ARTICLE IN PRESS

Dental Materials (2004) xx, xxx–xxx

www.elsevier.com/locate/dental

Influence of c-factor and layering technique

on microtensile bond strength to dentin
Sergej A. Nikolaenko, Ulrich Lohbauer, Matthias Roggendorf,
Anselm Petschelt, Walter Dasch*, Roland Frankenberger

Policlinic for Operative Dentistry and Periodontology, University of Erlangen-Nuremberg,

Glueckstrasse 11, D-91054 Erlangen, Germany

Received 7 January 2003; received in revised form 22 July 2003; accepted 12 August 2003

KEYWORDS Summary Objective. Due to polymerisation shrinkage of resin-based composites, a

Dentin bonding; C-factor; high configuration factor in deep Class I cavities leads to a certain amount of stress
Resin composites; when the material is bonded. The aim of this in vitro study was to evaluate the
Flowable composites; influence of c-factor and different layering approaches on bonding to dentin with three
Filled adhesives different adhesive systems.
Materials and methods. Dentin bond strengths of Z250 bonded with OptiBond FL,
Single Bond, and One Up Bond F were measured on flattened dentin surfaces without
cavity walls and on the cavity floor of Class I cavities (10 layering concepts). The resin
composite increments were applied horizontally, vertically and obliquely, both with
and without a flowable liner. The tests were carried out in a microtensile apparatus at
a crosshead speed of 1 mm/min after 24 h of storage at 37 8C in water. Mean bond
strengths were analysed using the Wilcoxon test and multiple comparisons according
to the Mann– Whitney U-test. Specimens having failed prior to the bond strength test
were included as 0 MPa.
Results. The groups bonded on flat surfaces exhibited significantly higher bond
strengths than specimens cut from filled cavities. Within the cavity groups, OptiBond
FL and Single Bond exhibited no significant differences, however, being above One Up
Bond F. Within the groups of each adhesive, major differences between the layering
concepts were detectable. Bulk technique led to low dentin adhesion at the cavity
floor, above all for Single Bond and One Up Bond F. Horizontal layers resulted in
significantly higher bond strengths than did vertical or oblique. Lining with a flowable
composite did not promote bond strength for OptiBond FL. For the other adhesives, a
lining improved adhesion when vertical or oblique layers were applied, for horizontal
increments no effect was evident.
Conclusions. The c-factor is an influencing factor for dentin adhesion. However,
using an appropriate layering technique, high bond strengths to deep cavity floors can
be achieved.
Q 2003 Published by Elsevier Ltd on behalf of Academy of Dental Materials. All rights
reserved.

*Corresponding author. Tel.: þ 49-9131-8534208; fax: þ 49-

9131-8533603.

0109-5641/$ - see front matter Q 2003 Published by Elsevier Ltd on behalf of Academy of Dental Materials. All rights reserved.
doi:10.1016/j.dental.2003.08.001
 ARTICLE IN PRESS
2 S.A. Nikolaenko et al.

