Journal of Nuclear Materials 509 (2018) 496e503

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Journal of Nuclear Materials

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

The effect of He ions irradiation on the micro-structure and property

of CLF-1 steel
Xiaonan Zhang a, Xianxiu Mei a, *, Xingzhong Cao b, Younian Wang a, Jianrong Sun c,
Pengfei Zheng d
a
Key Laboratory of Materials Modification by Laser, Ion and Electron Beams, Dalian University of Technology, Ministry of Education, Dalian, 116024, China
b
Institute of High Energy Physics, Chinese Academy of Sciences, Beijing, 100000, China
c
Institute of Modern Physics, Chinese Academy of Sciences, Lanzhou, 730000, China
d
Southwestern Institute of Physics, China National Nuclear Corporation, Chengdu, 610041, China

h i g h l i g h t s g r a p h i c a l a b s t r a c t

Lattice distortion and grain refine-

ment occurred in the damage layer of
the steel.

Amorphous region formed locally in
the bubble layer at a fluence of
1  1018ions/cm2.

Carbide particles showed a tendency
to decompose under the irradiation.

Surface damage threshold of CLF-1
steel was at the fluence of
1  1018He/cm2.

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

Article history: The irradiation resistance of CLF-1 steel was investigated by using He ion irradiation with an energy of
Received 16 January 2018 300 keV. After the irradiation, the structure of CLF-1 steel mainly remained martensitic structure, while
Received in revised form the lattice distortion and grain refinement occurred in the irradiation damaged layer. As irradiation
14 July 2018
fluence increased, the number of vacancies in CLF-1 steel increased, and the vacancies combined with the
Accepted 17 July 2018
Available online 18 July 2018
He atoms to form a bubble layer with the thickness of about 300 nm which located at the end of the He
ions range. In the bubble layer, local amorphous region formed and the carbide particles showed a
tendency to decompose. When the irradiation fluence was up to 1  1018ions/cm2, extensive blisters and
Keywords:
CLF-1 steel
a small amount of peelings appeared on the surface of CLF-1 steel. Due to grain refinement and
He ions dispersion of small carbide particles, the hardness of CLF-1 steel increased after the irradiation.
Irradiation damage © 2018 Elsevier B.V. All rights reserved.

1. Introduction isotope ions caused by the transmutation reaction, sputtering im-

In the radiation environment of fusion devices, the materials
will be exposed to fast neutron [1,2], helium ions, and hydrogen
* Corresponding author.
E-mail address: xxmei@dlut.edu.cn (X. Mei).
purity atoms and the high thermal load with the peak value of
10e20 MW/m2 [3e5], all of these can change the structure of the
materials, then worsening their performance. In order to ensure the
safety of fusion devices, it is necessary to choose materials with
excellent irradiated performance which can be applied in fusion
devices. The reduced activation ferritic/martensite (RAFM) steel is
considered as cladding and structural material which can be

