Received: 5 September 2019 Revised: 7 November 2019 Accepted: 11 November 2019

DOI: 10.1111/jerd.12552

RESEARCH ARTICLE

Does the application of surface treatments in different

sintering stages affect flexural strength and optical properties
of zirconia?

Sevcan Kurtulmus-Yilmaz DDS, PhD1 | Özay Önöral DDS, PhD1 |

Huseyin Aktore DDS, PhD2 | Oguz Ozan DDS, PhD1
1
Department of Prosthodontics, Faculty of
Dentistry, Near East University, Lefkosa,
Mersin 10, Turkey
2
DentX, Lefkosa, Mersin 10, Turkey
Correspondence
Sevcan Kurtulmus-Yilmaz, Department of
Prosthodontics, Faculty of Dentistry, Near
East University, Lefkosa, Mersin 10, Turkey.
Email: sevcankurtulmusyilmaz@gmail.com
Abstract
Objective: To investigate the influence of surface treatments conducted in pres-
intering and postsintering stages on flexural strength and optical properties of
zirconia.
Materials and methods: Specimens were milled from partially sintered zirconia blocks
in different geometries and divided into three main groups as presintered, post-
sintered, and control groups. Test groups were further divided into three subgroups
(n = 10) according to the surface treatments conducted (grinding, Er,Cr:YSGG laser
irradiation, air-borne particle abrasion [APA]). Four-point flexural strength (σ) test and
Weibull analysis were conducted. Color differences (ΔE00) and translucency parame-
ter (TPab) were calculated with a spectrophotometer. Surfaces of specimens were
scrutinized under FESEM. Data were statistically analyzed.
Results: Postsintered groups exhibited higher σ values (P < .05). Within all groups,
highest and lowest σ values were detected at postsintered and presintered APA
groups, respectively (P < .05). All ΔE00 values were above the perceptibility threshold
(ΔE00 > 0.8). Higher TPabvalues were obtained and deeper scratches were observed
in presintered groups.
Conclusions: Surface treatments performed at postsintering stage had a favorable
effect on the flexural strength of all specimens. Surface treatments performed before
sintering increased translucency and caused higher ΔE00 values.
Clinical significance: Surface treatments performed at different sintering stages can
alter mechanical and optical properties of zirconia.

KEYWORDS
monolithic zirconia, surface treatment, flexural strength, laser irradiation

1 | I N T RO D UC T I O N toughening capability when under stress.6-11 However, lack of glass

Zirconia is a white, semitranslucent, polymorphic ceramic that pre-
sents chemical inertness, improved biocompatibility, superior mechan-
ical strength, and thermal expansion coefficient similar to hard
tissues.1-5 It can, moreover, exhibit three different crystallographic
forms in response to temperature and offer transformation-
matrix in its crystallographic structure constrains optical properties,
thereby increasing opacity and leading to a nonesthetic appear-
ance.12-14 To overcome this drawback encountered in the clinical
practice, zirconia has been traditionally used as a core in fixed pros-
thetic restorations and veneered with low-fusing feldspathic ceramics.
With this bilayer approach, an important contribution has been put

J Esthet Restor Dent. 2020;32:81–90. wileyonlinelibrary.com/journal/jerd © 2019 Wiley Periodicals, Inc. 81

