Dental Materials (2006) 22, 189–194

www.intl.elsevierhealth.com/journals/dema

Effect of surface treatment of titanium posts

on the tensile bond strength
Petra Schmagea, Julie Sohnb, Mutlu Özcanc,*, İbrahim Nergiza
a
Department of Operative Dentistry and Periodontology, Dental School, University of Hamburg,
Hamburg, Germany
b
Private Practice, Hamburg, Germany
c
Department of Dentistry and Dental Hygiene, Faculty of Medical Sciences,
University of Groningen, Antonius Deusinglaan 1, NL-9713 AV Groningen, The Netherlands

Received 6 January 2005; accepted 7 April 2005

KEYWORDS Summary Objectives. Retention of composite resins to metal can be improved

Luting cements; when metal surfaces are conditioned. The purpose of this investigation was to
Root post; investigate the effect of two conditioning treatments on the tensile bond
Silanization; strength of four resin-based luting cements and zinc phosphate cement to
Silica coating; titanium posts.
Zinc phosphate Methods. The effect on tensile bond strength of (1) air-particle abrasion (50 mm
cement Al2O3) and (2) silica coating (30 mm SiOx) and silanization of tapered titanium posts
prior to luting with any of the four resin composite luting cements (Compolutew
Aplicap, Flexi-Flow cemTM, Panaviaw 21 EX, Twinlook) were evaluated. The posts
luted with zinc phosphate cement (Tenet) were considered as the control group.
Following endodontic preparation of 100 intact anterior human teeth with hand
instruments, the post spaces were prepared using the opening drills of the
corresponding size of the posts. All posts were cemented into the roots according
to the manufacturer’s instructions of each cement. The specimens were first stored
in water at 37 8C for 24 h and then subjected to thermocycling (5000 cycles, 5–55 8C,
30 s). The tensile strength values were measured on a universal testing machine at a
cross-head speed of 0.5 mm/min. Data were analyzed statistically using ANOVA and
corrected with Scheffé-test due to the significance levels (P!0.05).
Results and Significance. The composite resin luting cements did not show
significant differences (P!0.05) showing values between (352G76 N–475G104 N)
when the posts were air-abraded. After silica coating and silanization, significantly
higher (P!0.05) tensile strengths were obtained for Compolute w Aplicap
(600G123 N) than those of the other luting cements (Flexi-Flow cemTM:
191G62 N; Panaviaw 21 EX: 375G77; Twinlook: 430G78 N). No significant
differences (PO0.05) were found between the tensile strength of the posts luted
with zinc phosphate (414G102 N) and the resin composite cements. Silica coating

* Corresponding author. Tel.: C31 50 363 8528; fax: C31 50 363 2696.
E-mail address: mutluozcan@hotmail.com (M. Özcan).

0109-5641/$ - see front matter Q 2005 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.
doi:10.1016/j.dental.2005.04.015
190 P. Schmage et al.

and silanization revealed the highest tensile bond strength in posts luted with
Compolutew Aplicap but it was not effective for the other experimental groups. Zinc
phosphate cement exhibited tensile bond strength as good as resin composite
cements.
Q 2005 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Introduction in endodontic applications. Therefore the

