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The Effect of Surface Treatment

on the Shear Bond Strength of
Mutlu Özcan, Dr Med Denta
Luting Cement to a Glass- Hasan N. Alkumru, PhDb
Infiltrated Alumina Ceramic Deniz Gemalmaz, PhDc

Purpose: The aim of this study was to evaluate the effect of three different surface
treatments on the bond strength of four different luting cements—three bis-GMA–based
resin cements and a compomer cement—to In-Ceram. Materials and Methods: Eight In-
Ceram samples were used for each experimental group. The samples were randomly
assigned three treatment conditions: (1) etching for 90 seconds with 5% hydrofluoric acid
gel, (2) sandblasting (110-µm Al2O3), and (3) tribochemical silica coating. All samples
were silanated following the surface treatment. The luting cements were bonded to In-
Ceram specimens using Teflon tubes. All samples were thermocycled for 5,000 cycles
altering between 5 and 55°C with 30-second dwell times. The shear bond strength values
were measured in a universal testing machine with a cross-head speed of 1 mm/min.
Analysis of variance was used to analyze data. Results: The mean bond strengths varied
between 1.2 and 24.7 MPa. Conclusion: Shear bond strength of compomer cement
following tribochemical silica coating was significantly lower in comparison to resin
cements. Luting of In-Ceram with various resins provided varying degrees of bond
strengths that were significantly increased by the tribochemical silica-coating system.
Int J Prosthodont 2001;14:335–339.

M anufacturing dental crowns and fixed partial den-

tures (FPD) of porcelain fused to metal has been
widely used for about 40 years. However, conventional
metal-ceramic restorations still lack the translucency
of natural teeth. All-ceramic restorations have been in-
troduced to improve esthetics and to address concerns
regarding the use of specific intraoral base metals. An
all-ceramic system should provide ceramic restora-
tions, and possibly FPDs, with sufficient mechanical
strength to resist occlusal forces and excellent esthet-
ics and suitable biologic properties. The Vita In-Ceram
aAssistant Professor and Lecturer, Department of Prosthodontics,
·
Faculty of Dentistry, Marmara University, I stanbul, Turkey.
bProfessor and Lecturer, Department of Prosthodontics, Faculty of
·
Dentistry, Marmara University, I stanbul, Turkey.
cAssociate Professor and Lecturer, Department of Prosthodontics,
·
Faculty of Dentistry, Marmara University, I stanbul, Turkey.
Reprint requests: Dr Mutlu Özcan, Hacı Emin Efendi Sok,
· determining the mode of clinical failure observed
No. 10 D:4 Akay Apt, 80200 Nişantaşı Istanbul, Turkey. Fax:
+ 90 212 2328682. e-mail: mutluozcan@hotmail.com
ceramic system has shown greater flexural strength
than other ceramic or glass materials.1,2 Because of its
high strength, this ceramic has been suggested as the
all-ceramic system to be used for a three-unit anterior
FPD and also for resin-bonded FPDs.3,4 The clinical ap-
plication of a resin-bonded FPD requires a strong and
a stable resin bond to the ceramic. A stable bond to the
ceramic is also advantageous for other clinical appli-
cations such as inlays or crowns.
All-ceramic restorations luted with conventional
luting cements were reported to have poorer success
rates than crowns cemented and bonded with com-
posite resin cements.5–7 Previous investigations re-
vealed that most clinical failures initiate from the ce-
mentation or internal surface.8,9 This clinical result is
consistent with the discussed fracture-surface obser-
vations. In a finite element study,10 the effect of in-
ternal surface flows and cement voids in raising in-
ternal stresses was shown; this could be critical in
for glass-ceramic crowns. The failures originated from

Volume 14, Number 4, 2001 335 The International Journal of Prosthodontics

 Bond Strength of Luting Cement to Alumina Ceramic Özcan et al

Table 1 Materials Tested

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Luting agent Adhesive materials

