Journal of Alloys and Compounds 677 (2016) 121e126

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Journal of Alloys and Compounds

journal homepage: http://www.elsevier.com/locate/jalcom

Experimental and theoretical modelling of Vickers, Knoop

microhardness and laser damage threshold studies on
Ca0.9Nd0.1Ti0.9Al0.1O3 single crystals grown by optical floating zone
technique
G. Murugesan*, S. Kalainathan
Centre for Crystal Growth, School of Advanced Sciences, VIT University, Vellore 632 014, Tamil Nadu, India

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

Article history: Vickers and Knoop microhardness studies were done on the (200) face of Ca0.9Nd0.1Ti0.9Al0.1O3 crystals
Received 3 February 2016 grown by optical floating zone technique for various loads ranging from to 0.24e9.8 N. Various important
Received in revised form mechanical properties such as Vickers hardness, Knoop hardness, Young's (elastic) modulus, yield
20 March 2016
strength, stiffness constant which accounts for various industrial applications were determined. The
Accepted 23 March 2016
Indentation Size Effect (ISE) were observed for the grown crystal, four different models such as Meyer's
law, Hays-Kendall (HK) model, proportional sample resistance (PSR) model, elastic/plastic deformation
model (EPD) were used to determine the true hardness values. Among these four mechanical analysis
Keywords:
Oxide materials
models, HK approach seemed to be the best model to describe the mechanical properties of the grown
Rare earth alloys and compounds crystal. The variation of microhardness number for different orientations showed the presence of
Crystal growth microhardness anisotropy in the grown crystal. Laser damage threshold for the grown crystal was found
Mechanical properties to be 2.49 GWm
2.
© 2016 Elsevier B.V. All rights reserved.

1. Introduction strength, Stiffness constant and laser damage threshold, various

CaTiO3, a perovskite material plays a vital role in various ap-
plications due to its intrinsic properties. It has been used as a
synthetic rock (SYNROC) to store nuclear waste actinide materials,
as resonators and filters in microwave dielectric applications and a
host for rare earth ions (Nd3þ, Pr3þ) which can produce efficient
luminescence [1]. Single crystals doped with Nd shows strongest
laser transition from 4F3/2 to 4I11/2 which makes it suitable for
various applications in the field of laser science [1]. CaTiO3 is a
perfect host material for Nd3þ due to similar ionic radii of Ca2þ and
Nd3þ. The desired combination of optical, thermal and mechanical
properties of the host material plays a vital role in its application in
the field of laser technology. The optical, spectroscopic and laser
properties of laser materials are due to the dopant ions, whereas
the physical properties like thermal and mechanical properties are
highly influenced by host material. In order to elucidate the various
mechanical properties like hardness number, Elastic modulus, Yield
* Corresponding author.
E-mail address: gmurux@gmail.com (G. Murugesan).
measurements like Vickers, Knoop microhardness and laser dam-
age threshold measurements were taken. Earlier V. Gupta et al.
have shown the variation of Vickers hardness for various loads for
CaTiO3 single crystals grown by flux technique, where they have
done measurements for an applied load range from 0.098 to 0.98 N
[2].
Generally load dependence of hardness values vary with
different materials and experiments, so far four types of hardness
variation with applied loads are being reported (i) hardness value is
constant for various applied loads (load independent), (ii) variation
of hardness value with load maxima and minima, (iii) hardness
value decreases for load and becomes constant (indentation size
effect, ISE), (iv) hardness value increases for load and saturates for
higher loads (Reverse ISE) [3]. Theoretical approaches using
different models like Meyer's law, Hays-Kendall approach, pro-
portional sample resistance model (PSR) and elastic/plastic defor-
mation model (EPD) were used to estimate the microhardness
measurement results.
To our knowledge there are no reports on the mechanical
properties of Ca0.9Nd0.1Ti0.9Al0.1O3 (CNTAO) single crystals grown
by optical floating zone technique, this motivated us to perform the

