journal of dentistry 36 (2008) 822–827

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Evaluation of bond strength of various margin ceramics

to a zirconia ceramic

M. Erhan Çömlekoğlu a,*, Mine Dündar a, Mutlu Özcan b, M. Ali Güngör a,

Bülent Gökçe a, Celal Artunç a
a
Ege University, School of Dentistry, Department of Prosthodontics, Izmir, Turkey
b
University Medical Center Groningen, University of Groningen, Academic Center for Oral Health,
Clinical Dental Biomaterials, Groningen, The Netherlands

article info abstract

Article history: Objective: This study evaluated the bond strengths of four different margin ceramics based
Received 13 March 2008 on fluoroapatite and feldspath to a zirconia ceramic.
Received in revised form Methods: Zirconia cores (Zirconzahn) (N = 28, n = 7/margin ceramic group) were fabricated
30 May 2008 according to the manufacturers’ instructions (diameter: 4 mm; thickness: 2 mm) and ultra-
Accepted 31 May 2008 sonically cleaned. Four different margin ceramics (thickness: 5 mm) (Cerabien Zr, Noritake;
Ceramco PFZ, Ceramco; e.max, Ivoclar Vivadent and Triceram, Dentaurum) were vibrated
and condensed in a stainless steel mould and fired onto their zirconia cores. After trying the
Keywords: specimens in the mould for minor adjustments, they were again ultrasonically cleaned and
Shear bond strength embedded in PMMA. The specimens were stored in distilled water at 37 8C for 1 week and
Zirconia shear bond strength (MPa ! S.D.) tests were performed in a universal testing machine
Margin ceramic (crosshead speed: 0.5 mm/min). Failure modes were recorded under SEM.
Copy-milling Results: Significant effect of margin ceramic types were found on the bond strength values
(P < 0.05). The mean bond strength values of Ceramco margin ceramic to zirconia was
significantly lower (25.4 ! 4.5 MPa) (P < 0.05) than those of Cerabien (31.6 ! 6.4 MPa), e.max
(35.9 ! 8.4 MPa), and Triceram margin ceramic (38.8 ! 7.1 MPa) systems.
Conclusions: Margin ceramics, compatible with zirconia framework material tested in the
present study, exhibited high bond strength values. Variations in thermal expansion
coefficients might influence their bond strength values.
# 2008 Elsevier Ltd. All rights reserved.

1. Introduction conventional cements.4 Several different oxides such as

Various types of reinforced ceramic framework materials have
been introduced in restorative dentistry in an attempt to
improve the mechanical properties of ceramics.1–5 One such
example is zirconium dioxide (hereon: zirconia)-based mate-
rials. Zirconia is a biocompatible material with excellent
mechanical properties and low bacterial adhesion properties.
Restorations made of this material can be cemented with
Magnesia (MgO), Yttria (Y2O3), and Calcia (CaO) are added to
zirconia in order to stabilize their tetragonal and/or cubic
phases to form partially stabilized zirconia. When zirconia
polycrystal is processed with yttria, yttrium-stabilized tetra-
gonal zirconium polycrystal (Y-TZP) is obtained.5 The high
initial strength and fracture toughness of zirconia results from
a physical property of partially stabilized zirconia known as
transformation toughening.6

* Corresponding author at: Ege University, School of Dentistry, Department of Prosthodontics, Bornova 35100, Izmir, Turkey.
Tel.: +90 2323880327; fax: +90 2323880325.
E-mail address: erhancomlek@yahoo.com (M.E. Çömlekoğlu).
0300-5712/$ – see front matter # 2008 Elsevier Ltd. All rights reserved.
doi:10.1016/j.jdent.2008.05.019
 journal of dentistry 36 (2008) 822–827 823

