Effect of fatigue on fracture toughness and phase transformation of

Y-TZP ceramics by X-ray diffraction and Raman spectroscopy

Secil Karakoca Nemli,1 Handan Yilmaz,1 Cemal Aydin,1 Bilge Turhan Bal,1 Tulay Tras2
1
2

Department of Prosthodontics, Faculty of Dentistry, Gazi University, Ankara, Turkey

Department of Physics, Faculty of Science, Anadolu University, Eskis
ehir, Turkey

Received 14 April 2011; revised 23 August 2011; accepted 23 August 2011

Published online 21 November 2011 in Wiley Online Library (wileyonlinelibrary.com). DOI: 10.1002/jbm.b.31964
Abstract: The aim of this study was to evaluate the effect of
fatigue on fracture toughness and phase transformation of
yttria-stabilized zirconia polycrystal materials (Cercon and
Lava). The specimens were tested for indentation fracture
toughness either with or without being subjected to fatigue
(20,000 cycles, 2 Hz, 200 N load). X-ray diffraction (XRD) analysis was used to examine the phase composition of specimens. The indentation images were analyzed using Raman
spectroscopy at indentation center (p1), indentation corner
(p2), points on crack 100 lm (p3), and 200 lm (p4) away from
the corner and a point
80 lm away from the crack (p5).
Fracture toughness results were statistically analyzed by twoway analysis of variance (ANOVA); XRD and Raman spectroscopy results were analyzed by three-way ANOVA. Fracture
toughness of Cercon control (CC) and fatigue (CF) groups
were 6.8 and 6.9 MPaHm, respectively, with no signicant
difference (p > 0.01). Fracture toughness of Lava fatigue (LF;

7.3 MPaHm) was signicantly higher than Lava control (LC; p

< 0.01). XRD analyses showed CC and LC consisted of tetragonal zirconia, monoclinic zirconia detected after fatigue. After
indentation, relative amount of monoclinic phase signicantly
increased in CC, CF, and LC; decreased in LF. The Raman
spectroscopy results indicated that monoclinic fraction was
the highest at p2, subsequently at p1 and decreased at p3,
p4, and p5 for all groups. Mechanical cycling increased fracture toughness of Cercon and Lava, the second being signicant. Phase transformation was also detected after fatigue,
which is higher in Lava. Analysis of indentations showed that
transformation was highest was at the corner, second at cenC 2011 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl
ter. V
Biomater 100B: 416424, 2012.

Key Words: Y-TZP, fatigue, indentation fracture toughness,

phase transformation

How to cite this article: Nemli SK, Yilmaz H, Aydin C, Bal BT, Tras
 T. 2012. Effect of fatigue on fracture toughness and phase
transformation of Y-TZP ceramics by X-ray diffraction and Raman spectroscopy. J Biomed Mater Res Part B 2012:100B:416424.

INTRODUCTION

The fracture toughness (KIC) is dened as the mechanical

resistance of a material to crack propagation.1,2 The lower
fracture toughness may indicate the lower clinical reliability
of the ceramic restoration, because the KIC value denes the
critical stress intensity level at which catastrophic failure
occurs due to a critical microdefect.3 Different techniques
and different specimen geometries are currently used to
determine toughness.46 In several studies on dental
ceramics, the fracture toughness was determined using indentation fracture (IF) technique.2,4,68 Using this technique,
an approximate determination of relative fracture toughness
is assessed by introducing aws of controlled size, shape,
and location followed by direct measurement of the radial
cracks.6,9 The application of the IF in studying the behavior
and properties of brittle dental materials is specically
appropriate, because only small specimens sizes are
required, it is simple to apply, and the growth parameter is
similar to those crack expected in clinical conditions.4,6,9
However, this technique may result in high dispersion as a

result of difculties inherent in the accurate measurement

of crack length and subcritical crack growth.6,9,10
The development of dental material technologies has led
to the application of zirconia (ZrO2)-based ceramics in dentistry.11 One remarkable feature of zirconia is transformation toughening, which may explain the increased strength
and fracture toughness compared with other dental
ceramics. Zirconia is a polymorphic material that exists in
three different phases: monoclinic, tetragonal, and cubic. At
room temperature, pure zirconia is monoclinic and
extremely brittle. Alloying with yttria (Y2O3) can keep zirconia in a metastable tetragonal phase, which is called yttriastabilized zirconia polycrystals (Y-TZP). In response to mechanical stresses such as sandblasting, grinding, and impact
the Y-TZP crystals located at the crack tip undergo martensitic transformation to the monoclinic phase, which is
accompanied by an increase in volume of 34%.11,12 The
volume increase generates a compressive stress within the
material, which can slow down the crack propagation and
thus improves its fracture toughness and crack propagation

Correspondence to: S. K. Nemli; e-mail: secilkarakoca@yahoo.com

Contract grant sponsor: Gazi University (Scientic Research Project of the Rectorship); contract grant number: 03/2009-19

416

C 2011 WILEY PERIODICALS, INC.

