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The effect of heat treatments applied to superstructure porcelain on the

mechanical properties and microstructure of lithium disilicate glass ceramics

Article  in  Dental Materials Journal · April 2017

DOI: 10.4012/dmj.2016-365

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 Dental Materials Journal 2017; : –

The effect of heat treatments applied to superstructure porcelain on the

mechanical properties and microstructure of lithium disilicate glass ceramics
Hatice ÖZDEMİR and Alper ÖZDOĞAN

Faculty of Dentistry, Prosthodontics Department, Atatürk University, 25240 Erzurum, Turkey

Corresponding author, Hatice ÖZDEMİR; E-mail: dentist_hatice@hotmail.com

The aim of this study was to investigate that heat treatments with different numbers applied to superstructure porcelain whether
effects microstructure and mechanical properties of lithium disilicate ceramic (LDC). Eighty disc-shaped specimens were fabricated
from IPS e.max Press. Specimens were fired at heating values of porcelain in different numbers and divided four groups (n=5). Initial
Vickers hardness were measured and X-ray diffraction (XRD) analysis was performed. Different surface treatment were applied
and then Vickers hardness, surface roughness and environmental scanning electron microscopy (ESEM) analysis were performed.
Data were analyzed with Varyans analysis and Tukey HSD test (α=0.05). Initial hardness among groups was no significant different
(p>0.05), but hardness and surface roughness after surface treatments were significant different (p<0.05). Lithium disilicate
(LD) peaks decrease depended on firing numbers. ESEM observations showed that firing number and surface treatments effect
microstructure of LDC. Increasing firing numbers and surface treatments effect the microstructure of LDC.

Keywords: Lithium disilicate glass ceramic, Heat treatment, Microstructure, Mechanical properties

Some studies have shown that changes may occur

INTRODUCTION
Glass ceramics are the materials arousing interest in
restorative dentistry because of their excellent aesthetic
properties and biocompatibility1-3). These ceramics are
obtained by formation and solid state reaction from
SiO2-Li2O-Al2O3-K2O-ZrO2-P2O5 system2,4-6). LDC are
composed of needle-like LD crystals at the rate of about
70% impacted in the glass matrix containing SiO2, K2O,
MgO, Al2O3, P2O5 and other oxides2,4-7). LD crystals
which are interpenetrated and reinforced in the layered
structure have a length of 3–6 µm and a width of 0.5–0.8
µm8,9).
Due to their excellent mechanical properties,
LDCs have been increasingly used not only in veneers,
inlays, onlays and anterior single crowns but also
in posterior crowns and bridges7,10). The mechanical
properties of LDC play an important role in the success
of restorations. Studies are carried out to understand
the mechanical properties of LDCs such as micro and
nano dimensions9,11) fatigue12) and wear properties13).
Understanding and improving the mechanical properties
of LDCs can further improve the clinical applicability14).
These glass ceramics can only be fused by the
crystallization of a base glass that uses nucleation in
the hot application program in a conventional furnace,
and the crystal growth. This process should be carried
out at atmospheric pressure and restricted to the typical
maximum value in a furnace, the degree of which can
suddenly increase (5–30ºC/min)15).
Materials with different phases such as leucite-
reinforced glass ceramics should be extremely carefully
processed because their phases will react differently
throughout the heat application16-18). This situation
requires the thermal scheme of the conditions
encountered for the structural balance between phases.
in crystals, even in crystals that make up the main
structure depending on the dose applied19,20). Studies
have shown that routine laboratory thermal processing
such as glaze could be associated with the structural
and mechanical changes that reduce the fracture
strength of the ceramic material21-25). Therefore, these
thermal processes should be taken into account when
an attempt to estimate the long-term success of the
restoration is made26). In simple cases, superstructure
porcelains usually undergo 2–5 successive firings. The
fixed prosthetic restorations may sometimes need to be
fired more than normal due to several reasons such as
the change of the color, optimizing the aesthetics and
the requirement of porcelain addition. During these
operations, the substructure material is exposed to the
same heat treatment along with the superstructure
porcelain. In particular, it is necessary to know the
changes that may occur in the microstructure which
is caused by the excess firing of the materials with
different phases and how these changes would affect the
mechanical properties and clinical performance of the
material.
The external surface of dental restorative materials
must be polished and smooth; rough surfaces result
in decreased in flexural strength27), increased surface
staining on teeth due to the increased abrasion of
opposing tooth surfaces28) and the accumulation of
plaque and calculus29,30). In contrast with the external
surface of dental restorative materials, internal surface
of the restoration must be rough, as a rough surface
increases the bond strength of cement to the restoration.
Surface treatment to increase the roughness of the
internal surface is an imperative step for better
clinical performance of ceramic restorations31). Surface
treatments such as sandblasting and acid etching alter

