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Acta Materialia 61 (2013) 2966–2972

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Dislocation loop formation under various irradiations of laser

and/or electron beams
Zhanbing Yang 1, Seiichi Watanabe ⇑,2
Centre for Advanced Research of Energy and Materials, Faculty of Engineering, Hokkaido University, N13, W8, Kita-ku, Sapporo,
Hokkaido 060-8628, Japan

Received 21 November 2012; received in revised form 21 January 2013; accepted 25 January 2013

Abstract

A high-voltage electron microscope (HVEM) equipped with a laser head (laser-HVEM) was developed at Hokkaido University and is
used to investigate the surface modification of semiconductors and the behaviour of lattice point defects in metals under various irradi-
ations of laser (photon) and/or electron beams. In the present study, the annealing effect of pulsed laser irradiation on a face-centred-
cubic metal was experimentally investigated and theoretically calculated. The systematic assessment of dislocation loop evolution under
laser-electron sequential irradiation and laser-electron dual-beam irradiation was performed. Our results show that the rapid heating and
quenching that occurred during pulsed laser irradiation caused vacancies to be introduced at the surface of the specimen and to diffuse to
the interior, which led to the formation and growth of vacancy-type (V-type) dislocation loops. These loops gradually shrank and finally
disappeared during the subsequent electron irradiation of the sample. During laser-electron simultaneous dual-beam irradiation, the type
of loop formed, interstitial-type (I-type) or V-type loops, is determined by the relative intensities of the laser beam and electron beam,
which indicates that the loop type can be controlled by changing the relative intensities of the beams. Accordingly, models of dislocation
loop formation during various irradiations were proposed. The newly developed laser-HVEM instrument is expected to be employed in
the exploration of mechanisms in material science, as well as in other scientific fields.
Ó 2013 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Keywords: Radiation effects; Laser-HVEM; In situ; Lattice defects; Dislocation loop

1. Introduction diations was achieved via the continuous development of

Energetic beam irradiation introduces primary lattice
point defects, such as interstitial and vacancy defects, in
metals. These defects govern the changes in the microstruc-
ture and mechanical properties of the materials, such as the
formation and growth of dislocation loops and voids [1–3],
segregation near grain boundaries [4,5], precipitates [6,7],
embrittlement [8,9], creep [10,11] and hardening [8,12].
Over the past a few decades, the simulation of various irra-
⇑ Corresponding author. Tel./fax: +81 11 706 7886.
E-mail address: sw004@eng.hokudai.ac.jp (S. Watanabe).
1
The author designed and performed the experiments, collected and
analysed the data and wrote the paper.
2
The author designed the study, analysed the data and assisted in the
writing of the paper.
research instruments and methods to understand the
microstructural changes and the mechanisms governing
these changes that occur during irradiation.
With the development of transmission electron micros-
copy (TEM) in the 1940s [13], it became possible to observe
changes in the microstructures of materials before and after
irradiation. To directly observe the changes as they occur
during irradiation, which is useful for revealing the mecha-
nisms leading to such changes, instruments and methods
for in situ observation have been continuously under devel-
opment, and to date, in situ techniques have been the most
important and popular tools for the study of radiation
effects. For example, the use of a high-voltage electron
microscope (HVEM) since the 1960s [14] has made it pos-
sible to simulate the effects of neutron irradiation, except

