journal of dentistry 36 (2008) 822827

available at www.sciencedirect.com

journal homepage: www.intl.elsevierhealth.com/journals/jden

Evaluation of bond strength of various margin ceramics

to a zirconia ceramic
M. Erhan Comlekoglu a,*, Mine Dundar a, Mutlu Ozcan b, M. Ali Gungor a,
Bulent Gokce a, Celal Artunc a
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

Various types of reinforced ceramic framework materials have

been introduced in restorative dentistry in an attempt to
improve the mechanical properties of ceramics.15 One such
example is zirconium dioxide (hereon: zirconia)-based materials. Zirconia is a biocompatible material with excellent
mechanical properties and low bacterial adhesion properties.
Restorations made of this material can be cemented with

conventional cements.4 Several different oxides such as

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 tetragonal 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. Comlekoglu).
0300-5712/$ see front matter # 2008 Elsevier Ltd. All rights reserved.
doi:10.1016/j.jdent.2008.05.019

823

journal of dentistry 36 (2008) 822827

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 Frameworks 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 2025% 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 discrepancies of conventional metalceramic 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 cementation. 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 according to each manufacturers 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, build-up liquid
and liner

Ceramic type

Chemical composition

Manufacturer

Batch number

MB3 OD612

Cerabien Zr

Feldspathic

SiO2, Al2O3, Na2O, CaOK2O,

MgO, LiO2, B2O3, pigments

Noritake Dental Supply Co.,

Nagoya, Japan

Cerabien Zr forming liquid

Ceramco PFZ

Feldspathic

SiO2, Al2O3, Na2O, K2O,

SnO2, CeO2, pigments,
1.3-Butanediol Xi

Ceramco, Burlington,
NJ, USA

Ceramco PFZ margin liquid

E.max margin

Fluorapatite

SiO2, Al2O3, Na2O, K2O,

ZnO, CaO, P2O5, F, oxides,
pigments

IvoclarVivadent,
Schaan, Liechtenstein

E.max Zir liner build-up liquid

E.max margin build-up liquid
E.max Zir liner 2
Triceram

Feldspathic

SiO2, Al2O3, K2O, Na2O,

Li2O, CaO, BaO, MgO, B2O3, F

Dentaurum, Ispringen,
Germany

APEJQ
A3-06002487

06003649
JO6301

H33669
H32689
H12845
SMA 003F

824

2.1.

journal of dentistry 36 (2008) 822827

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
manufacturers 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, Tukeys 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). Representative SEM pictures are presented in Fig. 2ad.

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 allceramic restorations, compressive and tensile stresses have
been reported to accumulate on heavy load bearing areas like

journal of dentistry 36 (2008) 822827

Table 2 Failure types and distribution for each experimental group

Cerabien
Ceramco
E.max
Triceram

Adhesive
(A)

Cohesive
margin
ceramic
(CMC)

Cohesive
substrate
ceramic
(CSC)

2
5
1
1

4
0
4
4

0
0
0
0

Mixed
(M)

1
2
2
2

Adhesive (A) = failure between the zirconium framework and

margin veneering ceramic; cohesive in margin ceramic
(CMC) = failure only within the margin ceramic; cohesive in
substrate ceramic (CSC) = failure only within the zirconia ceramic;
mixed (M) = combination of A + CMC.

cervical finish lines.17 The margin ceramics should therefore

have high bond strengths to their frameworks in order to resist
these stresses and thereby prevent chipping of the restoration
at the cervical region. Thus, the bond strength test was used to
evaluate the adhesion of margin ceramic to a zirconia
framework. The bond strength values of veneering ceramics
to their core ceramics were reported to range between 23 MPa
and 41 MPa.18,19 In this study, mean bond strength values of
the tested margin ceramics to zirconia framework ranged
between 25 MPa and 39 MPa. Although the tested ceramics
were not veneering ceramics, the results of the present study
were compared with the results obtained with veneering
ceramic in previous studies since no data on margin ceramic
bond strength to zirconia framework were available in
reviewed literature.

825

Several factors such as lack of proper framework support,

internal defects, mismatch between the thermal coefficients
(t) of the veneering and core materials, direction, magnitude
and frequency of the applied load, as well as the residual
stresses induced by processing, were reported to be responsible for the cause of fracture of veneering ceramic on ceramic
core materials.2022 Compressive stresses are generated in the
veneering ceramic as a result of differences in t of both the
framework and the veneering ceramics.19 Guazzato et al.23
found that crack propagation occurred very often in the
proximity of the interface in the veneering ceramic. This
phenomenon indicates a region of high stress just above the
ceramiccore interface, and becomes more apparent at higher
t mismatch between the core and the veneering ceramic.
Although t of the three margin ceramics and zirconia framework used in this study were glassy matrix ceramics, t
mismatch of Ceramco-zirconia (9.1  10 6 K 1) and zirconia
framework (11  10 6 K 1) might have resulted in the significantly lower SBS results than those of the other groups. In
fact, all the ceramics tested were glassy matrix ceramics but
particle sizes and t may differ among different brands. In this
context, it can be anticipated that among the factors affecting
the bond strengths of the margin ceramics to the framework
material, t of the margin ceramics, rather than their chemical
compositions, might have influenced the results obtained.
Therefore the hypothesis was rejected.
Although failure types may not always correspond to bond
strength results, SEM images showed mainly adhesive failures
for Ceramco with which the lowest bond strength results were
obtained. On the other hand Cerabien, e.max and Triceram,
with higher bond strength values, exhibited more frequent
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) 822827

