Eur J Oral Sci 2017; 1–8 Ó 2017 Eur J Oral Sci

DOI: 10.1111/eos.12340 European Journal of

Printed in Singapore. All rights reserved
Oral Sciences

Chenmin Yao, Liqun Zhou,

Effect of silane pretreatment on the Hongye Yang, Yake Wang,
Hualing Sun, Jingmei Guo,
immediate bonding of universal Cui Huang
The State Key Laboratory Breeding Base of

adhesives to computer-aided design/ Basic Science of Stomatology (Hubei-MOST)

& Key Laboratory for Oral Biomedicine
Ministry of Education, School & Hospital of

computer-aided manufacturing lithium Stomatology, Wuhan University, Wuhan,

China

disilicate glass ceramics

Yao C, Zhou L, Yang H, Wang Y, Sun H, Guo J, Huang C. Effect of silane
pretreatment on the immediate bonding of universal adhesives to computer-aided
design/computer-aided manufacturing lithium disilicate glass ceramics.
Eur J Oral Sci 2017; 00: 1–8. © 2017 Eur J Oral Sci
The aim of this study was to investigate the effect of silane pretreatment on the uni-
versal adhesive bonding between lithium disilicate glass ceramic and composite
resin. IPS e.max ceramic blocks etched with hydrofluoric acid were randomly
assigned to one of eight groups treated with one of four universal adhesives (two
silane-free adhesives and two silane-containing adhesives), each with or without
silane pretreatment. Bonded specimens were stored in water for 24 h. The shear
bond strength (SBS) of the ceramic-resin interface was measured to evaluate bond Cui Huang, The State Key Laboratory
strength, and the debonded interface after the SBS test was analysed using field- Breeding Base of Basic Science of
emission scanning electron microscopy to determine failure mode. Light microscopy Stomatology (Hubei-MOST) & Key Laboratory
was performed to analyse microleakage and marginal sealing ability. Silane pretreat- for Oral Biomedicine Ministry of Education,
School & Hospital of Stomatology, Wuhan
ment significantly and positively influenced SBS and marginal sealing ability. For
University, Luoyu Road #237, Hongshan
all the universal adhesive groups, SBS increased and the percentage of microleakage District, Wuhan 430079, China
decreased after the pretreatment. Without the pretreatment, SBS and the percentage
of microleakage were not significantly different between the silane-containing uni- E-mail: huangcui@whu.edu.cn
versal adhesive groups and the silane-free groups. Cohesive failure was the main
fracture pattern. The results suggest that additional silane pretreatment can effec- Key words: glass-ceramics; microleakage;
tively improve the bonding strength and marginal sealing of adhesives to lithium shear bond strength; silane coupling agent;
disilicate glass ceramics. The bonding performance of silane-containing universal universal adhesives
adhesives without pretreatment is similar to that of silane-free adhesives. Accepted for publication January 2017

Ceramics are widely used in dentistry owing to their
aesthetic properties, their high flexural strength, and
their favourable cumulative survival rates (1, 2). Den-
tal ceramics are generally categorized into glass ceram-
ics and oxide ceramics based on their composition.
Computer-aided design/computer-aided manufacturing
(CAD/CAM) glass ceramic restorations, such as
veneers, inlays, onlays, and crowns, are being used
with increased frequency because this technology can
yield a highly uniform, quality structure (3). The per-
formance of lithium disilicate and machinable glass
ceramic, e.max CAD, is significantly better than that
of leucite-based Empress CAD for inlays and onlays
(4). As such, CAD/CAM lithium disilicate glass
ceramics should be comprehensively explored.
Hydrofluoric (HF) acid etching, followed by applica-
tion of a ceramic primer containing a silane coupling
agent, is a relatively effective treatment method for
glass ceramic bonding (5, 6). However, treatment pro-
cedures are tedious and considered a limiting factor
for clinicians. Therefore, simple and effective bonding
should be developed.
With advancements in chemistry, dental adhesives
have undergone modifications (7, 8) and have achieved
remarkable progress over two decades. Universal adhe-
sives are new products (9–11) that are potentially used
as a bonding agent for tooth structures and restora-
tions, such as ceramic, metal, and composite resins.
Novel universal adhesives can be used to simplify the
bonding process. Regarding various indirect restorative
substrates, some manufacturers of universal adhesive
argue that a separate primer is unnecessary for the
bonding of versatile adhesives.
Especially mentioned by the manufacturers, active
and stable silane coupling agents in universal adhesives
can achieve chemical bonding to glass ceramic surfaces
without using a separate ceramic primer. Hydrofluoric
acid is a suitable substance for micromechanical bond-
ing, and silane coupling agents are mainly used to pro-
mote chemical bonding between silica-phase glass
2 Yao et al.