Received Nov 7, 2016: Accepted Mar 14, 2017

doi:10.4012/dmj.2016-365 JOI JST.JSTAGE/dmj/2016-365
2 Dent Mater J 2017;
the surface topography by creating micro- and nano-scale
porosities of varying depth and width32). The resultant-
altered surface topography increases the surface area
for micromechanical bonding with resin cements33-35).
In the majority of the studies carried out, the effect
of different numbers of firing and pressing on the color,
surface roughness, hardness and microstructure of
LDCs has been examined. However, the possible effect
of the changes that may occur in the microstructure
of IPS e.max Press as a result of the heat treatment
applied to superstructure material on the mechanical
properties of LDCs has not been evaluated. The aim
of this study is to investigate whether changes occur
in the microstructural and mechanical properties of
LDC specimens fired at different heating values of
superstructure. The first hypothesis of our study is
that the firing process which is performed more than
normal would affect the hardness of the LDC. Our
second hypothesis is that the surface treatments applied
to LDC specimens which are fired more than normal
would affect the hardness and roughness. Our third
hypothesis is that changes would occur in the crystal
structure and size of the LDC specimens which are fired
more than normal as a result of the XRD analysis. The
changes that occur in the mechanical properties of IPS
e.max Press can be explained depending on the results
obtained from XRD.
MATERIALS AND METHODS
Preparation of the specimens
Eighty specimens were prepared in accordance with
the manufacturer’s instructions with the lost-wax
technique. The wax specimens with 10-mm-diameter
and 2-mm-thickness were taken to revetment, and the
revetment was exposed to pre-heat treatment at 850ºC
for 1-h after hardening. Following this heat treatment,
IPS e.max Press (Ivoclar Vivadent, Zurich, Switzerland)
ingots were pressed under pressure at 920ºC after 25
min of waiting time with 60ºC/min temperature increase
rate in EP 600 furnace in a way the initial temperature
was 700ºC. IPS e.max Press specimens extracted by
waiting for the cooling of the revetment were cleared by
sandblasting. The following procedures were applied by
dividing the obtained specimens into 4 groups.
Group 1: The obtained IPS e.max Press specimens
were exposed to heat treatment at a
temperature applied to the superstructure
porcelain without applying the
superstructure porcelain. They were first
exposed to the heat treatment applied
on the superstructure porcelain. These
processes; initial temperature is 403ºC;
temperature increase is 60ºC/min; final
temperature is 750ºC and waiting time is
6.5 min. The same specimens were then
subjected to the heat treatment which
is applied in the glazing process. These
processes; initial temperature is 440ºC;
temperature increase is 60ºC/min; final
: –
temperature is 740ºC and waiting time is
6.5 min. These processes were performed
considering the recommendations of the
manufacturer. These specimens fired in
normal number constituted the control
group.
Group 2: In addition to the heat treatments applied
in Group 1, the same heat treatments were
repeated 1 more time.
Group 3: In addition to the heat treatments applied
in Group 1, the same heat treatments were
repeated 2 more times.
Group 4: In addition to the heat treatments applied
in Group 1, the same heat treatments were
repeated 3 more times.
Ultimately, the specimens fired at the normal
heating values of superstructure porcelain and the
specimens fired 1, 2 and 3 times more than normal
were obtained. Specimens were prepared by the same
technician in the dental laboratory. A schematic
illustration of the present study is presented in Fig. 1.
Evaluation of the mechanical properties
1. Vickers hardness measurement
The initial Vickers hardness measurements of the LDC
specimens (n=5), which were fired at different heating
values of superstructure porcelain, the surfaces of which
were glazed with polishing and polishing discs were
performed. Hardness was measured using a Vickers
Microhardness tester (micromet 2001, Buehler, Bluff, IL,
USA) with a load of 9.8 N and dwell time of 20 s. A Vickers
diamond indenter was used for the measurement. The 2
indentation diagonals d1 and d2 created in the material
surface measured with the microscope on the hardness
