d e n t a l m a t e r i a l s 3 0 ( 2 0 1 4 ) e147–e162

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

Review

Aspects of bonding between resin luting cements

and glass ceramic materials

Tian Tian a , James Kit-Hon Tsoi b , Jukka P. Matinlinna b ,

Michael F. Burrow a,∗
a Oral Diagnosis and Polyclinics, Faculty of Dentistry, University of Hong Kong, Prince Philip Dental Hospital, Hong
Kong
b Dental Materials Science, Faculty of Dentistry, University of Hong Kong, Hong Kong

a r t i c l e i n f o a b s t r a c t

Article history: Objectives. The bonding interface of glass ceramics and resin luting cements plays an impor-
Received 7 January 2013 tant role in the long-term durability of ceramic restorations. The purpose of this systematic
Accepted 30 January 2014 review is to discuss the various factors involved with the bond between glass ceramics and
resin luting cements.
Methods. An electronic Pubmed, Medline and Embase search was conducted to obtain lab-
Keywords: oratory studies on resin–ceramic bonding published in English and Chinese between 1972
Glass ceramics and 2012.
Resin luting cements Results and discussion. Eighty-three articles were included in this review. Various factors that
Laboratory tests have a possible impact on the bond between glass ceramics and resin cements were dis-
Bonding cussed, including ceramic type, ceramic crystal structure, resin luting cements, light curing,
Systematic review surface treatments, and laboratory test methodology.
Conclusions. Resin–ceramic bonding has been improved substantially in the past few years.
Hydrofluoric acid (HF) etching followed by silanizaiton has become the most widely accepted
surface treatment for glass ceramics. However, further studies need to be undertaken to
improve surface preparations without HF because of its toxicity. Laboratory test methods are
also required to better simulate the actual oral environment for more clinically compatible
testing.
© 2014 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Contents

1. Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . e148
2. Materials and methods . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . e148
2.1. Search strategy . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . e148
2.2. Articles reviewed and data extraction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . e148

∗
Corresponding author at: Oral Diagnosis and Polyclinics, Faculty of Dentistry, University of Hong Kong, Prince Philip Dental Hospital, 34
Hospital Road, Sai Ying Pun, Hong Kong. Tel.: +85 28590553; fax: +85 28582532.
E-mail address: mfburr58@hku.hk (M.F. Burrow).
0109-5641/$ – see front matter © 2014 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.dental.2014.01.017
e148 d e n t a l m a t e r i a l s 3 0 ( 2 0 1 4 ) e147–e162

3. Results . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . e149
4. Discussion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . e149
4.1. Ceramics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . e149
4.2. Resin cements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . e149
4.2.1. The effect of resin cement on the ceramic-resin bond . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . e150
4.2.2. The effect of external factors on resin cements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . e150
4.3. Surface treatment. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . e151
4.3.1. Chemical conditioning methods . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . e151
4.3.2. Mechanical conditioning methods . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . e152
4.3.3. Comparison between different surface treatments . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . e153
4.4. Laboratory methodology . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . e153
4.4.1. Tensile and shear bond strength test . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . e153
4.4.2. Microshear & microtensile bond strength test . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . e158
4.4.3. Thermocycling and loadcycling . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . e158
4.4.4. Storage conditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . e158
5. Conclusion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . e159
Appendix A. Supplementary data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . e159
References. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . e159

micromechanical attachment and chemical bonding.