ceramics and composite resins through siloxane bonds
(12, 13). Silane coupling agent not only increases the
surface energy of ceramic to improve wettability (14, 15)
but also binds silicon dioxide (SiO2) and methacrylate
through a degradable functional group and a polymeriz-
able C=C double bond (16). However, this observation
remains controversial because researchers have yet to
determine whether silane-containing universal adhesives
are too simple to be satisfactory. Therefore, the efficacy
of silane constituents on the bonding of universal adhe-
sives should be verified. Although several studies have
reported the effectiveness of bonding of universal adhe-
sives to zirconia (17, 18), leucite-reinforced glass ceram-
ics (19), and short-fibre-reinforced composite resin
bonding (20), few studies have been performed that
analyse the efficacy of constituent silane in adhesives.
Therefore, to understand the importance of silane, we
selected CAD/CAM lithium disilicate glass ceramics and
other kinds of universal adhesives as materials.
The aim of this research was to examine the perfor-
mance of silane in universal adhesives and to investigate
whether additional silane is necessary to promote glass
ceramic bonding. Our overall research hypotheses were
as follows: (i) there is no difference in the bonding perfor-
mance between silane-containing universal adhesives and
silane-free adhesives, and (ii) there is no difference in the
bonding capabilities of groups pretreated or not with
additional silane.
Material and methods
Specimen preparation and the application of
adhesive systems
A schematic of the experiment is shown in Fig. 1. A total
of 120 lithium disilicate glass ceramic specimens (e.max
CAD; Ivoclar Vivadent, Schaan, Liechtenstein) were pre-
pared in a standard size (8 mm length 9 7 mm
width 9 2 mm height) using a low-speed cutting device
(IsoMet; Buehler, Evanston, IL, USA) and sintered
according to the recommended protocol. The specimens
were polished with #320, #400, #1,200, and #3,000-grit sil-
icon carbide (SiC) paper and a soft cloth using 0.5 lm grit
diamond paste under running water to establish a uniform
surface, etched with 9% HF acid (Ultradent, South Jor-
dan, UT, USA) for 90 s, and then rinsed with distilled
water for 15 s.
The etched blocks were randomly assigned to one of
eight groups treated with one of four universal adhesives,
with or without the use of additional silane pretreatment.
More specifically, the etched blocks were either directly
treated with universal adhesives or pretreated with ceramic
primer containing additional silane (RelyX Ceramic Pri-
mer; 3M ESPE, St Paul, MN, USA) for 20 s before appli-
cation of adhesive. The adhesives were two silane-free
universal adhesives [All Bond Universal (ABU); Bisco,
Schaumburg, IL, USA and Adhese Universal (ADU); Ivo-
clar Vivadent] and two silane-containing universal adhe-
sives [Clearfil Universal Bond (CUB); Kuraray Noritake
Dental, Tokyo, Japan and Single Bond Universal (SBU);
3M ESPE], as described in Table 1. The adhesives were
applied according to the manufacturer’s instructions and
polymerized using a light-emitting diode (LED) light-cur-
ing unit (Ivoclar Vivadent) with irradiance of approxi-
mately 1,100 mW cm 2.
Shear bond strength test
Polyvinyl chloride tubing with an inner diameter of 3 mm
and a length of 4 mm was filled with composite resin
(Charisma; Heraeus Kulzer, Hanau, Germany) and placed
at the adhesive interface. For two increments of 2 mm, the
composite resin was subsequently polymerized for 40 s
using the LED light-curing unit. The specimens (n = 80)
were stored in distilled water (37°C) for 24 h and then
were mounted into a steel fixture in a universal testing

Fig. 1. Schematic view of specimen preparation. (A) Standard lithium disilicate glass ceramic specimens (8 mm 9 7 mm 9 2 mm)
were embedded in resin, then processed for evaluation of shear bond strength (SBS). Failure modes of the fracture surfaces were
evaluated by field-emission scanning electron microscopy (FE-SEM). (B) Composite resin of 2 mm depth was built on the adhe-
sive layer. The specimen was longitudinally sectioned to produce slabs that were immersed in Basic Fuchsin solution. For micro-
leakage evaluation, the slabs were observed under light microscopy (LM).
 Effect of silane on bonding of universal adhesive 3

Table 1
Universal adhesives used in this study and application procedures

Abbreviation
used
Universal adhesive in this
(batch number) study Composition Application instructions pH

