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Experimental Study of Fracture Behavior of Magnesium

Single Crystals
V. Kaushika , R. Narasimhana,, R.K. Mishrab
a

Department of Mechanical Engineering, Indian Institute of Science,


Bangalore 560012, India. Tel: +91-80-22932959
b
General Motors Corporation, 30500 Mound Rd., Warren, MI 48090, USA

Abstract
In this work, the fracture behavior of magnesium single crystals is studied by conducting experiments with notched three point bend specimens of
three crystallographic orientations. In the first and second orientations, the
c-axis is along the normal to the flat surface of the notch, while in the third
it is aligned with the notch front. For all the orientations, in-situ electron
back scattered diffraction observations made around the notch root show profuse tensile twinning of {1012}-type. Further, in the first two orientations
basal and prismatic slip traces are identified from optical metallography. The
width of the most prominent twin saturates at around 120 - 150 m, while
twins continue to nucleate farther away to accommodate plastic deformation.
In all the orientations, crack initiation occurs before the attainment of peak
load and the crack grows stably along twin-matrix interface before deflecting at twin-twin intersections. Results show that profuse tensile twinning
is an important energy dissipating mechanism that enhances the fracture

Corresponding author.
Email address: narasi@mecheng.iisc.ernet.in (R. Narasimhan )

Preprint submitted to Materials Science and Engineering: A

November 30, 2013

toughness.
Keywords: Magnesium single crystals; Fracture behavior; Tensile twinning;
Fracture toughness; crack deflection; EBSD
1. INTRODUCTION
Magnesium alloys are well known for their mechanical properties such as
high specific strength at room temperature and low density as compared to
the commonly used aluminum alloys, making them prospective candidates for
applications in aerospace and automobile industries. However, poor corrosion
resistance and low fracture toughness (Yan et al., 2004) impedes their usage.
Most research pertaining to mechanical behavior of magnesium has focused
on understanding tension/compression asymmetry (Barnett, 2007; Knezevic
et al., 2010), stress-strain response (Wonsiewicz, 1966; Kelley and Hosford,
1968; Fernandez et al., 2011) and texture changes (Brown et al., 2005; Graff
et al., 2007). By contrast, few studies have been devoted to investigating the
fracture response of Mg.
Deformation twinning is particularly important in crystals of lower symmetry (e.g, HCP metals), where the Von Mises criterion for general deformation may not be satisfied due to the absence of five independent slip systems. Kelley and Hosford (1968), and Wonsiewicz (1966) investigated the
formation of different types of twins along with slip activities by conducting
channel die compression experiments on magnesium single crystals corresponding to various orientations. They concluded that extension of c-axis
is predominantly accommodated by {1012} tensile twins (TTs), owing to
their low critical resolved shear stress (CRSS), while contraction of c-axis

is accommodated through pyramidal< a + c > slip along with {1011} contraction twins (CTs). This claim was further substantiated by Yoo (1981)
who indicated that only {1012} tensile twin-type and {1011}, {1013} contraction twin-types are active in Mg. Recent experimental work has focused
on polycrystalline magnesium alloys owing to their application in structural
components. Studies by Barnett (2007) on alloy AZ31 have indicated that
extensive tensile twinning may enhance ductility of the alloy. Further, experimental observations by Knezevic et al. (2010) on AZ31 have shown that
formation of CTs cause strain hardening while TTs are found to contribute
very little to strain hardening. Also, they reiterate that extensive formation
of TTs enhances ductility.

In magnesium alloys the fracture toughness can be as low as 7-20 MPa m


(Yan et al., 2004; Somekawa and Mukai, 2006) which will impede their application as structural components. Therefore, the operative fracture mechanisms and crack growth resistance of magnesium alloys need to be carefully
investigated. To understand whether cleavage of basal {0001} plane (Schmid,
1931) and prismatic {1010} plane (Schiebold and Siebel, 1931) is observed
in magnesium, Reed-Hill and Robertson (1957) performed tension experiments on Mg single crystals with loading axis on the basal plane. These
experiments showed parting along {3034} habit plane unlike the commonly
observed basal cleavage in HCP metals. Further, they noted that for the
crystal orientations considered in their work, the fracture mechanism is unaffected by the presence of {1012} twins. From their channel die experiments,
Kelley and Hosford (1968) reported reduced ductility in Mg single crystals
oriented for compression along c-axis and attributed it to the formation of

