Dental Materials Journal 2016; 35(6): 881–887

Shear bond strength of a novel light cured calcium silicate based-cement to

resin composite using different adhesive systems
Hanan ALZRAIKAT1, Nessrin A. TAHA1, Deema QASRAWI1 and Michael F. BURROW2

1
Department of Conservative Dentistry, Jordan University of Science and Technology, P.O.Box 3030, Irbid 22110, Jordan
2
Chair of Biomaterials, Melbourne Dental School, The University of Melbourne, 720 Swanston Street, Victoria 3010, Australia
Corresponding author, Hanan ALZRAIKAT; E-mail: hjsa@just.edu.jo

The shear bond strength (SBS) of TheraCal LC to resin composite was evaluated in comparison to Mineral trioxide aggregate
(ProRoot MTA) and conventional glass ionomer cement (GIC) using two adhesive systems. A hole was prepared in 90 acrylic blocks
(6 mm diameter, 2 mm deep) then filled with TheraCal LC, MTA or Fuji IX (n=30/group). Each group was bonded with either an etch
and rinse or 1-step self-etch adhesive. Filtek Z250 composite was bonded to each capping material. Bond strength was tested in a
universal testing machine, and data were analyzed using 2-way ANOVA and Duncan’s Multiple range test (p<0.05). TheraCal LC
displayed the highest SBS (p<0.001). MTA bonded with the 1-step self-etch adhesive showed the lowest SBS (p<0.001), while SBS
of TheraCal LC and Fuji IX did not differ between either adhesive (p>0.05). TheraCal LC is the preferred choice in pulp capping
procedures when using resin composite restorations.

