Effect of silica coating combined to a MDP-based primer

on the resin bond to Y-TZP ceramic

Liliana Gressler May,1 Sheila Pestana Passos,1 Diana Barca Capelli,1 Mutlu Özcan,2
Marco Antonio Bottino,3 Luiz Felipe Valandro4
1
São Jose dos Campos Dental School, São Paulo State University (UNESP), SP, Brazil
2
Center for Dental and Oral Medicine, Clinic for Fixed and Removable Prosthodontics and Dental Materials Science,
Zurich, Switzerland
3
Department of Restorative Dentistry, São Jose dos Campos Dental School, São Paulo State University (UNESP),
São Jose dos Campos, SP, Brazil
4
Department of Restorative Dentistry, Division of Prosthodontics, Federal University of Santa Maria, Santa Maria, RS, Brazil

Received 24 February 2010; revised 21 April 2010; accepted 10 May 2010

Published online 5 August 2010 in Wiley Online Library (wileyonlinelibrary.com). DOI: 10.1002/jbm.b.31684

Abstract: The aim of this study was to evaluate the influence
of silica coating and 10-methacryloyloxydecyl dihydrogen
phosphate (MDP)-based primer applications upon the bond-
ing durability of a MDP-based resin cement to a yttrium stabi-
lized tetragonal zirconia (Y-TZP) ceramic. Ninety-six Y-TZP
tabs were embedded in an acrylic resin (free surface for adhe-
sion: 5
5 mm2), ground finished and randomly divided into
four groups (N ¼ 24) according to the ceramic surface condi-
tioning: (1) cleaning with isopropanol (ALC); (2) ALC þ phos-
phoric acid etching þ MDP-based primer application (MDP-
primer); (3) silica coating þ 3-methacryloyloxypropyl trime-
thoxysilane (MPS)-based coupling agent application (SiO2 þ
before testing. Another half of the specimens were stored (90
days) and thermo-cycled (12,000
) during this period (90d/TC)
before testing. A shear bond strength (SBS) test was per-
formed at a crosshead speed of 0.5 mm/min. Two factors
composed the experimental design: ceramic conditioning
strategy (in four levels) and storage condition (in two levels),
totaling eight groups. After 90d/TC (Tukey; p < 0.05), SiO2 þ
MDP-primer (24.40 MPa) promoted the highest SBS. The ALC
and MDP-primer groups debonded spontaneously during 90d/
TC. Bonding values were higher and more stable in the SiO2
groups. The use of MDP-primer after silica coating increased
the bond strength. V C 2010 Wiley Periodicals, Inc. J Biomed Mater

MPS-Sil); and (4) SiO2 þ MDP-primer. The MDP-based resin Res Part B: Appl Biomater 95B: 69–74, 2010.
cement was applied on the treated surface using a cylindrical
mold (diameter¼ 3 mm). Half of the specimens from each sur- Key Words: tribochemical treatment, coupling agents, bond-
face conditioning were stored in distilled water (37 C, 24 h) ing, adhesion, resin cement, Y-TZP

INTRODUCTION tetragonal to monoclinic phases.10–12 This is a controversial

High values of bond strength between resin cements and
feldspathic ceramics have been obtained in in vitro studies
using hydrofluoric acid etching alone1–3 and after sandblast-
ing,3 or silica coating,4 followed by the application of a sil-
ane onto the ceramic surface. However, some high-strength
ceramic materials, such as aluminum oxide and tetragonal
zirconium oxide polycrystalline ceramics (Y-TZP) are unaf-
fected by acid etching.5 Tribochemical silica coating pro-
duced the highest microtensile strength values for the glass
infiltrated zirconium-based ceramic when compared with
sandblasting.6 The use of air abrasion7,8 or silica coating
associated with application of silane8,9 seems to improve
the bonding results to Y-TZP ceramics. However, the current
information in the scientific literature does not yet permit
the recommendation of surface blasting because of the
reason that there would be a decrease in the fracture resist-
ance of these materials due to the transformation from the
question, since some studies showed opposing findings,
when silica coating procedures were applied even in long-
term conditions.13–15
Some potential bonding results have also been obtained
when the resin cement is based on a 10-methacryloyloxy-
decyl dihydrogen phosphate (MDP) monomer.7,8,16,17 Blatz
et al. 17 found superior long-term bonding strengths to Pro-
cera AllZirkon restorations when using a bonding/silane-
coupling agent containing this adhesive phosphate mono-
mer. After 150 days of storage, Wolfart et al.,7 when com-
paring two cements and air abrasion versus alcohol cleaning,
found that only the air abraded specimens bonded to Pana-
via F showed high bond strengths, whereas the other speci-
mens debonded spontaneously or showed very low bond
strengths.
Studies have shown that the decrease in storage time
and thermal cycling conditions produce a more prominent

