Silmeoglu Yagli et al.

BMC Oral Health (2024) 24:967 BMC Oral Health

https://doi.org/10.1186/s12903-024-04745-1

RESEARCH Open Access

The impact of aging and thickness on flexural

strength of various zirconia ceramics
Oyku Silmeoglu Yagli1 , Esra Talay Cevlik1* and Duygu Kurklu Arpacay2

Abstract
Background Effects of the aging process on the flexural strength of Y-TZP and different Y-PSZ ceramics of different
thicknesses were investigated.
Methods 300 disc-shaped samples (12 mm diameter, 0.8 and 1.5 mm thicknesses) were made from 5 different
zirconia materials 3Y-TZP LA, 4Y-PSZ, 5Y-PSZ, 3 + 5Y-PSZ and 4 + 5Y-PSZ. Experimental groups were artificially
aged in an autoclave at 134 °C, 2 bar pressure for 1 and 5 h; control groups were not subjected to any treatment.
Microstructural analysis was conducted using Scanning Electron Microscopy, and X-Ray Diffraction analysis
determined the crystalline phase content. The impact of aging on flexural strength was investigated with the use of
the biaxial flexural strength test. Data were analyzed using three-way ANOVA tests with a significance level of p < 0.05,
applying Bonferroni correction for multiple comparisons.
Results Statistically significant differences in flexural strength were observed among the materials and the material
thicknesses (p < 0.05), while there were no significant differences among the aging times (p > 0.05). The highest
mean flexural strength values were recorded in the case of the 3 Y-TZP-1.5 mm–5 h group (744.1 ± 61.2 MPa), which
was attributed to phase-transformation toughening. The lowest values were observed in the case of the 5 Y-PSZ-
1.5 mm–5 h (338.3 ± 34.8 MPa) group.
Conclusions Both material type and thickness significantly affect the flexural strength of zirconia ceramics, whereas
aging time does not; thus, material selection and thickness are crucial considerations for clinicians.
Keywords Degradation, Strength, Thickness, Yttria-stabilized tetragonal zirconia, Zirconia ceramics

Background alumina (Al2O3) as a stabilizer. This composition ensures

Yttria-stabilized zirconia polycrystalline (Y-TZP) ceram- stability in the tetragonal phase at room temperature
ics have been widely used in dental restorations due to and results in an opaque white structure. To enhance
their excellent mechanical properties and biocompat- the aesthetic properties of 3Y-TZP, the alumina content
ibility. The first generation of this material, known as can be reduced to 0.05%, creating second-generation zir-
‘3Y-TZP’, contains 3 mol% yttria and 0.25% by weight conia known as ‘3Y-TZP LA’ (Low Alumina) [1]. Both
generations of zirconia are noted for their superior flex-
ural strength and high fracture toughness [2] attributed
*Correspondence: to their small-scale grain size (~ 0.3–0.6 μm) [3–5] and
Esra Talay Cevlik
[email protected] transformation toughening [6]. This toughening mecha-
1
Faculty of Dentistry, Department of Prosthodontics, Aydın Adnan nism involves the metastable tetragonal grains trans-
Menderes University, Efeler, Aydın, Türkiye forming into monoclinic grains under stress, causing a
2
Faculty of Dentistry, Department of Prosthodontics, Izmir Democracy
University, Konak, Izmir, Türkiye 3–5% volume increase (martensitic transformation) that

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Silmeoglu Yagli et al. BMC Oral Health (2024) 24:967 Page 2 of 9

