Dental Materials Journal 2016; : –

Bonding effectiveness of composite-dentin interfaces after mechanical loading

with a new device (Rub&Roll)
Anelise Fernandes MONTAGNER1,2, Niek J OPDAM2, Jan L RUBEN2, Maximiliano Sérgio CENCI1
and Marie-Charlotte HUYSMANS2

1
Graduate Program in Dentistry, School of Dentistry, Federal University of Pelotas, Rua Gonçalves Chaves, 457, Fifth Floor, 96015560, Pelotas,
RS, Brazil
2
Department of Preventive and Restorative Dentistry, Radboud University Nijmegen Medical Centre, P.O. Box 9101, NL 6500 HB, Nijmegen, The
Netherlands
Corresponding author, Anelise Fernandes MONTAGNER; E-mail: animontag@[Link]

This study evaluated the effect of mechanical loading with a new device on the microtensile bond strength (µTBS) of adhesive systems
to dentin. Forty molars were divided according to adhesive systems: self-etch (ClearfilTM SE Bond —CSE) and etch-and-rinse (Adper
ScotchbondTM 1XT —ASB); and to aging (n=5): control; MC1-250,000; MC2-500,000; and MC3-750,000 mechanical cycles. Microtensile
bond strength was measured and fracture modes were analyzed. Data for µTBS were subjected to Kruskal-Wallis and post hoc tests
(p<0.05). Mechanical loading (p<0.001) and adhesive systems (p=0.024) affected µTBS values. The adhesive systems showed a similar
behavior, except in the MC3 group, which the self-etch CSE showed the highest µTBS. The new device promotes a decreasing of µTBS
as the number of cycles increased. Difference between materials was observed only after 750,000 mechanical cycles.

Keywords: Mechanical load, Adhesive systems, Microtensile, Bond strength, Loading

spaces available.
INTRODUCTION
Numerous in vitro studies to test the performance of
Dentists worldwide spend most of their time placing dentin adhesives systems focus on its relationship with
and replacing direct restorations. Therefore, the long- clinical performance. The potential relationship between
term survival of clinically placed restorations is an marginal adaptation found in vitro of class V restorations
important focus for dental research. The main reasons and the clinical longevity of class 5 restorations has
for failure of restorations on the long-term are fracture been demonstrated9). Moreover, Van Meerbeek et al.
and secondary caries1). Considering the high turnover demonstrated correlation between microtensile bond
of new materials on the market, it is important to test strength tests on aged samples by storing and the clinical
these materials first in vitro in a clinical relevant way, outcome of class V restorations10). In class 2 restorations,
in order to be able to predict possible clinical pathways aging by mechanical loading may play an even larger
of failure2,3). Therefore, aging processes resembling those role and therefore, it seems useful to include mechanical
taking place in the oral environment were introduced loading as an aging process to in vitro studies to compare
in laboratory testing procedures. Simulations of bonding capacities of dental adhesives.
thermal and mechanical stresses have been used to try High initial composite-dentin bond strength values
to reproduce these conditions. However, the popular are considered desirable, but durability of the bond
thermal cycling method has limited effect compared to over time is also of great interest, especially when the
mechanical aging3). adhesive is applied in load bearing restorations. Loading
Mechanical load cycles and forces applied are stress seems to be concentrated mostly at the interface
not standard in most studies, as well as methods and between the adhesive and the top of the hybrid layer4).
devices used to apply the force4,5). Most of those studies Sano et al.11) introduced the microtensile bond strength
use machines that apply the force on the sample in test to measure bonding of small areas surface (≈1 mm²),
just one direction, which seems quite different from and nowadays this test is accepted as the most useful
the continuous process of chewing forces and bruxism bond strength test showing a higher discriminative
clinically present to the tooth-restoration complex. power when compared to other tests3).
Moreover, forces applied in in vitro experiments show a So, in order to evaluate the effectiveness of a new
large variation from 15 to 60 N6-8). A main problem related device for application of mechanical loading the present
to the mechanical loading is that when multidirectional study uses the microtensile bond strength (µTBS) test to
forces are applied, devices become more complicated evaluate the effect of aging with mechanical loading on
and expensive. Moreover, the process is time-consuming the adhesive bond between tooth and restoration. The
as most devices only have a limited number of sample null-hypothesis tested is that the applied mechanical
loading does not influence microtensile bond strength
values.
Color figures can be viewed in the online issue, which is avail-
able at J-STAGE.
Received Nov 16, 2015: Accepted Mar 3, 2016
doi:10.4012/dmj.2015-395 JOI [Link]/dmj/2015-395
2 Dent Mater J 2016; : –