1. Introduction Micromechanical attachment can be created by acid etching
[10] and/or sandblasting [11], whilst a silane coupling agent
All-ceramic materials are well known for the esthetic abil- provides a chemical bond [12]. Various glass ceramics differ
ity of imitating tooth color. Recent developments in ceramic in chemical conformation and microstructure, so it might be
restoration fabrication techniques came about with ceram- necessary to establish bonding procedures according to the
ics possessing higher strength and toughness [1], making it glass ceramic type.
possible for wider applications in dentistry such as veneers, The ceramic and resin cement bond is subjected to a com-
inlays/onlays or dental implants [2–4]. plex environment in the oral cavity being influenced by several
Nowadays, there are increasing cases where the reten- extrinsic factors such as temperature change, saliva, daily food
tion of restorations is reliant on bonding, e.g. resin-bonded and drink intake, biting force and other habits. Consequently,
bridges. Hence, the quality of bonding is of increasing impor- laboratory testing should simulate these variables to enable
tance, and is a dominant factor required for the long-term the development of superior materials and surface prepara-
success of glass ceramic restorations. Compared with tra- tion methods that provide long-term durable bond strengths
ditional cements such as polycarboxylate or glass ionomer in the oral environment.
cement, resin luting cements were introduced to aid all- The aim of this systematic review was to evaluate lab-
ceramic restoration retention [5]. Resin cements not only oratory studies investigating the resin luting cement (resin
provide stronger and more durable bonding between ceramics cement) bond to dental ceramics.
and teeth, but can also achieve better esthetic outcomes and
maintain higher ceramic strength [6].
Ceramics in dentistry can be generally classified into
“oxide ceramics” and “glass ceramics” based on the chem- 2. Materials and methods
ical composition. Oxide ceramics are defined as a group of
ceramics containing not more than 15% silica with little or 2.1. Search strategy
no glass phase [7]. They can be subclassified into aluminium-
oxide/alumina ceramics, including glass-infiltrated alumina A search of the Pubmed library, Medline, Embase and the
ceramics, densely sintered alumina ceramic systems, and Cochrane library was performed on the literature available
zirconium-oxide/zirconia ceramics, including glass-infiltrated from 1972 to April 18, 2012. The keywords used were: ‘bond’,
and densely sintered zirconia ceramic systems. Because of ‘bonding’, ‘adhesive’, ‘adhesion’, ‘luting’, ‘resin cement’, ‘resin
their stable chemical structure, oxide ceramics have signifi- composite’, luting composite’, ‘luting agent’, ‘luting resin’,
cantly improved mechanical properties [8] and can be called ‘porcelain’, ‘ceramic’, ‘ceramics’. English and Chinese papers
“high strength core ceramics”. However, the surface cannot be were included in this search.
etched by hydrofluoric acid (HF), which is the usual chemical
means to condition the surface to obtain micro-mechanical
adhesion. These oxide ceramics are known as “acid-resistant 2.2. Articles reviewed and data extraction
ceramics” [9]. Nevertheless, caution should be drawn in using
such terminology as recent studies have only tested this type The included articles were independently reviewed by two
of ceramic with HF but not other acids. reviewers. Inclusion criteria were studies that evaluated bond-
It is accepted that adhesion between ceramics and ing aspects between the resin cement and glass ceramic
resin cements is provided by two major mechanisms: interface in laboratory tests;
 d e n t a l m a t e r i a l s 3 0 ( 2 0 1 4 ) e147–e162
Exclusion criteria were studies on:
(1) alumina-based or zirconia-based ceramic;
(2) brackets, posts or implants;
(3) evaluating ceramic/porcelain repair systems;
(4) tooth preparation, tooth conditioning, and resin-
enamel/dentin bonding;
3. Results
After searching and screening the database, a total of 83 arti-
cles were included. Owing to the high heterogeneity of studies
regarding preparation of materials, methods of testing and
outcome variables, it was not possible to analyze the data
quantitatively. Articles are summarized in Section 4 concern-
ing factors related to the ceramic-resin bond.
4. Discussion
4.1. Ceramics
Glass ceramics, also termed silica-based ceramics [13,14], are a
group of materials that have been widely used for all-ceramic
restorations since the 1970s. These can be further classified
as feldspathic, leucite-reinforced, fluormica glass or lithium
disilicate ceramic. HF etching has a distinctive effect on the
surface of these ceramics creating a uniformly porous surface
[9]. This distinctive effect has made this group of glass ceram-
ics dominate resin-bonded ceramic restoration construction
and therefore glass ceramics are the focus of the present
review.
Despite glass ceramics exhibiting lower mechanical
strength than oxide ceramics, the fracture resistance has
been shown to increase with resin cementation [15,16]. One
study suggested that using a relatively thin layer (approxi-
mately 100 ␮m) of resin cement bonded to leucite-reinforced
and lithium disilicate ceramics on HF treated surfaces and
silanization could significantly increase the biaxial flexural
strength compared with ceramics with the same surface
preparations but without resin cement application [16].
Several studies have suggested that various glass ceramic
types may produce different microstructures after different
surface treatments, which can consequently affect the bond
strength between ceramic and resin cement [17–22]. It was
demonstrated that a feldspathic ceramic exhibited a signif-
icantly higher shear bond strength than a leucite-reinforced
ceramic when luted with the same resin cement after 20,000
thermocycles [21]. When comparing leucite-reinforced and
lithium disilicate ceramic, one study [22] showed a resin
cement which luted to a leucite-reinforced ceramic had a
higher Vickers hardness. The authors attributed the differ-
ence to the variation of microstructure in the two ceramic
types. The SEM image of HF-etched lithium disilicate glass
ceramics showed a surface with a scaffold-like structure, com-
prising many small interlocking needle-like crystals without
orientation. Further, a second crystalline phase, consisting of
a lithium orthophosphate (Li3 PO4 ) of a much lower volume
was also reported. On the other hand, the microstructure of
HF-etched leucite-reinforced ceramic was less dense in crystal
structure and characterized by single leucite crystals, without
e149
interlocking between crystals. However, a further study
showed that the microtensile bond strength was significantly
higher for lithium disilicate ceramics than leucite-reinforced
ceramics with the same surface preparation [17]. It seems
there is little correlation between the hardness of resin cement
and the resin–ceramic bond strength. It is also worth noting
that a single application of silane coupling agent produced
the highest bond strength in the leucite-reinforced ceramic,
while HF acid etching combined with silanization created the
highest bond strength in the lithium disilicate ceramic. Thus,
ceramic type may need different surface preparation meth-
ods for optimal adhesion, however, no further explanation
was presented [17]. Another study [18] compared the micros-
hear bond strength between two leucite-reinforced ceramics,
GN-I® (GC Corporation, Tokyo, Japan) and ProCADTM (Ivoclar
Vivadent, Schaan, Liechtenstein). The results showed that
when using the same silane application, GN-I® presented a
higher bond strength than ProCADTM . Nevertheless, no com-
parison of chemical composition or microstructure of these
two materials was performed. Thus, it is unclear regarding
the exact mechanism of how the surface morphology of these
glass ceramics affected the resin–ceramic bond.
The different surface morphology of ceramics may also
affect adhesion. It was shown with the same unconditioned
glass ceramic surface, the microtensile bond strength of
RelyXTM Unicem (3M Espe AG, Seefeld, Germany) was sig-
nificantly higher than that of Multilink (Ivoclar Vivadent,
Schaan, Liechtenstein) and Panavia F (Kuraray Medical Inc.,
Tokyo, Japan). However, after HF etching and silanization of
the ceramic, statistically higher microtensile bond strength
values for RelyXTM Unicem and Multilink were obtained com-
pared with Panavia F. This suggests different resin cements
may have an individual bonding capability by varying surface
morphology with various surface treatments [23].
Ceramic translucency has been reported to have an effect
on the cured resin hardness [22,24–30]. Numerous factors
affect ceramic translucency, including thickness [31], crys-
talline structure [32], number of firings, repeated staining
cycles [33,34], grain size, pigment, number, size and distri-
bution of defects, and shade [35,36]. Results showed that
increasing thickness and opacity of glass ceramics produced
a statistically significant decrease in hardness of tested resin
cements [25,29,30]. Although the translucency of the ceramic
may affect resin cement polymerization, it seems to have no
or little effect on the bond strength between resin cement and
ceramic. It was illustrated that ceramic thickness, polymeriza-
tion mode, storage time, or combinations of these parameters
did not influence shear bond strength between lithium disili-
cate ceramics and resin cements [37].
4.2. Resin cements
The cementation procedure also plays a significant role in
the clinical success of indirect fixed restorations. The resin
cement links the restoration and tooth. Resin luting cements
can be classified as light-cured, self/auto-cured or dual-
cured based on polymerization mode, without considering the
dentin pretreatment method.
Since the 1970s, resin cements have been used to lute glass
ceramic restorations [7]. Resin cements exhibit some clinical
e150 d e n t a l m a t e r i a l s 3 0 ( 2 0 1 4 ) e147–e162
advantages over other conventional luting cements, e.g. zinc
phosphate, polycarboxylate and glass ionomer cements. Resin
cements can provide a clinically acceptable margin after
fatigue testing that has been shown to minimize leakage and
thus reduce the risk of caries and restoration failure [38]. Resin
cements have various shades that can offer a more natural
esthetic appearance compared with opaque conventional lut-
ing cements [39]. The requirement for a retentive tooth prepa-
ration is reduced for resin cements because of their adhesion
properties, thus preserving healthy tooth structure [5].
4.2.1. The effect of resin cement on the ceramic-resin bond
Resin cements exhibit a diverse bonding potential with glass
ceramics. Higher shear bond strengths were obtained when
using Variolink II (Ivoclar Vivadent, Schaan, Liechtenstein) or
RelyX Unicem bonded to HF etched and silanized lithium dis-
ilicate ceramics after thermocycling, compared to Panavia F
[40]. This result was supported by another study [23] using
the same ceramics and surface treatments. That study [23]
showed groups bonded with Multilink or RelyXTM Unicem had
higher microtensile bond strengths than the group bonded
with Panavia F in thermocycled conditions. Similar results
were also found in HF-etched and a silanized feldspathic
ceramic which were cemented with Noribond DC (Noritake
Dental Supply, Inc., Aichi, Japan) or Variolink II exhibited sig-
nificantly higher shear bond strengths than Panavia 21 for 3
and 150 days water storage [41]. Another study using ther-
mocycling showed Variolink II had a statistically higher shear
bond strength to lithium disilicate ceramics than Panavia 21,
Panavia F, RelyX Unicem and RelyX ARC groups [42]. However,
in that study, the surface treatments of the ceramic-cement
groups were inconsistent: Variolink II and RelyXTM ARC groups
used HF acid-treatment then silanization; for Panavia 21 and
Panavia F groups, phosphoric acid treatment and silaniza-
tion were used, and the RelyXTM Unicem group were directly
cemented without any surface treatment. Such variations in
surface treatment methods may lead to bias of the results
and invalidate comparisons. It seems that although Panavia
is regarded as a gold standard for resin cements, it shows rel-
atively low bond strength compared with other resin cements.
Some studies explained that the poor bonding performance of
Panavia F was due to the inhibition of polymerization by acidic
monomers present in the cement [43].
Resin cement factors that may influence the resin–ceramic
bond, including curing mode, elastic modulus, color shade and
the thickness have limited information available.
Compared with light-cured and dual-cured resin cements,
it was concluded that light activated materials performed bet-
ter than dual-cured cements [29]. Other studies showed that
dual-cured resin cements exhibited significantly higher extru-
sion shear bond strengths with a feldspathic ceramic than the
corresponding bond strengths for an auto-cured cement [44].
The elastic modulus of the luting agent seems to have
little effect on the stresses in a ceramic crown. A finite ele-
ment analysis study showed that when a resin cement with a
higher elastic modulus was replaced with a low elastic mod-
ulus cement, the magnitude of tensile stresses in the glass
ceramic did not decrease [45]. Another study observed there
might be a strong positive linear relationship between the
mean biaxial flexural strength of the feldspathic ceramics and
the flexural elastic modulus of different resin cements [46].
This indicated that the elastic modulus of resin cements may
have an effect on the strengthening of ceramics. However,
in that study [46], the ceramic surfaces were not condition-
ing, and may not reflect the clinical situation. Thus, further
research on the effect and relationship of resin cement elastic
modulus on surface treated ceramics is needed.
The shade of resin cement has little effect on the bond
between either ceramic or dentin. A microtensile bond test
compared two different shades of a dual-cured resin cement,
Variolink II, A3 and transparent (Tr), bonded to a feldspathic
ceramic. No significant difference was found between these
two shades using the same curing light and storage period (no
storage and 150 days storage) [47].
The bond strength between glass ceramics and resin
cements was postulated to decrease with an increase of resin
cement film thickness [48]. A finite element model experiment
demonstrated that an increase of cement thickness from 10 to
180 ␮m resulted in higher stresses developing within the resin
cement. This study further investigated, and showed, a resin
cement thickness less than 50 ␮m might create a better bond
to a glass ceramic compared to a film thickness of greater than
50 ␮m [49].
4.2.2. The effect of external factors on resin cements
Except for resin cement there can be other influential factors
for resin–ceramic bonding, some external factors, such as the
ceramic (which was discussed in the ceramic section) and the
light curing unit, can also have an impact on the polymeriza-
tion of resin cements and potentially affect the bond between
a resin cement and ceramic.
Three common types of light curing units are commercially
available, namely quartz halogen (QTH: quartz tungsten halo-
gen), light emitting diode (LED) and Xenon plasma arc (PAC).
QTH lights are the original device commonly used to acti-
vate resin-based materials. Nevertheless, several drawbacks
of QTH lights were found in the last decade, such as a limited
effective working time of around 100 h [50]. The heat gener-
ated in the bulb lead to the bulb degradation and ultimately
reduced polymerization capacity [51,52]. The LED system was
proposed for light curing to overcome the drawbacks of the
QTH. Compared with QTH lights, LED lights has the advantage
such as smaller size, lighter, lower heat and noise generation,
greater longevity of the output intensity and unit, and less
consumption of electricity [47]. Plasma-arc curing lights are
designed for high-speed polymerization which is a significant
time saving of the curing procedure, but the heat generated
can be high [53].
No difference in microtensile bond strength was found
between QTH and LED light-cured resin cements when stud-
ied [47]. Similar results were observed in a shear bond strength
study of a resin cement to ceramic and dentin when the
cement was polymerized using QTH light in standard mode
and a high-powered (1100 mW/cm2 ) LED light in exponen-
tial mode. However, the shear bond strength was significantly
lower when cured using LED in the fast and pulse modes. This
implies the light output energy of an LED unit may influence
the resin cement curing [51]. Further, higher hardness, were
observed with an LED compared with a QTH light [54] whilst
another study showed no difference between these two types
 d e n t a l m a t e r i a l s 3 0 ( 2 0 1 4 ) e147–e162
of curing unit [30]. The possible reason might be due to the
different time duration of light curing. When comparing QTH
light and plasma arc light units, 60-s QTH light source pro-
duced microtensile bond strength greater than those achieved
with a 9-s exposure with the plasma arc light [55].
It is worth noting that the long-term duration of
resin–ceramic bonding does not completely rely on a high
degree of polymerization and cement mechanical properties.
A longer and higher intensity of light exposure may enhance
the polymerization of the resin cement, but it may cause more
rapid shrinkage of the material which might be detrimental to
the bond due to rapid stress increase. Therefore, it is important
to use the curing time following the manufacturers’ instruc-
tions of the resin cement.
4.3. Surface treatment
The morphology and chemical properties of the ceramic sur-
face are very important factors for the ceramic-resin bond.
These properties can be achieved by application of chemical
conditioning agents and/or mechanical treatments by creating
a micromechanical and/or chemical bond to the resin cement.
4.3.1. Chemical conditioning methods
4.3.1.1. Hydrofluoric acid (HF) etching. Hydrofluoric acid is
an aqueous solution of hydrogen fluoride. It is a weak acid
because its H F bonding is relatively more stable than the
bonding of other strong acids (e.g. H Cl etching) [56], thus
the free hydronium ion (H3 O+ ) function is not strong. HF can
