Effect of silica coating and silanization on flexural and composite-resin

bond strengths of zirconia posts: An in vitro study

Anuar Antonio Xible, DDS, MSc,a Rudys Rodolfo de Jesus Tavarez, MS,b
Carlos dos Reis Pereira de Araujo, PhD,c and Wellington Cardoso Bonachela, PhDd
Bauru Dental School, University of Sao Paulo, Brazil
Statement of problem. The bond strength of composite resin cores to the smooth surface of prefabricated
zirconia-based ceramic posts is problematic because it might not be sufficient to ensure stability of the post-
and-core system. It is also not clear whether any alteration of the post surface to provide additional mechanical
or chemical retention would compromise flexural strength of the posts.
Purpose. This study tested the effect of a tribochemical treatment on the bond strength (BS) between zirconia-
based ceramic posts and composite resin and on the flexural strength (FS) of the posts.
Material and methods. For the BS test, 2 groups of specimens (n=10) were prepared as follows: In the
experimental (E) group, zirconia-based ceramic posts (Cosmopost), 21 mm long and 1.7 mm in diameter,
were treated with a tribochemical silica coating and silanization system (Rocatec). For the control (C) group,
zirconia-based ceramic posts were used as supplied by the manufacturer. For the 2 groups, posts were centered
and vertically positioned in a metal mold, and composite resin (Tetric Ceram) was polymerized around the posts
to form rings (6 mm diameter 3 4 mm height). All specimens were positioned in a universal testing machine,
and a load was applied axially on the protruding heads of posts in a shear push-out mode test until bond failure
(MPa). Fracture mode was assessed as cohesive, cohesive/adhesive, or adhesive. Following this, the FS of the
posts was measured in MPa using a 3-point bending test. Data were recorded and statistically analyzed using
the Student t test for both tests (a=.01).
Results. Mean fracture load values 6 SDs for the BS test were 28.1 6 2.3 MPa and 8.9 6 3.97 MPa for the
E and C groups, respectively. The mean FS values were 1544.9 6 214.1 MPa and 844.8 6 50.8 MPa for the E
and C groups, respectively. The tribochemically treated posts exhibited significantly higher values for both bond
strength to composite resin and resistance to fracture when compared to posts in the control group (P,.001).
Fracture analysis showed 100% cohesive/adhesive fractures for group E specimens and 100% adhesive fractures
for group C specimens.
Conclusions. The use of a tribochemical silica coating process and silanization on zirconia-based ceramic posts
increased both the bond strength to composite resin as well as the fracture strength of posts. (J Prosthet Dent
2006;95:224-9.)

CLINICAL IMPLICATIONS
A tribochemical treatment on the surface of the zirconia-based ceramic posts tested may be useful
for improving the bond strength with composite resin cores and enhancing post-and-core stability
without compromising the flexural strength of the posts.

D uring the last 2 decades, an increasing demand

for esthetic restorations led to the development of
several new ceramic crown systems with characteristics
similar to natural teeth, such as translucency and
fluorescence.1-5 However, their use in pulpless teeth
in conjunction with traditional post-and-core systems
may create esthetic problems. For example, light re-
flected from a metal post-and-core foundation may
This study was supported by FAPESP, Sao Paulo, Brazil, grant number
01/10245-3.
a
Graduate student, Department of Prosthodontics.
b
Graduate student, Department of Prosthodontics.
c
Professor, Department of Prosthodontics.
d
Associate Professor, Department of Prosthodontics.