induces compressive stresses at crack tips and halts crack decreasing material thickness [14]. Although research
propagation [1, 2, 7]. Subsequent developments involving has predominantly focused on the translucency and frac-
raising the yttria content to 5 mol% [2, 6], produced the ture strength of new generation zirconia [5, 15], there is a
third generation yttria-partially stabilized zirconia ‘5Y- paucity in vitro studies examining their mechanical prop-
PSZ’ while raising the yttria content to 4 mol% [2], cre- erties compared with traditional zirconia, and even fewer
ated the fourth generation ‘4Y-PSZ’ [2]. This creates an investigating how stabilizer content affects phase trans-
additional cubic phase [2, 6] which is incapable of under- formation and mechanical properties.
going phase transformation [4]. The third and fourth gen- The purpose of this study was to investigate the effects
eration zirconia exhibit less or no phase change [3, 4, 6] of aging duration (1 h and 5 h) on the flexural strength
and the flexural strength of PSZ variants varies from 700 of different generations of zirconia ceramics of varying
to 800 MPa and 600 to 900 MPa, respectively [8]. thicknesses (0.8 and 1.5 mm). Our hypothesis for the
The aesthetic properties of monolithic Y-TZP restora- study is: There is no statistically significant difference in
tions have been extensively studied. The absence of an the flexural strength values of different zirconia materi-
amorphous glass phase in zirconia reduces its translu- als, regardless of material thickness or aging time.
cency and enhances its opacity [9]. To address this, mul-
tilayered materials with color- and translucency gradients Methods
have been developed, mimicking the natural appearance The minimum sample size was calculated using data
of teeth in monolithic restorations [10]. In these systems, from previous research (the TP group with the low-
opacity is higher in the gingival region, while translu- est η2 value was selected in the study’s results section)
cency increases towards the incisal region, achieving [16] in the G*Power v.3.1.9.2 program (Heinrich Heine,
a natural tooth-like appearance. Advanced monolithic University of Dusseldorf, Dusseldorf, Germany). To
color and strength-gradient zirconia combine the ben- calculate the flexural strength differences between
efits of various zirconia generations, featuring a basal the study groups, an alpha error of 0.05 and a power
layer with improved mechanical properties (3Y-TZP or of 0.95 were established, resulting in a minimum esti-
4Y-PSZ) and a more translucent incisal layer (5Y-PSZ) mated sample size of 7 for each group. To enhance the
[11]. statistical power of the study and account for poten-
However, monolithic zirconia restorations are suscep- tial sample loss, 10 samples per group were included.
tible to low-temperature degradation (LTD) in moist Consequently, the study comprised a total of 300
environments, where exposure to water induces a slow specimens.
transition from the tetragonal to the monoclinic phase The disc-shaped specimens (final dimensions: 12 mm
[12, 13]. The layered manufacturing process of zirconia in diameter, 0.8 and 1.5 mm thickness) were designed
blanks may also negatively impact mechanical proper- to be positioned in the center of the zirconia ceramics,
ties [10]. It has been indicated that the impact of low- with the long axis of the discs parallel to the short axis
temperature degradation is more pronounced with of the zirconia ceramic discs (Fig. 1). Pre-sintered zir-
conia ceramic discs with a diameter of 98.5 mm and a
thickness of 18 to 20 mm, selected in accordance with
the specimen sizes, were placed in the milling unit. A
total of 300 specimens were fabricated from five dif-
ferent zirconia ceramics: 3Y-TZP LA (DD Bio ZX2
Color, Dental Direct, Germany), 4Y-PSZ (DD Cube
One ML, Dental Direct, Germany), 5Y-PSZ (DD Cube
X2 ML, Dental Direct, Germany) and color/strength-
gradient zirconia materials 3 + 5Y-PSZ (IPS e. max Zir-
CAD Prime, Ivoclar Vivadent, Schaan, Liechtenstein),
4 + 5Y-PSZ (IPS e. max ZirCAD MT Multi, Ivoclar
Vivadent, Schaan, Liechtenstein) by CAD/CAM (Den-
tal Wings Software, DWOS, Turkuaz Dental, Izmir,
Türkiye). Specimens were designed and milled in larger
proportions to compensate for 20–25% shrinkage after
sintering. After milling, the support points were cut to
separate the specimens. Before sintering, the support
point of the specimens were smoothened under run-
ning water using #600, #1000 and #1200 grit silicon
Fig. 1 The design of the zirconia ceramic discs carbide (SiC) papers (English Abrasives & Chemicals
Silmeoglu Yagli et al. BMC Oral Health (2024) 24:967 Page 3 of 9