objectives of this in vitro study were to compare
The use of passive tapered posts is often advised in the tensile strength of passive tapered titanium
order to avoid root fracture [1,2]. However, their posts luted after either air-particle abrasion with
retention to the root canals was reported to be less alumina particles as received from the
when compared with active posts or passive parallel manufacturer or silica coating followed by
posts. Therefore it is necessary to improve the silanization using four resin composite luting
retention when this kind of post is of choice [3,4]. cements and further to compare the results with
The anchorage obtained from post systems depends zinc phosphate cement.
on various factors but the common requirement
from all post systems is maximum retention against
tensile forces [5–8]. Materials and methods
The use of resin composite luting cements has
been reported to reveal superior post retention, Passive tapered titanium posts (Erlangen Post
less solubility and microleakage compared to zinc System, Brasseler USA, Savannah) with sandblasted
phosphate cements [3,9–19]. The higher retention surfaces (RZZ12.4 mm) of size II with 12 mm length
strengths are due to the bonding capacity of resin and 0.9 mm base diameter were used for the
composite to dentin walls in the root canal through experiments. A total of 100 newly extracted intact
chemical adhesion. However, resin composite human anterior teeth were stored in physiological
cements differ in chemistry and therefore they saline solution before use. The clinical crowns were
are reported to exhibit different performances with removed perpendicular to the long axis of the
regard to the retentive strength [10–13,17]. root by a band saw (Exact band system, Norder-
Earlier studies have shown that the retentive stedt, Germany). The root canals were
qualities of passive posts luted with zinc phos- endodontically prepared up to the ISO-file sizes of
phate cement could be mechanically increased by 045, 080, and 100, respectively to one size smaller
air-abrading the surface of the post [12,19,20]. In than the respective post space preparation
addition to air-borne particle abrasion, a new air- instrument. The post spaces were prepared using
abrasion technique based on tribochemical silica
coating has been introduced in different
applications in dentistry [21–26]. Silica coating
provides ultrafine mechanical retention by air-
abrasion, as well as chemicophysical bonding
between composite resin and the alloy using a
silane-coupling agent. In this technique, the
surfaces are air-abraded with 30 mm grain size
silica. The blasting pressure results in embedding
of silica particles on the surface rendering the
surface chemically more reactive to resin via
silane. Monomeric ends of the silane molecules
react with the methacrylate groups of the
adhesive resins by free radical polymerization
process [27–29].
Although the literature contains some reports on
the use of chemical conditioning techniques on
various alloys (see review Özcan et al., 1998) [30],
to the authors’ knowledge this method has not been Figure 1 The preparation drills of the Erlangen Post
investigated for conditioning titanium post surfaces System.
Retention of posts after conditioning root canals
Table 1 Nine experimental groups, for five cement
types and two surface conditioning systems.
Conditioning Luting cements Number of
methods samples
Air particle Compolutew 10
abrasionC Flexi-Flow ceme 10
silanization Panaviaw 21 EX 10
Twinlookw cement 10
Silica coatingC Compolutew 10
silanization Flexi-Flow ceme 10
Panaviaw 21 EX 10
Twinlookw cement 10
Tenet 10
the corresponding opening drills and the diamond
roughening instrument of the post system (Fig. 1).
The post spaces were then irrigated with 1.5%
sodium hypochlorite intensively and dried with
paper points (Roeko, Langenau, Germany).
Nine experimental groups, each containing ten
roots, were formed for five cement types and two
surface conditioning systems (Table 1). The effect
of two conditioning methods, namely (1) air-
particle abrasion (50 mm Al2O3), (2) silica coating
(30 mm SiOx)Csilanization, on the tensile bond
strength of tapered passive titanium posts were
evaluated after cementing the posts with four
resin composite luting cements [Compolutew Apli-
cap (3M ESPE, Seefeld, Germany), Flexi-Flow
ceme (EDS, South Hackensack, NJ, USA), Pana-
viaw EX 21 (J. Morita, Osaka, Japan), Twinlook
(Heraeus Kulzer, Dormagen, Germany)]. The posts
luted with zinc phosphate cement (Tenet Vivadent
Inc, Amherst, NY,USA) were considered as the
control group.
In the first group, the posts with air-abraded
