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Department of Physics, Center for Electron Microscopy and Key Laboratory of Acoustic and Photonic Materials and Devices, Wuhan
University, Wuhan 430072, China
bS Supporting Information
ABSTRACT: The deformation, fracture mechanisms, and the
fracture strength of individual GaN nanowires were measured in
real time using a transmission electron microscope scanning
probe microscope (TEM-SPM) platform. Surface mediated
plasticity, such as dislocation nucleation from a free surface
and plastic deformation between the SPM probe (the punch)
and the nanowire contact surface were observed in situ.
Although local plasticity was observed frequently, global plasticity was not observed, indicating the overall brittle nature of
this material. Dislocation nucleation and propagation is a
precursor before the fracture event, but the fracture surface shows brittle characteristic. The fracture surface is not straight but
kinked at (10-10) or (10-11) planes. Dislocations are generated at a stress near the fracture strength of the nanowire, which ranges
from 0.21 to 1.76 GPa. The results assess the mechanical properties of GaN nanowires and may provide important insight into the
design of GaN nanowire devices for electronic and optoelectronic applications.
KEYWORDS: GaN nanowire, nanomechanics, dislocation, plasticity, fracture, in-situ electron microscopy
nanowires were then manipulated to approach either a nanoindentor or a at-ended scanning tunneling microscopy probe
(STM) for in situ compression experiments. In the former, the
force-displacement could be directly measured and recorded by a
computer. The compression was displacement controlled with
the speed varying from 0.1 to 6.8 nm/s.
Figure 2a d and Supporting Information movie M1 show
that dislocations were nucleated from a free surface (Figure 2a,b),
and then propagated along a prismatic plane of the nanowire,
leading to a displacement of the upper segment with respect to
the lower segment of the nanowire (Figure 2c); eventually the
nanowire broke from the location where slippage had occurred
(Figure 2d). Dislocation nucleation from a free surface has been
observed in metallic nanomaterials,25,26 but it has not been
reported in semiconductor nanomaterials to our knowledge.
The result suggests that surface dislocation nucleation may be
a general phenomena to many nanostructured materials, regardless of their metallic, semiconducting, or ceramic nature.
Figure 2e i (Supporting Information movie M2) is another set
of data showing the slip event before the fracture of the nanowire.
There was an abrupt diameter change near the base of the
nanowire, causing a surface step as pointed out by an arrowhead
in Figure 2e. Slip or shear initiated from the step (Figure 2e),
propagated along a prismatic slip plane (Figure 2f), and
Received: January 1, 2011
Revised:
February 13, 2011
Published: March 18, 2011
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Nano Letters
LETTER
Figure 1. The cross-section of the GaN nanowire is triangular. (a) An atomic structural model of the cross-sectional view of the nanowire. The nanowire
with a growth direction of [1-210] is enclosed by the (000-2), (-1011), and (10-11) planes. (b) A TEM image showing the triangular cross-section of the
nanowire. The enclosed angles between dierent planes are consistent with the model shown in (a). (c) A plan-view of the triangular nanowire. (d) A
general electron diraction pattern from a GaN nanowire. Streaks along the (0002) diraction series indicated stacking faults in the nanowires.
Nano Letters
many nanowires (Supporting Information Figure S3). Dislocations were also observed near the fracture area (Figure 3i,
arrows). High-resolution transmission electron microscopy
(HRTEM) (Figure 3j) shows that the atomic scale fracture
surface is not at but kinked at (10-10) and (10-11) planes,
both of which are the slip planes in a hexagonal system.