Correspondence to: L. F. Valandro; e-mail: lfvalandro@hotmail.com

V
C 2010 WILEY PERIODICALS, INC. 69
TABLE I. Brand Names and Composition of the Adhesive Materials Used in the Study
Brand Name Code Use Composition Manufacturer Batch Number
V
R
ESPE -Sil MPS-Sil Silane coupling agent MPS, ethanol 3M ESPE, Seefeld, 0133
Germany
Clearfill SE MDP-primer Self-etching primer MDP, HEMA, hydrophilic Kuraray Medical, 00788A
bond primer dimethacrylates, Okayama, Japan
dl-camphorquinone,
N,N-diethanol-p-toluidine,
H2O
Clearfill porcelain Silane coupling agent MPS, bisphenol-a- 00215B
bond activator polyethoxy-dimethacrylate
Panavia F 2.0 PAN Resin cement Paste A: MDP, DMA, 512111
silanated silica,
dl-Camphorquinone,
others Paste B: DMA,
silanated barium glass,
sodium fluoride, others

MPS, 3-methacryloyloxypropyl trimethoxysilane; MDP, 10-methacryloyloxydecyldihydrogen phosphate; HEMA, 2-hydroxyethyl methacrylate;

DMA, dimethacrylates.

reduction when bonding to Y-TZP. As an evidence of these MATERIALS AND METHODS

difficulties, some studies have related very low or even null
bond strength values of cements to Y-TZP.7,18
As the tribochemical treatment and the MDP-based
coupling agent seem to be promising to obtain better
bonding between resin cements and Y-TZP, this study was
made to clarify the effect of these procedures on the bond
strength and durability. The outcome might be used as ref-
erence for clinical approach in the cementation of Y-TZP
restorations.
The objectives were to evaluate the influence of silica
coating and application of a MDP-based coupling agent
upon the bonding of a MDP-based resin cement to a Y-TZP
ceramic and to verify the stability of this bonding after stor-
age and thermo-cycling. The hypotheses were (1) silica coat-
ing would promote higher and more stable bond strength
and (2) aging would damage the resin bond when the Y-TZP
surface was only cleaned with alcohol (not coated by silicon
oxides).
Blocks from partially sintered yttria stabilized tetragonal
zirconia (In Ceram YZ 2000 cubes 40/15, Vita Zanhfabrik,
Bad Säckingen, Germany) were sectioned into 96 blocks,
with dimensions of 7.5
7.5
2.5 mm3, using a cutting
machine and diamond-coated disks. These blocks were sin-
tered using the manufacturer’s instructions (VITA ZYrcomat
furnace, Vita Zanhfabrik, Bad Säckingen, Germany). The final
block dimensions after sintering were 5
5
2 mm3 due
to 20–25% shrinkage. The specimens were embedded into
acrylic resin (JET, Clássico, Campo Limpo Paulista, São
Paulo, Brazil) leaving a 5
5 mm2 free surface for adhe-
sion. The specimens were ground finished, using 400-grit to
1200-grit silicon carbide paper (Wetordry Paper, 3M, Campi-
nas, SP, Brazil), with a rotating metallographic polishing
machine (PSK-2V, Skill-Tec, Penha, SP, Brazil) under water-
cooling. The specimens were then cleaned in an ultra-sonic
device (Vitasonic II, Vita Zahnfabrik, Bad Säckingen,
Germany) with distilled water for 5 min.

TABLE II. Experimental Groups According to the Surface Treatment and Storage Conditions

Code Surface Treatment Storage Groups

ALC (control) Surface cleaning 24 h G1

90 d/TC G2
MDP-primer ALC þ PAE þ MDP-primer 24 h G3
90 d/TC G4
SiO2 þ MPS-Sil SiO2 followed by MPS-Sil 24 h G5
90 d/TC G6
SiO2 þ MDP-primer SiO2 followed by MDP-primer 24 h G7
90 d/TC G8

ALC: cleaning with 96% isopropanol, under friction, for 10 s; PAE: phosphoric acid etching (K-etchant gel, Kuraray Medical, Okayama, Japan),
washing, drying; MDP-primer: MDP-based primer/silane coupling agent mixture (1 drop of porcelain bond activator þ 1 drop of clearfill SE bond
primer) applied with a brush for 10 s on the surface and left to dry in the air for 5 min; SiO2: surface silica-coating treatment performed with 30
lm silica–alumina particles (COJET Sand, 3M-ESPE) with an intraoral air abrasion device at the pressure of 2.8 bars, from a distance of 10 mm,
for 15 s; MPS-Sil: MPS coupling agent (Espe-Sil) applied with a brush for 10 s on the surface and left to dry in the air for 5 min; 24 h: storage in
distilled water at 37 C for 24 h, before performing the shear test; 90 d/TC: storage in distilled water at 37 C for 90 days; and 12,000 thermo-
cycles, from 5 to 50 C during the storage period.

