Dental Materials Journal 27(1)：7‐15, 2008

Mechanical and Thermal Cycling Effects on the Flexural Strength of Glass Ceramics
Fused to Titanium
Vanessa VÁSQUEZ1, Mutlu ÖZCAN2, Renato NISHIOKA1, Rodrigo SOUZA1, Alfredo MESQUITA1 and
Carlos PAVANELLI1
1
São Jose dos Campos Dental School, Department of Dental Materials and Prosthodontics, São Paulo State University, São
Jose dos Campos, Brazil
2
University Medical Center Groningen, University of Groningen, Department of Dentistry and Dental Hygiene, Clinical
Dental Biomaterials, Antonius Deusinglaan 1, 9713 AV, Groningen, The Netherlands
Corresponding author, Mutlu Özcan; E-mail: mutluozcan@hotmail.com

Received April 4, 2007/Accepted July 20, 2007

                                                         
This study evaluated the effects of mechanical and thermal cycling on the Áexural strength (ISO 9693) of three brands of
ceramics fused to commercially pure titanium (cpTi). Metallic frameworks of 25 3 0.5 mm dimensions (N＝84) were cast
in cpTi, followed by 150-μm aluminum oxide airborne particle abrasion at a designated area of the frameworks (8 3 mm).
Bonder and opaque ceramic were applied on the frameworks, and then the corresponding ceramic (Triceram, Super Porce-
lain Ti-22, Vita Titankeramik) was Àred onto them (thickness: 1 mm). Half of the specimens from each ceramic-metal com-
bination were randomly tested without aging (only water storage at 37ºC for 24 hours), while the other half were mechani-
cally loaded (20,000 cycles under 10 N load, immersion in distilled water at 37℃) and thermocycled (3,000 cycles, between
5‐55℃, dwell time of 13 seconds). After the Áexural strength test, failure types were noted. Mechanical and thermal
cycling decreased the mean Áexural strength values signiÀcantly (p<0.05) for all the three ceramic-cpTi combinations tested
when compared to the control group. In all the three groups, failure type was exclusively adhesive at the opaque ceramic-
cpTi interfacial zone with no presence of ceramic on the substrate surface except for a visible oxide layer.

Keywords: Flexural strength, Aging, Titanium

                                                         

