d e n t a l m a t e r i a l s 3 0 ( 2 0 1 4 ) e419–e424

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Effect of changes in sintering parameters on

monolithic translucent zirconia

Kamal Ebeid a,b,∗ , Sebastian Wille a , Amina Hamdy b , Tarek Salah b ,

Amr El-Etreby b , Matthias Kern a
a Department of Prosthodontics, Propaedeutics and Dental Materials, School of Dentistry, Christian-Albrechts
University at Kiel, Germany
b Department of Fixed Prosthodontics, Faculty of Dentistry, Ain Shams University, Egypt

a r t i c l e i n f o a b s t r a c t

Article history: Objectives. Aim of this study was to evaluate the effect of different sintering parameters on
Received 6 February 2014 color reproduction, translucency and biaxial flexural strength of monolithic zirconia.
Received in revised form Methods. Translucent zirconia discs having 15 mm diameter, 1 mm thickness, and shade
15 June 2014 A3 were milled and divided according to the sintering temperatures (1460 ◦ C, 1530 ◦ C, and
Accepted 5 September 2014 1600 ◦ C) into three groups (n = 30). Each group was later divided into three subgroups (n = 10)
according to the sintering holding time (1, 2, and 4 h). Easyshade spectrophotometer (Vita,
Bad Säckingen, Germany) was used to obtain the E between the specimens and the shade
Keywords: A3. Mean E values below 3.0 were considered “clinically imperceptible”, E values between
Dental materials 3.0 and 5.0 were considered “clinically acceptable” and E values above 5.0 were considered
Ceramics “clinically unacceptable”. Contrast ratio (CR) was obtained after comparing the reflectance
Zirconia of light through the specimens over black and white background. Biaxial flexural strength
Biaxial flexural strength was tested using the piston-on-three balls technique in a universal testing machine.
Translucency Results. Mean E results ranged from 4.4 to 2.2. Statistically significant decrease in the Delta
E was observed as the sintering time and temperature increased. CR decreased from 0.75 to
0.68 as the sintering time and temperature increased. No significant change in the biaxial
flexural strength was observed.
Significance. Sintering zirconia using long cycles and high temperatures will result in reduc-
tion of E and CR. Biaxial flexural strength is not affected by changes in the evaluated
sintering parameters.
© 2014 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

[1]. Zirconia restorations became very popular due to their

1. Introduction unique mechanical properties which made it possible to use
them in long span restorations [2,3]. Zirconia is polymor-
All ceramic restorations have proved to be a promising alter- phic in nature and exists in three forms: cubic, tetragonal,
native to metal-ceramic restorations mainly due to their and monoclinic. At room temperature zirconia is present in
excellent esthetics, chemical stability, and biocompatibility its monoclinic form and is stable up to 1170 ◦ C. Above this

∗
Corresponding author at: Department of Prosthodontics, Propaedeutics and Dental Materials, School of Dentistry, Christian-Albrechts
University at Kiel, Germany. Tel.: +20 1006084044.
E-mail address: kebeid@proth.uni-kiel.de (K. Ebeid) .

http://dx.doi.org/10.1016/j.dental.2014.09.003
0109-5641/© 2014 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.
e420 d e n t a l m a t e r i a l s 3 0 ( 2 0 1 4 ) e419–e424