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 Triceram) 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 ceramic (2 mm) ratio in this study was 1:1. When nominal core
ceramic thicknesses (0.51 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 comparisons 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 coremargin 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. Furthermore, 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 material 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, Istanbul, Turkiye for the processing of the zirconia specimens.

references

1. Kelly JR, Nishimura I, Campbell SD. Ceramics in dentistry:

historical roots and current perspectives. Journal of Prosthetic
Dentistry 1996;75:1832.
2. Libby G, Arcuri MR, La Velle WE, Hel L. Longevity of fixed
partial dentures. Journal of Prosthetic Dentistry 1997;78:
12731.
3. Strub JR, Stiffler S, Scharer P. Causes of failure following oral
rehabilitation: biological versus technical factors.
Quintessence International 1988;19:21522.
4. Ernst CP, Cohnen U, Stender E, Willershausen B. In vitro
retentive strength of zirconium oxide ceramic crowns using
different luting agents. Journal of Prosthetic Dentistry
2005;93:5518.
5. Denry I, Kelly JR. State of the art of zirconia for dental
applications. Dental Materials 2008;24:299307.
6. Piconi C, Maccauro G. Zirconia as a ceramic biomaterial, a
review. Biomaterials 1999;29:125.
7. Filser F, Kocher P, Weibel F, Luthy H, Scharer P, Gauckler LJ.
Reliability and strength of all-ceramic dental restorations
fabricated by direct ceramic machining (DCM). International
Journal of Computerized Dentistry 2001;4:89106.
8. Hannink RH, Kelly PM, Muddle BC. Transformation
toughening in zirconia-containing ceramics. Journal of
American Ceramic Society 2000;83:46187.
9. Raigrodski AJ, Chiche GJ, Potiket N, Hochstedler JL,
Mohamed SE, Billiot S, et al. The efficacy of posterior threeunit zirconium-oxide-based ceramic fixed partial dental
prostheses: a prospective clinical pilot study. Journal of
Prosthetic Dentistry 2006;96:23744.
10. Sundh A, Molin M, Sjogren G. Fracture resistance of yttrium
oxide partially-stabilized zirconia all-ceramic bridges after
veneering and mechanical fatigue testing. Dental Materials
2005;21:47682.
11. Komine F, Gerds T, Witkowski S, Strub JR. Influence of
framework configuration on the marginal adaptation of
zirconium dioxide ceramic anterior four-unit frameworks.
Acta Odontologica Scandinavia 2005;63:3616.
12. Nakamura T, Dei N, Kojima T, Wakabayashi K. Marginal
and internal fit of CEREC 3 CAD/CAM all-ceramic
crowns. International Journal of Prosthodontics 2003;16:
2448.
13. Schonenberger AJ, Felice A, Cossu M. Improving the
precision of esthetic ceramic margins: guidelines for
success. Journal of Esthetic and Restorative Dentistry
1994;6:14350.
14. Sailer I, Feher A, Filser F, Gauckler LJ, Luthy H, Hammerle
CH. Five-year clinical results of zirconia frameworks for
posterior fixed partial dentures. International Journal of
Prosthodontics 2007;20:3838.
15. OBoyle KH, Norling BK, Cagna DR, Phoenix RD. An
investigation of new metal framework design for metal

journal of dentistry 36 (2008) 822827

16.

17.

18.

19.

20.
21.

ceramic restorations. Journal of Prosthetic Dentistry

1997;78:295301.
Di Iorio D, Murmura G, Orsini G, Scarano A, Caputi S. Effect
of margin design on the fracture resistance of Procera allceram cores: an in vitro study. Journal of Contemporary Dental
Practice 2008;1:18.
Gungor MA, Kucuk M, Dundar M, Karaoglu C, Artunc C.
Effect of temperature and stress distribution on all-ceramic
restorations by using a three-dimensional finite element
analysis. Journal of Oral Rehabilitation 2004;31:1728.
Aboushelib MN, Jager N, Kleverlaan CJ, Feilzer AJ.
Microtensile bond strength of different components of core
veneered all-ceramic restorations. Dental Materials
2005;21:98491.
Anusavice KJ, Dehoff PH, Fairhurst CW. Comparative
evaluation of ceramicmetal bond tests using finite element
stress analysis. Journal of Dental Research 1980;59:60813.
Lawn BR. Fracture of Brittle Solids. 2nd ed. Cambridge:
Cambridge University Press; 1993. p. 739.
Wakabayashi N, Anusavice KJ. Crack initiation modes in
bilayered alumina/porcelain disks as a function of core/

22.

23.

24.

25.

26.

827

veneer thickness ratio and supporting substrate stiffness.

Journal of Dental Research 2000;79:1398404.
Sobrinho LC, Cattell MJ, Glover RH, Knowles JC.
Investigation of the dry and wet fatigue properties of three
all-ceramic crown systems. International Journal of
Prosthodontics 1998;11:25562.
Guazzato M, Albakry M, Quach L, Swain MV. Influence of
surface and heat treatments on the flexural strength of a
glass-infiltrated alumina/zirconia-reinforced dental
ceramic. Dental Materials 2005;21:45463.
zcan M. Adhesion of resin composites to biomaterials
O
in dentistry: an evaluation of surface conditioning
methods.. Groningen, The Netherlands: Facilitairbedrijf;
2003. p. 143-144.
zcan M, Gokce B, Comlekoglu E, Leite F,
Dundar M, O
Valandro LF. Comparison of two bond strength testing
methodologies for bilayered all-ceramics. Dental Materials
2007;23:6306.
Chai J, Tkahashi Y, Sulaiman F, Chong K, Lautenschlager EP.
Probability of fracture of all-ceramic crowns. International
Journal of Prosthodontics 2000;13:4204.