Construction and Building Materials 47 (2013) 1160–1166

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Construction and Building Materials

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Bilinear tension softening diagrams of concrete mixes corresponding

to their size-independent specific fracture energy
A. Ramachandra Murthy a, B.L. Karihaloo b,⇑, Nagesh R. Iyer a, B.K. Raghu Prasad c
a
CSIR Structural Engineering Research Centre, Chennai 600 113, India
b
School of Engineering, Cardiff University, Cardiff CF24 3AA, UK
c
Indian Institute of Science, Bangalore 560 012, India

h i g h l i g h t s

 A procedure for constructing bilinear tension softening diagrams of concrete mixes.

 The tension softening diagram corresponds to the size-independent fracture energy of the mix.
 Inverse identification based on hinge model.

a r t i c l e i n f o a b s t r a c t

Article history: The study of the fracture behaviour of concrete structures using the fictitious crack model requires two
Received 1 February 2013 fracture properties of the concrete mix, namely, the size-independent specific fracture energy GF, and the
Received in revised form 28 May 2013 corresponding tension softening relation r(w) between the residual stress carrying capacity r and the
Accepted 3 June 2013
crack opening w in the fracture process zone ahead of a real crack. In this paper, bi-linear tension soften-
Available online 4 July 2013
ing diagrams of three different concrete mixes, ranging in compressive strength from 57 to 122 MPa
whose size-independent specific fracture energy has been previously determined, have been constructed
Keywords:
in an inverse manner based on the concept of a non-linear hinge from the load-crack mouth opening plots
High strength concrete
Ultra high strength concrete
of notched three-point bend beams.
Fictitious crack model Ó 2013 Elsevier Ltd. All rights reserved.
Size independent specific fracture energy
Tensile stress
Crack width

1. Introduction
The non-linear theory of fracture mechanics based on the ficti-
tious crack model is generally employed for the analysis of cracked
concrete structures [1]. This model is based on the fact that an
extensive fracture process zone (FPZ) exists ahead of a real
traction-free crack in which concrete softens progressively due to
micro-cracking and other energy dissipation processes. This ten-
sion softening FPZ is included in the model as a fictitious crack
(or a cohesive zone), which means that this portion of the crack
cannot be continuous with full separation of its faces, as in a real
traction-free crack. The fictitious crack faces are able to transfer
some residual stresses across them which are not constant over
its length. It is known that under mode I loading the residual ten-
sile stress increases from zero at the tip of a real traction-free crack
to the full uni-axial tensile strength of concrete at the tip of the
⇑ Corresponding author.
E-mail address: KarihalooB@Cardiff.ac.uk (B.L. Karihaloo).
fictitious crack (Fig. 1). For the fictitious crack model (FCM), two
material properties of concrete, namely, the size-independent spe-
cific fracture energy, GF, and the corresponding tension softening
relationship r(w) relating the residual stress transfer capacity r
to the opening displacement w of the fictitious crack faces are
needed in addition to its tensile strength ft and Young’s modulus,
E. In practice, the r(w) relationship is generally assumed as linear,
bilinear, multi-linear or even an exponentially decaying curve with
the bilinear approximation being the most common [2]. The popu-
larity of the bilinear approximation of the tension softening dia-
gram (TSD) stems from the fact that it captures the two major
mechanisms responsible for the observed tension softening in con-
crete, namely micro-cracking and frictional aggregate interlock.
In a recent paper [3] the present authors have described an
extensive investigation into the determination of the size-indepen-
dent specific fracture energy GF of three different concrete mixes
ranging in compressive strength from 57 to 122 MPa. The size-
dependent specific fracture energy Gf of these mixes was first
determined by the RILEM work of fracture method [2]. Then the

0950-0618/$ - see front matter Ó 2013 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.conbuildmat.2013.06.004
 A. Ramachandra Murthy et al. / Construction and Building Materials 47 (2013) 1160–1166 1161

Fig. 1. (a) A real traction-free crack of length a0 terminating in a fictitious crack of length 1p whose faces close smoothly near its tip (K1 = 0), (b) The material ahead of the
fictitious crack tip is assumed to be linear, and (c) The material within the fracture process zone is softening; the area under softening curve equals fracture energy [2].

