Ceramics International 49 (2023) 21716–21721

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Ceramics International
journal homepage: www.elsevier.com/locate/ceramint

Analysis of zirconia mechanical properties after application of a protocol to

simulate clinical aging
Beshr Hajhamid a, Laurent Bozec a, Howard Tenenbaum a, Eszter Somogyi-Ganss a,
Grace M. De Souza b, *
a
Faculty of Dentistry, University of Toronto, 124 Edward St, Toronto, ON, M5G1G6, Canada
b
Department of Comprehensive Dentistry, School of Dentistry, University of Louisville, 501 S. Preston St., Louisville, KY, 40202, United States

A R T I C L E I N F O A B S T R A C T

Handling EditorDr P. Vincenzini In order to test the effects of hydrothermal and clinically related aging on zirconia, monolithic disc-shaped
samples were milled, sintered and polished from two high translucency zirconia , 3 mol % (HT) and 5 mol %
Keywords: (XT). Samples were divided into three groups: non-aged: control (CT); hydrothermal aging (HA - autoclave aging
Hydrothermal aging for 12.5 h at 134 ◦ C, 2 bar); in vitro clinically-related aging (CRA - chewing simulation for 1.2 million cycles
In vitro aging
followed by 50,000 thermocycles and acidic exposure in HCl, pH 1.2, for 15 h). Mechanical properties (flexural
Fatigue strength
strength, fatigue, hardness and elastic modulus) were analyzed and compared using the analysis of variance (at a
Clinically-related aging
level of 5% significance). In vitro clinically-related aging significantly decreased fatigue strength of XT zirconia
with no effects on HT zirconia. Surface hardness and elastic modulus were not affected (p = 0.591 and 0.392
respectively). Hydrothermal aging increased fatigue strength for both materials and decreased the surface
hardness and modulus of HT zirconia (p ≤ 0.001). Hydrothermal aging and in vitro clinically-related aging have
different effects on the mechanical properties of zirconia , when used to simulate five years of clinical service.

1. Introduction tetragonal zirconia has low translucency due to the non-uniform

Zirconia restorations are used widely in restorative dentistry due to
their excellent mechanical and aesthetic properties as well as their
known biocompatibility [1]. Dental zirconia, made of zirconium dioxide
(ZrO2), is composed of three temperature-dependent crystals: mono­
clinic (m), tetragonal (t) and cubic (c) [2]. Yttria, or Yttrium oxide
(Y2O3), is used commonly to stabilize cubic and tetragonal zirconia
crystals at room temperature. Three mol-% of Y2O3 is used to stabilize
the tetragonal crystals at room temperature to produce conventional
tetragonal zirconia, and alumina (Al2O3) is added (0.25 wt %) as a
sintering aid [3]. The tetragonal crystals have the highest density among
zirconia crystals, but are metastable under certain stimuli and can revert
back to a monoclinic crystal form (t-m transformation) [4]. Trans­
formation toughening is used to provide a positive impact on tetragonal
crystals’ metastability since the compressive stress associated with the
transformation can seal a crack from propagating and increase zirconia’s
toughness and flexural strength, something that is particularly impor­
tant when under occlusal function [4,5]. However, conventional
three-dimensional shape of tetragonal crystals, and the distribution of
Al2O3 along the tetragonal crystal boundaries [6,7] which has a negative
impact on its aesthetic properties. Thus, a new generation of high
translucency tetragonal zirconia was developed with lower Al2O3 con­
tent, known as ‘2nd generation zirconia’ [8]. Another approach to
improve the translucency of zirconia-based materials is to increase the
amount of isotropic cubic crystals [9]. Increasing yttria content from 3
to 4 or 5 mol % allows more than 50% of cubic crystals to be stabilized at
room temperature and results in improved optical properties [8]. These
materials are often referred to as ‘3rd generation zirconia’ but have
reduced mechanical properties as compared to conventional and 2nd
generation zirconia due to the higher concentration of cubic crystals and
the lack of transformation toughening [10].
A drawback of t-m transformation is known as low-temperature
degradation (LTD) which occurs when the metastable tetragonal crys­
tals are exposed to humidity and transform back to m spontaneously
over time [11,12]. This process leads to increased surface roughness
with the formation of microcracks through which water molecules can