make a metal-free ceramic crown appear gray and discol-
ored.2,4,6,7 To ensure a successful esthetic outcome, the
post-and-core system would need to be tooth colored,
reflecting and transmitting light in a manner similar to
a natural tooth.2,4,7,8
In recent years, nonmetal esthetic posts have become
available, made of either reinforced resins or high-
strength ceramics such as zirconia-based ceramics.2,4,6-9
Zirconia-based ceramics are composed of zirconium
dioxide, partially stabilized with yttrium oxide (ZrO2-
TZP; 3 mol% Y2O3), and exhibit a polymorphic struc-
ture with monoclinic, tetragonal, and cubic crystalline
phases. The monoclinic is the predominant phase at
room temperature and is stable up to 1170°C, when
it transforms into the tetragonal phase. Similar to

224 THE JOURNAL OF PROSTHETIC DENTISTRY VOLUME 95 NUMBER 3

XIBLE ET AL
metal transformations, a tetragonal to monoclinic trans-
formation (t / m) is also likely to occur in zirconia crys-
tals and is called a martensitic-like transformation.10
This martensitic-like transformation can be induced by
externally applied stress and is associated with a volu-
metric expansion (3% to 5%) of the crystalline struc-
ture.2,10 As a result, a propagating crack due to tensile
stress in the ceramic material will develop a correspond-
ing compressive stress at the tip of the crack, thus pre-
venting continued crack growth.10 The yttria–partially
stabilized tetragonal zirconia polycrystalline ceramics
(Y-TZP) have an elastic modulus of approximately 200
MPa, and a flexural strength (FS) of 820 MPa. These
properties are far higher than those exhibited by other
high-strength ceramics.11 External treatments such as
grinding or airborne-particle abrasion can induce an
external t / m, which, in turn, is likely to increase the
mean FS of zirconia-based ceramics.12 Severe grinding,
on the other hand, may introduce deep surface flaws that
act as stress concentrators and may decrease the mean
FS.11-13 Clinical indications for zirconia-based ceramics
include endodontic posts, implant abutments, complete
crowns, and fixed partial dentures.14
The zirconia-based ceramic posts are advocated for
use with heat-pressed glass ceramic or composite resin
as core materials.2,4,6,8 However, some authors have
suggested that the composite resin core and zirconia-
based ceramic post combination should be avoided
due to the possibility of insufficient bond strength.15-17
According to Yaman and Thorsteinsson,18 a stiffer and
more stable core material may diminish apical stress
and prevent the intrusion of a loaded post. Stability is
partially achieved by a strong link between the post
and core.19 Al-Harbi and Nathanson15 and Cohen
et al16 compared bond strength between zirconia-based
ceramic posts and composite resin with titanium posts
and composite resin and concluded that the first system
may not be clinically acceptable because of the low bond
strength values obtained. In another study, 5 types of
esthetic posts and composite resin core systems luted
to root dentin were analyzed after being subjected to
cyclic loading. The interfaces between the post-and-
core systems and root dentin were examined under scan-
ning electronic microscopy (SEM). The group with the
zirconia-based ceramic posts exhibited the highest gap
index at the post/root dentin interface. The authors
suggested that the bond strength (BS) between this
post and core might not be stable enough to resist mas-
ticatory loading and might play a direct role in its lack of
adhesion to dentin.17 Clinical reports have remarked on
the importance of post/core stability when suggesting
that it is one of the factors responsible for restoration
failures.3,5,20
Regarding the bonding mechanism between com-
posite resin and ceramics, hydrofluoric acid etching
and silanization can enhance the mechanical bond
MARCH 2006
THE JOURNAL OF PROSTHETIC DENTISTRY
strength of glass-ceramic materials to composite resin.
The acid etching partially removes the glassy matrix
and creates mechanical retentive areas where silane mol-
ecules lodge and link inorganic molecules of the ceramic
crystalline phase to organic molecules in the resinous
material.21-24 However, these techniques do not im-
prove the strength of the resin bond to high-strength ce-
ramics, such as the alumina or zirconia-based materials,
because they have little or no silica content.25-30
Some studies have shown that a tribochemical silica
coating may increase the BS between composite resin
and high-strength ceramics.26-30 Systems such as the
Rocatec system (3M ESPE; Seefeld, Germany) were in-
troduced primarily to improve the bond between metal
and composite resin. The system consists of an airborne
particle–abrasion pretreatment with Rocatec Pre pow-
der (110 mm aluminum oxide) to clean the metal sur-
face, then a silica coating with Rocatec Plus powder
(110 mm aluminum oxide, coated with silicon dioxide),
and finally, the application of silane. The silica coating
‘‘energizes’’ the substrate surface, which allows the silica
to adhere to it.26,27 Silane improves the bond between
the silica adhered to the substrate and the resin matrix.