(batch No.) (batch No.) Manufacturer

Panavia 21 (41172) Clearfil Liner Bond (41205) Kuraray

Clearfil Porcelain Bond (0060)
Variolink high viscosity Heliobond (560089) Vivadent
(911373) Monobond S (902340)
Sonocem (102 37409) Pertac Universal Bond (09842466) ESPE
Espe-Sil
Dyract Cem (P: 9609039 Prime & Bond 2 (950311) Dentsply/DeTrey
L: 9609009) Ceraprime (9603202)

cementation surfaces identified on the internal sur-
faces as the location of highest tensile stresses and/or
critical flaws; this is therefore the surface that needs
to be strengthened.
Etching silica-based ceramics with hydrofluoric
acid, ammonium bifluoride, or acidulated phosphate
fluoride gel creates a sufficient resin bond that is en-
hanced with a silane coating of the etched ceram-
ics.11–16 Etching and polymer coating of the surfaces
has also been shown to substantially improve the
strength of ceramic structures.17,18 This strengthening
effect may be caused by the elimination, blunting, or
bridging of cracks, or coatings may act to reduce the
ability of water to be transported to the crack tip,
which lessens the stress corrosion. However, neither
etching with these solutions nor adding silane results
in an adequate resin bond to the alumina-based In-
Ceram ceramic.19 An alternative roughening method
that relies on incorporation of plastic chips on the In-
Ceram core surface was also developed. However, it
was also reported not to enhance the bond strength
of the In-Ceram material.20 Therefore, an alternative
method of bonding to In-Ceram is needed.
The aim of this study was to evaluate the effect of
three different surface treatments on the bond strength
of In-Ceram ceramic to four different luting cements:
three bis-GMA–based resin luting agents and a com-
pomer cement.
Materials and Methods
Codes, batch numbers, and manufacturers of the ma-
terials tested are listed in Table 1. In-Ceram disks 2
mm thick and 16 mm in diameter were fabricated
with the slicker method according to the manufac-
turer’s recommendations. Eight samples were used for
each experimental group, and 12 experimental
groups consisting of eight specimens per group
yielded a total of 96 samples. Before initiating the
bonding procedure, the samples were embedded in
acrylic resin blocks, ensuring that one surface of the
disk remained uncovered for bonding procedures.
The exposed surface of each sample was ground
with 1,200-grit silicon carbide abrasive.
The samples were cleaned for 10 minutes in an ul-
trasonic bath (Bransonic Ultrasonic Cleaner) con-
taining ethylacetate, and 32 samples were randomly
assigned to each of three treatment conditions: (1)
etching for 90 seconds with 5% hydrofluoric acid gel
(IPS Ceramic etching gel, Vivadent), (2) sandblasting
for 14 seconds with alumina powder (Rocatec-Pre,
ESPE; mean particle size 110 µm) at 2.5 bars at a dis-
tance of 10 mm, and (3) tribochemical silica coating
(Rocatector, ESPE).
Upon completion of the surface-treatment proce-
dures, 32 samples of each group were divided into
four equal subgroups, each consisting of eight sam-
ples bonded with three different resin-based com-
posite luting cements (Panavia, Variolink, Sonocem)
and a compomer luting cement (Dyract Cem).
Bonding Procedure
Teflon (DuPont) tubes with an inner diameter of 5 mm
and height of 5 mm were filled with the luting cement.
The silane primer and bonding agents of each luting
cement recommended for each product were then
applied according to the manufacturers’ recommen-
dations to the ceramic surface, and the tubes were
bonded with the specified luting composite resin to
the ceramic surface with an alignment apparatus.
The apparatus consisted of parallel guides, the tube
holder, a silicone pad, and an added weight of 750
g. The apparatus ensured that the tube was perpen-
dicular to the sample surface. Excess resin was re-
moved from the bonding margin by the use of cotton
pellets, and an oxygen-blocking gel recommended for
each system was then applied according to the man-
ufacturer’s recommendations.
The samples were stored in distilled water at 37°C
for 24 hours and thermocycled between 5 and 55°C
for 5,000 cycles with 30-second dwell times. The
shear bond values were measured in a universal test-
ing machine (Zwick) with a cross-head speed of 1

