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Effect of MDP-Based Silane and Different Surface Conditioner Methods on

Bonding of Resin Cements to Zirconium Framework: Effect of MDP on
Bonding of Cements to Zirconium

Article  in  Journal of Prosthodontics · July 2017

DOI: 10.1111/jopr.12650

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Effect of MDP-Based Silane and Different Surface
Conditioner Methods on Bonding of Resin Cements
to Zirconium Framework
Hatice Özdemir, PhD, Nuran Yanikoğlu, DDS, PhD , & Nurdan Sağsöz, PhD
Department of Prosthodontics, Faculty of Dentistry, Atatürk University, Erzurum, Turkey

Keywords
Bonding; MDP; resin cement; surface
conditioner method; zirconium.
Correspondence
Hatice Özdemir, Atatürk University, Facullty
of Dentistry, Department of Prosthodontics,
Erzurum, 25040, Turkey.
E-mail: dentist_hatice@hotmail.com.
Presented as a poster in Congress of EPA,
2013, Finland, under the title “Effect of
different surface treatments on bonding of
resin cements to zirconium.”
This study was supported by Atatürk
University, Project of Scientific Research,
project number 2011–44.
The authors deny any conflicts of interest.
Accepted April 14, 2017
doi: 10.1111/jopr.12650
Abstract
Purpose: To determine the shear bond strength (SBS) between zirconium framework
and resin cements after different surface conditioner methods and after application of
10-methacryloyloxydecyl dihydrogen phosphate (MDP) based silane and a bonding
agent mix.
Materials and Methods: 128 disc-shaped zirconium-oxide specimens were prepared.
Specimens were placed in autopolymerizing acrylic resin. The bonding surface of
specimens was smoothed consecutively with 600-, 800-, and 1200-grit silicon carbide
papers under water cooling. Eight groups were prepared: CJ, Co-Jet; N, Nd-YAG
laser; E, Er-YAG laser; NS, Nd-YAG laser + silane; ES, Er-YAG laser + silane;
CJB, Co-Jet + bonding agent; NSB, Nd-YAG laser + silane + bonding agent; ESB,
Er-YAG laser + silane + bonding agent. SEM analysis was performed under 2000×
magnification. Dual- and self-cured resin cements were bonded to specimens, and
shear force was applied. Data were analyzed with one-way ANOVA and Tukey’s
multiple comparison test (p < 0.05).
Results: The SBS values differed from each other among the groups. While the
CJB group showed the highest values, the N group showed the lowest. The treatment
with MDP-based silane and bonding agent mix increased SBS values of each cement
belonging to each group. SB values of dual-cure resin cement were higher than those
of self-cure resin cements.
Conclusion: Different surface conditioner methods exhibit an important effect on
the SBS of resin cements to zirconium. The application of MDP-based silane and
bonding agent mix enhanced SB values.

Metal framework can be used to improve strength and frac-
ture resistance of fixed restorations. Researchers have investi-
gated new esthetic framework materials and techniques for this
purpose.1 Owing to its excellent mechanical properties, zir-
conium has emerged as an alternative framework material for
preparing all-ceramic restorations.2-4 Zirconium frameworks
are also a preferred choice for fixed restorations because of
their good fracture strength and esthetics; however, the bond
strength between zirconium and resin cements is a problem,
except when MDP is applied to zirconium framework or mixed
with resin cements.5
The strength of the framework material and the cementation
procedure are both important for achieving clinical success.6,7
Several surface conditioner methods have been applied to zir-
conium framework surfaces, and their efficiencies have been
evaluated; however, there is no consensus about the most effec-
tive surface conditioner method to increase the bond strength
between resin cement and zirconium framework.8 Different sur-
face conditioner methods such as acid etching and silanization
are used to enhance the bond strength of lithium-disilicate-
based, silica-based, leucite, and feldspathic ceramics.9-13 How-
ever, these surface conditioner methods do not have similar
effects on zirconium framework, owing to the absence of sil-
ica and glass phases in zirconium.14-19 Several studies have
shown that for enhancing the bond strength of silica-based,
glass-infiltrated alumina and zirconium, silica coating follow-
ing silanization can be useful for clinicians.15,19-22 Several tech-
niques, including the Co-Jet system, exist for silica coating and
silanization of framework surfaces.14,19,21-23 In this system, a
tribochemical silica coating is created on the metal ceramic
surface and all-ceramic systems for clinical applications such
as intraoral repairing.19,22,23
Lasers can also be used to roughen the surface of a framework
for enhancing the bond strength of resin cements.10,24-29 Er-
YAG lasers are typically used in dentistry owing to wavelength
and amount of absorption. Nd-YAG lasers are also preferred