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ORIGINAL RESEARCH REPORT

resistance. Besides mechanical stresses, tetragonal to monoclinic (tm) phase transformation can also be triggered by
thermal aging, chemical aging, and intermittent forces during mastication in the oral environment.1113 However,
under cyclic loading conditions, susceptibility of Y-TZP to fatigue is still remains unclear.
The stress-induced martensitic phase transformation
and phase compositions can be analyzed using X-ray diffraction analysis (XRD) or Raman spectroscopy. XRD is the most
commonly used method for the quantitative evaluation of
the phase transformation in Y-TZP materials with an advantage of being a nondestructive method.13 However, XRD
tends to be used for large area surface analyzes and no
local information can be obtained. Therefore, XRD measurements characterize the overall sample behavior.13,14 In addition, it has been reported that the information obtained by
XRD is not reliable when transformed fractions are smaller
than 5%.13 For these reasons, the XRD technique can be
considered as the rst step for investigating the surface
characterization of Y-TZP. For the local analysis of tm phase
transformation, Raman spectroscopy is an important tool
because the Raman spectra can be measured with a spatial
resolution down to 1 lm.15 Furthermore, the Raman spectrum of monoclinic ZrO2 is easily distinguished from that of
tetragonal ZrO2 by strong doublet at
185 cm1.16 It has
been widely used to examine phase transformations within
and around the Vickers indentations of Y-TZP- and ZrO2toughened alumina ceramics.14,1722 Raman spectroscopy
has also been used to identify and to map the distribution
of the crystalline phases at the fractured surfaces of Y-TZP
materials.16,17,23
According to the literature research, there is lack of information on the effect of fatigue on fracture toughness of
Y-TZP cores. In addition, the effect of fatigue on phase transformation of Y-TZP surfaces and phase transformation
within and around the Vickers indentation has not been
studied. The aim of this study was to evaluate the fracture
toughness of Y-TZP core ceramics before and after cyclic
loading, to assess the phase changes generated by fatigue
and Vickers indentations on the surface by using XRD and
to examine the effect of fatigue on the phase transformation
within and around the Vickers indentations by Raman
spectroscopy.

MATERIALS AND METHODS

Specimen preparation
Cercon base (Cercon, DeguDent, Hanau, Germany) and Lava
All-Ceramic System (Lava, 3M ESPE, Seefeld, Germany) YTZP core ceramics were investigated in the study. The specimens were provided by the manufacturers. Both Y-TZP
materials were composed of polycrystalline microstructure
and the specimens were milled from a partially sintered
blank in an enlarged size to compensate sintering shrinkage,
which is different for each system as it is about 30% for
Cercon and 2025% for Lava. Sintering temperature of Cercon was 1350 C and Lava was 1500 C. The sintering process led to densities from 99 to 100% of the theoretical

