d e n t a l m a t e r i a l s 3 4 ( 2 0 1 8 ) 1054–1062

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Challenges in luting fibre posts: Adhesion to the

post and to the dentine

Adriana Lemos Mori Ubaldini a , Ana Raquel Benetti b,∗ , Francielle Sato c ,
Renata Corrêa Pascotto a , Antonio Medina Neto c , Mauro Luciano Baesso c ,
Anne Peutzfeldt d
a Department of Dentistry, State University of Maringá, Av. Mandacaru 1550, 87080-0009 Maringá, PR, Brazil
b Department of Odontology, Faculty of Health and Medical Sciences, University of Copenhagen, Nørre Allé 20, 2200
Copenhagen, Denmark
c Department of Physics, State University of Maringá, Av. Colombo 5790, 87020-900 Maringá, PR, Brazil
d Department of Preventive, Restorative and Pediatric Dentistry, School of Dental Medicine, University of Bern,

Freiburgstrasse 7, 3010 Bern, Switzerland

a r t i c l e i n f o a b s t r a c t

Article history: Objective. To investigate the relationship between physicochemical interactions of resin lut-
Received 31 October 2017 ing cements with dentine and retention of fibre posts in root canals.
Received in revised form Methods. Retention of fibre posts (RelyX Fiber Post) was assessed by the pull-out method. The
20 March 2018 diffusion zone of the cements and their chemical interaction with dentine were estimated
Accepted 4 April 2018 by micro-Raman spectroscopy. Resin luting cements employing etch-and-rinse (Rely X Ulti-
mate and Variolink II), self-etch (Rely X Ultimate and Panavia F2.0), or self-adhesive (RelyX
Unicem 2) modes were investigated. Data were analyzed by analysis of variance followed by
Keywords: Tukey HSD tests.
Raman spectroscopy Results. The retention of the fibre posts decreased in the following order: RelyX Ulti-
Dental cements mate, etch-and-rinse mode > RelyX Unicem 2 ≥ RelyX Ultimate, self-etch mode ≥ Panavia
Resin cements F2.0 ≥ Variolink II (p < 0.05). One of the etch-and-rinse mode cements presented the deepest
Posts and core technique diffusion zone, while the other, along with the self-adhesive cement, produced the shallow-
Dowel est zone. Cements used in the self-etch mode showed intermediary diffusion into dentine
(p < 0.05). All resin luting cements showed some degree of chemical interaction with dentine,
the highest recorded for RelyX Ultimate used in the etch-and-rinse mode and the lowest for
Panavia F2.0 (p < 0.05). The retention of fibre posts in the root canal could be attributed nei-
ther to the mode of interaction of the luting cements with dentine nor to their ability to
diffuse into dentine.
Significance. Chemical interaction between the resin luting cement and the dentine paired
with adequate post pretreatment contribute positively to the retention of fibre posts.
© 2018 The Academy of Dental Materials. Published by Elsevier Inc. All rights reserved.