All-Bond Universal ABU MDP, Bis-GMA, HEMA, ethanol, water, Apply for 10–15 s, mild air-dry 3.2
(1200006111) initiators for at least 10 s, light cure for 10 s
Adhese Universal ADU MDP, Bis-GMA, HEMA, CQ, MCAP, D3MA, Apply for 20 s, mild air-dry for 5 s, 2.5–3.0
(SS4248) ethanol, water, highly dispersed silicon dioxide light cure for 10 s
Clearfil Universal CUB MDP, Bis-GMA, HEMA, CQ, hydrophilic Apply for 10 s, mild air-dry for 5 s, 2.3
Bond (01416) aliphatic dimethacrylate, colloidal silica, light cure for 10 s
accelerators, silane coupling agent
Single Bond SBU MDP, HEMA, silane, filler, dimethacrylate Mix Single Bond Universal 2.7
Universal resins, Vitrebond copolymer, dual cure activator with Single
(D-82229) ethanol, water, initiators Bond universal in a ratio of 1:1,
apply adhesive mixture for 20 s, dry
gently for 5 s, light cure for 10 s

Bis-GMA, bisphenyl A glycidyl methacrylate; CQ, camphorquinone; D3MA, decandiol dimethadrylate; HEMA, 2-hydroxyethyl methacry-
late; MCAP, methacrylated carboxylic acid polymer; MDP, 10-methacryloyloxydecyl dihydrogen phosphate.

machine (ZY-100K; Yangzhou, Jiangsu, China). The load
was applied at a constant crosshead speed of 1 mm min 1
until failure occurred. The maximum force to result in
fracture was recorded. The fracture region of the adhesive
interface was measured using a digital calliper. The maxi-
mum force and surface area of the adhesive interface were
used to calculate the shear bond strength (SBS) (which
was measured in MPa).
Failure mode analysis
After the SBS test was performed, the fracture surfaces
were subjected to ultrasonic cleaning and air-drying, sput-
ter coated with gold–palladium (Au–Pd) alloy (JFC-1600;
JEOL, Tokyo, Japan), and observed using field-emission
scanning electron microscopy (FE-SEM; Zeiss, Sigma,
Germany). The FE-SEM observations were carried out at
an operating voltage of 5 kV. The failure modes of the
the peripheral slabs were disregarded. A total of 40 slabs
(five slabs 9 eight groups) were collected. The slabs were
stored in distilled water (37°C) for 24 h and then coated
with two consecutive layers of nail varnish, except for an
area approximately 0.5 mm from the bonding interface to
allow tracing of staining agent. After coating, the speci-
mens were immersed in 0.5% Basic Fuchsin solution (23)
at 37°C for 24 h.
The Basic Fuchsin-stained bonded specimens were fixed
on glass slides and then polished with #800, #1,200,
#2,000, #3,000, and #5,000-grit SiC paper under running
water to remove the surface deposits and expose the
bonded interfaces of the specimens. After rinsing and
cleaning ultrasonically, we examined the ceramic–resin
interface using a light microscope (DP72; Olympus,
Tokyo, Japan). Fifteen images at 1009 magnification in
each group were randomly captured for quantity analyses.
IMAGE J ANALYSIS software was applied to calculate the per-

adhesive surface were recorded as adhesive failure (failure
occurring at the ceramic surface) or cohesive failure (fail-
ure occurring in adhesive or filling composite resin) (21,
22). The general conditions and typical regions of the frac-
tured surfaces were captured at 249, 5,0009, and 20,0009
magnifications. The images were processed with IMAGE J
ANALYSIS software (NIH, Frederick, MD, USA) to calcu-
late the percentages of adhesive and cohesive failures of
the fracture surfaces.
Specimens for microleakage evaluation
Forty etched blocks were randomly assigned into eight
groups (n = 5) according to pretreatment method and
which of the four different universal adhesives was used.
After applying the adhesives, composite resin build-ups
(2 mm increments) were placed and polymerized for 40 s
using the LED light-curing unit. The specimens were sec-
tioned longitudinally across the ceramic–resin interface
using a low-speed diamond saw to obtain slabs with
dimensions of 7 mm 9 4 mm 9 1 mm. To prevent the
results being influenced by either excessive or insufficient
amounts of resin at the ceramic-resin adhesive interface,
centage of microleakage in the adhesive layers.
Statistical analysis
Shear bond strength and the percentage of microleakage
are presented as mean  SD and were analysed using SPSS
version 23.0 (SPSS, Chicago, IL, USA). As the data were
normally distributed, two-way ANOVA was applied. Post-
hoc multiple comparisons were conducted using Tukey’s
test. The statistical procedures were performed at a signifi-
cance level of 0.05.
Results
Shear bond strength
An overview of the mean values and SD of SBS, as
well as the percentage of microleakage, is depicted in
Table 2. The two-way ANOVA revealed that, without
additional silane pretreatment, SBS was not signifi-
cantly different between either CUB or SBU (silane-
containing universal adhesives) and the two silane-free
4 Yao et al.