temperature a transformation occurs to the tetragonal phase thickness of 1 mm, and shade A3 were milled and divided
that is stable up to 2370 ◦ C. Beyond this temperature, zirconia into three groups (n = 30) according to the sintering hold-
assumes its cubic form [4]. ing time (1, 2, and 4 h). Each group was later divided into
Zirconia restorations are fabricated either in a partially three subgroups (n = 10) according to the sintering temperature
sintered state by soft machining followed by a final sinter- (1460 ◦ C, 1530 ◦ C, and 1600 ◦ C). All specimens were sintered as
ing cycle, or they are fabricated in a fully sintered state by milled in the manufacturers sintering furnace (Bruxzir Fast-
hard machining [5,6]. Hard machining may induce tetragonal- Fire, Glidewell, Frankfurt, Germany) at a heating and cooling
monoclinic transformation, introduce cracks, and wears the rate of 10 ◦ C per minute. The temperature was controlled using
milling hardware at a higher rate. Soft machining however is the furnace’s internal thermometer.
much easier, but may produce less accurate frameworks due to
the sintering shrinkage accompanied with the final sintering 2.1. Color evaluation
process [7].
The phenomenon of light scattering largely affects the Specimens were placed over a neutral gray background
translucency of dental ceramics. If the majority of light pass- (CIE L* = 62.1, a* = 1.3, b* = −0.02) and the CIELAB coordinates
ing through a ceramic is scattered, the material will appear were measured for each specimen using a spectrophotome-
opaque. However, if most of the light passing is transmitted ter (Easyshade compact, Vita Zahnfabrik, Bad Säckingen,
through the ceramic it will appear translucent [8]. The amount Germany). The Easyshade was set to the restoration mode
of light that is absorbed, transmitted, and reflected mainly and the shade A3 was selected. In this mode the color dif-
depends on the microstructure of the ceramic itself [9,10]. ference is determined by comparing the selected shade and
Differences in perceived color (E) can be determined the measured shade. For each specimen three measurements
using the CIELAB coordinates. The CIELAB system has pro- were taken at the center and their average was recorded.
vided a quantitative representation of color and it has been After each specimen was measured the Easyshade was recal-
extensively applied in dentistry to study esthetic materials, ibrated. Mean E values below 3.0 were considered “clinically
shade guides, and color reproductions [11–13]. The percep- imperceptible”, E values between 3.0 and 5.0 were considered
tibility and acceptability thresholds of the E vary widely “clinically acceptable” and E values above 5.0 were consid-
in literature mainly due to the diversity of observers, objec- ered “clinically unacceptable”.
tives, and methodologies among the studies [14,15]. Clinically
the tooth, restorations available, surrounding, and blending 2.2. Translucency evaluation
effect tend to expand the clinically acceptable range pre-
viously reported [16,17]. The mean E values as “clinically A quantitative measurement of translucency was obtained
imperceptible” (E < 3), “clinically acceptable” (E between 3 by measuring the CIELAB coordinates of the specimens after
and 5) and “clinically unacceptable” (E > 5) seem to be consis- backing with a white (CIE L* = 96.7, a* = 0.1, b* = 0.2) and black
tent with the clinical practice considering a non-color expert, (CIE L* = 10.4, a* = 0.4, b* = 0.6) background using the spec-
which usually is the patient’s condition [11,18,19]. trophotometer. For each specimen three measurements were
In order to overcome the main disadvantage of zirco- taken and their average was recorded. The contrast ratio (CR)
nia which is its opacity, the zirconia core is veneered with for each specimens was calculated according to the follow-
veneering porcelain to enhance its esthetics. However, the ing equation: CR = Yb /Yw where Y = [(L + 16)/116]3 × 100 and Yb
most common mode of failure that faced clinicians was the is the reflectance over a black background and Yw is the
chipping of this veneering porcelain while the zirconia core reflectance over a white background [8,11]. In all calculations
remained unaffected [20,21]. “0” is considered the most transparent and “1” is considered
The differences in sintering parameters of zirconia can the most opaque.
directly affect its microstructure and properties [22]. The
extent of this effect have become of interest in the field of 2.3. Surface roughness evaluation
dental research especially after the introduction of short sin-
tering cycles by manufacturers. Several authors have studied All specimens were cleaned ultrasonically in 99% isopropanol
the effect of the changes in sintering time and temperature on solution for 3 min and then dried with air. The average sur-
the translucency, grain size, and biaxial flexural strength of zir- face roughness (Ra) for the specimens was measured using
conia core ceramics; however the effect of these changes on a 3D laser scanning microscope (Keyence VK-X100, Keyence
the properties of monolithic nanozirconia remains in question GmbH, Neu-Isenbuerg, Germany). The wavelength of the laser
[10,23–25]. was 658 nm. Three separate areas were measured on each
The aim of this study was to evaluate the effect of specimen, the measured area was 500 ␮m × 750 ␮m and the
using different sintering times and temperatures on the color distance between the separate scans was over 3 ␮m. The mean
reproduction, translucency, surface roughness, biaxial flex- Ra for each specimen was later recorded.
ural strength, and the surface hardness of monolithic zirconia
ceramic. 2.4. Microstructure analysis