Keywords: TheraCal LC, MTA, Shear bond strength, Resin composite

of MTA, a recently introduced material, TheraCal LC

INTRODUCTION
In recent years, considerable attention has been directed
towards vital pulp therapy (VPT) in dentistry1). Vital
pulp therapy aims to preserve the vitality and health of
the dental pulp following carious exposure or traumatic
injury2). In permanent adult teeth, several procedures
have been described in order to preserve pulp vitality
which include ‘controlled’ excavation of deep caries
aiming to avoid pulp exposure followed by using
biomaterials as a protective layer (indirect pulp
capping)3), the use of biomaterials as a dressing over
the exposed pulp tissue in direct pulp capping, or using
the same biomaterials in pulpotomy procedures which
involve partial amputation of the dental pulp2,4-5).
Biomaterials that are advocated for use in VPT
procedures should possess certain characteristics such
as biocompatibility, the ability to maintain pulp vitality,
adhere to dentine and the restorative material, and
also to resist forces during restoration placement and
function6). Mineral trioxide aggregate has been used
for this purpose due to its numerous advantages such
as biocompatibility7,8), low solubility9), prevention of
bacterial leakage10), and its ability to release calcium
hydroxide11). However, it has certain shortcomings such
as difficulty in handling and a long setting time which
might lead to leakage, and loss of marginal adaptation12).
Furthermore, since MTA requires moisture for complete
setting, it is advocated to place a wet cotton pellet
over MTA after its application13), this will necessitate
additional appointments until the permanent restorative
material can be used to restore the treated tooth.
In order to overcome the reported short comings
Color figures can be viewed in the online issue, which is avail-
able at J-STAGE.
Received Feb 25, 2016: Accepted Jun 29, 2016
doi:10.4012/dmj.2016-075 JOI JST.JSTAGE/dmj/2016-075
(Bisco, Schamurg, IL, USA), has been developed. This
new material is marketed as a light-curable resin-
modified calcium silicate based MTA designed for direct
and indirect pulp capping procedures. TheraCal LC
contains approximately 45% Portland Cement (PC), 10%
radiopaque component (bismuth oxide), 5% hydrophilic
thickening agent (fumed silica), and approximately 40%
resin, by weight14). This new material has been reported
to have a shorter setting time, lower solubility and
higher flowability compared with conventional MTA14).
Glass ionomer cements have been used as liners,
particularly under resin composites, because of their
ability to chemically bond to enamel and dentin in
addition to their ability to release fluoride15). They are
also used as liners in indirect pulp capping procedures
with similar clinical efficacy to contemporary pulp
capping materials16).
The bond strength of restorative materials to pulp
capping agents has been an issue of concern, since
placement of a restoration following VPT procedures is
crucial to ensure their success17). In spite of the massive
advances in adhesive technology over the past decades,
the bonded interface to tooth structure remains the weak
point of an adhesive restoration18). The most commonly
used test to assess bond strength is the macro-shear
test which has gained popularity as a simple and
quick method. Moreover, it is a very popular test that
is commonly used to screen new adhesive formulations
on their bonding effectiveness19). Standardization of the
test protocol has been attempted by preparing specific
jigs such as the SDI rig (SDI, Bayswater, Victoria,
Australia) (Fig. 1a)19), which is used to aid in proper
adaptation and stabilization of the restorative material
to the bonded substrate.
882 Dent Mater J 2016; 35(6): 881–887
Fig. 1 Preparation of the samples and experiment set up used in the study: a) Shear bond
strength rig with the bonded specimen, b) Schematic illustration of the shear bond
strength test setup.
Several studies investigated SBS of restorative
materials including resin composite and GICs to various
pulp capping materials using several types of adhesive
systems17,20-23), however information regarding the bond
strength between resin composite and TheraCal LC
remains limited. Therefore the aim of the present study
was to compare SBS of TheraCal LC to resin composite
with that of MTA and a conventional GIC using two
bonding systems (i.e. etch and rinse system and 1-step
self-etch adhesive system). The null hypothesis tested
was that SBS of TheraCal LC to resin composite is
superior to that of MTA regardless of the adhesive
system used.
MATERIALS AND METHODS
The materials used in the current study, their
composition, mode of application and manufacturer
details are shown in Table 1.
Specimen preparation
A total of 90 acrylic blocks (2 cm high×2 cm wide)
containing a central hole 6 mm diameter and 2 mm deep
were prepared using cold cure acrylic resin material
(Metocryl, Metrodent, West Yorkshire, UK). Thirty
blocks were filled with either TheraCal LC, MTA,
or Fuji IX. TheraCal LC was inserted into each block
(n=30) in two increments of 1 mm using a syringe-tip,
then the cement’s surface was flattened using a metal
spatula then polymerized with a light emitting diode
light curing unit for 20 s (LED.B, Guilin Woodpecker
Medical Instrument, Guiln, Guangxi, China) with an
intensity of 1,200-mW cm2. ProRoot MTA, the powder
and liquid were mixed according to the manufacturer’s
instructions, and placed in the acrylic blocks using a
spatula and pressed flat with a glass slab. The MTA
samples were covered with a damp cotton pellet and
stored in an incubator at 100% humidity and 37°C for 48
h to allow complete setting.
For the GIC, Fuji IX capsules were mixed according
to manufacturer instructions, then extruded into the
acrylic blocks. The GIC surface of each sample was
flattened using a metal spatula. TheraCal LC and Fuji
IX samples were stored at 37o C in 100% humidity for 24
h prior to the bonding procedure.
Restorative material placement
TheraCal LC, MTA and GIC groups were divided into
two subgroups (n=15) according to the adhesive system
used to bond the resin composite (Table 1). Following
application of the adhesive system, each acrylic
specimen was placed into a shear bond apparatus (SDI
Shear Bond Strength Rig, SDI Limited, Bayswater) (Fig.
1a) to ensure stability of the sample during the bonding
procedure of resin composite to the capping materials.
A cylindrical stainless steel mold with an internal
diameter of 3.5 mm and height of 5.00 mm was placed
centrally over the bonding site of each capping material
in the acrylic specimen. The mold was filled with resin
composite in two layers of 2 mm each and each layer was
light-cured for 30 s. After polymerization, each bonded
assembly was removed from the jig then placed into a
container filled with distilled water for 24 h at 100%
relative humidity and 37° C before SBS testing.
Shear bond strength test
Shear bond strength was measured by mounting the
specimens in a universal testing machine (Computer
control electromechanical universal testing machine
model WDW-20, Jinan Chenda Tesing Machine
Manufacturing, China) and subjecting them to shearing
force at a crosshead speed of 1.0 mm/min using a 0.5
mm wide chisel (Fig. 1b). Shear bond strength was
calculated and expressed in MPa by dividing the peak
load at failure to the specimen surface area according to
the formula: SBS (MPa)=Load (N)/Area πr2 (mm2).
Fracture analysis
Following the SBS test, the fractured surfaces were
examined under a stereomicroscope (Stereomicroscope
model XTX-W5C, Proway Optics and Electronics,
Ningbo, China) at 20× magnification. The failure mode
was classified as follows: (1) adhesive failure, failure
at the capping material/resin composite interface, (2)
cohesive failure, failure within the capping material or
resin composite, and (3) mixed failure, a combination of
 Dent Mater J 2016; 35(6): 881–887 883