adhesives (ABU and ADU; P > 0.05). In addition, the
highest SBS was observed for SBU when groups were
pretreated with additional silane (P < 0.05). For all
universal adhesives, the groups with silane pretreatment
showed significantly higher SBS values (P < 0.05) than
did the groups without silane pretreatment.
Failure mode analysis
The failure modes are illustrated in Fig. 2A. Adhesive
failure exposed the ceramic surface, while cohesive fail-
ure fractured in adhesives or composite resins. Fre-
quency distribution and mean percentages of areas
assigned to failure modes were assessed. The results
revealed no significant differences in failure mode,
whether or not the adhesives were pretreated with
additional silane. For the immediate bonding, cohesive
failure was the main fracture pattern in all groups, and
the lowest percentage of cohesive failure was 66.3% in
the silane-pretreated CUB group (Fig. 2C).
FE-SEM observations
Figure 3 shows the representative FE-SEM images of
debonded specimens in ADU and CUB with/without
silane pretreatment. The FE-SEM images of specimens
with silane pretreatment showed no clear differences in
morphological appearance compared with specimens
not pretreated with silane. The debonded specimens
showed predominantly cohesive failure at lower magni-
fication. The fracture mainly occurred in universal
adhesives and composite reins.

Table 2 Microleakage data

Effect of silane pretreatment on shear bond strength (SBS) and The average percentage of microleakage values ranged
microleakage of four universal adhesives from 0.102  0.093 to 0.344  0.070, as shown in
Table 2. Without additional silane pretreatment, the
Test
Universal Silane percentage microleakage of the CUB (silane-containing
adhesive pretreatment SBS (MPa) Microleakage (%) universal adhesive) group was significantly higher than
that of the ADU (silane-free universal adhesive) group
ABU 17.540  3.142ab 0.285  0.139CD
+ 24.934  3.379cd 0.135  0.042AB (P < 0.05). With silane pretreatment, microleakage per-
ADU 17.778  2.370ab 0.210  0.056BC centages were not significantly different between groups
+ 27.298  3.622d 0.102  0.093A (P > 0.05). The microleakage percentage was signifi-
CUB 14.250  1.653a 0.344  0.070D cantly lower in groups that were pretreated with silane
+ 23.243  2.624c 0.140  0.118AB compared with groups that were not pretreated
SBU 18.143  2.636b 0.266  0.069CD (P < 0.05). Figure 4 shows the representative light
+ 32.962  2.919e 0.128  0.060AB
microscopy images for ABU and SBU with/without
, no silane pretreatment; +, silane pretreatment; ABU, All Bond silane pretreatment. Compared with the silane pretreat-
Universal; ADU, Adhese Universal; CUB, Clearfil Universal ment groups, the non-pretreatment groups of ABU and
Bond; SBU, Single Bond Universal. SBU presented higher degrees of Basic Fuchsin uptake
Values are given as mean  SD. Groups with the same super-
along the ceramic–resin interface. The images obtained
script lower-case letters (SBS) and superscript upper-case letters
(microleakage) are not statistically different (P > 0.05). from light microscopy revealed that the percentage of
microleakage decreased under pretreatment conditions.

Fig. 2. Failure mode distribution in the study groups. (A) Schematic view of failure mode. Failure within ceramic was classified
as adhesive failure mode, while failure within resin or adhesive was regarded as cohesive failure mode. AL, adhesive layer; GC,
lithium disilicate glass ceramic; R, composite resin. (B, C) Failure percentage of the different study groups. ABU, All Bond
Universal; ADU, Adhese Universal; CUB, Clearfil Universal Bond; SBU, Single Bond Universal.
 Effect of silane on bonding of universal adhesive 5

A B C

D E F

G H I

J K L

Fig. 3. Representative field-emission scanning electron microscopy (FE-SEM) images of the fracture surface. (A) Overview of the
Adhese Universal (ADU) group without silane pretreatment: nearly one-quarter of the specimens failed at the ceramic surface.
(B, C) Higher magnifications of the region showing adhesive failure. (D) Overview of the Clearfil Universal Bond (CUB) group
without silane pretreatment: cohesive failure dominated. (E, F) Higher magnifications of the region showing cohesive failure. (G)
Overview of the ADU group with silane pretreatment: fewer than one-quarter of the specimens failed at the ceramic surface. (H,
I) Higher magnifications of the transition zone. (J) Overview of the CUB group with silane pretreatment: cohesive failure domi-
nated. (K, L) Higher magnifications of the region showing cohesive failure. AF, adhesive failure mode; CF, cohesive failure mode.
Magnifications: A, D, G, J, 249; B, E, H, K, 5,0009; C, F, I, L, 20,0009.