boundary effect and P–d tail correction methods were applied to applicability to notched three-point bend (TPB) beams using a
determine the size-independent specific fracture energy of these bilinear approximation for r(w). During the inverse analysis, a load
mixes [3]. This paper describes the construction of tension soften- versus crack mouth opening displacement (P-CMOD) curve is ob-
ing diagrams (TSD) for these three different concrete mixes corre- tained for several trial r–w curves, each defined by a set of param-
sponding to their size-independent specific fracture energy using eters, and compared with the experimental P-CMOD curve until
the inverse analysis method. the difference between the measured and simulated results is min-
The tensile test is the most direct way to determine the stress- imized. The advantage of the non-linear hinge model is that it
crack opening relationship r(w) [4,5]. However, problems related yields closed-form analytical solutions for the entire load-crack
to gripping, load eccentricity and the determination of exact crack
location (for crack opening to be controlled) make the uniaxial
tension test difficult to perform. Moreover, the direct tension test
measures the average stress deformation response of the specimen
and not the true relationship of cohesive stress and crack opening
[6]. To avoid these difficulties, Li et al. [7] proposed a method based
on the J-integral to determine indirectly the stress-crack width rela-
tionship. However, this method involves the differentiation of
experimental results which affects the accuracy of the derived
r–w relationship. Recently, an inverse analysis method has been
developed to identify the fracture parameters of concrete from the
notched three-point bend and compact tension test results [6,8–12].
This inverse analysis is greatly simplified through the use of the
concept of a nonlinear hinge, first proposed by Ulfkjaer [13] in
which the flexural response of notched concrete beams is modelled
by the development of a fictitious crack at the notch tip in the
central region of the beam. The width of this region, proportional
to the beam depth, fixes the width of the non-linear hinge. It was
assumed that r(w) is linear. This model was further developed Fig. 2. Three-point notched bend beam with a non-linear hinge modelling the
by Stang and Olesen [14] and Olesen [15] to demonstrate its propagation of a crack at mid-section [10].
1162 A. Ramachandra Murthy et al. / Construction and Building Materials 47 (2013) 1160–1166

Fig. 3. A bilinear stress-crack opening relationship and the four different phases of crack propagation. Phase 0 = state of stress prior to cracking; Phases I–III = states of stress
during crack propagation [10].


opening displacement curve. However, since the P-CMOD curves Ee pre-cracked state
corresponding to the size-independent specific fracture energy
r¼ ð1Þ
rðwÞ ¼ gðwÞf t cracked state
have not been measured experimentally, the inverse procedure is
first applied to the experimental P-CMOD curves recorded in the where E is the elastic modulus; e is the elastic strain; w is the crack
RILEM work of fracture method and the resulting bilinear diagrams opening; ft is the uniaxial tensile strength; and g(w) is the function
are then scaled appropriately to reflect the size-independent spe- representing the shape of the stress-crack opening relationship,
cific fracture energy. normalized such that g(0) = 1. For the assumed bilinear shape
(Fig. 3), we have
2. Cracked hinge model

b1  a1 w; 0 6 w 6 w1
In the fictitious crack model, it is assumed that prior to crack gðwÞ ¼ ð2Þ
b2  a2 w; w1 6 w 6 w2
initiation from a starter notch, the material exhibits linear elastic
behaviour. After crack initiation, it is assumed that stresses may
be transmitted across the fictitious crack faces. These crack bridg- 1  b2
ing forces are taken to be a function of the crack opening displace- w1 ¼ ð3aÞ
a1  a2
ment given by the stress-crack opening relationship. The bending
failure of notched concrete beams may be modelled by the devel-
opment of a fictitious crack in an elastic layer ahead of the starter b2
w2 ¼ ð3bÞ
notch. The width of this layer is assumed to be proportional to the a2
beam depth. The basic idea of the non-linear cracked hinge model
is to isolate the part of the beam close to the propagating crack (i.e. where b1 = 1; and the limits w1 and w2 are given by the intersection
the part under maximum bending moment) as a short beam seg- of the two line segments, and the intersection of the second line
ment subjected to a bending moment and axial force. Fig. 2 shows segment with the abscissa, respectively (Fig. 3).
a typical notched TPB specimen. In the non-linear hinge model the An analysis of the hinge element allows the determination of
crack is viewed as a local change in the overall stress and strain the axial load N and bending moment M for any given angular
field. This change is assumed to vanish outside a certain band of hinge rotation 2u (Fig. 4). The problem now is solved in four
width s (Fig. 2). Thus, outside of this band the structural element stages, one for each phase of the crack propagation. Phase 0 repre-
is modelled using the elastic beam theory. The boundaries of the sents the elastic state, when no crack has formed from the initial
hinge are assumed to undergo only rigid body rotation and trans- notch, while phases I, II and III represent different stages of crack
lation. The constitutive relationship for each segment inside the propagation (Fig. 3). In phase I, the fictitious crack of length d is
hinge is assumed to be linear elastic in the pre-cracked state (phase such that the maximum crack opening is less than w1. In phase
0), while the cracked state is approximated by a bilinear softening II, a part of the fictitious crack of length d has a crack opening in
curve as shown in Fig. 3, excess of w1 but in the remaining part it is less than w1. In phase
III, a part of the crack has opened more than w2 and thus become
traction-free, while the opening of the remaining part is still less
than w2 or even less than w1.