surfaces, as received from the manufacturer,
were cemented without additional conditioning.
The second method was tribochemical silica
coating in which the specimens were conditioned
using the intraoral air abrasion device (Dento–
PrepTM, RØNVIG A/S, Daugaard, Denmark) at a
pressure of 2.5 bar from a distance of approxi-
mately 10 mm, for about 13 s with 30 mm SiOx
(CoJetw-Sand, 3 M ESPE, Seefeld, Germany) while
rotating the post manually until its surface
appeared grey under visual inspection by the
naked eye. Following this, silane coupling-agent
(ESPE-Sil, 3M ESPE, Seefeld, Germany) was applied
and allowed to evaporate for 5 min.
The conditioned posts in each group were
randomly assigned to be luted with one of the
following cements according to each manufac-
turer’s recommendations.
191
Compolutew Aplicap
The root canal was etched for 20 s using 37%
phosphoric acid, rinsed thoroughly and air-dried.
EBSw-multi Primer (3 M ESPE, Seefeld, Germany)
and EBSw-multi Bond (3M ESPE, Seefeld, Germany)
were rubbed into the canal for 20 s, respectively
and gently air-dried. The cement capsule was
activated for 2 s and mixed automatically in a
high-speed triturator (Rotomix, 3M ESPE, Seefeld,
Germany) for 10 s. This resin composite cement was
self-curing that set in 5 min.
Flexi-Flow ceme
This self-curing bis-GMA based cement was rec-
ommended to be used without any etching and
bonding agent application. Catalyst and base in
equal amounts were mixed manually on a treated
paper pad for 30 s. The cement was allowed to set
for 4 min.
Panaviaw 21 EX
The ED Primer (J. Morita, Osaka, Japan) was mixed
from liquid A and B and applied to the canal wall for
60 s and then dried with paper points. The catalyst
and base paste were mixed manually for 30 s. After
seating the post in the root canal, the cement was
protected from oxygen dispersion with OXYGUARD
II (J. Morita, Osaka, Japan) for 3 min and allowed to
polymerize for 4 min.
Twinlookw cement
The canal was first etched for 20 s using 37%
phosphoric acid, rinsed and dried thoroughly.
Adhesive bond II (Heraeus Kulzer, Dormagen,
Germany) was then rubbed into the canal, gently
air-thinned and light-polymerized for 20 s. Catalyst
and base paste were then mixed manually. This
dual-cured composite cement was light-polymer-
ized for 40 s from two directions. The irradiation
distance between the exit window and the resin
surface was maintained as close as possible to
obtain adequate polymerization and it showed
complete set through color change.
Tenetw
The cement was always mixed by the same
investigator on a cooled (6 8C) glass mixing slab at
constant room temperature of 20 8C, according to
the manufacturer’s directions. Powder was added
to the liquid in small increments and mixed
192
Figure 2 Tensile strength of the posts cemented with four resin composite cements after conditioning the post
surfaces where zinc phosphate cement was considered as a control group (**P!0.01, *** P!0.001).
thoroughly by using the majority of the mixing slab
to arrive at a creamy consistency where a small
portion of the mix did not drop from the spatula.
The post surfaces were lightly coated with the
cement before seating into the prepared post
spaces. Any surplus cement was then removed
with hand instruments and cotton pellets. The
cement was set after 10 min.
The specimens were first stored in water for 24 h
at 37 8C and then subjected to thermocycling for
5000 cycles between 5 and 55 8C. They were then
mounted in the jig of the universal testing machine
(Lloyd LRX, Lloyd Instruments Ltd, Fareham, UK)
and tensile force at a crosshead speed of
0.5 mm/min was applied to the posts until they
were debonded from the root canals.
The data were analyzed statistically using ANOVA
test and corrected with Scheffé-test due to the
significance levels (P!0.05) (SPSS-Version 7.0.
StatView 5.0, SAS Institute Inc., Cary, NC).
Results
The composite luting cements did not show
significant differences (P!0.05) when they were
only air-abraded showing values between
(352G76 N–475G104 N). After silica coating and
silanization, significantly higher (P!0.05) tensile
strengths were obtained for Compolutew Aplicap
(6002G123 N) than those of the other composite
resin luting cements (Flexi-Flow ceme:
P. Schmage et al.
1912G62 N; Panaviaw EX 21: 3752G77 N; Twinlook:
430G782 N). This value was also significantly higher
than that of the zinc phosphate group (414G102 N).
Significantly lower tensile bond strength values
were obtained for Flexi-Flow ceme (1912G62)
after silica coating when compared with the air-
particle abraded group (475G104 N) (Fig. 2).
Except for Compolutew Aplicap, silica coating