tester36). The hardness traces were observed with an
optical microscope. The objective magnification was at
×100. The hardness measurement was performed from 3
different points of each specimen and the mean of three
replications was recorded as the HV value of the each
specimen. Then, hardness measurement was performed
again by applying different surface treatments to the
specimen. Likewise, each specimen was averaged by
measuring from 3 different points of them. The surface
treatments applied are as following:
Acid-etching: 9.5% hydrochloric acid was applied
for 20 s. Afterwards, the acid was removed by washing
with pressurized water for 20 s, and the specimens were
dried.
Co-Jet application: The silanized Al2O3 powder
in 30 µm size was applied at 1 cm distance and under
2.84 bar pressure from different angles for 15 s by one
person with a pencil point Co-Jet device. The specimens
were not washed in order not to damage the silanization
formed on the surface of specimens.
Sandblasting: Al2O3 powder in 50 µm size was
applied at 1 cm distance and under 2.84 bar pressure
from different angles for 15 s by one person with a pencil
point sandblasting device. Then, the specimens were
washed for 30 s and dried.
 Dent Mater J 2017;
Fig. 1 Schematic illustration of Vickers hardness and surface roughness tests.
2. Measurement of surface roughness
The specimens (n=5) which were fired at heating values
of superstructure porcelain in different numbers and
applied various surface treatments were used for
the measurement of surface roughness. The surface
roughness evaluation (Ra values) were made with a
profilometry (Surtronic 25, Taylor Hobson, Leicester,
UK) calibrated with a cut-off value (λc) of 0.80 mm, an
evaluation length of 4-mm. Three measurements of
surface roughness were performed for each specimen,
and the mean average Ra values were used for the
statistical analysis.
Statistical analysis
The data on Vickers hardness were subjected to
analysis of variance using the IBM SPSS 20.0 statistical
package (Chicago, IL, USA) according to a 4*4 (Surface
treatment*Number of firing) factorial design in five
replicates. Similarly, the data on surface roughness
were subjected to analysis of variance according to a
3*4 factorial design in five replicates. The interactions
between surface treatments and number of firing were
investigated in terms of both hardness values and surface
roughness values. The Tukey HSD multiple comparison
test was performed to determine the differences between
the group means which were identified as significant
from the analysis of variance. The level of statistical
significance was set at 0.05 for all analyses.
Evaluation of the microstructure
1. XRD
XRD was performed to characterize the LDC crystallize
structure after repeated firing protocols and to analyze
the effect of the firing protocols on the LDC crystallites.
A specimen from each group was analyzed by XRD
: – 3
(EMPYREAN, PANalytical, Lelyweg, The Netherlands),
using a wavelength of 1.5419 (Kα), scan range from 10º
to 85º, the step size of 0.0131º and scan speed of 0.067º/s.
CuKα radiation was used. Peaks were identified the
crystal phase using the ICDDS#40-0376 database.
Diffraction patterns for IPS e.max Press ceramic, LD
(01-082-2396), lithium silicate (00-015-0519) and lithium
phosphate (00-048-0956) were used.
The graphics of the XRD analysis data were created
using Origin Pro 8.1 software program. The mean
crystal size of the LD was identified at 24.4º which was
the largest peak it showed in each group and in 0 4 0
plane. Debye equation37) was used while calculating the
crystal size.
λ
T=0.9
βcosθ
T is the average size of the crystal, λ is X-ray
wavelength (1.5419 Ǻ), θ is the angle where the peak is
observed and β is FWHM (full width at half maximum)
in radian in the selected peak. The peak analysis was
also carried out using the Gaussian curve fitting with
Origin Pro 8.1 software.
2. ESEM analysis
The ESEM image was taken from IPS e.max Press
specimens which were fired in different numbers and
applied various surface treatments. The changes that
may occur in the microstructure of the specimen surface
in the same surface treatment after firing in different
numbers were evaluated. ESEM images were recorded
by being taken at ×10,000 magnification using ESEM
tomography electron microscope without the need for
coating the specimens. ESEM is a direct descendant
4 Dent Mater J 2017; : –