Zirconia frameworks can be fabricated mainly with the
help of CAD/CAM or copy-milling techniques by means of
grinding a zirconia block. These blocks can be milled either in
the green, pre-sintered or completely sintered stage.7,8 Frame-
works made from green and pre-sintered zirconia are milled in
an enlarged form to compensate for the shrinkage that occurs
during sintering, which usually equals to 20–25% for partially
sintered frameworks.9,10 Completely sintered Y-TZP blocks are
prepared by pre-sintering at temperatures below 1500 8C and
then processed by hot isostatically pressed (HIP) technique at
temperatures between 1400 and 1500 8C under high pressure
in an inert gas atmosphere. This leads to a very high density in
excess of 99% of the theoretical density.5 The blocks can then
be machined using a specially designed milling system.
The milling of pre-sintered zirconia blocks is faster and
causes less mechanical damage to the material than milling of
fully sintered blocks.6 Compared to the milling method based on
pre-sintering, milling of fully sintered zirconia blocks is a time
consuming process that causes greater wear of the diamond
burs and is more expensive. Moreover, it has recently been
reported that questions remained regarding to the surface state
after hard machining of Y-TZP, while soft machining seemed to
lead to a more consistent final state, provided that the
machined restoration was left intact after sintering.5 Hence,
green-stage zirconia could be considered advantageous.
The milled frameworks are then veneered with feldspar or
glassy matrix ceramics appropriate for the zirconia ceramic
used. However, the mechanical properties of zirconia ceramic
are affected during the veneering stage performed at relatively
higher temperatures.11 The framework suffers from distortion
and shrinkage during sintering and veneering stages but this
does not consequently have a negative effect on the marginal
adaptation. The quality of the marginal adaptation has been
shown to influence the long-term success of restorations.11 In
terms of longevity, the clinically acceptable range of marginal
discrepancies is "120 mm. On the other hand, in CAD/CAM or
copy-milling systems, the marginal opening has been reported
to range between 60 mm and 300 mm.11,12
Margin ceramics are therefore formulated to compensate
for the marginal impurities in order to maintain accurate fit as
well as resistance to chewing forces. Their shrinkage after
firing/sintering has been minimized. Moreover, fluorescent
agents are added to optimize their aesthetics and opacity has
been balanced to mask the show-through of the more opaque
framework.13 In a recent clinical study on zirconia FPDs, the
overall survival rate was found to be 73.9% with marginal
integrity problems and thereby secondary caries (21.7%) and
ceramic chipping (15.2%) being major causes of failure.17 Also,
the most common chippings were observed at the cervical
areas of the reinforced all ceramic fixed-partial-dentures
(FPDs).14
It has been previously demonstrated that marginal dis-
crepancies of conventional metal–ceramic systems decreased
after the application of margin ceramics.15 Although it is not
commonly practiced, such marginal ceramics, made of either
feldspath or fluoroapatite, are also available to be used in
conjunction with zirconia FPDs. Since cervical areas of the FPDS
were reported to be more prone to stresses,16 the adhesion of
such margin ceramics to the core ceramic is of clinical
importance in order not to experience chippings after cementa-
tion. No study to date evaluated their durability on zirconia.
Although with fluoroapatite ceramic, high degree of luminous
reflectance and high translucency could be delivered, since they
are all glassy matrix ceramics, it can be hypothesized that both
feldspath or fluoroapatite types of margin ceramics would
perform comparable bond strength to zirconia.
Therefore, the objectives of this study were to compare the
adhesion of four individual margin ceramics to a processed
zirconia framework and evaluate the failure modes after
debonding.
2. Materials and methods
Core/margin ceramic combinations (N = 28, n = 7 per group)
were fabricated by one experienced dental technician accord-
ing to each manufacturer’s instructions. The brand names,
types, compositions, manufacturer and batch numbers of the
margin ceramics, modelling liquid and liners used in this
study are presented in Table 1.