https://doi.org/10.1016/j.jnucmat.2018.07.038
0022-3115/© 2018 Elsevier B.V. All rights reserved.
 X. Zhang et al. / Journal of Nuclear Materials 509 (2018) 496e503
applied in future fusion devices due to its high thermal conduc-
tivity, low thermal expansion coefficient, as well as good resistance
to irradiation-induced swelling and embrittlement [6]. Therefore,
the irradiation resistance of RAFM steel is well worth studying.
In order to explore the applicability of RAMF steels in the irra-
diation environment of fusion devices, many teams have conducted
researches on the irradiation resistance of RAMF steels. Such as the
F82H steel designed by Japan and Eurofer 97 steel designed by
Europe, they are widely studied for the irradiation resistance.
Yakushiji et al. [7] studied the surface erosion in F82H steel induced
by the synergic irradiation of proton and He ion by mass loss
measurement and scanning electron microscopy. Wang et al. [8]
observed the changes of the microstructure in F82H steel caused by
He ion irradiation, and revealed the change of deformation mech-
anism in the steel by tensile test which was transformed from
toughness to brittle. Dethloff et al. [9] investigated the distribution
of defect in Eurofer97 steel under neutron irradiation, and evalu-
ated the influence of the fluence and fluence rate on defects and
microstructure of the steel. Zhang et al. [10] used He ion to irradi-
ated Eurofer97 steel, observed the hardening and embrittlement
induced by the irradiation and the evolution of defects such as He
bubbles and dislocation. The anti-irradiation performance of CLAM
steel designed by China was also investigated by Wang et al. [11]
and Huang et al. [12]. They established a two-step model to simu-
late the evolution of defects and yield strength in the CLAM steel
under the irradiated condition of high temperature and low flu-
ence, and observed the influence of temperature and fluence on
structural evolution in the CLAM steel under high-energy heavy
ions irradiation, etc. These research results showed that RAMF steel
has excellent anti-irradiated performance. Thereinto, the CLF-1
steel developed by the Southwestern Institute of Physics of China
was also considered as a outstanding candidate of structural ma-
terial in the fusion, due to its excellent structural properties such as
refined grain strengthening, dislocation strengthening, etc. Chen
et al. [13] studied the weldability of CLF-1 steel in specific appli-
cation, as well as the stability of organization structure and per-
formance under high temperature. Xu et al. [14] studied the
retention of D in CLF-1 steel by gas driven permeation measure-
ment and investigated the effect of He ions irradiation on the
permeability and diffusion coefficient of D in the CLF-1 steel, etc.
However, for the CLF-1 steel during the irradiation, the relation
between the evolution of microstructure, defects and the changes
of performance is unclear, and this is very important for the CLF-1
steel as a candidate of structural materials in the nuclear fusion
reactor.
In the complex irradiation environment of fusion devices, high
energy neutron irradiation may cause severe displacement damage
up to 200dpa [15], and helium ion irradiation caused by trans-
mutation reaction can cause He retention and generate holes in the
materials, which lead to swelling [16], foaming, embrittlement [17],
peeling [18] and other series of degradation behavior of the ma-
terials, and this all shorten the service life of the material in fusion
devices. And He ion irradiation is an effective way to probe the
relation between the evolution of defects, structural and changes of
performance in CLF-1 steel. In this study, 300 keV He ions with high
fluence were used to irradiate CLF-1 steel in order to simulate
neutron irradiation in fusion environment, also the high fluence of
He ions is good for observing the bubbles, and the effect of irradi-
ation on the microstructure of the steel was observed by trans-
mission electron microscope. Meanwhile, the positron annihilation
technology which has been frequently used in the detection of
defect cluster in the material in recent years was used to indirectly
observed defect status of the steel under the He ion irradiation. And
the X-ray diffraction (XRD) was used to analysis of internal stress
generated in the steel, the irradiation effect on the mechanical
497
performance of the steel was demonstrated by micro-nano
indentor measurement and Nix-Gao model, and the relationship
between the microstructure, defects and mechanical performance
was analyzed by these results.
2. Experimental methods
The material used in this study was CLF-1 steel with the size of
8 mm  4 mm  2 mm and its detailed chemical compositions were
shown in Table 1. Surfaces of steels were mechanically polished to a
mirror finish and then cleaned ultrasonically with acetone and
alcohol prior to the irradiation experiment. In ion beam irradiation
experiment, the samples were irradiated with 300 keV He2þ ions to
four increasing fluencies of 1  1017ions/cm2,2  1017ions/
cm2,4  1017ions/cm2 and 1  1018ions/cm2 at the 320 kV highly
charged ion research platform in Institute of modern physics, Chi-
nese academy of sciences. The flux for all irradiation campaigns was
1.2  1013ions/cm2s. And during the irradiation, the sample holder
was cooled by water, the irradiation was proceeding at RT.
The displacement damage in the CLF-1 steel was calculated by