* Corresponding author.
E-mail addresses: Beshr.hajhamid@utoronto.ca (B. Hajhamid), l.bozec@dentistry.utoronto.ca (L. Bozec), Howard.Tenenbaum@sinaihealth.ca (H. Tenenbaum), e.
s.ganss@utoronto.ca (E. Somogyi-Ganss), grace.desouza@louisville.edu (G.M. De Souza).

https://doi.org/10.1016/j.ceramint.2023.03.311
Received 17 November 2022; Received in revised form 27 March 2023; Accepted 30 March 2023
Available online 1 April 2023
0272-8842/© 2023 Elsevier Ltd and Techna Group S.r.l. All rights reserved.
B. Hajhamid et al.
penetrate thus leading to t-m transformation in the sub-surface of zir­
conia [13].
Clearly, more understanding of issues that regulate and/or partici­
pate in the changes noted above needs to be investigated further. In
relation to this, hydrothermal aging in an autoclave has been introduced
to simulate the accelerated aging of zirconia to estimate the stability of
the zirconia crystals [14] that might correlate to longer term aging/use
in the mouth. A previous study suggested that 5 h of autoclave accel­
erated aging (134 ◦ C, 2 bar in steam) corresponds to two years of
intraoral aging [15]. However, intraoral aging of a material encom­
passes numerous other factors that may account for additional chal­
lenges to the stability of zirconia, including but not necessarily limited to
humidity and temperature. For example, mastication produces cyclic
loads on teeth and restorative materials [16]. In addition, eating and
drinking episodes result in pH and temperature variations [17] that
could play an essential role in the stability of zirconia crystals, affecting
the longevity of the restorations.
Many previous studies evaluated the effects of hydrothermal aging
on zirconia-based materials. Still, there is no evidence of the effect of
more clinically-related factors such as mastication, temperature and pH
variations on zirconia-based materials. Therefore, the objective of this
study was to compare the effect of in vitro clinically-related aging
including hydrothermal aging on the mechanical properties of zirconia-
based materials. We hypothesize that the different methods used for
simulation of aging decrease the mechanical properties of zirconia-
based materials, and that mechanical properties will be affected by
material composition.
2. Materials and methods
2.1. Sample preparation
Two high translucency forms of zirconia: 2nd generation (3 mol % -
Cercon HT Dentsply Sirona Prosthetics- HT) and 3rd generation (5 mol
% - Cercon XT- Dentsply Sirona Prosthetics- XT) were milled using
computer-aided design/computer-aided manufacturing (CAD/CAM)
technique to obtain 90 disc-shaped samples from each material. Samples
were sintered according to the manufacturer’s recommendations and
the final dimensions of the discs created had a diameter of 16 mm and a
thickness of 1.2 ± 0.2. All samples had one side polished using silicon
carbide papers (400, 600, 800 and 1200 grit, Buehler, Illinois, US) fol­
lowed by 0.3–0.6 μm diamond paste suspension using a rotary grinder
and polisher (Metaserv 250 Grinder/Polisher, Buehler) at a speed of 300
rpm. After being cleaned ultrasonically in acetone for 5 min and air-
dried, samples were annealed in a laboratory chamber furnace
(1200 ◦ C/2 h, CWF1300, Carbolite) to remove compressive stresses
occurring during sample preparation [18].
2.2. Aging
Samples from each material were distributed randomly into three
different groups (n = 30 per group) as follows: no treatment (Control,
CO), hydrothermal aging (HA), and in vitro clinically-related aging
(CRA).
CO–No aging was applied. Samples were stored in distilled water at
room temperature until tests were applied.
HA – zirconia samples were aged for 12.5 h in the autoclave (Ritter
M9 Midmark Sterilizer) at 134 ◦ C, with 2 bars of pressure [19]. Then,
samples were stored in distilled water at room temperature until further
testing.
CRA – this model was developed to simulate mechanical, thermal