The International Journal of Prosthodontics 336 Volume 14, Number 4, 2001

 Özcan et al Bond Strength of Luting Cement to Alumina Ceramic

Table 2 Bond Strength of Luting Agent to In-Ceram with Various Surface

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Treatments (MPa)*

Panavia 21 Dyract Cem Variolink Sonocem

Mean SD Mean SD Mean SD Mean SD

Acid etching 5.5 0.7 3.4 0.8 1.2a 1.1 1.4a 0.8
Sandblasting 12.9 2.0 10.2 0.7 0.9a 1.5 1.9a 1.3
Silica coating b
21.54 1.4 13.9 1.2 24.7b 4.2 21.5b 3.9
*The same superscripted letter indicates no significant differences between the material–surface treatment
combinations (P > .01). All groups not noted with superscripted letters showed significant differences.
SD = standard deviation.

Fig 1 SEM view of cohesive failure of Panavia 21 (p) at sand-

blasted In-Ceram (i) samples (original magnification  23.8).

Fig 2 (above right) Typical cohesive failure at In-Ceram (i) sur-

face luted with Panavia 21 (p) after application of Rocatec.
Large islands of composite remnants are observed (original
magnification  24).

Fig 3 (right) SEM view of a cohesive failure in Variolink (v) at

In-Ceram (i) surface treated with Rocatec (original magnification
 22).

mm/min. The blade started to shear 2 mm above lut-
ing resin on the In-Ceram sample. The force at which
the bond failed was recorded, and the bond strength
was calculated in MPa. The site of bond failure and
the surface morphology of the debonded specimens
were examined in a scanning electron microscope
(SEM) with an acceleration voltage of 12 kV.
The recorded shear bond strength values were an-
alyzed statistically using analysis of variance (ANOVA),
and the statistical differences were calculated using
Newman-Keuls test at significance levels of P < .01.
Results
ANOVA showed significant differences in bond
strength among the means with different luting agents
and surface treatments (Table 2). The highest values
were obtained with tribochemical silica coating.
Sandblasting gave higher values than acid etching for
Panavia and Dyract Cem, whereas there were no
differences for Variolink and Sonocem. Figures 1 to
3 show SEMs of debonded specimens with different
surface treatments. Larger islands of composite resin
could be observed after debonding in the sample
surfaces treated with silica coating than with the
other treatments.
Overall, tribochemical silica coating produced the
highest bond strengths for all four luting cements, fol-
lowed by sandblasting and hydrofluoric acid etching.
The differences in bond strength recorded for Variolink,
Sonocem, and Panavia 21 by tribochemical silica-
coated samples were not statistically significant,

