RESEARCH AND EDUCATION

Fracture strength and energy-dispersive spectroscopy analysis

of 3-unit fixed partial dentures fabricated from different
monolithic zirconia materials
Gülbahar Erdinç, DDS,a Mehmet Bülbül, DDS, PhD,b and Mutlu Özcan, DDS, DMD, PhDc

Fixed partial dentures (FPDs) ABSTRACT

can be manufactured from
metal, metal-ceramic, or
ceramic materials.1 Ceramic
systems can be used in FPD
production in the posterior
region, providing excellent es-
thetics, biocompatibility, and
high fracture strength. Yttria
2
partially stabilized tetragonal
zirconia polycrystal (Y-TZP)
ceramics have become popular
with their high mechanical
properties and can be ven-
eered with feldspathic porce-
lain to improve esthetics.
Statement of problem. Mastication forces in different regions affect the survival of multiunit
posterior restorations. The fracture strength of 3-unit posterior monolithic zirconia fixed partial
dentures (FPDs) and their fracture patterns require investigation.
Purpose. The purpose of this in vitro study was to evaluate and compare the fracture strength and
fracture pattern of 3-unit posterior FPDs fabricated from different monolithic zirconia materials.
Material and methods. Thirty 3-unit FPDs were fabricated from BruxZir, FireZr, and Upcera (n=10
per group). Energy-dispersive spectroscopy analysis was performed on 2 selected specimens from
each group. All specimens were exposed to a mastication simulator for 1.2×106 cycles and then
monotonically loaded to fracture at a crosshead speed of 1 mm/min. The surfaces of a selected
fractured specimen were examined at magnifications of ×25 and ×500 with scanning electron
microscopy. Conformity to normal distribution was evaluated with the Shapiro-Wilk test. One-
way analysis of variance was used to compare the normally distributed initial crack formation
load F initial (Fi) and catastrophic failure strength F maximum (Fm) means by group. Weibull
statistics were calculated by using the maximum likelihood estimation method. The chi-square
test was used to compare shape and scale parameters (a=.05).
3

However, the feldspathic por- Results. The mean Fm values were fail1878.9 N for Upcera, 2177.8 N for BruxZir, and 2229.4 N for
celain is susceptible to delam- FireZr. Upcera and BruxZir showed statistically significant differences for the Fm mean values
4 ,5 (P=.039). The differences between the fracture type distributions according to the groups were
ination and chipping.
statistically similar (P>.05). For Fi, Upcera presented the highest Weibull modulus value (2.199),
Therefore, monolithic zirconia FireZr had the lowest (1.594), while for Fm, BruxZir had the highest Weibull modulus value
restorations with altered (9.267) and FireZr the lowest (6.572).
composition and microstruc-
Conclusions. Using the zirconia materials BruxZir, FireZr, and Upcera resulted in high Fm values
ture have been introduced to
after aging procedures. With all materials, the fractures were most commonly found in the
improve the optical properties connector areas in the tested FPDs. (J Prosthet Dent 2023;-:---)
without significantly affecting
the mechanical properties, expanding their clinical in- monolithic zirconia crowns have sufficient fracture
dications.6-8 strength in the molar region, even if the crown thickness
Zirconia has been reported to have flexural or is reduced to 0.5 mm.11 This minimal preparation pre-
bending strength values between 900 and 1200 MPa and serves tooth tissue and increases crown retention.12
resistance to fracture values of approximately 9 to 10 Polished zirconia has also been reported to result in
MPa.9,10 In addition, in vitro studies have indicated that less wear on the antagonists than glazed zirconia.13

a
Assistant Professor, Department of Prosthodontics, Faculty of Dentistry, Karabük University, Karabük, Turkey.
b
Professor, Department of Prosthodontics, Faculty of Dentistry, _Istanbul Aydin University, _Istanbul, Turkey.
c
Professor and Head, Division of Dental Biomaterials, Clinic for Reconstructive Dentistry, Center for Dental and Oral Medicine, University of Zurich, Zurich, Switzerland.