be used for dissolution of the ceramic glass phase surface
by reacting with silicon dioxide. This increases the rough-
ness of the ceramic surface and consequently creates a
micromechanical interlock between the ceramic and resin lut-
ing cement. The reaction process is shown as:
SiO2 + 4HF → SiF4 (g) + 2H2 O,
SiO2 + 6HF → H2 SiF6 + 2H2 O
It is noteworthy that the dissolution process does not rely on
the “acidic” property of HF, but the fluoride substitution to oxy-
gen due to electronegativity in glass that forms the Si.F glass.
Thus, the term “acid etch” is misleading and therefore “HF
etching” is preferred. HF has a long history in the pretreat-
ment of silica-based ceramics before bonding. This was first
described by Horn et al. who showed a successful increase in
bond strength between a thin layer of porcelain and resin by
the application of HF [57,58], to obtain a tensile bond strength
of 7.5 MPa [58].
From the early 1990s, further studies were carried out in
order to analyze the effect of the concentration and etch-
ing time of HF on the bond strength between ceramics and
resin cements [59–66]. It was reported, where combinations
of HF concentrations (2.5%, 5.0%, 7.5%, 10%, 15%) and etching
times (0.5 min, 1 min, 2.5 min, 5.0 min, 7.5 min, 10 min) were
examined on feldspathic ceramics, that no direct and obvi-
ous correlation was found between the etching period and
etchant concentration. The best etching periods for 2.5%, 5.0%,
7.5%, 10%, 15% HF were 5 min, 7.5 min, 10 min, 1.0 min, 0.5 min
respectively. The group in which the ceramic was treated with
e151
10% HF for 1.0 min produced the highest shear bond strength
(11.66 ± 1.91 MPa) [62]. In another study that evaluated the
effect of 5% HF gel etching time on the surface of a feldspathic
ceramic showed a different outcome. This study found that
with an increase in etching time, the shear bond strength also
increased. The highest bond strength was achieved when the
ceramic surface was etched for 2 min, and beyond this etching
time, a reduction of the shear bond strength was observed [61].
This phenomenon could be explained by the over-etching of
the glass ceramic surface and adversely affecting strength [60].
It was shown that 16.8% HF etching for 30 s seemed to over-
etch the glass surface, resulting in lower bond strength than
16.8% HF etching for 5 s [67]. A very recent study showed that
4.9% HF gel treatment of a lithium disilicate ceramic for 2 min
produced the highest shear bond strength [66]. Barghi et al.
[64] reported that low leucite content ceramics etched with
9.5% HF gel for 1 min showed the highest shear bond strength.
They further revealed that with a similar concentration of HF,
the gel (9.5%) produced better bond strengths than a liquid
etchant (10.0%). Moreover, ceramics with various leucite con-
centrations could also have an effect on the bond strength. To
date, it seems that 4% and 10% HF etching for 1–2 min is the
most acceptable etching procedure for silica-based ceramics,
depending on the HF material state (gel or liquid) as well as the
number, size, and distribution of the crystals in the ceramic.
Some additional procedures have been attempted after the
HF was rinsed off with water in order to enhance the ceramic-
resin bond by eliminating excess acid [68]. One study evaluated
the application of a neutralizing powder on the HF etched
ceramic surface. It was not a recommended procedure for
surface treatments of oxide ceramics because a significant
reduction of microtensile bond strength in the neutralization
group was found [68]. Another study presented a similar result
in neutralization application [69]. Inasmuch as HF etch is not
acting as an acid to etch the surface, such studies were erro-
(1) neous in rationale and showed neutralization of the acid was
pointless.
(2)
4.3.1.2. Substitutes of HF. Although HF can effectively
enhance the bond between ceramics and resin, it is highly
corrosive, can be absorbed into the blood and bone through
the skin and may even lead to cardiac arrest [70]. Hence,
a number of chemicals were introduced to substitute HF,
e.g. phosphoric acid, acidulated phosphate fluoride and
ammonium hydrogenfluoride.
The phosphoric acid used in dentistry is orthophosphoric
acid, which is an inorganic acid with the chemical formula
H3 PO4 . It is mainly used to clean the ceramic surface and
create a rough surface for better bonding. However, a study
showed that the application of 40% phosphoric acid for 5 s or
60 s did not show any obvious morphological change on the
ceramic surface under SEM observation [67]. Obviously, the
acidity is not important in the etching process, whilst the role
of fluoride on the atomic displacement with silicon dioxide is
of greater importance.
Acidulated phosphate fluoride (APF) has a empirical for-
mula NaH3 PO4 F [17]. The APF acid seems to prefer depositing
on the leucite-based ceramic surface [17,71]. Ammonium
bifluoride (ABF) is a glass etchant with the chemical formula
e152 d e n t a l m a t e r i a l s 3 0 ( 2 0 1 4 ) e147–e162
NH4 HF2 . It reacts with the silica constituent of glass in the
following manner:
SiO2 + 4[NH4 ][HF2 ] → SiF4 + 4[NH4 ]F + 2H2 O
It was observed that ABF mainly attacks phase boundaries and
cracks that already exist or are induced by leucite, which as a
consequence, created a linear defect pattern. Such a pattern
was also observed when HF was applied for a shorter time and
lower concentration, which implies that ABF acts in a fashion
similar to a low concentration of HF acid [71,72].
4.3.1.3. Silanization. Silane coupling agents provide a chemi-
cal bond between the resin and glass ceramic. Silanes have an
inorganic group that reacts with Si OH on the ceramic sur-
face by a condensation reaction. They also have an organic
group that can chemically bond to methacrylate-based resins
[7]. Silanes have to be activated by acid hydrolysis with the use
of acetic acid.
Several silane coupling agents are used to enhance chem-
ical bonding between ceramics and resin composite [73–75].
The most commonly used silane in dentistry for ceramic–resin
bonding is 3-methacryloxypropyltrimethoxysilane (or
␥-methacryloxypropyltrimethoxysilane). The abbre-
viations of this silane has been published as MPS,
␥-MPTS or MTS [76]. MPS is found to enhance shear
bond strength of the resin–ceramic compared to 3-
methacryloxypropylmethyldimethoxysilane (MDS) [77]. It was
noted that blended silanes of 1,2-bis(trimethoxysilyl)ethane
(BTS) and MPS could significantly increase the shear bond
strength between a resin and a leucite-reinforced ceramic
after thermocycling [78]. Such a blended silane system was
shown in a laboratory study [79] to enhance shear bond
strengths between resin and zirconia, especially after ther-
mocycling. Thus it seems blended silane systems could
be a solution to enhance surface adhesion, particularly in
dentistry.
Silanes have been shown to reduce the contact angle
and increase the wettability of the ceramic surface [80].
The silane layer is normally around 10–50 nm thick. It was
found that cohesive destruction of layers occurs if a suc-
cessive number of silane layers are applied on the surface
[81]. Thus, it is recommended that a thin silane coating
on ceramic surface should occur in order to achieve sat-
isfactory bonding. On the other hand, heat treatment of
the silane is another method to reduce the silane coating
thickness [7]. A significant increase in microtensile bond
strength between leucite-reinforced ceramic and resin cement
occurred after drying the silane (MPS) with a 100 ◦ C warm
air stream [82]. However, some studies demonstrated that
heat treatment could not improve the shear bond strength
of the adhesion promoter MPS between a resin cement
and leucite-reinforced ceramic, but enhanced the bond per-
formance for 3-methacryloxypropylmethyldimethoxy silane
(MDS), 3-methacryloxypropyltriethoxysilane (MTES), and 3-
acryloxypropyltrimethoxysilane (ACPS). Thus, the chemical
composition of the silane primer plays a more important role
than heat treatment to optimize the bond between resin and
leucite-reinforced ceramics [76]. Another study showed that
heat treatment of the silane did not improve the bond strength
[83].
Further, not only the silane monomer, but also the other
(3) primer ingredients can have a considerable affect on adhesion
[18,77,78,80]. Experimental ceramic primers have been shown
to exhibit a higher ceramic bond durability than commer-
cial ceramic primers [78]. A significant increase in shear bond
strength between a resin and a leucite-reinforced ceramic
after thermo-cycling was observed when hydrochloric acid
(HCl) was added to the silane solution, in which HCl might
act as an accelerator during the hydrolysis reaction of the
methoxy part of the silane [78]. Thiophosphoric methacrylate
(MEPS) is also recommended to blend with the silane solu-
tion since MEPS can accelerate the hydrolysis of the silane
monomer and promote ceramic bonding [77].
One study discovered that when an appropriate silane
application method was used on the surface of leucite-
reinforced ceramics, no significant difference in the bonding
effect of a pre-activated MPS-based silane solution, acetic acid
and ethanol even when it was stored for up to 1 year at room
temperature [84].
4.3.2. Mechanical conditioning methods
4.3.2.1. Sand blasting. It is a process to roughen the ceramic
surface by blasting with alumina (Al2 O3 ) particles. Twenty five
to 50 ␮m alumina powder is commonly used in glass ceramics
at a pressure of 0.28 MPa [85,86].
4.3.2.2. Laser irradiation. Nd:YAG and Er:YAG lasers were eval-
uated in a bond strength test of glass ceramics [87,88]. SEM
observation revealed that the Er:YAG laser created irregular
lithium disilicate crystals on the surface. The higher the laser
power the greater the irregularities of the ceramic surface [88].
For feldspathic ceramics, it could be seen that the surface
was randomly melted and corroded without any fissures or
cracks when either an Nd:YAG or Er:YAG laser was applied to
a ceramic surface [87].
4.3.2.3. Tribochemical (TBC) silica-coating. Tribochemical
silica-coating is a sand blasting process that uses silica-coated
alumina particles to coat and blast the ceramic surface, which
involves blasting the powders with high pressure compressed
air on to the ceramic surface. The pressurized powders
generate kinetic energy that is absorbed by the surface and
subsequently partially melts it. The silica-coated alumina
powders are embedded into the ceramic surface and produce
a surface silica layer [89]. A silane coupling agent is then
applied onto the silica-coated surface. As a result, a strong
chemical bond can be formed between the ceramic and resin
cement. A commercial product, Rocatec System (3M-ESPE,
Seefeld, Germany) was reported to be an effective surface
preparation by combining tribochemical silica-coating with
silanization [86].
4.3.2.4. Pyrochemical silica-coating. This is a proprietary sur-
face treatment that was introduced as the Silicoater system
(Heraeus-Kulzer, Wehrheim, Germany). The substrate is
passed through a flame with the injection of a silane
solution. Then, a series of pyrochemical reactions occur
between 150–200 ◦ C and a silicon oxide intermediate layer
 d e n t a l m a t e r i a l s 3 0 ( 2 0 1 4 ) e147–e162
is produced on the ceramic surface. After the substrate is
cooled to room temperature, the silane coupling agent (3-
methacryloyloxypropyl trimethoxysilane) is applied to the
silicon oxide layer surface [90,91]. This system was first used
for enhancing the bond between resin and metal alloys.
Although silicon oxide is already present in glass ceramics
and this pyrochemical coating method was considered unnec-
essary, it was thought the deposition of a silica layer with
this technique might help to improve the bond [90]. It was
shown that a significantly higher bond strength was achieved
when this treatment was applied to a glass ceramic surface
[86,90,92].
4.3.3. Comparison between different surface treatments
The comparison of bond strengths of various surface treat-
ments is listed in Table 1. It has been shown that HF etching
on the ceramic can create higher surface roughness and
consequently a higher bond strength than other methods
[17,71,93,94]. Della Bona et al. [71] found that ceramics treated
with HF showed significantly higher tensile bond strength
values than acidulated phosphate fluoride and ammonium
bifluoride treatment while no statistically significant differ-
ence was found between acidulated phosphate fluoride and
ammonium bifluoride treated groups. It was also observed
that higher microtensile bond strengths in leucite glass ceram-
ics were obtained when treated with HF etching compared
with phosphoric acid [95]. Similar results were shown in
another study confirming that etching with HF was a more
effective surface treatment than phosphoric acid [67]. HF etch-
ing on a feldspathic ceramic surface also showed a higher
shear bond strength than either sandblasting or grinding
alone when stored for either 24 h or 6 months [94]. Despite
the common procedure for the ceramics, surface roughening
preparation including grinding, sandblasting and phosphoric
acid application are considered as a basic preparation process
of ceramics to obtain consistent adhesion.
It was reported that laser-irradiation preparation could pro-
vide similar bond strengths to glass ceramics as HF etching
[85,88]. Gokce et al. [88] revealed that the Er:YAG laser with
a power setting of 300 mJ exhibited the highest shear bond
strength and as high as HF treatment in lithium disilicate
ceramics. Thus, this laser treatment could possibly be used for
surface modification. However, it was pointed out in another
study [87] that the laser irradiation application with either
Er:YAG or Nd:YAG laser is not adequate for ceramic bonding
and it was suggested to combine laser application with HF
etching.
A durable resin–ceramic tensile bond could be obtained by
appropriate silane application without the need for HF etch-
ing of the ceramic surface [84,96]. It is accepted that HF etching
followed by silane coupling agent application is the typical sur-
face treatment on glass ceramics. Such a treatment provides
the highest bond strength of ceramic-resin bonding compared
to any single surface preparation [83,94,97–99]. Several other
surface roughening methods were carried out to evaluate the
effect of these treatments following silanization on ceramic
bonding. It was shown in one study that when the glass
ceramic surface was treated with sandblasting, polishing, HF
or phosphoric acid etching, the HF etching and sandblast-
ing groups exhibited the highest microshear bond strengths.
e153
However, when a silane coupling agent was applied after the
above treatments, no significant difference of bond strengths
among these groups was observed. This implies a silane cou-
pling agent plays an important role in the resin–ceramic bond
regardless which surface roughening preparation is used [67].
Nevertheless, other studies have shown that HF etching
combined with silanization produced a significantly higher
shear bond strength than the application of phosphoric acid
and the silane coupling agent [66,100]. The reason for the
difference in these results possibly lies with the different con-
centration of the acid, different etching time, different ceramic
and different bond tests.
It was suggested that the tribochemical silicoating method
combined with silanization achieves significantly higher shear
bond strengths on feldspathic ceramics compared with HF
etching followed by silane coupling agent application and after
thermocycling [92]. It was also suggested that tribochemical
treatment followed by silanization and application of func-
tional monomer substantially increased the bond strength of
leucite-reinforced glass ceramics [86].
Some researchers have used a variety of silane coupling
agents in combination with different brands of resin cements
as a bonding system [19,101]. Although such variations of
silane coupling agents with different resin cements might be
able to generate various results, the explanation of such a
combination is unclear and difficult to distinguish the bonding
effects whether promoted by the silane or resin cement.
A stronger bond strength was claimed to have been
obtained by an additional application of an unfilled resin after
HF acid etching and silanization [65,96]. However, another
study observed lower microshear bond strength values in
ceramics bonded using an unfilled resin adhesive after silane
coupling agent application compared with the silane coupling
agent alone, or when the silane coupling agent was mixed
with the bonding agent, regardless of the ceramic surface was
treated with HF or sandblasted [19]. Further, it was observed
that with the use of silane coupling agent and unfilled resin,
the effect of etching time of HF became insignificant, prob-
ably due to the unfilled resin over the silane could infiltrate
better into the cracks and fissures created by the HF, thus
strengthening the bond [65].
4.4. Laboratory methodology
A restoration in the oral cavity is challenged under a complex
and hostile environment. It is subjected to occlusal forces that
consist of shear, tensile, compressive and flexural stresses. In
addition, the restoration is immersed in saliva and exposed to
food and beverages with various pH, chemistries and temper-
atures. Various laboratory tests have attempted to simulate
oral conditions and accordingly predict clinical bonding per-
formance. Nevertheless, no single laboratory test can predict
the clinical resin–ceramic bonding capability satisfactorily. A
correlation with clinical studies is necessary.
4.4.1. Tensile and shear bond strength test
The most common tests for resin–ceramic bonding measure-
ments are shear and tensile bond strength tests. A shear bond
strength test is when the ceramic surface is constrained and
the resin composite is subjected to a force that is parallel to the
 e154
Table 1 – Comparison of bond strength of different surface treatments.
Authors Ceramic type Surface treatment Mean strength Test type Storage condition Comments
[MPa]
Chen et al. [1] a A (5%) (0 s) 0.0 SBS 24 h, 37 ◦ C, W
A (5%) (5 s) 12.3
A (5%) (30 s) 32.3
A (5%) (60 s) 35.9
A (5%) (120 s) 44.5
A (5%) (180 s) 41.0
Nogami et al. [2] a No treatment 8.8 SBS 24 h, 37 ◦ C, W L 4-META
L 0.0 E1 Porcelain Liner M
E1 18.9 E2 Tokuso Ceramics Primer
L/E1 30.7
B 0.0

