Letter

pubs.acs.org/NanoLett

Experimental Quantication of Resolved Shear Stresses for

Dislocation Motion in TiN
N. Li,*, A. Misra,, S. Shao, and J. Wang*,

Materials Physics and Applications Division, MPA-CINT and Materials Science and Technology Division, MST-8, Los Alamos
National Laboratory, Los Alamos, New Mexico 87545, United States

Department of Materials Science and Engineering, University of Michigan, Ann Arbor, Michigan 48109, United States
*
S Supporting Information

ABSTRACT: Experimental quantication of the critical

resolved shear stress (CRSS) at the level of unit dislocation
glide is still a challenge. By using in situ nanoindentation in a
high-resolution transmission electron microscope and strain
analysis of the acquired structural images, the CRSS for the
motion of individual dislocations on {110}011 slip system
and glide dislocation re-emission from a tilt grain boundary in
TiN are quantied. This work oers an approach to measure
the local stresses associated with dislocation motion in high-
strength materials.
KEYWORDS: In situ HRTEM, strain mapping, resolved shear stress, dislocation motion, TiN

N ucleation, motion, and reaction of dislocations in

crystalline materials are the elementary unit processes
for understanding mechanical properties. Experimental meas-
urements of the resolved shear stresses for nucleation and
motion of individual dislocations in crystalline materials,
although essential for integration with atomistic modeling to
enable materials design from rst-principles, remain elusive.
Nucleation of dislocations is a thermally activated process, and
the resolved shear stress (RSS) associated with dislocation
nucleation varies with the nucleation sources or sites, the
temperature, and the loading condition. At nite temperatures,
the critical resolved shear stress (CRSS) associated with the
onset of dislocation glide on a given slip system is often inferred
from experimentally determined yield strengths of oriented
single crystals.1,2 Corresponding to the inherent stochastic
nature of dislocation nucleation at nite temperatures, accurate
measurement of the dislocation nucleation stress is challenging
experimentally due to the complicated stress state in the
nucleation domain. When the complexity is ignored, an
estimate may be made through elasticity theory (for instance,
Hertzian elastic contact theory) corresponding to the loading
condition and the tested sample geometry.38 CRSS can be
calculated or estimated for specic loading and sample
geometry without considering temperature eect from
PeierlsNabarro model at continuum scale,911 molecular
statics modeling,1215 and rst-principles density functional
theory calculations.16 However, the CRSS associated with the
glide of dislocations could be measured if the dislocation
motion was observed under an imposed gradient stress eld. In
this work, we demonstrate an approach utilizing in situ
nanoindentation in a transmission electron microscope
(TEM) to measure the CRSS for dislocation motion in TiN,
a model system for a high Peierls stress material. Under a
gradient stress eld generated beneath the indenter, we
observed that dislocations glide away from the indenter and
stop at a point where presumably the local stress drops below
the CRSS. The local strains where the dislocation comes to a
stop are measured from the high-resolution (HR)TEM images
and used to compute the local stresses.
TiN is one of most thoroughly investigated transition metal
nitrides1721 and was chosen to be a representative material for
the demonstration of our approach. These compounds are
brittle at room temperature and show no evidence of
measurable plasticity.22 However, the transition-metal carboni-
trides are widely used to synthesize metalceramic composites
that exhibit high hardness, high melting point, low thermal
conductivity, high shock and wear resistance even at high
temperatures,23,24 and high resistance to radiation damage.25
Particularly, it has been shown that in nanolayered metal
ceramic composites such as Al-TiN, the conned ceramic
nanolayer can plastically codeform with the metallic nano-
layer.17,2629 Therefore, optimizing the strength and ductility of
metalceramic nanocomposites requires better understanding
of the active slip systems and critical stresses for dislocation
glide in ceramics at room temperature.17,27
There is less experimental measurement of the stresses
required for nucleation and glide of dislocations in ceramics.
Such experimental measurements are often carried out for a
small volume of materials at a high stress under a simple
loading (e.g., uniaxial tension and compression) or inden-
Received: February 26, 2015
Revised: June 2, 2015
Published: June 11, 2015

