Basic Research—Technology
Bonding over Dentin Replacement Materials
Naghmeh Meraji, DDS, MSc, DoIBoE,*
and Josette Camilleri, BChD, MPhil, PhD, FICD, FIMMM, FADM†
Abstract
Introduction: Dentin replacement materials are neces-
sary in large cavities to protect the pulp and reduce the
bulk of filling material. These materials are layered with
a composite resin restorative material. Microleakage
caused by poor bonding of composite resin to underlying
dentin replacement material will result in pulp damage.
The aim of this study was to characterize the interface
between dentin replacement materials and composite
resin and to measure the shear bond strength after
dynamic aging. Methods: Biodentine (Septodont, Saint
Maur-des-Fosses, France), Theracal LC (Bisco, Schaum-
burg, IL), and Fuji IX (GC, Tokyo, Japan) were used as
dentin replacement materials. They were then overlaid
with a total-etch and bonding agent or a self-etch primer
and composite resin or a glass ionomer cement. All com-
binations were thermocycled for 3000 cycles. The inter-
face was characterized using scanning electron
microscopy and elemental mapping. Furthermore, the
shear bond strength was assessed. Results: The Bio-
dentine surface was modified by etching. The Theracal
LC and Fuji IX microstructure was unchanged upon the
application of acid etch. The Biodentine and glass ion-
omer interface showed an evident wide open space,
and glass particles from the glass ionomer adhered to
the Biodentine surface. Elemental migration was shown
with aluminum, barium, fluorine, and ytterbium present
in Biodentine from the overlying composite resin. Cal-
cium was more stable. The bond strength between Ther-
acal LC and composite using a total-etch technique
followed by self-etch primer achieved the best bond
strength values. Biodentine exhibited the weakest
bond with complete failure of bonding shown after de-
molding and thermocycling. Conclusions:
Dynamic aging is necessary to have clinically valid data.
Bonding composite resin to water-based dentin replace-
ment materials is still challenging, and further alterna-
tives for restoration of teeth using such materials need
to be developed. (J Endod 2017;-:1–7)
From the *Department of Endodontics, School of Dentistry, Tehran University of Medical Sciences, Tehran, Iran; and †Department of Restorative Dentistry, Faculty of
Dental Surgery, University of Malta, Msida, Malta.
Address requests for reprints to Prof Josette Camilleri, Department of Restorative Dentistry, Faculty of Dental Surgery, University of Malta, Medical School, Mater Dei
Hospital, Msida - MSD 2090, Malta. E-mail address: josette.camilleri@um.edu.mt
0099-2399/$ - see front matter
Copyright ª 2017 American Association of Endodontists.
http://dx.doi.org/10.1016/j.joen.2017.03.025
JOE — Volume -, Number -, - 2017
Key Words
Biodentine, characterization, dentin replacement materials, dynamic testing, elemental
mapping, glass ionomer cement, shear bond strength, Theracal LC
P ulp capping materials
are used to protect the
pulp from thermal, chemical,
Significance
In vitro testing without the necessary aging may
have limited clinical significance because the
and other noxious stimuli.
material performance is not mimicked adequately.
Tricalcium silicate–based
materials such as mineral
trioxide aggregate (MTA) are commonly used for this purpose. MTA exhibits many dis-
advantages such as difficult handling, long setting time (1), induction of tooth discol-
oration (2–5), and incompatibility with other dental materials when layered (6, 7).
Second-generation tricalcium silicate–based materials exhibiting improved physical
properties were introduced in an attempt to overcome the disadvantages presented
by MTA.
Two such materials that are used as dentin replacement materials include Bio-
dentine (Septodont, Saint Maur-des-Fosses, France) and Theracal LC (Bisco, Schaum-
burg, IL). Both materials are tricalcium silicate based but are rather diverse.