Introduction the negative potential of cavity geometries on

dentin bond strengths. 19,20,24 The c-factor is
In contrast to the situation in the 1980’s, tooth- defined as the quotient between bonded and
colored materials such as resin-based composites unbonded resin composite surface resulting in
are today the materials of choice for most of the higher values for deeper cavities and vice versa.5
dental patients instead of, e.g. amalgam.1 – 3 Due Armstrong et al. previously investigated micro-
to polymerisation shrinkage of these materials, tensile bond strength and failure characteristics in a
successful adhesion to enamel and dentin is an high/low c-factor design.24 A similar approach was
indispensable prerequisite for clinical success,4 – 6 published by Nikaido et al., having also reported
otherwise gap formation would endanger the that the presence of a high c-factor corroborates
clinical success. On the other hand, polymerisation dentin bond strength to the cavity floor.19,20
shrinkage stress is only present when shrinking However, several questions are not answered,
materials are bonded. above all the influence of different layering
Enamel bonding is meanwhile accepted as concepts as meticulously analysed by Lutz et al.29
clinically strong and durable, because acidic etch- Besides the influence of different c-factors, the
ants, such as 30 – 40% phosphoric acid, create effect of different adhesives on dentin bonding
enamel microporosities allowing the penetration performance is still not completely understood.
of monomers consecutively generating microme- Therefore the present study was additionally
carried out with different adhesive approaches,
chanical retention.2,7 In contrast, dentin is an
i.e. two-step etch and rinse, three-step etch and
unpredictable substrate for adhesion due to facts
rinse, and self-etch ‘all in one’.
like tubular structure, high organic content, and
Altogether, the goal of the present in vitro
intrinsic wetness.8 – 10
investigation was to evaluate the effect of different
To solve the problem, different approaches are
c-factors and incremental techniques and three
reported in the literature of the field. The two main
adhesives by using a microtensile bond strength test
approaches today are still adhesives with total
(m-TBS).
etching and adhesives with self-etching primers,
both delivered as all-in-one systems or with
different bottles. Etching with different acids and Materials and methods
subsequent penetration of reactive primer mol-
ecules into the more or less decalcified dentin Specimen preparation and microtensile
surface is recommended.11 – 14 While one-bottle testing
adhesives combine primer and bonding resin in
one solution, conventional two-bottle systems have A total of ninety-nine caries-free human third
a separate primer acting as penetration promotor molars were used in this investigation. The teeth
for the later applied bonding agent.2,15 were stored in 0.1% thymol solution at ambient
Polar solvents, like acetone or ethanol, are often temperature for less than four weeks after extrac-
used as both water chasers and carriers of the tion and were consecutively debrided and examined
monomers to form a tight contact with the exposed to ensure that they were free of defects.
collagen network.16,17 Hybridising adhesive systems For low-c-factor groups, the occlusal enamel was
were reported to generate high bond strengths to removed by slow-speed diamond-saw sectioning
dentin in several studies.18 – 23 (Isomet, Buehler, Lake Bluff, IL, USA) under profuse
Filled adhesives like OptiBond FL and OptiBond water cooling (Fig. 1). A standardised smear layer
Solo Plus (Kerr, Orange, CA, USA), and Permaquik was created on the surface by wet-sanding with
(Ultradent Products Inc., Salt Lake City, UT, USA) 600-grit sandpaper for 60 s.28
form thicker layers and were reported to enhance For high-c-factor groups, parallel 4 £ 4 £ 4 mm3
marginal and internal adaptation of resin composite occlusal cavities were cut using coarse diamond
restorations.10,15,16,24,25 This may be due to the fact burs under profuse water cooling (80 mm diamond
that an oxygen inhibition of the bonding agent is less bur, Two-Striper Prep-Set, Premier, St Paul, USA),
problematic in thicker adhesive layers. In contrast, and finished with a 25 mm finishing diamond. Inner
unfilled adhesives form thinner layers, which may angles of the cavities were prepared rectangularly.
not be polymerised due to oxygen inhibition.15 To guarantee a rectangular relation between the
The majority of studies dealing with dentin bond bonded interface and the direction of the later
strengths were carried out on flat bonding cut m-TBS beam, the cusps were flattened 2 mm
surfaces.13,15,18,21,26,27 Only few data regarding and then the cavity floor was prepared parallel to
different c-factors are available that indicate the flattened cusps (Fig. 1).
 ARTICLE IN PRESS
Influence of c-factor and layering technique on microtensile bond strength to dentin 3

Figure 1 Schematic overview of specimen preparation with low c-factor (upper half) and high c-factor (lower half).

Thirty-three teeth were randomly assigned to one The intensity of the light was checked period-
of three dentin adhesives. The teeth were further- ically with a radiometer (Demetron/Kerr, Danbury,
more subdivided into eleven groups with c-factors CT, USA) to ensure that an intensity of 400 mW/cm2
of , 0.2 and , 4.0. The surfaces were treated with was always exceeded.
the adhesive systems OptiBond FL (Kerr), Single The peripheral areas of the reconstructed/filled
Bond (3M ESPE, St. Paul, MN, USA) and One Up Bond teeth were removed resulting in a 4 £ 4 mm2 square
F (Tokoyama, Tokyo, Japan) according to the manu- central area. The remaining specimen was sec-
facturers’ instructions (Table 1). tioned into four slices, which were sectioned again
The crowns of the flattened teeth were then to receive 20 resin – dentin beams.15,27 The saw was
reconstructed with four 1 mm-layers of a hybrid adjusted to steps of 1 mm, due to the thickness of
resin composite (Z250) each layer being light-cured the blade (300 mm) resulting in sticks with a cross-
for 40 s with a Translux CL curing unit (Heraeus – sectional area of 700 £ 700 mm2 (0.5 mm2). From
Kulzer, Dormagen, Germany). the resulting 60 central sticks of each group, 20
The Class I cavities were filled in 10 different were selected ðn ¼ 20Þ: These 20 sticks had to have
ways as shown in Fig. 2. In the groups with a lining, a a remaining dentin thickness to the pulp of
0.5 mm thin layer of flowable resin composite 2.0 ^ 0.5 mm.
(Filtek Flow) was brushed onto the cavity walls If more than 20 beams were collected with the
and floor and light-cured for 40 s. correct remaining dentin thickness, 20 sticks were

Table 1 Investigated adhesive systems, chemical compositions, and manufacturers.