Acrylic Resin, Ivoclar Vivadent, Mississauga, Canada)

MATERIALS AND METHODS
resulting in samples of 16 mm in height×14 mm width×10
Description of the device mm length (Fig. 1). After that, dentin surfaces were
The device for applying mechanical loading (Rub&Roll) polished using 600-grit SiC paper to create a uniform
is shown in Fig. 1 and described in detail elsewhere12). smear layer.
Basically, the Rub&Roll is a new device with Samples were assigned randomly to one of eight
multifunctional characteristics. The machine has one groups (n=5), receiving one of two adhesive systems
outer cylinder that is mounted fixed on a base, and an and one of four aging protocols. Dentin surfaces were
inside cylinder that fits centrally in the outer cylinder. treated with a self-etch adhesive system ClearfilTM SE
The inside cylinder, which is mounted on a rotation axle, Bond–CSE–(Kuraray Noritake Dental, Tokyo, Japan) or
contains 16 samples holders (20×14×10 mm dimensions) an etch-and-rinse adhesive system Adper ScotchbondTM
which are evenly distributed over the outer surface of 1XT–ASB–(3M ESPE, St. Paul, MN, USA) which was
the cylinder. The inner cylinder is rotating around the applied with wet-bonding technique. Both adhesive
axle, which is driven by an engine that can be adjusted systems were applied according to the manufacturer’s
according to the required rotation speed. In the space instructions as indicated in Table 1. Thin layers of resin-
between inside and outside cylinder a loosely fitting based composite (Clearfil™ AP-X, Kuraray Noritake
rod is placed, consisting of a metal rod inside a silicon Dental), approximately 1.5 mm in thickness, were bonded
tube. When the inside cylinder is rotated, this rod rolls incrementally to the cured adhesive, and each increment
over the samples protruding from the inner cylinder, was individually light-cured for 20 s using a LED curing
leading to cyclic loading of the samples. Silicon tubing of unit with an intensity of ≈900 mW/cm2 (FusionTM S7
1 mm thickness was used in this study, and the samples Curing Light, DentLight, Richardson, TX, USA). This
protruded 1 mm above the cylinder surface, resulting in resulted in restorations 4 mm in height. Aging protocols
a maximum load of 30 N. The actual applied force on the were (Fig. 1):
samples was measured with a force sensor mounted in 1. Control (no aging): samples were stored in
the surface of the outside cylinder. distilled water for 24 h, at room temperature;
2. MC1: mechanical loading for 1 week, 250,000
Specimens preparation cycles;
Forty extracted sound human third molars were selected, 3. MC2: mechanical loading for 2 weeks, 500,000
cleaned and stored in water. Anonymously collected cycles;
extracted human teeth were used, which does not require 4. MC3: mechanical loading for 3 weeks, 750,000
ethical committee approval in The Netherlands. Flat cycles.
occlusal superficial dentin surfaces were exposed using Before the samples were exposed to mechanical
200-grit SiC paper under running water, and complete aging, they remained in distilled water for 24 h.
removal of enamel was confirmed by stereomicroscopy
(M50 Leica Microsystems, Singapore) examination. Mechanical loading
Teeth were embedded in acrylic resin (ProBase Cold Samples were mounted into the Rub&Roll device

Fig. 1 Study Design: specimens preparation, adhesive and restorative procedures, ageing
groups, Rub&Roll device (general schematic overview of the Rub&Roll device —A,
closer overview of the cylinder inside the container —B), composite-dentin beams
production, microtensile test and SEM evaluation.
 Dent Mater J 2016; : – 3

Table 1 Study Material

Material Type Compositiona Application procedures Lot

1. Apply phosphoric acid for 15 s,

Etching agent: 35%
2. Rinse for 15 s,
phosphoric acid (pH 0.7)
3. Blot excess moisture using a
Etch-and-rinse Adhesive: Bis-GMA, HEMA,
Adper Scotchbond cotton pellet,
two-step dimethacrylates, 188103
1XT (3M ESPE) 4. Apply two adhesive coats under
adhesive system polyalkenoic copolymer,
pressure for 15 s,
ethanol, water,
5. Gently air thin for 5 s,
photoinitiator
6. Light-cure for 10 s.