70 MAY ET AL. SILICA COATING AND COUPLING AGENTS: EFFECT ON RESIN BOND TO Y-TZP

TABLE III. Summary of the Analysis of Variance (2-Way ANOVA)
Source DF
Surface treatment 3 4760.32
Storage 1 77.56
Surface treatment*storage 3 1367.44
Error 88
* Indicate the interaction of the factors.
Depending on the surface treatment and the storage
condition (Tables I and II), the 96 specimens were randomly
divided into eight groups (n ¼ 12).
After the surface treatment, the MDP-based resin cement
(Panavia F 2.0V, Kuraray, Tokyo, Japan) was handled and
R
applied to the ceramic surface using a split cylindrical mold
(diameter ¼ 3 mm). Light curing (SmartLite PS, Dentsply,
Kontanz, Germany) was performed for 40 s and the mold
was removed after 10 min.
Following the storage period, the shear bond strength
(SBS) test was performed in a universal testing machine,
EMIC DL-1000 (EMIC, São José dos Pinhais, PR, Brazil). The
load (load cell of 50 KgF) was applied using a knife-edge
set-up at a crosshead speed of 0.5 mm/min. Each specimen
was fixed in a custom-made device to ensure that the adhe-
sive interface was parallel and as close as possible to the
knife displacement axis. The shear strength was recorded in
N/mm2 (MPa). The cross-sectional interfacial area (A) was
7.07 mm2 (A ¼ pr2, where p ¼ 3.1416 and r, radius of the
bonding interface ¼ 1.5 mm).
The SBS of specimens that debonded spontaneously dur-
ing aging conditions was considered ‘‘zero’’ for statistical
analysis (Statistix for Windows, Analytical Software, Talla-
hassee, FL). Two-way ANOVA and post-hoc Tukey test (a ¼
0.05) were applied to analyze the SBS data.
The fractured surfaces of all tested specimens were analyzed
at 200
magnification, using an optical microscope (TM-505,
Mitutoyo, Kanagawa, Japan). Specimens with representative frac-
tures were selected, sputter-coated with gold (Denton Vacuum
DESK II, Denton Vacuum, Moorestown, NJ), and observed in
a scanning electron microscope (
1000) (JEOL-JSM-6360,
Tokyo, Japan) to confirm and illustrate the types of failure.
RESULTS
The results of the 2-way ANOVA are described in Table III.
Both tested factors and their interaction had an effect on
the MDP-based resin cement bond to Y-TZP. The F value
TABLE IV. Means and Standard Deviation of Shear Bond
Strength Results According to the Different Surface
Treatments and Storage Conditions
Bond strength (MPa)*
Surface Treatment 24 h 90 d/TC
EF
ALC (control) 3.64 (2.18) 0F
MDP-primer 6.67DE (3.24) 0F
SiO2 þ MPS-Sil 12.32BC (2.99) 17.19B (8.57)
SiO2 þ MDP-primer 11.78CD (2.34) 24.40A (5.43)
Tukey (p < 0.05); *Similar letters represent statistic similarity.
JOURNAL OF BIOMEDICAL MATERIALS RESEARCH B: APPLIED BIOMATERIALS | OCT 2010 VOL 95B, ISSUE 1
ORIGINAL RESEARCH REPORT
SS MS F P
1586.77 95.62 0.000
77.56 4.67 0.0333
455.81 27.47 0.0000
1460.35 16.59
(Table III) showed that the factor surface treatment exhib-
ited a large effect and was about 20 times more influential
upon the SBS than storage conditions.
SBS are presented in Table IV and Figure 1. It can be
observed that the control group (alcohol cleaning) and MDP-
primer application promoted low and unstable bond strengths,
presenting null bond strengths after aging (spontaneous
failures). Otherwise, silica coating developed higher and more
stable bond strengths, whether combined with 3-methacryloy-
loxypropyl trimethoxysilane (MPS)-based silane or when com-
bined with MDP-contend primer. Silica coating followed by the
application of a MDP-based coupling agent (MDP-primer) pre-
sented the highest mean values of bond strength.
The failure type is shown in Table V and some micrographs
(Figure 2) are used to illustrate the types of failure found in
this present study. Adhesive failures (between the resin cement
and Y-TZP surface) occurred for the majority of specimens.
DISCUSSION
This current study was conducted to evaluate the bond
strength of a MDP-based resin cement to a Y-TZP ceramic.
Tensile bond strength tests have been preferred to evaluate
the bond strength, since they have an appropriate design
that favors the occurrence of failure within the adhesive
interface complex. Alternatively, SBS tests were demon-
strated to be governed by the cohesive strength of the base
material used and not by the bond strength of the adhesive
interface, an inherent feature of the geometry of the shear
test arrangement.19 Despite the limitations of the shear test
in evaluating the bond strength in the adhesive interface, it
was chosen for three reasons: (1) the preparation of sticks
for a microtensile test did not have great success in a pilot
study, in which the major part of the sticks were lost by
debonding during cutting procedures, attributed to the
FIGURE 1. Bond strength values (MPa) according to the surface treat-
ment and storage conditions.
71
TABLE V. Number and Percentage of Failure Types After the Shear Bond Test
Failure Type