Ltd). All specimens were sintered as specified by the 1.311Xm

Fm =
manufacturer, and the sintering process removed any 1 + 0.311Xm
monoclinic phase on the surface of the specimens dur-
ing preparation [14]. The specimens underwent a biaxial flexural test in a
Specimens of five different zirconia ceramics were universal testing machine (Marestek, Marestek, Mares
divided into six subgroups, with 10 specimens in each Engineering, Istanbul, Türkiye). Each specimen was
test group. The test groups were labeled based on their placed on three 3.2-mm diameter stainless steel balls,
generic names, thickness, and aging time. (DD Bio ZX2 equidistantly placed from each other on a 10-mm
Color: 3Y, DD Cube One ML: 4Y, DD Cube X2 ML: 5Y, diameter circle. The load was applied at the center of
IPS e. max ZirCAD Prime: 3 + 5Y, IPS e. max ZirCAD the specimens by a cylindrical-loading piston (1.4 mm
MT Multi: 4 + 5Y. For example: 3Y-0.8-1 indicates that diameter) until a fracture occurred at a cross-head
DD Bio ZX2 Color with 0.8 mm thickness underwent 1 h speed of 1 mm/min according to ISO standards 6872.
of aging) The subgroups in each material that were not A computer attached to the test machine recorded the
aged were designated as the control groups. load at the time that specimens fractured. The formula
Specimens were artificially aged in an autoclave (HV- below was used to convert the test results from N to
50, Upright Autoclave, Hirayama, Manufacturing Corp, MPa in accordance with international standards (ISO
Saitama, Japan) at 134 °C, under 2 bar pressure, for 1 h 6872).
(n = 100) and 5 h (n = 100) according to ISO standards S = − 0.2387 P(X- Y)/d2.
13356. One hour of this ageing process at 134 °C is equiv- S: Maximum tensile stress (MPa),
alent to 3–4 years of in vivo function [17], while control P: Load causing fracture (N).
groups were not subjected to any aging condition. SEM X = (1 + v) ln(r2/r3)2 + [(1-v)/2] (r2/r3)2.
analysis was performed to examine the surface topogra- Y = (1 + v) [1 + ln(r1/r3)2] + (1-v) (r1/r3)2.
phy of one randomly selected specimen from each sub- (V): Poisson ratio (0.25).
group. A total of 30 specimens were gold-coated using a r1: Radius of the support circle (mm),
gold plating device (Quorum Q150 ES, Quorum Technol- r2: Radius of the loaded area (mm),
ogies Ltd, East Sussex, United Kingdom). Prepared speci- r3: Radius of the specimen (mm),
mens were examined under SEM (Carl Zeiss, Sigma 300 d: Thickness of the specimen at fracture origin (mm).
VP, Jena, Germany) at magnifications of X1000, X5000, Data was analyzed using IBM SPSS Statistic V25.0
X10000 and X25000. Crystal structure analyses of the (SPSS Inc., Chicago, IL, USA). The Shapiro-Wilk test,
specimens were performed with an X-ray diffractometer kurtosis-skewness values, and histogram graphs were
(XRD) (Bruker D8 Advance, Bruker AXS GmbH, Karl- used to detect normal distribution; the Levene test was
sruhe, Germany) using a monochromatic CuKα beam. performed for homogeneity of variance. Data were ana-
One specimen was randomly selected from each sub- lyzed using three-way Analysis of Variance (ANOVA)
groups placed in the sample holder of the device. XRD tests p < 0.05 set as significant, with Bonferroni cor-
scans were adjusted to 40 mA current and 40 kV voltage, rection for multiple comparisons. Descriptive analy-
and scanned between 20°- 40° 2θ angles with 0.019° step ses were used to present the results of the Xm and Fm
range. After the scans, diffraction graphs were produced results.
and analyzed using computer software compatible with
the system (EVA, Bruker AXS GmbH, Karlsruhe, Ger- Results
many). For each specimen, the highest peak values in SEM analysis
the regions where the density increased, and the diffrac- SEM images of one representative specimen from each
tion angles at which these values were observed, were groups are shown in Fig. 2. The surface morphology,
recorded. The monoclinic/tetragonal phase ratio (Xm) of grain boundaries and continuity of the specimens were
the phase-changed monoclinic zirconia compared to the evaluated. When the SEM images were examined, dete-
tetragonal phase was calculated using the equation below rioration in the surface morphology was observed after
[18]. Relative intensities of the monoclinic (111), mono- autoclave aging. Changes in topographic patterns caused
clinic (-111), and tetragonal phases are Im(111), Im(-111), by autoclave aging methods were found, and the textured
and It(111), respectively. surface appearance was noted on the specimen surfaces
of 3Y-0.8-5 and 3Y-1.5-5.
Im (111) + Im(−111)
Xm =
Im (111) + Im (−111) + It (101) XRD analysis
The Xm and Fm values are shown in Table 1. Depending
The monoclinic volume content (Fm) was calculated on the aging time and thickness, the relative intensities of
using the formula below: [19] the tetragonal and monoclinic phases differed among the
Silmeoglu Yagli et al. BMC Oral Health (2024) 24:967 Page 4 of 9

Fig. 2 Scanning electron microscope images of the materials (magnification 10000 X)

Table 1 Xm and Fm values by groups (%)

3Y 3Y 4Y 4Y 5Y
0.8 mm 1.5 mm 0.8 mm 1.5 mm 0.8 mm
Xm Fm Xm Fm Xm Fm Xm Fm Xm Fm
Control 0.05 0.07 0.03 0.04 0.04 0.05 0.03 0.04 0.04 0.06
1h 0.07 0.09 0.07 0.09 0.03 0.04 0.03 0.05 0.04 0.06
5h 0.20 0.20 0.17 0.21 0.06 0.08 0.06 0.08 0.05 0.06
5Y (3 + 5)Y (3 + 5)Y (4 + 5)Y (4 + 5 )Y
1.5 mm 0.8 mm 1.5 mm 0.8 mm 1.5 mm
Xm Fm Xm Fm Xm Fm Xm Fm Xm Fm
Control 0.04 0.06 0.04 0.05 0.06 0.07 0.03 0.04 0.06 0.08
1h 0.05 0.06 0.08 0.10 0.10 0.13 0.04 0.06 0.04 0.05
5h 0.05 0.06 0.18 0.22 0.13 0.16 0.03 0.04 0.05 0.06

materials. The Fm values shows similarity to the Xm val- Biaxial flexural strength
ues. The Fm values of 3Y and (3 + 5)Y groups differs with The mean biaxial flexural strength data are shown in
increasing aging time. A representative XRD pattern of Fig. 4. Based on three-way ANOVA results, there was a
the specimens of 3Y group were given in Fig. 3(a-b), (a) significant difference among the ceramics in terms of
represents the XRD graph of the 3Y-0.8 mm specimens, the mean flexural strength values (F = 187.907, p = 0.000,
while (b) represents 3Y-1.5 mm specimen. According to η2 = 0.736). Based on the Eta Square (η2) value, the impact
the result of the XRD analysis, monoclinic and tetragonal of materials on flexural strength is great (η2 > 0.14).
peak intensities differ in terms of aging time. In the 3Y There was a significant difference in the mean flex-
and (3 + 5)Y groups the monoclinic phase increased with ural strength values in terms of material thicknesses
the increase of the aging time. (F = 17.358, p = 0.000, η2 = 0.060) and, according to the Eta
Silmeoglu Yagli et al. BMC Oral Health (2024) 24:967 Page 5 of 9