1. Apply primer and leave it

Primer: MDP, HEMA
undisturbed for 20 s,
Dimethacrylate, monomer
Self-etch 2. Dry thoroughly with mild air
Clearfil SE Bond Water. Photoinitiator
two-step flow for 10 s, 041892
(Kuraray) Bond: MDP, HEMA
adhesive system 3. Apply bond,
Dimethacrylate, monomer
4. Gently air thin for 5 s,
Microfiller, Photoinitiator
5. Light-cure for 10 s.

Clearfil AP-X Hybrid light- Barium glass, silica colloidal,

1. Apply composite 2 mm thick,
(Kuraray) cure resin-based silicon dioxide, Bis-GMA, 1090AA
2. Light-cure for 20 s.
Shade A2 composite TEGDMA, photoinitiator
a
Bis-GMA (bisphenol glycidyl dimethacrylate); HEMA (2-hydroxyethyl methacrylate); MDP (10-methacryloyloxydecyl
dihydrogen Phosphate); TEGDMA (Triethylene glycol dimethacrylate)

and mechanical loading was applied by the rotation failures were included in the calculation of mean µTBS
movement of the inner cylinder (Fig. 1). In this study, as 0 MPa.
samples were loaded at 20 rpm, 0.4 Hz, and ±30 N.
Mechanical loading took place in distilled water, which Mode of failure determination
filled the outer cylinder. The distilled water was weekly All fractured beams were observed under
changed. stereomicroscope (M50 Leica Microsystems) and the
fracture mode was determined at 75× magnification.
µTBS test Images were captured by camera (Canon EOS 50D,
After aging, loaded and unloaded (control) samples were Canon, Melville, LA, USA). The fracture surfaces were
sectioned into beams (stick-shaped) with an approximate classified as: apparently interfacial (fracture occurred
cross-sectional area of 1 mm2, using a low speed within the adhesive interface, between the dentin and
diamond saw under continuous water-cooling, following composite); cohesive in dentin (fracture occurred at the
the nontrimming method (Fig. 1)13). This resulted in dentin portion); cohesive in composite (fracture occurred
50–75 beams for each experimental group. Each beam at the resin-based composite portion) or mixed failures
was measured for its cross-sectional dimensions using (designates a mixture of adhesive and cohesive failure
a digital caliper (Mitutoyo America, Los Angeles, CA, within the same fractured surface).
USA) to calculate the surface area. Beams were tested Subsequentially, selected fractured beams of each
for microtensile bond strength (µTBS) by attaching group (n=10), exhibiting a representative failure mode,
them with superglue gel (Cyanoacrylate Rite-Lok, 3M, were processed for field-emission-gun scanning electron
Bracknell, UK) adhesive to a movable jig, a modified microscopy (Fig. 1). Specimens were chemically fixed
Gerlaldeli’s jig, which is attached to the Universal by immersion in 2.5% glutaraldahyde in 0.1 M sodium
Testing Machine (Materials Testing Machine LS1, Lloyd cacodylate buffer for 6 h, and dehydrated in an ascending
Materials Testing, Hampshire, UK) at 1 kN. The beams series of ethanol: 50% for 5 min, 90% for 5 min, and finally
were stressed to failure in tension using µTBS tester at a 100% ethanol for 3 h. After that, specimens were dried
crosshead speed of 1 mm/min. The fractured beams were at room temperature followed by sputter coating with
removed from the apparatus and the modes of fracture gold and evaluated in a scanning electron microscope
were evaluated. (Feg-SEM, Philips XL30, Eindhoven, The Netherlands).
The bond strength (σ) in MPa was obtained with
the formula σ=F/A, where F=load for specimen rupture Statistical analysis
(N) and A=bonded area (mm2). To determine the area, The microtensile bond strength values, in MPa, were
the formula to calculate was A=b.h, where A=interfacial subjected to Levene Test to evaluate Homogeneity
area, b=base and h=thickness of slices. Pre-testing of Variances, and then, data were analyzed through
4 Dent Mater J 2016; : –

