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Scripta Materialia 64 (2011) 1125–1128

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Signature of surface energy dependence of partial dislocation slip

in a gold nanometer-sized protrusion
Sung Bo Leea,⇑ and Young-Min Kimb
a
Department of Materials Science and Engineering, Seoul National University, Seoul 151-744, Republic of Korea
b
Korea Basic Science Institute, Daejeon 305-333, Republic of Korea
Received 13 February 2011; revised 27 February 2011; accepted 4 March 2011
Available online 10 March 2011

The mechanical behavior of metallic nanowires has been intensively studied, demonstrating the strong sample-size dependence of
crystal plasticity. However, the effect of surface energy has not yet been fully resolved. Here we have used in situ high-resolution
transmission electron microscopy of gold nanometer-sized protrusions at room temperature to address this problem. Our experi-
mental results reveal that the slip of Shockley partial dislocations reduces the energy cost of creating the extra surface area resulting
from the dislocation slip (i.e. surface steps).
Ó 2011 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Keywords: In situ transmission electron microscopy (TEM); Nanostructured materials; Dislocation dynamics; Twinning

As is well evidenced, pure bulk metals are
strengthened by strain hardening by plastic deformation.
Plasticity in bulk metals occurs by the motion of disloca-
tions. During plastic deformation, dislocations multiply
and are pinned by other dislocations and defects, such
as grain boundaries, leading to strengthening. In contrast,
defect-free metallic nanowires with diameters up to tens
of nanometers do not exhibit such strain hardening
behavior, but display a very high elastic stress followed
by a drastic drop and pronounced strain softening, exhib-
iting a sharp yield point [1–5]. Such mechanical behavior
is also observed in dislocation-free metal whiskers [6].
Due to their limited sizes, yielding in nanowires is
determined by the surface nucleation and propagation
of 1=6h1 1 2i Shockley partial dislocations on the
{1 1 1} plane, rather than full dislocations [1–5,7–10].
Twinning, which occurs by successive emissions of
Shockley partials with the same Burgers vector on
neighboring slip planes [11,12], is also predicted to form
in nanowires [2,3]. As compared with such well-accepted
geometric size effects on partial dislocation slip, how-
ever, there is still a lack of detailed information on
how surface energy influences dislocation slip in
nanostructures.
Here, using in situ high-resolution transmission
electron microscopy (HRTEM) with a high-voltage
⇑ Corresponding author. Tel.: +82 2 880 8970; e-mail: bolee@
snu.ac.kr
transmission electron microscope, we have captured
the detailed dynamics of dislocation slip in Au nanome-
ter-sized protrusions (nanoprotrusions) at the atomic
scale at room temperature. Our real-time monitoring
discloses that the slip of some Shockley partial disloca-
tions cannot be explained by the stress state, but is fa-
vored by surface energy minimization.
For the experiment, 3 mm disks were cut from a pure
Au(1 1 0) single crystal (99.999% purity) (MaTeck
GmbH, Germany). Electron-transparent sections were
produced by ion milling with 3.5 kV Ar ions at an
incidence angle of about 3° from both sides (top and
bottom) in a Gatan precision ion polishing system
(PIPS). To obtain nanometer-sized protrusions, the pre-
pared, plan-view specimens were subjected to beam irra-
diation in a high-voltage electron microscope (Stuttgart
JEOL JEM-ARM1250 (JEOL Ltd., Japan) operated at
1.25 MeV (0.12 nm point-to-point resolution)) [13] at
600 °C for 45 min. At this high temperature, due to
the enhanced sputtering by the beam irradiation, many
nanometer-sized protrusions could be obtained, as
shown in Figure 1a. After cooling down to room
temperature at a rate of 15 °C min–1, the specimens were
observed using the same microscope as used for prepa-
ration of the protrusions. All the HRTEM observations
in the present study were made with the ½ 1 1 0 zone axis
of Au aligned parallel to the electron beam.
The nanoprotrusion shown in Figure 1a had twin
boundaries (TBs) (indicated by arrows), which had been
formed during observation at room temperature. To

1359-6462/$ - see front matter Ó 2011 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.
doi:10.1016/j.scriptamat.2011.03.008
 Author's personal copy