of the conventional SEM, but it also permits wet and
insulating samples to be imaged without prior specimen
preparation. A low gas pressure can be accommodated
around the sample. When this gas is water, hydrated
samples can be maintained in their native state.
Whether the gas is water or some other gas, ions formed
through collisions between electrons emitted from the
sample and the gaseous molecules drift back towards
the sample surface helping to reduce charge build up.
This eliminates the need for insulators to be subjected
to a conductive surface coating38).
RESULTS
Mechanical properties
Vickers hardness measurement results of IPS e.max
Press specimens are presented in Table 1. Vickers
hardness values between the groups were ranged in the
form of Group 4>Group 1>Group 3>Group 2, and it was
observed that the differences between the groups were
not statistically significant (p>0.05). The differences
between the hardness values which were measured
after applying the surface treatments were found to
be statistically highly significant (p<0.01). While the
specimens applied sandblasting showed the highest
hardness value, the specimens etched with acid showed
the lowest hardness value (p<0.01). Regarding the
sandblasted specimens, Group 1 showed the highest
hardness value, and Group 4 showed the lowest hardness
value. In the specimens applied Co-jet, Group 3 showed
the highest hardness value, and Group 1 showed the
lowest hardness value. In acid etching specimens, Group
4 showed the highest hardness value, and Group 2
showed the lowest hardness value. When we look at them
in general, the highest hardness value was observed
in the sandblasted specimens and the lowest hardness
value was observed in the acidified specimens.
The results of the analysis of variance which was
performed for the difference between hardness values are
presented in Table 2. According to the analysis results,
while the differences between the values measured as
a result of the surface treatments were statistically
significant, the differences between the groups which
were fired in different numbers were not found
statistically significant. In addition, the interactions
between the groups and surface treatments were found
statistically significant.
The surface roughness values observed in IPS
e.max Press specimens after surface treatments are
presented in Table 3. According to the data, in all
groups, the highest surface roughness values were
observed in the specimens etched with acid, and the
lowest surface roughness values were observed in the
specimens applied Co-Jet. Between the groups, while the
lowest surface roughness value was observed in Group
1, the highest surface roughness value was observed in
Group 4. Among all specimens, while the acid etching
specimens in Group 4 showed the highest value, the

Table 1 Vickers hardness means and standard deviation values of groups before and after surface treatments along with
the multiple comparison test results

Initial hardness Acid-etching Co-Jet Sandblasting Total

Groups n
Mean±SD Mean±SD Mean±SD Mean±SD Mean±SD

Group 1 5 564.30±(31.82)a 588.78±(23.18)ab 719.90±(40.04)b 1,140.32±(102.13)c 753.32±(243.09)

Group 2 5 534.06±(22.57) a
580.12±(34.19) a
765.2±(30.57) b
999.06±(72.83) c
719.63±(192.21)

Group 3 5 554.24±(10.62) a
611.10±(47.4) a
907.44±(20.33) b
899.10±(77.08) b
742.97±(171.22)

Group 4 5 575.82±(24.17)a 660.62±(71.69)ab 841.58±(58.17)b 810.82±(152.90)b 722.21±(138.90)

Total 20 557.10±(26.74)a 610.15±(54.24)b 808.55±(82.19)c 962.32±(158.97)d 734.53±(187.06)

* There are statistically significant differences between the values indicated by different letters (p<0.01).
Values are given in terms of HV.

Table 2 ANOVA results of Vickers hardness values of groups before and after different surface treatments

Variation df MS F Sig.