http://dx.doi.org/10.1016/j.jallcom.2016.03.178
0925-8388/© 2016 Elsevier B.V. All rights reserved.
122 G. Murugesan, S. Kalainathan / Journal of Alloys and Compounds 677 (2016) 121e126
microhardness studies on the grown crystals inorder to elucidate
its mechanical properties since it plays a vital role in proving the
host material to be mechanically stable. CNTAO can also be used as
a SYNROC for nuclear waste storage and mechanical studies for
SYNROC plays a vital role in determining its real importance inorder
to carry out risk analysis studies concerned in preparing, trans-
porting and storing nuclear waste [4]. CNTAO is also a potential
candidate for dielectric resonator and filters in microwave dielec-
tric applications where their mechanical studies play an important
role in device fabrications. We also intended to use different models
to predict the “true hardness” values for the grown CNTAO crystal.
2. Experimental details
Single crystals of CNTAO were grown by optical floating zone
technique in argon atmosphere [1]. The single phase of the com-
pound was determined by powder XRD and Rietveld refinement
was performed on the powder XRD pattern to an orthorhombic
structure with Pbnm (#62) space group and lattice parameters
a ¼ 5.3832 (1) Å, b ¼ 5.4343 (1) Å, c ¼ 7.6389 (2) Å, V ¼ 223.4677 Å3
and Z ¼ 4 [5]. The dielectric properties of the grown crystals
showed two kinds of relaxations at 436 K and 520 K corresponding
to relaxor behaviour due to Maxwell-Wagner relaxations and
conduction relaxation associated with doubly ionized oxygen va-
cancies respectively [6]. The mechanical properties of the grown
crystals were analyzed through Vickers and Knoop microhardness
tests. The grown crystal was in cylindrical shape which was cut in
the form of circular discs. The orientation of the grown crystals was
determined by XRD technique which was found to be (200) [1]. The
polished surface (200) was mounted on the base of the microscope.
The selected phase was intended with varying loads for a dwell
period of 10 s. Both Vickers and Knoop intender were attached to
the incident ray microscope (Muutoyo MH 112, Japan). Approxi-
mate square shaped Vickers indentation impressions were
observed, with the help of a calibrated micrometer (which is
attached to the eyepiece of the microscope) the length of the two
diagonals was measured. The loads were applied from 0.24 to 9.8 N,
around five indentations were made for each load and the average
d was calculated. Vickers Hardness number (Hv) was found by using
the standard formula,
P modification of Kick's law [2].
Hv ¼ 1:8544
d2
Were P is the load applied in Newton and d is the length of the
diagonal in micrometer. Knoop indentations were in rhombohedral
shape, the long diagonal length (d) was used to calculate Knoop
hardness number (Hk) using the following relation,
P
Hk ¼ 14:229 2
d
where P is the load applied in Newton and d is the length of the
long diagonal in micrometer.
3. Results and discussion
The indentation diagonal length, d for the (200) CNTAO crystal
increased non-linearly for increasing load as shown in Fig. 1 (a). The
indentation depth (h) was calculated using the d value [7]. The non-
linear behaviour is due to the penetration effect, for smaller loads
indenter penetrates only the surface layers which are nearer to the
surface under indentation resulting in stress over a small volume
[7]. The indentation size of Vickers and Knoop indentation
increased for various applied loads from 0.24 to 9.8 N.
The variation Hv for various loads is shown in Fig. 1 (b), the value
of Hv decreases non-linearly from 26.14 to 15.50 GNm
2 for various
loads ranging from 0.24 to 9.8 N. The error bars are plotted using
standard deviation method. A similar kind of behaviour is observed
in CaTiO3 and NiTiO3 single crystals grown by flux technique, where
the behaviour is modelled using Hays-Kendall approach [2]. The
microhardness values decreases nonlinearly and at higher loads it
saturates, this kind of nonlinear behaviour is due to the Indentation
Size Effect (ISE) which explains the decrease of hardness values
with increasing loads [3,8]. Various models like Hays-Kendall
approach, Proportional specimen resistance (PSR) model and
Elastic/Plastic Deformation (EPD) model have been proposed to
analyze the ISE behaviour [9e16]. In this report we have used all the
above three models to predict the reason behind ISE behaviour and
to find out the suitable model to determine the true hardness of the
material.
The ISE behaviour is explained by a simple model which relates
the applied load (P) and the indentation size (d) by the following
equation,
P ¼ K1dn (3)
n is the measurement of ISE behaviour which is the Meyer index
and K1 is the standard hardness constant. If the value of n > 2 the
material exhibits reverse ISE behaviour, whereas if the value of
n < 2 the material exhibits ISE behaviour [8].
The value of ‘n’ is calculated from the plot against log P and log
d (Fig. 2 (a)), which gives a straight line. The slope of the line after
least-square fitting yielded the value of n to 1.74 proving that the
material exhibits ISE behaviour.
The non-linear variation of microhardness with load for CNTAO
crystal can be explained qualitatively on the basis of penetration
depth of the intender [2,17]. For smaller loads the intender pene-
trates layers which are nearer to the surface under indentation
resulting in stress over a small volume. As the depth of penetration
increases the effect on layers which are away from the exposed
surface becomes larger resulting in stress over a large volume.
Variation of hardness constant value for various loads were also
explained by Brookes et al., where he explained the increases of
hardness constant value for low loads at early stages of plastic
deformation [18]. The decrease of hardness constant value for
various loads is better explained by Hays Kendall's law which is a
(1)
The law proposes that applied load is being affected by some
small resistance pressure W which is offered by the material under
investigation. The Hays and Kendall's law (modification of Kicks
law) is given below [2],
P
W ¼ K2d2 (4)
(2) K2 hardness constant independent of applied load and W is the
sample resistance pressure which represents the minimum load
required to cause an indentation [2]. The values of W and K2 are
obtained by plotting P vs d2. The slope of the plot yields the value of
K2 and the vertical intercept gives the value of W.
Fig. 2 (b) shows the plot between P vs d2 which is being linearly
fitted using least-square fitting. The calculated value of W and K2
was 0.114 N and 8.25 GNm
2 respectively. The load-independent
value of Hv is calculated by the application of Hays and Kendall's
law using the following formula [8],
HHK ¼ 1:8544K2 (5)
The load independent hardness value using Hays and Kendall's
approach was found to be 15.29 GNm
2. The plot between log (P-
W) vs log d shown in Fig. 2 (a) yields the value of n ¼ 2 proving the
 G. Murugesan, S. Kalainathan / Journal of Alloys and Compounds 677 (2016) 121e126 123