and acidic challenges occurring in the oral cavity. Zirconia samples were
embedded with polymethylmethacrylate (PMMA, Ivoclar Vivadent) in a
metallic holder and stabilized to the base of a chewing simulator
(Mechatronik CS 4.4, SD Mechatronik GMBH). The antagonist surface
was a 6 mm diameter spherical steatite indenter (SD Mechatronik
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Ceramics International 49 (2023) 21716–21721
GMBH) to simulate an opposing tooth. Samples were exposed to 1.2
million cycles in the chewing simulator with 0.5 mm vertical and hori­
zontal paths (0–50 N, 60 mm/min, artificial saliva, 37 ◦ C) [20]. After
this, samples were exposed to thermocycling between temperatures of
5 ◦ C and 55 ◦ C for 50,000 cycles (30 s in each bath, 15 s transfer time; SD
Mechatronik Thermocycler GMBH). Then, the acidic challenge was
applied by immersion of samples in simulated gastric fluid (pepsin-free
0.2% w/v sodium chloride in 0.7% v/v hydrochloric acid, pH = 1.2) at
25 ◦ C for 15 h (simulated gastric fluid, Ricca chemical company, Lot
#4004D83). Samples were rinsed with distilled water for 30 s and stored
in fresh distilled water at room temperature until further tests were
applied.
2.3. Mechanical properties
2.3.1. Flexural strength
Biaxial flexural strength was measured in 10 samples from each
group using the piston-on-three-ball configuration (6872–2015) in a
universal testing machine (Instron Model 8501). Disc-shaped samples
were placed on 3 mm supporting balls, positioned 120◦ from each other
in a 10 mm diameter circle (ISO Standard 6872:2015). The load was
applied perpendicular to the center of the sample with a speed of 1.0
mm/min. The load-to-failure was recorded for each sample and con­
verted into MPa.
2.3.2. Fatigue strength
Fatigue strength based on the staircase approach was analyzed using
the same fixture applied for the biaxial flexural strength test [21].
Samples were immersed in a container filled with distilled water at room
temperature (Instron Model 8501) and fatigue loading was applied for
100,000 cycles, at a frequency of 6 Hz. The parameters for the test were
set based on piston-on-three-ball flexural strength mean values: initial
load – 70% of the mean flexural strength; step size – 5% of the mean
flexural strength. If the sample failed before completing the 100,000
cycles of fatigue, the load applied to the next specimen was decreased by
one step size (5% of the mean flexural strength). If the sample survived
100,000 cycles, the load to the next specimen was increased by one step
size. This procedure was repeated until 15 samples were tested after the
first inversion of events.
2.3.3. Surface hardness and modulus
Following ultrasonic cleansing in acetone for a period of 10 min, the
surface hardness and modulus of samples were measured using a
nanoindenter (NHT3 – Anton Paar GMBH). A 50 nm radius Berkovich
diamond tip indenter was used to perform seven progressive multicycles
of loading and partial unloading at ten different locations on each
specimen (10 Hz, speed of penetration depth 2000 nm/min). Hardness
and elastic modulus values were determined using the Oliver-Pharr
method [22].
2.4. Statistical analysis
After checking for normal distribution of datapoints between the
samples for the values of flexural strength, fatigue resistance, hardness
and modulus, two-way analysis of variance (ANOVA) and Tukey post-
hoc test (SPSS Inc) were used to evaluate the effects of aging on me­
chanical and surface properties. The independent factors included zir­
conia composition and aging. The Dixon-Mood method was used to
determine the mean fatigue limits and standard deviation. A Kaplan-
Meier survival analysis was performed to determine the survival rate
of specimens after fatigue. An overall significance level of 5% was set for
all tests.
B. Hajhamid et al. Ceramics International 49 (2023) 21716–21721