Adhesive system Code Etchant Primer Bonding resin Manufacturer

OptiBond FL OP Etchant 37.5% Primer HEMA, GPDM, Adhesive bisGMA, HEMA, Kerr Orange CA,
phosphoric acid MMEP, ethanol, water, GPDM, barium–aluminum USA
initiators borosilicate glass,
disodium hexa-fluoro-silicate,
fumed silica
Single Bond SB Etchant 36% Primer þ adhesive 3M ESPE, St Paul MN, USA
phosphoric acid bisGMA, HEMA,
dimethacrylates,
polyalkenoic acid
copolymer, initiator,
3–8% water, ethanol
One Up Bond F OF Mixed all-in-one Tokoyama Tokyo
adhesive Mac-10, Japan
phosphate monomer,
MMA, bis-MPEPP,
HEMA, FASG
 ARTICLE IN PRESS
4 S.A. Nikolaenko et al.

Figure 2 Layering concepts for the high c-factor groups.

randomly selected. For the case that one or more of Bond strengths on flat surfaces were 47 MPa for
the selected sticks failed due to the sectioning OP, 46 MPa for SB, and 23 MPa for OF (Table 2) being
process, the percentage of prematurely failed statistically lower than OP and SB (p , 0:05; Mann –
specimens in relation to the total number of Whitney U-test).
selected specimens was recorded. The same (or The bond strengths in Class I cavities showed
approximated) percentage of the 20 final specimens groups being lowered by pre-test failures having
received 0 MPa as final m-TBS result. been included as 0 MPa. For the bulk fill tech-
The m-TBS beams were stored in distilled water nique, OP and SB showed significantly higher
for 24 h at 37 8C. values than OF (p , 0:05; Mann – Whitney U-test).
The sticks were mounted in a Zwick jaw device Applying horizontal layers exhibited bond strength
(Zwick, Ulm, Germany) with a special cyanoacry- as a function of the number of increments
late glue (Zapit, Dental Ventures of America, (Table 3). OP and SB had a similar performance
Corona, CA, USA) and tested using an universal with , 15 MPa for two horizontal layers and
testing machine model 4411 (Zwick, Ulm, Germany) , 30 MPa for four increments, being significantly
with a 50 N load cell traveling at a crosshead higher (p , 0:05; Wilcoxon test). The use of a
speed of 1 mm/min. m-TBS was determined by flowable composite as lining was not beneficial for
computing the quotient of maximum load (N) and bond strengths in the groups with horizontal
adhesion area. layering.
The groups with vertically applied layers showed
Statistical analysis worse results compared to the other layering
techniques (Table 3). In these groups, bond
The statistical analysis was performed using SPSS strengths were improved for SB and OF when a
10.0 for Windows (SPSS Inc., Chicago, IL, USA). The flowable was utilised (p , 0:05; Mann – Whitney U-
values were non-normally distributed (Kolmogorov – test). For SB and OF, the number of PTFs was quite
Smirnov test), therefore non-parametric tests were high with vertical layering, e.g. 60% when OF was
used to compute differences between dependent used with two vertical increments.
groups (Wilcoxon matched-pairs signed-ranks test)
and among independent groups (Mann – Whitney U-
test, correction method according to Bonferroni – Table 2 Results of dentin microtensile bond strength on flat
Holm) for pairwise comparisons at the 0.05 level of surfaces. Same superscript letter indicates no statistical
difference (p , 0:05; Mann –Whitney U-test).
significance.
m-TBS to flattened dentin (MPa) (SD)

Results OP 47.2 (14.8)A

SB 45.8 (17.4)A
An overview of the results is shown in Tables 2 OF 23.2 (15.1)B
and 3.
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Influence of c-factor and layering technique on microtensile bond strength to dentin 5

Table 3 Results of dentin microtensile bond strength to the cavity floor of deep Class I cavities.

m-TBS to floors of Class I cavities (MPa) (SD)