d e n t a l m a t e r i a l s 3 0 ( 2 0 1 4 ) e147–e162
E2 25.7
B/E2 29.7
No treatment 0.0 24 h, 37 ◦ C, W,TC
L 0.0
E1 2.3
L + E1 (mixed) 19.7
B 0.0
E2 9.7
B + E2 (mixed) 22.4
Taira et al. [3] b No treatment 6.8 SBS 60 min, RT, Dry; 24 h, 37 ◦ C, W
B + E1 16.7 E1 MDS
B + E1/L 33.0 E2 MTS
B + E2 18.1 E3 GC ceramic primer
B + E2/L 47.4 E4 Clearfil ceramic primer
B + E3 29.1 E5 Tokuso ceramic primer
B + E4 40.4 E6 Porcelain Liner M
B + E5 46.8 E7 Monobond Plus
B + E6 33.8 L Metal primer II
B + E7 26.3
Kara et al. [4] a F 2.33 SBS 7 d, RT, DW
A 0.71
G 0.46
Jedynakiewicz et al. [5] a A+E 26.2 SBS 24 h
H+E 26.7
c D+E 19.2
H+E 34.0
Ruttermann et al. [6] a A + E1 11 SBS 24 h, dry E1 Monobond S
F + E1 23 E2 Pyrosil Primer MP 94 E
I + E2 27 E3 experimental silane MPS
A + E3 12 E4 experimental silane MPS
A + E4 8 E5 Silane Primer
 B + E5 16 E6 Clearfil Procelain Bond Activator mixed
with SE Bond Primer
B + E6 16
A + E1 12 TC
F + E1 26
I + E2 30
A + E3 8
A + E4 8
B + E5 4
B + E6 16
Stewart et al. [7] a No treatment 0–4.0 SBS 24 h, 37 ◦ C, IS 4 resin cements for each treatment:
F 1.1–3.5 Nexus
E 9.2–20.6 Panavia 21