2015 American Chemical Society 4434 DOI: 10.1021/acs.nanolett.5b00791

Nano Lett. 2015, 15, 44344439
Nano Letters Letter

tations.38,30 For metals that have relatively low yield strength

and highly mobile dislocations, uniaxial tension or compression
tests are able to explore dislocation activity.48 However,
uniaxial tension or compression tests are not suitable for
measuring the nucleation and motion of dislocations in high
strength crystalline materials such as ceramics because of
fracture prior to plastic yield.22 Alternatively, nanoindentation
can locally achieve a high stress to enable nucleation and
motion of dislocations. At room temperature, Oden et al.18
reported evidence for dislocation motion in the TiN
indentation tests. By analyzing the postindentation micro-
structures of TiN, they characterized the dislocations to be 1/
2<110>{110} and estimated the critical resolved shear stresses
for nucleation of dislocations to be 3.7 GPa at the load when
pop-in occurs based on a Hertzian elastic contact. Minor et al.19
reported evidence of dislocation-based plasticity in TiN/MgO
thin lms at room temperature according to in situ indentation
tests in a TEM, but they did not measure the CRSS associated
with the motion of dislocations.
By using in situ indentation in a HRTEM, the dislocation
activity in terms of the nucleation, motion, and reactions has
been characterized.58,18,19 Beneting from the development of
quantitative TEM/scanning TEM (STEM) analysis,31 quanti-
tative measurements of displacement elds near defects can be
estimated.3236 In this work, we extended such eort to study
the CRSS associated with dislocation motion in a high strength
crystalline material, TiN, at room temperature using in situ Figure 1. (a) HRTEM image before the indentation test. The loading
indentation in a HRTEM. The primary glide dislocations were direction is perpendicular to TiN (001) plane. (b) HRTEM image of
characterized to be 1/2<110>{110}. Local strains were the nucleated GB after retracting the indenter. Three segments are
marked as GB-I, GB-II, and GB-III. Detailed structure analysis of GB-
calculated from the measured displacements corresponding to II is presented in Figure 2, and that of GB-I and GB-III is presented in
the atomic-column positions in HRTEM images and used to the Supporting Information.
compute the resolved stress for the glide of a dislocation in the
crystal and near a grain boundary.
The TiN lms were grown epitaxially on a single-crystal GB-I, GB-II, and GB-III, as shown in Figure 1, panel b. The
MgO (001) at 650 C. TEM foils of the TiN were prepared by diraction pattern inserted in Figure 1, panel b indicates that
traditional preparation method: mechanical polishing plus ion the grain boundary is a low angle tilt boundary around the tilt
milling. The foil is attached to a piezo-operated scanning axis of [001].
tunneling microscope (STM) probe with silver paint, which The observed dislocations and the grain boundary are further
served as one end of a Nanofactory TEMSTM platform. A characterized in the HRTEM images according to Burgers
chemical etched spherical tungsten tip with diameter of 50100 circuits39 (GB-I and GB-III can be found in Supplementary
nm was the other end of the platform.37,38 The STM probe Figures S1 and S2 of the Supporting Information). Taking the
with the tungsten tip was compressed onto the TEM foil. With GB-II as an example, the GB-II is characterized to be a low
indentation direction perpendicular to the (001) surface, four angle tilt grain boundary around the tilt axis [001] with the
of six slip systems {110}<110> could be favorably activated habit plane of (011) and the tilt angle of 14. By drawing the
with positive Schmids factor. With the electron beam direction Burgers circuit around the defects along the GB-II, we
along [100], the dislocations on 1/2<110>{110} slip systems determine two components of a Burgers vector associated
can be directly captured from the HRTEM images under the with each dislocation. Since the TEM image was taken with the
phase contrast mode. In situ nanoindentation studies were e-beam direction along TiN [100], the shortest distances
conducted at room temperature with a Nanofactory STM between the adjacent atoms that are projected on the (100)
platform inside a Tecnai G(2) F30 TEM. A Gatan charge- plane are associated with 1/2<010> and 1/2<001>. We thus
coupled device (CCD) camera was used to capture draw the Burgers circuit on the HRTEM images along the
deformation of the specimen during indentation with a rate <010> and <001>. As shown in Figure 2, panels IL, three