SRIM program [19] through detailed calculation with full cascade
damage model. The phase structure of unirradiated and irradiated
samples was studied by X-ray diffraction (XRD) with Cu Ka radai-
tion, and the damage morphologies in the steel under the irradia-
tion of maximum fluence were observed by transmission electron
microscope (TEM) with the operating voltage of 200 kV. The sam-
ples for TEM were prepared by focused ion beam (FIB) method. The
surface morphology of samples was characterized by scanning
electron microscope (SEM). The Doppler broadening spectroscopy
(DBS) of slow positron beam was used to analyze the depth dis-
tribution of defects induced by the irradiation in materials. This
measurement was carried out at room temperature on an energy
variable positron beam moderated from a 50 mCi 22Na radioactive
source using a HPGe detector. The changes of nanohardness of CLF-
1 steels were measured by micro-nanoindentor with a Vickers
indenter, the load was 300 mN, the load time was 20s, and the
measurements were carried out on the surface of samples.
3. Results and discussion
The distribution of displacement per atom (DPA) and He con-
centration with ion incidence depth in CLF-1 steel under the
maximum fluence (1  1018ions/cm2) were calculated by SRIM
programme, as shown in Fig. 1. The mean displacement threshold
energy of Fe and other elements is 40eV [20]. It can be obtained that
the distribution of DPA which was induced by ion irradiation
extended from the surface to the depth of approximately 900 nm,
and the peak value located at about 660 nm which was consistent
with the He ions range was 72dpa. The peak value of He concen-
tration distribution was about 5.6  105appm and it was at 710 nm.
Fig. 2 gives the grazing incidence X-ray diffraction (GIXRD)
spectrums of CLF-1 steel before and after He ion irradiation. It can
be seen that no observable structural variations were induced by
the irradiation, and the martensite was still the main structure of
the CLF-1 steel after the irradiation.
Compare the two illustrations in Fig. 3, which shows the XRD
spectrums of a-Fe (110) lattice plane in the CLF-1 steel unirradiated
and irradiated by the maximum fluence. Fig. 3a gives the XRD
Table 1
Chemical Composition of CLF-1 steel in wt.%.
C Cr W V Mn Ta O N Fe
0.11 8.5 1.5 0.25 0.5 0.1 0.002 0.03 Balance
498 X. Zhang et al. / Journal of Nuclear Materials 509 (2018) 496e503
Fig. 1. The depth dependent distribution curve for DPA and concentration of He ions in
CLF-1 steel after He2þ irradiation of 300 keV with a dose of 1  1018/cm.2.
Fig. 2. The GIXRD pattern of CLF-1 steel before and after different fluences of
He2þirradiation at the energy of 300 keV.
Fig. 3. The (a)GIXRD (b)q-2q XRD pattern of a-Fe phase(110)plane of CLF-1 steel before and after different fluences of He2þ irradiation at the energy of 300 keV.
spectrum of grazing incidence. The penetration depth of X-ray in
steel was about 5 mm [21], and the grazing incidence angle of X-ray
in this study was 1, thus the spectrum reflected the structural
information of irradiation layer with a depth about 90 nm. After
irradiation, the diffraction peak showed right-shift of about 0.06
which moved to high angle, indicating that the interplanar spacing
of irradiated layer in the steel decreased, that was compressive
stress among lattice planes produced which caused by He ions
bombardment. Fig. 3b gives the XRD spectrum of q-2q coupled scan.
The depth of structural information obtained by q-2q coupled scan
spectrum was deeper than that of the grazing incidence XRD
spectrum, it contained a large amount of information of the sub-
strate (the unirradiated area outside the He ions range was known
as the substrate). In Fig. 3b, the diffraction peak shifted to the low
angle area about 0.11 and its shifting direction was opposite to that
in Fig. 3a, which meant the interplanar spacing of steel increased
and tensile stress generated, that was the compressive stress
generated in the irradiated layer was balanced by the tensile inte-
rior stress [20]. More detailed peak shifting information is listed in
Table 2.
The full width at half maximum (FWHM) of the diffraction peak
of a-Fe (110) lattice plane evaluated from the XRD spectrum is also
listed in Table 2. In the XRD spectrum of grazing incidence,
compared to the unirradiated sample, the FWHM of the diffraction
peak increased from 0.19 to 0.23 after the irradiation of the
maximum fluence. While in the XRD spectrum of q-2q coupled
scan, the FWHM for the initial and irradiated CLF-1 steels was
0.25 and 0.30 , respectively. The formation of nanocrystals in the
irradiated damaged layer, that is such grain refinement would lead
to the broadening of the diffraction peak (nanocrystals can be
observed in the TEM analysis below). Meanwhile, the stress and the
lattice distortion caused by He ions injection were also the causes of
the diffraction peak broadening.
Table 2
FWHM and peak shift information of the GIXRD and q-2q XRD for the pristine and
irradiated CLF-1 steels.
FWHM 1  1018ions/cm2 Peak shift degree
pristine Direction
GIXRD 0.19 0.23 Right 0.06
q-2q XRD 0.25 0.30 Left 0.11
 X. Zhang et al. / Journal of Nuclear Materials 509 (2018) 496e503
During the process of He ions irradiation, the excited electrons
trace generated by the inelastic collision between the incident ions
with target atoms would heat the lattice through electronic-
phonon coupling and cause local thermalization, thus the thermal