Table 1 – Margin ceramics used in this study

Brand name of margin Ceramic type Chemical composition Manufacturer Batch number
ceramic, build-up liquid
and liner

Cerabien Zr Feldspathic SiO2, Al2O3, Na2O, CaOK2O, Noritake Dental Supply Co., MB3 OD612
MgO, LiO2, B2O3, pigments Nagoya, Japan
Cerabien Zr forming liquid APEJQ
Ceramco PFZ Feldspathic SiO2, Al2O3, Na2O, K2O, Ceramco, Burlington, A3-06002487
SnO2, CeO2, pigments, NJ, USA
1.3-Butanediol Xi
Ceramco PFZ margin liquid 06003649
E.max margin Fluorapatite SiO2, Al2O3, Na2O, K2O, IvoclarVivadent, JO6301
ZnO, CaO, P2O5, F, oxides, Schaan, Liechtenstein
pigments
E.max Zir liner build-up liquid H33669
E.max margin build-up liquid H32689
E.max Zir liner 2 H12845
Triceram Feldspathic SiO2, Al2O3, K2O, Na2O, Dentaurum, Ispringen, SMA 003F
Li2O, CaO, BaO, MgO, B2O3, F Germany
824 journal of dentistry 36 (2008) 822–827

2.1. Preparation of the core ceramics

Zirconia core specimens (diameter: 4 mm, height: 2 mm) were

produced by a copy-milling system (Zirconzahn, Bruneck,
Italy) using prefabricated blanks of zirconia (ICE Zirkon,
Zirconzahn, Bruneck, Italy) and then sintered. All of the core
materials were ultrasonically cleaned (Quantrex 90, L&R
Ultrasonics, Kearny, NJ, USA) for 15 min in ethanol and
deionized water and air-dried.

2.2. Preparation of the core-veneer assemblies

The individual veneering ceramics for the zirconia ceramic

cores were condensed at a thickness of 2 mm, positioned on
top of a platinum foil and backed by a glass slide leading to
specimens with 5 mm in diameter and 5 mm in height.
Manufacturers of e.max and Triceram margin ceramics
required an obligatory liner application at the interface
whereas the other two were instructed to be applied directly
to the core ceramic without liners. Ceramic powder for dentin
of four different types of zirconium margin ceramics was
mixed on a glass slab using the mixing liquid as recommended
by each manufacturer. The mould was carefully filled with the
creamy mixture of margin ceramic and condensed. Excess
liquid was removed by applying a piece of adsorbing paper
(Kimwipes1Lite 200, Kimberly Clark Corp., Roswell, GA, USA)
onto the surface of the specimen. After condensation, the
mould was removed, leaving the non-sintered specimen
behind on the platinum foil. The test specimens on the
platinum foil, were then transferred to a firing tray, and
sintered in a calibrated ceramic furnace (Programat P90,
Ivoclar, Schaan, Liechtenstein) in accordance with each
manufacturer’s instructions. Following the firing process,
the specimens were tried in the mould for minor adjustments,
ultrasonically cleaned as described above and embedded in
auto-polymerized polymethylmethacrylate (PMMA) resin
(Palapress, Vario, Heraeus Kulzer, Wehrheim, Germany).
The specimens were stored in distilled water at 37 8C for 1
week.
2.3. Shear bond strength test
Specimens were mounted in the jig of the universal testing
machine (Autograph Model AG-50kNG, Shimadzu, Kyoto,
Japan) and the shear force was applied to the core/veneer
ceramic interface until fracture occurred. They were then
loaded at a crosshead speed of 0.5 mm/min and the stress–
strain curve was analysed.
2.4. Failure analysis
Complementary to the bond strength tests, failure modes
were examined at 150# magnification under the scanning
electron microscope (SEM) (JEOL JSM-5200, Kyoto, Japan) at the
fracture site. The failure between the zirconium framework
and margin veneering ceramic was defined as ‘adhesive’. The
failure within either the framework or margin ceramic
material was defined as ‘cohesive’. The term ‘mixed’ failure
was used to describe the combination of these two failure
types.
Fig. 1 – Mean shear bond strength (MPa) of the tested
margin ceramics to zirconia.
2.5. Statistical analysis
Statistical analysis was performed using SPSS 15.0 for
Windows (Chicago, IL, USA). The means of each group were
analysed by one-way analysis of variance (ANOVA). Due to
significant difference between the groups, Tukey’s test was
used to determine the significant differences between ceramic
systems. P values less than 0.05 were considered to be
statistically significant in all tests.
3. Results
Significant effect of margin ceramic types were found on the
bond strength values (P < 0.05). The mean bond strength
values of Ceramco margin ceramic (25.4 ! 4.5 MPa) (P < .05) to
zirconia was significantly lower than those of Cerabien
(31.6 ! 6.4 MPa), e.max (35.9 ! 8.4 MPa), and Triceram margin
ceramic (38.8 ! 7.1 MPa) systems (Fig. 1).
Failure analysis revealed predominantly adhesive type of
failures for Ceramco while in Cerabien, e.max and Triceram
mainly cohesive failures were observed (Table 2). Representa-
tive SEM pictures are presented in Fig. 2a–d.
4. Discussion
In this study, the shear bond strengths of four different margin
ceramics to a zirconia core ceramic were evaluated. Margin
ceramics have been developed to restore the marginal
impurities caused by the inherent shrinkage behavior of
framework materials. Their reduced shrinkage properties as
well as sealing ability for metal or opaque zirconia framework
collar show-through around the cervical region, propose
advantages for clinical use of margin ceramics.13 In addition
to their optical advantages, margin ceramics should basically
also demonstrate good adhesion to their frameworks. In all-
ceramic restorations, compressive and tensile stresses have
been reported to accumulate on heavy load bearing areas like
 journal of dentistry 36 (2008) 822–827 825