oxygen during casting when conventional casting and

INTRODUCTION
Although there is a growing trend for metal-free res-
torations in the dental profession, failures associated
with such materials are also being reported ― indi-
cating that there is still place for metal-ceramic Àxed
partial dentures (FPD). Furthermore, extensive oral
rehabilitation could be achieved with metal-ceramic
FPDs only. However, the high cost of noble alloys
and the potential biological hazards of base metal
alloys pose some concerns for practical application.
To circumvent these concerns, commercially pure
titanium (cpTi) and some of its alloys were intro-
duced for the construction of dental prostheses1).
  According to the American Society for Test-
ing and Materials (ASTM), cpTi is available in four
different grades (grade I to IV). It is based on the
incorporation of small amounts of oxygen, nitrogen,
hydrogen, iron, and carbon during puriÀcation pro-
cedures, whereby each grade has different physi-
cal and mechanical properties. Grades I and II are
the most commonly used types in the production of
metal-ceramic FPDs1). In implants and implant-sup-
ported FPDs, cpTi and its alloys exhibit remarkable
advantages due to their excellent biocompatibility,
corrosion resistance, high strength, and low modulus
of elasticity1-4).
  However, cpTi has a high melting point and it
is active at high temperatures. For these reasons,
it may become fragile if it reacts with atmospheric
investing methods are used5). Furthermore, tempera-
tures above 800℃ increase the oxygen-rich titanium
oxide layer on the surface, so called α-case, which
impairs the mechanical compatibility of the titanium-
ceramic system6-9). It should also be mentioned that
cpTi has a low thermal expansion coefÀcient that
makes it a difÀcult substrate for ceramics to bond
onto.
  To the end of better compatibility with cpTi,
ceramics to meet this speciÀc purpose have been
developed1). These ceramics, so called low-fusing
ceramics (LFC), melt at temperatures lower than
800℃. Moreover, they have thermal expansion coef-
Àcients close to that of titanium, thereby reducing
the thermo-mechanical stresses at the interface and
allowing satisfactory bonding of the two elements10).
By virtue of the advances in dental technology, the
α-case layer can also be controlled almost com-
pletely through improved casting techniques. This
is done by induction in an inert atmosphere of argon
or helium gas and with the use of refractory invest-
ments that contain oxides such as magnesium,
yttrium, and zirconium11-13).
  The success of metal-ceramic FPDs hinges on
a durable adhesion between ceramic and the metal
substructure9,14,15). In today s dentistry, cpTi compat-
ibility with ceramics, refractory materials, and spe-
cial casting systems are not widely studied. These
studies should indeed be undertaken with a view to
8 Ceramic-titanium Áexural strength
improving the success rate of metal-ceramic FPDs1).
The cpTi-ceramic adhesion could be tested in sev-
eral ways. These tests can be classiÀed according to
the nature of the applied stress, such as shear, ten-
sile, Áexural strength, or torsion test. However, to
date, there is still no consensus as to which method
is more valid for clinical applications16). In addition,
these methods often do not involve the fatigue com-
ponent of mechanical tests, thereby rendering the
results unrealistically optimistic to a certain extent.
  To better predict the clinical behaviors of dif-
ferent materials and material combinations, their
mechanical fatigue tests should be carried out in a
wet environment17,18). In this connection, thermo-
cycling that is based on temperature alternations
induces repeated stress to the metal-ceramic inter-
face18,19). During thermocycling, differences between
the thermal expansion coefÀcients of the two com-
ponents could affect adhesive strength. However, a
combination of both mechanical and thermal cycling
could be considered a more aggressive way of aging
the ceramic-metal interface.
  Undisputedly, cpTi and its alloys have many
advantages and favorable properties over the other
dental alloys. However, controversies exist in the lit-
erature regarding the adhesion of ceramics to these
alloys7,20-22). Therefore, the objectives of this study
were twofold: (1) to evaluate the effects of mechanical
and thermal cycling on the Áexural strength of three
brands of ceramics fused to cpTi; and (2) to asses the
type of failure at the ceramic-alloy interface.
MATERIALS AND METHODS
Materials used
Three brands of ceramics ― namely, Triceram, Super
Porcelain Ti-22, and Vita Titankeramik ― were
used in combination with cpTi in this study. Brand
names, manufacturers, and batch numbers of the
ceramic types and titanium are presented in Table 1.
Fabrication of metallic frameworks
Rectangular acrylic templates (25 3 0.7 mm) were
Table 1 Brand names, indications, compositions, and manufacturers of dental ceramics and titanium used in this study
Brand name Ceramic Type
Triceram Low-fusing ceramic
Super Porcelain Ti-22 Low-fusing ceramic
Vita Titankeramik Low-fusing ceramic
Commercially pure titanium (Tritan)
used for the fabrication of frameworks. A wax sprue
(Horus, Herpo Produtos Dentários Ltd., São Paulo,
Brazil) was attached perpendicular at one end of the
template and connected to a central wax rod of 5 mm
diameter (Wax Wire for Casting Sprues, Dentaurum,
Pforzheim, Germany). The assembly was mounted in
a silicone ring and poured with investment material
(Rematitan® Ultra, Dentaurum JP Winkelstroeter
KG, Pforzheim, Germany) that was mixed at a ratio
of 100 g of powder to 14 ml of liquid. After the
investment material set, the silicone ring and sprue
former were separated from the investment mold.
Metallic frameworks were cast in cpTi (N＝84) in an
electrical induction furnace (Rematitan® Autocast,
Dentaurum) under argon gas. Elimination of sprues
and separation of metallic strips were performed
with the aid of carbide disks at low speed.
  After removal from the investment mold, mar-
gins of the frameworks were trimmed to the Ànal
dimensions of 25 3 0.5 mm. Surfaces of the speci-
mens that would receive the ceramic layer were
treated with airborne particle abrasion with 150-μm
aluminum oxide (Korox, Bego, Bremen, Germany).
This was done at an angle of 45 for 10 seconds,
and from a distance of approximately 2 cm under 2
bar pressure. Frameworks were then ultrasonically
cleaned in isopropyl alcohol (Vitasonic II, Vita
Zahnfabrik, Bad Säckingen, Germany) for Àve
minutes and allowed to dry at room temperature.
Application of ceramic layer
An area of 8 3 mm was marked on the cpTi frame-
works with a graphite pencil. Then, the bonder
of each ceramic was applied in a thin layer with a
brush. After Àring, opaque ceramic paste ― con-
sisting of opaque ceramic powder mixed and homog-
enized with liquid in a container connected to a dis-
penser ― was applied on the bonder. Thickness of
the ceramic layer corresponding to dentin ceramic
(1 mm) was standardized by positioning the frame-
works in a metallic template. After removal from
the assembly, ceramic was Àred. Due to shrinkage,
a second layer was applied and then the specimens
Manufacturer Batch number
Dentaurum, Ispringen, Germany 003
Noritake, Nagoya, Japan 60506
Vita Zahnfabrik, Bad Säckingen, 2370
Germany
Dentaurum J.P. Winkelstroeter KG, 098
Pforzheim, Germany
 VÁSQUEZ et al. 9