of three frames/s. The compressive displacement rate is 0.1 types of dislocations are identied. When the Burgers circuit is
nm/s to minimize sample vibration during indentation. closed with two additional vectors 1/2[001] and 1/2[010]
Figure 1, panels a and b show two HRTEM images before (Figure 2I,J), the dislocation thus has the Burgers vector 1/
loading and after unloading during the indentation test. 2[011 ] and is referred to be bf. The glide plane is determined to
Nucleation, glide, and pileup of dislocations were recorded in be (011). When the Burgers circuit is closed with only one
Supplementary Movie 1 of the Supporting Information and are additional vector 1/2[001] (referred to as bp1 and marked in
summarized as follows. The dislocations nucleate from surfaces Figure 2L), the vector bp1 is one component of a dislocation
in contact with the indenter and glide into the sample. These with the Burgers vector 1/2<101> or 1/2<101> on the glide
dislocations stop at a certain distance from the indenter, pile up, plane (101) or (101). As schematically shown in Figure 2,
and form a grain boundary. On the basis of the faceted panel b, the Burgers vector of the dislocations 1/2<101>(101)
morphology of the boundary, we marked it as three segments, and 1/2<101>(101) has only one component 1/2<001> that is
4435 DOI: 10.1021/acs.nanolett.5b00791
Nano Lett. 2015, 15, 44344439
Nano Letters
Figure 2. (a) Magnied atomic conguration of GB-II. The GB-II is a
low angle tilt grain boundary with the habit plane of (011) and the tilt
angle of 14. (b) Schematic illustration of slip systems <110>{110}.
(IL) Magnied atomic structures showing three types of dislocations
identied by drawing the Burgers circuit. The dislocation bf has the
Burgers vector 1/2[011]. The dislocations bp1 and bp2 own vectors 1/
2[001] and 1/2[010] on [100] projection view. They are one
component of a dislocation with the Burgers vector 1/2<101>.
Figure 3. (a) A representative HRTEM image in which a rectangle outlines a region around a center at the atom r0 = (x0,y0). The ith atom positions
with the vector ri with respect to the center. (b) The unit cell for calculation of the strains ijk at the ith atom position. Strain elds of strain
components (c) xx and (d) yy in the HRTEM image. Gaussian distributions of the strains (e) xx and (f) yy.
4436
Letter
projected on the (100) plane. When the Burgers circuit is
closed with only one additional vector 1/2[010] (referred to as
bp2 and marked in Figure 2L), the vector bp2 is one component
of a dislocation with the Burgers vector 1/2<110> or 1/2<110>
on the glide plane (110 ) or (110). In the observed region, the
habit plane of the GB-II is close to (011). Corresponding to
crystallography of TiN and characterization of dislocations
along the GB, the formation of the GB can be described based
on the formation of dislocations pileup. The full dislocation, bf
= 1/2[011 ] , glide on (011 ) and stop where the stress decreases
below the CRSS, resulting in a pile up on the (011) plane and
the formation of a tilt grain boundary. The average spacing
between the adjacent dislocations along the GB is measured to
be L = 1.3 nm. According to Franks formula,40,41 we obtained
the tilt angle = sin1(bf/L) = 13.4, where bf = 0.299 nm
associated with a full dislocation 1/2<110>, consistent with the
experimental measurement (14).
After the indenter was removed from contact (Figure 1b), a
grain boundary was clearly discerned at a distance of 25 nm
away from the surface, and analysis of HRTEM images revealed
the GB to be composed of an array of glide dislocations on the
(011) plane. The GB formation at a characteristic distance
below the indenter contact is attributed to the gradient stress
eld generated by the indentation and the low mobility of
dislocations in TiN at room temperature. We extracted the
critical strains and resolved shear stresses corresponding to the
point where the glide dislocations come to a stop from an
analysis of the acquired HRTEM images, as described further.
Before we discuss the CRSS estimation, we describe the
essential details of strain analysis method. Figure 3, panel a
shows a HRTEM image that was taken from an undeformed
TiN lm. A rectangle outlines a region around a center at the
atom r0 = (x0,y0). There are N+1 numbers of atoms inside the
rectangle. By using the peak pairs analysis (PPA), the ith atom
positions with the vector ri with respect to the center. We rst
calculate the strains ijk at ri, for i = 0...N. The volume average
strains at r0 are calculated according to rjk0 = (1/(N +
1))iN= 0ijk. Figure 3, panel b shows the unit cell for calculation
of the strains ijk. Around the atom at ri, we search for eight