Journal of Prosthodontics 0 (2017) 1–6 

C 2017 by the American College of Prosthodontists 1
Effect of MDP on Bonding of Cements to Zirconium Özdemir et al

Table 1 Experimental groups and surface treatments

Group n Treatments

CJ 16 Silica coating with CoJet-Sand (CoJet Sand; 3M ESPE, Seefeld, Germany) perpendicular to the surface from a distance
approximately 10 mm for a period of 15 seconds at 2.8 bar pressure.
ND 16 Nd:YAG laser irradiation (Smartlife; DEKA, Calenzano, Italy) at power output: 2 W (100 mJ/pulse, 12 Hz) for 2 minute from a
distance approximately of 1 mm.
ER 16 Er:YAG laser irradiation (Smart 2940D PLUS; Deka) at power output: 2 W (200 mJ/ pulse, 10 Hz) for 10 seconds from a
distance approximately 1 mm.
NDS 16 Same as group ND plus the zirconium surfaces were coated with silane coupling agent and allowed to air dry for 5 minutes.
ERS 16 Same as group ER plus the zirconium surfaces were coated with silane coupling agent and allowed to air dry for 5 minutes.
CJB 16 Same as group CJ plus bonding and silane coupling agent were mixed according to the manufacturer’s recommendations
and the literature.36 The mixture was applied and air-thinned for 3 seconds with air spray.
NDSB 16 Same as group ND plus bonding and silane coupling agent mixture were applied as with group CJB.
ERSB 16 Same as group ER plus bonding and silane coupling agent mixture were applied as in group CJB.