Table 2 Firing procedures of the dental ceramics tested

Ceramics Starting Drying Time Final Temperature Holding time
Temperature (ºC) (min) Temperature (℃) rate of increase (min)
(℃/min)

Triceram

Bonder 500 4 795 65 1

Opaque 500 4 795 65 1

First dentine layer 500 6 755 40 1

Second dentine layer 500 4 755 40 1

Super Porcelain Ti-22

Oxidation 500 3 800 50 3

Bonder 500 5 800 50 1

Opaque 500 5 780 50 1

First dentine layer 500 7 760 40 1

Second dentine layer 500 7 760 40 1

Vita Titankeramik

Bonder 400 6 800 60 1

Opaque 400 2 790 110 1

First dentine layer 400 6 770 50 1

Second dentine layer 400 6 770 50 1

were submitted for Ànal glaze Àring (Table 2).
  Twenty-eight specimens for each ceramic-cpTi
combination were randomly divided into two sub-
groups: mechanical and thermal cycling versus only
stored in distilled water for 24 hours at 37℃ (control
group) prior to Áexural strength test.
Mechanical and thermal cycling
Mechanical cycling of the specimens was carried
out in a mechanical cycling machine (custom made,
Paulista State University, Dental School, UNESP,
Sao Jose dos Campos, Brazil). The latter was devel-
oped to simulate the mechanical forces generated
during the chewing cycle. The device employed for
this test was composed of two bases, 2 cm apart from
each other, on which cylinders (radius: 1.0 mm) were
placed to allow specimens to be positioned parallel to
the ground and perpendicular to the axial load. An
upper rod with a 1 mm diameter tip was Àxed on a
plier to apply a 10 N load for 20,000 times at a fre-
quency of 1 cycle per second. The device for testing
was placed on the machine base that contained a
thermostat to allow testing in an aqueous medium at
a constant temperature of 37℃.
  Subsequently, the specimens were thermocycled
for 3,000 cycles between 4℃ and 55℃ in deionized
water (Nova Etica, São Paulo, Brazil). Dwelling time
at each temperature was 10 seconds, and the trans-
fer time from one bath to the other was Àve seconds.
  The process of subjecting the specimens to
20,000 times of mechanical cycling followed by 3,000
times of thermal cycling is regarded as the aging
procedure.
Flexural strength test
Flexural tests were performed in a universal test-
ing machine (Instron 4301, Instron Corp., Norwood,
MA, USA). The load was applied at a constant speed
of 1.5 mm per minute until fracture occurred (Figs.
1(a)‐(d)). The formula according to the guidelines
of ISO 969323) was adopted for the calculation of
data obtained from the Áexural strength test. The
load that led to initial separation of materials was
obtained in kilogram force (kgf). It was converted to
Newton (N) for the calculation of Áexural strength
according to the following equation:
where P is the maximum load upon fracture (N), I
the distance between two supports (mm), and b the
10 Ceramic-titanium Áexural strength

Fig. 1 (a) Final shape and dimensions of ceramic-alloy specimen; (b) cross-section dimensions of
specimen according to ISO 9693; (c) application of axial force; (d) separation of ceramic from
titanium surface.