1359-6454/$36.00 Ó 2013 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.actamat.2013.01.056
 Z. Yang, S. Watanabe / Acta Materialia 61 (2013) 2966–2972
for collision cascades, due to the introduction of Frenkel
pairs (FPs, referring to an interstitial atom and a vacancy)
by electron beam irradiation [15]. Meanwhile, the combina-
tion of ion irradiation with TEM was developed for in situ
observation of the simulation of high numbers of atomic
displacements and collision cascades [16]. The actual envi-
ronment inside nuclear reactors and in outer space is com-
plex due to the simultaneous existence of high-energy
neutrons and electromagnetic radiation [17] instead of a
single energetic radiation beam. HVEM allows for the
in situ observation of electron beam irradiation and utilizes
a large chamber that can be conveniently connected to
other instruments; since the 1970s it was coupled to an
accelerator for the in situ observation of the introduction
of FPs and atomic displacements resulting from multi-
beam irradiation [18–24].
During heavy-ion irradiation, vacancies and interstitials
are simultaneously introduced by cascade damage with a
high concentration of vacancies surrounded by interstitials
[25]. However, electron irradiation creates randomly dis-
tributed vacancies and interstitials (FPs). Because pulsed
laser beam irradiation causes rapid heating and quenching
in materials [26] and the laser head can be easily connected
to other equipment, the first laser HVEM was developed in
2007 at Hokkaido University [27] to provide an environ-
ment of randomly distributed FPs with an additional
source of vacancies.
Laser-HVEM has already been used in situ to observe
the formation of V-type dislocation loops under irradiation
with a single laser beam. Furthermore, using laser-HVEM,
two new methods for measuring vacancy migration energy
were also proposed [28], breaking new ground in this field
after little advancement during the previous 30 years.
Although the in situ observation of dislocation loop forma-
tion under single electron irradiation or single laser beam
irradiation has been reported [28], the mechanisms of dislo-
cation loop formation under laser-electron simultaneous
dual-beam irradiation, a new method for studying lattice
point defects, are unknown.
In the present study, both experimental studies and the-
oretical calculations were performed to investigate the
annealing effects of pulsed laser beam irradiation on com-
mercial SUS316L steel. Dislocation loop evolution under
single laser beam irradiation, laser-electron sequential irra-
diation and laser-electron simultaneous dual-beam irradia-
tion was systematically and experimentally studied.
Moreover, models of dislocation loop formation under
the various irradiations of laser and/or electron beams were
proposed according to the results and analysis. In the
future, laser-HVEM is expected to be coupled to accelera-
Table 1
Chemical composition of present SUS316L steel (mass%).
C Si Mn P S
0.013 0.20 1.28 0.024 0.0010
2967
tors for the in situ observation of multi-beam irradiation.
This instrument can be employed not only in the evaluation
of the surface modification of materials [27] and in the
study of irradiation damage in metals [28] but also in
broader scientific research, such as nanotechnology and
the study of irradiation effects on polymer materials and
foods.
2. Experimental
2.1. Material preparation
Commercial SUS316L austenite stainless steel, which is
commonly employed in core internals in boiling water reac-
tors, was used in the experimental investigations in the
present study. Table 1 lists the chemical composition of
the material. Sheets of the steel were mechanically thinned
to a thickness of 0.15 mm. Discs measuring 3 mm in
diameter were punched from the sheets and jet-electron-
milled for use as TEM specimens in the laser-HVEM irra-
diation experiments. The thickness of the irradiated area
was determined to be 300–550 nm.
2.2. Laser-electron dual-beam irradiation
Single laser beam irradiation, laser-electron sequential
irradiation and laser-electron dual-beam irradiation of
the TEM specimens were performed using laser-HVEM
(HVEM: Hitachi, H-1300). The laser-HVEM instrument
was first described in Refs. [27,28]. A schematic of the
laser-electron simultaneous dual-beam irradiation of a
TEM specimen is provided in Fig. 1. The diameter of the
laser beam in this study was measured to be 1.5–2 mm;
the typical diameter of the electron beam for irradiation
is 2 lm. Because the diameter of the laser beam is larger
than that of the electron beam, the dual-beam irradiation
area is divided into three parts, which are designated as
A, B and C in Fig. 1.
2.3. Experimental methods
To investigate the annealing effects of the pulsed laser
beam (Nd:YAG laser, Inlite II, Continuum) irradiation
of the material, a bulk sample of SUS316L was first irradi-
ated with a single laser beam in air at room temperature for
15,000 pulses with an energy density of 124 mJ cm2. The
central wavelength was 532 nm, and the pulse repetition
rate was 2 Hz. After laser irradiation, the surface of the
sample was studied by scanning electron microscopy
Ni Cr Mo V Al N
13.32 17.24 2.04 0.04 0.014 0.0396