Table 1
Mechanical properties of NSC, HSC and UHSC.

Mix Steel fiber by vol. Cylinder Split Modulus Size-

(length = 13 mm compressive tensile of independent
dia. = 0.18 mm) strength strength elasticity specific
(MPa) (MPa) (GPa) fracture
energy, GF
(N/m)
NSC – 57.1 4.0 35.8 184.5
HSC 2% 87.7 15.4 37.9 6194.7
UHSC 2% 122.5 20.7 43.0 13760.7
Fig. 4. Geometry, loading and deformation of the hinge element [10].
 A. Ramachandra Murthy et al. / Construction and Building Materials 47 (2013) 1160–1166 1163

4000

3500 6000
Model Test
Test Model
3000 5000
Load, N

2500

Load, N
4000
2000
3000
1500
2000
1000

500 1000

0 0
0 0.05 0.1 0.15 0.2 0.25 0.3 0.35 0.4 0 0.05 0.1 0.15 0.2 0.25 0.3
CMOD, mm CMOD, mm
(a) NSC - 500x50x100 mm (notch to depth ratio =0.1) (b) NSC- 1000x50x200 mm (notch to depth ratio =0.2)

4500 14000
4000 Model Model
Test 12000 Test
3500
10000
3000

Load, N
Load, N

2500 8000

2000 6000
1500
4000
1000
500 2000

0 0
0 0.5 1 1.5 2 2.5 3 3.5 4 0 0.5 1 1.5 2 2.5 3 3.5 4
CMOD, mm CMOD, mm
(c) HSC – 250x50x50 mm (notch to depth ratio =0.1) (d) UHSC- 650x50x130 mm (notch to depth ratio =0.3)
Fig. 5. Load-CMOD curves generated by the hinge model and average experimental load-CMOD curves.

Table 2
Bilinear softening parameters for NSC based on size-dependent Gf.

Beam dimensions (mm) Notch to depth ratio a1 (mm1) a2 (mm1) b2 ft (MPa) w1 (mm) w2 (mm) Gf (N/m) r1 (MPa)
250  50  50 0.1 19.780 3.570 0.243 3.013 0.047 0.068 117.3 1.323
0.2 22.560 3.400 0.238 2.982 0.039 0.070 85.3 1.344
0.3 22.671 3.780 0.261 3.112 0.034 0.078 57.7 1.358
500  50  100 0.1 10.657 1.253 0.316 2.919 0.073 0.252 135.3 1.370
0.2 12.654 1.086 0.328 2.561 0.058 0.302 107.5 1.285
0.3 14.134 1.121 0.359 2.732 0.049 0.321 95.5 1.290
1000  50  200 0.1 12.960 2.760 0.571 3.121 0.042 0.206 153.0 1.281
0.2 15.345 1.987 0.478 2.938 0.039 0.240 126.3 1.271
0.3 16.112 2.130 0.550 3.012 0.032 0.258 109.3 1.276
Avg. 16.604 2.295 0.371 2.932 0.046 0.199 109.7 1.311

Table 3
Bilinear softening parameters for HSC based on size-dependent Gf.