2. Materials and methods Three specimens were selected randomly from each sub-
group for X-ray diffraction (XRD) surface analysis to detect
Ninety translucent shaded zirconia ceramic discs (Bruxzir, the amount of tetragonal and monoclinic phases available.
Glidewell, Frankfurt, Germany) with a diameter of 15 mm, a The specimens were placed in the holder of a diffractometer
 d e n t a l m a t e r i a l s 3 0 ( 2 0 1 4 ) e419–e424 e421

Fig. 1 – Piston-on-three balls biaxial flexural strength test.

(Seifert XRD 3000 PTS, GE GmbH, Munich, Germany) and sub-

jected to Cu K␣ radiation. The spectrum was recorded within
the range of 20–40◦ , a step size of 0.02◦ and a scan time per Fig. 2 – Biaxial flexural strength of subgroups sintered
step of 10 s. Voltage and current were set to 40 kV and 40 mA. using different sintering times and temperatures.
One specimen from each subgroup was cleaned, dried, gold
sputter coated (Bal-Tec SCD 050, Leica Mircosystems, Wet-
zlar, Germany) and examined under 10,000× magnification 2.6. Vickers hardness evaluation
using a scanning electron microscope (XL 30 CP, Philips, Sur-
rey, England) to calculate the average grain size using a base A piece from each broken specimen from each subgroup was
of at least 150 grains. randomly selected and tested for Vickers hardness using an
indentation tester (ZHV10, Zwick, Ulm, Germany). An inden-
tation was made on each specimen under a loading mass of
2.5. Biaxial flexural strength testing
5 kg and dwell time of 10 s. The diagonal length was mea-
sured using an optical microscope (20×) and the hardness was
Specimens were tested for biaxial flexural strength using
calculated from the following equation [26,27]:
piston-on-three ball technique in a universal testing machine F
(Zwick Z010, Zwick, Ulm, Germany). A 10 mm diameter metal- VHN = 1.8544 ×
lic platform was constructed, above which rested three 3.2 mm d2
diameter steel balls that were equidistant from each other. where VHN is the Vickers hardness number, F is the applied
Each disk was placed centrally on the steal balls and load load expressed in kg, and d is the mean length of the diagonals
was applied by a piston of 1.4 mm diameter and 0.5 mm/min of the indentation (mm).
crosshead speed using the universal testing machine (Fig. 1).
The fracture load for each specimen was recorded and the 2.7. Statistical analysis
biaxial flexural strength was calculated using the following
equation: The data collected was checked for normal distribution and
analyzed using two-way analysis of variance (ANOVA), fol-
−0.2387P(X − Y) lowed by Tukey’s HSD test (SPSS v20, Chicago, IL, USA) at a
S=
d2 significance level of P ≤ 0.05 to determine the effect of the
changes in sintering time and temperature on each of the
where: S, biaxial flexural strength (MPa); P, fracture load (N); d,
variables tested.
specimen disk thickness at fracture origin (mm). X and Y were
determined as follows:
3. Results
 r2 2  1 −    r2 2
X : (1 + ) ln +
r3 2 r3 Regarding the color evaluation, two-way ANOVA revealed sig-
nificant differences in the E between the subgroups when
  r1 2   r1 2 sintered using different sintering temperatures and times
Y : (1 + ) 1 + ln + (1 − ) (P ≤ 0.05). Tukey’s HSD tests revealed that there was a sig-
r3 r3 nificant decrease in the E as the sintering temperature
increased. It also revealed that there was no significant dif-
 is Poisson’s ratio (0.25), r1 is the radius of the support ference in the E between the 2 and 4 h sintering holding
circle, r2 is the radius of the loaded area, and r3 is the radius times however, both showed a significant decrease when
of the specimen. compared to the 1 h sintering holding time (Table 1). None of
e422 d e n t a l m a t e r i a l s 3 0 ( 2 0 1 4 ) e419–e424