1. Introduction
∗
Corresponding author.
E-mail address: arbe@sund.ku.dk (A.R. Benetti).
The failure pattern of adhesively-luted fibre posts differs from
https://doi.org/10.1016/j.dental.2018.04.001 that of metal posts: whereas fibre posts often fail due to
0109-5641/© 2018 The Academy of Dental Materials. Published by Elsevier Inc. All rights reserved.
 d e n t a l m a t e r i a l s 3 4 ( 2 0 1 8 ) 1054–1062
debonding, metal posts often cause root fracture [1–3]. Thus,
debonding of adhesively-luted posts has been reported to rep-
resent 37% of all failure modes [4,5]. In order to minimize
such failures, efficient adhesion to two distinct substrates is
required: (1) to the surface of the post and (2) to the dentine of
the root canal.
Poor adhesion of luting cements to the surface of fibre posts
is a well-known problem, and good adhesion to the post can
be challenging to obtain [6–8]. Retention of adhesively-luted
posts is influenced by the composition of the post [9]: higher
debonding rates have been observed for glass fibre (49%) com-
pared to carbon fibre (29%) and quartz (26%) fibre posts [4].
Additionally, gaps or defects often encountered in excessively
thick cement layers around the posts contribute negatively
to post retention [10,11]. The influence of the cement film
thickness on retention of adhesively-luted posts becomes
noticeable when these have not been pretreated [12]. Aiming
to improve the overall retention of fibre posts, a number of
surface pretreatments have been proposed, focusing mainly
on increasing micromechanical and/or chemical interaction
between the posts and the resin luting cements [6,8,13–15].
Moreover, good mechanical properties of the luting cement
and its ability to adhere to the root dentine are important
contributing factors for the retention of posts. Resin luting
cements fulfill both of these requirements and thus provide
considerable advantages for the luting of fibre posts. Despite
these desirable properties, both clinical [10] and in vitro studies
[2,11,16–18] have reported the fragile link to lie at the interface
between the resin luting cement and dentine. This observation
may reflect the sensitivity of the adhesive luting technique
towards application in the root canal, considering the diffi-
culties associated with appropriate surface treatment of the
dentine, control of the humidity, evaporation of solvents from
the adhesives, insertion of the luting cement into the canal
without air entrapment, and finally adequate polymerization
of the cement. Some of these aspects are more troublesome for
certain adhesive strategies of the luting cement than for oth-
ers. Initially, 3-step etch-and-rinse adhesives were shown to
provide reliable adhesion to root dentine [19,20]. More recently,
however, a systematic review of in vitro literature demon-
strated superior retention of fibre posts to dentine with the
use of self-adhesive resin cement [21]. This positive finding for
self-adhesive resin cements can be attributed, at least in part,
to reduced technique-sensitivity gained through the elimina-
tion of the numerous steps involved in etching and application
of primer and adhesive. Additionally, self-adhesive cements
contain functional methacrylate phosphoric acid and/or car-
boxylic esters that chemically interact with hydroxyapatite
[22,23]. Despite advances in understanding the underlying
adhesion mechanisms between these functional methacry-
lates and hydroxyapatite [24–27], the contribution of chemical
adhesion or micromechanical retention to the final bond
strength to dentine is not fully understood. Analysis of the
interface between dentine and resin luting cements usually
focuses on the infiltration into dentine or on the degree of
conversion of adhesives and cements [28–30], and even when
combined with mechanical tests [20], these analyses offer lim-
ited information about the physicochemical interactions with
the dental tissues.
1055
Therefore, the purpose of this study was to investigate the
relationship between physicochemical interactions of resin
luting cements with dentine and the retention of fibre posts
in root canals. The influence of two surface pretreatments for
the posts was also assessed. The working hypotheses of this
study were that the retention of fibre posts is influenced by
(1) the mode of interaction with dentine of the resin luting
cement and (2) the pretreatment of the fibre post.
2. Materials and methods
Five resin luting cements were included in this study. Regard-
ing the mode of interaction with dentine, these cements were
used in combination with etch-and-rinse or self-etch adhe-
sives, or without any adhesive (self-adhesive cement). For one
of the cements, a universal adhesive was used in the etch-and-
rinse as well as in the self-etch mode. The investigated luting
cements along with their respective adhesives and manufac-
turers are listed in Table 1. In order to avoid the influence of
the mechanical properties on the outcome of the study, lut-
ing cements with similar flexural strength and modulus of
elasticity were selected. These properties were determined as
described below and before initiation of the retention test and
the interface analysis. Film thickness of the luting cements
was also assessed and used as an estimate of their viscosity.
2.1. Flexural strength and modulus of elasticity
Flexural strength and modulus of elasticity of the luting
cements were obtained from three-point flexural strength
tests based on the procedure described in ISO 4049 [31]. Five
specimens were fabricated from each luting cement. The
cements were either mixed manually or using an automix tip
(see details in Table 1). Thereafter, the cement was inserted in
a rectangular mold (25 mm × 2 mm × 2 mm) and light-cured at
950 mW/cm2 (bluephase, Ivoclar Vivadent, Liechtenstein) at 5
overlapping sites on the top and on the bottom surfaces. The
specimens were stored at 37 ◦ C for 7 days prior to testing in a
universal testing machine (Instron 5566, High Wycombe, UK)
and then loaded at a cross-head speed of 0.75 mm/min until
fracture. Flexural strength was registered and the modulus of
elasticity of the luting cements was calculated from the linear
part of the stress–strain curve.
2.2. Film thickness
Film thickness of the luting cements was assessed in a dark
room based on the procedure described in ISO 4049 [31]. The
thickness of two glass plates separated by two polyester strips
was measured to an accuracy of 0.001 mm. This value (A) was
registered before testing each luting cement. A constant vol-
ume (0.05 mL) of the cement was deposited in the center of
the polyester strip covering the lower glass plate. The sec-
ond polyester strip and the upper glass plate were centered
and placed on top of the luting cement. A load of 150 N was
applied centrally to the specimen for 180 s. The load was then
removed and the specimen was irradiated (bluephase, Ivoclar
Vivadent, Liechtenstein) through the center of the upper glass
plate for 80 s. The thickness of the combined glass plates,
1056 d e n t a l m a t e r i a l s 3 4 ( 2 0 1 8 ) 1054–1062