stress generated [22]. The thermal recovery induced by thermal
stress would annihilate the defects in the steel, consequently
reduced the dislocation density nearby the defect and promoted
the grain growth. Meanwhile, due to the continuous bombardment
of He ions, a large number of He ions captured electrons in the
incident process and became He atoms, then they stranded in the
lattice to form bubbles. This introduced the lattice distortion and
the defects, as well as increased the density of dislocation, which
result in the generation of stress among lattice planes and grain
refinement [20]. In the irradiation process, both of the mechanisms
existed simultaneously. In this study, the latter played a leading
role, so the grain size of CLF-1 steels decreased.
Fig. 4 shows the depth distribution of S parameters and S-W plot
for the CLF-1 steel before and after irradiation. The positrons
annihilated with defects in the material, and emitted two photons
with the energy of 0.511 MeV. Due to the Doppler effect, the energy
shift widen the energy of photons. The variation of vacancies in
CLF-1 steel could be analyzed through studying the distribution of
electron momentum which was obtained by the shape of peak with
the energy of 0.511 MeV. The S parameter conveyed the informa-
tion of the positron annihilated with low momentum electrons
Fig. 4. (a)S-depth curves (b)S-W plot for the CLF-1 steel before and after He2þ irra-
diation of different fluences.
499
around defects, and the W parameter represented characteristic
signals of elements as the positron annihilated with high mo-
mentum electrons [23]. The accelerated energy range of the posi-
trons injecting into CLF-1 steel was 0e30 keV, and the
corresponding injected depth was given by the following formula:
Z ¼ ðA=rÞEn (1)
A was the empirical parameter depending on the material, r was
the density of the material. For the CLF-1 steel in this study, A was
40 [24], r was 7.97 g/cm3, and N was1.62 [25]. In Fig. 4a, compared
with the initial CLF-1 steel, the S parameter of CLF-1 steel increased
significantly after He ions irradiation, indicating that a large num-
ber of vacancies were introduced into the steel by the irradiation. In
the depth from 100 nm to 400 nm, the S parameter decreased with
the fluence increased. The electrons, which were existing in the
subsurface of the steel, was absorbed by injected He ions and then
form He atoms. Then, He atoms combined with vacancies to form
small bubbles. With the fluence increased, blisters even spalling
appeared on the surface of the steel (Fig. 6e). These may caused the
S parameter of subsurface layer decreased with the increase of the
fluence, due to the fact that vacancy defects were more attractive to
positrons than helium bubbles [26]. This depth was shallow than
that calculated by SRIM program, which may be mainly caused by
the surface swelling and blisters induced by He ions irradiation as
well as depth distribution of positrons in the material. The S
parameter increased with the fluence in the range of
400 nme700 nm, reflecting that ion irradiation introduced more
defects into the steel by the cascade collision. When the depth
exceeded the He ions range, the S parameter also increased with
the fluence, that was to say the defects diffused deeper in the CLF-1
steel. While the S parameter decreased with the increase of depth
under the same fluence, indicating that the diffusion of defects
weakened with the increase of depth. In the S-W plot of CLF-1 steel
before and after the irradiation, the slope showed in Fig. 4b
changed, indicating that the He ions irradiation induced different
types of defects into the steel [27], that was the accumulated va-
cancies merged to clusters and combined with He atoms to form He
bubbles as the fluence increased.
Chose the smooth surface without blisters to analyze the
structure and cross-sectional morphology of CLF-1 steel. The cross-
sectional TEM sample was obtained by focusing ion beam tech-
nology (FIB), and the microstructure of CLF-1 steel under the irra-
diation with a fluence of 1  1018/cm2 is shown in Fig. 5. Fig. 5a
gives a sectional morphology of the steel. There was a white band,
which was a He bubble layer induced by the irradiation, formed at
the end of ion range. And its local magnifying image is shown in
Fig. 5b. The thickness of He bubble layer was about 300 nm. Wang
et al. [11] reported the simulated results obtained by the rate theory
model and the enhanced model. The result showed that the He
bubbles were in the incubation and nucleation period when the
irradiated damage was less than 0.02dpa. Under low temperatures
(T < 0.2 Tm), the nucleation of He bubbles could be explained by
“diatomic nucleation model " [28], namely ignoring thermal va-
cancies, two He atoms would be attracted each other to form a
stable nuclei and the binding energy was 0.63 eV, the formation of
He bubbles in this model was controlled by the diffusion of He
atoms [16]. When the irradiated damage was greater than 0.02 dpa,
He bubbles began to grow by absorbing a large number of vacancies
and He atoms. So as the fluence increased, the irradiation damage
in materials was more serious, also the bubbles would become
bigger and could be observed more easily. In this study, the damage
induced by He ions irradiation was up to 72dpa, thus evenly
distributed He bubbles with a diameter range of 5e15 nm can be
observed in Fig. 5c.
500 X. Zhang et al. / Journal of Nuclear Materials 509 (2018) 496e503