Table 1 Materials used in the study, composition, mode of application and manufacturer information

Material Manufacturer Composition Mode/Steps of application

AeroSil 8.0%, biocompatible hydrophilic

resin 42.5% (Bis-GMA 20%,
BISCO Dental
biocompatible resin-FDA 77.25%, 1. Apply in incremental layers.
TheraCalTM Products,
modifying agent 2.4%; initiating agent (Layer is not to exceed 1 mm in depth)
LC® Schaumburg,
0.32%, stabilizer for the initiating 2. Light cure each increment for 20 s.
IL, USA
agent 0.032%), active ingredients in
MTA 44.5%, and barium sulfate 5%

ProRoot®
Dentsply Tricalcium silicate, bismuth oxide,
Mineral
Tulsa Dental, dicalcium silicate, tricalcium aluminate, Mix powder/liquid ratio: 1/3.
Trioxide
OK, USA calcium sulfate dehydrate or gypsum
Aggregates

Powder:Alumino-fluorosilicate glass. 1. Shake the capsule then push the plunger.

GC FujiTM GC, Tokyo,
Liquid: Polyacrylic acid, polybasic 2. Mix for 10 s in amalgamator.
IX GP® Japan
carboxylic acid, water. 3. Load the capsule into applier and apply.

ScotchbondTM Etchant: 37% H3PO4 1. Apply 35% phosphoric acid etchant 15 s.

Adper TM
3M ESPE, Adhesive: dimethacrylates, HEMA, 2. Rinse and dry with paper points.
Single St. Paul, colloidal silica, polyalkenoid acid 3. Apply 2 coats of adhesive.
bond 2 IL, USA copolymer, ethanol, water, 4. Gentle air stream.
photoinitiator 5. Light-polymerize 10 s.

1. Dry surface.
Bifunctional acrylate, acidic acrylate,
2. Apply adhesive.
Dentsply functionalized phosphoric acid ester,
Xeno® V+ 3. Agitate for 20s.
Tulsa Dental water, tertiary butanol, initiator,
4. Gentle air stream.
stabilizer.
5. Light-polymerize 10 s.

Filtek™ Z250
Universal Zirconia/silica filler, UDMA,
3M ESPE Light cure for 30 s.
Restorative Bis-GMA and Bis-EMA resins.
System

adhesive and cohesive failure.
Statistical analysis
Statistical analysis was done using commercially
available software (SPSS 10.0, SPSS, Chicago, IL,
USA). Means and standard deviation of the SBS of
resin composite to each pulp capping material using the
bonding systems was calculated. Two-way ANOVA was
used to determine the effect of the adhesive systems,
the materials and the cumulative effect of these two
factors on SBS. Post hoc comparisons were carried out
using the Duncan’s multiple range test (p<0.05). The
assumption of normality was established using Leven’s
test of homogeneity.
RESULTS
Analysis of data with two-way ANOVA demonstrated a
statistically significant effect of the capping material as
a factor on SBS to resin composite (p<0.05); however,
there was no significant influence of the adhesive
system on the SBS (p=0.886). Comparison of means,
standard deviations and statistical analysis of the SBS
among the tested groups is presented in Table 2. The
TheraCal LC groups displayed the highest SBS values to
resin composite using both adhesive systems compared
with MTA and Fuji IX (p<0.05). The SBS of MTA to
composite was the lowest among all tested groups, with
the lowest value reported using the 1-step self-etch
adhesive system. There was no significant difference in
SBS of TheraCal LC to resin composite between the two
adhesive systems; similarly, GIC had comparable values
of SBS regardless of the adhesive system used.
A summary of fracture patterns is given in Table 3.
Representative stereomicroscopic photo images of the
failure modes are shown in Fig. 2. In the TheraCal LC
group equal numbers of mixed and cohesive in composite
failure modes were observed when using the etch and
rinse adhesive system, failure modes in the 1-step self-
etch adhesive system group were mostly mixed (Fig.
2b). In the MTA group, failure was mostly adhesive
particularly for the1-step self-etch adhesive system
(Fig. 2c). GIC displayed similar fracture patterns for
both adhesive systems with the samples failing mostly
cohesively within the GIC (Fig. 2d).
884 Dent Mater J 2016; 35(6): 881–887

Table 2 Mean values and standard deviation (SD) of SBS (MPa) of tested material to resin composite using two adhesive
systems

Bonding System

Capping Material Etch and rinse system (Group 1) 1-step self-etch system (Group 2)

Mean (SD) Mean (SD)