density.24,25 For each material, 20 disk-shaped (15 mm in

diameter and 1 mm in thickness) specimens were provided.
Twenty specimens for each core material were randomly
divided into two groups of 10. Group 1 consists of control
specimens, which were abbreviated as CC and LC for Cercon
and Lava, respectively. Specimens in group 2 were subjected
to fatigue testing under cyclic loading in a mechanical cycling machine (Instron 8801, Instron, Canton, MA) and were
abbreviated as Cercon fatigue (CF) and Lava fatigue (LF) for
Cercon and Lava, respectively. The specimens were placed
on 3 hardened steel supporting balls with diameter of 3.2
mm that were positioned 120 apart on a support circle
with a diameter of 10 mm. The specimens were placed concentrically on the supporting balls. An upper rod with a 1.6
mm diameter tip induced 200 N loads for 20,000 times,
with a frequency of 2 Hz. The cycling was conducted at
room conditions (22 6 1 C and 60 6 5% relative humidity). All measurements were performed on the compression
side of the mechanically cycled specimens.
Fracture toughness determination
The fracture toughness of materials with and without cyclic
loading was determined by IF technique.10 The specimens
were embedded in acrylic resin (Panacryl; Arma Dental, Istanbul, Turkey) cylinders. Disk surfaces were ground on a
grinder-polisher machine (Ecomet3; Buehler, Lake Bluff, IL)
using 30 lm diamond wheels and polished using a ceramic
surface polishing kit (Sof-lex Finishing and Polishing System,
3MESPEAG, Seefeld, Germany). Each polishing wheel was
applied to surfaces of the specimens approximately for 20 s
at a rate of 350 rpm. After surface treatment, all specimens
were ultrasonically (Euronda; Erosonic Energy, Italy)
cleaned in distilled water for 10 min to remove debris. First,
standard Vickers loads of the hardness testing machine
(Vickers; Fritz Heckert, Leipzig, Germany) were evaluated to
determine the optimum load to meet the criteria of acceptable crack pattern on two Y-TZP materials. The criteria for
acceptability were: (1) all cracks emanated from the corner
of the Vickers indent, (2) presence of only four radial cracks
with c/a >2, and (3) no crack chipping and branching.10
The average crack length (c) was obtained from the measurement of the radial cracks (2c) over two orthogonal radial directions. A load of 30 kg was used to generate these
acceptable radial cracks on specimens of CC, CF, LC, and LF
groups. Each specimen was indented at three equidistant
locations such that each was
4.5 mm away from the disk
center, with an angle of 120 between them with a dwell
time of 15 s. Readings were recorded under the microscope
of the indentation machine. Measurements were performed
immediately after each indentation. The fracture toughness
was calculated as described by Anistis et al.10:
K 0:016  E=H1=2  P=c3=2 ;

(1)

where H P/2a2, in which K is the fracture toughness of

the material (MPaHm), E is the elastic modulus, P is the
load applied (N), a is the indent half diagonal (m), and c is
the crack length measured from the center of the indent

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(m). Elastic modulus values were 215 GPa for Cercon and
210 GPa for Lava, which were determined in a previous
study.23
XRD analysis
XRD analysis was used to examine the phase composition of
the control and mechanically cycled specimens before and
after IF toughness testing. The specimens were analyzed by
X-ray diffractometer (Rigaqu-Geirex X-ray difraktometer,
Japan) using Cu-Ka radiation. Scans were performed at 40 kV,
40 mA, 0.018/step, step interval from 20 to 34 2y degrees,
where y is the angle of reection. The relative amount of the
monoclinic phase (Xm) was calculated based on the method
of Garvie and Nicholson,26 which is most commonly applied
to determine the phase composition of zirconia powders and
compacts with randomly distributed m and t phases at any
distance from the surface exposed to XRD analysis:
Xm Im1 Im2 =Im1 Im2 It ;

(2)

where I is the intensity detected by the detector at angular

position 2y degrees from the diffraction, t the tetragonal
peak, m1 and m2 are the two major monoclinic peaks.
Raman spectroscopy
The images of indentations and radial cracks were located
with the optical system of the microscope (20x optical
objective) and analyzed using a Raman spectrometer (Senterra; Bruker Optics GmbH, Ettlingen, Germany) to identify
the distribution of the crystalline phases the indentation
center (p1), indentation corner (p2), two points located on
the crack 100 lm (p3), and 200 lm (p4) away from the
corner and at a point located at
80 lm away from the
crack and indent edge (p5). Figure 1 shows schematic diagram of a Vickers impression and localization of the points
those Raman spectra taken from. The Raman laser, at a
wavelength of 520 nm and 20 mW power at sample, was
focused on these regions. Spectral integration time was 16
s, and the resolution was 3 cm1.
From the net peak height intensities of the monoclinic
(180 and 190 cm1) and tetragonal (147 cm1) ZrO2
phases, the monoclinic fraction (fm) was calculated using
the method of Kim et al.16 First, the Raman intensity monoclinic ratio (Xm) was calculated according to the equation:
Xm

Im 180cm1 Im 190cm1
Im 180cm1 Im 190cm1 It 147cm1

(3)

I is the net peak intensities at the corresponding Raman

shifts and was calculated assuming a sloped linear baseline
crossing the background level.16 The monoclinic fraction
was than obtained from the equation:
fm

r
0:13
0:19 
 0:56
Xm  1:01

(4)

The technique was accurate to detect the monoclinic fraction in the tetragonal-rich (fm < 0.3) two phases zirconia.16
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FIGURE 1. Schematic diagram illustrating the points where Raman

spectra taken from; (1) indentation center (p1), (2) indentation corner
which is
100 lm away from the center (p2), (3) 100 lm away from
the corner on the crack (p3), (4) 200 lm away from the corner on the
crack (p4), (5) 80 lm away from the crack and indent edge (p5).