Table 1 – Luting cements and respective adhesives used according to the mode of interaction with dentine:
etch-and-rinse, self-etch, or self-adhesive. Summary of the pretreatments of root dentine and luting procedures.
Luting cements Pretreatment of root dentine
Etch-and-rinse RelyX Ultimate Adhesive Resin Cement 1. Etching for 15 s
3 M Deutschland GmbH Dental Products 2. Rinsing for 15 s
Neuss, Germany 3. Drying with paper points
Lot 485095 4. Application of Scotchbond
Universal (Lot 484421) for 20 s
5. Removal of excess
6. Air-drying for 5 s
Luting procedure
1. Application of the cement in
the canal with automix tip
2. Insertion of post
3. Removal of excess
4. Light-curing for 40 s

Variolink II 1. Etching for 15 s 1. Mixing of pastes in 1:1 ratio for

Ivoclar Vivadent AG 2. Rinsing for 15 s
Schaan, Liechteinstein 3. Drying with paper points
Lot N51474 4. Application of Excite F DSC
(Lot R26067) for 20 s
5. Removal of excess
6. Air-drying for 5 s
10 s
2. Application of the cement in
the canal with spiral drill
3. Insertion of post
4. Removal of excess
5. Light-curing for 40 s

Self-etch RelyX Ultimate Adhesive Resin Cement 1. Application of Scotchbond 1. Application of the cement in
3 M Deutschland GmbH Dental Products Universal for 20 s the canal with automix tip
Neuss, Germany 2. Removal of excess 2. Insertion of post
Lot 485095 3. Air-drying for 5 s 3. Removal of excess
4. Light-curing for 40 s

Panavia F2.0 1. Application of ED Primer II 1. Mixing of pastes A and B in 1:1

Kuraray Medical Inc. (liquid A Lot 0312AA, liquid B ratio for 20 s
Okayama, Japan Lot 0184AA) for 30 s 2. Application of the cement in
Lot 0537AB (paste A) 2. Removal of excess the canal with spiral drill
Lot 0273AA (paste B) 3. Air-drying for 5 s 3. Insertion of post
4. Removal of excess
5. Light-curing for 40 s

Self-adhesive RelyX Unicem 2 Automix Self-Adhesive No further treatment 1. Application of the cement in
Resin Cement the canal with automix tip
3M ESPE AG Dental Products 2. Insertion of post
Seefeld, Germany 3. Removal of excess
Lot 485664 4. Light-curing for 40 s