{1011} twins.
Yan et al. (2004) noted that there is a transition in fracture mechanism
from brittle to ductile with decrease in constraint level in AM60 Mg alloy.
Similar transition was observed by Mukai et al. (2001) in AZ31 Mg alloy
with refinement in grain structure. Somekawa et al. (2009) and Somekawa
et al. (2010) conducted fracture experiments on coarse-grained (grain size of
50 m) and fine-grained (grain size of 5 m) AZ31 Mg alloy, respectively.
They noted that in the fine-grained alloy, sub-grain structures form near
the crack tip promoting blunting and ductile fracture occurs by void growth
and coalescence. On the other hand, the formation of TTs near the crack
tip in the coarse-grained alloy causes premature crack growth along the twinmatrix interface leading to slightly lower fracture toughness. Somekawa et al.
(2009) attributed the reason for crack growth along the twin-matrix interface to dislocation pile up at the twin boundary and incompatibility in the
strains at the interface. By contrast, experiments by Yu et al. (2012) on Mg
single crystals indicated that nanotwins formed near the crack tip to shield
it and promote crack blunting. Similar observations of crack blunting due to
formation of tensile twins were made by Govila (1970) in Be single crystals.
In order to obtain a clear understanding of the fracture behavior of Mg,
a systematic study of interaction of tensile twins with a notch or crack tip
under mode I loading needs to be conducted. Also, the dependence of lattice
orientation with respect to the notch surface or crack plane on twin evolution and fracture resistance should be examined. These issues may be better
studied using Mg single crystal fracture specimens rather than with a polycrystalline Mg alloy. Such a study will allow for tracking the evolution of

individual twins, their interaction with neighboring twins of the same and
different variants and also with a notch tip. To this end, systematic fracture
experiments using pre-notched three point bend specimens of Mg single crystals are conducted within a scanning electron microscope (SEM). Specimens
having three different crystallographic orientations are considered. In two of
the orientations, the normal to the flat surfaces of the notch coincides with
the c-axis, whereas in the third the notch front is aligned along the c-axis.
In-situ observations on the evolution of twins near the notch are made using electron backscattered diffraction (EBSD). Also, optical metallography
is performed on the unloaded specimens to examine the slip and twin traces
and the crack path. Fractographic observations are conducted to understand
the operative fracture mechanism. The results show that in all orientations
studied, profuse TT formation occurs ahead of the notch tip and contributes
to toughening. However, crack growth occurs along boundary of a prominent twin and gets deflected at twin-twin intersections. In a follow-up work
(Kaushik et al., 2013), finite element simulations are conducted to provide
further insights on the mechanics of fracture of Mg single crystals.
2. Experimental Procedure
2.1. Specimen details
The experiments are conducted using edge-notched three point bend
(TPB) specimens as shown in Fig. ??. Three orientations are chosen in
this study. In the first and second orientations, referred to in the sequel as
orientations A and B, the normal to the flat surface of the notch (X2 axis)
is aligned along [0001]. In orientation A, the notch front (X3 axis) is along
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[1210] direction and the crack growth direction (X1 axis) is along [1010]. In
orientation B, the above mentioned notch front and crack growth directions
are interchanged. Orientation C mimics the basal-textured magnesium alloys with the c-axis along X3 , while [1210] and [1010] are along X2 and X1 ,
respectively. The dimensions of the tested specimens pertaining to the three
orientations are summarized in Table 1.
2.2. Specimen preparation and test set-up
The specimens are cut using electric discharge machining (EDM) from
short cylinders of Mg single crystals, grown from seed crystals. A notch of
radius ro = 200 m is machined using EDM up to the center of each specimen
along the width. The specimens are chemically polished with 83% ethanol,
10% HCL, and 7% HNO3 , followed by etching and electropolishing. After
preparing the specimens, EBSD scans in the form of inverse pole figures
(IPF) and image quality (IQ) maps are obtained to check the correctness of
the initial lattice orientation.
The experiments are carried out in LEO-1550 SEM so that it is possible
to make detailed in-situ observations of crack initiation and growth. It is
coupled with EBSD hardware to obtain scans at intermediate loading stages.
This hardware, obtained from EDAX, USA, has a resolution of up to 1 m
supplemented with high speed cameras to expedite the data acquisition. The
SEM is also fitted with a miniature three point bend (TPB) stage procured
from DEBAN, UK, to conduct the fracture tests. The TPB stage is mounted
in the SEM such that it is tilted at an angle of 700 with respect to the horizontal plane. This angle is optimum for acquiring good quality EBSD patterns.
It is ensured that the load on the specimen remains at zero before conducting
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the experiment. The load cell of the TPB stage has a maximum capacity of
200 0.2 N. A lead-screw attached to the loading pin, threaded clockwise at
one end and anti-clockwise at the other imparts displacement to the loading
pin at a rate between 0.1 mm/min to 1.5 mm/min. For the present experiments, a displacement rate of 0.1 mm/min is used. The test is interrupted
at different stages to capture EBSD data and SEM images in the loaded condition. It has been noticed that slip traces on single crystal specimens can
be better visualized using an optical microscope (Patil et al., 2009; Biswas
et al., 2013). Hence, in some cases the specimen is unloaded and taken out
in order to observe it using an optical microscope. The optical images are
taken using Zeiss Axio Vert.A1 microscope. The surface profilometry was
conducted using a Vecco profilometer.
3. Results and discussion
3.1. Load versus displacement curves
The recorded load (P) versus load point displacement () curves are
shown in Fig. ??(a) for all three orientations. The P- curves for all three
orientations show a bilinear behavior until peak load is reached. Thus, for
the sake of illustration, the curve for orientation B has been divided into
parts HI and IJ in Fig. ??(a). The part HI of the curve with a steep slope
depicts an overall elastic response, while IJ with a reduced slope indicates
elastic-plastic behavior. Numerous serrations are observed in the elasticplastic regime (part IJ) of the load-displacement curve. In order to visualize
the serrations better, a magnified view of a region between points E ( =
0.2 mm) and F ( = 0.3 mm) of the P- curve for orientation B is shown
7

