Effects of Silane Application on Luting Fiber Posts

Using Self-adhesive Resin Cement

Ariene Arcas Lemea / André Luis Pinhob / Luciano de Souza Gonçalvesc /
Lorenço Correr-Sobrinhod / Mario Alexandre Coelho Sinhoretie

Purpose: To evaluate the effects of different glass-fiber post surface treatments on the bond strength to root
dentin.
Materials and Methods: Fifty bovine incisors were used in this study. After removing the crowns, the teeth were
endodontically treated. The roots were randomly divided into five groups according to post surface treatment.
The groups were as follows: CO (Control) – no treatment; G1 – RelyX Ceramic Primer (silane) only; G2 – silane
and Solobond M; G3 – silane and Scotchbond Adhesive; G4 – silane and Excite. For post cementation, RelyX
Unicem was used according to the manufacturer’s recommendation and the roots were stored in a light-proof
container with 100% relative humidity for 24 h. The specimens were transversally sectioned. Subsequently, the
cervical, middle, and apical regions of the root were positioned in a push-out device and tested at 0.5 mm/min
using a universal testing machine (Instron). The data were statistically analyzed with two-way ANOVA and Tukey’s
post-hoc test. The fractured specimens were then observed under a stereoscopic loupe at 60X magnification.
Results: No significant difference in bond strength was found among the groups that received a silane or silane
plus an adhesive system (p > 0.05). However, the CO (no silane) showed the lowest bond strength. Regarding
G1, G2, G3, and G4, the cervical region of the root canal attained better bond strengths than did the middle or
apical regions. The most frequent failure mode occurred at the cement/dentin interface.
Conclusion: Silane application may be necessary to improve the adhesion of fiber posts luted with the self-adhe-
sive resin cement evaluated here. The application of an adhesive layer between the fiber post and resin cement
did not have any influence on the bond strength when the silane coupling was previously used.
Keywords: bond strength, fiber post, push-out, resin cements.

J Adhes Dent 2013; 15: 269–274. Submitted for publication: 04.08.11; accepted for publication: 08.06.12
doi: 10.3290/j.jad.a28881

F iber posts are becoming increasingly popular in den-

tal practice for several reasons. They have a modulus
of elasticity closer to dentin than to ceramic or metal
posts and cores.26 In addition, they can be luted with
a PhD Student, Department of Restorative Dentistry, Dental Materials, Pi-
racicaba Dental School, University of Campinas, Piracicaba, SP, Brazil. Idea,
hypothesis, experimental design, performed experiments, wrote manuscript.
b Dentist, Department of Restorative Dentistry, Dental Materials, Piracicaba
Dental School, University of Campinas, Piracicaba, SP, Brazil. Performed
experiments in partial fulfillment of requirements for a degree.
c Professor, Biomaterials Division, Uberaba Dental School, University of Uber-
aba, Uberaba, SP, Brazil. Idea, hypothesis, experimental design, contributed
substantially to discussion.
d
Professor, Department of Dental Materials, Piracicaba Dental School, Univer-
sity of Campinas, Piracicaba, SP, Brazil. Idea, proofread manuscript.
e Professor, Department of Restorative Dentistry, Piracicaba Dental School,
University of Campinas, Piracicaba, SP, Brazil. Idea, hypothesis, experimen-
tal design, performed statistical evaluation, proofread manuscript.
Correspondence: Ariene Arcas Leme, Department of Restorative Dentistry,
Dental Materials, Piracicaba Dental School, State University of Campinas-UNI-
CAMP, Limeira Av. 901, PO Box 52, Piracicaba, São Paulo; Brazil 13414-903.
Tel: +55-19-9769-5653. e-mail: arienearcasleme@gmail.com
adhesive systems associated with resin cements, which
enables a more homogeneous stress distribution in
the root.1 Furthermore, with the use of fiber posts, a
lower number of catastrophic root fractures have been
found.4,29
Because the epoxy resin surrounding fibers has a high
cross-linking density, the bond to a methacrylate-based
resin is not possible or nearly nonexistant.20 This is based
on the fact that bis-GMA- (bis-phenol-A diglycidyl dimeth-
acrylate) and TEG-DMA-based (triethylene glycol dimeth-
acrylate) resins are incapable of penetrating into the sur-
face of prefabricated fiber posts, so the phenomenon
of interdiffusion cannot occur.20 However, even with few
quartz or glass fibers exposed at the fiber-post surface,23
the silanization procedure has been described as an im-
portant pretreatment to increase the bond strength to
resin cements. Silanes have a dual reactivity, because the
organic functional part (vinyl, allyl, amino, and isocyanato)
can polymerize with an organic matrix, while the alkoxy
groups (methoxy and ethoxy) reacts with an inorganic sub-
strate.21 Thus, this procedure has been recommended as
a pre-treatment for the fiber-post surface.

