.de (C. Heintze). ried out with the UNAT device (asmec GmbH) using a Berkovich in-

0168-583X/$ - see front matter Ó 2009 Elsevier B.V. All rights reserved.
doi:10.1016/j.nimb.2009.01.122
1506 C. Heintze et al. / Nuclear Instruments and Methods in Physics Research B 267 (2009) 1505–1508

Table 1
Chemical composition (wt%).

SS 304 Eurofer’97 Fe–9 at.%Cr

Cr 19.120 8.820 8.4
Ni 9.110 0.020 0.07
Mn 1.700 0.470 0.03
W – 1.09 –
V – 0.2 0.002
Ta – 0.13 –
C 0.025 0.110 0.02
P 0.026 0.005 0.012
Si 0.490 0.040 0.09
N 0.680 0.020 0.015
Cu 0.166 0.0016 –

Table 2
Origin and heat treatment.

Material Heat treatment Remark

Fig. 2. Load dependence of hardness of SS 304 SA in unirradiated condition and ion-
SS 304 SA Solution annealed Delivered by EDF, Les Renardier irradiated at 300 °C up to 1 dpa.
Eurofer’97 Normalized (980 °C/27 min/AC) Manufactured by
and tempered (760 °C/90 min/AC) Böhler (Austria),
production nr. T512,
batch 249, heat 83698,
in detail in [4] for SS 304 SA and Eurofer’97 and taken into account
plate 14.5 mm
Fe–9 at.%Cr Normalized (1050 °C/3 h/AC) Manufactured by SCK-CEN, Mol in the present discussion. The load dependence is further modified
and tempered (730 °C/4 h/AC) by the irradiation-induced formation of a harder damage layer. If
the indentation depth is smaller than about 10% of the thickness
of the damage layer, the hardness value should be representative
denter. Indentation loads in the range from 2 to 50 mN corre- of the layer. Otherwise, the hardness is a composite value
sponding to a maximum indentation depth from about 100 nm approaching substrate hardness at large indentation depth. It is
to 1 lm were applied. Corrections for system stiffness, indenter important to note that a one-step irradiation does considerably
area function and thermal drift were performed. The hardness val- complicate interpretation because of the graded nature of the dam-
ues for each load were determined from at least 10 load-depth age layer (Fig. 1).
curves analyzed according to [3]. For Fe–9 at.%Cr (300 °C, 1 dpa) For SS 304 SA (300 °C, 1 dpa) we have observed an irradia-
the irradiated region was characterized by means of TEM. tion-induced hardness increase of 0.5 to 1 GPa at low loads.
There is a hardness increase of 0.23 GPa at an indentation load
3. Results of 5 mN for Eurofer’97 (300 °C, 1 dpa). However, this increase
is not significant taking into account the error range and the re-
The load dependence of hardness obtained for the three materi- sults at the other indentation loads. In contrast a hardness in-
als in the unirradiated and ion-irradiated conditions is summarized crease is evident for the 10 dpa irradiation. It should be noted
in Figs. 2–4. The room temperature measurements are not included that a monotonous increase of hardness with increasing fluence
as the scatter bands coincide with the corresponding 300 °C/1 dpa is not in contradiction with the measurements. For Fe–9 at.%Cr a
irradiations of each material, i.e. no effect of irradiation tempera- significant increase of hardness was found for the 1 dpa irradia-
ture could be resolved. tion. However no further increase was observed for 10 dpa indi-
For the unirradiated conditions we have observed the well- cating a saturation-like behaviour in contrast with the finding
known indentation size effect (ISE). This effect was investigated for Eurofer’97.

Fig. 1. Damage profile calculated by SRIM for a three-step irradiation up to 1 dpa using energies of 500 keV, 2 and 5 MeV and fluences of 1.8  1014, 2.9  1014 and
5.6  1014 cm 2, respectively, (solid line) and for a one-step irradiation (dotted line).
 C. Heintze et al. / Nuclear Instruments and Methods in Physics Research B 267 (2009) 1505–1508 1507

Fig. 3. Load dependence of hardness of Eurofer’97 in unirradiated condition and

ion-irradiated at 300 °C up to 1 and 10 dpa.