TheraCal LC 12.84 (1.56) ab

14.78 (3.51)a

MTA 7.50 (2.22)d 4.61 (2.56)e

Fuji IX 9.88 (3.82)c 11.08 (2.58)bc

Means within the table with different superscripts differ significantly (p<0.05)
a,b,c,d

*p-Value of ANOVA test of these means was <0.001

Table 3 Fracture modes of the tested materials after the shear bond test

Bonding system

Mode of failure Etch and rinse system 1-step self-etch system

TheraCal LC MTA Fuji IX TheraCal LC MTA Fuji IX

Adhesive 0 9 2 2 14 1

Mixed 7 0 3 7 0 2

Cohesive in composite 7 0 0 2 0 0

Cohesive in capping material 1 6 10 4 1 12

Fig. 2 Images of fractured samples showing: a) Cohesive
failure in resin composite bonded to TheraCal
LC. b) Mixed failure of resin composite bonded to
TheraCal LC (R: resin composite, T: TheraCal LC).
c) Adhesive failure in MTA groups. d) Cohesive
failure within GIC in Fuji IX group.
DISCUSSION
Over the years, MTA has been increasingly used in
various clinical procedures in general dentistry such
as furcation repair, root resorption and pulp capping
procedures in primary and permanent teeth24). In
recent years new materials such as the light cured
MTA-like material (TheraCal LC) have been produced
to overcome the difficulties in handling as well as the
long setting time of conventional MTA14). In addition to
biocompatibility and bioactivity of pulp capping
materials, their bond strength to restorative materials
is important for the quality of fillings and success of
restorations since good bonding produces an adhesive
joint that is capable of spreading stress relatively evenly
over the region of the lining-filling interface17) which
will aid tolerating stresses created by polymerization
shrinkage of overlying resin composite restorations.
The null hypothesis postulated in the current study
was accepted. Regardless of the adhesive system used
in the current study, TheraCal LC produced the highest
SBS to resin composite with the self-etch adhesive
showing higher bond strengths than the etch and rinse
system, although this was not statistically significant.
Similar trends were observed with the GIC while MTA
displayed the opposite result.
Cantekin25) investigated the bond strength of
TheraCal LC and ProRoot MTA to resin composite using
 Dent Mater J 2016; 35(6): 881–887
a 2-step etch and rinse adhesive, and also a Silorane-
based composite. The highest SBS values were in the
TheraCal LC group when bonded to the resin composite
(19.3 MPa). In the current study similar trends were
observed with the TheraCal LC group despite a lower
SBS value (12.84 MPa). The difference in SBS may
be related to the different adhesive system and resin
composite material used which have been reported as
significant factors that may influence bond strength19).
The higher evaporation pressure of acetone present in
2-step etch and rinse system used by Cantekin compared
with ethanol solvent present in Single Bond 2 adhesive
may have resulted in greater monomer infiltration and
thus creating higher bond strengths26). In addition, the
bond area in the current study (3.5 mm diameter) was
greater than that used by Cantekin (2 mm diameter).
It is well established that the larger the bonded area
will produce lower SBS values27), due to the increased
probability of the presence of critical sized defects28).
The higher SBS value of TheraCal LC compared
with MTA and Fuji IX may be due in part to the resin
content in TheraCal LC; which provides a chemical bond
with the composite. Moreover, TheraCal LC contains a
hydrophilic resin monomer that makes it an excellent
adhesion promoter enhancing bond strength26,29,30). On
the other hand, the lack of resin content in MTA and
conventional GIC indicates that their bond to resin
composite is purely micromechanical31).
Several studies evaluated SBS of resin composite to
MTA compared with several pulp capping biomaterials
bonded using different adhesive systems20,21,23,32-34)
with variable results. Tunc et al.23) evaluated the bond
strength of White MTA (WMTA) to a resin composite
and a compomer using an etch and rinse system
(Adaper™ Single Bond, 3M ESPE) and a 1-step self-etch
adhesive system (Prompt L-Pop, 3M Dental Products, St
Paul, MN, USA) after a 48 h storage of the MTA. The
reported SBS values were higher than in the current
study for both adhesive systems (13.22 and 10.73 MPa
vs. 7.50 and 4.61 MPa respectively) similar to the
findings by Atabek et al.33). The difference in the reported
values may be due to the smaller bonded area used by
Tunc et al.23) and different 1-step self-etch adhesive
used. The reported values showed significantly higher
SBS using etch and rinse system which is in agreement
with the current study for MTA.
Altunsoy et al.32) studied the SBS of MTA (Angelus),
Biodentine and Calcium Enriched Mixture (CEM) to a
flowable composite using a 1-step self-etch system and
reported lower values compared to the current study
(2.01 MPa vs. 4.61 MPa), in spite of the long setting time
allowed for MTA (72 h vs. 48 h). Therefore, other factors