Beam dimensions (mm) Notch to depth ratio a1 (mm1) a2 (mm1) b2 ft (MPa) w1 (mm) w2 (mm) Gf (N/m) r1 (MPa)
250  50  50 0.1 1.033 0.141 0.398 6.785 0.675 2.830 4109.5 2.055
0.2 1.163 0.143 0.399 6.541 0.589 2.789 3679.7 2.061
0.3 1.088 0.142 0.410 6.593 0.623 2.891 3479.7 2.123
0.4 1.079 0.139 0.404 6.634 0.634 2.901 2923.0 2.093
500  50  100 0.1 1.199 0.127 0.355 7.012 0.601 2.789 4396.3 1.955
0.2 1.177 0.126 0.345 7.123 0.623 2.745 4155.3 1.899
0.3 1.167 0.129 0.364 6.984 0.613 2.802 4020.0 1.987
0.4 1.125 0.127 0.370 6.897 0.631 2.912 3397.0 2.001
Avg. 1.129 0.134 0.381 6.821 0.623 2.832 3770.1 2.021

2.1. Application of hinge model to TPB application of the load is shifted relative to the mouth of the starter
crack, dg
The opening displacement at the mouth of the pre-existing star-
ter crack (CMOD) in TPB specimens consists of three contributions. CMOD ¼ dCOD þ de þ dg ð4Þ
These are the opening due to the crack emanating from the starter
crack, dCOD, the opening due to elastic deformation, de, and the dCOD is the crack opening at the bottom of the crack in the hinge,
opening due to geometrical considerations because the line of that is, at y = hg (Figs. 2 and 4),
1164 A. Ramachandra Murthy et al. / Construction and Building Materials 47 (2013) 1160–1166

Table 4
Bilinear softening parameters for UHSC based on size-dependent Gf.

Beam dimen-sions (mm) Notch to depth ratio a1 (mm1) a2 (mm1) b2 ft (MPa) w1 (mm) w2 (mm) Gf (N/m) r1 (MPa)
250  50  50 0.1 0.649 0.149 0.461 11.625 0.987 3.092 10405.3 3.654
0.2 0.759 0.158 0.473 11.562 0.876 2.987 8148.5 3.867
0.3 0.811 0.133 0.399 11.576 0.886 2.998 6798.8 3.254
0.4 0.764 0.159 0.447 11.434 0.913 2.812 4406.3 3.457
400  50  80 0.1 1.206 0.153 0.462 11.576 0.510 3.023 11452.8 4.453
0.2 1.169 0.154 0.459 11.435 0.532 2.984 8733.8 4.321
0.3 1.097 0.151 0.467 11.568 0.562 3.102 7036.8 4.432
0.4 1.138 0.155 0.466 11.598 0.543 3.003 4976.8 4.432
650  50  130 0.1 1.571 0.139 0.419 11.315 0.405 3.012 11945.3 4.112
0.2 1.559 0.131 0.411 11.285 0.412 3.121 8306.8 4.034
0.3 1.688 0.119 0.384 11.462 0.392 3.230 6981.5 3.876
0.4 1.622 0.126 0.399 11.413 0.401 3.176 5961.5 3.987
Avg. 1.174 0.144 0.437 11.487 0.618 3.045 7929.5 3.989

sft ð1  bi þ 2ah hÞ energy. Details of the mix proportions, specimen preparation,