Some authors report that a Rocatec tribochemical silica
coating provides durable resin bonds to glass-infiltrated
aluminum oxide ceramics with Bis-GMA-based com-
posite resin cements.14,26,27 An advantage of this system
is that silica-coating units are available for use in both the
dental laboratory and dental office. Other silica-coating
methods were either ineffective with alumina ceramics
or technically complicated.14
The manufacturer of a zirconia-based ceramic post
(Cosmopost; Ivoclar Vivadent, Schaan, Liechtenstein)
states that the post surfaces should not be altered in
any manner.2,9 Nevertheless, the influence of a tribo-
chemical treatment on the fracture strength or BS of
the posts with composite resin requires further investi-
gation. Thus, the purpose of this study was to evaluate
the effect of a tribochemical treatment on the BS and
mode of failure between composite resin cores and
zirconia posts and on the FS of zirconia posts.
MATERIAL AND METHODS
This study consisted of 2 parts: testing the effect
of a tribochemical treatment (Rocatec; 3M ESPE) on
the BS and mode of failure between a composite resin
core material and zirconia-based ceramic posts, and
determining the FS of zirconia-based ceramic posts.
Thirty-four cylindrical zirconia posts with tapered ends
(Cosmopost), 21 mm long and 1.7 mm in diameter,
were selected and allotted to each group for the 2 tests.
For BS testing, 20 posts were divided into 2 groups of
10 each according to surface treatment. In the experi-
mental (E) group, posts were treated with the Rocatec
system. The first step of the tribochemical treatment is
225
THE JOURNAL OF PROSTHETIC DENTISTRY
Fig. 1. Metal mold with zirconia dowel in place. (A) Zirconia
dowel; (B) primary mold; (C) secondary split mold; (D) trans-
verse pin.
commonly carried out with Rocatec-Pre (3M ESPE) to
clean the material surfaces. This step was omitted since
the post manufacturer had already performed a similar
procedure with 50-mm aluminum oxide airborne-particle
abrasion. In the second step, Rocatec Plus (3M ESPE)
airborne-particle abrasion was performed at 2.8-bar
pressure with the instrument tip held perpendicular to
the posts at a distance of 1 cm. Posts were rotated during
this procedure so that the abrasive was directed to the
entire post surface for 13 seconds on each side. The treat-
ment was confined to a 10-mm band around each post, 2
to 12 mm from the coronal end. Next, silane (Rocatec
ESPE-Sil; 3M ESPE) was applied and allowed to air
dry for 5 minutes. A metal mold was used to form com-
posite resin rings around each post (Tetric Ceram; Ivo-
clar Vivadent). For this procedure, a primary custom
metal mold was fabricated with a hole, 1.9 mm in diam-
eter in the center of the mold along its long axis, to
accommodate the posts vertically. A secondary split
mold was made to fit on top of the base mold. Placed
together, the 2 molds created a space 6 mm in diameter
and 4 mm high for forming resin rings around the coro-
nal portion of the post specimens (Fig. 1). A transverse
pin through the center of the primary mold, 13 mm
from the top surface, stabilized post positions while
composite resin rings were formed. In this way, all spec-
imens had 4 mm of post extending coronally to the
molded composite resin rings (Fig. 2). The composite
resin was inserted, following the incremental technique
described by Rueggeberg and Jordan,31 in 2 layers of
2 mm each, using a spatula (No. 9; Thompson Dental,
Missoula, Mont). The rings surrounded the posts in
the area of tribochemical treatment. Each layer was light
polymerized for 40 seconds with a light unit (Visilux; 3M
ESPE) delivering 450 mW/mm2. The tip of the light
unit was positioned vertically on top of the posts, at
the same distance from the composite resin for all speci-
mens. In the control (C) group, the posts were tested
226
XIBLE ET AL
Fig. 2. Prepared specimen. (A) Zirconia dowel; (B) composite
resin ring.