Fig. 1. (a). Variation of indentation length (d) and indentation depth (h) for various applied loads. (b) Variation of Vickers hardness value for various applied loads. Inset shows as
grown CNTAO crystal and polished CNTAO disc.

Fig. 2. (a) Variation of applied load (log P) & Newtonian resultant pressure (log P-W) with diagonal length (log d) for CNTAO crystal, (b) variation of applied (P) with square of
diagonal length.

validity of Hays and Kendall's law which involves the concept of gives the value of C2 which was found to be 7.638 GNm
2. Using
resistance pressure (W) offered by the material. this value the load independent hardness value is calculated by the
An alternate model to address the ISE behaviour is the propor- following formula [8],
tional specimen resistance (PSR) model. The PSR model is described
by the following relation [8], HEPD ¼ 1.8544*C2 (9)

P The calculated load independent hardness value using EPD

¼ a1 þ a2 d
d
Where a1 is the surface energy which evolves from the energy
dispersion of the surface cracks, a2 parameter used to calculate load
independent microhardness. The values of a1 and a2 are deter-
mined from the least square fitting of the straight line from the P/
d vs d graph as shown in Fig. 3 (a). The value of load independent
microhardness is determined by the following equation [8],
HPSR ¼ 1:8544a2
The calculated values of a2 and HPSR were 7.55 GNm and
14 GNm
2.
Further Elastic/plastic model was used to describe the ISE
behaviour, the dependence of indentation size on the applied load
is given by the equation [8].
P ¼ C2 (de þ d)2
Where C2 is the load independent hardness constant, de is the
elastic deformation. The least square fitting of P1/2 vs d (Fig. 3 (a))
(6) model is found to be 14.16 GNm
2. Table 1 gives the comparison of
load independent hardness values predicted from the Hays-
Kendall, PSR and EPD models. The load independent hardness
values depicted from PSR and EPD model seems to be far away from
the intrinsic value showing its inconsistency in explaining the ISE
behaviour. The hardness values calculated using Hays-Kendall
approach seems to match well with the hardness value in the
plateau region proving that this approach is suitable to calculate the
load independent hardness values for CNTAO crystal.
(7) The yield strength (sy) of the (200) plane for CNTAO crystals for