in Fig. ??(b). The load drops, giving rise to a saw-tooth like appearance,
are found to correspond with the nucleation of twins which result in sudden
increments in tensile strain (Reed-Hill, 1972).
From in-situ observations in the SEM, the crack initiation stage is noted
and indicated by o on the P- curves (refer Fig. ??(a)). Also, the peak
load is marked by . In all cases, the crack initiates before the peak load
is attained and grows in a slow, stable manner. On comparing the three
orientations, it can be seen that orientation C hardens the most (has the
largest slope of P- curve in the inelastic regime) and attains the highest
peak load, while orientations A and B have similar (but lower) hardening
rates.
3.2. Twin nucleation and growth at the notch root
EBSD data was acquired at different stages of loading and post-processed
to obtain IPF and IQ maps of the scanned surface. Fig. ??(a) represents the
IPF of the as-polished specimen, for orientation A. In the IPF, the lattice
vector parallel to specimen surface normal at any point on the surface characterizes the orientation of that point which is displayed within a standard
triangle in the stereographic projection using a color code. The region F
indicated in the IPF shown in Fig. ??(a) corresponds to unindexed data.
Surface damage during polishing may be responsible for giving rise to the
unindexed data. However, other than this small region, the rest of the surface in Fig. ??(a) is free of residual strains.
Fig. ??(b)-(d) correspond to IQ maps of orientation A at different stages
of deformation. The OIM software identifies the different twin types by coloring the twin boundary with a specific color. For example, TT is identified by
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red color in the IQ maps (refer Fig. ??(b)-(d)). It can be observed from the
above figures that wedge-shaped twins labeled as W and V have nucleated at
the notch root and grown in the region ahead of it. It appears that twin W
is the prominent one (as can be seen from the greater width and length) and
is the first to nucleate at the notch root. The width of this twin is measured
using the image processing software Image-J and is plotted against load P
using a solid curve in Fig. ?? along with similar variation for orientation B
to be discussed subsequently. From the curve it can be seen that up to P
= 2.5 N the twin width increases slowly (since the specimen is experiencing
predominantly elastic deformation). Beyond this load level, an accelerated
growth of the twin width is observed up to P = 5 N followed by a phase
where the twin width saturates at a value of about 120 m. The last phase
coincides with nucleation of twins farther away from the notch root (refer
Fig. ??(d)). It can be concluded that once the growth of the initially formed
twin near the notch root tends towards saturation, new twins nucleate farther
away rapidly to accommodate plastic deformation.
Twin growth occurs due to motion of the twinning dislocations into the
matrix (Christian and Mahajan, 1995). At early stages of deformation this
dislocation motion takes place with fewer obstacles and interactions and
hence, requires lower stresses. At later stages, due to greater dislocation
interactions, higher stresses are required to cause dislocation motion. These
dislocation interactions and the consequent hardening resist twin growth,
promoting the tendency for the twin width to saturate. Also, the twins that
nucleate early grow with less hindrance as compared to the ones that nucleate
later.