Discussion silane-containing universal adhesives was not better

Based on the results of the present study, the first null
hypothesis, ‘There is no difference in the bonding per-
formance between silane-containing universal adhesives
and silane-free adhesives’, cannot be rejected. Without
the additional silane pretreatment, SBS results showed
that neither the CUB group nor the SBU group (silane-
containing universal adhesives) differed significantly
from the two silane-free groups. The percentage
microleakage of the CUB group was higher than that
of the ADU group. Therefore, the effectiveness of
than expected. The deactivation of the constituent
silane in some universal adhesives may be attributed to
the complex interaction among different components.
CHEN et al. reported that the incorporation of bisphe-
nyl A glycidyl methacrylate (Bis-GMA) resin signifi-
cantly inhibits the action of silane-containing porcelain
primers and inhibits the chemical reaction between
silane primer and lithium disilicate glass ceramic (24).
The CUB adhesive contains not only silane but also
Bis-GMA. The two components coexisting in one
6 Yao et al.

A B

C D

Fig. 4. Representative light microscopy images of margin sealing. All Bond Universal (ABU) and Single Bond Universal (SBU)
groups without (A, B) and with (C, D) silane pretreatment. AL, adhesive layer; GC, lithium disilicate glass ceramic; R, composite
resin. The pointer indicates the area of existing microleakage.

bottle may have a negative influence on the efficiency
of a universal adhesive. Additionally, prehydrolyzed
silane stored in one bottle has a relatively short shelf-
life and may reduce the effectiveness (25).
The results of the present study showed that among
the groups given additional silane pretreatment, the
SBS was highest for SBU and the microleakage of the
four universal adhesives did not significantly differ.
This finding indicates that the additional silane was
more effective when SBU was applied. The composi-
tions and numbers of steps differ among various adhe-
sives and hence may account for their different
performances (26). The functional monomer, methacry-
loxydecyl phosphate (MDP), is an essential component
when adhesives are used to bond to tooth tissues
(27–29). Although MDP may not contribute to glass
ceramic bonding, all universal adhesives in this study
contained this component. Consequently, another dis-
tinct component may explain this difference. The SBU
adhesive contained Vitrebond Copolymer (VCP) (30),
which is a type of methacrylate-modified polyalkenoic
acid copolymer. For SBU, SEZINANDO et al. (31)
revealed a chemical interaction between VCP and
hydroxyapatite, using Fourier transform infrared
(FTIR) spectroscopy and phosphorus-31 nuclear mag-
netic resonance (31P NMR). In addition, the VCP could
potentially reduce variation between application proce-
dures by allowing bonding to moist or to dry dentin
(32). Although few studies regarding VCP and ceramic
bonding have been performed, this component may
contribute to less technical sensitivity and its use could
result in improved performance.
Our results showed that the bond strength of the
pretreated universal adhesive groups was higher, and
their microleakage percentages were lower, than those
of the non-pretreated groups. This finding indicates
that additional silane pretreatment played a positive
role. Therefore, the second null hypothesis, ‘There is
no difference in bonding capabilities of groups pre-
treated or not with additional silane’, should be
rejected. A ceramic primer containing 3-methacryloxy-
propyltrimethoxysilane (MPS), which is a commonly
used and effective silane component, was used in this
study to improve bond strength. The dominant mecha-
nism is that silane molecules can react with water to
form three silanol groups (–Si–OH) from the corre-
sponding methoxy groups (–Si–O–CH3). The silanol
groups then continuously react with the glass ceramic
surface to form a siloxane network (–Si–O–Si–O–).
Additional silane pretreatment contributes to form a
uniform and functional layer that is beneficial for
adhesion of resin to glass substrate. Then, the mono-
meric ends of silane can react with methacrylate
groups of composite resins through free-radical poly-
merization (33), mainly because silane monomers con-
tain C=C bonds (25). Therefore, silane creates a
bridge between glass substrate and composite resins.
Through the polymerization between silane and
methacrylate monomer and between methacrylate
monomer and another methacrylate monomer, a
strong bond between glass substrate and resin is
formed. Although some universal adhesives contained
silane coupling agent, an effective silane may be insuf-
ficient to form a strong siloxane network.