Biodentine is a water-based cement presented as a powder in a capsule composed of
tricalcium silicate cement, zirconium oxide, and calcium carbonate. The liquid in the am-
pule is composed of water, calcium chloride, and a water-based polymer (8, 9).
Biodentine exhibits a short and clinically suitable setting time and was introduced as
an alternative to MTA to be used as dentin replacement material. On the other hand,
Theracal LC is a resin-modified light curable material used as a liner under composite
restorations. The cement component is Portland type, and it includes a radiopacifying
material and a silicon oxide additive in a resin matrix (10). Theracal LC does not include
water for material hydration, and thus it depends on the water taken up from the envi-
ronment and its diffusion within the material. The hydration of this material may be
compromised when compared with water-based materials such as Biodentine (8).
The manufacturer suggests placement of permanent restoration immediately after curing.
The bond strength between restorative and pulp capping materials is important for
the success of restorations (11). Etch-and-rinse adhesive systems exhibit stronger
bonding than self-etch adhesive systems (12). Bonding composite resins to novel dentin
replacement materials requires adequate research on the material interactions and inter-
facial characteristics. Etching of Biodentine has been shown to result in destruction of the
material microstructure and enhanced leakage through the Biodentine composite inter-
face (13). Furthermore, layering with composite resin has been investigated (14–19),
and Biodentine was shown to be weak. It has been suggested that the final restoration
with composite resin should be placed after at least 6 weeks using either a self-etch
or total-etch bonding system (18). Theracal LC had higher bond strength values than Bio-
dentine when layered with either composite or glass ionomer cement. The glass ionomer
Bonding over Dentin Replacement Materials 1
Basic Research—Technology
cement overlayering resulted in lower bond strengths than composite
resin. Composite resins applied with self-etching adhesives increased
the bond strength of Theracal LC. However, the application of etch-
and-rinse adhesives improved the adhesion of composite resins to Bio-
dentine (17). All the studies investigated interfaces of aged static systems,
and no characterization was performed.
The aim of the current study was to characterize and evaluate the ad-
equacy of different bonding systems to layer composite or glass ionomer
cement over 3 dentin replacement materials (Biodentine, Theracal LC,
and Fuji IX glass ionomer [GC, Tokyo, Japan]) using dynamic aging.
Materials and Methods
Three dentin replacement materials were used in this study:
Biodentine, Theracal LC, and Fuji IX. Mandibular molars extracted for peri-
odontal reasons were used in this study. Twenty-four teeth are selected to
enable 3 teeth per dentin replacement/restorative material combination.
The teeth were caries free and without restorations present. They were
checked under a stereomicroscope to make sure that there were no micro-
cracks visible. The roots were embedded in cold-cured epoxy resin
(EpoxyFix; Struers, Ballerup, Denmark) to avoid interaction of any fluids
seeping in from the apices through the root canal and into the pulp cham-
ber, thus affecting the materials. Occlusal cavities 6 mm  4 mm and 4 mm
deep. The pulpal floors were covered with Biodentine, Theracal LC, or Fuji
IX. Biodentine was mixed according to the manufacturer’s instructions,
was placed over the cavity floor, and was allowed to set for 15 minutes.
Theracal LC was syringed on the cavity floor and light cured for 20 seconds
at 600 mW/cm2 using an light-emitting diode light source. Fuji IX was
mixed according to the manufacturer’s instructions and placed over the
cavity floor without prior cavity conditioning. A 2-mm layer was placed
for each material, leaving a 2-mm cavity to be filled with restorative mate-
rial. The height was checked with a vernier caliper.
The adequacy of layering with composite using different adhesive
systems was assessed by using 2 different bonding systems.
1. Total etch and bond (Excite F; Ivoclar, Schaan, Lichtenstein) pre-
ceded by etching with 37% phosphoric acid for 30 seconds
2. Self-etch adhesive (AdheSe One F, Ivoclar)
The bonding systems were applied and cured for 10 seconds
according to the manufacturer’s instructions. After application of the
bonding system, the pulp capping materials were layered with light-
curing composite resin (Evetric, Ivoclar) for 20 seconds for each layer.