width (mm) and d the thickness (mm) of the speci-
men.
  Specimens were analyzed under a stereomi-
croscope (Stemi 2000-C, Carl Zeiss, Gottingen, Ger-
many). Images were digitally recorded with a cam-
era (Cybershot, Model DSC-S85, Sony, Tokyo, Japan),
which was connected to the microscope, for metal
surface characterization and assessment of failure
modes. In this study, failure types were classiÀed
as follows: (a) adhesive failure along the interfacial
region between opaque ceramic and ceramic-metal
interaction zone; (b) inside the interaction zone;
and (c) cohesive failure along the interfacial region
between metal and the interaction zone9).
Statistical analysis
Statistical analysis was performed using STATIS-
TICA for Windows (version 5.5, StatSoft Inc., Tulsa,
OK, USA) and Statistix for Windows (version 8.0,
Analytical Software Inc., Tallahassee, FL, USA).
The means of each group were analyzed by two-way
analysis of variance (ANOVA), with Áexural strength
as the dependent variable and the ceramic-metal
combination and aging condition as the independent
factors. P values less than 0.05 were considered to
be statistically signiÀcant in all the tests. Multiple
comparisons were made by Tukey s adjustment.
RESULTS
Table 3 presents the two-way analysis of variance
(ANOVA) results for the experimental conditions.
Interaction between ceramic type and aging factor
was not statistically signiÀcant (p＝0.168) (ANOVA,
Tukey s test). In Table 4, it was shown that mechan-
ical and thermal cycling decreased the mean Áex-
ural strength values signiÀcantly (p<0.05) for all the
three ceramic-cpTi combinations tested (27.4 4.1‐
28.5 5.4 MPa) when compared to the control group.
In the latter group, tests were performed after 24-
hour water storage at 37℃ (32.5 4.3‐38.5 2.3
MPa).
 VÁSQUEZ et al. 11

  Results of Tukey s multiple comparison test systems). There was no presence of ceramic on the
established that only Vita Titankeramik-cpTi system substrate surface, except for a visible layer of dark
showed a signiÀcantly higher value than those of titanium oxide. Representative images of original
other ceramic-cpTi combinations in the control group cpTi-ceramic substrate and cpTi surfaces after Áex-
(p<0.05) (Fig. 2). ural strength test are illustrated in Figs. 3(a)‐(g).
  Stereomicroscope images at 25 magniÀca-
tion showed exclusively adhesive failure mode at the
opaque ceramic-cpTi interfacial zone in all the exper- Table 4 Mean ( standard deviation) Áexural strength
imental groups (Triceram-cpTi, Super Porcelain Ti values (MPa) of ceramic-cpTi combinations with
22-cpTi, and Vita Titankeramik-cpTi metal-ceramic and without mechanical and thermal cycling.
Same superscript letters indicate no signiÀcant
differences (Tukey s test, α＝0.05)
Table 3 Results of two-way analysis of variance (ANOVA)
Mechanical- and
for ceramic type, cycling fatigue conditions, and Experimental thermal-cycling Mean (SD)
their interaction according to Áexural strength Groups
data (*: p<0.05) Without With
Triceram-cpTi 32.5 4.3a,b,c 28.4 5.3b,c 30.5 5.1
Effect DF SS MS F P (Group 1)
Cycling 1 594.00 594.00 22.78 0.001* Super 35.4 7.6a,b 28.5 5.4b,c 32 7.3
Groups 2 38.21 19.11 0.73 0.488 Porcelain Ti-22-
(metal-ceramic) cpTi (Group 2)

Vita 38.5 2.3a 27.4 4.1c 32.8 6.8

Interaction 2 97.76 48.88 1.87 0.168 Titankeramik-
Residue 36 938.74 26.08 cpTi (Group 3)
Total
41 1668.72 Mean (SD) 35.5 5.5 35.5 5.5
* Statistically signiÀcant difference at the level of 5%. * Means followed by equal letters do not differ statistically

Fig. 2 Mean Áexural strength values according to the experimental conditions established by the variables of ceramic
type and aging (20,000 times of mechanical cycling followed by 3,000 times of thermal cycling).
12 Ceramic-titanium Áexural strength