Fig. 3 XRD graphs of a specimen taken from subgroups of 3 Y-TZP material

Fig. 4 Flexural strength values

Square (η2) value, thickness has a moderate effect on the moderate effect on the flexural strength, the interac-
flexural strength of the materials. tion of thickness*aging (F = 0.176, p > 0.05, η2 = 0.001)
No statistically significant difference was found in and material*thickness*aging time (F = 0.551, p > 0.05,
terms of the aging (F = 0.916, p > 0.05, η2 = 0.007). While η2 = 0.016) had no effect on flexural strength.
the interaction of the independent variables in terms of The post hoc Bonferroni test indicated that the dif-
material*thickness (F = 5.376, p = 0.000, η2 = 0.074) and ference among the groups was statistically significant
material*aging (F = 2.381, p = 0.017, η2 = 0.066) have a (p < 0.05) except between the 4Y and (3 + 5)Y groups
Silmeoglu Yagli et al. BMC Oral Health (2024) 24:967 Page 6 of 9

(p ˃ 0.05) Table 2. Statistically, the highest mean flexural their flexural strength. The results showed no significant
strength values were observed in the 3Y group, followed interaction between material type, thickness and aging
by the 4Y, (3 + 5)Y, (4 + 5)Y, and 5Y groups respectively, time. However, there are significant differences in the
while no significant difference was found between the flexural strength values based on material type and thick-
4Y and (3 + 5)Y groups. The mean flexural strength value ness, while aging times did not have a significant effect.
of the materials with 1.5 mm thickness was statistically This results in partial acceptance of the null hypothesis.
higher than with regard to 0.8 mm thickness (p = 0.000). Previous studies have used various specimen shapes
Three-way ANOVA followed by post hoc Bon- in in vitro settings, such as disc-shaped [5, 7, 12, 20–22],
ferroni tests were conducted, and according to the rectangular, [20] and bar-shaped specimens [16, 23].
results, the material*thickness interactions of (3 + 5) Disc-shaped specimens in particular have been pro-
Y and (4 + 5)Y materials had statistically signifi- duced with different diameters (12 mm [12], 14 mm [21],
cant effects (p = 0.002, p = 0.000) in terms of flexural 15 mm [5, 7, 20]) and thicknesses (0.5 mm [5], 1 mm
strength values (p < 0.05). In both materials, the flex- [20], 1.2 mm [7, 12] 1.3 mm [21]). The use of mono-
ural strength increased as the thickness increased. The lithic Y-TZP restorations in crowns necessitates a tooth
material*thickness interactions of 3Y, 4Y and 5Y groups reduction of 0.5 to 1.5 mm or more to accommodate the
did not have a statistically significant effect on flexural ceramic layer thickness [23]. One study [24] reported
strength (p > 0.05). Only in the case of the 3Y group did that the optimal concealing thickness varies depend-
the material*aging interaction give statistically significant ing on the substructure material and that a minimum
results in terms of flexural strength (p = 0.012). There was thickness of 0.8 mm is required for zirconia copings on
a statistically significant difference between the control nickel-chromium alloy abutments. In another study [25],
and 5-hour aging time groups in terms of 3Y material disc-shaped specimens of 0.8 and 1.5 mm thickness were
(p = 0.016). The flexural strength value of the 3Y-control fabricated to assess the impact of yttria content on Y-TZP
was less than of the 3Y-5 h aging group. translucency and masking ability, with results showing
that all zirconia specimens effectively masked titanium at
Discussion a minimum thickness of 1.5 mm. In the present study, as
In this study, zirconia materials 3Y-TZP LA (DD Bio ZX2 noted above disc-shaped 12 mm in diameter specimens
Color), 4Y-PSZ (DD Cube One ML), 5Y-PSZ (DD Cube were fabricated with a thickness of 0.8 and 1.5 mm.
X2 ML) and color/strength-gradient zirconia materials Autoclave treatment is frequently used as an acceler-
3 + 5Y-PSZ (IPS e. max ZirCAD Prime), 4 + 5Y-PSZ (IPS ated aging test for zirconia ceramics [26]. However, the
e. max ZirCAD MT Multi) were examined to compare correlation between autoclaving duration and the aging
time measured in vivo remains a controversial issue [27].
Table 2 Pairwise comparison of the materials It has been reported that 1 h of aging in an autoclave at
Materials Mean Standard p 134 °C and 2 bar pressure corresponds to 3–4 years of
difference error
aging in the oral environment [28]. This aging procedure
DD Bio 4Y 65.069 13.147 0.000*
ZX2Color
has been applied in various studies with different aging
5Y 312.121 13.147 0.000*
(3Y) durations [13, 16, 21, 22]. In the present study, the auto-
(3 + 5)Y 81.183 13.147 0.000*
clave aging times were equivalent to approximately 3–20
(4 + 5)Y 222.068 13.147 0.000*
years in a clinical intraoral environment reflecting the
DD Cube 3Y -65.069 13.147 0.000*
One ML 5Y 247.052 13.147 0.000*
estimated lifetime of zirconia service.
(4Y) (3 + 5)Y 16.114 13.147 1.000
Transformation toughening is a process in which
(4 + 5)Y 156.999 13.147 0.000* stress induces the transformation of tetragonal crystals
DD Cube 3Y -312.121 13.147 0.000* to monoclinic crystals in stabilized zirconia. This trans-
X2ML 4Y -247.052 13.147 0.000* formation is associated with a significant volume expan-
(5Y) (3 + 5)Y -230.938 13.147 0.000* sion of 3–5%, which generates compressive stresses that
(4 + 5)Y -90.053 13.147 0.000* prevent crack opening and increase resistance to crack
IPS e.max 3Y -81.183 13.147 0.000* propagation [29].
ZirCAD 4Y -16.114 13.147 1.000 A study investigated the flexural strength of disc-
Prime 5Y 230.938 13.147 0.000* shaped specimens of four different zirconia materials
(3 + 5)Y (3Y-TZP, 4Y-TZP, 5Y-TZP, and 6Y-TZP) after autoclave
(4 + 5)Y 140.885 13.147 0.000*
IPS e.max 3Y -222.068 13.147 0.000* aging [20]. The results indicated that 3Y-TZP zirco-
ZirCAD MT 4Y -156.999 13.147 0.000* nia exhibited higher flexural strength compared to
Multi 5Y 90.053 13.147 0.000* other cubic-containing zirconia materials. It has been
(4 + 5)Y
(3 + 5)Y -140.885 13.147 0.000* stated that higher yttria content stabilizes zirconia with
*P < 0.05 more cubic crystals, eliminating the transformation
Silmeoglu Yagli et al. BMC Oral Health (2024) 24:967 Page 7 of 9