Surface Treatment Storage n A C-cer C-cem Mix

ALC (control) 24 h 12 9 (75%) 0 0 3 (25%)

90 d/TC 12 12 (100%) 0 0 0
MDP-primer 24 h 12 10 (83%) 0 0 2 (17%)
90 d/TC 12 12 (100%) 0 0 0
SiO2 þ MPS-Sil 24 h 12 3 (25%) 0 1 (8%) 8 (67%)
90 d/TC 12 12 (100%) 0 0 0
SiO2 þ MDP-primer 24 h 12 12 (100%) 0 0 0
90 d/TC 12 12 (100%) 0 0 0

A, adhesive failure; C-cem, cement cohesive failure; C-cer, ceramic cohesive failure; Mix, partially C-cem and partially A.

resistance to cutting the Y-TZP ceramic that likely produces
excessive vibration, heating, and damage to the adhesive
interface, which did not survive during cutting; (2) the low
values of resin bond strength to Y-TZP impeded the cut-
ting—this outcome may argue against microtensile test,
when testing low values of bond strength are present; (3)
in a pilot shear test, 100% of the specimens failed at the ad-
hesive interface, so the measured stresses likely addressed
the adhesive strength more closely than the cohesive
strength of the cement. Likewise, Valandro et al.20 found a
higher percentage of adhesive failures when comparing
shear to microtensile bond strength when evaluating the
bond strength between a resin cement and a high-strength
ceramic (zirconia/alumina-based ceramic). In addition, those
authors did not observe significant differences in the bond
strength results between both the tests.
Surface cleaning with isopropanol (ALC) or the applica-
tion of a MDP-based coupling agent (MDP-primer) produced
very low bond strength values after 24 h of storage. The
weak adhesion may be attributed to the poor chemical and
micromechanical bond mechanisms.6,21 All specimens in
these groups failed after the extended storage time, either
before or during thermocycling. These long-term findings of
when the Y-TZP surface was cleaned with alcohol were simi-
lar to those obtained by Özcan et al.18 Water sorption may
determine cement hydrothermal degradation during
aging.16,22,23 The weak bonding to Y-TZP demonstrated in
these groups probably facilitated water infiltration, sorption,
and degradation of the cement at the bonding interface.17
The highest values of bond strength observed in this
present study occurred when the Y-TZP was coated with sili-
con oxides (SiO2 groups) combined with either the MPS-Sil
or MDP-primer (Table IV). Tribochemical silica coating is a
type of surface treatment in which the ceramic surface is
abraded with aluminium-oxide particles modified with silica,
and the blasting pressure results in the embedding of silica
particles on the ceramic surface.5 The COJETV R system

includes this air abrasion procedure associated with the

FIGURE 2. Scanning electron micrographs for a MDP-primer/24 h
specimen: (a) adhesive-cohesive failures (Mix)—residue of cement left
in the right side of the bonding surface, near the border, in both
images.
application of a MPS-based coupling agent (MPS-Sil), which
may result in chemical bonding between the silica-coated
ceramic surface and the cement.6 The efficacy of this surface
treatment has been demonstrated in previous studies in
high-purity alumina5,24 and in zirconia ceramics5,15,25 in
which the silica coating and silanization improved the resin
bonding to ceramic. All of these studies are in agreement
with the results from the current investigation, which indi-
cated that the tribochemical approach is very helpful in
improving the resin bonding to a Y-TZP ceramic. The mecha-
nisms likely associated with this enhancement of bonding