without any surface treatment. To ensure complete
cleanliness of the post surfaces, the surfaces were cleaned
with 32% phosphoric acid solution (Uni-Etch with BAC
(benzalkonium chloride); Bisco, Schaumburg, Ill) for
15 seconds. Next, they were rinsed thoroughly and
completely dried using strong air pressure for at least 5
seconds with a clean, dry-air syringe. Posts were
positioned in the same mold, and composite resin rings
were formed and polymerized following the same steps
used for group E. Specimens were removed from the
metal mold (Fig. 2), and additional light polymeriza-
tion was provided for 40 seconds on each side of the
composite resin rings with the same light-polymeriza-
tion unit. All specimens were stored in distilled water
at 37°C for 48 hours.
To test BS, the primary mold was used as a holding
device. Specimens were positioned in the mold, which
was locked in place in a universal testing machine
(Kratos P-2000; Kratos, Sao Paulo, Brazil). At this
time, the transverse mold pin was removed to allow free
vertical movement of posts in the primary mold. A load
was applied along the long axis of the specimens with
a flat-headed metal cylinder positioned on top of post
heads protruding beyond the composite resin rings. The
push-out force, applied at a crosshead speed of 0.5
mm/min, continued until bond failure occurred and
the cores separated from the posts (Fig. 3). The BS
values were recorded in MPa.
Tests for FS were next accomplished using a new set
of posts, divided into 2 groups of 7 each according to
surface treatment. Because previous pilot studies and
published data13 have shown small standard deviations
in this test using Cosmopost posts, 7 post specimens
per group were considered sufficient for FS testing.
Thus, in the E group, the Rocatec system was again
used to provide the tribochemical surface treatment as
described previously. The C group did not receive any
surface treatment. For the 3-point bending test, posts
were placed in a device with supports spaced 12 mm
apart, with the cylindrical segment centered and the
tapered portions positioned away from the supports so
that only the cylindrical portion of the posts was loaded.
Thus, for the posts in the E group, load was delivered in
VOLUME 95 NUMBER 3
XIBLE ET AL
Fig. 3. Specimen in position for testing. (A) Specimen;
(B) primary mold locked in the testing machine; (C) metal
cylinder of testing machine on top of dowel.
the area where the tribochemical treatment was per-
formed. Specimens were tested to fracture using a uni-
versal testing machine (Kratos P-2000; Kratos) at a
crosshead speed of 0.5 mm/min. The data for the BS
and FS tests were recorded and statistically analyzed
(SPSS 11 for Macintosh; SPSS Inc, Chicago, Ill) using
the Student t test. The P value was set at .01 to lower
the probability of Type I error for both tests.
An initial screening of the entire rounded post surface
was done using a stereomicroscope (SM98-90HF; Swift
Optics, San Jose, Calif) at 340 magnification. One non-
blinded operator assessed the fracture mode for the BS
test as 1 of 3 types: (1) cohesive – composite resin sur-
rounding the entire post bond area; (2) cohesive/
adhesive – evidence of composite resin adhering to any
part of the post bond surface; or (3) adhesive – no trace
of composite resin found on the post surface. Because
no specimen was assessed as the type 1 mode of failure,
3 specimens assessed either as type 2 or 3 were arbitrarily
selected for SEM and energy dispersive spectroscopy
(EDX) (XL 20; Phillips Electronics, Eindhoven,
Netherlands) analysis. One surface was selected from
each specimen and analyzed by 1 blinded operator to
confirm the assessment performed under stereomicro-
scopy investigations.