Vol 15, No 3, 2013 269

Leme et al
Table 1 Manufacturer, lot, and compositions of resin cement and adhesive systems used
Material Manufacturer/Lot
RelyX Unicem 3M ESPE; St Paul, MN, USA /
338573
RelyX Ceramic Primer 3M ESPE / 6XK
Solobond M VOCO; Cuxhaven, Germany /
640977
Excite Ivoclar Vivadent; Schaan,
Liechtenstein / L11777
Adper Scotchbond Multi 3M ESPE / 5PJ
Purpose Adhesive
Bis-GMA: bis-phenol-A diglycidyl dimethacrylate; HEMA: hydroxyethyl methacrylate.
The possibility that silane coupling agents may be
weakened due to hydrolysis has been suggested.2,16,22,27
Therefore, the application of a hydrophobic unfilled resin
layer (ie, a bond layer utilizing a three step total-etch
and two step self-etch adhesive systems) has been pro-
posed to promote increased wetting of the substrate16
and to protect the silane layer.12 This layer system might
strengthen the silane-based bonding interphase. How-
ever, the unfilled hydrophobic resin is not the only com-
monly applied agent on post surfaces after silanization.
Adhesive systems composed of a hydrophobic and hy-
drophilic monomer blend that are dissolved in organic
solvents are currently applied after silanization as well.
The presence of the remaining solvent can negatively af-
fect the polymerization of adhesive systems,34 reducing
the rate of polymerization.6
A retrospective study identified debonding as the most
frequent reason for failure in the performance of fiber
posts.13 There are difficulties inherent to adhesive ce-
mentation to the root dentin, such as the restricted ac-
cess of light to initiate photoactivation of the adhesive
system and resin cement,8,9,18 inadequate dentin morph-
ology13 for attaining a stable bond to the root dentin near
the apical portion of the root canal,31 and a high ratio of
the bonded to unbonded surface (C-factor) at the long, thin
cement layer5 that can lead to gap formation.28 Therefore,
there are doubts about the fiber post and resin cement
system regarding its bond strength, both between the
post and the resin cement and between the resin cement
and the root dentin. The aim of this in vitro study was to
investigate the push-out bond strength of glass-fiber posts
luted with self-adhesive resin cement using different post
surface treatments, specifically in the root canal. The hy-
potheses of the present study were: (1) application of a
silane coupling agent is necessary to bond a self-adhesive
resin cement to the fiber post surface; (2) application of
silane plus an additional adhesive layer on the glass-fiber
post surface can improve the bond strength to resin ce-
ment; (3) there are differences in the bond strength of
fiber posts in different root regions.
270
Composition
Methacrylate monomers containing phosphoric acid groups,
methacrylate monomers, initiator, stabilizers
Pre-hydrolyzed, single-phase silane, ethanol (70%-80%),
water (20%-30%)21
Bis-GMA, HEMA, phosphate methacrylates, butylated hydroxytoluene,
acetone, camphorquinone, amine, accelerator
Phosphonic acid acrylate, HEMA, bis-GMA, dimethacrylate,
highly dispersed silica, ethanol, catalysts, stabilizers
bis-GMA, HEMA, initiators, stabilizers
MATERIALS AND METHODS
Fifty freshly extracted bovine incisors with mature apices
were selected for the study. The teeth were cleaned
and cut perpendicularly along the long axis below the
cementoenamel junction using a slow-speed diamond
saw (Isomet 1000, Buehler; Lake Bluff, IL, USA) to
obtain 16-mm root lengths. The root canals were end-
odontically treated by the same operator. The working
length was established 1 mm short of the apex using
a #60 K File (Dentsply-Maillefer; Tulsa, OK, USA) as
apical master file. During instrumentation, the canals
were irrigated with 1 ml of 5.25% NaOCl (Proderma;
Piracicaba, SP, Brazil). The canals were filled with gutta-
percha and Sealer26 (Dentsply-Maillefer) endodontic
sealer using the lateral condensation technique with a
finger spreader (Dentsply-Maillefer). The cervical open-
ings of the root canals were then sealed with a eugenol-
free provisional restorative material (Coltosol, Colténe;
Altstätten, Switzerland) and immersed in distilled water
at 37°C. After one week, the gutta-percha was removed
with Gates-Glidden drills (Dentsply-Maillefer), leaving
5 mm of space for apical sealing. The root canals were
standardized to a depth of 10 mm using size #3 post-
hole drills supplied by the tapered fiber-post system
(Exacto, Angelus; Londrina, PR, Brazil). The teeth were
randomly divided into 5 groups according to the glass-fi-
ber post surface treatment: CO (control) – no treatment;
G1 – RelyX Ceramic Primer (silane) only; G2 – silane and
Solobond M; G3 – silane and Scotchbond Adhesive; G4
– silane and Excite. The manufacturer, lot, and compo-
sition of the materials used in this study are shown in
Table 1.
All fiber posts were immersed in 96% ethanol, ultrason-
ically cleaned for 5 min and dried with oil-free air for 1 min.
They were also randomly divided into 5 groups (n = 10)
and treated as shown in Table 2. Four 10-s light-activation
(1200 mW/cm2) exposures were performed at right an-
gles using an LED source (UltraLume LED 5, Ultradent;
South Jordan, UT, USA). The root canals were then rinsed
with distilled water and left moist, using absorbent paper
The Journal of Adhesive Dentistry
 Leme et al

