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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
Ege University, School of Dentistry, Department of Prosthodontics, Izmir, Turkey
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

Magnesia (MgO), Yttria (Y2O3), and Calcia (CaO) are added to
Various types of reinforced ceramic framework materials have zirconia in order to stabilize their tetragonal and/or cubic
been introduced in restorative dentistry in an attempt to phases to form partially stabilized zirconia. When zirconia
improve the mechanical properties of ceramics.1–5 One such polycrystal is processed with yttria, yttrium-stabilized tetra-
example is zirconium dioxide (hereon: zirconia)-based mate- gonal zirconium polycrystal (Y-TZP) is obtained.5 The high
rials. Zirconia is a biocompatible material with excellent initial strength and fracture toughness of zirconia results from
mechanical properties and low bacterial adhesion properties. a physical property of partially stabilized zirconia known as
Restorations made of this material can be cemented with 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.
journal of dentistry 36 (2008) 822–827 823

Zirconia frameworks can be fabricated mainly with the well as resistance to chewing forces. Their shrinkage after
help of CAD/CAM or copy-milling techniques by means of firing/sintering has been minimized. Moreover, fluorescent
grinding a zirconia block. These blocks can be milled either in agents are added to optimize their aesthetics and opacity has
the green, pre-sintered or completely sintered stage.7,8 Frame- been balanced to mask the show-through of the more opaque
works made from green and pre-sintered zirconia are milled in framework.13 In a recent clinical study on zirconia FPDs, the
an enlarged form to compensate for the shrinkage that occurs overall survival rate was found to be 73.9% with marginal
during sintering, which usually equals to 20–25% for partially integrity problems and thereby secondary caries (21.7%) and
sintered frameworks.9,10 Completely sintered Y-TZP blocks are ceramic chipping (15.2%) being major causes of failure.17 Also,
prepared by pre-sintering at temperatures below 1500 8C and the most common chippings were observed at the cervical
then processed by hot isostatically pressed (HIP) technique at areas of the reinforced all ceramic fixed-partial-dentures
temperatures between 1400 and 1500 8C under high pressure (FPDs).14
in an inert gas atmosphere. This leads to a very high density in It has been previously demonstrated that marginal dis-
excess of 99% of the theoretical density.5 The blocks can then crepancies of conventional metal–ceramic systems decreased
be machined using a specially designed milling system. after the application of margin ceramics.15 Although it is not
The milling of pre-sintered zirconia blocks is faster and commonly practiced, such marginal ceramics, made of either
causes less mechanical damage to the material than milling of feldspath or fluoroapatite, are also available to be used in
fully sintered blocks.6 Compared to the milling method based on conjunction with zirconia FPDs. Since cervical areas of the FPDS
pre-sintering, milling of fully sintered zirconia blocks is a time were reported to be more prone to stresses,16 the adhesion of
consuming process that causes greater wear of the diamond such margin ceramics to the core ceramic is of clinical
burs and is more expensive. Moreover, it has recently been importance in order not to experience chippings after cementa-
reported that questions remained regarding to the surface state tion. No study to date evaluated their durability on zirconia.
after hard machining of Y-TZP, while soft machining seemed to Although with fluoroapatite ceramic, high degree of luminous
lead to a more consistent final state, provided that the reflectance and high translucency could be delivered, since they
machined restoration was left intact after sintering.5 Hence, are all glassy matrix ceramics, it can be hypothesized that both
green-stage zirconia could be considered advantageous. feldspath or fluoroapatite types of margin ceramics would
The milled frameworks are then veneered with feldspar or perform comparable bond strength to zirconia.
glassy matrix ceramics appropriate for the zirconia ceramic Therefore, the objectives of this study were to compare the
used. However, the mechanical properties of zirconia ceramic adhesion of four individual margin ceramics to a processed
are affected during the veneering stage performed at relatively zirconia framework and evaluate the failure modes after
higher temperatures.11 The framework suffers from distortion debonding.