RESULTS
Composite resin to zirconia post BS values 6 SD ver-
sus surface treatment were 28.1 6 2.3 MPa and 8.9 6
3.9 MPa for the E and C groups, respectively. There
was a significant difference (P,.001) between groups,
with post surfaces treated with the tribochemical silica
coating and silanization treatment exhibiting a signifi-
cantly higher value. The FS values versus surface treat-
ment were 1544.9 6 214.1 MPa and 844.8 6 50.8
MARCH 2006
THE JOURNAL OF PROSTHETIC DENTISTRY
Fig. 4. Photomicrograph of tribochemical-treated zirconia
dowel confirming cohesive/adhesive fracture mode observed
(original magnification 333). Composite resin can be
observed on only small percentage of visible area. (A) Non-
treated ceramic surface area; (B) tribochemically treated
ceramic surface area; (C) composite resin adhered to tribo-
chemically treated ceramic surface area.
MPa for the E and C groups, respectively. A significant
difference (P,.001) was found between the 2 groups,
demonstrating a strengthening effect on the zirconia
posts by the tribochemical treatment and silane
application.
Stereomicroscopy confirmed by SEM analysis re-
vealed a significant amount of composite resin remain-
ing on the surfaces of the post specimens treated with
the tribochemical treatment and silanization, demon-
strating a 100% cohesive/adhesive fracture mode for
the core material. The total amount of residual compos-
ite resin was estimated to be between 20% and 30% of
the area of each post (Fig. 4). Conversely, there was an
absence of composite resin material on the surfaces of
the nontreated C group; thus, the mode of failure was
determined to be 100% adhesive (Fig. 5). No completely
cohesive fracture was found. The EDX analysis showed
a change of the surface post. The nontreated speci-
mens demonstrated a surface composed primarily of Zr
(56.02%w), O (27.24%w), and Y (5.45%w). Some traces
of Al (0.76%w) were also found. In comparison, post
surfaces treated with the tribochemical treatment and
silanization had less Zr (41.25%w) and Y (4.43%w),
but more Al (2.93%w) and O (38.55%w). A trace of
Si (0.78%w) was also present.
DISCUSSION
It has been shown that the design of the coronal por-
tion of a post plays an important role in the retention of
core material.9,19 The reported low BS values between
zirconia-based ceramic posts and composite resin may
be attributed to the smooth surface of the posts.15,16
Therefore, surface treatments might be tested to
227
THE JOURNAL OF PROSTHETIC DENTISTRY
Fig. 5. Photomicrograph of nontribochemically treated
zirconia dowel surface showing adhesive mode of fracture
(original magnification 325).
improve the BS. Unlike with silica-based ceramics, hydro-
fluoric acid etching followed by a silane application on
a zirconia-based ceramic surface does not enhance the
BS between them.2,6,14 Although the manufacturer of
Cosmopost does not recommend altering post sur-
faces,2,9 in this study it was found that the alteration
caused by tribochemical treatment followed by silaniza-
tion improved BS with composite resin. This may be
attributed to 2 different mechanisms. First, microscopic
irregularities created by the 110-mm aluminum oxide
silica-coated airborne-particle abrasion (Rocatec Plus;
3M ESPE) may provide mechanical retention. Madani
et al25 and Awliya et al28 showed that treatment with
airborne-particle abrasion was more effective in producing
a high BS between composite resin and a high-strength
ceramic substrate when compared with hydrofluoric
acid, grinding with a diamond rotary cutting instru-
ment, or polishing treatments. The second mechanism
relies on a special coating generated by the adhesive layer
of silica followed by the silane application. More than
airborne-particle abrasion, Rocatec Plus powder (3M
ESPE) consists of regularly shaped Al2O3 particles coated
with silicon dioxide (SiO2). By this mechanism, the SiO2 is
tribochemically transformed and is consequently able to
bond to metal alloys and high-density ceramics.26,27,30
Silane bonds chemically to the silica layer and to the sub-
sequently applied composite resin.26,27,30 In the present
study, composite resin adhered to treated post surfaces
(Fig. 4) increased the amount of incorporated Al
(2.93%w) and O (38.55%w) seen in the EDX analysis.
This suggests the effectiveness of the silica layer provided
by the silica-coated aluminum oxide airborne-particle
abrasion (Rocatec Plus); it seemingly increases the BS
values between composite resin and zirconia.