82
forth in the enhancement of optical properties.15-18 However, cata-
strophic failures including fracture, chipping, and delamination associ-
ated with these challenging restorations have been widely declared in
clinical reports.6,19-22 This can be attributed to the veneer ceramic
that may not be resistant enough to withstand the occlusal forces, to
the thermal expansion coefficient difference between core and
veneering ceramic, and to insufficient wettability of veneering.4,6
Additionally, zirconia presents a low thermal diffusivity that can result
in thermal incompatibility, cause residual stress formation within por-
celain, and subsequently lead to different failure modes.6
In response of high demand for preventing catastrophic complica-
tions, full-contour (monolithic) zirconia (FCZ) restorations that do not
require veneering were introduced.23-26 This monolayer approach has
simplified procedures due to the elimination of veneering stage, and
24
conservative tooth preparation can be feasible. FCZ restorations,
furthermore, offer better clinical performance not only mechanically
but also optically than its predecessor since the zirconia used in
monolithic restorations differs from conventional zirconia in terms of
translucency. Even so, for better biomimetic characterization, the
optical properties can also be enhanced by immersion in coloring liq-
uids, addition of metallic pigments to the preliminary zirconia powder,
or painting zirconia with liners.23-26
As poor bonding can lead to both biological and mechanical com-
plications, the establishment of a durable bond between ceramic and
luting cement by the genesis of chemical bonds and mechanical inter-
locking has been considered as a pivotal factor for the long-term via-
27-30
bility of a restoration. Different micromechanical (mechanical,
chemical, and laser treatments) and chemical bonding techniques (sili-
con coatings, use of coupling agents) have been developed as
attempts to achieve superior bond quality between zirconia and luting
30-33
cement. Among these techniques, the drive to use
micromechanical-based protocols such as air-borne particle abrasion
(APA),5,34,35 diamond grinding (G),30 multiphase glass ceramic
coating,30 low fusing porcelain coating,36 selective infiltration
32,36 30
etching, application of zirconia particle suspension, gas plasma
treatment,34,37 application of phosphate monomers with fusing glass
beads,38 argon-ion bombardment,28,34 acid-etching with highly corro-
sive acid combinations,30 and laser irradiation (LI)3,5,9,27 has increased
in intensity. Acid-etching is commonly recommended as a surface
treatment to roughen the intaglio of silica-based ceramics, but zirconia
ceramic does not susceptible to chemical conditioning with acid due
to the lack of silica content.33-36,38 Although favorable effects of sur-
face treatments on the bond strength have been well-documented in
a systematic review,30 the possibility that surface treatments may
compromise mechanical1,34 and optical properties23 of zirconia resto-
rations has also been asserted.
Surface treatments are commonly applied subsequent to
sintering.1,5 However, application of surface treatment just before
sintering process may offer a number of benefits: (a) as surface treat-
ments tend to form flaws and sharp crevices, sintering can diminish
the extent of these crack precursors by smoothening them,
(b) sintering can decrease the amount of relative monoclinic phase
formed by surface treatments, (c) regarding better mechanical
KURTULMUS-YILMAZ ET AL.
interlocking of zirconia with resin cement, surface treatments before
sintering can be more effective in increasing roughness due to the soft
characteristics of presintered zirconia, and (d) milling of soft blocks is
easier and less abrasive on the instruments.9,33,35
To the best knowledge of authors, the effect of surface treat-
ments on the bond strength of zirconia was well-assessed.3,5,29,35
However, data regarding the influence of surface treatments in differ-
ent sintering stages on optical properties and flexural strength of FCZ
restorations are limited. Therefore, it was aimed in the current study
to evaluate the flexural strength and optical properties of zirconia
specimens subjected to three different surface treatments
including G, Erbium, chromium-doped yttrium, scandium, gallium and
garnet (Er,Cr:YSGG) LI, and APA in presintering and postsintering
stages. In accordance with intra-group and inter-group (Control, APA,
LI, and G) measurements, the null hypothesis was that there would be
no statistically significant effect of surface treatment and sintering
process on the data of translucency parameter, color difference, and
flexural strength of zirconia.
2 | MATERIALS AND METHODS
2.1 | Preparation of zirconia specimens
The schematic setup of the experiment is presented in Figure 1. All
specimens were virtually designed according to the test method on an
open-source three-dimensional modeler software (FreeCAD, Version