Furthermore, layering with a glass ionomer cement (Fuji IX) was also
performed. No material preparation was necessary when layering
with glass ionomer cement. The teeth were thermocycled for 3000 cy-
cles at 5 C and 55 C. The dwell time in each bath was 20 seconds, and
the transfer time between the 2 baths was 10 seconds following ISO
11405:2015 (20) instructions.
Scanning Electron Microscopy and Elemental Mapping
After thermocycling, the teeth were surface dried, sectioned longi-
tudinally, and polished with progressively finer grits of diamond discs
and abrasive solution (Tegramin 20; Struers, Ballerup, Denmark).
The specimens were then mounted on an aluminum stub, carbon
coated, and viewed under a scanning electron microscope (Zeiss
MERLIN Field Emission SEM; Carl Zeiss NTS GmbH, Oberkochen,
Germany). Scanning electron micrographs of the material interfaces
were captured at 1000 magnification; energy-dispersive spectroscopy
was performed followed by elemental mapping of the materials and the
interface, thus determining if elemental migration between the dentin
replacement material and the overlying composite occurred.
2 Meraji and Camilleri
Shear Bond Strength
Plexiglass blocks (n = 120) containing a central hole 4 mm in in-
ternal diameter and 2 mm in height were prepared by computer
numeric control (CNC) laser cutting (LaserProI; GCC, New Taipei
City, Taiwan) and filled with 1 of the dentin replacement materials eval-
uated in this study (ie, Biodentine, Theracal LC, or Fuji IX [n = 45
each]). Split plexiglass blocks with a central hole 2 mm in internal
diameter and 2 mm in height were also prepared with CNC laser cutting
and placed and fixed on the filled blocks in a way that the smaller 2-mm
diameter hole was positioned in the center of the 4-mm diameter hole
filled with dentin replacement materials. Then, the specimens of each
main experimental group were divided into 3 subgroups according
to the filling protocol used: Excite F total etch and bond preceded by
etching with 37% phosphoric acid, AdheSe One F self-etch adhesive,
and Fuji IX.
Subsequently, the split molds were removed, and specimens were
thermocycled as indicated previously. The specimens were tested for
shear bond strength using a universal testing machine (Z050; Zwick/
Roell, Ulm, Germany) with a chisel-edge plunger aimed at the dentin
replacement material/adhesive interface with a speed of 0.5 mm/min.
Shear bond strength in Nmm 2 was calculated by dividing the peak
load at failure by the specimen surface area. Failure modes were eval-
uated by a single operator under a stereomicroscope (Olympus SZ30;
Olympus, Tokyo, Japan) at 20 magnification and categorized into 1 of
3 types:
1. Adhesive: 100% adhesive failure between the dentin replacement
materials and the filling materials
2. Cohesive: 100% cohesive failure within the dentin replacement
materials or filling materials
3. Mixed: Mixed failure composed of adhesive and cohesive failure of
the dentin replacement materials or the filling materials. For this
category, a descriptive evaluation was also included.
Statistical Analyses
Data were evaluated using SPSS software (PASW Statistics 18; SPSS
Inc, Chicago, IL). Parametric tests performed as Kolmogorov-Smirnov
tests on the results indicated that the data were normally distributed.
Analysis of variance with P = .05 and the Tukey post hoc test were
used to perform multiple comparison tests.
Results
Scanning Electron Microscopy and Elemental Mapping
The scanning electron micrographs showing the material inter-
faces of each dentin replacement material are shown in Figure 1A.
Some cracks were visible in the materials, and this was not considered
as an important finding because the materials were subjected to vacuum
conditions.
Biodentine exhibited changes in the material microstructure,
particularly when etched. In the total-etch method, the materials were
well compacted together (Fig. 1A). With the self-etch adhesive, some
areas seemed to have separated. The glass ionomer became completely
dissociated from the Biodentine, leaving an uneven surface in
Biodentine. Theracal LC exhibited a more uniform interfacial region.