and silanization did not increase the tensile bond
strength of titanium posts but this group revealed
the highest values among all experimental groups.
No significant differences (PO0.05) were found
between the tensile strength of the posts luted with
zinc phosphate (4142G102 N) and the resin compo-
site cements under the conditions of this study.
Discussion
The retention of an adhesively cemented post
relies on the adhesion of the cement both to the
post surface, to the root canal walls and to the
bonding agent if one is used. It is therefore
important to find a reliable luting method that
provides an ideal bond between the root canal-
luting cement and the post in order to improve
the survival rate of the posts. Although there are
not so many reports on the adhesively cemented
posts, failure was reported to occur clinically at
the metal/resin interface [31].
Numerous methods have been introduced for
conditioning the alloy surfaces however they all
Retention of posts after conditioning root canals
work differently on various alloys [30]. From those
methods electroetching has been suggested widely
but it was not effective on titanium and noble alloys
[12,32]. For this reason, in this study air-particle
abrasion with Al2O3 or silica coating in combination
with silanization was employed. From the two
conditioning methods tested, the group air-abraded
with alumina particles showed no favorable results
in all cement groups when compared with the
golden standard zinc phosphate cement. Thin and
homogeneous cement with thin film thickness is of
great importance for a passive fit providing
remarkable increase in retentive strength. Most
probably, sufficient tensile bond strength values
were obtained with the zinc phosphate cement
since the rough surface offered mechanical reten-
tive interlockings into which the cement flows and
then sets. Tribochemical silica coating is based on
chemical adhesion between the glass fillers of the
luting composite and the silanized surfaces of
the post. Since the silica layer is attached well
to the titanium, this provides a basis for silanes to
enhance the resin bond. Particular increases in
strength were observed for Compolutew Aplicap.
Similar findings were obtained in previous studies
with highly filled composites [29,33–35]. One might
expect the same phenomena on the post surface
after air-abrasion with Al2O3. However surface
roughening alone evidently did not provide
additional adhesion of the resin-based luting
cements after this conditioning.
Silica coated posts luted with Compolutew
Aplicap had higher tensile strengths than all other
resin composites and zinc phosphate cement.
However, silica coating produced no increase in
the group cemented using Twinlookw. The results
could be attributed to the differences in the filler
content of these two cements or the voids
incorporated during handling because Twinlookw
and Flexi-Flow ceme were manually mixed
cements. Silica coating was not effective with
Panaviaw 21 EX, although it is a resin composite
luting cement containing phosphate monomer
(MDP) and is reported to offer good bonding ability
to all substrates and especially to titanium [13–15,
17,36]. Although Wegner and Kern [37] reported
better long-term results with MDP containing
cements than using the tribochemical silica coating
procedure, Özcan et al. [38,39] did not observe
significant differences between MDP and Bis-GMA
containing resin cements when tribochemical silica
coating was employed. The question still needs to
be addressed in future studies whether the luting
cement alone and/or the combination with the
conditioning method play the crucial role in the
adhesion to the alloy surfaces.
193
In clinical conditions, the post and core
restorations are not only subjected to tensile
stresses but also to compressive, shear, trauma or
fatigue forces and even to torsional or rotational
forces produced by functional tooth contacts. Thus,
further studies are required to test the adhesion of
surface treated posts in combination with adhesive
cements at various testing conditions.
Conclusions
1. Air-particle abrasion of the post surface with
alumina particles did not improve the tensile
bond strengths of the titanium posts luted with
resin composite cements but did improve those
luted with zinc phosphate cement.
2. Silica coating and silanization revealed the
highest tensile bond strengths in posts luted
with Compolute w Aplicap but it was not
effective for the other experimental groups.
3. Zinc phosphate cement exhibited tensile bond
strengths as good as resin composite cements.
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