Fig. 3 (a) Representative image of ceramic specimen Àred onto cpTi and optical microscopic images of specimens ( 25)
after Áexural strength test: (b)‐(c) Triceram-cpTi; (d)‐(e) Super Porcelain Ti-22-cpTi; (f)‐(g) Vita Titankeramik-
cpTi. Clear appearance of cpTi metal surface is seen as well as blur appearance of oxide layer on the ceramic
surface. Metal and oxide surfaces are indicated by an arrow for each ceramic-cpTi combination
 VÁSQUEZ et al.
DISCUSSION
The clinical performance of metal-ceramic FPDs
is usually estimated by mechanical strength tests,
which assess the adhesion between a ceramic and the
metal substrate. The nature of metal-ceramic bond-
ing has been studied extensively, and it is funda-
mentally based on three mechanisms: micromechani-
cal retention, compressive adaptation, and chemical
bonding9,15,24).
  In dental materials research, Áexural strength
test is considered as the most appropriate method
to measure bond strength between two materi-
als4,10,14,18,19,21,25-28). Some authors would recommend
three-point bending test29,30), while others would
advocate four-point or biaxial Áexure strength test to
evaluate metal-ceramic adhesion31). According to ISO
969323), Áexural strength test should be preferred
over the other methods because the stresses it simu-
lates closely represent the stresses that occur in den-
tal prostheses with multiples elements.
  The α-case layer that formed on the surface of
melted cpTi alloys provided good chemical stability.
However, at the same time, this intermediate oxide
layer could impair the chemical reactions between
cpTi and the bonder ceramic components, thereby
weakening the cpTi-ceramic bonding. It is note-
worthy that this oxide layer is often not strongly
adhered to the metal surface and that it is porous,
brittle, and incompatible with ceramics. It was
therefore little wonder that the oxide layer itself or
the interface between the oxide layer and the alloy
has been shown to be responsible for metal-ceramic
fractures3,6,14,28). In a bid to circumvent the incompat-
ibility problem between the α-case layer and ceram-
ics, a ceramic bonder corresponding to each ceramic
material was thus used in this study.
  Besides, composition of the investment mate-
rial and casting procedure also inÁuence the forma-
tion of α-case layer. For this reason, some authors
advocated the use of Mg-based investment materi-
als32), while others suggested Zr-modiÀed Mg-based
investment materials33). Addition of these elements
increases the thermal expansion coefÀcient of the
investment material and limits its interfacial reactiv-
ity with cpTi at high temperatures. In the present
study, the investment material used was in compli-
ance with the manufacturer s recommendations.
  The pressure at which liquid titanium was
injected into the investment32), and the temperature
at which this procedure was performed, could also
inÁuence the consequential adhesion of ceramics to
cpTi22). Within this context, ceramics have been spe-
ciÀcally developed to make their Àring onto cpTi pos-
sible at temperatures below 800℃, so as to prevent
excessive formation of oxides on the metallic frame-
work surface2). The ceramic systems employed in
13
this study presented low Àring temperatures for each
layer ― between 750 and 800℃. Lautenschlager
and Monaghan2), Wang and Fenton1), and Esquivel
et al.10) proposed improved adhesion between ceram-
ics and cpTi with so-called ultra-low fusing ceramics,
whereby the Àring temperatures range between 650
and 850℃9). These ceramics decrease the transfor-
mation phase of cpTi, resulting in a stable oxide layer
and good adhesion of the ceramics. Failure analysis
also indicated a visible dark zone of oxide layer.
  Differences in thermal expansion coefÀcient
between the metal and ceramic can produce resid-
ual stresses along the interface, which can result in
debonding or fracture of the ceramic9,21,22). Thermal
expansion coefÀcients of the ceramics used in this
research varied between 8.4 and 8.9 10‐6K‐1, being
very close to each other. Thus, non-signiÀcant differ-
ences among the ceramics tested could be explained
on this ground. In the present study, results of the
control group without mechanical and thermal aging
(32.5‐38.5 MPa) corroborated with the Àndings of
Yilmaz and Dincer14) and White et al.17) ― where low-
fusing ceramics were also used. However, between
the studies of Pröbster et al.19) and Yilmaz and
Dincer14), the Áexural strength values showed great
variations ranging from 14 MPa to 37 MPa. None-
theless, results of the current study ― both the con-
trol group without aging and even after aging ― were
higher than the recommended minimum value of 25
MPa as established by DIN 13.92734).
  In terms of specimen dimensions, Yoda et al.4)
suggested that the speciÀcations of ISO 969323) did