polyester strips, and cement was registered (B). The difference from a distance of approximately 2 cm. The posts were rinsed
between measurements A and B was defined as the cement with ethanol (99.9% vol, Kemethyl A/S, Køge, Denmark) and
film thickness. Five replicates were produced for each luting allowed to dry completely. Silane (Silane Bond Enhancer, Pulp-
cement. dent Corporation, Watertown, MA USA, Lot 121206) was then
applied to the surface of the posts with a microbrush and
allowed to dry completely.
2.3. Retention of fibre posts
One hundred and fifty (n = 15 per group; 5 luting cements; 2
post pretreatments) human incisors were used in this experi-
One-hundred and fifty glass fibre posts (RelyX Fiber Post #
ment. The teeth from anonymous donors had been extracted
2, 1.6 mm, 3 M Deutschland Gmbh Dental Products, Neuss,
for therapeutic reasons and kept in 0.5% chloramine until
Germany, Lot 192891206) were divided into two groups accord-
the start of the experiment. Teeth with incomplete apexifi-
ing to the designated surface treatment. Pretreatment of the
cation, root canal treatment or root caries were not used. The
posts were carried out following the results of a pilot study
selected teeth were sectioned at the cemento-enamel junc-
which found post pretreatment necessary to reduce the num-
tion, perpendicularly to their long axis, in a cutting machine
ber of adhesive failures between the fibre posts and the luting
(Accutom, Stuers, Copenhagen, Denmark), leaving 11 ± 1 mm
cements. Half of the posts were coated with a universal adhe-
of root. The roots were kept in deionized water until prepara-
sive (Scotchbond Universal, 3 M Deutschland Gmbh Dental
tion of the root canals. Root canals were prepared to a depth of
Products, Neuss, Germany, Lot 484421). The adhesive was
7 mm with a canal drill (RelyX Fiber Post Drill size 2, 3 M ESPE
actively applied for 20 s, air-dried for 5 s, and light-cured for
AG Dental Products, Seefeld, Germany), irrigated with 0.5%
20 s prior to cementation of the posts. The other half of the
sodium hypochlorite (product nr. 060538, Retroplast Trading
posts was sandblasted and coated with silane. Sandblast-
ApS, Denmark) during drilling, and were finally rinsed with
ing was performed with aluminium oxide particles (average
deionized water. Subsequently, the canals were dried with
diameter 50 ␮m, Korox 50, BEGO Bremer Goldschlägerei Wilh.
paper points (Absorbent Points, Kerr Italia SpA, Scafati SA,
Herbst GmbH & Co., Bremen, Germany, Lot 1010699) for 15 s
at 4 bar (Basic Duo, Renfert GmvH & Co., Hinzingen, Germany)
 d e n t a l m a t e r i a l s 3 4 ( 2 0 1 8 ) 1054–1062
Italy) and treated according to the recommendations from the
manufacturer of each luting cement.
Prior to luting of the posts, the canals in 60 roots were
etched for 15 s with 38% phosphoric acid gel (Etch-Rite Dental
Etching Gel, Pulpdent Corporation, Watertown, MA USA, Lot
120417), rinsed with deionized water for 15 s and dried with
paper points before application of one of the two etch-and-
rinse adhesives for 20 s (Scotchbond Universal, etch-and-rinse
mode, or Excite F DSC; n = 30). In 60 other roots, the canals
were treated with one of the two self-etch adhesives (Scotch-
bond Universal, self-etch mode for 20 s or ED Primer II for
30 s; n = 30), with no previous etching. Excess of adhesive was
removed with paper points and the canals were air-dried for
5 s. No light-curing was performed at this point. In the 30
remaining roots, no further treatment of the canals was per-
formed.
The pretreated fibre posts were then luted in the root canals
at 37 ◦ C. RelyX Ultimate Adhesive Resin Cement was used for
luting in the canals pretreated with Scotchbond Universal, in
the etch-and-rinse as well as in the self-etch mode. Variolink
II was used for luting in the canals pretreated with Excite F
DSC. Panavia F2.0 was used for luting in the canals pretreated
with ED Primer II, and finally, Rely X Unicem 2 Automix was
used for luting into canals that had not received any pre-
treatment. The luting cement was inserted in the root canals
followed by insertion of the pretreated post. Excess of cement