The materials contacted each other well. The same was observed for
the glass ionomer and composite combination. The self-etch adhesive
exhibited a better interface than the total-etch adhesive. The total-etch
adhesive resulted in pulling away of the glass ionomer from the compos-
ite surface with remnants of glass particles adhering to the composite at
the interface.
JOE — Volume -, Number -, - 2017
 Basic Research—Technology

Figure 1. (A) Backscattered scanning electron micrographs at 1000 magnification of the dentin replacement materials shown in the lower part of the micro-
graph layered with composite resin using either a total-etch bond technique or a self-etching primer or with no material preparation and layered with glass ionomer
cement. The restorative material is shown in the top part of the micrograph. (B) Elemental maps of aluminum, barium, fluorine, and ytterbium showing elemental
migration of the elements form composite in the top part of the map to the Biodentine in the lower part of the map.

JOE — Volume -, Number -, - 2017 Bonding over Dentin Replacement Materials 3

Basic Research—Technology

Figure 1. (continued).

The energy-dispersive spectroscopic images of the materials Aluminum, barium, fluorine, and ytterbium, which are the constit-
and the interface are shown in Supplemental Figure S1 uents of the composite, were all present in Biodentine (Fig. 1B). The
(Supplemental Fig. S1 is available online at www.jendodon.com) aluminum and fluorine present in Fuji IX also migrated to Biodentine.
and the list of elements present for each material in Table 1. These elements were present in the energy-dispersive spectroscopic
Once the presence of an element was known, it could be mapped. plots of the interface (Supplemental Fig. S1). The calcium was more sta-
The elemental maps for all the material combinations are shown ble, and only a minor band of calcium was present within the composite.
in Supplemental Figure S2(Supplemental Fig. S2 is available online The calcium migration in Fuji IX could not be mapped because both Fuji
at www.jendodon.com). The area devoid of any elements is the IX and Biodentine contained calcium.
bonding agent, which is composed of organic components that Material interactions between Theracal LC and the composite
were not mapped. The silicon was present in all the materials; could not be mapped because most of the elements present in Theracal
thus, the elemental exchange between the materials could not LC were also part of Evetric. Ytterbium was present in the Theracal LC
be mapped. The energy-dispersive spectroscopic analysis ex- material bulk. Calcium was once more stable and did not migrate in the
hibited a peak overlap between aluminum and ytterbium, phos- composite. The interaction between Evetric and Fuji IX showed migra-
phorus and zirconium, and silicon and strontium. Thus, these tion of barium and ytterbium from Evetric to Fuji IX.
interactions also could not be mapped. Carbon also was not
included in the maps because all the specimens were carbon
coated for electrical conductivity. Shear Bond Strength
The results of the shear bond strength of composite resin and glass
ionomer cement to underlying dentin replacement materials are shown
TABLE 1. Elemental Composition of the Materials Used in the Study in Figure 2. The composite resin with the self-etch primer was lost from
all the Biodentine samples during thermocycling. The glass ionomer
Elements Biodentine Theracal Fuji IX Evetric was dislodged from over the Biodentine and Theracal LC at the demold-
Al — O O O ing stage, showing the weakness of both bonds. The use of self-etch
Ba — O — O primers resulted in a weaker bond for Theracal LC (P = .036), but there
Ca O O O —
F — — O O
was no difference for Fuji IX (P = .803) compared with the total etch
P — — O — and bond technique. The Biodentine exhibited the weakest bond
Si O O O O strength even with the total etch and bond technique compared with
Sr — O O — the other materials under study (P < .001 and P < .012 for Theracal
Yb — — — O LC and Fuji IX, respectively). Layering with glass ionomer cement is
Zr O O — O
not recommended for all dentin replacement materials tested.

