Evaluation of fracture toughness of ceramic inserts

by indentation techniques

I.A. Choudhury*, M. Azuddin, and C.H. Tee
Department of Engineering Design and Manufacture, University of Malaya, Malaysia
imtiaz@um.edu.my


Abstract
The fracture toughness, hardness and mode of crack of Al
2
O
3
- TiC, Al
2
O
3
- SiC
w
, and Si
3
N
4
ceramic
inserts have been evaluated by using Vickers indentation method at room temperature. Al
2
O
3
- TiC inserts were
taken from three different manufacturers while Al
2
O
3
- SiC
w
, and Si
3
N
4
ceramics were from a single
manufacturer. Five indentation loads ranging from 98 N 490 N were applied to each specimen mirror polished
prior to indentation.
Results show that hardness does not vary significantly with the indentation load. Three alumina ceramic inserts
from three manufacturers exhibited different hardness and toughness. Hardness of silicon nitride ceramic insert
was the lowest among all the ceramic inserts tested. The toughness of silicon nitride appeared to be the highest.
With regard to the mode of crack, alumina ceramic did not show Palmqvist type at all. All the cracks were of
median type irrespective of load. Silicon nitride on the other hand marginally exhibited median type at higher
load. However, at the lowest load, crack mode was Palmqvist type.

Keywords: Ceramic, Fracture toughness, Vickers indentation, Machining.

1. INTRODUCTION
Fracture toughness is the ability of a material to
resist the growth of a pre-existing crack or flaw. This
is one of the most important mechanical properties of
a brittle material like ceramic. The fracture toughness
of material is characterized by the energy per unit area
which is required to create new crack surfaces, and
thereby propagate a crack through the material. This
value is known is the critical intensity factor (K
IC
) and
is determined at the time of crack extension. However,
determination of this value is often a complicated
process that involves preparation of specimens with
well defined sharp cracks of known length [1]. The
accuracy and repeatability of this method is
questionable as its validity as a fracture toughness. It
can be sensitive to the surface preparation technique
and to the residual stress near the surface.

The indentation method as opposed to the
conventional ways (single-edge notched beam or
chevron notched beam or double cantilever beam) is
considered to be simpler to determine K
IC
for brittle
materials [2-5]. This technique requires only a small
polished area on the specimen surface from which a
large number of data points can be generated rapidly.
The Vickers indentation method is well known.
Surface crack associated with Vickers indentation are
now widely used to determine facture toughness of
ceramics and cermets. Cracks associated with Vickers
indentation impression are widely used as artificial
defects of known size for the fracture toughness
measurement of ceramics. Quantitative relations
between surface crack length due to indentations and
the fracture toughness have been reported in many
literatures [6-9]. Certain assumptions in these analyses
about crack and deformation zone geometry may not
be applicable for a given material. Crack profiles
induced by indentation are of two types: (i)
median/radial type and (ii) Palmqvist type.
In the median type, fracture toughness of a material is
given by
3
2
c
P
K
IC

= , where is a constant to be
determined for any given indentation/specimen
system, c is the crack radius, and P is the indentation
load [10]. In the Palmqvist type crack, the average
length of the crack, l, emanating from the corners of
Vickers indentation test might be a measure of the
relative toughness at low loads. Some researches have
distinguished Palmqvist crack from median crack by
using different ratios of
a
c
or
a
l

= 1
a
c
.
According to them, the crack profile is median if
5 . 2
a
c
and it is Palmqvist type if 5 . 3
a
c
. A
simple way to differentiate between them is to polish
away the surface layers. The median crack will remain
connected to the corner of the diagonal while the
Palmqvist crack will become detached as shown in
Figure 1. Indentation fracture theory concerns two
basic types of contacts: (i) sharp indenters and (ii)
blunt indenters. In sharp indenters, the contact is
essentially plastic up until fracture while in blunt
indenters; the contact is all elastic up to the point of
fracture [11]. In this paper, sharp indenter has been
used to ascertain the relationship of the fracture data to
the ratio
a
c
of different ceramic inserts used for metal
cutting applications.

- 175 -
Proceedings of the 1st International Conference & 7th AUN/SEED-Net
Fieldwise Seminar on Manufacturing and Material Processing



2. EXPERIMENT PROCEDURE
2.1 Test Materials
The materials used in the investigation are the
ceramic inserts used in metal cutting. Three different
types of ceramic inserts were selected. Al
2
O
3
TiC
ceramic inserts were taken from three different
manufacturers and these are categorized as alumina-I,
alumina-II and alumina-III ceramic. The actual coding
given by the manufacturers are not revealed in order to
hide the identity of manufacturers. The other two
types were Al
2
O
3
SiC whisker



and Si
3
N
4
ceramics. Figure 2 shows all inserts and
Table 1 shows their code and dimensions. All
indentations were made into mirror polished surfaces.
The surface of each insert was polished successively
with 9, 6, and 3 m diamond suspensions to obtain
mirror surfaces appropriate for indentation.