Table 1 – Mean E and standard deviation () of test Table 4 – Mean grain size in ␮m and standard deviation
groups sintered using different sintering times and () of test groups sintered using different sintering times
temperatures. and temperatures.
Sintering temperature/◦ C Sintering holding time/h Sintering Sintering holding time/h
temperature/◦ C
1 2 4
1 2 4
1460 4.4 (0.3)a 4.0 (0.1)d 3.8 (0.1)d
a d
1530 3.1 (0.1)b 2.8 (0.3)e 2.9 (0.1)e 1460 0.55 (0.10) 0.64 (0.11) 0.79 (0.15)d
1600 2.4 (0.1)c 2.2 (0.1)f 2.2 (0.1)f 1530 0.65 (0.13)b 0.77 (0.13)e 0.92 (0.25)e
1600 0.89 (0.19)c 1.0 (0.11)f 0.92 (0.14)f
Means with different superscript letters are significantly different
at the 95% confidence level. Means with different superscript letters are significantly different
at the 95% confidence level.

the subgroups showed any unacceptable color results, with the

sintering temperatures 1460 ◦ C and 1530 ◦ C subgroups show- Table 5 – Mean VHN and standard deviation () of test
ing clinically acceptable results and the sintering temperature groups sintered using different sintering times and
1600 ◦ C showing clinically imperceptible color results. temperatures.
Concerning translucency, two-way ANOVA revealed signif- Sintering Sintering holding time/h
icant differences in CR between the subgroups when sintered temperature/◦ C
with different sintering temperatures and times (P ≤ 0.05).
1 2 4
Tukey’s HSD tests revealed that there was a significant
1460 1456 (212)a 1504 (123)a 1497 (138)a
decrease in CR when comparing the sintering temperatures
1530 1553 (111)a 1548 (77)a 1437 (74)a
1460 ◦ C to the 1530 ◦ C and 1600 ◦ C. It also revealed that there
1600 1461 (108)a 1507 (71)a 1415 (60)a
was a significant decrease in CR when comparing the 1 and
Means with different superscript letters are significantly different
2 h sintering holding times to the 4 h (Table 2).
at the 95% confidence level.
As for the surface roughness measurements, the results
showed that there was a decrease in the mean Ra as the sin-
tering temperature and time increased, however this decrease Regarding microstructure analysis, all specimens analyzed
was not statistically significant. The highest mean Ra mea- using XRD showed only tetragonal ZrO2 phase character-
sured was with specimens sintered with a holding time of 1 h istics peaks. None of the samples showed any tetragonal-
at a temperature of 1460 ◦ C (1.030 ␮m) while the lowest mean monoclinic transformation. However, samples showed a
Ra measured was with the specimens sintered with a holding significant increase in the average grain size as the sintering
time of 4 h at a temperature of 1600 ◦ C (0.826 ␮m) (Table 3). temperature increased. Samples sintered at 2 and 4 h sintering
holding time also showed a statistically significant increase in
the average grain size when compared to samples sintered at
a 1 h sintering holding time (Table 4).
Table 2 – Mean CR and standard deviation () of test
The mean biaxial flexural strength of subgroups ranged
groups sintered using different sintering times and
temperatures. from 906 MPa to 1000 MPa. However, there was no statistically
significant difference between subgroups (Fig. 2).
Sintering Sintering holding time/h
The mean Vickers hardness of subgroups ranged from
temperature/◦ C
1437 to 1553 VHN. Again, there was no statistically significant
1 2 4 difference between the subgroups concerning their surface
1460 0.75 (0.02) a
0.75 (0.03)a
0.71 (0.01)c hardness (Table 5).
1530 0.72 (0.01)b 0.71 (0.01)b 0.69 (0.01)d
1600 0.71 (0.01)b 0.70 (0.01)b 0.68 (0.01)e
4. Discussion
Means with different superscript letters are significantly different
at the 95% confidence level.
The use of the Vita Easyshade spectrophotometer to measure
color and translucency by assessing the CIELAB coordinates of
Table 3 – Mean Ra and standard deviation () of test specimens is widely used in the field of dental research [12,14].
groups sintered using different sintering times and Spectral reflectance which is used in this study together with
temperatures. direct transmission and total transmission are the three ways
Sintering Sintering holding time/h used to measure translucency [28]. We calculated the contrast
temperature/◦ C ratio which was used by several authors to obtain a quanti-
tative measure of translucency [8,29,30]. Our results showed
1 2 4
that there was a decrease in the E from 4.4 to 2.2 and the
1460 1.030 (0.190)a 1.023 (0.164)a 0.991 (0.198)a
contrast ratio from 0.75 to 0.68 as the sintering temperature
1530 1.026 (0.304)a 0.878 (0.215)a 1.069 (0.086)a
and time increased. This could be attributed to the assump-
1600 0.898 (0.191)a 0.957 (0.242)a 0.826 (0.161)a
tion that the sintering process reduces the pores between the
Means with different superscript letters are significantly different
grains and increases the final density of zirconia, thus produc-
at the 95% confidence level.
ing less light scattering and more light transmission leading
 d e n t a l m a t e r i a l s 3 0 ( 2 0 1 4 ) e419–e424 e423