dCOD ¼
E ð1  bi Þ
where s is the width of the hinge, ah = d/hg, h = hgEu/sft, u is half of
the hinge rotation and the parameter bi can be obtained from
sai ft
bi ¼
E results of NSC, HSC and UHSC beams. The optimized coefficients
de in Eq. (4) can be found from handbooks [16]. The contribution
from dg has been found to be negligible for the specimen geometries
tested. The applied load in the TPB specimen is related to the nor-
malized bending moment l(h) through the following relation [10]
2
2 ft hg t
P¼ lðhÞ
3 L
where L is the total length of the beam.
In the cracked phases I–III, the solution for P can be obtained in
an iterative manner from the following implicit equation [10]
lext ðPÞ  ljint ðh; PÞ ¼ 0
where lext(P) represents the external normalized moment on the
hinge which can be determined from the force balance condition
(see Fig. 1b), while ljint ðh; PÞ is the internal normalized moment
capacity of the hinge given by analytical expressions corresponding
to the actual phase of the crack propagation. These expressions have
been obtained by considering the force and moment equilibrium of
the hinge in each crack propagation phase [14].
The value of h corresponding to each phase is calculated from
the analytical expressions given in [14,17]. Then for this value of
h the normalized moment, l(h) and the crack length, ah are calcu-
lated, followed by the theoretical CMOD and load P (from Eqs. (7)
and (8)). Finally, the sum of squares of the errors between the
theoretical and experimental values of the load is minimized with
respect to the three unknown parameters of the bilinear TSD
ð5Þ
and testing are given in [3].
Load – CMOD curves have been generated by using the above
inverse procedure for various beams with different notch to depth
ratios. Fig. 5 shows the typical load – CMOD curves generated from
hinge model and the corresponding RILEM work of fracture test
ð6Þ
al, a2 and b2 obtained by using the hinge model and minimizing
the difference between the theoretical and recorded load-CMOD
curves are given in Tables 2–4.
From Tables 2–4, it can be observed that the bi-linear parame-
ters obtained from the inverse analysis are highly dependent on
the size of the specimen, notch to depth ratio and specific fracture
ð7Þ energy (Gf). For the NSC used in the present investigation it varied
between w1 = 0.032 mm for a specimen with W = 200 mm and a/
W = 0.3 to w1 = 0.073 mm for a specimen with W = 100 mm and
a/W = 0.1 (Table 2). Similarly, it varied between w2 = 0.068 mm
for a specimen with W = 50 mm and a/W = 0.1 to w2 = 0.321 mm
ð8Þ for a specimen with W = 100 mm and a/W = 0.3 (Table 2). For the
HSC (Table 3), w1 varied between 0.589 mm (W = 50 mm, a/
W = 0.2) and 0.675 (W = 50 mm, a/W = 0.1) whereas w2 varied
between 2.745 mm (W = 100 mm, a/W = 0.2) and 2.912 mm
(W = 100 mm, a/W = 0.4). For the case of UHSC (Table 4), w1 varied
between 0.392 mm (W = 130 mm, a/W = 0.3) and 0.987 mm
(W = 50 mm, a/W = 0.1) whereas w2 varied from 2.812 mm
(W = 50 mm, a/W = 0.4) to 3.230 mm (W = 130 mm, a/W = 0.3).
Since the variation in w1 and w2 for a particular mix is consider-
able, these values cannot be used directly for design of concrete
structures. The parameters obtained from the inverse analysis have

1Xn
min ðP  Pexp Þ2 ð9Þ
ða1 ;a2 ;b2 Þ n
0

where n is the total number of the observations representing the se-

lected entries of h, i.e. the selected values of P on the experimentally
recorded load-CMOD diagram.

3. Results and discussion

Prismatic notched specimens made up of normal strength con-

crete (NSC), high strength concrete (HSC) and ultra high strength
concrete (UHSC) were subjected to three-point bending in accor-
dance with the RILEM procedure [2]. The HSC and UHSC mixes con-
tained steel fibres. Table 1 gives the mechanical properties of the
three mixes, together with the size-independent specific fracture Fig. 6. Bilinear tension softening diagram.
 A. Ramachandra Murthy et al. / Construction and Building Materials 47 (2013) 1160–1166 1165

Table 5
Elastic properties and parameters of the bilinear softening diagram corresponding to the size-independent specific fracture energy GF.

Mix fc (MPa) ft (MPa) E (GPa) a1 (mm1) a2 (mm1) b2 w1 (mm) w2 (mm) r1 (MPa) GF (N/m)
NSC 57.1 2.60 35.8 5.495 2.295 0.727 0.085 0.317 1.382 184.5
HSC 87.7 10.01 37.9 0.989 0.134 0.404 0.697 3.018 3.113 6194.7
UHSC 122.5 13.455 43.0 0.640 0.144 0.546 0.915 3.786 5.566 13760.7

12
16
3
10 14

Tensile stress, MPa

2.5

Tensile stress, MPa

12
Tensile stress, MPa

8
2 10
6
1.5 8

4 6
1
4
0.5 2
2

0 0 0
0 0.1 0.2 0.3 0.4 0 1 2 3 4 0 1 2 3 4
Crack width, mm Crack width, mm Crack width, mm
(a) NSC (b) HSC (c) UHSC
Fig. 7. Bilinear stress-crack opening relationship for NSC, HSC and UHSC corresponding to their GF.