Table 1 Code and dimensions of ceramic inserts
Insert Code Dimensions
Alumina-I
(Al
2
O
3
TiC)
DNGA 255 14 5 mm
Alumina-II
(Al
2
O
3
TiC)
DNGA 255 14 5 mm
Alumina-III
(Al
2
O
3
TiC)
DNGN 255 14 5 mm
Alumina
whisker
(Al
2
O
3
- SiC
w
)
DNGA 255 14 8 mm
Silicon nitride
(Si
3
N
4
)
DNGA 255 14 8 mm


2.2 Indentation Tests
Vickers microhardness pyramid shaped sharp
diamond indenter with the angle between the opposite
faces at the vertex of 136
0
was used to apply four
indentation loads of 98 N, 196N, 294 N, and 490 N on
the polished surface of each insert. A minimum
number of fourteen indentations were made at each
load on each surface. The load was applied with a
dwell time of 15 seconds. Vickers crack produced as a
result of the applied load have been observed and
measured in a high magnification Nikon optical
microscope. The main cracks emanating from the four
corners were measured and then the total main crack
length was divided by 4. The samples producing well-
defined cracks were only considered in all
calculations. The length (2a) of the diagonal shown in
Figure 1 is used to calculate Vickers hardness from
the following equation:
( )
2
2
854 . 1
a
P
HV

= (1)

where, P is the applied load in kg
f
and 2a is the length
of the diagonal in mm. Fracture toughness was
calculated from the following equation [10].
( )

5 . 1
5 . 0
203 . 0

=
a
c
HVa
K
Ic
(2)

where, HV is Vickers hardness, a is half-diagonal
length in mm, c is crack length from the centre of
indentation in mm, and is a constraint factor ( 3).

- 176 -
I.A. Choudhury, M. Azuddin, and C.H. Tee, Evaluation of fracture
toughness of ceramic inserts by indentation techniques, 175-180


3. RESULT AND DISCUSSION
3.1 Crack System Mode
Vickers indenter produces at least two types of
cracks, (i) median crack and a (ii) Palmqvist crack.
Usually low toughness material exhibits median crack
system while high toughness material shows
Palmqvist crack. However, most material exhibits
both median and Palmqvist crack under different load.
The median crack system will remain connected to the
corner of the indent while the Palmqvist crack system
will be detached from the indent. Figure 3 (a) (d)
shows the surface morphology of cracks at a
minimum load



of 98 N and Figure 4 (a) (d) shows the surface
morphology of cracks at a maximum load of 490 N for
five different insert samples. The crack systems
appear to be of median type irrespective of the applied
load. In some samples, however, ill-defined cracks
were observed at higher loads and these can be seen in
Figure 5 (a) (d).

3.2 Indentation Load, Fracture Toughness and
Vickers Hardness
Harness and fracture toughness may vary with
the indentation load as these affect the indent size and
crack length, which depend on sample dimension and
microstructure.



- 177 -
Proceedings of the 1st International Conference & 7th AUN/SEED-Net
Fieldwise Seminar on Manufacturing and Material Processing


Hence the selection of Vickers indentation load
is critical to measure the hardness and fracture
toughness of materials. Figure 6 shows variation of
hardness with indentation loads for different ceramic
inserts. The hardness of Al
2
O
3
TiC ceramic inserts
from three suppliers vary within 19 to 23 GPa when
the indented load is 98 N. At 490 N indentation load,
the variation reduces to 19 21 GPa. Si
3
N
4
ceramic
insert exhibited minimum hardness among all the
inserts which is about 16 GPa. The toughness of
ceramic inserts is presented in Figure 7 at various
loads. Si
3
N
4
ceramic insert has the maximum
toughness compared to alumina ceramics. At low
load, Al
2
O
3
TiC ceramic inserts exhibited higher
hardness than at higher load. The micro hardness can
be regarded as the ease degree of plastic flow for
materials. The hardness may be considered as an
indirect measurement of the transformation yield
stress. The relationship between fracture toughness
and hardness exhibits an inverse dependence of K
Ic
on
the hardness. Since the ease degree of yielding can be
regarded as that of transformation, a reverse
relationship between fracture toughness and hardness
can be expected [12].