Surface treatment 3 695,455.291 177.466 0.000

Numbers of firing 3 5,321.853 1.358 0.264

Surface treatment* Numbers of firing 9 45,688.313 11.659 0.000

Error 64 3,918.818 — —

MS: Mean square

 Dent Mater J 2017; : – 5

specimens applied Co-Jet in Group 2 showed the lowest
value.
The results of the analysis of variance which
was performed to determine whether the differences
between the surface roughness values were statistically
significant are presented in Table 4. According to the
results, while the differences between the surface
treatments were found to be statistically highly
significant (p<0.01), the groups which were fired
in different numbers were found to be statistically
significant (p<0.05). The interaction between the groups
and surface treatments were found statistically no
significant (p>0.05).
Microstructural evaluation
1. XRD analysis
XRD results for the IPS e.max Press was repeated firing
are shown in Fig. 2. LD (Li2Si2O5) was the major phase in
all of the specimens tested. All the specimens contained
a minor phase of lithium silicate (Li2SiO3) and lithium

Table 3 Surface roughness means and standard deviation values after multiple firing and different surface treatments
along with the multiple comparison test results

Surface Group 1 Group 2 Group 3 Group 4 Total

treatments Mean±SD Mean±SD Mean±SD Mean±SD Mean±SD

Acid-etching 2.26±(0.44) 2.72±(0.48) 2.86±(1.00) 3.42±(0.62) 2.82±(0.75)b*

Co-Jet 1.50±(0.33) 1.42±(0.29) 1.82±(0.44) 1.79±(0.24) 1.63±(0.35)a

Sandblasting 2.11±(0.55) 2.68±(0.50) 2.57±(0.66) 2.71±(0.27) 2.52±(0.53)b

Total 1.96±(0.54)a* 2.27±(0.74)ab 2.42±(0.82)ab 2.64±(0.79)b 2.32±(0.75)

* There is a statistically significant difference between the values indicated by different letters (p<0.01).
Values are given in terms of Ra.

Table 4 ANOVA results of the surface roughness values after multiple firing and different surface treatments

Variation df MS F Sig.

Surface treatment 2 7.575 27.516 0.000

Numbers of firing 3 1.215 4.415 0.008

Surface treatment* Numbers of firing 6 0.253 0.921 0.488

Error 48 0.275 — —

MS: Mean square

Fig. 2 X-ray diffraction peaks related to groups.

6 Dent Mater J 2017; : –

phosphate (Li3PO4). The major peaks of LD phase were
observed at the 2θ values of 24.4º (0 4 0), 23.85º (1 3 0)
and 24.88º (1 1 1). The major peaks of the lithium silicate
are found at 2θ values of 33.03º (2 0 0) and 58.89º (3 3 0).
The lithium phosphate phase peaks were at 21.14º (1 1
1) and 24.44º (2 0 0).
This is predicted by the XRD standard files for LD
(ICDDS#40-0376). LD peaks decrease from Group 1
to 4, respectively. Likewise, the height of the lithium
phosphate peaks decreased from Group 1 to 4. The peaks
of the lithium silicate have the lowest density among
other phases (Fig. 2).
The data regarding the average sizes of the LD
crystals after firing in different numbers are presented
in Table 5. While the largest crystal size was observed in
Group 2, the smallest crystal size was observed in Group
4. When we compare the relationship between crystal
size and hardness, it is seen that the hardness decreases
as the crystal size increases.
2. SEM Findings
When the ESEM images of the acid etched specimens
were evaluated, it was seen that the glass matrix
was dissolved and the rod-shaped LD crystals were
formed (Fig. 3). While the gaps between the rod-shaped
crystals were clearly seen in all other groups except

Table 5 The mean crystal sizes (nm) of lithium disilicate after different numbers of firing at 24.4º peak and 0 4 0 plane

Groups Crystallite size (nm)