d e n t a l m a t e r i a l s 3 0 ( 2 0 1 4 ) e147–e162
F+E 8.4–23.1 RelyX ARC
A 10.3–19.0 Calibra
A+E 16.0–21.7
No treatment 0 6 m, 37 ◦ C, IS
F 0
E 1.6–19.3
F+E 4.2–23.8
A 6.2–15.6
A+E 15.9–21.8
Matsumura et al. [8] a F+B 17.1, 18.1 SBS 24 h, 37 ◦ C, W E1 Clapearl Bonding Agent
F + B + E1 21.5, 32.4 E2 Clearfil Porcelain Bond
F + B + E2 32.0, 33.8 E3 Panavia Ceramic Primer
F + B + E3 18.1, 31.3 2 resin cements for each treatment:
F+B 1.4, 11.4 24 h, 37 ◦ C, DW; TC Clapearl DC
F + B + E1 23.0, 33.0 Panavia 21
F + B + E2 20.5, 32.2
F + B + E3 12.5, 30.3
Brum et al. [9] d No treatment 24.96 SBS 24 h, RT, dry; 24 h, 37 ◦ C, W; TC
A+E 44.47
F+E 31.05
Hooshmand et al. [10] b E (stored for 15 min) + M 30.28 TBS 24 h, RT, dry adhesive effectiveness will not
deteriorate when stored for up to 1 year
E (stored for 2 h) + M 25.70
E (stored for 1 m) + M 25.70
E (stored for 6 m) + M 26.5
E (stored for 1 y) + M 30.23
E (stored for 15 min) + M 17.8 24 h, boiling water
E (stored for 2 h) + M 14.0
E (stored for 1 m) + M 18.5
E (stored for 6 m) + M 14.8
E (stored for 1 y) + M 19.1