Fig. 5. The TEM image of the CLF-1 steel after He2þ irradiation with the fluence of 1  1018/cm2(a)the cross-section morphology image (b)He bubble layer (c)the magnified image of
b (d)the magnified HRTEM image of A region in a (e) the corresponding FFT pattern of the white box C in d: a-Fe[111] (f) the corresponding FFT pattern of the white box D in d: MC
phase[332] (g)the carbide particle in B region of a (h) the SAED pattern of the carbide particle in g.

Fig. 5d is the magnified HRTEM image of region A in Fig. 5a, a
large number of nanocrystals with diameters of 2e8 nm were
observed and the amorphous region with long-range disordered
was formed locally in the damaged layer. Fig. 5e is the Fast Fourier
Transform(FFT) pattern of the white box region C in Fig. 5d, which
can be obtained that a-Fe phase nanocrystalline formed in the
damaged layer. The formation of nanocrystalline widened the X-ray
diffraction peak. In the previous studies on the ion irradiation of
RAFM steel, no amorphous region was observed even the irradiated
displacement damage reached 60dpa [29]. In this study, during the
process of irradiation with 300 keV He ions, the displacement
damage was up to 72dpa, the chemical disorder caused by the
serious cascade damage during the irradiation could lead to the
increase of free energy of crystal phase and make the amorphous
transformation happen [30]. Meanwhile, the generation and ag-
gregation of point defects such as interstitials, vacancies and
interstitial-vacancy compounds would increase the crystal lattice
energy, when the concentration of point defects exceeded the
critical value, the free energy of the crystal phase was higher than
that of metastable amorphous phase, then transition from crystal to
amorphous would happen [31]. In addition, the implantation of
energic ions would result in the formation of local melting zones in
the material, the heat of melting zones dissipated in the substrate
rapidly, then the target atoms was frozen in a disordered state, this
also prompted the formation of amorphous region with local long-
range disordered. During the formation of amorphous regions,
defects such as dislocations in the region would migrate to the
interface nearly, and annihilated in the interface. Yu et al. [32]
observed this phenomenon in situ in Fe alloy under Kr ions irra-
diation. According to the calculation results of SRIM in Fig. 1, the
concentration of He atoms was very high in the damaged layer, and
a large number of He bubbles were formed to destroy the lattice
structure, and a large number of interfaces introduced by the
nanocrystalline provided annihilation points for dislocation. Thus
the decrease of the number of dislocation was observed in Fig. 5d.
The white box D in Fig. 5d shows the carbide particle in the irra-
diation damaged layer, and the corresponding FFT pattern is given
in Fig. 5f, the particle was MC phase. Fig. 5g (magnified image of
region B in Fig. 5a) gives the carbide particle in the substrate, and
Fig. 5h was the corresponding selected area electron diffraction
pattern, the particle was MC phase. Some carbon particles with a
diameter of dozens of nanometers could be seen in the substrate,
while in the irradiated damaged layer, these were almost invisible,
only several small particles with a small diameter of a few nano-
meters could be observed. This indicated that the carbide particles
had a trend of decomposition caused by the irradiation.
In Fig. 4a, the S parameters decreased in the depth from 100 nm
to 400 nm which meant the generation of He bubbles, and this
 X. Zhang et al. / Journal of Nuclear Materials 509 (2018) 496e503
Fig. 6. The SEM morphology images of CLF-1 steel before and after different fluences of He2þ irradiation at the energy of 300 keV (the inset is the magnified morphology images of
the damaged area in the white box).
results was consistent with the observation of He bubble layer in
Fig. 5. Moreover, the curve of S parameter in Fig. 4a revealed the
diffusion of the defect, which was consistent with the phenomenon
in Fig. 5a that there was still a small amount of He bubbles in the
region beyond the ion range.
The surface morphology images of the CLF-1 steel before and