3. Results Table 2
Surface hardness and elastic modulus of zirconia-based materials before and
3.1. Flexural strength after aging. Different letters in each column represent 5% significance among
the groups.
A significant effect of aging (p ≤ 0.001), material (p ≤ 0.001) and Material Aging Surface hardness GPa (±SD) Surface modulus GPa (±SD)
interaction between material and aging (p ≤ 0.001) was observed for HT CO 20.1 (2.0)a
273.6 (18.9)a
flexural strength, as shown in Table 1. The lowest flexural strength was HA 13.0 (0.9)b 208.6 (34.6)b
observed for XT zirconia after CRA (315.4 ± 79.6 MPa) and the highest CRA 20.0 (4.3)a 261.8 (18.4)a
flexural strength among groups was recorded for HT zirconia after HA XT CO 18.8 (2.6)a 255.7 (18.0)a
(865.3 ± 179.3 MPa). HA 19.2 (2.0)a 259.7 (40.7)a
CRA 18.7 (2.8)a 251.3 (34.33)a

3.2. Fatigue strength
Aging (p ≤ 0.001), material (p ≤ 0.001) and interaction (p = 0.003)
had a significant effect on fatigue resistance (Table 1).
The staircase results showed that there was a decrease in the strength
of zirconia, ranging between 25.6% and 38.6% (Table 1). The number of
survival-failure and the range of cycles for failure are reported in
Table 1, and Fig. 1 shows the staircase profile for each zirconia after
aging. The fatigue strength of XT zirconia significantly decreased after
CRA (211.6 ± 13.6 MPa) compared to CO group (310.5 ± 4.2 MPa). The
fatigue strength of HT zirconia was unaffected by CRA. Hydrothermal
aging increased fatigue strength for both types of zirconia compared to
the control group, as observed in Table 1.
There were no significant differences in the fatigue survival rates
among the groups (Kaplan-Meier and the Long Rank test (Mantel-Cox) p
= 0.924, Fig. 2).
3.3. Surface hardness and modulus
4. Discussion
This study investigated the effect of in vitro aging on the mechanical
properties of two different high translucency forms of zirconia: 2nd
generation zirconia (3 mol % - Cercon HT); and 3rd generation (5 mol %
- Cercon XT). These in vitro methods are used often to estimate the
degradation of dental zirconia is hydrothermal aging [14] in ways that
might yield information relating to their predicted functionality in the
oral cavity as restorations. At the same time, one study estimated that 5
h of autoclave aging represents 15–20 years of clinical service of
biomedical zirconia [23], another study estimated that 5 h of autoclave
aging simulates two years of clinical service for dental zirconia [15]. It
seems that in general, the correlation between hydrothermal aging and
clinical aging of zirconia has not been clarified. In relation to this, other
studies have shown the lack of correlation between hydrothermal aging
and chewing simulation [24–26], which is just one of the factors ac­
counting for the clinical degradation of zirconia. Therefore, this study
applied, what we believe to be a more in vitro clinically-related model of
stressors to which zirconia restorations might be exposed in order to
simulate challenges occurring in the mouth with the use of the methods.
These included the use of mechanical, chemical and thermal stresses,
There was a significant effect of aging (p ≤ 0.001) and the interaction between
material and aging on hardness (p ≤ 0.001) and modulus (p ≤ 0.001). In
contrast, the material composition was not significant on hardness (p = 0.094)
and modulus (p = 0.327). The lowest surface hardness (13 ± 0.9 GPa) and
modulus (208.6 ± 34.6 GPa) were observed for HT zirconia after hydrothermal
aging, as reported in Table 2.
which taken together could represent more closely the environment to
which zirconia restorations would be exposed clinically. To reiterate,
this in vitro clinically-related model replicated some of the oral chal­
lenges, various intraoral chewing forces, temperature changes and
acidic challenge faced by dental restorations in the mouth. The extent of
each of those regimens was determined to simulate 5 years of clinical
aging based on information published previously [15,27–29].
The study hypothesis, that the different methods used for aging
decreased the mechanical properties of zirconia-based materials, was
accepted. The results showed that hydrothermal aging for 12.5 h had no
significant effect on the flexural strength of zirconia, as previously re­
ported in a study that investigated hydrothermal aging for up to 20 h
[12].
However, hydrothermal aging significantly increased the strength of
zirconia after 100,000 fatigue cycles, as based on the use of the staircase
method. This effect of hydrothermal aging on HT zirconia might be
related to the volumetric expansion that occurs during fatigue cycling
associated with the transformation toughening mechanism of tetragonal
crystals to monoclinic at the superficial layer, resulting in the concen­
tration of the compressive stresses that prevent the initial propagation of
cracks. In support of these study results, a previous study by this team
showed a transformation of 40% from tetragonal to monoclinic for HT
zirconia after autoclave aging for 12.5 h [30]. The same study showed
0% of monoclinic crystals on HT and XT zirconia after sintering, pol­
ishing, and annealing when the same protocol reported in this study was
used [30].
An increase in fatigue strength of 2nd generation zirconia as a
consequence of hydrothermal aging has been reported previously [31].
In in vitro clinically-related aging, the results showed a significant
decrease in flexural strength and fatigue resistance of XT zirconia only.
Both zirconia formulations used in this study contained different levels
of metastable tetragonal crystals. Based on the manufacturer’s descrip­
tion,5 and 9% of yttria are used to stabilize tetragonal and cubic crystals
in HT, and XT zirconia, respectively. HT zirconia is composed solely of
tetragonal crystals after sintering (i.e., 100%), while XT contains 50%