0.16.6704, Jurgen Riegel, Ulm, Germany). The standard tessellation
language (STL) data were generated and transferred to the computer-
aided design–computer-aided manufacturing (CAD-CAM) machine for
the fabrication of the specimens. Specimens were subtracted from
cold-isostatic pressed, partially sintered zirconia blocks (GC Initial Zir-
conia Disk HT 18 mm, GC America/Second Generation 3Y-TZP
Ceramic with 4.5%-5.6% Yttria content) with the aid of a 5-axis milling
machine (Sirona inLab MC X5, Dentsply Sirona, Pennsylvania) in three
different dimensions in accordance with the method applied
(Figure 1). For flexural strength test, bar-shaped specimens
(2 × 20 × 4 mm); for color measurement, square-shaped specimens
(0.8 × 10 × 10 mm); and for topographic analysis, disc-shaped speci-
mens (height: 1 mm; diameter: 8 mm) were prepared. All specimens
were subjected to wet-polishing with 600-, 800-, and 1200-grit SiC
papers for 15 s by using a grinder-polisher device (Phoenix Beta
Grinder-Polisher, Buehler) at 300 rpm. Hence, irregularities were mini-
mized and surface-texture standardization was achieved.
2.2 | Surface treatment methods
Specimens with the same geometries were divided into three main
groups as presintered, postsintered, and control groups. Presintered
and postsintered groups were further divided into three equal sub-
groups (n = 10/subgroup) according to the surface treatment methods
applied, as presented in Figure 1. Specimens from the control group
remained untouched. For LI group, the entire intaglio surface of each
specimen was irradiated by an Er,Cr:YSGG laser (Waterlase MD,
KURTULMUS-YILMAZ ET AL.
FIGURE 1 Schematic setup of experiment
Biolase, Irvine, California) for 20 s with the aid of a MG6 sapphire tip
on a noncontact hard tissue mode at an energy level of 4 W, a repeti-
tion rate of 20 Hz, and a pulse duration of 140 μs with water/airflow
of 65% and 55%, respectively. For APA group, 110-μm Al2O3 (Korox,
Bego, Bremen, Germany) particles were used to abrade the entire
intaglio surface of each specimen for 20 s at an air pressure of 2 bar
from a distance of 10 mm. For G group, the entire intaglio surface of
each specimen was grinded using a contra-angle handpiece (Synea
WA-65LT, W&H Dental, Bürmoos, Austria) under constant water
cooling with a coarse diamond bur (#842G, Meisinger, Neuss, Ger-
many) for 20 s in a forward-backward sweeping motion. After grinding
of each specimen, the diamond bur was replaced. The tip of the
contra-angle handpiece was aligned to allow only horizontal move-
ment in order to ensure that the entire surface was uniformly grinded
and thus standardized in terms of pressure and grinding direction. By
using a digital caliper, specimens were re-evaluated from five different
points in terms of height to ensure equal amount of grinding. Addi-
tionally, care was taken for the achievement of parallelism between
the specimen and tip of the contra-angle. For the specimens in
presintered groups, surface treatments were conducted before
sintering process; while same surface treatments were performed
after sintering process for the specimens in postsintered groups. To
simulate laboratory steps, all of the specimens were immersed in col-
oring liquid (inCoris T21 coloring liquid A2, Sirona, USA) for 15 s and
then sintered (Sirona inFire HTC speed, Dentsply Sirona, Pennsylva-
nia) at 1450 C !
for 8 h. To achieve standardization,
abovementioned procedures were performed by single calibrated
operator (H.A.).
83
2.3 | Test procedures
To conduct four-point flexural strength test in accordance with ISO
6872:2015 guideline, a table-top universal test machine (EZtest-
500 N, Shimadzu Cooperation) was used. Each specimen with a 45!
chamfer at major edges was positioned on the assembly containing
two supportive steel rods and a 16 mm test span. The treated surface
of each specimen was aligned downward and towards the tension
side. Loading rods (compression side) were in contact with untreated
layer of specimens. With 1 mm/min crosshead speed, specimens were
loaded until failure occurs. The fracture load was recorded in order to
calculate the flexural strength (σ) in MPa as: σ = 3PL/4wb,2 where
P refers to the fracture load in Newton, L refers to the length of test
span in millimeters, w refers to the width of the specimen in millime-
ters, and brefers to the thickness of the specimen in millimeters.
On the data of flexural strength (n = 10/subgroup),26,39,40 Weibull
analysis was conducted to calculate Weibull modulus and thereby, to
determine characteristic strength of the material for reliability. Failure
probability was calculated using the following function (ISO
6872:2015):
#! " $
σ m
P f = 1 − exp −
σ0
where Pf refers to failure probability, σ refers to flexural strength, σ 0
all refers to characteristic strength at fracture probability of 63.21%, and
m refers to Weibull modulus which is equal to the slope of the ln(ln
[1/(1 − Pf)]) vs in lnσ plots.
84 KURTULMUS-YILMAZ ET AL.