The minimum monoclinic fraction that can be detected by

this method is about 0.01.21
Statistical analyses
The fracture toughness results were statistically analyzed by
two-way analysis of variance (ANOVA), with Y-TZP types and
being or not subjected to mechanical cycling as the independent variables.
Relative amount of monoclinic phase, which was determined by XRD, was statistically analyzed by three-way
ANOVA with repeated measures on one variable. The independent variables were Y-TZP types, being or not subjected
to mechanical cycling, and data before or after indentation
of the specimen.
The results of monoclinic fraction, which was determined by Raman spectroscopy was statistically analyzed by
three-way ANOVA with repeated measures on one variable.
The independent variables were Y-TZP types, being or not
subjected to mechanical cycling, and the point analyzed
with Raman spectroscopy.
For all statistical analyses, Duncan multiple range test
was used to determine any signicant differences among
the groups with a signicance level of 0.01 (SPSS 18, SPSS,
Chicago, IL).
RESULTS

All Y-TZP specimens were mechanically cycled survived. IF

toughness of control and fatigue group of Cercon were 6.8
and 6.9 MPaHm, respectively, and there was no signicant
difference between groups (p > 0.01). Fracture toughness
of fatigue Lava (7.3 MPaHm) was signicantly higher than
control Lava (6.6 MPaHm; p < 0.01; Table I). Images of the
indentation hardness tests for each group are shown in
Figure 2.
According to the XRD patterns, control group of Cercon
and Lava consisted of tetragonal zirconia (50-1089), and
monoclinic zirconia (37-1484) detected after fatigue testing
of these specimens (Table II). Monoclinic phase was found

FRACTURE TOUGHNESS AND PHASE TRANSFORMATION OF Y-TZP

ORIGINAL RESEARCH REPORT

TABLE I. Comparison of the Mean Fracture Toughness

Values between Control and Fatigue Groups of a Material
Fracture Toughness (MPaHm) (SE)

Control
Fatigue

Cercon

Lava

6.8 (0.10) A
6.9 (0.11) A

6.6 (0.13) b
7.3 (0.1) a

Same characters (vertically) indicate that fracture toughness were

not statistically signicantly different between control and fatigue
groups of the material (p > 0.01).
The bold alphabets in the tables are used to indicate statistical signicances between the values.

at the surfaces of both control and fatigue groups of two

materials after IF toughness test (Table II). In addition, comparison of relative amount of monoclinic phase (%) before
and after IF toughness testing was made within groups (Table
III). In CC, CF, and LC groups, relative amount of monoclinic
phase were signicantly increased after indentation; however,
a signicant decrease was found in LF group (p < 0.01).

Raman spectra obtained from of p1p5 of a specimen

from each group are shown in Figure 3. The Raman spectroscopy results of the fraction of the monoclinic phase are
presented in Table IV. Three-way ANOVA showed no signicant inuence of the Y-TZP type (p > 0.01) and being or not
subjected to mechanical cycling (p > 0.01). Comparing the
monoclinic phase fractions measured at ve points of indentation images, the highest monoclinic fraction was found at
the p2, indentation corner, with a signicant difference. The
indentation corner was located
100 lm away from the
center of the indent. The second highest monoclinic fraction
was at p1. The monoclinic fraction found at p3, p4, and p5
were statistically lower than p1. No signicant difference
was found between monoclinic fraction of p3, p4, and p5.

DISCUSSION

The clinical failure of all-ceramic restorations is often associated with their brittleness and low fracture toughness.7 A
range of fracture toughness values of all-ceramic materials

FIGURE 2. Vickers indentations and cracks of a specimen from (a) Cercon control, (b) Cercon fatigue, (c) Lava control, and (d) Lava fatigue
groups. [Color gure can be viewed in the online issue, which is available at wileyonlinelibrary.com.]