toughening mechanism [30]. This result can be attrib- discrepancy between the present study and the previ-
uted to the more stable phase of cubic zirconia, which ous study [14] regarding the decrease in flexural strength
reduces stress-induced transformation toughening [31]. over time, could be attributed to the shorter aging time,
In alignment with the findings of the previous study in the present study.
[20], the average flexural strength in the 5Y groups The interaction between material type and thickness
examined in the present study was below 500 MPa. has a statistically significant effect on flexural strength
Consequently, it is recommended that full-contour in the (3 + 5)Y and (4 + 5)Y groups, with flexural strength
crowns and three-unit fixed prostheses that do not increasing with thickness in these groups. However, this
involve molar restorations be used. However, the (3 + 5) interaction is not observed in other groups. Although the
Y group exhibited a greater amount of tetragonal struc- flexural strength of the 5Y-0.8 group was higher than the
ture due to transformation toughening phenomenon. 5Y-1.5 group, this difference was not statistically signifi-
As a result, the flexural strength for (3 + 5)Y group was cant. In another study [34] it was concluded that increas-
greater than 500 MPa but did not exceed 800 MPa. ing the 5Y-TZP zirconia crown thickness resulted in a
Therefore, it is suitable for fabricating prostheses moderate but statistically insignificant increase in frac-
involving molar restorations with a span of no more ture force. These findings are in line with the present
than four units, and multi-unit bridges with a maximum study’s results. According to the manufacturer’s instruc-
of two pontics. Conversely, in the present study, the 3Y tions, the required minimum thickness for (3 + 5)Y and
groups demonstrated the highest strength. Thus, 3Y is (4 + 5)Y materials is 0.8 mm in the anterior region and
recommended for the fabrication of prostheses involv- 1.0 mm in the posterior region. The results of our study
ing partially or fully covered substructure for crowns support these guidelines. In the posterior region, where
and bridges of any span [32]. However, in [20] there was greater forces are applied, material thickness becomes
a partial discrepancy between the results, as the flexural crucial. For areas subjected to high forces (such as pos-
strength of 3Y-TZP decreased with aging. In contrast, terior crowns, long span bridges, and patients with brux-
the present study observed that the 3Y control group ism), it is recommended to increase the thickness of
had lower flexural strength values compared to the 3Y these materials.
group aged for 5 h, a result which may be attributed to Over the years, studies [20–22] assessing the amount
the transformation toughening mechanism [29]. of transformation and the biaxial flexural strength have
Various in vitro studies have demonstrated that the presented conflicting results. This discrepancies are
mechanical properties of 5Y-PSZ ceramics are inferior to attributed to the varying parameters used in aging. Some
those of 3Y-TZP and 4Y-PSZ ceramics [30, 33, 34]. One studies did not observe any significant impact on the
study [6] reported that zirconia with 5.5% and greater phase transformation after up to 5 h aging in an autoclave
than 6% mol Y2O3 content were resistant to hydrother- [36–38], resulting in nearly 25.4% monoclinic phase at
mal aging for up to 54 h. The results of the present study the surface [37].
support these findings [6]. One study [39] reported that the volume fraction
In another study [35], it was found that an increase in change of the monoclinic phase depends on the brands
the thickness of monolithic zirconia leads to an increase of translucent zirconia after hydrothermal treatment.
in its flexural strength. Yet, another study [14] reported Another study [40] proposed that using the equation (19)
that both thickness and the flexural strength of the mate- may lead to inaccurate estimations of monoclinic phase
rial increased simultaneously, while prolonged aging fraction (Fm) in zirconia material containing a signifi-
time resulted in decreased flexural strength. Our find- cant amount of cubic phase. It was suggested that X-ray
ings showed a statistically significant difference in the diffraction (XRD) analyses can enhance the accuracy
flexural strength between the two specimen thicknesses, of phase composition determinations. However, since
with the mean flexural strength of the 1.5 mm specimens XRD analysis was performed on a single specimen
being significantly higher. These results align with those from each subgroup in the present study, it is not pos-
reported in the aforementioned studies [14, 35]. However, sible to make a statistical evaluation in terms of flexural
unlike one of the previous studies [14], no significant dif- strength results. The highest Xm values were obtained
ference was observed between aging times in terms of in the 3Y-0.8-5 (0.20%), 3Y-1.5-5 (0.17%), (3 + 5)Y-0.8-5
flexural strength values. The interaction between mate- (0.18%), (3Y + 5)-1.5-5 (0.13%) groups. These discrepan-
rial type and aging has statistically significant effect only cies in Xm values may be related to tetragonal-to-mono-
in the case of the 3Y groups. Specifically, the 3Y control clinic phase transformation in materials with 3 mol%
group exhibited lower flexural strength values compared yttria content. Additionally, the 3Y and (3 + 5)Y groups
to the 3Y-5 group, which may be attributed to the trans- exhibited higher flexural strength values compared to
formation toughening mechanism. Also the results of the other groups. When the Xm values are interpreted
another study [21] support the present study’s result. The alongside the flexural strength results, it can be inferred
Silmeoglu Yagli et al. BMC Oral Health (2024) 24:967 Page 8 of 9