To carry out color and translucency measurements, a clinical spec-
trophotometer (VITA Easyshade Compact, VITA Zahnfabrik, Germany)
was used in “tooth single” mode and calibrated in accordance with the
manufacturer's instruction before every single measurement. Care
was taken for positioning measuring tip at the center of the specimen
and for achieving full-contact between tip of device and measuring
surface. For each specimen, three measurements were sequentially
performed and average L*, a*, and b* values were recorded. Color dif-
ferences between control group and test groups on the gray backing
(L* = 61.7, a* = 1.4, b= −0.3) were calculated by using CIEDE2000
(ΔE00) formula:
(SUPRA 55, Carl Zeiss Ag, Germany). All specimens were made con-
ductive for current by coating with a thin layer of platinum/palladium
before positioning on the stub. Subsequently, investigation was done
at an acceleration voltage of 15 kV and a magnification of
×1000-25 000 by one blind calibrated examiner. Supposition of nor-
mal distribution was accepted with respect to the results of Shapiro-
Wilk test (P > .05) and obtained data were, therefore, subjected to
two-way analysis of variance (ANOVA) and Bonferroni post hoc tests
by using a statistical analysis package (IBM SPSS Statistics v23, IBM
Corp) (α = 0.05).

sffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
! 0 "2 ! " ! "
3 | RESULTS
* ∆L ∆C0 2 ∆H0 2 ∆C0 ∆H0
∆E00 = + + + RT
kL SL kC SC kH SH kC SC kH SH
The mean values for flexural strength (σ), color difference (ΔE00),
translucency parameter (TPab), Weibull characteristic strength (σ 0), and
where ΔL0 , ΔC0 , and ΔH0 represents the differences in lightness,
Weibull modulus (m) of specimens underwent to different surface
chroma, and hue between two specimens in CIEDE2000; RT repre-
treatment procedures are demonstrated in Tables 1 and 2.
sents the rotation function that accounts for the interaction between
In comparison with control and presintered groups, postsintered
chroma and hue differences in the blue region. SL, SC, and SH represent
groups exhibited statistically higher σ values (P < .05). Within all
the weighting functions, and kL, kC, and kH, named as parametric fac-
groups, postsintered APA group revealed the significantly highest σ
tors, represent correction terms for experimental conditions. In the
value; whereas the significantly lowest σ value was observed at
current study, aforementioned parametric factors were set to 1. ΔE00
presintered APA group (P < .05). Among presintered grinding,
values lower than 0.8 were considered as imperceptible,
presintered 4 W LI, and control groups; no significant difference was
0.8 < ΔE00 < 1.8 values were considered as clinically acceptable, and
detected in terms of σ (P > .05).
the ones greater than 1.8 were considered as clinically unacceptable
Statistically highest ΔE00 was determined at presintered LI group
color change.41
(ΔE00 = 5.3), followed by presintered APA group (ΔE00 = 3.1). No sta-
Translucency of the specimens was determined with translucency
tistically significant ΔE00 was found among other groups (P > .05);
parameter (TPab). Measurements were performed over a white and a
whereas, ΔE00 values of postsintered LI and grinding groups were
black background. TPabwas assessed by obtaining the color difference
below the acceptability threshold (ΔE00 < 1.8). All ΔE00 values for all
of the specimen on white and black backgrounds with the following
groups were above the perceptibility threshold (ΔE00 > 0.8).
function; where subscript W and B refer to the color coordinates mea-
Among control and postsintered groups, the difference was not
sured over white (L* = 96.2, a* = 0.2, b= −0.3) and black (L* = 11.5,
statistically significant in terms of TPab (P > .05); while higher TPab
a* = 0.6, b= −0.8) backgrounds, respectively.
values were observed at presintered groups (P < .05). The TPabvalue
h& was highest at presintered LI group. When TPabvalues were compared
'2 & '2 & '2 i1=2
TPab= L*W − L*B + a*W − a*B + b*W − b*B within postsintered groups, no statistically significant difference was
detected among surface treatment methods (P > .05).
For topographical data, the surfaces of specimens were scruti- In accordance with Weibull distribution, highest m-value was
nized under field emission scanning electron microscope (FESEM) obtained with the control group. Among the treated groups,