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TABLE II. Comparison of Relative Amount of Monoclinic

Phase (%) Between Control and Fatigue Groups of a Material
before Indentation Fracture Toughness Testing
Relative Amount Monoclinic Phase (%)
Before Indentation (SE)

Control
Fatigue

Cercon

Lava

0 (0) B
0,44 (0.04) A

0 (0) b
2.22 (0.1) a

Same characters (vertically) indicate that relative amount of monoclinic phase were not statistically signicantly different between control and fatigue groups of the material (p > 0.01).
The bold alphabets in the tables are used to indicate statistical signicances between the values.

were reported as 1 to 3 MPaHm for lithium disilicate glass

ceramics,2,3,7,9 35 MPaHm for glass-inltrated alumina
ceramics,7,27 45.5 MPaHm for glass-inltrated zirconia/alumina ceramics.1,11,28,29 Typical fracture toughness values in
the literature range from 6 to 8 MPaHm for Y-TZP.8,11,28,30
In this study, the fracture toughness values for Cercon (6.8
MPaHm) and Lava (6.6 MPaHm) are in agreement with
these results. However, the effect of mechanical cycling on
the fracture toughness of Y-TZP has not been reported in
the literature. The fracture toughness values of fatigue
groups of Cercon (6.9 MPaHm) and Lava (7.3 MPaHm)
materials led to rejection of study hypothesis that cyclic
loading causes a decrease in fracture toughness of Y-TZP
core ceramics.
Aging of Y-TZP can have detrimental effects on its mechanical properties. It has been reported that subcritical
cracks propagate and fuse with the preexisting ssures with
repetitive stresses during chewing cycle, thereby weaken
the material.31,32 Therefore, fatigue tests are very important
in order to evaluate the mechanical performance of ceramic
materials.32 However, studies have focused on the effect of
fatigue on strength,3134 whereas there is no information on
the effect of fatigue on fracture toughness, which is an important mechanical property with its ability to indicate serviceability of a material in the oral cavity. In the previous
studies, a range of different mechanical cycling regimes differing in numbers of cycles and stress limits were used.31
35
Mechanical cycling, which dental restorations, are subjected to during chewing function was simulated with an
upper limit of 200 N and a lower limit of 20 N in the present study. Thus, the results of these studies do not directly
corroborate but complement one another. As physiological
chewing forces were reported to be ranging between 20

and 120 N depending on food consistency,36 the cycling

load used in the present study might be used for the estimation of restorations performance under more severe conditions like bruxism. The mechanical cycling regime of 20,000
cycles applied in this study corresponds to initial in vivo service period with a low specimen fracture risk.21 Kim et al.16
indicated an increased probability of specimen fracture during fatigue loading after 50,000 cycles. Therefore, since the
aim of this study was to evaluate the effect of mechanical cycling on Y-TZP cores without specimen fracture prior to fracture toughness tests, 20,000 cycles was applied.32
Indentation technique used in the present study was
performed by generating precracks propagated from 30 kg
load Vickers indentations on the specimens. This load was
selected by trial and error that was used to produce a c/a ratio  2. Fischer and Marx3 stated that precaution must be
taken in selecting a working range of indentation loads if the
test surface contains residual stresses prior to indentation.
Under cyclic loading, growth and propagation of subcritical
cracks may lead to stress formation on Y-TZP surfaces.31
Therefore, in the present study considering the probable differences of mechanically cycled specimens from control specimens of the same material, determination of optimum load
was performed separately for control and fatigue groups.
The effects of mechanical cyclic fatigue in ceramics have
also been studied using the repeated indentation (indentation fatigue) method.3741 Indentation fatigue is dened as
the gradual damage accumulation in the surface layer
caused by local cyclic compressive loading. In this method,
Vickers preindentations are made with standard loads of
300, 200, and 150 N, expecting that these would produce a
system of lateral cracks of some standard size and depth.
The indentations are then repeatedly indented using different load ranges until chipping occurs.37,41 Indentation fatigue behavior of zirconia ceramics has been studied.37,38
Matsuzawa et al.37 investigated indentation fatigue of four
kinds of zirconia ceramics (3Y-TZP, 6Y-FSZ, Mg-PSZ and CeTZP). They reported that each material showed different indentation fatigue behaviors where 3Y-TZP has highest resistance against chipping. Guiu et al.38 indicated that both zirconia-toughened alumina and tetragonal zirconia were
susceptible to mechanical cyclic fatigue effects. They evaluated fatigue behavior of the materials using three different
(pushpull fatigue, slow crack-growth, and repeated indentation) techniques.
In the present study, Cercon (6.8 MPaHm) showed no
differences in fracture toughness value after 20,000 cycles