2968 Z. Yang, S. Watanabe / Acta Materialia 61 (2013) 2966–2972
Fig. 1. Schematic of the laser-electron simultaneous dual-beam irradia-
tion of a TEM specimen using laser-HVEM. Area A: centre of the dual-
beam irradiation. Area B: edge of the dual-beam irradiation area where
the electron beam intensity is weaker than that of area A but the intensity
of the laser beam is maintained. Area C: single laser beam irradiation area.
(SEM; JEOL 7001 FA). Then, a cross-sectional specimen
was cut from the bulk sample in the top-down direction
using a focused ion beam (FIB; JEOL 9200) and examined
via TEM to investigate the interior of the sample.
The sample was irradiated with a single laser beam for
10 min and with a dual laser-electron beam for 20 min
using laser-HVEM at 723 K, a temperature at which both
interstitials and vacancies are thermally mobile in the mate-
rial. The central wavelength and the pulse repetition rate
were the same as those used to study the bulk sample
(532 nm and 2 Hz, respectively), but the laser beam energy
density was greatly reduced to 24 mJ cm2 to avoid
destroying the sample with the pulsed irradiation. Addi-
tionally, to introduce defects into the specimen, the energy
density employed in this study was significantly lower than
that of the laser-ion dual-beam irradiation used to control
nanoparticle precipitates at the surface of semiconductors
[29]. Electron irradiation was performed using HVEM at
1000 kV with a typical damage rate of 2  103 dpa s1.
During the single laser beam irradiation, the electron beam
intensity used in the TEM observation was kept as low as
possible to avoid altering the sample.
For the laser-electron sequential irradiation, the sample
was thermally annealed for 90 min at 723 K after the
10 min single laser beam irradiation at the same tempera-
ture to obtain large V-type loops. The sequential electron
irradiation was performed at 540 K, a temperature at
which only interstitials are thermally mobile and have a
slow diffusion rate. With the large loop size and the lower
electron irradiation temperature, the development of V-
type loops during the subsequent electron irradiation is
expected to be slower than that at 723 K and should be
clearly observable in situ and recordable.
The analysis of the nature of the dislocation loop and
the examination of the microstructure after irradiation
and the cross-sectional specimens were performed using a
JEM-2000FX transmission electron microscope.
3. Results and discussion
3.1. Annealing effects of pulsed laser beam irradiation on the
specimen and origin of vacancies by laser
Cracks at the surface layer of the bulk sample were
clearly visible after laser irradiation, as shown in the
SEM image in Fig. 2a. Fig. 2b presents a TEM image of
the cross-sectional plane that was cut from the bulk sample
in the top-down direction. From the figure, the depth of the
cracks is determined to be in the range of 300–400 nm. A
partial area of the sample marked in orange in Fig. 2b is
magnified in Fig. 2c to show the surface of the sample,
where the lath-like microstructure is clearly visible.
For the specimen irradiated with a laser beam with an
energy density of 24 mJ cm2 using laser-HVEM, neither
crack nor a lath-like microstructure was observed in the
cross-sectional plane due to the lower energy density
employed, but a heated surface layer with a width of
100–150 nm can still be distinguished from the internal
microstructure by a dark line parallel to the surface, which
is marked by a white dotted line in Fig. 2d. Due to techni-
cal limitations, the width of the cross-sectional plane (i.e.
the thickness of corresponding area of the TEM foil) was
thicker than the irradiated area of the TEM sample (350–
550 nm).
Both the cracks and the lath-like microstructure clearly
indicate that the surface of the sample was heated and
quenched during the laser irradiation. In this study, the
laser pulse repetition rate was 2 Hz, and the duration of
each pulse was 5–6 ns. The surface of the specimen was
heated to T1 during the duration of the pulse and then
quenched to the experimental temperature (T0) during the
0.5 s interval between successive pulses. The formation of
the lath-like microstructure in the surface layer is due to
the quenching.
The relationship between the quantity of heat and T1
can be expressed as:
Z T1 Z T1
Q ¼ mcp DT ¼ mf ðT ÞdT ¼ qVf ðT ÞdT ð1Þ
T0 T0
where Q is the heat from the laser irradiation; m and V are
the mass and volume of heat absorbed per section of the
material, respectively; q is the mass density of the material;
and cp is the thermal capacity of the material. For Fe, cp is
given by [30]:
cp ¼ a þ b  103 T þ c  105 T 2 þ d
 106 T 2 cal K1 mol1 ð2Þ
The values of the parameters (a, b, c and d) are shown in
Table 2.From the experimental results obtained with differ-
ent laser energy densities and Eq. (1), it is very clear that
the depth of the heated surface layer is dependent on the
laser beam energy density and the identity of the irradiated
material. In the case of laser irradiation in air at room tem-
perature (T0 = 298 K), the surface layer of the specimen is
 Z. Yang, S. Watanabe / Acta Materialia 61 (2013) 2966–2972 2969