in different fields of dentistry.30 The bond strength of compos-
ite resins to ceramic increases after Nd-YAG laser application
enhances the formation of ceramic surface disorganizations.25
Furthermore, Nd-YAG laser application is suitable for zirco-
nium frameworks, owing to zirconium framework’s strength
and comparatively low heat conductibility.31 Another study re-
ported that Nd-YAG laser application followed by air abra-
sion enhanced the bond strength between resin cement and
zirconium framework.28,29 Based on these studies, it can be
assumed that laser application along with some surface condi-
tioner method would have a positive effect on the shear bond
strength (SBS) of resin cement to zirconium framework. This
study attempts to evaluate the SBS of resin cements to zirco-
nium framework after Er-YAG and Nd-YAG laser application
along with an MDP-based silane and bonding agent mix, with
the goal of increasing the SBS of resin cements to zirconium-
oxide ceramics.
Blatz et al32 determined that the application of MDP-based
silane and a bonding agent mix followed by air abrasion may
enhance the SBS of resin cements to zirconium. In parallel with
this result, several authors reported that the application of MDP-
based silane and bonding agent mix followed by air abrasion
increased the bond strength of resin cements to zirconium and
alumina-oxide framework.32-34
The purpose of this study is to determine the SBS between
different resin cements and zirconium framework after the ap-
plication of various surface conditioner methods and an MDP-
based silane and bonding agent mix. The null hypothesis is that
the application of a silica coating and an MDP-based silane and
bonding agent mix after laser application increases the SBS of
resin cements to zirconium framework.
Materials and methods
This study evaluated the SBS between zirconium framework
and different resin cements. A total of 128 disc-shaped (di-
ameter: 10 mm; thickness: 2 mm) zirconium-oxide ceramic
specimens were fabricated from ingots according to the manu-
facturer’s recommendation. Zirconium specimens were placed
in autopolymerizing acrylic resin (Imıcryl, SC, Konya, Turkey)
blocks. The bonding surface of the zirconium specimens was
smoothed with 600-, 800-, and 1200-grit silicon carbide papers
under water cooling to standardize the roughness of specimens.
All specimens were ultrasonically cleaned and dried with oil-
free air before applying surface conditioner method. The fol-
lowing eight surface conditioner method groups were studied:
CJ, Co-Jet; N, Nd-YAG laser; E, Er-YAG laser; NS, Nd-YAG
laser + silane; ES, Er-YAG laser + silane; CJB, Co-Jet +
bonding agent; NSB, Nd-YAG laser + silane + bonding agent;
ESB, Er-YAG laser + silane + bonding agent. The silane agent
was prepared by mixing an equal amount of Clearfil SE Bond
primer and Clearfil Porcelain Bond Activator (Kuraray Medical
Inc., Okayama, Japan). The Clearfil SE Bond system was used
as the bonding agent. Surface conditioner methods and their
applications are defined in detail in Table 1. After completing
each surface conditioner method to determine its effect on the
specimen surface, one specimen from each group was randomly
selected and examined by SEM at 2000× magnification.
Next, composite resin cylinders were attached to the speci-
men surfaces using dual-cure (Panavia F 2.0; Kuraray Noritake
Dental Inc., Tokyo, Japan) and self-cure (Multilink N; Ivoclar
Vivadent AG, Schaan, Liechtenstein) resin cements. The resin
cements were applied according to the manufacturer’s instruc-
tions. The zirconium specimens attached with composite resin
were placed under a 1 kg load in a press,32,35,36 and overflowing
cement was removed with a brush from margins. The dual-
cured resin cement was cured by LED light for 40 seconds,
and oxygen-blocking gel (Oxyguard II; Kuraray Noritake Den-
tal Inc.) was processed for 10 minutes before lifting the press.
The self-cured resin cement was self-polymerized, and oxygen-
blocking gel was processed for 60 minutes before lifting the
press.19,22 The specimens attached with composite resin cylin-
ders were washed with water and stored in distilled water at
37°C for 24 hours. The SBS was determined using a univer-
sal testing machine (Instron, Model 2710-003; Instron Corp.,
Norwood, MA) with a 0.5 mm/min crosshead speed. The spec-
imens were placed in a universal testing machine, and SBS was
recorded in megapascals (MPa) when separation occurred. Data
were analyzed by least square ANOVA using the general linear
model (GLM), and Tukey’s multiple range tests were used to
determine the significance of differences in the SBS among the
groups (p < 0.05) (SPSS 20.0).

2 Journal of Prosthodontics 0 (2017) 1–6 

C 2017 by the American College of Prosthodontists
Özdemir et al Effect of MDP on Bonding of Cements to Zirconium