2 various loads ranging from 0.24 to 9.8 N are determine by the
relation [2]. The yield strength for various loads were varying from
8.75 to 5.16 GNm
2, the variation of yield strength for various loads
is shown in Fig. 3 (b). The average values of yield strength for
CNTAO crystal are calculated to be 6.11 GNm
2. The load inde-
pendent yield strength values using all three models are being
(8) tabulated in Table 1. The Youngs modulus is calculated using
Vickers hardness number [8]. The calculated Youngs modulus was
1501.31G Pa, the load independent Youngs modulus is given in
Table 1.
124 G. Murugesan, S. Kalainathan / Journal of Alloys and Compounds 677 (2016) 121e126

Fig. 3. (a) Variation of applied load/diagonal length (P/d) & square root of applied load (P)1/2 with diagonal length (d), (b) Variation of yield strength and stiffness constant (inset)
with applied loads for CNTAO crystal.

Table 1
Load independent mechanical parameters obtained from various theoretical models.

Parameters (Hays-Kendall approach) (PSR Model) (EPD Model) Plateau region

Load independent Vickers hardness value (Hv) 15.29 GNm
2 14 GNm
2 14.16 GNm
2 15.77e15.5 GNm
2
Load independent Knoop hardness value (HK) 15.08 GNm
2 13.75 GNm
2 13.95 GNm
2 15.87e15.3 GNm
2
Elastic modulus (E0) 1253.22 GPa 1147.48 GPa 1160.60 GPa 1292.56e1270.43 GPa
Yield strength (sy0) 5.096 GNm
2 4.666 GNm
2 4.72 GNm
2 5.256e5.166 GNm
2
Stiffness constant 6.6483  1017 Pa 5.6980  1017 Pa 5.8124  1017 Pa 7.01e6.80  1017 Pa

The stiffness constant is determined using Wooster's empirical

formula [19]. The variation of stiffness constant for different loads is
shown as inset in Fig. 3 (b). Higher values of stiffness constant show
that the binding force between the atoms are stronger.
The Knoop hardness (Hk) is plotted against the applied load
which is shown in Fig. 4 (a). The Knoop hardness number decreases
as the load increases similar to Vickers microhardness. In a similar
way the ISE behaviour is analyzed by the three models (Hays-
Kendall, PSR and EPD models).
Using the Meyer's law in Equation (1) the Meyer index was
calculated from the plot between log d vs log P (Fig. 4 (b)), the
calculated Meyer index (n) is found to be 1.74. Generally the value
of n should be equal to 2 on application of Kicks law, but for us it
was <2.
The reason is due to the non-linear variation of hardness values
for applied loads which is due to the ISE behaviour. We applied the
Hays-Kendall approach to depict the load independent hardness
value using the following formula [3],
Hk ¼ 14:229K2 (10)
Where K2 is the constant independent of the applied load, the
least square fitting of plot P vs d2 (shown in Fig. 5 (a)) give the
values of K2 and W. The determined values of W and K2 were
0.1414 N and 1.06 GNm
2 respectively. The load independent
hardness value is determined using Equation (10) and it was found
to be 15.08 GNm
2, this value lies closer to the hardness values in
the load independent region (plateau region in Fig. 4 (a)) proving
the consistency of Hays-Kendall approach.
The least square fit of plot between log (P
W) vs log d (shown in
Fig. 4 (b)) gave the value of n to be 2.09 (nearly equal to 2) proving
that Hays-Kendall approach is applicable and gives better results.
The formula to calculate load independent hardness value using
PSR model is given below [3],
HPSR ¼ 14.229*a2 (11)

Fig. 4. (a) Variation of Knoop hardness values (HK) for different applied loads, inset shows the microhardness anisotropic behaviour of CNTAO crystal, (b) variation of applied load
(log P) & Newtonian resultant pressure (log P-W) with diagonal length (log d) for CNTAO crystal.
 G. Murugesan, S. Kalainathan / Journal of Alloys and Compounds 677 (2016) 121e126 125

Fig. 5. (a) Variation of applied (P) with square of diagonal length, (b) Variation of applied load/diagonal length (P/d) & square root of applied load (P)1/2 with diagonal length (d).