at the canal opening was removed with a microbrush. The
luting cements were then light-cured for 40 s at 950 mW/cm2
(bluephase, Ivoclar Vivadent, Liechtenstein) by positioning the
light-tip as close to the post as possible. A summary of the den-
tine pretreatments and cementation procedures is presented
in Table 1.
All roots with luted posts were stored in water at 37 ◦ C
for 7 days. Retention of the posts in the root canals was
then assessed in a universal testing machine (Instron 5566,
High Wycombe, UK) by means of the pull-out method. A stop
made of resin composite was fabricated around the coronal
portion of the post in order to improve gripping by the pull-
out accessory. Resin composite was also used to level the
roots during testing in a manner that allowed pulling out the
posts in a direction parallel to their insertion axis. The luted
posts were extracted from the roots at a crosshead speed of
1.0 mm/min and the maximum removal force was registered.
Subsequently, the posts were studied at ×18 magnification in
a stereomicroscope (Nr. 509088, Ernst Leitz GmbH, Wetzlar,
Germany) under illumination (American Optical Corporation,
model 365E, Buffalo NY, USA) in order to determine the fail-
ure pattern. Failures were classified as (1) mostly adhesive
between cement and post (AP); (2) mixed (M); (3) mostly adhe-
sive between cement and dentine (AD).
2.4. Micro-Raman spectroscopy
The diffusion zone of the resin luting cements and their chem-
ical interaction with root dentine were assessed by means
of micro-Raman spectroscopy (MRS). Posts were luted into
roots from additional teeth (n = 3 for each resin luting cement)
following the dentine pretreatments and luting procedures
described previously (Table 1). The roots with luted posts were
sectioned in halves along their longitudinal axis with a water-
1057
Fig. 1 – Representative Raman spectra of the adhesive
interface (in this case RelyX Unicem 2 Automix). Each
measurement is represented by a numbered line on the
z-axis (specimen shift). The light gray lines represent the
cement, the black, bold lines represent the diffusion zone,
and the black, slim lines the dentine.
cooled diamond disc (Diamond Wheel 012 x fine, South Bay
Technology Inc, CA, USA) mounted in a low-speed cutting
machine (Isomet 1000, Buehler, Lake Bluff, IL, USA). The root
sections with exposed adhesive interfaces were rinsed with
distilled water in an ultrasonic bath for 5 min to remove the
debris smeared on the specimen surface during cutting. Since
the post from one of the halves was consumed during cutting,
only half of each root was available for the MRS analysis.
The analysis was performed with a SENTERRA dispersive
Raman microscope (Bruker Optik GmbH, Ettlingen, Germany).
The spectra were excited by a 785 nm laser source and regis-
tered at the spectral range of 450–1800 cm−1 . The laser beam
was focused on the specimen with a ×100 objective lens.
The spectral resolution was 3–5 cm−1 , the detector’s integra-
tion time was 3 s, and the spectrum collected at each point
was the average result of 60 consecutive readings. In order to
improve signal to noise ratio, the detector temperature was
decreased to −90 ◦ C. All spectra were systematically collected
under identical conditions.
Raman spectra were acquired at the cervical root area,
mapping the interface starting from the luting cements and
moving towards the dentine [30,32–34] at 1 ␮m intervals by
using the computer controlled x–y–z stage (Fig. 1). Spectra
were collected along 2 line-scans, each 20 ␮m long, with 30 ␮m
space between lines. In order to avoid dehydration of the speci-
mens, gauze soaked in distilled water was kept in contact with
the dentine during MRS data collection.
The diffusion zone of the cements into dentine was identi-
fied through the Raman band peak at 1113 cm−1 (␯C O C),
which is representative of the carbon chain in the resin
monomer present in all the investigated materials [34,35] (Ori-
gin, Northampton, MA, USA). The evolution of peak intensities
of this Raman band behaved as in a sigmoidal shaped function.
1058 d e n t a l m a t e r i a l s 3 4 ( 2 0 1 8 ) 1054–1062