neighbors when the distance |rij| (rij = rj ri) is less than (2 +
2)a/4, where a is the lattice constant of TiN. With the ideal
DOI: 10.1021/acs.nanolett.5b00791
Nano Lett. 2015, 15, 44344439
Nano Letters
lattice as the reference, we calculated the strains ijk using the
least-squares determination of the strain ellipsoid described by
Hoagland et al.42 (also see the details in the Supporting
Information). Figure 3, panels c and d show the strain elds of
two components, xx and yy, that are calculated using the
aforementioned method with respect to the HRTEM image in
Figure 3, panel a. It was noticed that the strain eld is spatially
nonuniform, but the mean strain in the region is close to zero.
Figure 3, panels e and f show Gaussian distributions of the
strains in the region xx and yy, respectively. The mean strains
are equal to zero, and the standard deviation is about 0.005.
To determine the critical resolved shear stress associated
with the glide of 1/2<110>{110} dislocations, we analyze the
strains in the HRTEM image where part of the GB forms and
stops migration during continuous indentation. In Figure 4,
Figure 4. (a) A HRTEM snapshot taken from Supplementary Movie 1
in the Supporting Information, in which part of the GB formed and
stopped migration during continuous indentation. The red dashed line
indicates the stable GB compared to the yellow dashed line (the nal
GB position). Magnied image of the region in the white square in
panel a with respect to the elapsing time of (b) 1 s and (c) 31 s,
respectively. (d) Strain components (xx, yy, and xy) in panel b with
the distance from the contact to the indenter. (e) Strain components
(xx and yy) in panel c with the distance from the contact to the
indenter. xy is not shown with relatively smaller value compared to xx
or yy.
4437
Letter
panel a, the red dashed line indicates the stable GB that does
not migrate during continuous indentation. For reference, the
yellow dashed line indicates the nal GB after the indenter is
removed. We magnied the region (marked in a white square)
in Figure 4, panels b and c with respect to the time. When the
indenter makes contact with the surface (Figure 4b), the strains
analyzed with the aforementioned method are close to zero
with the error bar of 0.5% (Figure 4d). Figure 4, panel e shows
the variation of the strains with distance from the contact as the
GB forms. Both strains xx and yy are compressive. The strain
xy is oscillatory around zero and thus ignored in the stress
analysis. By using the linear elasticity theory with the measured
strains, we calculate the CRSS associated with the 1/2[011 ]
(011) slip system. As plotted in Figure 4, panel c, we found that
the CRSS at the GB (10 nm from the contact) is close to 2.0
0.5 GPa. This is in good agreement with the Peierls stress of
1.45 GPa calculated from the rst-principles density functional
theory.43 It is worth pointing out that the interaction force due
to multiple dislocations in the formation of the GB was ignored
in our analysis since it decays exponentially with distance from
the GB and is insignicant in magnitude compared to the
Peierls stress contribution to CRSS.
The mechanical response of the GB under continuous
indentation is shown in the Supplementary Movie 2 of the
Supporting Information. Figure 5, panel a shows the structure
Figure 5. Snapshots of the GB-II under compression with respect to
the elapsing time of (a) 5.3 and (b) 13 s, respectively. (c) Strains xx,
yy, and xy and the corresponding resolved shear stress in the region
marked as a red rectangle in panel a. (d) Schematic illustrating the
migration behavior of GB-II.
of the GB at 5.3 s. The tilt angle between the two grains
increases from 14 to 16.3. This is ascribed to dislocation
activities in the grain-II, as observed in the Supplementary
Movie 2 of the Supporting Information. In the rst 5.3 s,
dislocations nucleate from surfaces, glide toward the GB-II, and
are blocked at the GB-II. As a consequence, dislocation density
at the GB-II and the tilt angle increase. Most importantly, the
nucleation and glide of dislocations in the grain-I were not
observed; instead, Moire fringes were observed near the GB.
The formation of Moire fringes results from the overlap of two
dierent grains along the electron beam direction.44 With
continuous indentation, Moire pattern expands in the grain-I, as
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Nano Lett. 2015, 15, 44344439
Nano Letters
shown in Figure 5, panel b. The average spacing between two
adjoining fringes is measured to be 1.2 nm, corresponding to
a 10.1 tilt between the two overlapped grains. It is worth
mentioning that the tilt angle between the two grains across the