Considering that constituent silane in universal adhe-
sives does not markedly improve chemical bonding
between glass ceramics and composite resins, and that
additional silane is more beneficial in this case, we sug-
gested that additional silane pretreatment is essential for
strong bonding of resin to glass ceramic. A previous
study similarly reported that an additional silanization
step cannot be omitted if the repair protocol comprises
HF acid etching for CAD/CAM aesthetic restorative
materials (34). Another study also reported that the use
of a separate silane primer or silane freshly mixed with
the adhesive is recommended to bond glass-rich ceramics
(35).
In this study, SBS and microleakage percentage were
analysed. Microleakage of the ceramic–resin interface
remains a challenge for clinicians. On the one hand,
insufficient sealing could allow the penetration of bacte-
ria and increase the clinical failure rate of restorations.
On the other hand, in the evolution of dental adhesives,
increasingly higher concentrations of water and hydro-
philic solvent have been used, which increases the ten-
dency to create micro-size bubbles in the adhesive
layer, resulting in phase separation (36, 37). Therefore,
marginal adaptation is a crucial factor that influences
the bonding of restorations. Assessment of microleak-
age combined with measurement of SBS provides a
more comprehensive observation of bonding perfor-
mance and further clarifies the mutual importance of
these indices. However, the relationship between
microleakage and bond strength remains unclear. For
instance, a previous study showed no statistically signif-
icant correlation between the two indices (38), while
another study found that an inverse relationship existed
between these indices (39). Basically, microleakage was
negatively correlated with SBS in this study.
Some manufacturers of universal adhesive have
claimed that additional ceramic primer was unnecessary
for the bonding of multiple-component adhesives. In
this short-term study, the bond strength of silane-con-
taining universal adhesives was not significantly higher
than that of silane-free adhesives. Additional silane pre-
treatment played an important role in promoting glass
ceramic bonding. Taking all the above-mentioned
results together, the application of additional silane
remains to be significant for bonding glass ceramics.
However, most adhesive restoratives are limited by
their durability (40, 41). Thus, further studies of univer-
sal adhesives regarding aging in vitro and medium- and
long-term clinical outcomes in vivo should be
conducted. Moreover, a more stable chemical
ceramic–resin bond should be developed by improving
silanization to universal adhesives.
Within the limitations of the present study, the results
indicate that additional silane pretreatment can effec-
tively improve bonding strength and marginal sealing on
lithium disilicate glass ceramic bonding. Without
pretreatment, the performance of silane-containing uni-
versal adhesives in terms of immediate bonding is similar
to that of silane-free adhesives. Therefore, the con-
stituent silane in universal adhesives could not com-
pletely replace the use of additional silane pretreatment
Effect of silane on bonding of universal adhesive 7
in the present stage, and additional silane is clinically
recommended.
Acknowledgements – This study was financially supported by
grants 81371191 from the National Nature Science Foundation of
China.
Conflicts of interest – The authors of this manuscript declare no
conflict of interest.
References
1. WOLFART S, ESCHBACH S, SCHERRER S, KERN M. Clinical out-
come of three-unit lithium-disilicate glass-ceramic fixed dental
prostheses: up to 8 years results. Dent Mater 2009; 25: e63–
e71.