Bulk Horizontal layers Vertical layers Oblique layers

2 4 4a 2 4 4a 2 4 4a

OP 11.8BC 16.0B 31.6A 30.2A 15.7B 18.1B 19.4B 17.6B 16.9B 19.8B
(8.8) (5.6) (8.2) (8.4) (6.7) (6.9) (8.1) (12.0) (10.6) (7.7)
PTF (%) 15 0 0 0 0 0 0 25 10 0

SB 8.7C 12.7BC 29.9A 30.5A 8.6C 9.8C 18.8B 10.7BC 15.6B 19.5B
(10.9) (13.5) (8.1) (10.2) (12.3) (14.0) (8.0) (12.7) (15.9) (10.0)
PTF (%) 55 45 0 0 55 60 0 55 45 5
OF 5.0D 14.8BC 16.9B 17.6B 7.0C 12.4BC 18.9B 6.5CD 12.4BC 15.5B
(11.3) (14.9) (15.4) (14.2) (10.0) (15.0) (11.2) (10.8) (14.6) (13.2)
PTF (%) 80 45 45 25 60 50 15 70 50 20
a
With lining. PTF: Pre-test failures (%) for each group. Same superscript letter indicates no statistical difference (p , 0:05; within
materials: Wilcoxon test; between materials: Mann–Whitney U-test).

For the groups layered obliquely, a tendency was investigation. This confirms the findings of other
found in favor of the flowable lining method, how- studies dealing with microtensile testing.21,28
ever, not being statistically significant ðp . 0:05Þ: Shono et al. reported in recent investigations
using the m-TBS methodology, that bonding to
flattened dentin surfaces exhibits differences at
Discussion variable distances from the pulp, potentially
resulting in regional dentin bond strength differ-
The objective of this in vitro study was to clarify the
ences.22 Therefore, only the very central areas of
influence of three adhesives and layering tech-
the specimens were used to obtain a reliable
niques on bond strength to dentin when different
randomisation of test specimens like in previous
configuration factors were present. The c-factors
studies.15,27
given by the cut flattened surfaces and the cavities
According to the suggestion of Pashley et al.,
do not automatically determine the really existing
statistics have been carried out with n ¼ 20 as
individual c-factors of each applied increment of
number of specimens under investigation per
resin composite. On the other hand, the crucial first
experimental group.21
layer of resin composite exhibited similar c-factors
Several studies excluded specimens that failed
in the cavity groups which did not result in similar
bond strengths. during the sectioning process. This may be wrong,
The method utilised for bond strength testing because there may have been a certain amount of
was the microtensile bond test reported to be well- force to produce the failure during sectioning, so
suited for the evaluation of bond strengths to one could estimate this individual force as more
enamel and dentin.22,23,26 This methodology gives than 0 MPa. Another approach is to count the
the opportunity to investigate interfacial bond individual number of so-called pre-test failures
strengths on small areas below 1 mm2. Macro (PTF).32 This definitively is an honest way to
shear and tensile bonding procedures work with qualitatively describe some deficiencies. However,
larger bonding areas with diameters of up to when e.g. in the case of a weaker adhesive 50% of
5 mm.26,30,31 When dentin is used as a bonding the beams of one tooth cannot be tested due to
substrate to evaluate adhesive systems reaching early failure during the machining process, the
critical bond strengths over , 15 MPa, shear and other 50% of specimens may not really represent a
tensile procedures tend to produce non-uniform realistic bond strength image of the adhesive
stresses during the debonding process resulting in potential of the particular adhesive tested.
cohesive fractures in dentin.30,31 However, cohe- Early failures during specimen sectioning have
sive fractures in dentin do not represent the been frequently observed especially in deep cav-
clinically relevant failure mechanism in real ities during the present study. Therefore, the
cavities. This particular problem can be prevented authors decided to analyse differently in compari-
with microtensile testing because the predominant son to previous studies resulting in lower bond
failure is also adhesive during the present strength values. Furthermore this illustrates that
 ARTICLE IN PRESS
6 S.A. Nikolaenko et al.