Table 2 – Failure types and distribution for each experi- Several factors such as lack of proper framework support,
mental group internal defects, mismatch between the thermal coefficients
Adhesive Cohesive Cohesive Mixed (t) of the veneering and core materials, direction, magnitude
(A) margin substrate (M) and frequency of the applied load, as well as the residual
ceramic ceramic stresses induced by processing, were reported to be respon-
(CMC) (CSC) sible for the cause of fracture of veneering ceramic on ceramic
Cerabien 2 4 0 1 core materials.20–22 Compressive stresses are generated in the
Ceramco 5 0 0 2 veneering ceramic as a result of differences in t of both the
E.max 1 4 0 2 framework and the veneering ceramics.19 Guazzato et al.23
Triceram 1 4 0 2
found that crack propagation occurred very often in the
Adhesive (A) = failure between the zirconium framework and proximity of the interface in the veneering ceramic. This
margin veneering ceramic; cohesive in margin ceramic phenomenon indicates a region of high stress just above the
(CMC) = failure only within the margin ceramic; cohesive in ceramic–core interface, and becomes more apparent at higher
substrate ceramic (CSC) = failure only within the zirconia ceramic; t mismatch between the core and the veneering ceramic.
mixed (M) = combination of A + CMC.
Although t of the three margin ceramics and zirconia frame-
work used in this study were glassy matrix ceramics, t
mismatch of Ceramco-zirconia (9.1 # 10$6 K$1) and zirconia
cervical finish lines.17 The margin ceramics should therefore framework (11 # 10$6 K$1) might have resulted in the sig-
have high bond strengths to their frameworks in order to resist nificantly lower SBS results than those of the other groups. In
these stresses and thereby prevent chipping of the restoration fact, all the ceramics tested were glassy matrix ceramics but
at the cervical region. Thus, the bond strength test was used to particle sizes and t may differ among different brands. In this
evaluate the adhesion of margin ceramic to a zirconia context, it can be anticipated that among the factors affecting
framework. The bond strength values of veneering ceramics the bond strengths of the margin ceramics to the framework
to their core ceramics were reported to range between 23 MPa material, t of the margin ceramics, rather than their chemical
and 41 MPa.18,19 In this study, mean bond strength values of compositions, might have influenced the results obtained.
the tested margin ceramics to zirconia framework ranged Therefore the hypothesis was rejected.
between 25 MPa and 39 MPa. Although the tested ceramics Although failure types may not always correspond to bond
were not veneering ceramics, the results of the present study strength results, SEM images showed mainly adhesive failures
were compared with the results obtained with veneering for Ceramco with which the lowest bond strength results were
ceramic in previous studies since no data on margin ceramic obtained. On the other hand Cerabien, e.max and Triceram,
bond strength to zirconia framework were available in with higher bond strength values, exhibited more frequent
reviewed literature. cohesive failures within the margin ceramic. However, since