Kruskal-Wallis Test (tested variables were: material and the highest µTBS values and MC3 showed lower µTBS
aging times conditions) and a post hoc Dunn’s Test. Pre- values when compared to other aging conditions. So
testing failures were included in the calculation of mean with increasing mechanical load cycles, bond strength
µTBS as 0 MPa. Differences in distribution of failure values decreased. The adhesive systems showed similar
mode distribution among groups were analyzed using results at control, 1 and 2 weeks aging, but after 3 weeks
Chi-square test. Additionally, the relationship between aging CSE showed significantly higher µTBS values
µTBS values and the type of fracture mode was analyzed than ASB. So, CSE was more stable trough time than
with one-way ANOVA. All tests were conducted using a the ASB adhesive. Mean µTBS varied from 17.9 up to
statistical software package (SPSS, version 19, Chicago, 37.4 MPa.
IL, USA). The statistical significance was set at p<0.05.
Mode of fracture
RESULTS There was no relation between the bond strength values
and the type of fracture (ANOVA, p=0.726). A higher
Bond strength frequency of pre-testing failures was observed for the
The results are shown in Table 2. There was a significant loaded groups, statistically significantly so for ASB
difference between the adhesive systems (p=0.024) and along the aging conditions (p=0.004, Chi Square Test)
among the different aging time according to the Kruskal- (Table 2). Regarding fracture modes, there was no
Wallis test (p<0.001). MC1 (250,000 cycles) and MC2 difference between the materials (p=0.461); however for
(500,000 cycles) showed similar results, but these were CSE, the control group showed more cohesive failures
different from the control and MC3 (750,000 cycles). than the aged groups (Chi Square Test, p=0.029)
For both adhesive systems, the control group showed (Table 3). Figure 2 shows some representative fracture

Table 2 Means of µTBS values, in MPa, standard deviations (±SD), pre-testing failures [PF] and number of beams tested
(*n) from each group

Time % % %
24-h MC1 Aging MC2 Aging MC3 Aging
Reduction Reduction Reduction
Bond Bond Bond Bond
between between between
Strength Strength Strength Strength
24 h and 24 h and 24 h and
(MPa) (MPa) (MPa) (MPa)
Materials MC1 MC2 MC3

Adper 37.4 (14.0) Aa 24.4 (12.6) Ab 24.7 (10.5) Ab 17.9 (9.5) Bc

Scotchbond 45.0 45.1 63.5
1XT [2] a
*60 [13] b
*58 [14] b
*60 [19] c *53

Clearfil SE 34.0 (12.2) Aa 25.0 (14.2) Ab 24.7 (10.5) Ab 22.7 (10.7) Ac

32.4 33.6 37.3
Bond [3] a
*60 [8] a
*60 [9] a
*60 [7] a *60

For each line, values ​​with different small letters indicate significant difference among the aging times, within the same
adhesive system (p<0.05).
For each column, values ​​with different capital letters indicate significant difference (p<0.05) between the adhesive systems,
within the same aging time.

Table 3 Number and percentage of mode of failure using different adhesive system and aging conditions

Aging MC1 MC2 MC3

24-h
(1 week/250,000 cycles) (2 weeks/500,000 cycles) (3 weeks/750,000 cycles)

Adhesive AI CR CD M AI CR CD M AI CR CD M AI CR CD M

Adper 31 1 0 28 26 3 2 27 22 1 2 35 22 0 1 30
Scotchbond
51.7% 1.6% 0% 46.7% 44.8% 5.2% 3.5% 46. 5% 36.6% 1.6% 3.4% 58.4% 41.5% 0% 1.8% 56.7%
1XT

Clearfil SE 26 8 3 23 28 0 2 30 2 5 2 26 21 1 4 34
Bond 43.4% 13.3% 5% 38.3% 46.7% 0% 3.3% 50% 45.1% 8.3% 3.3% 43.3% 35% 1.6% 6.7% 56.7%

AI=apparently interfacial; CR=cohesive in resin-based composite; CD=cohesive in dentin; M=mixed

 Dent Mater J 2016; : – 5

Fig. 2 Representative scanning electron micrographs of the most occurred fractures.

Dentin sides of fractured beams are shown. (A): Apparently interfacial fracture along
the composite-dentin interface of Control CSE group in a lower power magnification
(75×). Note that the failure started in the corners of the beams (white arrows). (B): a
higher magnification of 2,000× shows that the failure occurred inside the hybrid layer.
(C): Mixed fracture with a predominance of adhesive failure of ASB at 2-week aging.
(D): Higher magnification (2,000×).