3.3 Crack Profiles
Figure 8 shows the relation between the
indentation load and crack length to diagonal ratio. All
alumina ceramic exhibited median type of crack
irrespective of indentation load as c/a ratio was higher
than 2.5. With the increase of load, magnitude of c/a
increased and at higher load, crack profile is certainly
of median type. In case of Si
3
N
4
ceramic, crack profile
at the lowest load of 98 N exhibits Palmqvist type
while at higher load, it may be marginally in the
transition zone. In Figures 9 (a) and (b) the crack
length, c, as a function of indentation load PP
2/3
for
alumina-II and alumina whisker respectively are
plotted to see how the plot fits to satisfy the median
crack system. The median cracks c, follow a 2/3
power dependence on indentation load. These figures
indicate that the relation between the crack length, c,
and indentation load satisfies the condition
3
2
KP c = for the median crack system, where K is a
function of the Youngs modulus, hardness, and
fracture toughness of the material and the geometry of
the indenter.

4. CONCLUSIONS




- 178 -
I.A. Choudhury, M. Azuddin, and C.H. Tee, Evaluation of fracture
toughness of ceramic inserts by indentation techniques, 175-180




Results and analyses of this study have
revealed that median crack mode is dominant
in Al
2
O
3
ceramics irrespective indentation
load. However for Si
3
N
4
ceramic, crack mode
is marginally median type. At lower load, it is
Palmqvist type.
Hardness does not vary much with indentation
load. Al
2
O
3
ceramic inserts from three different
manufacturers exhibited different hardness
both at lower and higher indentation loads. The
variation however decreases at higher load.
The variation however decreases at higher
load. Si
3
N
4
ceramic has lower hardness than
the alumina ceramics.
At the maximum indentation load of 490 N,
alumina-I ceramic has the minimum fracture
toughness when compared with alumina-II and
alumina-III ceramics. While at the smallest
load of 98 N, alumina-I ceramic has the
highest fracture toughness when compared
with alumina-II and alumina-III ceramics.
Fracture toughness of alumina whisker ceramic
is higher than rest of the alumina ceramics.
Fracture toughness of Si
3
N
4
ceramic is higher
than the alumina ceramics. This is in good
agreement with in situ observations of material
properties. Compared with alumina ceramics,
Si
3
N
4
has lower hardness and better toughness.

REFERENCE
1. P.D. Warren, Determining the Fracture
Toughness of Brittle Materials b Hertzian
Indentation, J. of European Ceramic Society,
15 (1995), 201-207.
2. A.G. Evans and E.A. Charles, Fracture
Toughness Determination by Indentation, J. of
American Ceramic Society, 59 (1976), 371-
372.
3. K. Niihara, R. Morena, and D.P.H. Hasselman
in Fracture Mechanics of Ceramics 5 edited
by R.C. Bradt, A.G. Evans, P.P. Hasselman,
and F.F. Lange (Plenum, New York, 1983),
97-105.
4. B.R. Lawn, A.G. Evans, and D.B. Marshall,
Elastic/Plastic Indentation Damage in
Ceramics: the Median/Radial System, J. of
American Ceramic Society, 63 (1980), 574-
581.
5. G.R. Anstis, P. Chantiku., B.R. Lawn, and
D.B. Marshall, A Critical Evaluation of
Indentation Techniques for Measuring
Fracture Toughness, J. of American Ceramic
Society, 64 (1981), 533-538.
6. K. Niihara, R. Morena, and D.P.H.
Hasselman, Evaluation of K
Ic
of Brittle Solids
by the Indentation Method with Low Crack-
to-Indent Ratios, J. of Material Science, 1
(1982), 13-16.
7. M.T. Laugier, Palmquist Indentation Crack
Analyses for Toughness Determination in
WC-Co Composites, J. of Key Engineering
Materials, 32 (1989), 77-84.
- 179 -
Proceedings of the 1st International Conference & 7th AUN/SEED-Net
Fieldwise Seminar on Manufacturing and Material Processing

8. D.K. Shetty, I.G. Wright, P.N. Mincer and
A.H. Clauer, Indentation Fracture of WC-Co
Cermets, J. of Material Science, 20 (1985),
1873-1882.
9. Z. Li, A. Ghosh, A.S. Kobayashi, and R.C.
Bradt, Indentation Fracture Toughness of
Sintered Silicon Carbide in the Palmqvist
Crack Regime, J. of American Ceramic
Society, 72 (1989), 904-911.
10. K.M. Liang, Evaluation by Indentation of
Fracture Toughness of Ceramic Materials, J.
of Materials Science, 25 (1990), 207-214.
11. Y. Bisrat and S.G. Roberts, Residual Stress
Measurement by Hertzian Indentation, J. of
Material Science and Engineering, A288
(2000), 148-153.
12. J.D. Lin and L.G. Duh, Fracture Toughness
and Hardness of Ceri- and Yttria-doped
Tetragonal Zirconia ceramics, J. of Material
Chemistry and Physics, 78 (
13. 2002), 253-261.
- 180 -