2. SULAIMAN TA, DELGADO AJ, DONOVAN TE. Survival rate of
lithium disilicate restorations at 4 years: a retrospective study.
J Prosthet Dent 2015; 114: 364–366.
3. PEUMANS M, HIKITA K, DE MUNCK J, VAN LANDUYT K, POI-
TEVIN A, LAMBRECHTS P, VAN MEERBEEK B. Effects of cera-
mic surface treatments on the bond strength of an adhesive
luting agent to CAD-CAM ceramic. J Dent 2007; 35: 282–
288.
4. BELLI R, PETSCHELT A, HOFNER B, HAJTO J, SCHERRER SS,
LOHBAUER U. Fracture rates and lifetime estimations of
CAD/CAM all-ceramic restorations. J Dent Res 2016; 95:
67–73.
5. BRENTEL AS, OZCAN M, VALANDRO LF, ALARCA LG, AMARAL
R, BOTTINO MA. Microtensile bond strength of a resin cement
to feldpathic ceramic after different etching and silanization
regimens in dry and aged conditions. Dent Mater 2007; 23:
1323–1331.
6. TIAN T, TSOI JK, MATINLINNA JP, BURROW MF. Aspects of
bonding between resin luting cements and glass ceramic mate-
rials. Dent Mater 2014; 30: e147–e162.
7. PASHLEY DH, TAY FR, BRESCHI L, TJADERHANE L, CARVALHO
RM, CARRILHO M, TEZVERGIL-MUTLUAY A. State of the art
etch-and-rinse adhesives. Dent Mater 2011; 27: 1–16.
8. VAN MEERBEEK B, YOSHIHARA K, YOSHIDA Y, MINE A, DE
MUNCK J, VAN LANDUYT KL. State of the art of self-etch
adhesives. Dent Mater 2011; 27: 17–28.
9. ZHANG ZY, TIAN FC, NIU LN, OCHALA K, CHEN C, FU BP,
WANG XY, PASHLEY DH, TAY FR. Defying ageing: an expec-
tation for dentine bonding with universal adhesives? J Dent
2016; 45: 43–52.
10. TAKAMIZAWA T, BARKMEIER WW, TSUJIMOTO A, BERRY TP,
WATANABE H, ERICKSON RL, LATTA MA, MIYAZAKI M. Influ-
ence of different etching modes on bond strength and fatigue
strength to dentin using universal adhesive systems. Dent
Mater 2016; 32: e9–e21.
11. TSUJIMOTO A, BARKMEIER WW, TAKAMIZAWA T, WATANABE
H, JOHNSON WW, LATTA MA, MIYAZAKI M. Influence of
duration of phosphoric acid pre-etching on bond durability
of universal adhesives and surface free-energy characteristics
of enamel. Eur J Oral Sci 2016; 124: 377–386.
€
12. SODERHOLM KJ, SHANG SW. Molecular orientation of silane
at the surface of colloidal silica. J Dent Res 1993; 72: 1050–
1054.
13. QUEIROZ JR, BENETTI P, OZCAN M, DE OLIVEIRA LF, DELLA
BONA A, TAKAHASHI FE, BOTTINO MA. Surface characteriza-
tion of feldspathic ceramic using ATR FT-IR and ellipsome-
try after various silanization protocols. Dent Mater 2012; 28:
189–196.
14. SUN R, SUANSUWAN N, KILPATRICK N, SWAIN M. Characteri-
sation of tribochemically assisted bonding of composite resin
to porcelain and metal. J Dent 2000; 28: 441–445.
15. MAY LG, PASSOS SP, CAPELLI DB, OZCAN M, BOTTINO MA,
VALANDRO LF. Effect of silica coating combined to a MDP-
based primer on the resin bond to Y-TZP ceramic. J Biomed
Mater Res B Appl Biomater 2010; 95: 69–74.
8 Yao et al.
16. SAKAI M, TAIRA Y, SAWASE T. Silane primers rather than heat
treatment contribute to adhesive bonding between tri-n-butyl-
borane resin and a machinable leucite-reinforced ceramic.
Dent Mater J 2011; 30: 854–860.
17. KIM JH, CHAE SY, LEE Y, HAN GJ, CHO BH. Effects of mul-
tipurpose, universal adhesives on resin bonding to zirconia
ceramic. Oper Dent 2015; 40: 55–62.
18. XIE H, LI Q, ZHANG F, LU Y, TAY FR, QIAN M, CHEN C.
Comparison of resin bonding improvements to zirconia
between one-bottle universal adhesives and tribochemical sil-
ica coating, which is better? Dent Mater 2016; 32: 403–411.
19. KIM RJ, WOO JS, LEE IB, YI YA, HWANG JY, SEO DG. Per-
formance of universal adhesives on bonding to leucite-rein-
forced ceramic. Biomater Res 2015; 19: 11.
20. TSUJIMOTO A, BARKMEIER WW, TAKAMIZAWA T, WATANABE
H, JOHNSON WW, LATTA MA, MIYAZAKI M. Relationship
between mechanical properties and bond durability of short
fiber-reinforced resin composite with universal adhesive. Eur
J Oral Sci 2016; 124: 480–489.