T A B L E 1 Mean values for flexural strength (σ), Weibull characteristic strength (σ 0), and Weibull modulus (m) of specimens underwent to
different surface treatment procedures including air-borne particle abrasion (APA), grinding (G), and laser irradiation (LI)

Flexural strength (μm) Weibull parameters

Test groups Mean SD Group m 95% confidence interval σ0 95% confidence interval
Control 903.58 67.71 a 15.44 11.67-19.16 934.2 914.54-954.34
APA Pre-S 612.17 58.26 b 12.24 8.53-15.65 637.6 624.51-651.39
Post-S 1235.46 211.46 c 6.31 5.81-8.44 1332.03 1227.07-1452.57
G Pre-S 865.65 114.91 a 8.23 6.35-10.56 917.9 880.74-957.86
Post-S 983.45 149.72 d 7.53 5.16-9.78 1046.8 1010.8-1085.06
4 W LI Pre-S 897.78 81.92 a 12.35 8.63-15.76 935.3 906.7-965.52
Post-S 971.4 182.82 d 6.28 5.51-8.36 1043.3 1017.42-1070.4
KURTULMUS-YILMAZ ET AL. 85

T A B L E 2 Mean values for color

ΔE00 TPab
difference (ΔE00) and translucency
parameter (TPab) of specimens subjected Test groups Mean SD Statistical group Mean SD Statistical group
to different surface treatment
Control x x x 12.94 0.32 a
procedures including air-borne particle
abrasion (APA), grinding (G), and laser APA Pre-S 3.1 1.02 a 13.72 0.49 b
irradiation (LI) Post-S 2.3 0.87 b 12.68 0.54 a
G Pre-S 1.7 1.13 b 13.59 0.45 c
Post-S 1.6 0.49 b 12.82 0.49 a
4 W LI Pre-S 5.3 1.1 c 14.84 0.39 d
Post-S 1.4 0.35 b 12.7 0.43 a

including microretentive grooves and crevice formations which were

more remarkable in presintered group.