The notation used for the various tensile twin variants is indicated in
Table 2. Further, the table summarizes the angle made by each twin variant
with the notch line for orientations A, B and C which are denoted by a ,
b and c , respectively. Here, positive is measured in the counterclockwise
sense with respect to the notch line (i.e., X1 axis). The twin traces observed
in the IPF/IQ maps are identified by comparing the angles made by them
with the X1 axis against the values indicated in this table. In this manner,
the twin variants seen in Fig. ?? for orientation A (as well as for other
orientations to be discussed below) are summarized in Table 3. For example,
the twin trace labeled as W in Fig. ?? corresponds to variant TT1 or TT2 .
Fig. ??(a) shows the IPF of the as-polished specimen for orientation B. It
can be seen from the figure that unlike orientation A, the as-polished surface
of this specimen has twins induced during polishing. These twins are labeled
as E and F and will be referred to in the sequel as polishing twins. The
lattice orientation inside these twins is represented by HCP unit cells along
with that of the matrix which is marked by G. It can be seen that, the
lattice has rotated by 86 degrees inside the twinned region with respect to
the matrix. Fig. ??(b)-(d) show the IPF maps of orientation B at various
load levels. Polishing twin E acts as an obstacle for nucleation and growth
of twins in the region above the notch line and, hence, predominant twin
activity takes place only below the notch line.
In general, twin growth can occur by lengthening and widening of an individual twin or through coalescence with adjacent twins of the same variant
(Ostrikov, 2012). The growth of twin F occurs by the second mechanism as
seen in Fig. ??(b)-(d) where twin M nucleates at the notch root and coalesces

10

with twin F. Twin trace X also grows through twin-twin coalescence. The
lengthwise extension of twin L is obstructed by twin F and it grows only
through widening. This obstruction takes place due to twin boundary incoherency and geometric incompatibility (Christian and Mahajan, 1995; Ostrikov, 2012). Similarly, lengthwise extension of twin X is hindered by twin
Y as seen in Fig. ??(c) and ??(d). On the upper half above the notch line,
the growth of twin U is deterred by the polishing twin E and a secondary
twin T forms inside the latter as shown in Fig. ??(b). These intersecting
twins do not cross each other.
The width of twin F which appears to have grown to the maximum extent
is plotted against the load P in Fig. ??. The twin widening trend in this case
is similar to that exhibited by the prominent twin in orientation A. Thus,
there is an initial slow growth phase when the specimen experiences predominantly elastic deformation, followed by rapid widening and saturation at a
value of about 140 m.
In Fig. ??, EBSD maps for orientation C are presented corresponding
to different load levels. Fig. ??(a) represents the IPF of the as-polished
specimen. In Fig. ??(b)-(d), IPF maps around the notch root with increase
in load are shown. On examining Fig. ??(b) and (c), it can be observed
that unlike in orientations A and B, TTs nucleate away from the notch
root (especially close to the load application zone) and extend towards the
notch with increase in load level (see for example, TTs marked as K and
N). As before, the TT variant to which these twins correspond is identified
and indicated in Table 3. The HCP unit cell is shown in Fig. ??(c) inside
twinned regions K and N as well as in the matrix (marked as O). With further