   
to be scaled following the procedure of Abdalla and Karihaloo [10] 1 r1 1 r GF
ft w1 þ w2 ¼ ft w1 þ 1 w2 ð12Þ
so that they correspond to the true GF of the concrete mix that is 2 ft 2 ft Gf ða; WÞ
independent of the shape and size of the test specimen.
The coordinates of the knee of the bilinear diagram predicted by
the hinge model are related as follows (Fig. 6)
3.1. Parameters of bilinear TSD corresponding to GF
r1
The procedure to obtain the size-independent specific fracture ¼ 1  a1 w1 ð13Þ
ft
energy GF for a concrete mix from the size-dependent Gf(a, W)
measured in the laboratory can be found in the literature From Fig. 6 we obtain an additional equation for the slope a2 of
[18–20]. The area under the softening curve (Fig. 6) obtained using the true bilinear diagram
the hinge model is not equal to GF but to the measured Gf(a, W), r1
(see Tables 2–4). It can be observed that the area under the bilinear ¼ ðw2  w1 Þa2 ð14Þ
ft
TSD is generally less than the true GF. Thus, whilst the true GF of the
NSC, HSC and UHSC are 184.5 N/m, 6194.7 N/m and 13760.7 N/m By using the Eqs. (12)–(14), the parameters w1 and w2 can be
respectively (Table 1) the average area under the bilinear TSD is determined.
only 109.7 N/m (Table 2) for the case of NSC, 3770.1 N/m (Table 3) It is assumed that the slope a2 of the tail part of the bilinear dia-
for HSC and 7929.5 N/m for UHSC (Table 4). gram is not sensitive to a and W. The parameters of the bilinear
The size-dependent fracture energy (i.e. the area under the TSD corresponding to GF values of three concrete mixes used in this
bilinear TSD) is given by study are given in Table 5. The TSDs are plotted in Fig. 7.
 
1  r
Gf ða; WÞ ¼ ft w1 þ 1 w2 ð10Þ 4. Conclusions
2 ft
where the superscript  denotes the average parameters of the For the analysis of cracked concrete structures using the non-
bilinear diagram obtained from the hinge model (Tables 2–4). linear theory of fracture mechanics based on the fictitious crack
The size-independent specific fracture energy (i.e. the area un- model, two fracture properties of concrete are needed, namely,
der the bilinear TSD corresponding to GF) can be similarly written the specific fracture energy GF and the corresponding tension soft-
as ening relationship r(w). In this paper, it has been shown how the
1 r1 parameters of a bilinear approximation of the tension softening
GF ¼ ft ðw1 þ w2 Þ ð11Þ relation r(w) corresponding to the recorded load-CMOD diagrams
2 ft
of the TPB specimens can be inferred through an inverse analysis
where w1, w2 and r1, which are to be determined, are the bilinear based on the concept of a non-linear hinge. The procedure has been
diagram parameters corresponding to the true fracture energy GF, demonstrated on normal strength, high strength and ultra high
and ft is the direct tensile strength of the mix obtained from an strength concrete mixes for which the size-independent specific
independent test, say a split cylinder test, fst. It is assumed that fracture energy GF was previously determined [3]. It is shown that
ft = 0.65 fst [21] the parameters of the bilinear diagram vary with the shape and
The hinge model parameters corresponding to Gf (a, W) can be size of the test specimen just as the specific fracture energy
scaled to the size independent specific fracture energy GF as Gf(r, W) measured using the RILEM work-of-fracture method.
1166 A. Ramachandra Murthy et al. / Construction and Building Materials 47 (2013) 1160–1166
However, when these parameters are appropriately scaled using
the procedure proposed by Abdalla and Karihaloo [10] so that they
correspond to the size-independent GF of the concrete mix, then
these parameters are also independent of the specimen size and
shape. The size-independent GF and the bilinear softening diagram
corresponding to it can be used in the fracture analysis of struc-
tures made from the respective concrete mix using the fictitious
crack model [1].
Acknowledgements
The first author’s visit to Cardiff University is funded by Raman
Research Fellowship awarded to him by CSIR, India. He acknowl-
edges with thanks the valuable technical suggestions and support
provided by his colleagues, Dr. G.S. Palani, Mr. S. Maheshwaran,
Ms. Smitha Gopinath, V. Ramesh Kumar, and B. Bhuvaneswari,
and by the staff of Advanced Materials Laboratory, CSIR-SERC dur-
ing the course of the experimental investigation. His contribution
to this paper is being published with the permission of the Direc-
tor, CSIR-SERC, Chennai, India.
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