TABLE III. Comparison of Relative Amount of Monoclinic Phase (%) Before and After Indentation Fracture Toughness Testing
Within a Group

Relative amount monoclinic phase (%) before indentation

Relative amount monoclinic phase (%) after indentation

Cercon
Control (SE)

Cercon
Fatigue (SE)

Lava
Control (SE)

Lava
Fatigue (SE)

0 (0) B
0.83 (0.07) A

0.44 (0.04) b
0.7 (0.06) a

0 (0) Y
0.7 (0.06) X

2.22 (0.1) x
0.86 (0.04) y

Same characters (vertically) indicate that relative amount of monoclinic phase were not statistically signicantly different within a group
before and after indentation fracture toughness (p > 0.01).
The bold alphabets in the tables are used to indicate statistical signicances between the values.

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FRACTURE TOUGHNESS AND PHASE TRANSFORMATION OF Y-TZP

ORIGINAL RESEARCH REPORT

FIGURE 3. Raman spectra obtained from of p1p5 of a specimen from (a) Cercon control, (b) Cercon fatigue, (c) Lava control, and (d) Lava fatigue groups. [Color gure can be viewed in the online issue, which is available at wileyonlinelibrary.com.]

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TABLE IV. The Mean Values of Monoclinic Phase Fraction

(%) at Each Point Measured

Point
1
2
3
4
5

Number of Specimens/
Number of
Points Measured
40/40
40/40
40/40
40/40
40/40

Mean Monoclinic
Phase Fraction*
B

0.26
0.57 A
0.028 C
0.019 C
0.032 C

SE
0.014
0.02
0.002
0.002
0.004

*Mean monoclinic phase fraction of the points analyzed were not

statistically different (p > 0.01).
The bold alphabets in the tables are used to indicate statistical signicances between the values.

at 200 N (6.9 MPaHm) while fracture toughness of Lava

specimens (6.6 MPaHm) showed signicantly different
increase after cycling (7.3 MPaHm). These differences may
arise from different material formulation and processing
method of Lava and Cercon specimens. It has been reported
that the mechanical properties of Y-TZP depend on the grain
size.29,36,42 The grain size of the core materials used in the
present study has been reported as 0.20.3 lm for Cercon
and 0.1 lm for Lava.43,44 Also, the increase in biaxial exural strength of Lava core-veneer system after fatigue has
been reported in a previous study.23
The tetragonal-to-monoclinic transformation is studied
using XRD and Raman spectroscopy. Comparison of quantitative XRD and Raman analysis of the tetragonal/monoclinic
two phase zirconia were previously reported and the global
behavior has been found similar for two techniques.45 In
this study, these two techniques have not been compared,
because they were used for different purposes. The phase
composition of the surfaces of Y-TZP materials after mechanical cycling and indentation testing was detected by XRD.
Raman spectroscopy has been used to characterize and
identify the phase transformations within and around the
Vickers indentations owing to its ability to perform local
analysis of tm phase transformation.
Temperature and moisture are known as factors that
enhance tm phase transformation of Y-TZP ceramics and
affect their mechanical properties31,36; however, the effect of
cyclic loading on phase transformation of Y-TZP has not
been addressed. In this study, XRD analyses of the specimens revealed that as sintered control specimens consisted
of 100% tetragonal zirconia (50-1089) monoclinic phase
(37-1484) detected after cyclic loading. The phase transformation, even in small amounts, may be attributed to the
subcritical crack growth behavior of Y-TZP under cyclic loading.31,34 The transformation characteristic is dependent on
the grain size, yttria content, and grade of constraint
exerted on them by matrix.12 Therefore differences in grain
size, yttria content, and sintering conditions may lead these
materials to exhibit different degrees of phase transformation under cyclic loading. Considering the transformation
toughening is a function of the concentration of monoclinic
phase, the high fracture toughness value of LF group may
be explained by the high relative amount of monoclinic
phase. The inuence of monoclinic phase content on the

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NEMLI ET AL.