after the He irradiation are shown in Fig. 6. The surface of the un-
irradiated CLF-1 steel was smooth and flat (Fig. 6a). As the irradi-
ation fluence increased to 4  1017ions/cm2, the surface maintained
flat and no obvious irradiation damage could be observed(Fig. 6d).
Irregularly shaped blisters with the size of 10e80 nm distributed
uniformly on the surface of the steel accompanied by small area of
spalling when the fluence was up to 1  1018ions/cm2. Defects such
as grain boundaries, dislocations, vacancies and so on existed in the
CLF-1 steel. During the injection, He ions would recombine with
electrons and become He atoms in the process of slowing down.
Besides the diatomic nucleation, vacancies which was inherent and
induced by the ion irradiation would capture [33] He atoms to
formed He-V compound, and then the compound grew up by
absorbing He ions and vacancies. The stress among He-V com-
pounds was proportional to the pressure inside bubbles, the pres-
sure increased as the He ion irradiated continuously. When the
pressure inside the bubble was large enough to produce the stress
exceeded the surface strength of the CLF-1 steel, the blisters
501
appeared on the surface of the steel, then delamination and spalling
occurred. And the He-V compounds also resulted in the lattice
distortion in the steel, which was consistent with the result of the
peak shift in the XRD diffraction patterns.
Fig. 7a gives the variation of micro-nano hardness with depth of
the CLF-1 steel before and after He ions irradiation with different
fluence. With the increase of the depth, the hardness of the steel
decreased. The curve could be divided into two parts, the inden-
tation depth of the first part was less than 210 nm, and in this part,
the hardness decreased relative sharply with the increase of depth.
This was introduced by the indentation size effect (ISE) on the
surface of the samples [34]. According to the simulation results of
SRIM, the projected range of 300 keV He ions was 662 nm in the
CLF-1 steel. And It is suggested that the deformation region under
the nano-indenter tip is 5e7 times than the indentation depth [35].
In this study, the indentation depth was 1 mm, so the depth of
deformation zone was 5-7mm. The depth of deformation zone was
far greater than that of the irradiated damage area, so substrate
effect contributed. The second part of the micro-nano hardness-
depth curve was corresponded to a region of depth greater than
210 nm, which was affected by the soft substrate effect (SSE). It can
be seen from the figure that the hardness of the irradiated layer of
CLF-1 steel increased after He ion irradiation with different fluence.
Due to the SSE, the actual hardening induced by the irradiation
502 X. Zhang et al. / Journal of Nuclear Materials 509 (2018) 496e503
Fig. 7. (a) The depth-dependent variations of hardness and (b) the plot of H2 versus 1/h for CLF-1 steel before and after different fluences of He2þ irradiation at the energy of
300 keV.
should be higher than the measured value. According to the
traditional hardening model, the defect cluster hinder the dislo-
cation movement and lead to the hardening of the metals [36,37]:
pffiffiffiffiffiffiffi
DHf Nd
where N,d was the number density and average diameter of the
defect cluster, respectively. The hardening of materials was pro-
portional to the number and size of defect clusters. In the result of
TEM (Fig. 5), compared with the substrate, under the irradiation
fluence of 1  1018/cm2, the density of dislocation loops in the
irradiation damaged layer of CLF - 1 steel decreased, while irradi-
ation made carbide particles have a tendency to decomposition
(Fig. 6e&f). The small carbide particles dispersing in the CLF-1 steel
would cause hardening by preventing the dislocation movement.
Meanwhile, as the results shown in Fig. 3, during the process of He
ions irradiation, the stress generated among the crystal planes led
to lattice distortion and grain refinement, this had the pinning ef-
fect on the slip of dislocation. These two points aforesaid might be
the main source of the irradiation hardening. Fig. 7b gives the H2-1/
h curve of CLF-1 steel before and after He ions irradiation with