11

increase in load to a level of 9.6 N, faint trace of twin Z which belongs to


a different variant as compared to K and N forms as seen from Fig. ??(d).
Thus, from Table 3 it can be noted that three types of twin traces form due
to deformation around the notch root in orientation C. This is in contrast
to orientations A and B where only two types of twin traces occur during
deformation (apart from the pre-existing polishing twins).
Fig. ??(d) shows that except for a small region R about 150 m in size
surrounding the notch root profuse tensile twinning has taken place ahead
of the notch. It is well known that TTs can lead to c-axis extension. Since,
c-axis is aligned parallel to specimen thickness for this orientation, this observation implies that predominant region ahead of the notch experiences
out-of-plane bulging which will be confirmed later from surface profile maps.
This is contrary to known behavior exhibited by isotropic plastic solids which
show out-of-plane contraction on the free surface (Narasimhan and Rosakis,
1990). In region R, no TT traces are observed which suggests that there
is no c-axis extension in this region. High resolution EBSD images did not
show any CT activity as well in region R. In order to ascertain if dislocation
activity (especially on pyramidal< a + c > system which can cause out-ofplane contraction) occurs close to the notch root, a TEM study needs to be
performed. This study, however, has not been conducted in the present work.
3.3. Observations of slip and twin traces from optical metallographs
Optical microscopy is used to observe slip traces on the specimen surface
which are otherwise difficult to perceive from in-situ SEM images. An optical
metallograph of a fractured specimen corresponding to orientation A is shown
in Fig. ??(a). The slip traces are classified as S1 and S2 corresponding to basal
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and prismatic slip systems, respectively. From Fig. ??(a), S1 slip traces can
be noticed at the notch flanks and beyond the extended crack tip, whereas
the region around the extended crack shows S2 slip traces. Also, faint twin
traces belonging to two variants can be perceived in Fig. ??(a). On closely
examining Fig. ??(a), slip traces inside a twinned region (secondary slip
traces) can be observed. Thus, it can be seen that RQ representing slip trace
S1 in the matrix region is deflected by 860 in the twinned region (see trace
QP).
Since the flat surface of the notch coincides with basal plane in both
orientations A and B, the slip activities are found to be identical as can
be seen from Fig. ??(b). Thus, S1 slip traces are observed along the notch
flanks while S2 slip traces are noticed in the region ahead of the notch where
crack extension has occurred. Also, secondary slip traces (i.e., within twins)
are observed in the magnified region of the fractured sample corresponding
to orientation B in Fig. ??(c). Thus, in this figure, HI and JK are S1 slip
traces in the untwinned region, whereas IJ is the deflected slip trace inside
the twinned region by 860 .
3.4. Twin volume fraction development through the thickness
As seen in Sec. 3.2, the IPF and IQ maps show profuse tensile twinning around the notch root for all three orientations studied in this work.
Twinning is a three-dimensional phenomenon, whereas the twin traces observed on the free surface are intersections of the twin boundaries with the
surface. Hence, in order to get a perspective of the 3D nature of the twin
boundaries, EBSD data for orientation A was obtained at the quarter-plane
and mid-plane of the specimen in addition to the free surface. To this end,
13

the unloaded specimen was chemically polished and etched (so that external
straining of the crystal is prevented) to reduce the thickness up to the desired
plane (quarter-plane and mid-plane) and subjected to EBSD analysis. The
IQ plots taken around the notch root for orientation A at the free surface,
quarter-plane and mid-plane after unloading the specimen from a load of 5.8
N are shown in the Fig. ??(a)-(c). On examining these figures, it may be
seen that the development of twin traces in all three planes is similar. In
fact, many twins can be seen to extend completely through the specimen
thickness (see for example, the twin marked as W).
The average twin volume fraction (ftta ) is quantified at the three planes
indicated above in order to understand its through-thickness variation. For
this purpose, a planar region PQRS is chosen as shown in Fig. ??(a)-(c).
The area enclosed in this region is first calculated precisely using Image-J
software. Next, the area enclosed by each individual twin is determined by
constructing a polygon along its periphery and calculating the area enclosed
by it. The average twin volume fraction ftta considering a thin slice of material
can then be defined as the ratio of the total area enclosed by all the twins
in the planar region PQRS to the area of this region. By employing this
procedure, the average twin volume fraction at the free surface, quarterplane and mid-plane are evaluated to be 0.24, 0.27 and 0.25, respectively.
Thus, it can be concluded that in orientation A twin volume fraction does
not vary much through the thickness.
In Fig. ??(d) and (e), IQ plots for orientation C at the free surface and
mid-plane obtained after unloading the specimen from a load of 18.3 N are
shown. On comparing Fig. ??(d) and (e), it may be seen that there is a

14

strong 3D character to the development of TTs near the notch root in this
case. Thus, there is more profuse distribution of twin traces in the mid-plane
as compared to the free surface. Indeed, many of the twin traces seen at
the mid-plane cannot be observed on the specimen free surface. Further, the
twins appear wider (i.e., they have grown or coalesced more with adjacent
twins) in the mid-plane than on the free surface. However, three TT variants
can be noticed on both the surfaces (as opposed to two in case of orientation
A). Also, the twin traces do not extend up to the notch root in both the
mid-plane and free surface. In other words, in a small neighborhood of the
notch root, no TTs are observed, which is in contrast to orientation A.
As before, the average twin volume fraction within the rectangular region
PQRS marked in Fig. ??(d) and (e) is determined using image processing. It
is found that the average twin volume fraction ftta at the mid-plane is 0.89 and
is greater than that at the free surface which is 0.78. Therefore, orientation
C, unlike orientation A, shows considerable through thickness variation of
twin volume fraction.
3.5. Energy release rate J and average twin volume fraction ftta versus load
The energy release rate J was computed from the load-displacement
curves presented in Fig. ??(a) using the deep crack formula given by Rice
et al. (1973). This can be written as:

J=

A
,
Bb

(1)

where is a shape factor, b is the uncracked ligament length (W -a), B is


the specimen thickness and A is area under the P- curve. The shape factor

15

is generally taken to be 2 for deeply cracked bend specimens in isotropic


plastic solids (see Rice et al., 1973). However, in the context of Mg single
crystals it is calibrated to be 1.65 by comparing with J computed using the
domain integral method from finite element analysis results (Kaushik et al.,
2013).
The energy release rate J determined by the above procedure is plotted
against load P for all the three orientations in Fig. ??(a) up to crack initiation
stage, which is marked on each of the curves by o. The J values at crack
initiation are 12.21, 4.5 and 10 N/mm for orientations A, B and C, respectively. The notched fracture toughness value Jc of orientation A is slightly
higher than orientation C but it is more than twice that of orientation B.
Although crack initiation load Pc of configuration C is much more than that
of A (refer Fig. ??(a)), it does not reflect in the notched fracture toughness
value. This is because the total work done (comprising predominantly of
plastic dissipation) up to load Pc is greater for orientation A as compared to
the other two orientations.
As in Sec. 3.4, average twin volume fraction ftta is computed over a rectangular region surrounding the notch root from the IPF or IQ maps on
the specimen free surface which were presented earlier (see, for example,
Fig. ??(a)). The evolution histories of ftta are plotted against load P for
all the three orientations in Fig. ??(b). This figure indicates that the twin
growth rates for orientation A and B are similar in the early stages although
for the latter ftta starts evolving from a non-zero initial value due to presence
of polishing twins. However, ftta in this case saturates at a value of about 0.2
as load increases while that for orientation A continues to enhance steeply.

16

Also, although the width of the prominent twin close to the notch root in
orientation A and B saturates at a low load level (refer Fig. ??), the twin
volume fraction around the notch continues to increase as an outcome of
progressive nucleation of twins farther away. In contrast to orientations A
and B, twin volume fraction evolves gradually with load for orientation C.
The trends exhibited by the energy release rate J versus load P for the
three orientations in Fig. ??(a) corroborate well with the evolution histories
of average twin volume fraction around the notch root shown in Fig. ??(b).
This confirms that energy dissipation in all three orientations occurs predominantly due to tensile twins. Thus, the fast twin volume fraction evolution
exhibited by orientation A leads to rapid dissipation in the inelastic zone
and high toughness. Also, the lowest Jc displayed by orientation B despite
its similarity with orientation A may be attributed to saturation in average
twin volume fraction. This has occurred due to presence of pre-existing polishing twins which have impeded the nucleation and growth of deformation
twins around the notch root.
3.6. Extended crack trajectories
On referring to Fig. ??(a), it can be seen that the crack grows in an inclined manner before deflecting instead of following a straight path typically
observed in isotropic plastic solids subjected to mode I loading. Also, it can
be noted from Fig. ??(a) that the crack extends initially along a twin boundary MN which is parallel to twin W (refer Fig. ??). When it encounters a
twin-twin intersection point N, it is deflected along line NO (which is parallel
to twin V indicated in Fig. ??). Fig. ??(a) shows a SEM image of specimen
corresponding to the same orientation, where the crack growth segment MN
17

is seen to be parallel to the twin trace BC. It is noticed that further crack
growth seems to occur along two different twins nucleating at the extended
crack tip O. This suggests that twin formation during crack growth may also
dictate the crack growth direction.
Similar observations can be made in the specimen corresponding to orientation B from Fig. ??(c). The extended crack MN grows into a twin or
along a twin boundary and gets deflected at the intersection point N of two
twins belonging to different variants. The deflected crack NO grows along the
twin-matrix boundary. Thus, it can be concluded that twin-matrix interface
is the preferred crack growth path due to strain incompatibility and high
stress concentrations (Somekawa et al., 2009). Indeed, it has been observed
in Fe-Si single crystals (Berry, 1959 and Hull, 1960) that slip steps formed
at the twin-matrix interface due to dislocation dissociation into partials produces a line of weakness that increases the stress concentration. The scanning
electron micrograph shown in Fig. ??(b) confirms deflection of crack path (as
segments MN-NO) for the specimen pertaining to orientation B. The crack
also forks at point N. Thus, a faint trace of a micro-crack NP which extends
along MN but has arrested subsequently can be perceived. This suggests
that at the intersection point N of two twins, deflection of the crack is favored from an energetic standpoint (i.e, it possibly results in higher energy
release rate). The above issue will be addressed in a follow-up work from
finite element simulations incorporating discrete twins near the notch root
(Kaushik, et.al., 2013).