points (Dentsply; Petropolis, RJ, Brazil). After this, the
self-adhesive resin luting agent, RelyX Unicem (3M ESPE;
St Paul, MN, USA) of shade A2 was inserted into the root
canal and applied on the fiber post surface, following the
manufacturer’s instructions. The fiber post was seated in
the root canal using finger pressure. The excess resin ce-
ment was removed with a #5 explorer (Duflex, S.S. White;
Rio de Janeiro, Brazil), and the remaining resin cement
was light polymerized for 60 s from the top. After glass-
fiber post cementation, each root was acid etched for 15
s on the cervical surface and rinsed for 30 s. Excess water
was removed with absorbent paper points, and a core was
constructed with resin composite (Charisma, shade A2,
Heraeus Kulzer; South Bend, IN, USA).
The specimens were stored in a light-proof container in
100% humidity at 37°C for 24 h. Each root was cut perpen-
dicularly to the long axis with a slow-speed water-cooled
diamond saw (Buehler) to produce three 1-mm-thick seg-
ments corresponding to the cervical, middle, and apical
regions of the root canal.
The push-out bond strength test was performed using a
universal testing machine (model 4411, Instron; Canton,
MA, USA) at a crosshead speed of 0.5 mm/min. Each slab
was positioned with the apical surface facing the plunger
tip and in contact with only the fiber post. The push-out
bond strength (Bs) in MPa was calculated using the math-
ematic formula Bs = F/π(R+r)[(R-r)2 + h2 ]0.5, where F is
the load to failure in N, π is the constant 3.14, R is the
coronal radius in each segment, r is the apical radius in
each segment, and h is the thickness of the segment in
millimeters. The results in MPa were submitted to two-way
ANOVA and Tukey’s post-hoc test with _ = 0.05. After
testing, the fractured specimens were observed under a
stereoscopic loupe at 60X magnification to identify the
failure mode. Representative specimens were sputter
coated with gold and observed using scanning electron
microscopy (SEM) (JEOL, JSM-5600LV; Tokyo, Japan).
Table 2 Treatments applied in each group
Groups Fiber-post surface treatment
Control None
G1 A silane layer (RelyX Ceramic Primer) was applied
using a microbrush and air dried for 30 s.
G2 A silane layer was applied, air dried for 30 s,
followed by a layer of an acetone-based adhesive
system (Solobond M). Excess solvent was
removed, light polymerization was performed for
40 s.
G3 A silane layer was applied, air dried for 30
s, followed by a layer of adhesive (bottle #3,
Scotchbond Multi Purpose Plus).
G4 A layer of silane was applied and air dried for 60
s, and the adhesive system (Excite) was applied.
Excess solvent was removed, light polymerization
was performed for 40 s.
RESULTS
The results of the push-out bond strength test for all
groups are shown in Table 3. There was a statistically
significant difference among the root regions (p < 0.05)
and among the fiber-post surface treatments (p < 0.05).
The control group had the worst results, followed by the
silane and adhesive groups. In the control group, there
was no difference among the root regions. For the other
groups, however, the cervical region showed higher
strengths than did the middle or apical regions.
Examinations of the fractured specimens revealed that
the most frequent failure type occurred at the resin ce-
ment and dentin interface (RD), followed by mixed failure
(mixed) and those at the fiber post and resin cement (PR)