Group 1 60.7

Group 2 66.1

Group 3 65.6

Group 4 33.2

Fig. 3 Environmental scanning electron microscope images of all groups (original

magnification ×10,000 for all specimens).
A: Acid-etching, B: Co-Jet, C: Sandblasting.
 Dent Mater J 2017;
for Group 3, it was seen in Group 3 that the reticular
structure extending between the rod-shaped crystals
and the crystals was fused. When the SEM images of
the specimens applied Co-jet were analyzed, more
retentive areas were observed in Group 3 in parallel
with the surface roughness values. Retentive areas
were irregularly shaped, and it was seen that the spaces
between them were covered with silica as a result of the
fact that the surface hit the surface of the silica-coated
Al2O3 sand. Very few irregularly-shaped retentive areas
which were similar were seen in Groups 1 and 2. In the
SEM images of the sandblasted specimens, Group 2
showed the surface topography with the most retentive
areas. Group 2 also had the highest values in terms
of surface roughness values. Similarly, Groups 1 and
3 had numerous irregularly-shaped retentive areas.
The needle-like crystals could not be observed because
there was no change in the glass matrix as a result of
sandblasting and Co-jet application.
DISCUSSION
The aim of this study is to evaluate the changes that
occur in the mechanical properties and microstructure of
LDC as a result of repeated firing procedures at heating
values of superstructure porcelain and different surface
treatments. The obtained results do not support our
first hypothesis and they support our second hypothesis.
Although a statistically significant difference was not
observed between the initial hardness values among four
groups which were fired in different numbers, significant
differences were found between the hardness values
measured after applying different surface treatments.
When the initial hardness values were analyzed, while
Group 4 showed the highest hardness value, Group 2
showed the lowest hardness value, but the differences
between them were not found statistically significant.
When the hardness values measured after surface
treatments were analyzed, statistically significant
differences were found between the groups and surface
treatments. Although the sandblasted specimens
showed the highest hardness values, the acid etched
specimens showed the lowest hardness values. Tang
et al.39) examined the effect of multiple pressing on the
mechanical properties and microstructure of IPS e.max
Press and reported that the specimens which were
pressed 2 times showed significantly higher Vickers
hardness values compared to the specimens which
were pressed once. They stated that this situation was
associated with the porosity and density of the material.
In other studies similar to this study, they also reported
that the hardness increased as the density of material
increased but its porosity decreased40-43).
Hardness, which affects the finishability,
polishability, and occlusal wear resistance of restorative
material, is an important property44). Materials with
a high degree of hardness exhibit greater abrasion
resistance and are difficult to polish. Substructure
materials, which become harder after a multiple-
firing protocol, may have the advantage of improved
: – 7
resistance to prevent material failures45). Apart from this
advantage, substructure materials with excessive
hardness may have a disadvantage, as it is difficult to
roughen the surface of excessively hard material. This
drawback may be effect the success of cementation of
this type of substructure materials due to decreased
microretention. In the present study, Group 4 showed
the highest initial hardness and surface roughness
values after surface treatment. Excessive firing up to
four times seems to have had no negative effect on the
mechanical properties of the IPS e.max Press. However,
clinicians should carefully consider the number of
firings of restorations. An excessive firing protocol not
only affects the hardness of substructure materials but
also influences the final color of restorations. O’Brien
et al.46) observed noticeable differences in the color of
ceramic specimens that were fired 3 and 6 times. In
addition, Uludağ et al.47) reported that perceptive color
changes occured after the number of firings increased.
For this reason, clinicians should avoid redundant firing
protocols.
Gorman et al.48) examined the effect of the
repressing process on the strength and microstructure
of IPS e.max Press, and reported that repressing of the
ceramic remaining from the first pressing did not create
a significant difference in hardness.
Li et al.49) examined the effect of the increased
annealing temperature on the microstructure and
mechanical properties of LDC and reported that the
hardness decreased as the temperature increased. They
also reported that the hardness of the LDC crystals
decreased as their sizes increased. This situation shows
parallelism with our study. It was also observed in this
study that there was an inverse proportion between the
hardness values and the crystal size among groups. This
situation is compatible with the Hall-Petch equation.
Because according to this equation, the hardness of the
material decreases as the crystal size increases50).
Gonuldas et al.51) examined the effect of the repeated