different fluences. Nix-Gao model [38] was used to fit the metrical
hardness data to analyze the range whose hardness was influenced
by the irradiation damage. It could be seen that in the unirradiated
steel, its H2 -1/h curve demonstrated good linearity. After He ions
irradiation, the slope of the H2 -1/h curve of the steel changed in the
depth at 210 nm, and this inflection point indicated that the hard-
ness of the steel was affected by the soft substrate effect [20].
The hardness values at the infinite depth in CLF-1 steel which
were calculated from the least square fitting of hardness data in the
ISE region in Fig. 7b according to Nix-Gao model were listed in
Table 3. The SSE was excluded in these values, and the relative
reliable hardness of helium-implanted steel could be obtained. It
could be seen that the hardness increased after the irradiation
which induced by small carbide dispersion and the grain refine-
ment. The SSE could be confirmed by comparing the hardness
values listed in Table 3 and read form the curve in Fig. 7a.
Table 3
The hardness at infinite depth (H0) obtained from Nix-Gao model.
Fluence(ions/cm2) pristine 1  1017 2  1017 4  1017
H0(GPa) 2.44 3.78 4.25 4.83
The CLF-1 steel has a relative good structural stability under He
ion irradiation with the energy of 300 keV. While as the ions
bombarded the steel continuously, a local amorphous region was
formed in CLF-1 steel, and a large number of He bubbles were
produced. This result of the formation of He bubbles which directly
(2)
observed by TEM were confirmed by the indirect measurement of
positron annihilation spectrum: falling S parameters and the
change in the slope of S-W curve showed numerous vacancy
clusters produced in CLF-1 steel after He ions irradiation, as He ions
injected sostenuto, vacancy clusters would combined with He
atoms to form He bubble clusters. These clusters induced by the
irradiation led to the lattice distortion, then the stress among the
lattice plane generated and the grain refinement occurred. Mean-
while, large amount of defect clusters and cascade damage would
cause the chemical disorder and increase the free energy of the
crystal phase, which could lead to the transformation of crystal to
amorphous state. The accumulation of the He bubble clusters
increased the internal pressure of bubbles, when the pressure in-
side the bubble exceeded the surface strength of the CLF-1 steel, the
delaminations and spallings occurred. The defect clusters also
increased the migration rate of target atoms and the free energy of
the lattice, which caused the decomposition of carbide particles in
the irradiated damaged layer. These small carbide particles
dispersed in the steel, along with the stress among lattices and the
grain refinement, resulted in the irradiation hardening of steel
jointly. Due to the SSE, the improvement of the hardness measured
by micro-nanoindentor was slightly lower than the actual value,
and this was verified by the results obtained by the fitting and
extrapolation in Nix-Gao model.
4. Conclusion
As a candidate of cladding/structural material applied to the
fusion device, CLF-1 steels mainly maintained martensitic structure
under 300 keV He ions irradiation, while compressive stress
generated among crystal lattices and the grain refinement
occurred. A large number of vacancies produced by the irradiation
on the subsurface of CLF-1 steel, and they were combined with the
projected He ions and formed a He bubble layer with the thickness
about 300 nm. In the He bubble layer, a local amorphous region
formed, and carbide particles therein had a tendency to decom-
1  1018
pose. As the fluence reached 1  1018ions/cm2, blisters and spalling
appeared on the surface of CLF-1 steel. After the irradiation, the
4.34
hardness of CLF-1 steel increased.
 X. Zhang et al. / Journal of Nuclear Materials 509 (2018) 496e503
Acknowledgements
This work is financially supported by the National Science
Foundation of China (No.11675035 and No. 11375037. The experi-
mental work was carried out at the 320 kV platforms for multi-
discipline research with highly charged ions at the Institute of
Modern Physics, CAS.
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