some problems in deep cavities may arise from a significant differences in bond strengths to the
clinical point of view. So the inclusion of 0 MPa- cavity floor when different incremental techniques
specimens had a strong influence on the results of are applied in deep Class I cavities.
the present study: Placing the composite in bulk Comparing the different layering concepts, it
resulted in 5 MPa according to the protocol of this was shown as crucial, where the first increment is
study, however, conventional statistical analyses bonded. Only when the first increment has been
would have revealed 25 MPa. A more detailed view bonded to the cavity floor, acceptable bond
is given in Table 3 displaying the influence of strengths and percentages of 0 MPa-specimens
different percentages of prematurely failed speci- were observed (Table 3). The vertically and
mens in different groups under investigation. obliquely layered fillings frequently exhibited
For an additional fatigue simulation, chewing almost no adhesion of the restorative to the cavity
simulation of the involved specimens would have floor. This may have contributed to the fact that a
been possible19,20 to further stress the bonded joint tight adaptation with a plugger can be achieved
between resin and dentin. This could be the goal of more easily in a horizontal than a strictly vertical
further investigations for more optimisation of the way, potentially leading to voids within the stressed
layering concept. Also long-term storage space interface.
could affect the results.23,32 However, the present With the different adhesives used in the present
study showed, e.g. a 45% PTF rate for OF with two investigation, a clear advantage for OptiBond FL and
horizontal layers which is already poor and alarming Single Bond is evident from the bond strength results.
without additional fatigue or long-term storage In the OP groups even with vertical and oblique
approaches to obtain evidence about resin –dentin layering acceptable bond strengths combined with
bonding of contemporary adhesive systems. few 0 MPa-specimens resulted in the cavity tests.
An important point for dentin bond strengths is Single Bond and One Up Bond F performed worse than
the individually formed thickness of the bonding did OF when few layers were applied into the Class I
agent.15,33,34 The thicker adhesive layers in the cavities. Furthermore, it would be interesting to
OptiBond FL control groups may have contributed learn how the applied layering concepts influence
to slightly higher dentin bond strengths. However, dentin adhesion to the vertical cavity walls. This is
there was no statistical difference to Single Bond. the aim of further studies.
This observation is reflected by the work of Compared to the results of Nikaido et al.,20 SB
Armstrong et al., not having found differences in revealed higher values for m-TBS. Nikaido et al.
cavities for OptiBond FL and an unfilled experimen- found overwet zones responsible for the poor
tal version of OptiBond FL also tending to reject the performance of SB concluding this particular
elastic cavity wall theory.24 adhesive to be technique-sensitive. According to
On the other hand, Choi et al. reported that findings from a previous study,27 the intrinsic
thicker layers of an adhesive providing a low moisture in SB seems to be sufficient to avoid too
modulus of elasticity are capable of reducing the much water left in the cavity. On one hand this
interfacially acting polymerisation stress of resin confirms the terminus technique sensitivity, on the
composites.35 When Class I cavities are involved, other hand the results are not comparable with the
not only the c-factor but also the characteristics of present investigation, because 0 MPa-specimens
deep dentin as adhesion substrate may contribute were not excluded.
to lower bond strengths.36,37 Altogether, SB and OP revealed better overall
The use of lining materials providing a lower dentin bonding performance than the simplified
modulus of elasticity may result in inhomogeneous bonding agent OF. A solely self-etching system may
stress distribution near the bonded interface.38 provide less technique sensitivity due to the absence
It is a well-known fact from the literature that a of total etch/wet bonding requirements, however,
high c-factor is a risk factor for bonding because the more old-fashioned adhesive systems OP and SB
polymerisation stresses may be enlarged. Feilzer produced more promising results overall.
et al. showed that under simulated clinical circum-
stances the resulting stress may be too high to be
counteracted by dentin bonding.39 Conclusions
On the other hand, bulk application may not
allow sufficient light polymerisation of the solely † The presence of a high c-factor is a risk for
light-curing materials. Therefore layering concepts debonding within the resin – dentin interface.
have been described as mandatory when working † For deep Class I cavities, horizontal layering is
with resin-based composites. The different results the most promising way to get a good bond to the
displayed in Table 3 demonstrate that there are cavity floor.
 ARTICLE IN PRESS
Influence of c-factor and layering technique on microtensile bond strength to dentin 7

† Using four horizontal increments, OptiBond FL thermal cycling and mechanical loading on bond strength of
and Single Bond achieved higher bond strengths a self-etching primer system to dentin. Dent Mater 2002;18:
269—75.
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† For Single Bond and One Up Bond F, lining with a Cox CF, Hickel R, Tagami J. The in vitro dentin bond
flowable composite improved bond strengths strengths of two adhesive systems in class I cavities of human
when vertical layers are applied. molars. J Adhes Dent 2002;4:31—9.
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Shono Y, Fernandes CA, Tay F. The microtensile bond test. A
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