Fig. 2 – Representative plot of the diffusion zone (in this case RelyX Unicem 2 Automix), where the Raman mapping spectra
at 1113 cm−1 (␯C O C) is plotted according to the specimen shift position and fitted to the Boltzmann function.

Therefore, the experimental data in this study was fitted to an

S-shaped curve best described by the Boltzmann function [36],
and the analytical fitting followed the procedure described in
details in a previous publication [37]. According to this proce-
dure, the sigmoidal fitting was applied on the peak intensity
corresponding to the resin monomer (1113 cm−1 ) permeation
into dentine within the analyzed area (Fig. 2). The Boltzmann
fitting was applied in each of the 6 scans from each cement.
The depth of the diffusion zone was averaged first for each
root and subsequently for each cement.
Chemical interactions at the interface were investigated
through the analysis of characteristic peaks that represent
the mineral component in dentine (961 cm−1 — ␯1 phos-
phate symmetric stretch) and the CH2 group of methacrylate
monomers (1458 cm−1 — deformation ı of CH2 ) [33]. The ratios
between these intensity peaks (961 cm−1 /1458 cm−1 ) were cal-
culated for every Raman mapping point on the z-axis and
were plotted as a function of distance from the interface
(Fig. 3).
Fig. 3 – The ratio between peaks at 961 cm−1 /1458 cm−1 for
each luting cement plotted as a function of the distance
2.5. Statistical methods
from the interface (0 = interface).