1126 S. B. Lee, Y.-M. Kim / Scripta Materialia 64 (2011) 1125–1128

Figure 1. (a) Initial microstructure of the nanoprotrusion. Alternating twin (T) and matrix (M) lamellae with a spacing of a few nanometers are seen.
(b) Time sequence of HRTEM images taken at the white-boxed region shown in (a). The shift of the crystal block above the slip plane relative to that
below in the left direction resulted in the downward migration of the TB. (c) Schematic diagram of the shift at the ½ 1 1 0 zone axis, marked as D1.

identify the character, i.e. Burgers vector, of Shockley dislocation slip was typically observed in twin lamellae,
partial dislocations participating in dislocation slip, a se- the dislocation is accepted as the trailing partial, which,
quence of HRTEM images (Fig. 1b), was taken of the when added to the leading partial, gives full dislocation
region marked by a white box in Figure 1a. The exper- slip. (For a real-time movie, see the Supplementary
imental images matched well with a simulated image information.)
produced with imaging parameters of a thickness of About 2 min after the images in Figure 1 were taken,
2.3 nm and an overfocus of 38 nm. (For details of the the white-boxed region was observed to have a micro-
image simulation, see the Supplementary information twin of two atomic layers in thickness (i.e. composed
on the image simulation of the HTREM images and of two parallel and neighboring stacking-fault planes),
the video editing. Movie files corresponding to Figs. 1–3
are uploaded as Supplementary videos 2–4, respectively.
The movies are real-time at 25 fps and have views of lar-
ger areas than those printed in the figures.) Figure 1b
shows that the TB at 0 s (indicated by the dashed line)
migrated downwards by one (1 1 1) interplanar spacing
of Au after 0.24 s. As shown in the second panel of
Figure 1b (0.12 s), the migration was accomplished via
a shift of the crystal block above the slip plane in the left
direction relative to the block below. This is schemati-
cally displayed in Figure 1c. As depicted at the bottom
of Figure 1c, the shift at the ½1 1 0 zone axis (i.e. when
viewed from the ½1 1 0 direction), marked as D1, corre-
sponds to the slip of a 1=6½2 1 1 or 1=6½1 2 1 Shockley
partial dislocation on the (1 1 1) plane. However, these
two dislocations cannot be differentiated from each
other in the HRTEM images of the ½1 1 0 zone axis
(Fig. 1c). It should be noted that the slip plane was lo-
cated below the initial TB, that is, in the matrix region
(M), not in the twin lamella (T), as shown in the second
panel of Figure 1b. The partial dislocation slip was typ-
ically captured in other matrix regions, suggesting that
the partial dislocation is considered as the leading par-
tial for creating stacking faults and thus twins. (For a
real-time movie, see the Supplementary information.)
By examining crystal shifts in slip planes located at
twin lamellae, we could identify the trailing partial dislo-
cation for erasing a stacking fault. Figure 2 was also ta-
ken at the same region as in Figure 1a, but 30 s after.
As shown in the second panel of Figure 2a, the crystal
Figure 2. Time sequence of HRTEM images showing a crystal-block
block above a slip plane, which was located at the twin
shift along a slip plane located at the twin lamella (T). In (a), the
lamella (T), shifted to the left relative to the block below crystal block above the slip plane shifted to the left relative to the block
the plane, resulting in the upward migration of the TB below the plane, resulting in the upward migration of the TB (0.16 s).
(0.16 s). Figures 2b and 1c (bottom) illustrate that the (b) The shift, marked as D2, corresponds to the slip of a 1/6½1 1 2
shift, marked as D2, corresponds to the slip of a Shockley partial dislocation on the (1 1 1) plane (see also Fig. 1c
1=6½1 1 2 Shockley partial dislocation. Since the partial (bottom)).
 Author's personal copy

S. B. Lee, Y.-M. Kim / Scripta Materialia 64 (2011) 1125–1128 1127

Figure 3. (a) Time sequence of HRTEM images monitoring the detwinning of the microtwin. (b) The possible partial dislocations responsible for the
shift on plane 2 is marked as A and B by the dashed arrows. (c) Schematic diagram of the comparison of areas of surface steps formed by the shift
along plane 3 (1/6½1 1 
2) (left) and by the leading partial slip (right). The areas shaded in gray indicate surface steps formed by partial dislocation slip
on one surface side. The dashed rectangle shows the lower crystal part below the slip plane and the solid one the upper crystal part above.