Fig. 5. TEM micrograph for Fe–9 at.%Cr (1 dpa, 300 °C).

material, TEM [8] revealed loops of mean diameter 13 nm and

Fig. 4. Load dependence of hardness of Fe–9 at.%Cr in unirradiated condition and
ion-irradiated at 300 °C up to 1 and 10 dpa.
The TEM investigation revealed a distribution of dislocation
loops in Fe–9 at.%Cr ion-irradiated at 300 °C up to 1 dpa (Fig. 5).
4. Discussion
number density 1.7  1021 m 3 and SANS [9] indicated the pres-
ence of three-dimensional irradiation-induced features of mean
diameter 2 nm. The ratio of magnetic and nuclear scattering im-
plies that the clusters are different from pure vacancy clusters,
i.e. they must contain Cr. The formation of dislocation loops is also
confirmed by TEM investigations performed for Fe–9.7 at.%Cr irra-
diated at room temperature up to 1 dpa [2].
Each of the irradiation-induced features listed above contrib-
utes to the hardening and is therefore a potential candidate to ex-
plain the observed increase of hardness. In the present stage of
investigation it is not possible to separate the individual contribu-
tions or to quantify the expected hardness increase.
The measurements (Fig. 6), although limited to only two data
points for each material, revealed a difference in the fluence
dependence of the irradiation-induced hardness change of Euro-
fer’97 and Fe–9 at.%Cr even though their composition is similar
with regard to the Cr-content. While we have observed an increase
of the irradiation-induced hardness change with fluence (compat-
ible with a proportionality to the square root of fluence) up to
10 dpa for Eurofer’97, the data indicate a saturation-like behaviour
for Fe–9 at.%Cr. This finding clearly shows the synergistic effect of

For a tentative interpretation of the results we assume that the

damage in units of dpa is the dominant parameter. We therefore
ignore the effect of secondary parameters such as type and energy
of particles and flux.
For the same lot of SS 304 SA a TEM investigation of neutron-
irradiated samples (0.8 dpa, 330 °C) revealed the presence of dislo-
cation loops with average diameter of 4.7 nm and number density
4.5  1022 m 3 [5]. Voids or He bubbles were observed only at
much higher dose.
For neutron-irradiated Eurofer’97 (1.5 dpa, 300 °C) the presence
of loops of mean diameter 16 nm and number density 2  1021 m
3
was estimated by means of TEM [6]. An irradiation-induced in-
crease of the total intensity was observed in a small-angle neutron
scattering (SANS) investigation of neutron-irradiated (2.7 dpa,
300 °C) Eurofer’97 [7]. The features were tentatively interpreted
as nanovoids or bubbles [7].
Our own TEM investigation into ion-irradiated Fe–9 at.%Cr
(1 dpa, 300 °C) revealed a distribution of dislocation loops. For Fig. 6. Fluence dependence of the irradiation-induced hardness change in Euro-
the neutron-irradiated condition (1.5 dpa, 300 °C) of the same fer’97 and Fe–9 at.%Cr at an indentation load of 5 mN
1508 C. Heintze et al. / Nuclear Instruments and Methods in Physics Research B 267 (2009) 1505–1508
additional alloying elements (e.g. C and Mn) on the kinetics of irra-
diation hardening.
5. Conclusion
Nanoindentation is a useful tool to determine the irradiation-
induced hardness change in the damage layer of ion-irradiated iron
base alloys. However care has to be taken to account for the inden-
tation size effect and for the influence of the damage profile on the
measured hardness value. A three-step irradiation is suitable to ap-
proach a rectangular damage profile and to derive the hardness in-
crease representative of the damage in units of dpa, whereas a one-
step irradiation is not sufficient.
An irradiation-induced hardness change has been demonstrated
for all materials and microstructural evidence of hardening fea-
tures has been collected. No influence of irradiation temperature
could be resolved in the studied temperature range, but a differ-
ence in fluence dependence of the irradiation-induced hardening
was shown for Eurofer’97 and Fe–9 at.%Cr. This difference is likely
to be caused by the presence of additional alloying elements in
Eurofer’97.
Acknowledgement
The examined materials were kindly provided by EDF R&D, Prof.
R. Pippan (University of Leoben) and SCK-CEN, Mol.
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