Table 2 Results of one-way ANOVA

Discussion
Self-cure df Mean square F
The results of the present study indicate that the SBS is affected
Surface treatment 7 33.285 34.49∗∗∗ by different surface conditioner methods and resin cements. The
Error 56 0.965 CJ group and the groups using an MDP-based silane and bond-
Dual-cure df Mean square F
ing agent attached with MDP-based resin cement demonstrated
the highest bond strength. These results partially supported the
Surface treatment 7 56.437 67.157∗∗∗ hypothesis of the present study. Specimens with laser appli-
Error 56 0.840 cation showed the lowest bond strengths, and the application
of MDP-based silane and bonding agent followed by Nd-YAG
***
: p < 0.001. laser application had no positive effect on SBS. Nevertheless, it
is important to note that the application of a silane agent and an
Table 3 Means and standard deviation of each group, Tukey compar- MDP-based silane and bonding agent mix followed by Er-YAG
isons, and Student’s t-test results laser application enhanced the bond strengths of resin cements
to zirconium framework.
Surface t test Although the fracture-load resistance and maximum strength
treatments N Self-cure Dual-cure p for in vitro zirconium frameworks have been demonstrated,
CJ 8 4.30 ± 0.87b 5.51 ± 0.84c 0.013∗ they also show durable bonding with cements.37-39 MDP-based
ND 8 1.18 ± 0.43d 2.13 ± 0.31d <0.0001∗∗∗ monomers were essentially produced to enhance the bond
ER 8 2.11 ± 0.79d 2.75 ± 0.37d 0.052ns strength to metal oxides.40 MDP acts as an adhesive functional
NDS 8 2.26 ± 0.36cd 2.34 ± 0.56d 0.748ns monomer and powerfully bonds with metal oxides existing on
ERS 8 3.80 ± 0.88bc 6.46 ± 1.56bc 0.001∗∗ the surface of the pure base metal.39,41 Based on the periodic
CJB 8 6.55 ± 1.30a 9.07 ± 0.92a 0.001∗∗ table, zirconium is a metal. Therefore, MDP monomers will
NDSB 8 6.53 ± 0.89a 7.36 ± 1.32b 0.159ns show the same effects on the zirconium surface. As a result of
ERSB 8 5.26 ± 1.67ab 7.36 ± 0.68b 0.005∗∗ coating with an inactive zirconium oxide film, the surface prop-
Total 64 4.00 ± 2.13 5.37 ± 2.65 0.002 erties of the zirconium are conferred to the metal surface.8 As
soon as MDP is applied to the zirconium surface, the phosphate
Means in columns with different superscripts are significantly different at p < ester of MDP connects to the hydroxyl groups of zirconium.8,40
0.01; * : p < 0.05, ** : p < 0.01, *** : p < 0.001, ns: nonsignificant. The hypothesis of the present study was that the bond strength
can be enhanced by applying an MDP-based silane and bond-
Results ing agent mix followed by silica coating and laser applica-
tion. The results of the present study support the hypothesis of
Table 2 summarizes the one-way ANOVA results. The SBS this study. In contrast with our findings, de Souza et al,42 da
showed significant differences among the groups depending Silva et al,43 and Xie et al44 reported that using MDP-based
on the surface-conditioning method and resin cement (p < primers had no positive effect on the bond strength of resin
0.01). The evaluation of the interaction between the surface- cements. Manufacturers have noted that universal adhesives
conditioning method and the resin cement was statistically sig- and zirconium primers act as MDP enhances the bond strength
nificant (p < 0.001). to zirconium. MDP was improved to provide attachment with
Table 3 lists the SBS values. While the CJB group showed bis-GMA and metal oxides such as zirconium and alumina.33
the highest SBS values (p = 0.001), the ND group showed the Chemical retention is very important for bonding cements to
lowest SBS values (p < 0.001) for two different resin cements. oxide ceramics. Therefore, different cement systems have been
The application of MDP-based silane and the bonding agent suggested to clinicians for providing durable bond strength to
mix increased the SBS of each cement belonging to each group. fixed restorations.45 For chemical retention, MDP-based resin
But the NDS (p = 0.748) and NDSB (p = 0.159) groups showed cements may be the most suitable cements owing to the chem-
no significant differences. The SBS values of the dual-cure resin ical bonding of MDP to zirconium or alumina.45-47 According
cement are higher than those of the self-cure resin cement, to Özcan and Bernasconi, MDP-based resin cements provide
and the difference among the resin cements was statistically a stronger bond strength than other cement types when tested
significant. with different test methods.48 Wolfart et al45 reported that the
Multiple comparisons among the groups were evaluated with application of MDP-based composite resin on the ceramic sur-
Tukey’s HSD test (Table 3). There were statistically significant face followed by air abrasion provided the highest bond strength
differences among the groups at p < 0.01. values. de Oyagüe et al49 claimed that the 10-MDP-based ce-
Figure 1 shows the SEM images of the zirconium specimens ments appears to be the most appropriate system for bonding
after surface conditioner method (Co-Jet application, Nd-YAG, zirconium surfaces. In the present study, dual-cure resin cement
and Er-YAG laser application). Those specimens subjected to showed higher SBS values than self-cure resin cement. Panavia
Co-Jet application showed a relatively large number of retentive F 2.0 dual-cure resin cement is an MDP-based resin cement,
and irregular areas. Further, those specimens subjected to Er- and its polymerization can be increased by use of LED light
YAG and Nd-YAG laser application showed nonretentive and curing. Depending on these, dual-cure resin cement showed a
regular areas. high SBS value.