as shown in the first panel of Figure 3a. The two stack-
ing-fault planes in the lamella were indicated by long-
dashed lines with numbers 1 and 2 in the second panel
of Figure 3a. The width of the center part of the region
was decreased from 2.5 nm (Fig. 1a) to 1.7 nm; this is
attributed to the sputtering effect of the high-energy
electrons. Figure 3a shows that the microtwin at 0 s dis-
appeared after 0.12 s by erasing the stacking faults on
planes 1 and 2. For plane 1, the crystal block above
the plane shifted to the left relative to the atomic layer
below the plane. (See the movement of the blue circle
relative to the red one in Fig. 3a). The shift corresponds
to a Burgers vector of 1=6½1 1 2, which was of the trail-
ing partial dislocation, as observed in Figure 2a.
For plane 2, as demonstrated in the first to third pan-
els of Figure 3a (0–0.12 s), the atomic layer above the
plane shifted to the right relative to the crystal block
below the plane, also removing the stacking fault on
the plane. (See also the movement of the red circle
relative to the black one.) The shift was the reverse of
that shown in Figure 1b and c (D1) in the HRTEM im-
age (i.e. when viewed from the ½1 1 0 direction), thus
indicating that the Shockley partial dislocation for the
shift on plane 2 would be the reverse of, or at an angle
of 60° with, the leading partial (1=6½2 1 1 or 1=6½1 2 1)
(indicated as B and A by dashed arrows, respectively,
in Fig. 3b), which are not differentiated from each other
in the HRTEM image. The partial for plane 2 is not con-
sidered as being caused by the intrinsic compressive
stress, because this is neither the leading nor the trailing
partial, which will be discussed in detail below.
For plane 3, as shown in the second to fifth panels of
Figure 3a (0.12–0.20 s), the upper crystal block above
the plane shifted to the right relative to the block below,
causing the TB to migrate downwards. Since plane 3 was
located at a matrix region, the shift along the plane is
equivalent to forming a new stacking fault. However,
the shift corresponds to D2, indicating that it did not
occur by the slip of the leading partial shown in Figure 1,
but by the slip of a partial dislocation of 1=6½1 1  2
(Fig. 3b). This slip was not anticipated by the present
stress state. (For a real-time movie for Fig. 3, see the
Supplementary information.)
Since the specimens were examined at room tempera-
ture under the illumination of a high-energy electron
beam, it might be argued that the slip of the Shockley
partial dislocations originated from beam irradiation ef-
fects. However, as is well evidenced, beam irradiation
produces clusters of point defects, such as interstitials
and vacancies, which lead to the formation of Frank
loops, which show the stacking fault feature [14,15].
Put another way, the formation of these faults by beam
irradiation does not involve dislocation slip, as sug-
gested by Kiritani et al. [14]. Thus we conclude that
the partial dislocation slip observed here (Figs. 1–3)
did not result from beam irradiation. Moreover, no
significant beam heating effects are expected due to the
high thermal conductivity of Au (318 W m1 K1), the
temperature rise being calculated to be negligible
(DT = 0.035 K) [16]. However, since the 1250 keV
electron beam used was comparable to the electron dis-
placement threshold energy (1320 keV for Au) [16], dis-
placement of atoms and atomic surface diffusion would
be significantly enhanced, concomitantly facilitating the
nucleation and propagation of partial dislocations.
Thus, the partial dislocation slip under no external
mechanical stress shown in Figures 1–3 is likely to be in-
duced by an intrinsic stress existing within the
nanoprotrusion. A plausible explanation for its origin
is compressive stresses intrinsically placed inside the
nanostructure induced by large tensile surface stress,
as demonstrated for Au nanowires by Diao et al.
[17,18]. Diao et al. [18] showed by atomic simulations
using the embedded atom method that, for Au nano-
wires with square cross-sections, the induced compres-
sive stresses amount to several GPa at nanometer-scale
wire thicknesses, leading to an asymmetry in the ten-
sion–compression yielding and even inducing reorienta-
 Author's personal copy
1128 S. B. Lee, Y.-M. Kim / Scripta Materialia 64 (2011) 1125–1128
tions at critical sizes for h1 0 0i wires [17,18]. For h1 0 0i
nanowires, due to the intrinsic compressive stresses,
elastic contraction occurs upon relaxation, followed, be-
low a critical size, by yielding, elastic contraction and
yielding alternating with each other during the simula-
tion [18]. Though the shape of the nanoprotrusion in
the present study was complicated, the width of the re-
gion of interest (ROI) (indicated by the white box in