e155
 e156
Table 1 – (Continued)
Authors Ceramic type Surface treatment Mean strength Test type Storage condition Comments
[MPa]
Liu et al. [11] b1 B (37%) + E1 16.31 ␮SBS No storage b1 ProCAD
B (37%) + E2 16.43 b2 GN-I
B (37%) + E3 20.39 E1 GC Ceramic Primer
b2 B (37%) + E1 21.16 E2 Clearfil Ceramic Primer
B (37%) + E2 19.64 E3 Porcelain Liner M
B (37%) + E3 23.02
b1 B (37%) + E1 12.00 TC
B (37%) + E2 13.90
B (37%) + E3 12.04
b2 B (37%) + E1 13.22
B (37%) + E2 15.94
B (37%) + E3 16.09
␮SBS 24 h, 37 ◦ C, DW

d e n t a l m a t e r i a l s 3 0 ( 2 0 1 4 ) e147–e162
Naves et al. [12] b A (10%) (10 s) + E 19.4
A (20%) (10 s) + E 22.3
A (40%) (10 s) + E 22.2
A (60%) (10 s) + E 17.8
A (120%) (10 s) + E 15.3
A (10%) (10 s) + E + J 17.4
A (20%) (10 s) + E + J 21.3
A (40%) (10 s) + E + J 21.1
A (60%) (10 s) + E + J 24.7
A (120%) (10 s) + E + J 20.4
Della Bona et al. [13] b A (9.6%) 9.9 ␮TBS 30 d, 37 ◦ C, W
C (4.0%) 0
E 27.2
A+E 20.6
C+E 13.6
d A (9.6%) 41.7
C (4.0%) 19.1
E 30.1
A+E 56.1
C+E 36.9
Saavedra et al. [14] b A+E 10.2 ␮TBS No storage
A+K+E 6.8
A+E 6.1 MC
A+K+E 5.0
Amaral et al. [15] a A (9%) (60 s) (gel) 14.4 ␮TBS No storage
A (4%) (60 s) (gel) 14.3
A (5%) (60 s) (liquid) 12.7
A (5%) (60 s) (liquid) + K 14.2
A (9%) (60 s) (gel) 13.9 24 h, 37 ◦ C, DW; TC
A (4%) (60 s) (gel) 15.5
A (5%) (60 s) (liquid) 12.4
A (5%) (60 s) (liquid) + K 10.6
De Carvalho et al. [16] a A+E 17.6 ␮TBS 7 d, 37 ◦ C, DW
A+E+M 19.0
E+M 9.1