patterns of the studied groups. more clinically relevant. Until now, the device is only
described in a technical paper12) and the present study is
DISCUSSION the first to establish its functionality. Future research
has to confirm the validity of the device, and it should
The present study investigated the influence of aging as be compared to other devices for cyclic loading on the
applied by a new mechanical loading device on adhesive market. However, a gold standard for mechanical aging
bond strength and the results demonstrate that the of restorations is not available, probably because of the
aging method results in a decreasing μTBS. Therefore, complicated nature of most devices.
the null-hypothesis was rejected. The new device used In this study, mechanical loading statistically
to apply cyclic mechanical loading, the “Rub&Roll”, influenced the microtensile bond strength values for all
is a relatively simple construction compared to other the aged conditions tested. It was observed that with
devices and has as a main advantage the high number of an increasing number of mechanical cycles, the µTBS
samples that can be subject to testing at once. Moreover, decreased significantly with 32% up to 63%, depending
the cylindrical construction enables to include liquids, on the number of cycles applied. Clinically, most bonded
such as erosive drinks and abrasive foodstuffs in the interfaces are subject to some degree of cyclic loading due
process. This opens a lot of opportunities for further to masticatory function and parafunctional habits, and
research investigating relations between cyclic loading this may vary with the size and position of the restoration
and wear aspects. Samples are loaded with compressive and individual risk of the patient14). It is difficult at this
force from the occlusal restoration in direction to the moment to establish which kind of cyclic loading protocol
adhesive interface. As the device operates, the force is the most clinically relevant. In the present study, 30 N
is not applied exactly perpendicularly to the adhesive of force was applied up to a frequency of 750,000 cycles.
interface during the whole cycle, which is probably A previous study suggested that 150,000 cycles at 60 N is
6 Dent Mater J 2016; : –

able to simulate six months of oral masticatory stresses5), and because of that, the µTBS values related to cohesive
which is five times less but at a higher force than applied fractures should be viewed cautiously or can even be
in the present study. Future research should establish discarded out of the statistical analyses as they do
which kind of cycling protocol could be considered as no represent true interfacial bond strength23,24). In
clinically representative, although increased number the present study, there was no statistical difference
of cycles is probably favorable for that purpose. Clinical between groups and the mode of fracture, as the
loading force will also show large individual variation, most prevalent fractures were apparently interfacial
and people with parafunctional habits will probably and mixed. This supports a study reporting that the
apply higher and more frequent forces to the tooth mode of fracture may also be associated with the kind
restoration complex. A small number of mechanical of gripping device25). The device used in this study
cycles may not be able to produce a significant decrease was a [Link]-BIOMAT jig, which is a modified
in bond strength6-8). Geraldeli’s microtensile testing jig26). The jig is designed
The number of pre-testing failures in the present to ensure that a pure tensile force is applied to the test
study confirmed the effect of the mechanical aging on specimen, but still bending forces may occur during load
the adhesive interface. A higher frequency of pre-testing application due to non-parallel specimen alignment, the
failures can be a predictor for diminished bond strength bonding surface being non-perpendicular to the specimen
values, which is in accordance with other studies15). gripping surface, and uneven gripping forces. The
However, in the present study this effect was not mixed failures in the present study were predominantly
statistically significant for the self-etch adhesive system adhesive ones, as fractures commonly started at the
that was more stable on the long term than the etch- borders, occurring from the corners through the center of
and-rinse type. the sticks-shaped samples, which were predicted by finite
Apart from mechanical loading, thermocycling and element analyses in this geometry of the sample27).
water storage can play a role in the aging process of
the tooth restoration interface resulting in a decreased CONCLUSION
bond strength after combined thermal and mechanical
loading15). This may be due to the degradation of the In conclusion, the new Rub&Roll device was able to
adhesive interface by combined hydrolytic deterioration promote mechanical loading on samples and an increased
of the resin polymer and the exposed collagen16). This number of load cycles resulted in decreased µTBS values.
degradation in the hybrid layer has also been described Moreover, differences between the materials occurred
after 6 months water storage17), also when no cyclic when a higher number of cycles were applied.
loading was applied18). In the present study, samples
were stored and loaded in water, but the time that the ACKNOWLEDGMENTS
samples remained in contact with water (1 up to 3 weeks)
is deemed too short to have a significant effect19). The first author would like to thank the Brazilian
It was observed that the number of load cycles founding agencies CAPES for the financial support and
plays a significant role in the decrease of adhesion. Both scholarships during the ‘Sandwich’ PhD. The authors of
adhesive systems showed a similar performance for the this manuscript certify that they have no proprietary,
control and 1 and 2 weeks aging groups, but for the 3 financial, or other personal interest of any nature or
weeks aging groups differences between the adhesive kind in any product, service, and/or company that is
systems were found, and the two-step self-etch adhesive- presented in this article.
CSE showed higher µTBS values and a more stable
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