Acknowledgements
that transformation toughening likely occurred in these This article is extracted from Oyku Silmeoglu Yagli’s PhD dissertation entitled
groups, whereas it was not observed in others. “Evaluation of Different Aging Times on Flexural Strength of Zirconia Ceramics”,
According to the SEM analysis conducted in the pres- supervised by Asist. Prof. Dr. Esra Talay Cevlik and Assoc. Prof. Dr. Duygu Kurklu
Arpacay. Authors extend their sincere gratitude to Dr. Dt. Baykal Yılmaz for
ent study, the control groups exhibited shallower and, his invaluable support. As this study is conducted in vitro, the acquisition of a
more uniform surfaces, whereas the test groups with Clinical Trial Number was not required.
extended aging showed greater surface degradation. The
Author contributions
susceptibility to low-temperature degradation of zirco- Authors planned the study. OS performed the material and methods and
nia ceramics used in the oral cavity may vary, and this collected the data. DKA and ETC analyzed and interpreted the data and
factor should be considered in the application of mono- ETC was a major contributor in writing the manuscript. All authors read and
approved the final manuscript.
lithic zirconia materials. The clinical use of translucent
zirconia is important, as indicated by the literature, as Funding
materials with high cubic phase and yttria content are This study is self-funded. The authors do not have any financial interest in the
companies whose materials are included in this article.
more stable.
A limitation of the present study was the use of disc- Data availability
shaped specimens, which do not mimic the geometry of All data generated or analyzed during this study are included in this published
article.
crown-bridge restorations. However, designing and pro-
ducing these specimens from the middle of monolithic
Declarations
color and strength-gradient materials provides an advan-
tage in that it mimics the color and strength-gradient Ethics approval and consent to participate
properties of crown-bridge restorations. XRD analysis Ethics approval was obtained from the Non-Interventional Clinical Research
Evaluation Commission of the Faculty of Dentistry, Aydın Adnan Menderes
was used to examine the phase transformation in this University (protocol no: 2021/13; date: 07.04.2021).
study. For a more comprehensive understanding of the
phase transformation mechanism and in order to evalu- Consent for publication
Not applicable.
ate the cubic phase content of highly translucent zirconia
materials, it is recommended that detailed phase analysis Competing interests
Raman spectroscopy or Rietveld analysis and refinement The authors declare no competing interests.