The data were checked for normality using the Shapiro–Wilk

test (p > 0.05). Flexural strength, modulus of elasticity, film
thickness, as well as results on depth of the diffusion zone
and the ratio 961 cm−1 /1458 cm−1 were analyzed by one-way
analysis of variance. Retention of posts was analyzed by two-
and one-way analysis of variance. When statistically signif-
icant differences were identified, the Tukey HSD multiple
comparison test was applied. Type of failure results were
analyzed by the Kruskal–Wallis test. Pearson bivariate test
was used to test for possible correlations between reten-
tion of posts sandblasted and pretreated with silane and (i)
cement film thickness, (ii) depth of the diffusion zone, and
(iii) 961 cm−1 /1458 cm−1 ratio. The level of significance for all
comparisons was determined at ˛ = 0.05.
 d e n t a l m a t e r i a l s 3 4 ( 2 0 1 8 ) 1054–1062 1059

Table 2 – Flexural strength (MPa), modulus of elasticity (GPa), and film thickness (␮m) of the resin luting cements (mean
values and standard deviations). Different superscript letters identify significant differences among the cements for a
given property.
Luting cement Flexural strength (MPa) Modulus of elasticity (GPa) Film thickness (␮m)
RelyX Ultimate Adhesive Resin Cement 83.7 (4.5)a 7.3 (0.3)a 36.1 (4.7)b
a a
Variolink II 91.9 (4.1) 7.3 (0.6) 47.4 (2.8)a

Panavia F2.0 91.2 (6.0)a 7.5 (0.3)a 48.4 (4.9)a

a a
RelyX Unicem 2 Automix 91.5 (5.3) 7.5 (0.2) 33.4 (2.9)b

Table 3 – Retention (N) of posts (mean values and standard deviations) and type of failure (for the number of specimens,
n) according to post pretreatment (n = 15). Different superscript letters identify significant differences among the cements.
Mode Luting cement Post pretreatment

Universal adhesive Sandblasting and silane

Retention (N) Type of failure* (n) Retention (N) Type of failure* (n)
a
Etch-and-rinse RelyX Ultimate Adhesive 399.1 (43.1)ab 13 AP 421.5 (69.3) 6 AP
Resin Cement
2M 1M
0 AD 8 AD

Variolink II 198.0 (44.1)f 0 AP 250.8 (68.4)ef 1 AP

1M 0M
14 AD 14 AD

Self-etch RelyX Ultimate Adhesive 302.5 (76.5)cde 6 AP 342.7 (90.3)bcd 1 AP

Resin Cement
6M 1M
3 AD 13 AD

Panavia F2.0 267.0 (72.0)def 4 AP 294.8 (60.3)cde 2 AP

1M 0M
10 AD 13 AD

Self-adhesive RelyX Unicem 2 Automix 319.5 (60.3)cde 9 AP 353.2 (60.1)ab 1 AP

3M 2M
3 AD 12 AD
∗
AP = mostly adhesive between cement and post; M = mixed; AD = mostly adhesive between cement and dentine.

except for RelyX Unicem 2 Automix (Table 3). Additionally,

3. Results the distribution of type of failure varied not only with the lut-
ing cements (p < 0.001) but also with the post pretreatment
The four luting cements were confirmed to possess statis-
(p < 0.001). Posts that had been sandblasted and treated with
tically similar flexural strengths (p = 0.119) and moduli of
silane tended to have fewer adhesive failures between cement
elasticity (p = 0.179) (Table 2). Significantly higher film thick-
and post (AP) compared to posts that had been pretreated with
nesses were registered for Variolink II and Panavia F2.0,
universal adhesive (Table 3).
implying increased viscosity of these two cements when com-
The depth of the diffusion zone of the resin luting cements
pared to RelyX Ultimate and RelyX Unicem 2 (Table 2).
into dentine varied with statistical significance. RelyX Ulti-
The retention of the posts was significantly influenced by
mate Adhesive Resin Cement used with the adhesive in the
the luting cement (p < 0.001) and by the post pretreatment
etch-and-rinse mode resulted in a deeper diffusion zone than
(p = 0.001), whereas no significant interaction between lut-
did Variolink II, the other etch-and-rinse cement, and the self-
ing cement and post pretreatment was identified (p = 0.915).
adhesive cement RelyX Unicem 2 Automix (Table 4). The ratio
The retention of posts provided by the luting cements
between the peaks at 961 cm−1 and 1458 cm−1 , which is indica-
decreased in the following order: RelyX Ultimate, etch-
tive of the extent of chemical interaction with dentine, was
and-rinse mode > RelyX Unicem 2 ≥ RelyX Ultimate, self-etch
significantly higher for RelyX Ultimate used with the adhesive
mode ≥ Panavia F2.0 ≥ Variolink II (Table 3). The significant dif-
in etch-and-rinse mode than for Panavia F2.0 (Table 4, Fig. 3).
ferences in the retention of posts could not be explained by
Finally, no correlation was found between the retention of
the mode of interaction with dentine (etch-and-rinse = self-
posts and (i) the cement film thickness (R = −0.796, p = 0.053) or
etch = self-adhesive; p > 0.05).
(ii) the depth of the diffusion zone (R = 0.628, p = 0.128). How-
Sandblasting and silane application did not result in supe-
ever, a borderline, positive correlation was found between
rior retention of the fibre posts in the root canal compared
to pretreatment of the posts with the universal adhesive,
1060 d e n t a l m a t e r i a l s 3 4 ( 2 0 1 8 ) 1054–1062