firing process on the surface roughness of the ceramic
and reported that the surface roughness decreased as
the number of firing increased. They reported that this
situation resulted from the differences that occurred in
the size of pores within the ceramic as a result of the
repeated firing processes. In the present study, the
surface roughness also increased proportionally as the
number of firing increased as a result of the repeated
firing processes in LDC specimen applied different
surface treatments and in the acid applied specimens.
Although the surface roughness of the specimens which
were acid etched was more, the surface roughness of
the specimens applied Co-jet was less. This situation
can be associated with the fact that the changes in
the microstructure of LDC crystals caused by different
numbers of firing lead to dissolutions of different sizes
in the glass matrix with the acid application and that
rod-shaped LD crystals become apparent.
The abrasion potential of ceramic materials depends
on various factors, such as the microstructure, surface
roughness, and fracture toughness52). In vitro studies
8 Dent Mater J 2017;
have demonstrated that polished ceramics produce
less wear on opposing enamel than on glazed ceramics;
thus, researchers recommend polishing the adjusted
area instead of glazing it52,53). In the present study, the
surface hardness, surface roughness and microstructure
changed after multiple firing and different surface
treatments. For these reasons, the abrasion potential of
IPS e.max Press on opposing enamel may be negatively
altered.
A study examining the effect of surface treatments
on the hardness and roughness of LDC was not found
in the literature review carried out. The data we have
obtained as a result of the study can be beneficial to the
literature in this regard. The data we have obtained
give information about the mechanical properties of
LDC restorations which are fired at heating values
of superstructure porcelain more than normal due to
several reasons. While sandblasting was the surface
treatment that mostly increased the surface hardness in
LDC specimens which were fired more than normal, acid
etching affected at the least level. In addition, while acid
etching was the surface treatment that mostly increased
the surface roughness in contrast to hardness, Co-Jet
application was the process that decreased at the least.
This situation indicates that mechanical properties were
affected by the subsequently applied surface treatments
in addition to the changes occurring in the microstructure
of the LDC crystals after the excessive firing. In
particular, acid etching can be suggested to increase the
mechanical connection of the LDC restorations which
are excessively fired with cement.
The data obtained as a result of the XRD analysis
also support our study hypothesis. The density of the
peaks shown by LD decreases as the number of firing
increases. This situation is also an indicative of a
change in the microstructure. Furthermore, the fact
that the mean crystal sizes measured at 24.4º and 4 0
4 plane where the highest peaks were observed were
different indicates that the microstructure was also
changed. When we evaluate the changes occurring in
the microstructure with the mechanical properties, we
can say that the hardness decreases as the crystal size
increases. However, a connection cannot be established
between the hardness and surface roughness values
measured after surface treatments. This can also be
associated with different changes in the microstructure
of the LDC caused by different surface treatments. The
rod-shaped LD crystals that come out depending on
the dissolution of the glass matrix as a result of acid
etching cannot be observed in the specimens applied
sandblasting and Co-Jet. Therefore, this situation affects
the mechanical properties.
CONCLUSIONS
Within the limitations of this study, the following
conclusions were drawn;
1. The multiple firing protocol at heating values of
superstructure porcelain affect the microstructure
of LDC. In the XRD analysis, it was observed
: –
that the density of the LD peaks decreased as the
number of firing increased.
2. Different surface treatments applied to LDC
specimens fired at grater heating values of
superstructure porcelain than normal affected
hardness and surface roughness in different
ways. While the sandblasted specimens had the
hardest surface, the acid-etched specimens had
more surface roughness.
Changes in mechanical properties and
microstructure were observed in the LDC exposed
to more heat treatments applied to superstructure
porcelain than normal. The optimum properties for IPS
e.max Press probably emerge from the normal firing.
In contrast, no material mechanical properties appear
to change significantly with excessive firing. Although
the results of present study showed that excessive firing
is possible, the researchers observed some qualitative
differences in excessively fired specimens. Essentially,
conclusive support for excessive firing process cannot
yet be provided. It is better to decrease the number of
firing as much as possible.
The summary of this article had been presented as Oral
presentation, 20. International Congress of Esthetic Dentistry,
2016, istanbul, Turkey.
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