Moire fringe region remains the same (16.3). Thus, we
proposed a possible mechanism as illustrated in Figure 5, panel
c based on the motion of GB dislocations to account for the
response of the GB.45,46 In Figure 5, panel c, the two light
brown planes represent the front and back surfaces of the TEM
foil. The e-beam direction is perpendicular to the two planes of
the foil. Before the formation of Moire fringes, all GB
dislocations align on the (011) plane, showing a sharp low
angle tilt grain boundary (light blue plane and marked as GB-
II). Under indentation, GB dislocations start to glide away from
the GB-II. Because of the nonuniform pinning eect of surfaces
and possible dislocation intersections,4648 GB dislocations
may not fully move away from the GB-II. Part of a GB
dislocation may glide away from the GB-II plane, schematically
shown in Figure 5, panel c. As a result, the sharp GB-II plane
partially migrates and forms a curved GB plane (the blue plane
and several red dislocation lines on it in Figure 5d), which
results in the formation of Moire fringes during in situ TEM
observation. We further studied the critical activation stress
corresponding to the formation of Moire fringes, that is, the
glide of grain boundary dislocations. We calculated strains in
the region beneath the boundary (marked as a red rectangle in
Figure 5a). Figure 5, panel c shows strains xx, yy, and xy in the
region. The average strains xx, yy, and xy in the region are
2%, 3.5%, and 0.0%, respectively. Corresponding to the
glide of 1/2[011] dislocations on (011) plane, we calculated
the resolved shear stress in the region, and the average RSS is
approximately 4 GPa. This is much higher than the CRSS of 2
GPa for an isolated dislocation, which implies a strong pinning
eect due to the like-sign dislocation array along the GB. Such
RSS is equivalent to a uniaxial compression or tension stress
along <001> at the onset of yield of 4 GPa based on single
dislocation CRSS of 2 GPa, and 8 GPa based on CRSS of
4 GPa for dislocation emission from tilt boundary. Typically,
bulk TiN cannot approach such high tension or compression
yield stress without cracking, although room-temperature
plasticity of TiN has been inferred in nanolayered Al-TiN
composites.17,27
In summary, we have characterized plastic deformation of
TiN at room temperature with the glide of 1/2<110>{110}
dislocations that nucleate from surfaces beneath an indenter.
The CRSS corresponding to the glide of an isolated dislocation
was estimated to be 2 GPa, and the CRSS corresponding to
the emission of dislocations from the low angle tilt grain
boundary is 4 GPa. More importantly, we demonstrated the
possibility to experimentally measure the critical stresses
associated with the glide and emission of dislocations in TiN
at room temperature using in situ indentation in a HRTEM.
This approach is applicable for crystalline materials that have
high strength and are brittle at room temperature.
ASSOCIATED CONTENT
*
S Supporting Information
HRTEM images of GB-I and GB-III in the TiN. Strain analysis
method. In situ indentation of the single crystal, TiN, played at
15 speed (3 frames/sec) and showing the nucleation, glide,
and pileup of lattice dislocations at room temperature. In situ
indentation of the bicrystal, TiN, played at 10 speed (3
frames/sec) and showing the mechanical response of the low
4438
Letter
angle tilt grain boundary at room temperature. The Supporting
Information is available free of charge on the ACS Publications
website at DOI: 10.1021/acs.nanolett.5b00791.
AUTHOR INFORMATION
Corresponding Authors
*Phone: +1 505 665 1857. E-mail: nanli@lanl.gov.
*Phone: +1 505 667 1238. E-mail: wangj6@lanl.gov.
Author Contributions
N.L. performed in situ indentation experiments. N.L., S.S. and
J.W. performed theoretical analysis. A.M. and J.W. supervised
the entire project. All authors commented on the manuscript.
Notes
The authors declare no competing nancial interest.
ACKNOWLEDGMENTS
This work was supported by the U.S. Department of Energy
(DOE), Oce of Science, Oce of Basic Energy Sciences. This
work was performed, in part, at the Center for Integrated
Nanotechnologies, an Oce of Science User Facility operated
for the U.S. DOE, Oce of Science. Los Alamos National
Laboratory is operated by Los Alamos National Security, LLC,
for the National Nuclear Security Administration of the U.S.
DOE under Contract No. DE-AC52-06NA25396. We
appreciated the valuable discussion with Prof. J.P. Hirth and
R.G. Hoagland at Los Alamos National Laboratory.
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4439 DOI: 10.1021/acs.nanolett.5b00791

Nano Lett. 2015, 15, 44344439