4 | DISCUSSION

Conditioning the surface of zirconia restorations is important to

FIGURE 2 Weibull distribution of all experimental groups
presintered LI group demonstrated superior reliability (m = 12.4),
followed by presintered APA, presintered grinding, postsintered grind-
ing, postsintered LI, and postsintered APA, respectively. Weibull
graphs are depicted in Figure 2. The representative FESEM micro-
graphs of all groups are shown in Figures 3–5. The specimen from
control group showed a typical untreated zirconia surface. An
increased surface irregularity for all treated specimens was detected.
Grinding group exhibited scratch-like formations parallel to the propa-
gation direction of grinder. Deeper scratches were observed in
presintered grinding group. LI specimens distinctively revealed blister-
like globules with micro-crevices. Diameters of the globules were
smaller in presintered LI group. This caused a more porous surface
topography. APA specimens demonstrated an irregular pattern
obtain a higher bonding strength between luting cement and inner
surface of restoration. Surface treatment procedures are generally
applied after sintering process of zirconia which may promote phase
transformation42 and microcracks43,44 leading a decrease in reliability
of material.35,43 Treating the zirconia surface before sintering process
has been reported to provide rougher surfaces31,43,45 and higher bond
strength values when compared to postsintering application.35,43
Since the studies that evaluated the mechanical and optical properties
of zirconia subjected to surface treatment before sintering is very lim-
ited, current study was conducted.
In the present study, surface treatments applied to the zirconia
specimens in presintering stage increased the TPab value and
decreased the flexural strength. Same surface treatments carried out
at the post sintering stage exhibited no influence on TPabvalue; while
increased the flexural strength. Moreover, lower ΔE00 values were
detected in specimens subjected to surface treatments in post-
sintering stage. Therefore, the null hypothesis was rejected.
APA is one of the most widely used protocol for modifying the
surface topography of zirconia prior to cementation.29 It functions by
removing loose contaminated surface, forming microretentive
grooves, enlarging effective contact surface, and enhancing wettabil-
ity on the intaglio surface of zirconia.11,22,27,29,34,38 Different types of
particles ranging between 25- and 250-μm can be used for hitting the
surface at high speed.9,22,38 Moon et al suggested that APA con-
ducted in presintering stage is a reliable surface treatment that
improves bond strength without compromising flexural strength.35
However, this is not consistent with the present study. It is proved
that heat treatment, such as sintering, after APA diminished the
extent of the flaws, also known as crack precursors, smoothened
sharp crevices, and decreased the amount of relative monoclinic
phase.9,33,35 However, heat treatment is not the only factor indirectly
affecting the flexural strength of zirconia. Despite of these favorable
effects, the influence of abrasives on presintered and postsintered
86 KURTULMUS-YILMAZ ET AL.

FIGURE 3 Representative photomicrographs of control and air-borne particle abraded groups (original magnification ×1000, ×10 000)

FIGURE 4 Representative photomicrographs of presintered and postsintered grinding groups (original magnification ×1000, ×10 000)