Table 2
Parameters used in the calculation of the cp of Fe [30].
Temperature (K) a b c d
298–800 6.734 1.749 0.692 5.985
800–1000 62.967 61.140 148.0 –
1000–1042 153.419 166.429 – –
1042–1060 465.166 427.222 – –
1060–1184 134.305 79.862 696.012 –
1184–1665 5.734 1.998 – –
1665–1809 5.888 2.367 – –

an energy density of 24 mJ cm2 at T0 = 723 K using the

laser-HVEM, T1 is calculated to be 1090 K, assuming that
the thickness of the surface layer is 100 nm, as determined
from Fig. 2d. It is clear that although the thickness and
laser beam energy density are different between the bulk
sample and the TEM specimen, both of them can be heated
to similarly high temperatures using pulsed laser beam
irradiation.
The vacancy concentration (CV) at equilibrium is deter-
mined as a function of temperature, T, according to the fol-
lowing equation:
 
Ef
C V ¼ exp ð3Þ
kT
where Ef is the vacancy formation energy and k is the
Boltzmann constant. For the laser irradiation in the pres-
ent study, it is obvious that C V ;T 1 > C V ;T 0 . When the va-
cancy concentration is at equilibrium at T1, a vacancy
supersaturation is created by quickly quenching the sample
to the working temperature (T0). Therefore, vacancies are
created in the heated surface layer of the specimen because
of the heating and quenching processes in pulsed laser
beam irradiation.