THE JOURNAL OF PROSTHETIC DENTISTRY 1.e1

1.e2
Clinical Implications
Clinicians should comply with the recommended
connector size of monolithic zirconia to prevent
fractures.
Polished monolithic zirconia may be considered the best
option for posterior FPDs in patients with a grinding or
clenching habit.14
The high strength of Y-TZP has been associated with
transformation toughening, creating compressive stresses
in the areas near the crack surface that slow crack pro-
gression.15-18 However, when this phase transformation
occurs spontaneously in the presence of water or steam,
it creates roughness and microcracks on the surface of
the material and causes low-temperature degradation
(LTD), which decreases strength.11,19 Monolithic resto-
rations may have increased phase transformation as they
are directly exposed to the mastication loads and saliva
that have been reported to decrease the flexural strength
of monolithic zirconia.20-25 Fracture strength has been
considered critical to understanding the clinical potential
and limitations of dental ceramics.26 Therefore, the cur-
rent study aimed to evaluate the fracture strength and
clinical applicability of different 3-unit monolithic zirco-
nia FPDs after mastication simulation by measuring
fracture strength and with energy-dispersive spectros-
copy analysis of the fracture patterns. The null hypothesis
was that no difference would be detected in the initial (Fi)
and maximal fracture (Fm) strength properties and frac-
ture patterns of the different tested zirconia materials
after thermomechanical aging.
MATERIAL AND METHODS
The left mandibular first premolar and first molar in a
typodont model (Frasaco GmbH) were prepared for FPD
abutments having a 1-mm-wide chamfer finish line with
diamond rotary instruments (6856 L-016; Brasseler Inc).
Three-dimensional digital images of the prepared model
were created with a dental laboratory scanner (Dental
Wings 7 Series; Dental Wings), and cobalt-chromium
replicas of the area to be restored (Co-Cr SP2-Pulver;
Amann Girrbach AG) were produced to use in mastica-
tion simulation. According to the manufacturer’s rec-
ommendations, all connectors were designed to be
greater than 9 mm2. The specimens (n=10) were milled
from green stage zirconia blocks (BruxZir Shaded; Gli-
dewell Direct GmbH, FireZr; Glidewell Direct GmbH,
Upcera; Shenzhen Upcera Dental Technology Co) on a
milling unit (D15; Yenadent) and sintered in a furnace
(Tegra Speed; Yenadent) according to the manufacturers’
recommendations. Specimen size calculation was based
on mean Fmax values and determined using data from a
THE JOURNAL OF PROSTHETIC DENTISTRY
Volume - Issue -
Table 1. Properties of monolithic zirconia blocks
Brand Composition
Sinterization
Temperature Manufacturer
BruxZir ZrO2+HfO2+Y2O3+Al2O3>99.9 1580  C Prismatik
Shaded Y2O3=5.15±0.2 Dentalcraft
Al2O3 <0.5
FireZr ZrO2+HfO2+Y2O3+Al2O3>99.9 1530  C Prismatik
Y2O3=5.15±0.2 Dentalcraft
Al2O3 <0.5
Upcera ZrO2+HfO2+ Y2O3 >99.6 1480  C Liaoning
Y2O3=5.2 Upcera
Al2O3 <0.5
previous study.3 The properties of monolithic zirconia
blocks are shown in Table 1.
The specimens were ultrasonically cleaned in distilled
water for 10 minutes (BioSonic UC300; Coltène). Energy-
dispersive spectroscopy (EDS) was performed to deter-
mine the differences in the elemental composition and
chemical structure of the monolithic zirconia FPD surface
on 2 specimens from each group. Energy-dispersive
X-ray spectroscopy (EDAX) images were captured
(Hitachi TM4000 II Benchtop SEM; Hitachi) using the
following operating parameters: 15.0 kV accelerating
voltage and magnification×500. Each measurement was
repeated 3 times, and the mean value recorded.
All specimens were luted to the abutments with a
composite resin-based cement (Panavia 21; Kuraray
Noritake). Mastication simulation was performed with a
Ø8-mm stainless steel ball with 49-N loading force. A
total of 1.2×106 cycles (custom-made mastication simu-
lator; University of Zurich) were performed to simulate
5 years of clinical service.12 The movements were applied
at a frequency of 1.67 Hz. Thermocycling was performed
at 5  C to 55  C for 60 seconds, along with the cyclic
mechanical loading in the mastication simulator. All
specimens survived in the mastication simulator without
decementation.
Each specimen was mounted in a universal testing
machine (Z010; Zwick/Roell) and was then mono-
tonically loaded to fracture at a crosshead speed of 1 mm/
min. The load was vertically transferred onto the middle
pontic center via a Ø6-mm stainless steel ball. The
maximum fracture (Fm) load was measured until the
crown failed, and the initial (Fi) force to initiate fracture
was recorded in N.
The fracture sites of the specimens were inspected
with an optical microscope (Digital microscope, VHX
2000D; Keyence), and fracture types were classified ac-
cording to their regions. A fractured specimen was
selected for fractographic analysis. Fracture patterns of