Figure 4a c (Supporting Information movies M10, M11) and
Figure 4g,h (Supporting Information movie M12) are higher
magnication images showing the local plasticity in GaN nanowires under compression. The nanowire is a single crystal with a
triangular cross-section and a diameter of 135 nm, and dislocations are present near the top surface (Figure 4a), possibly
introduced unintentionally during the alignment of the probe
with the nanowire. As the punch pushed on the nanowire, the
nanowire collapsed near the punch and nanowire contact surface,
forming a mushroom-shaped heavily plastically deformed zone
(Figure 4b,c). Detailed structural investigation indicated that the
lattice in the deformed zone was heavily distorted with small
nanocrystals broken o the nanowire (Figure 4d), and a high
density of dislocations were observed in the heavily deformed
zone (Figure 4e). The Burgers vector of the dislocation was
determined to be 1/3[-2110] and the slip plane is (01-1-1).
These results show that there is signicant surface plasticity
in the GaN nanowires, and that the plastic deformation is
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Nano Letters
LETTER
Figure 5. Force-displacement plot (a) and fracture strength (b) of GaN nanowires with dierent diameters.
suggest that a small plastic event may not be reected in the forcedisplacement curve, which was also observed in metallic pillars.27
We found that the fracture strength of GaN nanowires
increases with a decreasing diameter (Figure 5b), and the reason
for this size eect may be related to the strain gradient induced by
bending during the compression. Because the aspect ratio in our
nanowire is usually larger than 5, bending or buckling usually
occurred in the compression experiments, which introduced a
strain gradient in the nanowire.
The local plasticity observed in GaN nanowire is dierent
from the global plasticity observed in metallic pillars in which
dislocations quickly run out of the surface of the pillars before
new dislocations are nucleated, leading to a dislocation starvation
state in the pillar.28 33 In GaN nanowires, the dislocations were
nucleated from the punch and nanowire contact surface, and
then piled in the contact area until a local plastic zone was
formed. The local plasticity was caused by surface roughness of
the nanowire and the punch. Similar local plasticity may also exist
in metallic materials.
It is interesting to compare our results with recent compression experiments of Si and GaAs nanopillars.34,35 In the case of Si
pillars, in uniaxial compression tests pillars having a diameter
exceeding a critical value develop cracks, whereas smaller pillars
show ductility comparable to that of metals.34 The critical
diameter is between 310 and 400 nm. This kind of brittle to
ductile transition under a critical diameter was not observed in
GaN nanowires. In the case of GaAs nanopillars, ductile plasticity
was observed in pillars with a diameter of 1 m.35 The diameter
of all the GaN investigated in our studies is less than 500 nm, yet
no global plasticity was observed in these nanowires. It is noted
that our nanowires are in their pristine state before the in situ
compression experiments, while the Si and GaAs pillars were
fabricated by focused ion beam (FIB), and it is well-known that
FIB can cause signicant damage to semiconductor materials. It
is possible that the FIB damage may contribute to the large
plasticity observed in the Si and GaAs pillars. However, this needs
further experimental conrmation. We do nd that the fracture
strength in GaN nanowires is similar to that observed in GaAs
pillars, implying that the strength of GaAs pillars was not aected
by FIB process.
The dislocation slip and lattice plane shearing-initiated fracture
agrees well with the recent simulation results in Si nanowires.36,37
ASSOCIATED CONTENT
bS
AUTHOR INFORMATION
Corresponding Author
*E-mail: jhuang@sandia.gov.
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Nano Letters
ACKNOWLEDGMENT
We acknowledge support from Sandias Solid State Lighting
Science Energy Frontier Research Center, funded by DOE BES,
and the NNSAs Laboratory Directed Research and Development program. A part of this work was performed at the Center
for Integrated Nanotechnologies, a U.S. DOE, BES user facility.
Sandia National Laboratories is a multiprogram laboratory
managed and operated by Sandia Corporation, a wholly owned
subsidiary of Lockheed Martin Corporation, for the U.S. Department of Energys National Nuclear Security Administration
under contract DE-AC04-94AL85000. H.Z. thanks Chinese
Scholarship Council for nancial support. S.X.M. acknowledges
NSF CMMI 08 010934 through University of Pittsburgh and
Sandia National Laboratories support.
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