Table 1
Flexural strength and fatigue resistance results for zirconia-based materials after hydrothermal aging (HA) and clinically-related aging (CRA). Different letters in each
column represent 5% significance among groups.
Material Aging Flexural strength MPa (±SD) Fatigue resistance MPa (±SD) Strength decrease (%) Numbers of Cycles to failure

Failure Survival

HT CO 778.8 (94.4)a 548.7 (113.9)b 29.6% 6 9 314 - 61,496

HA 865.3 (179.3)a 661.8 (65.3)a 25.6% 7 8 149 - 50,924
CRA 721.9 (160.6)a 512.8 (80.9)b 29% 7 8 1422–50,106

XT CO 505.4 (85.2)b 310.5 (4.2)d 38.6% 8 7 827 - 26,132

HA 484.6 (67.4)b 347 (64.1)c 28.4% 6 9 3665–71,065
CRA 315.4 (79.6)c 211.6 (13.6)e 32.9% 6 9 250 - 15,089

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B. Hajhamid et al.
Fig. 1. Staircase profile for all tested groups. The orange line represents the mean fatigue limit. The black shaded triangle indicates failure, whereas the white shaded
triangle indicates the survival of the sample. The arrow represents the first sample prior to the inversion of events. (For interpretation of the references to colour in
this figure legend, the reader is referred to the Web version of this article.)
Fig. 2. Staircase survival analysis plot obtained by Kaplan-Meier and the Long
Rank test for number of cycles before failure (MPa).
tetragonal and 50% of cubic crystals due to the higher yttria content.
Metastable tetragonal crystals are dense and provide better mechanical
properties compared to stabilized cubic crystals [32]. In fact, the
compositional differences and crystalline structure of both
zirconia-based materials indicate that transformation toughening is
possibly only occurring in HT zirconia due to the higher presence of
tetragonal crystals in the bulk of the material, and no significant trans­
formation toughening occurs after CRA aging. This could also explain
why there was no significant effect of the in vitro clinically-related
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Ceramics International 49 (2023) 21716–21721
protocols on the strength of the HT zirconia. A previous study showed
only 5% of tetragonal to monoclinic transformation for HT zirconia after
aging using the same clinically-related aging model used in this study
[30]. The results of the current study are in concert with findings re­
ported previously where the flexural strength of 2nd generation zirconia
(IPS e.-max ZirCAD) could not be demonstrated even after being
exposed to one million cycles of chewing simulation [26]. This was also
demonstrated in another study where there were no changes in the
flexural strength of 2nd generation zirconia following 5000 cycles of
thermocycling [33]. It might also be postulated that the results reported
here regarding a lower rate of transformation toughening in XT are not
related solely to the content/concentration of tetragonal crystals as
compared to HT zirconia but also because cubic crystals are larger in size
than tetragonal crystals which could decrease the mechanical properties
of the material during aging. A previous study reported an average grain
size of 0.51 μm for HT zirconia and 1.49 μm for XT zirconia [30]. Smaller
crystal sizes are more resistant to mechanical stresses and thus to crack
propagation, which makes HT zirconia more resistant to fracture than a
material with larger grain size, like XT zirconia [34]. Furthermore,
smaller crystals size limits the dislocation of crystalline boundaries,
resulting in increased mechanical properties of zirconia [35]. This might
help explain the observed reduction in strength of XT zirconia after in
vitro clinically-related aging. Another explanation might be related to
the combination effect of chewing simulation with 50 N of loading force
in artificial saliva with the temperature and acidity changes during the
aging therefore, cracks may propagate into the bulk of XT zirconia under
the stress of the chewing simulator, with a low rate of transformation
toughening, and the presence of temperature and acidic changes.
Nanoindentation was used to detect the effects of aging on the sur­
face hardness and modulus of the zirconia sub-types. The indenter
B. Hajhamid et al.
reading was obtained from non-defective regions by chewing simulation
for each sample due to the machine sensitivity. The findings suggested
that there are similar hardness values as well as similar and modulus of
elasticity measures for both forms of zirconia after being exposed to the
in vitro clinically-related aging model. There was no effect on the surface
hardness and modulus of extra high translucency in the different forms
of zirconia following hydrothermal aging. On the other hand, hydro­
thermal aging decreased the surface hardness and modulus of HT zir­
conia. Hydrothermal aging leads to volume expansion associated with t-