not entirely represent those of metal-ceramic dental
restorative systems and Troia et al.28) attributed this
to non-uniformity of ceramic thickness. For this rea-
son, ceramic thickness was standardized at 1 mm in
this study.
  The effects of mechanical and thermal cycling
simulate ― to a certain extent ― the effects of the
clinical service which dental materials are subjected
to in the oral environment. In dental materials
research, most in vitro experiments are performed
using static mechanical tests that do not address
the aggressive oral environment. It is known that
the oral environment is able to induce physicochemi-
cal alterations in dental materials. Temperature
changes provide conditions for occurrence of deg-
radation in an aqueous environment35). They also
encourage mechanical fatigue of the materials them-
selves or their interfaces, which is triggered by the
repeated chewing action36,37). As for the water stor-
age of ceramic materials, it decreases the latter s
mechanical properties38). The reduction may be
related to the solubility of different oxides. This
process may be higher in ceramics designed for use
with cpTi because of the presence of alkaline metallic
oxides35) ― which was also evident from the failure
14 Ceramic-titanium Áexural strength
analysis of this study.
  Previous studies which investigated the adhesion
between metal and laboratory resin or between metal
and ceramics disclosed reduced adhesion after ther-
mal cycling18,19,39-41). In the study of Tróia Jr et al.28),
the same form of thermal variation and metallic sub-
strate (cpTi) as the present study were investigated.
However, it was found that thermal cycling did not
exert any inÁuence on adhesion of ceramic with this
metal. Nonetheless, this factor became more sig-
niÀcant and pronounced in more drastic conditions
as those employed in the study of Shimoe et al.42),
where extended thermal cycling (100,000 cycles) was
performed. As a result, a 30％ reduction in mean
bond strength was observed. In this study, the chief
focus was on the combined effects of mechanical and
thermal cycling. On this ground, extended thermal
cycling was not performed.
  According to Scherrer et al.36), all materials and
their combinations should be subjected to fatigue
conditioning before mechanical testing is performed.
Mechanical fatigue is a helpful means to predict the
clinical behavior of dental restorative systems in
order to avoid catastrophic failures in vivo37). Some
factors inherent to mechanical cycling may also
inÁuence the outcome. In this study, the applied
load was 10 N and the number of cycles was 20,000
times at a frequency of 1 Hz as described by Itinochi
et al.43). As for thermal cycling, the number of cycles
adopted and the temperature alterations employed
were based on previous reports18,19,28). Thermal
cycling induces repeated stress at the metal-ceramic
interface, thereby weakening the bond between the
two components28,44,45). In this connection, Tróia et
al.28) suggested that extended immersion times in
each bath might produce higher tension at the metal-
ceramic interface. On this note, Pröbster et al.19) and
Leibrock et al.45) suggested that 6,000 thermal cycles
would correspond to Àve years in physiological condi-
tions.
  In this study, reduction in mean Áexural
strength was evident after aging. Although previous
studies that investigated ceramic-cpTi bond strength
did not incorporate the aging conditions19,28), other
studies sought to achieve the same research objective
by modifying fatigue variables such as load magni-
tude and type of load (such as repetitive or dynamic
load)18). Therefore, with a view to making study
results comparable, there seems to be a need to stan-
dardize the aging parameters.
  In clinical situations, many metal-ceramic FPD
failures are in the form of ceramic fractures with
metal exposure. While the search is still on for a
better ceramic-compatible metal/alloy with improved
clinical performance, clinicians should in the mean-
while bear in mind that ceramic-metal bonding is
susceptible to mechanical and thermal fatigue.
CONCLUSIONS
Mechanical cycling for 20,000 times followed by ther-
mal cycling for 3,000 times decreased the mean Áex-
ural strength values signiÀcantly for all the three
ceramic-cpTi combinations tested when compared to
the control group ― where tests were performed after
mere 24 hours water storage at 37℃. All tested
ceramic-cpTi combinations showed adhesive fail-
ure with a visible oxide layer on the cpTi substrate,
indicating that the weakest link was still between
ceramic and the titanium oxide assembly.
ACKNOWLEDGEMENTS
This investigation was Ànancially supported by a
grant, Grant No. 01166/04, from FUNDUNESP
(Fundação para Desenvolvimento da Universidade
Estadual Paulista).
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