4 Meraji and Camilleri JOE — Volume -, Number -, - 2017


Figure 2. Shear bond strength results of composite resin and glass ionomer overlaid over 3 dentin replacement materials using 2 etching/priming methods of
bonding the composite resins (means  standard deviation).
The types of failures are shown in Table 2. The dominant mode of
failure in all evaluated subgroups was cohesive with the exception of
Theracal LC bonded to composite resin via self-etch adhesive, which
showed a dominant mixed mode of failure (Fig. 3).
Discussion
The current study investigated the effectiveness of different
methods of layering dentin replacement materials. Biodentine and
Theracal LC were selected because they are the materials most indicated
for this purpose because of their calcium-releasing ability, which is
beneficial to the dental pulp. Glass ionomer cement was used as a con-
trol because the sandwiching of composite resin to glass ionomer
cement is a standard technique in operative dentistry. Bonding systems
and composite resins were procured from the same company. None of
the dentin replacement materials has a recommended brand to be used
for the restoration of teeth. Two dentin bonding systems were used in
the current study. ExciTE F and AdheSe One F are light-curing,
fluoride-releasing, bonding systems. The latter is a self-etch adhesive
system, whereas the former is a single-component adhesive used in
conjunction with the total-etch technique. The use of fluoride-
containing and -releasing bonding systems has become popular
because of their ability to prevent postoperative sensitivity.
The tooth to material assembly for characterization and assess-
ment of bond strength was thermocycled using ISO specifications
(20). Thermocyling is an in vitro process in which specimens are
subjected to temperature limits similar to those experienced in the
oral cavity. This procedure can produce potential negative effects on
bonding because of dissimilar coefficients of thermal expansion
TABLE 2. Failure Modes in Different Experimental Groups
Biodentine
Mode of Glass ionomer
failure Total-etch Self-etch cement
A 0 — —
C 60% (9/15) — —
M 40% (4/15) — —
A, adhesive failure; C, cohesive failure; M, mixed failure.
JOE — Volume -, Number -, - 2017
Basic Research—Technology
between different restorative materials (21–23). Therefore, in the
current study, the specimens were thermocycled to evaluate the
adhesive efficacy in specimens under circumstances similar to that of
the oral cavity. This step has been omitted in previous studies
evaluating the bonding efficacy of restorative materials to Biodentine
and Theracal LC (14–19). The specimens were only aged and thus
not processed in conditions similar to the oral cavity like the
methodology used in the current study.
Plexiglass molds were fabricated by CNC laser cutting to achieve bet-
ter precision in the dimensions of the filling material in comparison with
cylindrically shaped plastic tubes used in previous studies (12, 17–19).
Furthermore, their split feature enables demolding with minimal force
transferred to the lining-filler interface.
Characterization of the interface and elemental mapping was
performed. Characterization is an important step in the research of
materials because one can investigate any changes happening to the
material during processing and testing. In a previous study, the layer-
ing of MTA with glass ionomer cements had been investigated, and the
glass ionomer was shown to interfere with the setting of the MTA. In
addition, elemental migration of strontium from the glass ionomer
and bismuth from MTA was shown (6). Biodentine, although also
water based and with a similar chemical composition to MTA, has a
shorter setting time and thus should be less affected by layering and
preparation procedures. Acid etching of Biodentine was shown to
lead to both structural and chemical changes to the material surface
(13), as shown also in the current study. The maps allow the location
of each element within the structure and have been used in previous
studies on interfacial characteristics of dental materials with tooth
structures (24–26).