18

3.7. Fracture surface morphology


Fractography is performed in order to understand the underlying fracture
mechanism. The specimens were broken manually in liquid nitrogen so that
the fracture surface features remain preserved. Fig. ??(a) shows the SEM
fractograph of the specimen corresponding to orientation B, where the region
above the red line denotes the fracture surface formed due to deformation of
the specimen during three point bend loading. A high magnification image
of zone A indicated in the Fig. ??(a) is displayed in Fig. ??(b). This figure
shows that the fracture surface slants towards the free surface starting from
the ridge denoted as PQ. This suggests that the fracture surface does not
necessarily conform to the boundary of a twin at the notch root as implied
above on the basis of the optical image taken on the free surface (Fig. ??(c)).
Instead, it possibly cuts into the twinned region in the specimen interior.
On either side of the ridge PQ, one observes slanted surfaces which contain elongated parallel stripes (see, for example, those marked by RS and
TU). These stripes correspond to the intersection of parallel twins (belonging to a variant different from the one along which the crack has extended)
with the fracture surface (see Fig. ??(b)). The surfaces of the stripes are
relatively smooth implying that they have been sheared as the crack propagates. However, some dimples may be seen inside the stripes which have
been shown encircled in Fig. ??(b). These dimples possibly arise due to dislocation activity in the twinned region and the matrix. The vertical stripes
below the red line in Fig. ??(a) have formed when the specimen was broken
open manually.

19

3.8. Surface profilometry


As mentioned in Sec. 3.2, tensile twinning ahead of the notch in the case
of orientation C suggests occurrence of out-of-plane bulging. In order to
confirm this hypothesis, surface profilometry scans are carried out for this
case up to a distance of 200 m, 350 m, 550 m and 850 m, in front of the
notch root which are shown in Fig. ??(a)-(d). In each of the above figures, 2D
contour maps of the surface as well as variations of the surface profile along
horizontal lines XY are displayed. In the contour maps, the blue and green
regions experience out-of-plane contraction whereas the yellow and red zones
show out-of-plane bulging. On examining Fig. ??(a), it can be seen that close
to the notch root there is out-of-plane contraction which is also confirmed
from the line plot of the surface profile taken along XY. At a distance of
110 m from the notch root (refer Fig. ??(b)), it can be seen that the data
along XY can be divided into 3 regions. Regions P and R correspond to
out-of-plane bulging, whereas region Q pertains to out-of-plane contraction.
Fig. ??(c) and (d) represent surface profiles farther away from the notch and
show that there is out-of-plane bulging with almost no region of contraction.
It should also be noted that out-of-plane extension increases with distance
from the notch root (i.e., as the load application zone is approached).
The out-of-plane bulging at large distances ahead of the notch root which
give rise to tensile twinning as seen in Fig. ??(b) - (d) can be rationalized
as follows. The uncracked ligament ahead of the notch tip is subjected to
bending and hence comprises of zones experiencing tensile and compressive
normal stress 22 which are separated by a plastic hinge point. This point is
found to be close to the notch tip (Kaushik et.al., 2013). Thus, the normal

20

stress on the plane ahead of the notch tip is tensile very close to the notch
root (region R in Fig. ??(d)) and farther away, it becomes compressive. This
compressive normal stress on the ligament, coupled with the compressive
contact stress field close to the loading pin at the edge of the specimen causes
out-of-plane extension due to plastic incompressibility. The numerical results
of Kaushik et.al.(2013) also corroborate with the difference in twin activity
between the mid-plane and free surface for this orientation (Fig.8(d),(e)).
4. Summary and Conclusions
In this work, experiments have been conducted using notched three point
bend specimens to study the mode I fracture response of magnesium single
crystals. Three crystallographic orientations referred to as A, B and C were
chosen for this study. The main observations / conclusions from the work
are summarized below.
The load-displacement curves for the three orientations show that the
hardening rates corresponding to orientation A and B (wherein the caxis is perpendicular to the flat surfaces of the notch) are similar, while
that of orientation C (in which c-axis is parallel to the notch front) is
significantly higher.
Optical metallographs corresponding to orientations A and B reveal
basal and prismatic slip traces. The metallographs also show deflection of basal slip traces by about 860 inside the twinned region (i.e.,
secondary slip).