3.2. Dislocation loop formation under single laser beam

irradiation

A large number of faulted dislocation loops formed and

grew during the 10 min single laser beam irradiation, which
was performed at 723 K using laser-HVEM. To obtain
large loops, as shown in Fig. 3, thermal annealing was

Fig. 2. Annealing effects of laser beam irradiation (15,000 pulses) of the

bulk sample and the TEM specimen. (a) SEM image of the surface of the
bulk sample after 15,000 laser irradiation pulses at room temperature in
air. (b) Cross-sectional plane view of the specimen cut from the bulk
sample from the surface to the interior by FIB after laser irradiation. (c)
Higher magnification of the marked area in (b). (d) Cross-sectional plane
view of the specimen cut from the TEM specimen by FIB after single laser
beam irradiation using laser-HVEM at 723 K.

assumed to be 350 nm (the crack depth is 300–400 nm in

Fig. 2b). The T1 value calculated using Eq. (1) was deter- Fig. 3. Image of dislocation loops after laser irradiation for 10 min and
mined to be 1017 K. Similarly, for laser irradiation with subsequent annealing for 90 min at 723 K.
2970 Z. Yang, S. Watanabe / Acta Materialia 61 (2013) 2966–2972
performed for 90 min at the same temperature after the
laser irradiation. A vacancy supersturation was not gener-
ated during the thermal annealing; however, the vacancies
were thermally mobile and able to migrate to the existing
loops, which acted as sinks for the vacancies, allowing loop
growth to continue.
The growth of dislocation loops under single laser irra-
diation has been observed in situ, and the loops were found
to be V-type [28] using the inside–outside method [13,31].
The steady growth of loops during the in situ observation
period and the continual existence of the loops during
and after the long thermal annealing process indicate that
the loops nucleated in the interior of the specimen instead
of at the surface layer. Otherwise, if the loops had nucle-
ated at the surface layer, the loops would have shrunk or
suddenly disappeared during irradiation and thermal
annealing because of the surface sink effect. Thus, the V-
type dislocation loop formation and growth in the interior
of the specimen support the finding that vacancies are
introduced by laser irradiation, and actually diffuse from
the heated surface layer to the interior of the specimen
and then form V-type loops.
The production rate of vacancies in a TEM specimen by
pulsed laser irradiation can be calculated as follows.
According to Eq. (3), CV,1090K = 3.7  107 when the tem-
perature is 1090 K and Ef is 1.39 eV [32]. The laser beam
pulse repetition rate is 2 Hz, which means that these vacan-
cies are produced every 0.5 s. The simple evaluation of
defect production rate under pulsed laser irradiation is [33]:
L ¼ C V =t
7 1
Thus, L is 7.4  10 s in the present study.
The model of dislocation loop growth during laser irra-
diation and the associated rate equations have been
reported in the literature [28].
3.3. Evolution of dislocation loops during laser-electron
sequential irradiation
As discussed previously, in the case of laser-electron
sequential irradiation, dislocation loops first formed and
grew under single laser irradiation. During sequential elec-
tron irradiation, the dislocation loops that were observed
in situ gradually shrank and finally disappeared, as shown
in Fig. 4a–d.
Fig. 4. In situ observation of the shrinking and disappearance of V-type dislocation loops during sequential electron irradiation at 540 K.
As mentioned in Section 2.3, sequential electron irradia-
tion was performed at 540 K. FPs were introduced during
electron irradiation, but the vacancies were stable and only
the interstitials were thermally mobile at this temperature.
Thus, it is obvious that the shrinking and disappearance of
the dislocation loops during electron irradiation is the
result of the diffusion of the interstitials and their subse-
quent reaction with the loops. Only the recombination of
the interstitials and vacancies (I + V = 0) can lead to the
loop disappearance, which also indicates that single laser
beam irradiation introduces V-type loops into the material.
3.4. Dislocation loop formation under simultaneous dual-
beam irradiation
As shown in Fig. 1, the dual-beam irradiation area is
divided into three parts because of the difference in the
diameters of the laser beam and electron beam. Accord-
ingly, the effect of simultaneous dual-beam irradiation on
dislocation loop formation is also divided into three parts,
as shown in Fig. 5a.
Area A is the centre of the laser-electron simultaneous
dual-beam irradiation, where the intensity of the electron
beam is highest. In this area, dislocation lines can be
observed instead of dislocation loops in Fig. 5a, and voids
are also visible as shown in Fig. 5b, which is the enlarged
image of the marked area in Fig. 5a. Vacancies are simul-
taneously introduced by two processes during the dual-
beam irradiation, i.e. by FP production due to the electron
ð4Þ irradiation, and by thermal annealing due to the laser heat-
ing. The recombination of the interstitials and vacancies
(I + V = 0), which leads to a lack of visible dislocation
loops, acts as the dominant process in area A. Since the
electron irradiation creates equal numbers of vacancies
and interstitials and the laser irradiation creates mainly
vacancies, it is understandable that the voids in area A
are a result of the excess (no balanced by interstitial pro-
duction) vacancies produced by laser.
Area B corresponds to the edge of the electron-irradi-
ated area, which means that the laser beam intensity is
the same as that in area A, but the electron beam intensity
is weaker. In area B, the behaviour of I + V = 0 is one of
the two main processes associated with defects behaviours,
but it is no longer the dominant process. Meanwhile, the
ratio of vacancy to interstitial production is higher in area
 Z. Yang, S. Watanabe / Acta Materialia 61 (2013) 2966–2972
Fig. 5. Formation of dislocation loops and voids under laser-electron
simultaneous dual-beam irradiation for 20 min at 723 K. (a) Formation of
dislocation loops under dual-beam irradiation. Area A: dual-beam
irradiation; area B: laser and weak electron beam irradiation; area C:
single laser irradiation. (b) Enlarged view of the marked area in (a). Voids
formed under laser-electron simultaneous dual-beam irradiation at 723 K.
B than that of area A, and the excess vacancies clusters
form small dislocation loops. Therefore, the existence of
loops after irradiation indicates the increase in the effect
of the laser irradiation in area B.
Fig. 6. Analysis of the nature of the dislocation loop formed in area C using the inside–outside method: (a) g>0, s>0; (b) g>0, s<0; (c) tilted by large angle.
2971
Electron irradiation can be neglected in area C because
of its significantly lower intensity, and area C can therefore
be treated as a single laser beam irradiation area. Large
loops are clearly observed in area C, as shown in Fig. 5a.
The nature of the loops was also analysed using the
inside–outside method. As shown in Fig. 6a–c, for g (dif-
fraction vector) > 0, the loops first decreased in size when
s (deviation parameter) was changed from s > 0 to s < 0
(from Fig. 6a to b). The loops subsequently increased in
size when the sample was tilted at a large angle (from
Fig. 6b to c). The result showed that the loops formed in
area C were V-type, which is in agreement with previous
reports in the literature [28].
It is obvious that the dominant factor determining the
type of dislocation loop that forms under laser-electron
simultaneous dual-beam irradiation is the relative intensi-
ties of the laser beam and electron beam. Consequently,
the interesting phenomena described here demonstrate that
the formation of different types of loops in materials can be
controlled by careful selection of the irradiation beam
intensities.
3.5. Models of dislocation loop formation during irradiations
of laser and/or electron beams
Based on an intuitive understanding of the lattice point
defect behaviour during various irradiations and on the
experimental results and analysis, models of dislocation
loop formation during single electron beam irradiation,
single laser beam irradiation, laser-electron sequential irra-
diation and laser-electron simultaneous dual-beam irradia-
tion are provided in Fig. 7a–d, respectively.
During single electron beam irradiation (see Fig. 7a),
FPs are introduced and I-type dislocation loops quickly
form and grow because the interstitials are able to migrate
more easily than the vacancies. Under single laser beam
irradiation as shown in Fig. 7b, only vacancies are intro-
duced in the surface layer of the specimen. The vacancies
then diffuse into the interior of the specimen, form V-type
dislocation loops and contribute to the loop growth. In the
case of laser-electron beam sequential irradiation, V-type
dislocation loops are first introduced by laser irradiation,
as indicated by the dotted loops shown in Fig. 7c. During
the subsequent electron irradiation, interstitials easily
2972 Z. Yang, S. Watanabe / Acta Materialia 61 (2013) 2966–2972

(a) (b) (c) (d)

Fig. 7. Models of dislocation loop formation under different laser and/or electron beam irradiation configurations.

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