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 2. Materials and methods
shown to influence the long-term success of restorations.11 In
terms of longevity, the clinically acceptable range of marginal Core/margin ceramic combinations (N = 28, n = 7 per group)
discrepancies is "120 mm. On the other hand, in CAD/CAM or were fabricated by one experienced dental technician accord-
copy-milling systems, the marginal opening has been reported ing to each manufacturer’s instructions. The brand names,
to range between 60 mm and 300 mm.11,12 types, compositions, manufacturer and batch numbers of the
Margin ceramics are therefore formulated to compensate margin ceramics, modelling liquid and liners used in this
for the marginal impurities in order to maintain accurate fit as 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
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 Fig. 1 – Mean shear bond strength (MPa) of the tested
required an obligatory liner application at the interface margin ceramics to zirconia.
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 2.5. Statistical analysis
by each manufacturer. The mould was carefully filled with the
creamy mixture of margin ceramic and condensed. Excess Statistical analysis was performed using SPSS 15.0 for
liquid was removed by applying a piece of adsorbing paper Windows (Chicago, IL, USA). The means of each group were
(Kimwipes1Lite 200, Kimberly Clark Corp., Roswell, GA, USA) analysed by one-way analysis of variance (ANOVA). Due to
onto the surface of the specimen. After condensation, the significant difference between the groups, Tukey’s test was
mould was removed, leaving the non-sintered specimen used to determine the significant differences between ceramic
behind on the platinum foil. The test specimens on the systems. P values less than 0.05 were considered to be
platinum foil, were then transferred to a firing tray, and statistically significant in all tests.
sintered in a calibrated ceramic furnace (Programat P90,
Ivoclar, Schaan, Liechtenstein) in accordance with each
manufacturer’s instructions. Following the firing process, 3. Results
the specimens were tried in the mould for minor adjustments,
ultrasonically cleaned as described above and embedded in Significant effect of margin ceramic types were found on the
auto-polymerized polymethylmethacrylate (PMMA) resin bond strength values (P < 0.05). The mean bond strength
(Palapress, Vario, Heraeus Kulzer, Wehrheim, Germany). values of Ceramco margin ceramic (25.4 ! 4.5 MPa) (P < .05) to
The specimens were stored in distilled water at 37 8C for 1 zirconia was significantly lower than those of Cerabien
week. (31.6 ! 6.4 MPa), e.max (35.9 ! 8.4 MPa), and Triceram margin
ceramic (38.8 ! 7.1 MPa) systems (Fig. 1).
2.3. Shear bond strength test Failure analysis revealed predominantly adhesive type of
failures for Ceramco while in Cerabien, e.max and Triceram
Specimens were mounted in the jig of the universal testing mainly cohesive failures were observed (Table 2). Representa-
machine (Autograph Model AG-50kNG, Shimadzu, Kyoto, tive SEM pictures are presented in Fig. 2a–d.
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– 4. Discussion
strain curve was analysed.
In this study, the shear bond strengths of four different margin
2.4. Failure analysis ceramics to a zirconia core ceramic were evaluated. Margin
ceramics have been developed to restore the marginal
Complementary to the bond strength tests, failure modes impurities caused by the inherent shrinkage behavior of
were examined at 150# magnification under the scanning framework materials. Their reduced shrinkage properties as
electron microscope (SEM) (JEOL JSM-5200, Kyoto, Japan) at the well as sealing ability for metal or opaque zirconia framework
fracture site. The failure between the zirconium framework collar show-through around the cervical region, propose
and margin veneering ceramic was defined as ‘adhesive’. The advantages for clinical use of margin ceramics.13 In addition
failure within either the framework or margin ceramic to their optical advantages, margin ceramics should basically
material was defined as ‘cohesive’. The term ‘mixed’ failure also demonstrate good adhesion to their frameworks. In all-
was used to describe the combination of these two failure ceramic restorations, compressive and tensile stresses have
types. 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 values. Variations in thermal expansion coefficients might
cannot be stated that the shear strength values correlate with influence the bond strength values of margin ceramics to
the failure types. The question remains to be answered in zirconia.
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 Acknowledgements
considered a practical option to monitor the adhesive
performance of ceramics. Considering the nature of the The authors would like to thank Stephan Fiorillo, master
mandibular movement against maxilla, shear forces do have technician from IvoclarVivadent for supplying the zirconia
clinical relevance. However, the results should be confirmed frameworks and ZirkonZahn Asya Dental Laboratory, İstan-
with supplementary data using fatigue tests in more complex bul, Türkiye for the processing of the zirconia specimens.
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
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