Where a2 load independent constant which is determined from

the plot shown in Fig. 5 (b). The slope of the plot yielded the value Table 2
Comparison of various Laser damage threshold values for various laser host
of a2 to be 0.967 GNm
2, using this value the load independent materials.
hardness constant was found to be 13.75 GNm
2.
Later on EPD model was used to determine the load indepen- S.no Material Damage threshold (GW/cm2) Ref

dent hardness value by the following formula [3], 1. Nd:YAG 0.8e5.3 [22]
2. Nd:YAlO3 1.1e2.6 [22]
3. Nd:CaWO4 1.0e3.0 [22]
HEPD ¼ 14.229*C2 (12)
4. Nd:BeL 1.3 [22]
5. CNTAO 2.49 Present work
From the least square fitting of the plot between P1/2 vs
d (shown in Fig. 5 (b)) gave the value of C2. The calculated value of
load independent hardness value using EPD model was found to be
damage threshold values for various Nd laser materials measured
13.95 GNm
2.
using a 10-ns Q-switch laser system operated at 1.06 mm range are
The crystal anisotropy was studied over the range from 0 to
tabulated in Table 2 for comparison. It shows that CNTAO has a
360 in 30 steps. The inset in Fig. 4 (a) shows the nonlinear vari-
better laser damage threshold value which proves its potential
ation of Knoop microhardness with the indentation direction
application as host for Nd in laser applications.
revealing the existence of hardness anisotropy in the grown crystal.
The variation in the observed hardness values with loads is due to
4. Conclusion
the crystal structure, slip systems and the crystal orientation pre-
sent in the grown crystal. High resolved shear stress yields larger
The mechanical properties of CNTAO grown single crystal by
indentation impressions which directly give high hardness values
optical floating zone technique were analyzed. Using the experi-
and low shear stress gives low hardness values. The yield stress for
mental results the Vickers, Knoop hardness, Young's modulus, yield
perfectly oriented slip plane will be low, thus the orientation of slip
strength, stiffness constant were calculated which can be accoun-
systems plays a main role in the directional variation of hardness
ted for potential industrial applications of laser host materials. The
values [20,21].
hardness values decreases at lower loads exhibiting ISE behaviour.
We have already shown CNTAO to be a perfect laser host crystal
Various models were used to determine the true hardness (load
used for diode laser-pumped solid-state lasers [1]. Various prop-
independent hardness) values, among that Hays-Kendall approach
erties like high absorption coefficient, high laser damage threshold
seems to be the best model to determine load independent hard-
value, optical and mechanical properties makes a crystal suitable
ness values and other mechanical properties. Laser damage
for high power and stable diode pumped solid-state lasers. In order
threshold was found to be 2.49 GW/cm2 which was nearly equal to
to determine the laser induced damage threshold for CNTAO crystal
various other laser host materials proving it to be a better host for
laser damage threshold studies were done using a Q-switched
laser material.
Nd:YAG laser operating in (TEM00) mode of l ¼ 1064 nm with
pulse duration of 10 ns and repetition rate of 10 Hz. The diameter of
the laser beam was 0.8 mm. The crystal was placed at the focus of Acknowledgements
the convex lens with a focal length of 30 cm. With the help of power
meter the laser energy density for damage was recorded. The sur- GM thanks Dr. R. Nithya, MSG, IGCAR for helping to grow CNTAO
face laser damage threshold for the crystal was calculated by the crystals. This work has been carried out at UGC-DAE Consortium for
following formula, Scientific Research, Kalpakkam Node, Kokilamedu.

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