mechanical properties of the Y-TZP has been reported by

previous studies.8,32,34,36 However, it has to be pointed out
that excessive tm transformation may lead to the formation
of surface aws that can be deleterious to the in vivo performance of Y-TZP ceramics.29
Surface treatment methods such as sandblasting, grinding, impact, and milling exert surface damage, micro cracks
and tm phase transformation on Y-TZP surfaces.8,36 This
transformation was reported between 5 and 15% in the literature.8,24,25,36 In the present study, very small quantity of
monoclinic zirconia content of indented Y-TZP surfaces was
found compared to that of ground, sandblasted and fractured Y-TZP surfaces.43 This may be explained by the fact
that once an indentation produced with the sharp indenter,
crack propagation will travel at very high speeds, giving no
sufcient time for tm phase transformation.27
To characterize and quantify the phase transformation
around Vickers indentations in Y-TZP materials several studies were conducted.14,1820 Behrens et al.20 placed Vickers
indentations (500 N) on polished surfaces of Y-TZP specimens. They reported that maximum monoclinic fraction
(
0.5) occurs at a distance of about 100 lm from the center of the indent, which is approximately the position of the
edge of the indent. They also reported a gradual decrease to
zero within a zone extending 100 lm from the edge. These
ndings are in a strong agreement with the present study.
Behrens et al.20 explained that tm transformation is more
easily induced by tensile and shear stresses which greatest
at the edge whereas compressive stresses are higher in the
centre. Outside of the indented region bulk material of YTZP is resistant to phase transformation. The similar results
were also reported on indent-induced phase transformation
of Y-TZP.14,20,22 On the other hand, Reece et al.18 investigated monoclinic phase content around the Vickers indentation in zirconia-based materials and reported a linear
decrease in phase transformation with distance from the
center of the indentation in Y-TZP while Ce-TZP exhibited
maximum transformation at the indentation corner.
The present study which investigated the phase transformation within and around the Vickers indentation including radial cracks revealed that two Y-TZP materials, both
control and fatigue groups, exhibited similar indent-induced
phase transformation behavior in the so called region. However it is known that during indentation loading, the indentinduced stresses not only cause tm transformation around
the indent but also transformation occurs below the base of
the indent.1820 Further research is needed on the effect of
fatigue to bulk material.
The mechanical cycling regime used in the present study
corresponds to a initial clinical service period, but prolonged cycling experiments are needed to evaluate fatigue
behavior of both types of Y-TZP materials. In addition, cyclic
loading during mastication, dental ceramics are susceptible
to the effects of thermal and chemical fatigue as well as to
the effects of cyclic mechanical fatigue.46 It has been recognized that zirconia suffers from low temperature degradation in a humid environment via alterations in its crystalline
structure and dental Y-TZP has an increased susceptibility to

FRACTURE TOUGHNESS AND PHASE TRANSFORMATION OF Y-TZP

ORIGINAL RESEARCH REPORT

crack propagation.43,47,48 Therefore the evaluation of fatigue

behavior of dental ceramics under such conditions is a primary request for successful application of all-ceramic prostheses in dentistry.31 However, fatigue investigations including the simultaneous effect of water and cyclic loading are
limited in the literature.31,43,48 Further research might be
needed on the effect of chemical and/or thermal fatigue of
the materials tested in this study by considering aqueous
environment of the mouth.
CONCLUSIONS

This study presented the results of fracture toughness and

phase transformation of Cercon and Lava Y-TZP core materials before and after cyclic loading applied to simulate functional loading. Within the limitations of the study, following
conclusions can be made:
1. Fatigue with mechanical cycling for 20,000 times did not
cause any statistically signicant difference in the fracture toughness of Cercon while signicant increase was
observed in the fracture toughness of Lava.
2. XRD analyses revealed that fatigue caused tm phase
transformation on the surfaces of sintered Cercon and
Lava specimens being higher in Lava. After Vickers indentation produced by a load of 30 kg, relative amount of
monoclinic zirconia increased on the surfaces of specimens except the specimens of Lava fatigue group.
3. Raman spectroscopy analyses of the Vickers indentation
revealed that the highest tm phase transformation
occurred at corner of the indentation and the second
highest transformation found at the centre of the indentation. The monoclinic fraction found at the points located
at 100 lm and 200 lm away from the corner on the
crack and at the region located
80 lm from the crack
and indent edge were statistically lower than indent center and no signicant difference was found between these
three points.
ACKNOWLEDGMENTS

The authors thank Yeliz Kasko Arc for statistical analyses.

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