Although in this study the strength of the resin bond
to zirconia posts was enhanced with a tribochemical
treatment, it is contrary to the manufacturer’s
228
XIBLE ET AL
recommendation and raises concerns regarding the ef-
fect such a treatment may have on zirconia posts sub-
jected to masticatory loads. Fischer et al13 suggested
that the presence of flaws on post surfaces is responsible
for their tendency to fracture when stressed. As with
other ceramic materials, airborne-particle abrasion may
also cause flaws that result in strength reduction. The
FS of prefabricated zirconia-based ceramic posts has
been reported to be approximately 820 MPa. Kosmac
et al12 used a biaxial flexural test to verify the effect of
aluminum oxide airborne-particle abrasion on zirconia
discs and found an improvement in FS (1239.0 MPa)
when compared to specimens not airborne-particle
abraded (1021.0 MPa). The authors noted that the
aluminum oxide airborne-particle–abrasion process is
enough to remove a considerable amount of material
from zirconia surfaces. Furthermore, even low stresses
developed during this process may cause a transforma-
tion of surface crystals from a tetragonal (t) to a mono-
clinic (m) phase, with consequent volume expansion.
Superficial grains could readily transform and expand
under the stress caused by the impact of alumina parti-
cles. However, a grain within the material is constrained,
surrounded on all sides by other grains that act uni-
formly from all directions, in a similar fashion to hydro-
static pressure when a material is submerged in a liquid.
This hydrostatic constraint tends to inhibit phase
changes within the bulk of the material. In the present
study, the tribochemical treatment may have caused
the t / m transformation in the experimental posts
and might explain the significant improvement in FS
found in the E group. This is in agreement with Oblak
et al,9 who found an increase in FS of zirconia posts sub-
jected to airborne-particle abrasion with 110-mm alumi-
num oxide particles.
In spite of the initial improvements in BS between
composite resin and zirconia posts found in this study,
in a previous study, Wegner and Kern30 reported that
150 days of water storage can lower the tensile strength
of bonds between composite resin and Rocatec-treated
zirconia surfaces by almost one third of the initial
strength. The present study did not assess the role of
water storage in the BS test since the interface between
the composite resin core and zirconia post is not con-
sidered to be exposed to water under normal clinical
conditions.20 On the other hand, in a recent study,
Hooshmand et al24 analyzed the role of a heat treatment
following the application of silane on the BS between
composite resin and feldspathic ceramics. The authors
found that the composite-resin bond to a ceramic sur-
face, in the group that received a heat treatment after
silane application, was as good as the bond to ceramic
groups in which surface treatments included microme-
chanical retention provided by airborne-particle abra-
sion or hydrofluoric acid etching. They also found that
storage in water did not weaken BS. The authors
VOLUME 95 NUMBER 3
XIBLE ET AL
attribute this improvement in retentive values to
the elimination of silane by-products with the heat
treatment.
The role of water storage and silane on the bond
between composite resin and zirconia-based ceramics
requires further study to determine the effect of each
component of the tribochemical treatment on strength
enhancements, both BS and FS. It must be noted that
the results reported in this initial study were obtained
under static loading. However, clinically, dental restora-
tions are exposed to stresses and thermal interactions far
more complex than those incorporated in laboratory
tests. Consequently, it is logical that in vivo failures
may occur at stress levels lower than those reported in
this study.
CONCLUSIONS
Within the limitations of this study, the following
conclusions were drawn:
1. The use of a tribochemical silica coating and silaniza-
tion significantly increased (P,.001) the BS between
zirconia-based ceramic posts and composite resin
cores, and also changed the mode of failure from
adhesive to cohesive/adhesive for the 2 materials
tested.
2. There was a significant increase (P,.001) in the FS of
the tested zirconia-based ceramic posts after treat-
ment with a tribochemical silica coating and silane.
The authors thank Dr Dan Nathanson, Goldman School of Dental
Medicine, Boston University, for the support and guidance he
provided.
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Copyright Ó 2006 by The Editorial Council of The Journal of Prosthetic
Dentistry.
doi:10.1016/j.prosdent.2005.12.010
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