72 MAY ET AL. SILICA COATING AND COUPLING AGENTS: EFFECT ON RESIN BOND TO Y-TZP

are the fine surface roughness, enlargement of the bonding
area,5,26–28 and the silica layer resulting on the Y-TZP sur-
face that bonds chemically to the silane agent.5,6,17,26–29 The
silane agent would then be able to bond to the resin cement
through cross-links with the methacrylate groups and
increase the ceramic surface energy, improving the wettabil-
ity to resin.17,27,30
Two different behaviors regarding the effect of the stor-
age time and TC were observed in this study. When the Y-
TZP surface was not silica coated, the cement/Y-TZP bond-
ing was not able to resist the ‘‘aging’’ conditions, resulting
in spontaneous debonding (null adhesion). However, when
the Y-TZP surface was silicated, the bond strength to the Y-
TZP ceramic was stable (SiO2 þ MPS-SIL and SiO2 þ MDP-
primer groups). The increase of bond strength perceived in
the SiO2 þ MDP-primer group over the extended storage
time is contrary to the results that have been reported by
many authors regarding the bond degradation to Y-TZP in
long-term studies.7,8,18,31 A reason for this difference could
be a residual cure in the studied cement. Pace et al.32
reported an increase in flexural strength of a dual MDP-
based cement after 1-month storage and associated this to a
possible continued polymerization. However, this hypothesis
has not been confirmed and this fact would need further
investigation. In this study, the use of a MDP-based coupling
agent after silica coating was apparently protective of the Y-
TZP/resin cement bonding. Luthy et al.33 also found a slight
but nonsignificant increase in the bond strength to a tetrag-
onal stabilized zirconia when a dual MDP-based resin
cement was used and a significant increase when a self-cur-
ing MDP-based resin cement was used.
The use of a MDP-based coupling agent after silica coat-
ing (SiO2 þ MDP-primer group) resulted in higher bond
strengths when compared to the use of MDP-based primer
without previous silica coating (MDP-primer group). This
study showed that the use of a MDP-primer alone provided
no durable bonding if silica deposition by air abrasion on
the Y-TZP surface was not made before.34 This result indi-
cates that the micro-retention pattern (micro-mechanical ad-
hesion) appears be important in maintaining long-term
bonding. When only the coupling agent was applied, weak
adhesion of the resin cement to zirconia might result, since
the linkage of Al-O-Si is hydrolyzed in oral conditions.25,28,35
When silica coating was performed, the resin cement was
able to adhere to the silica present on the ceramic surface
through the MDP-primer, producing greater and more dura-
ble bonding values. Additionally, it can be hypothesized that
the MDP-primer may have better chemical bonding to sili-
con oxides than zirconium oxides.
The use of a MDP-based coupling agent instead of a
MPS-based agent after silica coating had a better result in
terms of long-term bonding. It could be speculated to be
due to the presence of a phosphate ester group, which
bonds directly to surface oxides and to a methacrylate
group, which bonds to the resin matrix of the luting resin.36
The findings of Akgungor et al.37 and Yang et al.34 corrobo-
rate this hypothesis, that the MDP-containing coupling
agents produce high and durable bond strength.
JOURNAL OF BIOMEDICAL MATERIALS RESEARCH B: APPLIED BIOMATERIALS | OCT 2010 VOL 95B, ISSUE 1
ORIGINAL RESEARCH REPORT
The analysis of the surfaces after failure demonstrated
the predominance of adhesive failures (Table V), which vali-
dated the use of the shear test in this particular study, using
Y-TZP as a base material in the specimen design. Figure 2
illustrates adhesive and mixed types of failure that were
observed after the SBS test.
The first hypothesis of the study was rejected, since the
surface treatment influenced MDP-based resin/Y-TZP bond-
ing and the second hypothesis was accepted, since 90 days
of water storage and thermo cycling affected the bond
strength. These results provide an evidence of the possible
performance of resin to Y-TZP ceramic bonding under differ-
ent surface treatment strategies. Silica coating combined
with the use of a MDP-based coupling agent seems to be
promising. However, more information is necessary about
the consequences of silica coating upon the fracture
strength of Y-TZP ceramics, mainly over fatigue conditions,
before the indication of clinical use for this type of surface
treatment.
CONCLUSION
Silica coating followed by the use of a MDP-based coupling
agent was the best option among the alternatives tested in
this study for bonding a MDP-based resin cement to a Y-TZP
ceramic. Silica coating presented a relevant influence upon
the bond strength and bond durability.
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SILICA COATING AND COUPLING AGENTS: EFFECT ON RESIN BOND TO Y-TZP