m transformation and lowers the hardness of the material due to low
local atomic density [36]. A previous study reported increased surface
roughness of tetragonal zirconia after hydrothermal associated with
grain pull-out, which may affect the indenter reading during loading and
unloading cycles [25]. In agreement with this study, a previous inves­
tigation demonstrated a significant decrease on the surface hardness and
modulus of 2nd generation zirconia following 15 h of autoclave hy­
drothermal aging and similarly there were no changes for 3rd generation
zirconia [37].
The study also hypothesized that mechanical properties will be
affected by material composition, which was partially accepted. The
results showed that HT zirconia has significantly higher strength
compared to XT zirconia. This is mainly related predominantly to the
crystalline composition of the different forms of zirconia as discussed
above. XT zirconia contains fewer tetragonal crystals than HT zirconia
and this difference is likely to be playing a role in our findings suggesting
that XT zirconia had evidently inferior mechanical properties as
compared to HT zirconia. Previous studies showed that 3rd generation
zirconia has lower strength than 2nd and 1st generations [10,37]. On the
other hand, surface hardness and elastic modulus were not affected by
the material composition. There was no significant difference in surface
hardness and modulus between XT and HT zirconia. Even though the
previous study reports correlation between the surface hardness and
crystalline size and the hardness, in which zirconia with smaller crys­
talline size exhibited higher surface hardness [38]. The crystalline
structure size and the indenter size may affect the result reported. The
average size cubic and tetragonal crystals is 1 μm and the radius of the
indenter tip is 50 nm. The comparatively small size of the indenter may
result in testing the hardness and modulus at the grain boundary and
creating variability in the reported data.
The current study investigated the effect of hydrothermal aging and
in vitro clinically-related aging simulating five years of clinical service
on two high translucency zirconia. This study aimed to replicate some of
the mechanical, thermal and acidic challenges occurring in the oral
cavity. However, it did not reproduce real oral challenges as close as one
would like, since oral challenges such as biofilm formation, saliva
buffering effect, and different dietary effects were not included.
Furthermore, more effort should be made to simulate the clinical sce­
nario in a laboratory setting such as using zirconia crowns instead of
disc-shaped samples. By using zirconia in the shape of crowns, it might
be more relevant when considering the application of forces, particu­
larly those that might be tangential to the unidirectionally applied forces
used in this model system. Future studies might evaluate the effect of the
aging model on additional physical and chemical properties of zirconia
including but not limited to crystalline structure analysis, roughness and
optical properties. Additionally, this study did not investigate the effects
of glazing or any other surface alterations required for provision of
clinically acceptable crown restorations on the zirconia properties.
Finally, the current study tested only two high translucency zirconia and
did not evaluate the effects of the aging, for example, on conventional
and currently in use 1st generation zirconia. We also suggest that future
studies should be done to investigate the effects of the aging model on
the zirconia bonding to human enamel.
5. Conclusion
Within the limitations of this study.
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Ceramics International 49 (2023) 21716–21721
• The clinically-related aging model developed caused a decrease in
both flexural strength and fatigue resistance of 3rd generation zir­
conia, with no changes in the 2nd generation. In terms of mechanical
properties, the 2nd generation seems to be a better alternative as a
permanent restorative material.
• Hydrothermal aging increased flexural strength and decreased the
surface hardness of 2nd generation zirconia. Hydrothermal aging
also increased the fatigue resistance of both zirconia-based materials.
• Hydrothermal aging failed to reproduce the changes imposed by
clinically-related aging failed to zirconia-based materials.
Funding
This work was funded by the National Sciences and Engineering
Research council of Canada (NSERC discovery grant #2018-04979).
Declaration of competing interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
Acknowledgment
The authors are thankful to XXXXX for their help in specimens
milling and sintering.
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