Volume 14, Number 4, 2001 337 The International Journal of Prosthodontics

 Bond Strength of Luting Cement to Alumina Ceramic
whereas the bond strength of Dyract Cem by tribo-
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chemical silica coating was significantly lower than the
others (P < .01; Table 2).
Discussion
The effect of acid etching and sandblasting on the
bond strength of luting cement to In-Ceram was not in
compliance with the results of the previous studies
performed on feldspathic porcelains. It has been pre-
viously reported that the bond strength of feldspathic
porcelain is greater when etched than when sand-
blasted.15,21,22 The differences in bond strength can be
explained on the basis of differences in morphology be-
tween etched and sandblasted samples. Hydrofluoric
acid dissolves either the glassy or crystalline compo-
nents of the ceramic depending on the acid concen-
tration and the composition of the material etched.
The use of hydrofluoric acid produced microundercuts,
whereas sandblasting formed a rougher surface that did
not contain a large number of undercuts.
The results of this study showed that acid etching
did not improve bond strength. Hydrofluoric acid
etching did not create a microretentive surface on In-
Ceram because of its high alumina content, and it was
almost ineffective for etching of the glass phase for mi-
cromechanical bonding. Moreover, treatment of the
surface by sandblasting produced a micromechanical
roughening. In a previous study, it was shown that In-
Ceram could be etched with boiling sulfuric acid.19
However, all of the etched samples were found to
have debonded after 150 days of storage in isotonic
saliva solution because of a weakened bond to the su-
perficial alumina particles as a result of etching.22
Therefore, the development of alternative methods of
bonding to In-Ceram was needed.23 The results of this
study showed that the bond increased greatly by the
use of tribochemical silica coating. Silica coating of
In-Ceram with the Rocatec system increased the sil-
ica content effectively and provided a basis for silanes
to enhance the resin bond.24
Evaluation of fractured surfaces on SEM revealed
the presence of small remnants of luting cements on
acid-etched and sandblasted samples, whereas in
samples treated with Rocatec, in agreement with
high retention values, greater surfaces of attached
composite were observed (Figs 1 to 3).
Apart from varying bond strengths with different
surface treatments, differences in bond strengths were
also observed with different luting cements. This may
be dependent on both composition differences of
silane primers and luting cements.
The composite resins absorb water to a certain
point. During water storage, the resin composites
absorb water, which is a time-dependent event and
The International Journal of Prosthodontics
Özcan et al
takes days or weeks to reach culmination. In the pre-
sent study, the samples were subjected to shear test
after 5,000 thermocycles according to ISO amend-
ment 10477.25
Shear bond strength of Dyract Cem following tri-
bochemical silica coating was significantly lower in
comparison to resin cements. It is probable that lower
bond strength occurred because of the lower resin
content of Dyract Cem, which enabled formation of
fewer polysiloxane bonds. The lower bond strength
of Dyract Cem can also be attributed to the lower
flexural strength of the material that causes early
fracture of the mechanically locked sections from mi-
cromechanical undercuts.26
The values found for resin luting cements in com-
bination with tribochemical silica coating are in ac-
cordance with the results of previous studies. In a few
studies27,28 performed on In-Ceram, relevant values
of bond strength were reported. The small variations
in measurements may be a result of small variations
in methodology. It can be stated that by using resin
cements in combination with the Rocatec system,
shear bond strength values higher than 20 MPa can
be achieved for In-Ceram. In two earlier studies28,29
that questioned the optimum bond strength necessary
for a successful restoration, it was shown that the fail-
ure pattern changes from cohesive failures in porce-
lain to adhesive failures between the composite resin
and porcelain when bond strength is 13 MPa.
However, the bond strength of composite resin to
porcelain required for clinically successful perfor-
mance still remains to be determined.
Conclusions
Within the limitations of this in vitro study:
1. Luting of In-Ceram with various resins provided
varying degrees of bond strengths that were sig-
nificantly (P < .01) increased by the tribochem-
ical silica-coating system in comparison to acid
etching or sandblasting.
2. Shear bond strength of compomer cement fol-
lowing tribochemical silica coating was signifi-
cantly lower (P < .01) in comparison to resin ce-
ments.
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Literature Abstract

Histologic evaluation of the bone integration of TiO2 blasted and turned

titanium microimplants in humans.

The purpose of this study was to evaluate the human bone tissue response to two surfaces
available on commercial implants. Twenty-seven patients received two microimplants each
during implant surgery. The test implants were grit blasted with TiO2 particles, and the turned
implants served as controls. After the healing period, the microimplants and surrounding tissue
were removed with a trephine burr. A three-dimensional profilometer was used to characterize
the surface roughness of the implants and histomorphometry to calculate the mineralized
bone-implant contact and the amount of bone area within the threads. The results demon-
strated significantly more bone in contact with the TiO2-blasted implants than with the turned
ones and significantly more bone inside the threaded area for the blasted implants in the
mandible.

Ivanoff C-J, Hallgren C, Widmark C, Sennerby L, Wennerberg A. Clin Oral Implants Res 2001;12:128–134.
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pital, S-431 80 Mölndal, Sweden—A. Mohei, Institute for Postgraduate Dental Education, Jönköping, Sweden

Volume 14, Number 4, 2001 339 The International Journal of Prosthodontics