d e n t a l m a t e r i a l s 3 0 ( 2 0 1 4 ) e147–e162
E 10.9
Akyil et al. [17] a No treatment 8.02 ␮TBS 24 h, 37 ◦ C, DW; TC G1 Er:YAG
A 17.01 G2 Nd:YAG
F 14.58
G1 5.28
G2 6.51
F+A 9.08
G1 + A 12.25
G2 + A 11.73
Peumans et al. [18] b No treatment 12.8 ␮TBS 24 h, 37 ◦ C, W
B 19.1
B+E 27.4
B+E+J 34.0
A 37.6
A+E 34.6
A+E+J 34.5
TBS, tensile bond strength; SBS, shear bond strength; ␮TBS, microtensile bond strength; ␮SBS, microshear bond strength; W; water; DW, distilled water; RT, room temperature; TC, thermocycling; MC,
mechanical cycling; IS, isotonic saline solution.
a, feldspathic ceramics; b, leucite reinforced ceramics; lithium disilicate ceramics.
A, HF etching; B, phosphoric acid; C, acidulated phosphate fluoride (APF); D, ammonium bifluoride (ABF); E, silane coupling agent; F, sand blasting; G, Laser irradiation; H, tribochemical silica-coating;
I, Pyrochemical silica-coating; J, unfilled resin; K, HF neutralization; L: monomer; M: silane heat treatment.