zirconia layer can be dissimilar in terms of surface hardness.33 The strength. This is in agreement with previous studies33,46 and can be
findings of current study showed that the APA protocol performed linked to transformed zone depth. It has been documented that APA
before the sintering process had an unfavorable effect on the flexural with 110-μm Al2O3 particles removes 60-μm of the ceramic.47
KURTULMUS-YILMAZ ET AL.
FIGURE 5 Representative photomicrographs of presintered and postsintered 4 W LI groups (original magnification ×1000, ×10 000)
Principally, using bigger (110-μm) abrasive particles increases the
depth of transformed zone, the content of monoclinic phase (t ! m
transformation) in the subsurface layer, tendency to propagate micro-
cracks, and finally decreases flexural strength.9,33,48 Although the
amount of monoclinic phase is decreased to a negligible level after
sintering48; it is thought that a deeper transformed zone may be
formed in presintered soft zirconia and it is a fact that this may endan-
ger the flexural strength.33 This hypothesis was reinforced with the
aid of FESEM micrographs as specimens abraded prior to sintering
exhibited rougher surfaces including deeper pits and sharpen crevices.
Although it is thought that this may be prevented by decreasing the
particle size, another study conducted by Karakoca and Yılmaz has
shown that small size abrasives cannot produce sufficient surface
roughness for micromechanical interlocking.49 Kosmac et al reported
that APA with 110-μm Al2O3 particles after sintering caused micro-
cracks in the surface of zirconia ceramic, but these microcracks did
not exceed the compressive layer as the phase transformation arising
from APA was able to neutralize their propagation.50 This is in accor-
dance with the present study.
Grinding is another popular surface treatment for improving bond
strength of zirconia to resin cements.3,8 It is also common during clini-
8
cal adjustment of restorations and functions by increasing surface
46
roughness for mechanical interlocking. Despite being easy to apply
in dental practice, excessive grinding tends to form surface micro-
cracks that act as crack initiation sites and thereby, degrade flexural
87
strength and reduce reliability.30,50 Additionally, stress and heat gen-
erated locally during this process may trigger reverse phase transfor-
mation on the zirconia surface, and adversely affect the mechanical
success of zirconia.1,7,8,50 However, as already extensively docu-
mented in the literature, adequate amount of controlled-grinding with
diamond burs under constant water-cooling enhances mechanical
properties of the material.7,18 This statement is compatible with the
present study. When compared with the mean flexural strength values
of the control group, it was observed that the value of presintered
grinding group was lower. However, the difference between two
groups was not statistically significant (P < .05). According to the
results of this study, it can be asserted that the grinding process per-
formed in the presintering stage has no detrimental effect on the flex-
ural strength values of the specimens. In the postsintering stage, it
enhanced the flexural strength significantly (P > .05). These findings
can be correlated with transformation-toughening capability.18
Different laser systems including erbium-doped yttrium aluminum
garnet (Er:YAG), carbon dioxide (CO2), femtosecond lasers (Ti-sap-
phire, Yb-dobed), neodymium-doped yttrium aluminum garnet (Nd:
YAG), and Er,Cr:YSGG laser can be used to irradiate the surface
topography of zirconia.3,5,22,30 Er,Cr:YSGG laser system that removes
inorganic substance from the surface with the aid of micro-explosions
and vaporization was used as a surface treatment in this study.22
According to the results, LI presented no influence on the flexural
strength of presintered specimens. Contrary, LI conducted at
88
postsintering stage exhibited improvements in flexural strength. This
finding may be explained by the preservation of the monoclinic phase
by minimizing the heat increase as a result of conducting irradiation
9
under constant water-cooling. Ghasemi et al suggested 3 W Er,Cr:
YSGG LI as an alternative surface treatment for zirconia after sintering
process.51 Another study by Saade et al proved that Er,Cr:YSGG LI
with a 5.5 W power-output enhanced the bonding ability to zirco-
11
nia. As high laser-power settings may lead to overheating and
undermine zirconia's structural properties, irradiation time and power-
output of lasers should be well-considered.9,52 Although 2-3 W power
output is strongly recommended for bilayer zirconia restorations5;
higher but not detrimental power output should be preferred for
monolithic restorations as laser energy is transmitted through ceramic
in accordance with thickness of the mass. This hypothesis was
reinforced with the aid of a study as reported that the highest flexural
strength value was detected in zirconia specimens irradiated by 4 W
Er,Cr:YSGG laser.46 Accordingly, same laser parameters were used in
this study.
For the assessment of structural reliability of a material, Weibull
analysis is used. Higher Weibull modulus leads to a structural superi-
ority and greater reliability. 46
Moreover, Weibull moduli of manifold
ceramics are in the range from 5 to 15. 53
In accordance with the
results of this study, the Weibull moduli of all test groups were found
within the range of reliability. Although all postsintered groups pres-
ented lower m-value than control group, they exhibited higher σ and
σ 0 values than control group. This is also consistent with previous
studies that presented lower m-value but higher σ value for APA
48,50
group.
According to the pairwise comparisons, it seems that APA at post-
sintered stage is more capable of making micromechanical roughening
and presenting higher flexural strength values, which is in agreement
9
with a previous study. A possible explanation for this superiority can
be a compressive layer that forms as a result of transformation-
toughening and significantly decelerates crack propagation.8 Unlike