zirconia specimens were observed at different magnifi-
cations and 5 kV accelerating voltage with a scanning
electron microscope (SEM) (Hitachi TM4000 II Benchtop
SEM; Hitachi) at ×25 and ×500 magnifications to estab-
lish the point of initiation of fracture.
Erdinç et al
- 2023
Table 2. Comparison of Fi and Fm values according to groups
Upcera BruxZir FireZr
Force Mean ±SD Mean ±SD Mean ±SD
Fi 403.6 ±221.9 966.9 ±692.5 345 ±236
Fm 1878.9 ±313a 2177.8 ±250.8ab 2229.4 ±365.1b
df, degree of freedom; F, test statistics; SD, standard deviation. Different superscripted
letters in same column show significant differences (P<.05).
Data were analyzed with a statistical software pro-
gram (IBM SPSS Statistics, v23; IBM Corp). Conformity
to normal distribution was evaluated by using the
Shapiro-Wilk test. One-way analysis of variance
(ANOVA) was used to compare the normally distributed
Fi and Fm means by group. The chi-square test was used
to compare the fracture types according to the regions.
Regression analysis was performed based on the fracture
strength data to determine the Weibull modulus and
characteristic strength, and Weibull statistics were
calculated with the maximum likelihood estimation
method to interpret the predictability and reliability of
monolithic zirconia materials.27 The chi-square test was
used to compare shape and scale parameters. Analysis
results in quantitative data mean ±standard deviation
and median (minimum-maximum) and categorical data
were presented as frequency (percentage) (a=.05).
RESULTS
The Fi mean values of the different brands (403.6 N for
Upcera, 966.9 N for BruxZir, and 345 N for FireZr) were
statistically similar (P=.423). A statistically significant
difference was found in the Fm mean values of Upcera
and BruxZir (P=.039) (1878.9 N for Upcera, 2177.8 N for
BruxZir, and 2229.4 N for FireZr) (Table 2). EDS evalu-
ation and images for each group are presented in
Figure 1.
Most specimens fractured in the connector region. No
significant difference was observed between the fracture
type distributions according to the groups (P>.05). Only 1
specimen of the FireZr brand fractured at both connec-
tors (Table 3). The fracture patterns of the specimens are
shown in Figure 2.
For Fi, Upcera had the highest Weibull modulus value
(2.199), while FireZr had the lowest Weibull modulus
value (1.594) (Table 4). While no significant difference
was observed between the distributions of the shape
parameters according to the groups (P=.760), there was a
statistical difference between the distributions of the scale
parameters (P=.030), because of the significant difference
between Upcera and BruxZir. For Fm, BruxZir had the
highest Weibull modulus value (9.267), and FireZr had
the lowest Weibull modulus value (6.572). The differ-
ences between the distributions of the shape parameters
according to the groups were statistically similar (P=.545)
(Table 5). However, a statistically significant difference
Erdinç et al
1.e3
was found between the distributions of the scale pa-
rameters (P=.029), between all groups (Fig. 3). Figure 4
F df P shows an SEM image of FireZr.
1.049 2 .423
3.653 2 .039
DISCUSSION
This study compared the fracture strength of commer-
cially available monolithic zirconia FPDs. Based on the
results of the current study, the null hypothesis was
accepted for the initial fracture load Fi. However, since
material types showed a significant difference in
maximum fracture strength Fm, the null hypothesis could
be partially rejected.
A standard test procedure is lacking for mechanical
and thermal cycling to investigate the fatigue resistance
of FPDs. In the present study, referencing a previous
study, specimens were exposed to 1.2×106 cycles, corre-
sponding to 5 years of clinical service, in a mastication
simulator.12
Yucel et al28 reported that ceramic crowns seated on
dies without cementation showed significantly lower
fracture resistance during the load-to-failure test than
those bonded on dies. In addition, another study re-
ported that monolithic zirconia crowns cemented on
occlusal grooved abutments showed lower fracture
resistance compared with crowns cemented on flat
occlusal surface abutments.10 In the present study, the
anatomic contour specimens were cemented with com-
posite resin cement on the abutments to simulate the
clinical conditions and improve the fracture testing.
The mean Fm values were 1878.9 N for Upcera,
2177.8 N for BruxZir, and 2229.4 N for FireZr, acceptable
fracture load values compared with previous studies10
that identified many factors related to the fracture
strength of zirconia, including the microstructure,
cementation of the restorations, sintering procedure, fa-
tigue test used, and direction and location of the load
applied.10
The fracture strength values after artificial aging
suggested that all the monolithic zirconia materials were
suitable for posterior restorations.1 Oblak et al3 reported
lower fracture resistance than in the present study,