Table 4 – Depth of the diffusion zone (␮m), according to the Boltzmann analysis, and ratio between peaks at
961 cm−1 /1458 cm−1 of the luting cements at the interface (mean values and standard deviations). Different superscript
letters identify significant differences among the cements.
Luting cement Diffusion zone Ratio
(␮m) 961 cm−1 /1458 cm−1
RelyX Ultimate Adhesive Resin Cement (etch-and-rinse mode) 3.5 (0.4)a 5.1 (1.5)a

Variolink II 2.2 (0.6)b 3.1 (0.8)ab

ab
RelyX Ultimate Adhesive Resin Cement (self-etch mode) 2.1 (1.3) 3.1 (0.3)ab

Panavia F2.0 2.2 (1.1)ab 2.2 (0.2)b

b
RelyX Unicem 2 Automix 1.8 (0.6) 4.5 (1.4)ab

the retention of posts and (iii) the ratio between peaks at cements (0 up to 2 ␮m) [22], and no hybrid layer forma-
961 cm−1 /1458 cm−1 (R = 0.808, p = 0.049). tion at all for the self-adhesive cement [43]. In fact, previous
work using high-resolution electron microscopy reported the
self-adhesive cement to interact only superficially with den-
4. Discussion tine and enamel [22]. Considering the self-adhesive mode, a
layer of hydroxyapatite-depleted collagen remains between
The retention of fibre posts has previously been shown to
RelyX Unicem 2 and the unaffected dentine, and the adhesion
depend on the composition [38] and mechanical properties
mechanism differs from that of self-etch adhesives for which
[39] of the resin luting cement. In this study, resin cements
distinct demineralization and hybridization at the interface
of similar flexural strength and modulus of elasticity were
has been observed [23].
selected, thus allowing us to focus on the physicochemical
It is important to emphasize that the present study
interactions of the resin luting cements with dentine.
employed the MRS technique. This technique has been used to
Earlier work has reported superior retention of fibre posts
analyze the diffusion zone of adhesive materials into the den-
luted with resin cements that employ etch-and-rinse adhe-
tal hard tissues based on chemical differences between these
sives [40,41] on the grounds of increased micromechanical
substrates, and consequently looks at the distinct spectra in
retention due to the separate etching step. Nonetheless, a sys-
the transition layers within the adhesive interface [34,37].
tematic review [21] suggested the use of self-adhesive resin
In short, MRS identifies the representative bands of dentine
cements to improve fibre post retention into root canals, as
(P O) and resin monomer (C O C) which then allows for the
the etching and bonding steps are not needed, rendering
calculation of the diffusion zone by the Boltzmann analytical
the technique less sensitive. The present study found signif-
method [37]. This gives a quantitative measure of the penetra-
icant differences in retention of the fibre posts among the
tion of resin monomers into the dental tissue independently of
resin luting cements tested, but the differences could not
the presence of a true hybrid layer [37] and differs from the fre-
be attributed to the mode of interaction of the resin lut-
quently used imaging techniques based on the visualization
ing cements with dentine; therefore the first hypothesis was
of the demineralization zone and/or the hybrid layer.
rejected. The present results are in agreement with those of
Monomer infiltration has been considered of importance
Bitter et al. [42] who found significantly higher bond strengths
for bond quality [43]. In the present study, however, no correla-
for the self-adhesive cement RelyX Unicem when compared to
tion between retention of posts and the depth of the diffusion
the self-etch cement Panavia F and the etch-and-rinse cement
zone was found, and our results indicate that cement diffu-
Variolink II.
sion into dentine is not the most relevant factor for adhesion.
The mode of interaction of the resin luting cement with
By analyzing the 961 cm−1 /1458 cm−1 ratio, distinct levels of
dentine did not influence post retention or the cements’
chemical interaction at the interface between the resin lut-
diffusion into dentine. The Boltzmann analysis showed the
ing cements and dentine were identified (Fig. 3). A significant,
deepest diffusion zone into dentine for one of the cements
although borderline, positive correlation was found between
employing separate etching (RelyX Ultimate, etch-and-rinse
the retention of posts and the 961 cm−1 /1458 cm−1 ratio. Our
mode) but not for the other etch-and-rinse cement (Variolink
findings demonstrate that the more intense the chemical
II), which displayed a diffusion zone statistically equal to
interaction of the luting cement with dentine, the higher
that of the two self-etch cements (RelyX Ultimate, self-etch
the retention of the fibre posts. However, complex interac-
mode, and Panavia F2.0) and the self-adhesive cement (RelyX
tions between the different variables involved in the retention
Unicem 2). Our results are corroborated by previous work that
of posts are at play and future research on the physico-
also employed the Boltzmann analytical method and which
chemical interactions between fibre posts and their respective
reported the diffusion zone into dentine to be 2.5 ± 0.3 ␮m
interfaces with dentine and cement may help improving our
for a self-etch cement (Multilink) and 1.8 ± 0.4 ␮m for a self-
understanding.
adhesive cement (RelyX Unicem 2) [37].
The retention of fibre posts was also found to be sig-
However, the fact that diffusion into dentine was not influ-
nificantly influenced by the post pretreatment, leading to
enced by the mode of interaction with dentine differs from
acceptance of the second hypothesis. According to our results,
findings of earlier studies using imaging techniques, which
pretreatment of posts with sandblasting and silane applica-
reported thicker hybrid layers (5–7 ␮m) for the etch-and-rinse
tion improved retention of the fibre posts when compared
mode of interaction [32], thinner hybrid layers for self-etch
 d e n t a l m a t e r i a l s 3 4 ( 2 0 1 8 ) 1054–1062
to pretreatment with the universal adhesive. This finding is
in corroboration with numerous previous studies which have
reported roughening of the post by sandblasting [13,44,45] or
silicatization [46] to be the most effective pretreatment of fibre
posts. It is noteworthy that in the present study the combi-
nation of sandblasting and silane generally led to a different
failure pattern as compared to the pretreatment consisting
of application of a universal adhesive. Indeed, sandblasting
followed by silane treatment resulted in only 15% failures
at the interface between the cement and the post as com-
pared to 43% following application of universal adhesive. This
observation is in agreement with previous findings [11,47],
and is an indication that the adhesive interface with den-
tine could in fact be tested in the current study. The finding
that pretreating the posts with the universal adhesive resulted
in a relatively high number of adhesive failures between the
posts and the cement may be explained by the fact that the
composite resin matrix surrounding the fibres was practically
completely cured, thus allowing no chemical reaction between
the resin monomers of the adhesive and the composite resin
matrix of the post [7]. A high degree of crosslinking of the com-
posite resin matrix also limited interdiffusion of monomers
from the adhesive into the surface of the posts [7,8] and hin-
dered the formation of an interpenetrating polymer network,
which might otherwise have improved the adhesion between
the post and the cement [6–8,15]. Indeed, because of the higher
incidence of failures between the post and the luting cement,
pretreatment of fibre posts with the universal adhesive cannot
be regarded as the pretreatment of choice.
5. Conclusion
Within the limitations of this study, it can be concluded that
chemical interaction between resin luting cements and den-
tine is important for the retention of fibre posts in root canals.
In contrast, the mode of interaction of the luting cements with
dentine, their depth of diffusion into dentine, and their viscos-
ity had no or limited effect on the retention of fibre posts.
Acknowledgements
The study was supported by the Faculty of Health and
Medical Sciences, Department of Odontology, University of
Copenhagen, and the Brazilian funding agencies FINEP (Finan-
ciadora de Estudos e Projetos) and CAPES (Coordenação de
Aperfeiçoamento de Pessoal de Nível Superior). The authors
acknowledge 3M Denmark for the donation of materials.
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