to better translucency and optical characteristics [31]. This A limitation of this study is that only one brand of zirconia
assumption was consistent with our results as increasing the was investigated. The results may not apply for other brands
sintering temperature and time led to an increase in the aver- of monolithic nanozirconia thus other brands may require
age grain size of zirconia. Also the increase in the sintered further investigations. In addition, the effect of aging was not
density of the zirconia may lead to a more uniform crystalline investigated in our study and therefore also requires further
arrangement thus promoting better specular reflection, light investigation.
transmission and a better perception of color.
Concerning the contrast ratio, our results were similar to a
study performed by Jiang et al. [24], where sintering tempera- 5. Conclusions
tures 1350 ◦ C, 1400 ◦ C, 1450 ◦ C, and 1500 ◦ C were used and their
effect on the translucency of zirconia core discs was measured. On the basis of the results and condition of this study, the
They concluded that as the sintering temperature increased following conclusions can be drawn:
the translucency of the discs increased. Our results were also
in agreement with Stawarczyk et al. [25] as they concluded 1. Increasing the sintering temperature and time will lead to
that there was a decrease in the CR of regular zirconia core enhanced color reproduction and translucency of shaded
material specimens having 0.5 mm thickness from 0.85 to 0.70 monolithic nanozirconia ceramic.
as the sintering temperature increased from 1300 to 1700 ◦ C. 2. There is a direct relation between zirconia grain size and
A non-contact laser profilometer was used in this study as the sintering temperature and time.
there were questions regarding the accuracy of contact pro- 3. Changing the sintering parameters within the selected
filometry with assumptions saying that they underestimate range will not cause any tetragonal-monoclinic phase
the surface roughness thus present a smoother surface [32]. transformation of zirconia ceramic.
Since we had no significant differences between the subgroups 4. Changing the sintering parameters within the range
regarding the surface roughness, we can assume the fact that selected will have no effect on the surface roughness, biax-
the reduction in the pores between the grains is not enough to ial flexural strength, and surface hardness of monolithic
produce a significant difference, we can also assume the fact nanozirconia ceramic.
that the changes in the contrast ratio and E are mainly due to
changes in the microstructure rather than changes in surface
morphology. Acknowledgments
Simulating pure bending and preventing edge loss can be
achieved best using the piston-on-three ball technique for The authors wish to express appreciation for technical assis-
testing the biaxial flexural strength, as the specimens in this tance and laboratory support of Frank Lehmann, Detlev
technique are resting on the stainless steel ball which form a Gostomsky, and Rüdiger Möller, of Department of Prosthodon-
smaller diameter than the specimen itself [33,34]. In our study tics, Propaedeutics and Dental Materials, School of Dentistry,
there was no effect on the biaxial flexural strength as the sin- Christian-Albrechts University at Kiel and also Prof. Klaus
tering parameters changed. Our results are in agreement with Rätzke from the Institute of Materials Science, Christian-
the results of a study conducted by Hjerppe et al. [35], who Albrechts University at Kiel.
used different rising and holding times for sintering zirconia. This study was supported by Glidewell, Frankfurt, Germany
Stawarczyck et al. [25] also found no significant differences in which provided the materials used.
the biaxial flexural strength of zirconia core material when the
sintering temperature was raised from 1400 ◦ C to 1550 ◦ C, how- references
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below these temperatures. In a similar study by Jiang et al.
[24], they concluded that raising the sintering temperature
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