be performed. Multi-layered discs possess a complex

Received: 6 June 2024 / Accepted: 13 August 2024
multi-compositional structure, making it challenging
to pinpoint the exact location of phase transformation,
given that did not occur uniformly across all layers.
Since this study was conducted in vitro, artificial aging References
conditions cannot fully replicate the oral environment. 1. Stawarczyk B, Keul C, Eichberger M, Figge D, Edelhoff D, Lümkemann N. Three
Therefore, it is difficult to establish a linear relationship generations of zirconia: from veneered to monolithic. Part I. Quintessence Int.
2017;48(5).
between the results of these studies and the longevity of 2. Zhang Y, Lawn B. Novel zirconia materials in dentistry. J Dent Res.
restorations. 2018;97(2):140–7.
3. Harada A, Shishido S, Barkarmo S, Inagaki R, Kanno T, Örtengren U, et al.
Mechanical and microstructural properties of ultra-translucent dental
Conclusions zirconia ceramic stabilized with 5 mol% yttria. J Mech Behav Biomed Mater.
Within the limitations of this study, it was concluded 2020;111:103974.
that: 4. Kolakarnprasert N, Kaizer MR, Kim DK, Zhang Y. New multi-layered
zirconias: composition, microstructure and translucency. Dent Mater.
2019;35(5):797–806.
1. Flexural strength varies depending on the type of 5. Inokoshi M, Shimizu H, Nozaki K, Takagaki T, Yoshihara K, Nagaoka N, et al.
zirconia material used, with 3Y-TZP LA (DD Bio Crystallographic and morphological analysis of sandblasted highly translu-
cent dental zirconia. Dent Mater. 2018;34(3):508–18.
ZX2 Color) exhibiting the highest flexural strength 6. Camposilvan E, Leone R, Gremillard L, Sorrentino R, Zarone F, Ferrari M, et al.
values among those examined. Aging resistance, mechanical properties and translucency of different yttria-
2. The thickness of the zirconia material significantly stabilized zirconia ceramics for monolithic dental crown applications. Dent
Mater. 2018;34(6):879–90.
influences its flexural strength. 7. Pereira GK, Guilardi LF, Dapieve KS, Kleverlaan CJ, Rippe MP, Valandro LF.
3. Aging time does not affect the flexural strength Mechanical reliability, fatigue strength and survival analysis of new poly-
values. crystalline translucent zirconia ceramics for monolithic restorations. J Mech
Behav Biomed Mater. 2018;85:57–65.
8. Yousry M, Hammad I, Halawani ME, Aboushelib M. Translucency of recent
Material selection and thickness are crucial factors that zirconia materials and material-related variables affecting their translucency:
clinicians must consider. However, the aging time did not a systematic review and meta-analysis. BMC Oral Health. 2024;24(1):309.
9. Heffernan MJ, Aquilino SA, Diaz-Arnold AM, Haselton DR, Stanford CM, Vargas
significantly affect the zirconia samples evaluated in this MA. Relative translucency of six all-ceramic systems. Part I: core materials. J
study. Prosthet Dent. 2002;88(1):4–9.
Silmeoglu Yagli et al. BMC Oral Health (2024) 24:967 Page 9 of 9