Fig. 2 – SEM images (150T) of the typical failure types for each margin ceramic tested: (a) cohesive failure within the margin
ceramic Cerabien; (b) cohesive failure within the margin ceramic Ceramco; (c) mixed failure type in e.max. The arrow
indicates the cohesive failure in the margin ceramic; (d) cohesive failure within the margin ceramic Triceram.
826 journal of dentistry 36 (2008) 822–827
in all groups, also some mixed failures were observed, it
cannot be stated that the shear strength values correlate with
the failure types. The question remains to be answered in
future studies whether the bond strength results or solely the
failure types should be considered to assess the performance
of adhesion. The test method used in this study can still be
considered a practical option to monitor the adhesive
performance of ceramics. Considering the nature of the
mandibular movement against maxilla, shear forces do have
clinical relevance. However, the results should be confirmed
with supplementary data using fatigue tests in more complex
geometries such as an FPD. Also, the behavior in terms of
adhesion and microleakage of margin ceramics cemented to
the dentin warrants further research. To this point, shear bond
test could be considered as a screening test among all battery
of tests.24
Some ceramic systems advise application of liners on the
core ceramic. Selenium-based feldspathic porcelain liners are
used for masking the opaqueness of zirconia core ceramics.
Depending on the test method used, pretreatment of the core
with liners was not shown to affect the bond strength of
veneering ceramic to the core ceramic. While an increasing
effect was found in flexural strength tests,5 the use of a liner
between zirconia and veneering ceramic was not found to
increase the microtensile bond strengths.25 In this study,
manufacturers of some margin ceramics (e.max and Tri-
ceram) required an obligatory liner application at the interface
whereas others were instructed to be applied directly to the
core ceramic without liners. However, the obtained mean
bond strengths for Ceramco for instance did not reveal any
significant differences between liner applied e.max and
Triceram margin ceramics.
From the clinical point of view, the thickness of the core
ceramic is important and small variations can affect the
strength of the restoration.26 It has been suggested that thicker
ceramic cores lead to bulk fractures in veneer ceramics under
fracture resistance tests. Zirconia core (2 mm)–margin cera-
mic (2 mm) ratio in this study was 1:1. When nominal core
ceramic thicknesses (0.5–1 mm) in bilayered all-ceramic
materials are considered in single or multiple unit FPDs, this
may not seem clinically relevant.21 The objective of this study
was solely to observe the adhesion properties of margin
ceramics designed for zirconia framework and make compar-
isons between available products. Nevertheless, the obtained
bond results could be considered sufficient when compared to
bond strengths to the dental tissues. Future studies may
consider also the core–margin ceramic ratio. This may be
particularly important when tooth preparation has wider
finish lines especially when the abutment teeth are prepared
more than once such as replacement of existing metal–
ceramic FPDs with zirconia-based ceramic materials. Further-
more, the right choice and use of margin ceramics may
eliminate chipping problems at the cervical margins of
zirconia FPDs.
5. Conclusions
Margin ceramics, compatible with zirconia framework mate-
rial tested in the present study, exhibited high bond strength
values. Variations in thermal expansion coefficients might
influence the bond strength values of margin ceramics to
zirconia.
Acknowledgements
The authors would like to thank Stephan Fiorillo, master
technician from IvoclarVivadent for supplying the zirconia
frameworks and ZirkonZahn Asya Dental Laboratory, İstan-
bul, Türkiye for the processing of the zirconia specimens.
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