presintered APA group, all postsintered groups exhibited superficial
depressions as detected in FESEM micrographs and hence a remark-
able increase in flexural strength of zirconia.
Translucency of a material can be defined as the numerical equiva-
lent of relative light transmission, and is completely associated with
the interaction between the material and the incident light.2,12 Con-
trast ratio, transmittance, and translucency parameter can be pre-
ferred for the quantitative measure of translucency.2 Translucency
parameter has been selected in the current study and the material has
been defined as opaque when the TPabvalue is closing to zero. Since
the light scattering coefficient of zirconia is more than the light
absorption coefficient, the incoming light is scattered. The light scat-
tering is inversely proportional to translucency and is closely related
to the particle size of the mass.12 Material with a larger particle size
produces fewer grain boundaries, leading to an increase in translu-
cency. 25
In order to achieve standardization for the measurements of
translucency, single type of zirconia ceramic has been used. However,
increase in particle size may result in an increase in the number of
micropores and adversely affect the mechanical properties of the
KURTULMUS-YILMAZ ET AL.
mass by increasing tendency to transformation.12,25 Particle size is
dependent on zirconia brand, sintering temperature, and dwelling
time.2,12 It has been reported in several studies that higher sintering
temperatures not only influence particle size, but also cause uneven
disintegration of yttria content within material. This results in
increased cubic phase in the composition which leads to a decrease in
flexural strength.25 Therefore, the specimens used in this study were
sintered at 1450! in accordance with the manufacturer's recommen-
dation. Importantly, in this study, TPab values of only presintered
groups increased. This can be correlated with surface roughness since
the surfaces of the presintered specimens are not as smooth as the
postsintered ones. If the surface texture of a mass is smooth, the
incoming light is reflected into a single outgoing direction by pre-
senting equal angles of reflectance and incidence. This phenomenon
is known as specular (mirror-like) reflection and deteriorates translu-
cency of the mass.54 Supportively, a study conducted by Wang et al
reported that higher reflectance, lower transmittance, and lower TPab
values were detected at smoother surfaces.55 However, the surface
texture was evaluated on SEM images in this study. Findings should
be strengthened by surface roughness test. Not only surface texture
but also thickness of the mass can influence TPabvalue as decreasing
thickness increases translucency.56 This may be the reason why the
presintered groups offer higher TPab values. As expectedly, surface
treatments performed in presintering stage allow the removal of more
material from the surface.33 This decreases the total thickness of the
mass, and thereby increases TPabvalue significantly.
ΔE is the term used to define the numerical distance between two
colors. Mathematically, ΔE less than 0.8 gives imperceptibility, ΔE
ranging from 0.8 to 1.8 gives clinically acceptability; while ΔE greater
than 1.8 gives clinically unacceptable color change.39 Instead of using
CIELAB formula which lacks perceptual uniformity,57 CIEDE2000 was
preferred in order to calculate ΔE in the present study. This revised
formula introduced parametric constant coefficients as environmental
corrections and weighting functions as positional corrections, thus
enhancing the performance for blue and grey colors.57,58 Especially RT
function is added to reduce the interaction between chroma and hue
in blue area.57 Moreover, this complex formula is more accurate and
represents an ellipse for color difference, unlike CIELAB. This ellipse
has a major axis in the way of saturation and thereby corresponds bet-
ter with the nature of human color perception.59 With respect to ΔE
data, only a statistically significant difference was observed among
the ΔE values of test groups in presintering stage. Again, this can be
attributed to the surface smoothness and thickness of the mass that
can cause alterations in ΔE values in presintering stage.33,55,56
The current study has several limitations. The oral cavity condi-
tions that can aggravate grinding-induced surface flaws and initiate
low-temperature degradation were not simulated, only three surface
treatments were compared, one size of APA particles was used, TP00
formula which would create difficulty to compare results with previ-
ous studies was not preferred, and fractography was not performed.
Further studies need to be conducted.
KURTULMUS-YILMAZ ET AL.
5 | CO NC LUSIO NS
Within the scope of this comparative study, following consequences
were drawn: (a) surface treatments performed at postsintering stage
had a favorable effect on the flexural strength of all specimens,
(b) although APA group at presintering stage demonstrated lowest
flexural strength among others; same group exhibited highest flexural
strength at postsintering stage, (c) G and LA treatments performed at
presintering stage did not detrimentally affect flexural strength values.
On the other hand, same treatments at postsintering stage lead to
superior flexural strength values. (4) Surface treatments performed in
presintering stage had a favorable effect on translucency parameter
of all specimens. There was no statistically significant influence of sur-
face treatments on translucency parameter at postsintering stage,
(e) higher ΔE values were detected for all groups in presintering stage.
CONF LICT OF IN TE RE ST
Authors have no conflict of interest.
ORCID
Sevcan Kurtulmus-Yilmaz https://orcid.org/0000-0001-8792-1977
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How to cite this article: Kurtulmus-Yilmaz S, Önöral Ö,
Aktore H, Ozan O. Does the application of surface treatments
in different sintering stages affect flexural strength and optical
properties of zirconia? J Esthet Restor Dent. 2020;32:81–90.
https://doi.org/10.1111/jerd.12552