Journal of Prosthodontics 0 (2017) 1–6 

C 2017 by the American College of Prosthodontists 3
Effect of MDP on Bonding of Cements to Zirconium
Figure 1 SEM observation of the zirconium after surface treatments at 2000× magnification (A) Co-Jet group; (B) Er:YAG laser group; (C). Nd: YAG
laser group.
In the present study, the Co-Jet system enhanced the bonding
of resin cements to zirconium framework. The mechanism is
as follows: (1) formation of a topographic structure enabled
micromechanical retention with resin cements, (2) chemical
retention allowed bonding between silane and silica-coated zir-
conium surface, and (3) creation of a chemical bond allowed at-
tachment between MDP and zircona oxides.50 A silica coating
may support chemical retention at the zirconium-resin inter-
face. In the Co-Jet system, the application of alumina particles
modified by silica led to the formation of a silica layer on the
zirconium surface.51 In light of these findings, the application
of MDP-based silane and bonding agent mix followed by silica
coating is suggested to enhance the SBS between zirconium
and resin cement. The silane agent not only supports chemical
bonding but also improves the surface energy of the substrate
and surface wettability of resin cements.22
Laser irradiation is an alternative method to conventional
surface conditioning methods.50 Akyıl et al52 reported that Er-
YAG laser application enhanced resin cement bonding to a
zirconium-oxide ceramic; however, Akyıl et al52 and Stübinger
et al53 reported that Er-YAG laser should not be applied to
zirconium. Cavalcanti et al27 reported that Er-YAG laser ap-
plication with a power setting of 200 mJ/pulse and 10 Hz for
5 seconds was a suitable method to enhance the bond strength of
zirconium to resins. In contrast, in a separate study, Cavalcanti
et al26 reported that Er-YAG laser application with a power
setting of 200 mJ/pulse and 10 Hz for 5 seconds decreased
the bond strength compared with that of an untreated surface.
Murthy et al54 reported that hydrofluoric acid etching and air
abrasion resulted in higher bonding values than CO2 laser ap-
plication for a zirconium crown bonded with resin. Yassaei
et al55 observed that sandblasting was a more effective method
than Er-YAG laser application and HF acid etching for bond-
ing orthodontic brackets to zirconium. Akyıl et al52 reported
the untreated and Co-Jet treated surfaces showed higher bond
strength than a surface with Nd-YAG laser application. Based
on these findings, we infer that the application of a silane and an
MDP-based silane and bonding agent mix following Er-YAG
laser application is likely to enhance the bond strength of resin
cement to zirconium. The application of a silane and an MDP-
4 Journal of Prosthodontics 0 (2017) 1–6 
Özdemir et al
based silane and bonding agent mix following Nd-YAG laser
application had no positive effect on SBS. Er-YAG laser ap-
plication with different power output effects the bond strength.
Therefore, optimum laser power output must be selected to in-
crease the bond strength between zirconium and resin cement.
In the present study, the results of Er-YAG laser applied at
200 mJ/pulse and 10 Hz as suggested by Cavalcanti et al27
supportes the suggestion.
The most commonly used methods for evaluating bond
strength are tensile and SBS tests. The SBS test was selected in
the present study because it is easy to perform and is therefore
highly advantageous.40
Graphite powder was not used, a limitation of this study.
The application of graphite powder increases the effect of laser
beams.56 If graphite powder had been used, the results would
likely be different. Furthermore, MDP-free and MDP-based
silane agent will be compared in a future study. Furthermore,
different parameters will be applied for both Er-YAG and Nd-
YAG laser application.
Conclusions
In accordance with this study’s limitations, the following con-
clusions can be drawn:
1. Different surface conditioner methods exerted an impor-
tant effect on the SBS of resin cements to the zirconium
framework.
2. The application of silane and bonding agent mix on the
zirconium surface had a positive effect on the SBS due
to MDP-based silane. Therefore, the dual-cure resin ce-
ment showed higher SBS values than the self-cure resin
cement.
3. An MDP-based silane and bonding agent mix increased
the SBS of resin cements to the zirconium framework.
Acknowledgment
The authors wish to thank Memiş Özdemir for his professional
assistance with the statistical analysis.
C 2017 by the American College of Prosthodontists
Özdemir et al
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