21

Profuse tensile twinning is observed in all the orientations. In orientations A and B, TT formation commences from the notch root and
spreads outwards, whereas in orientation C, TTs are observed to nucleate near the loading edge and grow towards the notch root but they
do not extend up to it. This behavior has relevance to polycrystalline
Mg alloys that have a basal texture. Indeed, in a rolled Mg alloy AZ31
which has a basal texture profuse TT formation ahead of a crack tip
which leads to strong changes in texture has been recently observed
(Prasad et al., 2013).
The surface profile scans for orientation C show out-of-plane bulging
of the specimen ahead of the notch tip except very close to it. Here,
surface profiles show that there is some contraction. Thus, the TTs
accommodate extension along the c-axis (i.e., thickness direction).
The width of the most prominent twin near the notch root in orientations A and B is found to evolve rapidly at small load levels, but
saturates at around 120-150 m, while twins continue to nucleate farther away to accommodate plastic deformation.
The evolution of average twin volume fraction ftta taken over a rectangular region around the notch root on the specimen free surface with
respect to load corresponding to all three orientations corroborate well
with similar histories of the energy release rate J. It is found that
orientation A has the highest notched fracture toughness followed by
orientation C. The low fracture toughness of orientation B can be attributed to the tendency of ftta to saturate at small loads owing to the
22

presence of polishing twins which impede the growth of new twins for
this case.
Crack initiation occurs just before attainment of the peak load and it
grows stably along the twin-matrix interface before deflecting at twintwin intersections. The fractographs show some penetration of the
crack into the twin and traces of other tensile twin variants intersecting
the fracture surface.
The present study has shown that profuse tensile twinning can cause enhancement in fracture toughness through large plastic dissipation. On
the other hand, if only a few prominent tensile twins form near a notch
root (as in the case of orientation B), large plastic strain may accumulate at the twin-matrix interface leading to premature crack initiation
and low toughness. Thus, this work suggests that an important way
of enhancing the toughness of Mg alloys is to ensure that homogenous
TT nucleation occurs easily so that plastic dissipation gets distributed
over many twins rather than being restricted to a few prominent ones.
Some of the experimental observations such as the occurrence of profuse
tensile twinning in orientation C which causes out-of-plane extension and
deflection of the crack at twin intersections require further analysis. Hence,
to gain additional insights on the mechanics of fracture, finite element simulations using crystal plasticity theory will be reported in a follow-up work
(Kaushik et.al., 2013). This will enable understanding the 3D nature of
plastic slip, twin volume fraction and stress distribution.

23

Acknowledgement
The authors gratefully acknowledge General Motors Research and Development Centre, Warren, Michigan, USA, for financial support through the
sponsored project GM/IISC/SID/PC20037. The authors are thankful to Mr.
Robert Kubic Jr. for his valuable assistance in the experimental work. The
authors are also thankful to Dr. Michael J. Lukitsch for his help in obtaining
the surface profilometry scans.

24

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28

Table 1: Various dimensions of the specimens (see Fig. ??) pertaining to the three orientation considered in the study.

Orientation

2r0

Thickness t

(m)

(mm)

(mm)

(mm)

(mm)

400

4.0

2.0

12.0

1.63

400

4.0

2.2

12.0

1.50

400

4.0

2.0

12.0

1.70

Table 2: Nomenclature used for representing the six tensile twin variants of a HCP crystal
and the angles a , b , c made by traces with the notch line for orientation A, B and C.

Variant

Twin Plane

Twinning shear Direction

T T1

(1012)

[1011]

43.2

0.0

90.0

T T2

(1012)

[1011]

43.2

0.0

90.0

T T3

(1102)

[1101]

T T4

(1102)

[1101]

25.1

39.0

30.0

T T5

(0112)

[0111]

25.1

39.0

30.0

T T6

(0112)

[0111]

25.1

29

25.1 39.0

30.0

39.0 30.0

Table 3: Summary of the observed twin traces of orientations A, B and C which are
identified using the nomenclature given in Table 2

Orientation

Twin trace

Corresponding TT variant

TT1 / TT2

TT3 / TT5

TT1 / TT2

TT3 / TT6

TT3 / TT6

TT3 / TT6

TT4 / TT5

TT4 / TT5

TT4 / TT5

TT4 / TT6

TT3 / TT5

TT1 / TT2

30

a0

b
x2
h
A

31

x1