Table 3 Mean push-out bond strength in MPa (standard deviation) by root region and failure mode (%) for all
groups

Groups Root region (MPa) Failure mode (%)

Cervical Middle Apical RD Mixed PR
Control 2.39(1.43)Ab 2.78(0.91)Ab 2.92(1.20)Ab 32 39 29

G1 9.65(3.39)Aa 4.11(1.06)Ba 4.04(2.43)Ba 62 31 7

G2 11.21(5.61)Aa 4.53(1.98)Ba 4.38(1.21)Ba 45 29 26

G3 11.23(4.99)Aa 5.96(1.71)Ba 5.12(2.60)Ba 42 34 24

G4 9.43(3.54)Aa 5.26(2.11)Ba 5.26(1.75)Ba 51 31 18

RD: failure at resin cement/dentin interface; PR: failure at the fiber post/resin cement interface. Different superscript capital letters in rows and small letters
in columns indicate statistically significant difference (p < 0.05).

Vol 15, No 3, 2013 271

Leme et al

a b

c d
Fig 1 SEM images of the failure modes. a: failure at the resin cement/glass-fiber post adhesive interface. Note the thick adhesive
layer (*) and the occurrence of voids in the resin cement layer (arrow); b: failure at the resin cement/dentin bond interface; c: cohe-
sive failure in the resin cement; d: mixed failure.

interface. The respective failure modes for each group are
shown in Table 3 and examples of failure types in Fig 1.
The SEM image in Fig 1a also display the occurrence of
voids in the resin cement layer (arrow). Figure 2a shows
no sign of microdefects between the fiber post and the
Bond component of the Scotchbond Multi-Purpose Plus
adhesive system, when this interface remained intact af-
ter the push-out test. Only a superficial interaction was
observed between RelyX Unicem self-adhesive cement
and root canal dentin (Fig 2b).
DISCUSSION
The literature indicates different protocols for glass-fiber
post surface treatment before cementation, with the
goal of enhancing the bond strength of fiber posts to the
root dentin.17,20,23,30 In the present study, the efficacy
of silane with or without the application of an adhesive
layer was investigated. According to the results, the ap-
plication of silane is recommended, although the appli-
cation of an adhesive layer on the fiber-post surface did
not improve the retentive strength and it created a new
interface that can be prone to failure.
No differences in push-out bond strength were found
among the groups that used only the silane or silane
plus an adhesive layer, thus failing to confirm the sec-
ond hypothesis. This resulted in an additional step that
increased chairtime and the possibility of errors due to
the formation of a thick adhesive layer, which may have
been the reason behind the increased failures between
the fiber post and resin cement for G3 (Fig 1a). Adhesive
systems with a blend of organic solvents, hydrophobic
and hydrophilic components were applied on the fiber-post
surfaces after the silane was dried. The type and concen-
tration of solvents in the adhesive system must be known.
Excess solvent in the adhesive layer has been reported as
one possible reason for failure,34 as it induces the forma-
tion of water bridges in the adhesive layer34 and leads
to plasticization and decreased cohesive strength. How-
ever, the active application of an adhesive improves the
volatilization of solvents, resulting in higher bond strength
values.19 In this study, all adhesive systems were applied
by pressing the microbrush against the post surface and
then air drying for 30 s before light polymerization. There-
fore, the solvent volatilization led to adequate adhesive
polymerization, preventing adverse effects on the bond
strength between the fiber post and resin cement.