possibly because of the higher number of units in the
restoration, the differences in the material’s microstruc-
ture, or the differences in the aging procedure. Using
data from dental laboratories, Sulaiman et al29 reported a
2.6% fracture rate in 1779 restorations with multiple-unit
fixed dental prostheses in place for more than 5 years.
Elsayed et al25 reported decreased mechanical prop-
erties after aging with the increase of yttrium oxide in
zirconia ceramics. The 3Y-TZP had higher fracture
strength, with an average of 7820 N compared with 4 and
5Y-TZP. The present study found a statistically significant
difference between Upcera and BruxZir regarding frac-
ture values. The Y2O3 content of Upcera is slightly higher
THE JOURNAL OF PROSTHETIC DENTISTRY
1.e4
Chemical Composition
Group B (Wt%)
Zr 73.25
O 20.22
Si 6.52
K 2.33
Na
AI
Figure 1. Energy-dispersive spectroscopy evaluation and images of each group (left to right: BruxZir, FireZr, Upcera), including chemical composition.
Al, aluminum; K, potassium; Na, sodium; O, oxygen; Si, silicon; Zr, zirconium.
than that of BruxZir, but all materials tested were 5Y-TZP
zirconia materials. Considering the results of the study by
Elsayed et al,25 the higher Y2O3 content can explain the
lower fracture values compared with 3Y-TZP and the
lower values of Upcera compared with BruxZir in the
present study.
The Weibull modulus (m) is a shape parameter where
higher m values indicate comparable fracture stress
values enabling the prediction of the expected strength of
a material.22,27 Thus, the Weibull modulus has been
generally referred to as the reliability factor of the tested
parameter. Weibull modulus values show the variability
of Fi or Fm values in different groups in the present study.
High modulus values indicate that the measurements are
close to each other and that the specimens have little
variability, while low m values suggest that the mea-
surements show high variability and have different dis-
tributions of Fm or Fi values. The shape and scale
parameters were evaluated. A statistically significant
difference (P=.029) was found between the distributions
of parameters according to the groups for Fm, showing
more reliable results for BruxZir, corresponding to the
higher fracture strength observed.
The fractures were predominantly in the connector
areas in the tested FPDs. The connector design has been
reported to significantly influence the fracture resistance
and survival of zirconia FPDs.16 Although the connector
area was prepared according to the manufacturer’s
recommendation in the present study, all fractures were
associated with the connector area. Consistent with the
results of the current study, Rosentritt et al30 reported
that, in their study with 3-unit zirconia FPDs, fractures
always occurred in the connector areas between the
pontic and the crowns or nearby crown margins. How-
ever, Villefort et al31 evaluated the fatigue limit of
anatomic contour 3-unit FPDs and reported that the
THE JOURNAL OF PROSTHETIC DENTISTRY
Volume - Issue -
Group F (Wt%) Group U (Wt%)
53.6 72.1
21.38 21.03
18.78 6.88
1.58
2.3
Table 3. Comparison of fracture type distributions by groups n (%)
Fracture Type** Upcera BruxZir FireZr c 2* df P Adj. P
Distal connector 8 (80) 3 (30) 7 (70) 10.992 4 .027 .051
Mesial connector 2 (20) 7 (70) 4 (40)
*Pearson chi-square. **Multiple response.
fractures originated from both the connector and the
pontic area. The connector area must be at least 7.0 mm2,
especially for long-span FPDs. Increasing the connector
thickness improves the fracture strength of the restora-
tion, but a thick connector may adversely affect peri-
odontal health and esthetics.1
SEM was used to inspect the fracture origin, fracture
pattern, and crack propagation path in the present study.
A brittle material’s strength depends upon the size of the
most significant defect present.22,27 In the SEM images,
the origin (starting point of crack propagation), mirror
(smooth origin surrounding region), and mist area
(microsplitting as a result of energy conversion to addi-
tional fracture surface area) were observed and confirmed
by the fracture pattern. All fractures were associated with
the connector area when the specimens were examined,
a few of which also involved the crown margin.
EDS is a precise and nondestructive method of eval-
uating the material’s mineral component and has been
widely used in dental material studies.32 EDS involves
specimen bombardment with a high-voltage electron
beam that generates different wavelengths for each type
of mineral. Changes in the wavelength of the radiation
emitted by the specimen define changes in mineral
concentration.33 In the present study, content differences
between the groups were determined. BruxZir and
Upcera presented quite similar weight percentages
regarding the detected chemical elements of zirconium
(Zr), oxygen (O), and Si (silicon). However, the sintering
Erdinç et al
- 2023 1.e5