Theracal LC Glass ionomer cement
Glass ionomer
Total-etch Self-etch cement Total-etch Self-etch
0 0 — 0 0
80% (12/15) 46.66% (7/15) — 73.3% (11/15) 60% (9/15)
20% (3/15) 53.33% (8/15) — 26.66% (4/15) 40% (6/15)
Bonding over Dentin Replacement Materials 5
Basic Research—Technology
Figure 3. Stereomicroscopic images of the failure modes in different experimental groups under 20 magnification. (A) Cohesive mode of failure in Biodentine–
total-etch. (B) Cohesive mode of failure in Theracal LC–total-etch. (C) Mixed mode of failure in Theracal LC–self-etch. (D) Cohesive mode of failure in glass
ionomer cement–self-etch. (E) Mixed mode of failure in glass ionomer cement–total-etch.
In addition to the changes in the microstructure of Biodentine after
etching and overlaying with composite, elemental migration of
aluminum, barium, ytterbium, and fluorine was shown. The effect that
these elements have on the chemistry of Biodentine is not known. The
migration of aluminum from Portland cement–based materials to the
plasma and liver of test animals has been reported (24). Aluminum
has detrimental effects on the human organs and has been implicated
in Parkinson disease (25). The migration of bismuth to the tooth struc-
ture causes tooth discoloration (26), and zinc from zinc oxide–based
restorative material impaired the setting of MTA (6). Elemental migration
and its effect on the adjacent structures need to be investigated further.
Calcium migration from one material to the other was shown to be min-
imal. The presumed migration of calcium from tricalcium silicate–based
materials to the adjacent tooth structure is the basis of bioactivity of these
materials and is implicated in increases in bond strength. The calcium-
rich zone formed in the tooth structure adjacent to Biodentine has been
termed the mineral infiltration zone (27). This calcium migration has
been discredited by other researchers (28, 29). In the current study,
the calcium was shown to be stable and not to migrate.
Overlaying both Biodentine and Theracal LC with glass ionomer
cement resulted in a very weak bond because all the specimens were
dislodged during the demolding stage. A weak bonding between these
dentin replacement materials and glass ionomer has been reported
(17). Thus, glass ionomer cement is not indicated for the restoration
of teeth in which Theracal LC and Biodentine are used as dentin replace-
ment materials. Thermocycling also resulted in the loss of the composite
using self-etch adhesive. Previous studies evaluating the bond strength
of composite to Biodentine omitted the thermocycling; thus, the data
obtained are questionable (15, 16, 18, 19).
6 Meraji and Camilleri
Biodentine exhibited the lowest shear bond strength when
compared with Theracal LC and GIC regardless of the bonding tech-
nique. This was predictable because of the resin-based composition
of Theracal LC and GIC. Previous studies also pointed out the lower
bond strength of Biodentine (15, 18). The dominant cohesive mode
of failure in Biodentine specimens may reflect a low cohesive
strength of the material itself (18).
The shear bond strength of all dentin replacement materials was
lower when self-etch adhesive was used, especially in Biodentine
specimens, which debonded during thermocycling in accordance to
a previous study (14). Conversely, other researchers found that the
placement of composite resin using self-etch adhesive systems over
Biodentine resulted in better shear bond strength (16). This difference
in the results can be caused by differences in the methodology between
the 2 studies such as thermocycling and the different brands of bonding
systems used.
Conclusions
Bonding composite resin to water-based dentin replacement ma-
terials is still unsuccessful, and further alternatives for the restoration of
teeth using such materials need to be developed. Dynamic aging of the
test specimens is necessary to mimic the oral environment.
Acknowledgments
Supported by ERDF (Malta) for the financing of the testing
equipment through the project ‘‘Developing an Interdisciplinary
Material Testing and Rapid Prototyping R&D Facility’’ (ref no. 012).
JOE — Volume -, Number -, - 2017

The authors thank Dr Gilles Richard and Mr Nicolas Gautier of
Septodont and Ms Sarah Peterson of Bisco for the materials and Ing
James Camilleri of the Department of Metallurgy and Materials
Engineering for his technical expertise.
The authors deny any conflicts of interest related to this study.
Supplementary Material
Supplementary material associated with this article can be
found in the online version at www.jendodon.com (http://dx.doi.
org/10.1016/j.joen.2017.03.025).
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