e157
e158 d e n t a l m a t e r i a l s 3 0 ( 2 0 1 4 ) e147–e162
bonding interface. However, in reality, the experimental pro-
cedure makes it very difficult to perform a “true” shear bond
strength test. Traditionally, a load is applied at the interface
between a resin composite cylinder and the ceramic. Ideally,
one method uses a loading blade that is placed as close as
possible to the bonding interface and moves parallel with the
bonded interface, which could then cause a localized stress
concentrated at the loaded area. Another method places a wire
loop close to the bonding area to theoretically reduce the stress
concentration. It was demonstrated in a finite element anal-
ysis (FEA) model [102] that blade loading causes higher stress
concentration at the bonding area than the wire-loop loading
effect. The reason is the load is applied at one point and fewer
nodes can be loaded with the blade, whilst the wire-loop sur-
rounds the specimen to better distribute stresses. These two
loading methods develop a bending moment, inducing ten-
sion and compression that consequently leads to failure [103].
Further, FEA [102] showed a non-uniform stress distribution at
the bonding interface, thus deviations from a true shear force
measurement occurs.
Tensile bond strength tests can be performed by using
ceramic specimens bonded to a substrate (tooth or resin com-
posite), and then applying two sets of forces directed away
from each other and perpendicular to the bonding interface.
It is quite difficult to control the alignment of specimens, and
non-uniform stress distribution across the bonding surface
also occurs, but is easier to control.
Della Bona et al. [104] compared the shear and tensile bond
strengths between resin and ceramics by using both laboratory
tests as well as FEA analysis. The tensile bond strength test
provided a more uniform stress distribution at the interface
whilst the shear bond strength test gave a result of cohesive
strength of the substrate material which is actually an inher-
ent property of the material but not the true bond strength.
It was concluded that the tensile bond strength test seemed
to be a more valid method to evaluate the bond strength than
shear bond strength test.
The commonly used shear and tensile bond strength tests
are associated with several limitations that question the relia-
bility of these tests in terms of accuracy and clinical relevance
[8,9,18]. Uneven stress distribution causes fracture initiation
from flaws that occur at the interface or within the bulk of the
material in areas of stress concentration. These defects, due
to their random and uneven nature, cannot be controlled and
thus can lead to considerable variations in test results [11].
4.4.2. Microshear & microtensile bond strength test
To overcome the non-uniform stress created in conven-
tional shear and tensile bond strength tests, microshear and
microtensile bond tests were developed to improve the test
methods. In principle, the microshear and microtensile bond
strength tests use specimens with a cross-sectional area of
approximately 1 mm2 . Lowering the cross-sectional area leads
to a greater uniformity of the stress distribution. Moreover,
these tests tend to lead to less cohesive failure in the sub-
strates and more adhesive failure at the bonding interface
[17,23], which is thought to offer more accurate results for
evaluating the ‘true’ bonding potential between the ceramic
and resin luting cement [105].
It was noticed that the bond strength values obtained
from microshear or microtensile bond strength tests are
higher than corresponding macro-scale tests [106]. This can
be explained by Griffith’s Law [107], showing larger test
specimens have a higher possibility of having defects, thus
decreasing the measured strength.
As restorations are under a combination of different forces
in the oral environment and no single laboratory test can
satisfactorily predict bonding potential, therefore conducting
different bond strength tests was suggested for better predic-
tion of performance [108]. When a glass ceramic was bonded
with different resin cements (Duo-link, Nexus 2, Variolink
II), Duo-link showed the highest shear bond strength whilst
Variolink II showed the highest tensile bond strength. Thus,
different resin cements might express different bond poten-
tials for different tests [108]. However, the failure mode was
not clearly described, thus it is difficult to interpret the overall
result and as failure type is an important piece of information.
4.4.3. Thermocycling and loadcycling
In order to better simulate the oral environment, the ther-
mocycling and loadcycling tests can be applied to simulate
the aging and fatigue. In thermal cycling, specimens are sub-
jected to between 1000 and 100,000 cycles between 5 and 55 ◦ C
[80,87,98]. In principle, thermal cycling could generate hoop
stresses at the bonding interface which is caused by a mis-
match in the thermal expansion coefficient between different
materials [109]. Several studies showed that thermocycling
could significantly decrease the bond strength between resin
cement and ceramic [110,111]. However, a recent study [112]
indicated thermocycling increased the microtensile bond
strength between resin cement and ceramics without consid-
ering the type of resin cement. The reason for this different
result might be due to the relatively short number of cycles
(6000), thus resulting in a shorter water storage and fatigue
time. All these factors might lead to an increase in the degree
of conversion of the resin cement and consequently generate a
higher bond strength. However, in resin–dentin bonding ther-
mal cycling is regarded as an inappropriate factor and there
seems to be little use to include this method in dentin bond-
ing studies [113]. At present, whether thermocycling has an
effect on the ceramic–resin bond is still unclear. Thus, further
studies are needed to clarify this point.
Load cycling (or mechanical cycling), is used much less in
resin–ceramic bonding tests compared with other methods.
An older study showed that loading with 60 N for 20 times
did not decrease the bond strength between the resin cement
and ceramic, however some specimens were debonded dur-
ing the loading and should be have excluded in the evaluation
[44]. Another study showed that specimens subjected to a
load of 1,400,000 cycles showed a significant decrease of the
resin–ceramic bond strength [68]. Due to the paucity of stud-
ies, no conclusion can be made to determine if fatigue testing
influences the durability of the resin–ceramic bond.
4.4.4. Storage conditions
The longevity of the bond between resin cement and ceramic
may be influenced by storage time and conditions that can
replicate the oral environment [114]. It has been demonstrated
that resin storage in water leads to hydrolytic degradation of
 d e n t a l m a t e r i a l s 3 0 ( 2 0 1 4 ) e147–e162
the bond [115]. Several studies revealed a notable decrease of
bond strength between resin and ceramic after water storage
of 24 h to 1 year [47,93,116].
Different storage media might also play a role in bond
degradation, e.g. a resin cement may exhibit greater hydrolytic
degradation in ceramic–resin bonding when stored in artificial
saliva compared with distilled water [117]. To date, most stud-
ies have mostly used distilled water as the storage medium,
which may not lead to the accurate results of durability of
the resin–ceramic bond in oral conditions. It is recommended
that a longer storage time and an artificial saliva storage
medium should be applied in laboratory tests investigating
resin–ceramic bonds.
5. Conclusion
It has been realized that the bond between glass ceramics and
resin cements are one of the key factors to long-term clinical
success. Intense research activity has brought many contribu-
tions to the understanding on ceramic–resin bonding in the
past few years. Based on scientific and clinical evidence, it
seems to be clear that HF etching and silanization are neces-
sary for the surface treatment of a glass ceramic restorations.
However, the optimal bonding procedure remains controver-
sial. More research is needed to develop a substitute for HF.
Improvements on resin cements are also needed. In addition,
laboratory tests need to better simulate the oral environment
and consequently obtain more reliable data correlated with
clinical performance.
Appendix A. Supplementary data
Supplementary data associated with this article can be found,
in the online version, at http://dx.doi.org/10.1016/j.dental.
2014.01.017.
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