Figure 2. Images from fractured specimens. A, Most common fracture pattern at connector region. B, Fracture origin (blue arrow), fracture depth
progressing toward abutment tooth, and exposure of abutment framework (blue star).

Table 4. Weibull analysis results for Fi

Shape (m) Scale
Shape (%95 CI) S. Error Scale (%95 CI) S. Error
Upcera 2.199 (1.128 e 4.288) 0,749 458.646 (300.418 e 700.212)a 99.009
BruxZir 1.831 (0.751 e 4.465) 0,833 1095.98 (569.434 e 2109.43)b 366.135
FireZr 1.594 (0.939 e 2.704) 0,430 386.161 (250.427 e 595.465)ab 85.329
2
c 0.549 7.046
df 2 2
P* .760 .030

Scale expressed as scale or span parameter showing what tested values would be if 63.2% of material failed. Higher scale values indicate more spread of data. *Chi-square test. Different
superscripted letters in same column show significant differences (P<.05).

Erdinç et al THE JOURNAL OF PROSTHETIC DENTISTRY

1.e6 Volume - Issue -

Table 5. Weibull analysis results for Fm

Shape (m) Scale
Shape (%95 CI) Std Scale (%95 CI) Std
Upcera 6.982 (4.341 e 11.23) 1.693 2006.49 (1826.58 e 2204.12)a 96.171
BruxZir 9.267 (5.841 e 14.701) 2.182 2289.09 (2131.97 e 2457.8)b 83.051
FireZr 6.572 (4.156 e 10.391) 1.536 2382.83 (2155.57 e 2634.04)c 121.856
P* .545 .029
*Chi-square test. Different superscripted letters in same column show significant differences. Scale expressed as scale or span parameter, showing what tested values would be if 63.2% of material
failed. Higher scale values indicate more spread of data.