10. Kaizer MR, Kolakarnprasert N, Rodrigues C, Chai H, Zhang Y. Probing the inter- 26. ISO 13356. Implants for Surgery - Ceramic Materials Based on Yttria-Stabilized
facial strength of novel multi-layer zirconias. Dent Mater. 2020;36(1):60–7. Tetragonal Zirconia (Y-TZP). 2008.
11. Schönhoff LM, Lümkemann N, Buser R, Hampe R, Stawarczyk B. Fatigue 27. Lughi V, Sergo V. Low temperature degradation-aging-of zirconia: a critical
resistance of monolithic strength-gradient zirconia materials. J Mech Behav review of the relevant aspects in dentistry. Dent Mater. 2010;26(8):807–20.
Biomed Mater. 2021;119:104504. 28. Chevalier J, Grandjean S, Kuntz M, Pezzotti G. On the kinetics and impact of
12. Wille S, Zumstrull P, Kaidas V, Jessen LK, Kern M. Low temperature degrada- tetragonal to monoclinic transformation in an alumina/zirconia composite
tion of single layers of multilayered zirconia in comparison to conventional for arthroplasty applications. Biomaterials. 2009;30(29):5279–82.
unshaded zirconia: phase transformation and flexural strength. J Mech Behav 29. Hannink R, Pascoe R. Ceramic Steel? Nat (London). 1975;258(5537):703–4.
Biomed Mater. 2018;77:171–5. 30. Holman CD, Lien W, Gallardo FF, Vandewalle KS. Assessing Flexural Strength
13. Flinn BD, Raigrodski AJ, Mancl LA, Toivola R, Kuykendall T. Influence of aging Degradation of New Cubic containing Zirconia materials. J Contemp Dent
on flexural strength of translucent zirconia for monolithic restorations. J Pract. 2020;21(2):114–8.
Prosthet Dent. 2017;117(2):303–9. 31. Hannink RH, Kelly PM, Muddle BC. Transformation toughening in zirconia-
14. Zhuang Y, Zhu Z, Jiao T, Sun J. Effect of aging time and thickness on low-tem- containing ceramics. J Am Ceram Soc. 2000;83(3):461–87.
perature degradation of dental zirconia. J Prosthodont. 2019;28(1):e404–10. 32. ISO 6872: 2015. Dentistry-Ceramic materials. 2015.
15. Pecho OE, Ghinea R, Ionescu AM, de la Cruz Cardona J, Paravina RD. Del Mar 33. Spies BC, Zhang F, Wesemann C, Li M, Rosentritt M. Reliability and aging
Pérez M. Color and translucency of zirconia ceramics, human dentine and behavior of three different zirconia grades used for monolithic four-unit fixed
bovine dentine. J Dent. 2012;40:e34–40. dental prostheses. Dent Mater. 2020;36(11):e329–39.
16. Kim H-K, Kim S-H. Effect of hydrothermal aging on the optical proper- 34. Rosentritt M, Preis V, Behr M, Strasser T. Fatigue and wear behaviour of zirco-
ties of precolored dental monolithic zirconia ceramics. J Prosthet Dent. nia materials. J Mech Behav Biomed Mater. 2020;110:103970.
2019;121(4):676–82. 35. Karbasian N, Fathi A, Givehchian P, Nosouhian S, Jamshidian M, Almassi F, et
17. Kontonasaki E, Rigos AE, Ilia C, Istantsos T. Monolithic zirconia: an update al. Comparative assessment of flexural strength of monolithic zirconia with
to current knowledge. Optical properties, wear, and clinical performance. different thicknesses and two sintering techniques. Clin Experimental Dent
Dentistry J. 2019;7(3):90. Res. 2024;10(3):e856.
18. Garvie RC, Nicholson PS. Phase analysis in zirconia systems. J Am Ceram Soc. 36. De Souza GM, Zykus A, Ghahnavyeh RR, Lawrence SK, Bahr DF. Effect of
1972;55(6):303–5. accelerated aging on dental zirconia-based materials. J Mech Behav Biomed
19. Toraya H, Yoshimura M, Somiya S. Calibration curve for quantitative analysis of Mater. 2017;65:256–63.
the monoclinic-tetragonal ZrO2 system by X‐ray diffraction. J Am Ceram Soc. 37. Egilmez F, Ergun G, Cekic-Nagas I, Vallittu PK, Lassila LV. Factors affecting the
1984;67(6):C–119. mechanical behavior of Y-TZP. J Mech Behav Biomed Mater. 2014;37:78–87.
20. Kengtanyakich S, Peampring C. An experimental study on hydrothermal 38. Stawarczyk B, Frevert K, Ender A, Roos M, Sener B, Wimmer T. Comparison
degradation of cubic-containing translucent zirconia. J Adv Prosthodont. of four monolithic zirconia materials with conventional ones: contrast ratio,
2020;12(5):265. grain size, four-point flexural strength and two-body wear. J Mech Behav
21. Amarante JEV, Pereira MVS, De Souza GM, Alves MFRP, Simba BG, Dos Santos Biomed Mater. 2016;59:128–38.
C. Effect of hydrothermal aging on the properties of zirconia with different 39. Putra A, Chung K-H, Flinn BD, Kuykendall T, Zheng C, Harada K, et al. Effect
levels of translucency. J Mech Behav Biomed Mater. 2020;109:103847. of hydrothermal treatment on light transmission of translucent zirconias. J
22. Pereira G, Amaral M, Cesar P, Bottino M, Kleverlaan C, Valandro L. Effect of Prosthet Dent. 2017;118(3):422–9.
low-temperature aging on the mechanical behavior of ground Y-TZP. J Mech 40. Ha S-R, Choi Y-S. Effect of hydrothermal aging on dental multilay-
Behav Biomed Mater. 2015;45:183–92. ered zirconia for monolithic restorations: an in vitro study. Ceram Int.
23. Shen J, Xie H, Wu X, Yang J, Liao M, Chen C. Evaluation of the effect of low- 2021;47(12):17057–68.
temperature degradation on the translucency and mechanical properties of
ultra-transparent 5Y-TZP ceramics. Ceram Int. 2020;46(1):553–9.
24. Tabatabaian F, Taghizade F, Namdari M. Effect of coping thickness and back-
ground type on the masking ability of a zirconia ceramic. J Prosthet Dent. Publisher’s note
2018;119(1):159–65. Springer Nature remains neutral with regard to jurisdictional claims in
25. Cho Y-E, Lim Y-J, Han J-S, Yeo I-SL, Yoon H-I. Effect of yttria content on the published maps and institutional affiliations.
translucency and masking ability of yttria-stabilized tetragonal zirconia
polycrystal. Materials. 2020;13(21):4726.