21. WANG C, NIU LN, WANG YJ, JIAO K, LIU Y, ZHOU W, SHEN
LJ, FANG M, LI M, ZHANG X, TAY FR, CHEN JH. Bonding
of resin cement to zirconia with high pressure primer coating.
PLoS One 2014; 9: e101174.
22. KERN M, BARLOI A, YANG B. Surface conditioning influences
zirconia ceramic bonding. J Dent Res 2009; 88: 817–822.
23. ASCHENBRENNER CM, LANG R, HANDEL G, BEHR M. Analysis
of marginal adaptation and sealing to enamel and dentin of
four self-adhesive resin cements. Clin Oral Investig 2011; 16:
191–200.
24. CHEN L, SHEN H, SUH BI. Effect of incorporating BisGMA
resin on the bonding properties of silane and zirconia pri-
mers. J Prosthet Dent 2013; 110: 402–407.
25. LUNG CY, MATINLINNA JP. Aspects of silane coupling agents
and surface conditioning in dentistry: an overview. Dent
Mater 2012; 28: 467–477.
26. MUNOZ MA, LUQUE I, HASS V, REIS A, LOGUERCIO AD, BOM-
BARDA NH. Immediate bonding properties of universal adhe-
sives to dentine. J Dent 2013; 41: 404–411.
27. YOSHIHARA K, YOSHIDA Y, HAYAKAWA S, NAGAOKA N, IRIE
M, OGAWA T, VAN LANDUYT KL, OSAKA A, SUZUKI K, MIN-
AGI S, VAN MEERBEEK B. Nanolayering of phosphoric acid
ester monomer on enamel and dentin. Acta Biomater 2011; 7:
3187–3195.
28. ZHOU L, WANG Y, YANG H, GUO J, TAY FR, HUANG C.
Effect of chemical interaction on the bonding strengths of
self-etching adhesives to deproteinised dentine. J Dent 2015;
43: 973–980.
29. YOSHIDA Y, NAGAKANE K, FUKUDA R, NAKAYAMA Y, OKAZA-
KI M, SHINTANI H, INOUE S, TAGAWA Y, SUZUKI K, DE
MUNCK J, VAN MEERBEEK B. Comparative study on adhesive
performance of functional monomers. J Dent Res 2004; 83:
454–458.
30. CHEN C, NIU LN, XIE H, ZHANG ZY, ZHOU LQ, JIAO K,
CHEN JH, PASHLEY DH, TAY FR. Bonding of universal adhe-
sives to dentine–Old wine in new bottles? J Dent 2015; 43:
525–536.
31. SEZINANDO A, SERRANO ML, PEREZ VM, MUNOZ RA, CEBAL-
LOS L, PERDIGAO J. Chemical Adhesion of Polyalkenoate-
based Adhesives to Hydroxyapatite. J Adhes Dent 2016; 18:
257–265.
32. KIM J-Y, CHO G-Y, ROH B-D, SHIN Y. Effect of curing mode
on shear bond strength of self-adhesive cement to composite
blocks. Materials 2016; 9: 210.
33. O€ ZCAN M, VALLITTU PK. Effect of surface conditioning meth-
ods on the bond strength of luting cement to ceramics. Dent
Mater 2003; 19: 725–731.
34. ZAGHLOUL H, ELKASSAS DW, HARIDY MF. Effect of incorpo-
ration of silane in the bonding agent on the repair potential
of machinable esthetic blocks. Eur J Dent 2014; 8: 44–52.
35. YOSHIHARA K, NAGAOKA N, SONODA A, MARUO Y, MAKITA
Y, OKIHARA T, IRIE M, YOSHIDA Y, VAN MEERBEEK B. Effec-
tiveness and stability of silane coupling agent incorporated in
‘universal’ adhesives. Dent Mater 2016; 32: 1218–1225.
36. TAKAMIZAWA T, BARKMEIER WW, TSUJIMOTO A, SCHEIDEL
DD, WATANABE H, ERICKSON RL, LATTA MA, MIYAZAKI M.
Influence of water storage on fatigue strength of self-etch
adhesives. J Dent 2015; 43: 1416–1427.
37. VAN LANDUYT KL, SNAUWAERT J, DE MUNCK J, PEUMANS M,
YOSHIDA Y, POITEVIN A, COUTINHO E, SUZUKI K, LAMBRECHTS
P, VAN MEERBEEK B. Systematic review of the chemical com-
position of contemporary dental adhesives. Biomaterials 2007;
28: 3757–3785.
38. FORTIN D, SWIFT EJ Jr, DENEHY GE, REINHARDT JW. Bond
strength and microleakage of current dentin adhesives. Dent
Mater 1994; 10: 253–258.
39. PRATI C, SIMPSON M, MITCHEM J, TAO L, PASHLEY DH. Rela-
tionship between bond strength and microleakage measured
in the same Class I restorations. Dent Mater 1992; 8: 37–41.
40. VAN MEERBEEK B, PERDIGAO ~ J, LAMBRECHTS P, VANHERLE G.
The clinical performance of adhesives. J Dent 1998; 26: 1–20.
41. LIU Y, TJADERHANE L, BRESCHI L, MAZZONI A, LI N, MAO J,
PASHLEY DH, TAY FR. Limitations in bonding to dentin and
experimental strategies to prevent bond degradation. J Dent
Res 2011; 90: 953–968.