Probability Plot for F Max

Probability Plot for F Initial Weibull - 95% CI
Weibull - 95% CI 99
99
90
90 80
80 70
70 60
60 50
50 40
40 30

Percent
30
Percent

20
20
10
10
5
5
3
3 2
2
1
1
00

00

00

00
0

10 0
70

80
90

10 100 1000 10000

15

20

30
F Initial F Max
Table of Statistics Table of Statistics
Shape Scale AD* F C Shape Scale AD* F C
2,19872 458,65 2,479 5 0 6,98231 2006,49 1,493 10 0
1,83115 1095,98 3,655 3 0 9,26655 2289,09 1,799 10 0
1,59356 386,16 1,768 9 0 6,57167 2382,83 1,559 10 0

Upcera BruxZir FireZr Upcera BruxZir FireZr

A B
Figure 3. Two-parameter Weibull probability graph based on modulus distribution of shape and scale values for all groups tested. A, Fi. B, Fm. AD,
Anderson-Darling statistics.

protocol differed, with 1580  C being recommended for
BruxZir and 1480  C for Upcera. The higher sintering
temperatures resulted in higher flexural strength,
consistent with Kim et al,34 who stated that the final
temperature in induction furnaces should be increased
rapidly to provide sufficient sintering with higher fracture
strength.
A slight variation in the zirconia composition,
microstructure differences, or sintering procedures may
lead to considerable changes in the material’s proper-
ties.26 Dental manufacturers have continued to develop
monolithic zirconia materials for different indications.
More in vivo and in vitro studies are needed to recognize
these new materials better.
Limitations of this in vitro study include the lack of
precise intraoral conditions such as acid exposure, and the
influence of dentin as an abutment structure was not
considered. Research can be performed by using dentin
abutments prepared from extracted teeth to produce more
accurate results. However, the use of extracted teeth may
complicate the preparation of standard specimens. In
addition, efforts should be made to simulate periodontal
resilience during fatigue testing of the specimens to ach-
ieve more reliable fracture resistance results.
CONCLUSIONS
Based on the findings of this in vitro study, the following
conclusions were drawn:
1. The zirconia materials tested for 3-unit FPDs
demonstrated clinically acceptable fracture strength
values.

THE JOURNAL OF PROSTHETIC DENTISTRY Erdinç et al

- 2023
Figure 4. Scanning electron microscope image of FireZr, showing origin
(starting point of crack propagation, blue star), mirror (smooth origin
surrounding region), and mist area (microsplitting as result of energy
conversion to additional fracture surface area, blue circle).
2. As the connector areas were prone to fracture, the
ideal thickness of connectors should be established
during the design of the FPDs.
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Corresponding author:
Dr Gülbahar Erdinç
Department of Prosthodontics
Faculty of Dentistry
Karabük UniversitydDemir Çelik Campus
Karabük, 78100
TURKEY
Email: gbaharerdinc@gmail.com
Acknowledgments
The authors thank Mr Kiren Mätzener and Dr Nadin Al-Haj Husain from the
University of Zürich (Center of Dental Medicine, Division of Dental Biomaterials,
Clinic for Reconstructive Dentistry, Zurich, Switzerland) for their assistance with
the experimental procedures.
CRediT authorship contribution statement
Gülbahar Erdinç: Conceptualization, Data curation, Formal analysis, Investiga-
tion, Methodology, Resources, Software, Visualization, Writing - original draft,
Writing - review & editing. Mehmet Bülbül: Conceptualization, Formal analysis,
Funding acquisition, Project administration, Supervision, Validation, Writing e
review & editing. Mutlu Özcan: Conceptualization, Data curation, Investigation,
Methodology, Resources, Software, Visualization, Validation, Writing e review &
editing, Funding acquisition, Supervision.
Copyright © 2023 by the Editorial Council for The Journal of Prosthetic Dentistry.
https://doi.org/10.1016/j.prosdent.2023.03.011
THE JOURNAL OF PROSTHETIC DENTISTRY