272 The Journal of Adhesive Dentistry


a b
Fig 2 SEM images of the adhesive interfaces between the glass-fiber post and Scotchbond adhesive (a) and between the resin ce-
ment and the root dentin (b). No hybrid layer was produced by the self-adhesive resin cement (*) and endodontic sealer remained
inside the dentinal tubule (arrow).
A previous study observed that if a silane layer is ap-
plied, airborne-particle abrasion is not necessary.33 How-
ever, silane combined with an acidic primer has been
shown to increase the microshear bond strength when
luting to ceramics.32 In G1, RelyX Unicem was applied in
intimate contact with the silanized post, as opposed to
the groups treated with adhesive systems, which were not
composed of acidic monomers. Although RelyX Unicem
is not a conventional self-etching adhesive system, its
composition still includes phosphate monomers, which
can lead to behavior similar to that observed with those
acidic adhesive systems. Compared to the other groups,
the group without silane attained the worst result with
the highest rate of failures between the resin cement
and fiber post. Aiming to better simulate clinical condi-
tions, all luting procedures were carried out in root dentin
specimens. Using this approach, it was difficult ensure
that all the failures would occur only at the investigated
interface (ie, between fiber post and resin cement). Thus,
it can be speculated that if significant adhesion were
obtained between the resin cement and root dentin, the
failure mode would be predominantly between the fiber
post and resin cement. This result is in agreement with
that of another study which concluded that although the
self-adhesive cement RelyX Unicem is capable of adhering
to fiber-post surfaces through methacrylated phosphoric
esters, silanization was able to improve the bond of this
material to the post.17 In contrast, a recent study24 found
no difference regarding silane application for luting fiber
posts using RelyX Unicem.
The second hypothesis was partially accepted. No dif-
ference in regional bond strength was observed for the
control group, which attained the worst results for all three
root canal regions evaluated. For the experimental groups
(G1 to G4), the cervical region of the root displayed bet-
ter bond strengths than did the middle or apical regions;
these results corroborate those of other studies.5,25 The
higher bond strength in the cervical region could be the
result of higher light intensity initiating better resin cement
Vol 15, No 3, 2013
Leme et al
polymerization in the cervical region than in the middle
and apical regions.8,18 In addition, the dentin substrate
in the cervical region is more prone to adhesion than is
the apical region.11 Another difficulty in the apical region
is the thicker and more compacted smear layer, which is
difficult to remove even after phosphoric-acid etching.31
When the self-adhesive resin cement is used, the etch-
ing procedure is not performed prior to luting. As such,
the bond relies predominantly on the interaction between
the material and smear layer. Examinations of the failure
mode showed that the most fragile point of the fiber post
and the resin cement luted to the root dentin was the
cement/dentin interface. The self-adhesive resin cement
RelyX Unicem is incapable of forming a truly hybrid layer
in the root dentin3,7 the way that adhesive systems can.10
A significant interaction was obtained between the resin
cement and dentin when the luting procedure with RelyX
Unicem was performed under pressure.14 In SEM images
of the fractured specimens, it was possible to observe
dentinal tubules without tag formation (Fig 2b), with the
bond relying only on a superficial interaction between the
resin cement and root dentin. However, in another study,
the best bond strength was observed when the self-adhe-
sive resin cement was used, compared to luting materi-
als associated with etch-and-rinse adhesive systems. The
authors justified this with occurrence of fractures in resin
tags.3 Previous studies have reported on the difficulty self-
adhesive cements have in crossing the thick smear layer
formed during root canal preparation.3,15 Voids were also
present in the resin cement layer (Fig 1a), which could
be related to the viscosity of the material. These voids
act as potential sites of stress concentration and crack
propagation.
A good bond between the fiber post and resin cement
or core resin is expected to ensure the quality of the
final restoration. Although only one pre-hydrolyzed silane
was tested, fiber-post silanization is recommended when
using RelyX Unicem self-adhesive resin cement. Further
studies are necessary to verify the effect of different si-
273
Leme et al
lane coupling agents with other self-adhesive resin ce-
ments. In this study, the weakest point was observed at
the interface between the resin cement and the root den-
tin. Further studies are needed to investigate the bonding
mechanisms of these materials to substrates in order to
elucidate and promote better bond strengths.
CONCLUSIONS
Within the limitations of this study, it can be concluded
that the bonding of the self-adhesive resin cement to the
glass-fiber post was improved by application of the si-
lane coupling agent on the post surface. The application
of an additional adhesive layer between the fiber post
and resin cement did not have any influence on the bond
strength when the silane coupling was previously used.
ACKNOWLEDGMENTS
The authors are grateful to Angelus, 3M ESPE, VOCO, and Ivoclar
Vivadent for providing the materials for research.
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