Fig. 1a) ranged from 2.49 nm (Fig. 1b) to 1.743 nm
(Fig. 3a) and its thickness was only 2.3 nm. It is thus ex-
pected that the ROIs with such small cross-sectional
areas receive large compressive stresses.
For the detwinning process shown in Figure 3, as
mentioned above, the slip on plane 1 occurred by the
trailing partial. However, the partial dislocation slip
along plane 2 is different from the trailing partial, mak-
ing its generation appear exceptional. The generation of
the Shockley partial responsible for the shift on plane 2
needs to be understood in the context of a possible size
effect on the generation of defects. With the reduction in
size to the nanometer scale, surface energy is likely to
play a significant role in the generation of defects. If a
trailing dislocation erases the stacking fault formed by
a leading partial, generating full dislocation slip, two
surface steps will form on opposite surface sides, each
surface step corresponding to h0 1 1i perfect slip and
resulting in an increase in surface energy. This corre-
sponds to the slip on plane 1.
For plane 2, let us assume that, of the possible two
partials, A and B, A is responsible for the shift
(Fig. 3b) and one of the possible leading partials, e.g.
1=6½2 1 1, acts as the leading partial. The shift by the slip
of partial A will result in full dislocation slip, generating
surface steps corresponding to h0 1 1i perfect slip
(Fig. 3b). This will increase the surface energy, its situa-
tion being the same as that along plane 1. Thus the slip
of A would not be preferred from the energy point of
view. Assuming that partial B is responsible for the shift,
since the partial slip was just the reverse of that of the
leading partial, its slip will remove the previously
formed surface step and thus lead to a decrease in sur-
face energy. This slip should be energetically favorable
and we presume that, since both partials were forbidden
in terms of the stress condition, the shift of –D1 (Fig. 3b)
occurred by the slip of B, rather than A.
The slip of the partial on plane 3 is also explained by
surface energy minimization. Since the nanoprotrusion
was prepared and thinned by beam sputtering, it is rea-
sonable to regard the ROI of the nanoprotrusion
(Fig. 1a) as having a rectangular cross-section with the
above-specified width and thickness. For plane 3, the
step formed 
pffiffiffiby the slip of the partial, 1=6½1 1 2, has an
area of a= 6  the thickness of the ROI (t) on one sur-
face side (Fig. 3c). Since plane 3 was located in a matrix
region and the slip on the plane formed a new stacking
fault, for energy considerations, the step area should be
compared with that formed by the leading partial. The
step formed by the leading partial shown pffiffiffi inpffiffiffiFigure 1
would have an area of roughly a= 6  ( 3=2  the
width (w) of the ROI + 1/2  t) and, considering
1.7 nm for w and 2.3 nm for t, is larger than that by
the partial of 1=6½1 1 2 (Fig. 3c). Thus we know that
the latter partial, rather than the leading partial, is fa-
vored considering surface energy minimization. (For
plane 3, a rectangular cross-section of the nanoprotru-
sion was assumed. However, if different shapes or
dimensions are assumed, different conclusions will be
made. For a circular cross-section, different slip direc-
tions will give no step-area difference. We accept that
such possibilities even seem to suggest that geometrical
factors are critical in deformation mechanisms in nano-
scale materials, which awaits further detailed study.)
A final remark is in order. The types of leading and
trailing partial dislocations observed in a larger nanopro-
trusion (Figs. 1 and 2) underwent a change when its
dimensions were decreased even further, as demonstrated
in Figure 3. We suggest that such a tendency clearly indi-
cates the surface energy dominance in the deformation
mechanism with decreasing size, even violating the expec-
tation from the stress condition (Fig. 3). For nanostruc-
tures, due to their limited size, the nucleation and
propagation of Shockley partial dislocations is expected
to be strongly influenced by surface energy. The present
results support this tenet. Our results suggest that surface
energy is a relevant parameter for analyzing nanoscale
deformation mechanisms, providing a firm foundation
for optimizing theoretical models and atomistic simula-
tions of the mechanical behavior of nanostructures.
This work was financially supported by the Na-
tional Research Foundation (NRF) of Korea funded by
the Ministry of Education, Science and Technology
(2010-0028176).
Supplementary data associated with this article can
be found, in the online version, at doi:10.1016/
j.scriptamat.2011.03.008.
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