such as polishing of MTA surface, type of restorative
materials and bonding surface area may have affected
the outcomes.
It has been previously shown that longer storage
times of MTA enables it to reach its optimal physical
properties which resulted in higher strength values and
lower solubility35). Oskoee et al.17) evaluated the SBS of
MTA to Filtek Z250 using Single bond etch and rinse
885
system. The results showed lower SBS compared with
the current study (4.65 MPa vs. 7.50 MPa) which can
be attributed to the shorter storage period allowed for
MTA setting (24 h vs. 48 h in the current study), since
it has been shown that acid etching procedures affected
the hardness and strength of ProRoot MTA after mixing
and may lead to displacement of MTA in a cavity and
therefore affect its sealability33,36).
In the current study, SBS of the conventional
GIC to resin composite was lower than TheraCal LC
but significantly higher than MTA. Several factors
such as the flow (viscosity) of GIC may be related to
its bond strength to resin composite since it affects
its adaptability to the surface; low adaptability may
lead to partial defects on the restoration margin and
small voids which may affect bond strength values to
composite37). In addition, the lack of chemical bond
between conventional GICs and composite in addition to
the low cohesive strength of GICs lead to bond strengths
that are likely to be lower38). The lower bond strength to
Fuji IX in comparison to TheraCal LC may be attributed
to the difference in cohesive strength of these materials.
Moreover, during GIC placement, air bubbles may occur
within the material which could lead to generation of
stress concentration points39). This can also imply that
in the GIC subgroups, the bond strength to composite
is higher than the cohesive strengths of the capping
materials.
A number of previous studies have reported that
optimal bond strength to resin composite was achieved
using an etch and rinse system since 35% phosphoric
acid effectively removes the smear layer which in turn
creates a clean surface for better micromechanical
retention with composite, in addition to its ability to
produce deeper and more retentive microporosities in
enamel and dentin20,23,31,33,36). The lesser performance of
self-etch adhesives has been attributed to: 1) combining
the acidic hydrophilic monomer and hydrophobic
monomers into a single step may interfere with the
adhesive polymerization; 2) the intrinsically low
strength of the adhesive and 3) the inferior degree of
monomer polymerization due to the solvent/oxygen
inhibition effect during light polymerization of these
adhesives20). A number of studies reported that higher
bond strength values to composite were achieved using
1-step self-etch adhesive systems22,40,41), which was
attributed to a high pH value and better wettability
from solvents22), and to the presence of 5% fillers content
in the 1-step self-etch system which caused a decreased
shrinkage stress leading to higher bond strength to
composite41). This is in agreement with the results of the
current study for TheraCal LC and GIC. Furthermore,
it has been suggested that aggressive etching of GIC
using phosphoric acid weakens the cement surface by
preferential dissolution of the filler particles42). The
zone of weakened cement is therefore more likely to fail
cohesively when debonded from resin, possibly resulting
in lower bond strengths40).
MTA exhibited higher bond strength to composite
when using the etch and rinse system which is in
886 Dent Mater J 2016; 35(6): 881–887
agreement with previous studies20,23,33). The surface of
MTA samples etched with phosphoric acid observed
in previous studies36,41) showed a crystalline structure
that is eroded and cracked following phosphoric acid
treatment. This may have contributed to the higher
bond strength compared with the weaker acid treatment
from the self-etch adhesive system. Furthermore, the
water content of MTA could have interfered with the
polymerization of the self-etch adhesives20) thereby
resulting in reduced MTA-adhesive bond strength values
and therefore, more adhesive failures of Xeno V+to MTA
were found.
To accomplish a successful restorative procedure
when two different materials are used, there should
be an appropriate bond between the two materials43).
Generally, the bond is acceptable when fracture occurs
inside each material rather than in the bonded interface
(i.e. cohesive rather than adhesive)44). Failure mode
analysis showed a greater number of samples exhibited
mixed and cohesive failures within the capping material
in the TheraCal LC and GIC groups respectively
compared with MTA which mainly showed adhesive
failure modes which may indicate a stronger bond in
the former groups. The higher rate of cohesive failure in
tested samples suggests a higher bond strength which
has been reported by previous researchers.
It has been previously established that exposure
of MTA to a low pH environment may influence its
physical and chemical properties. In this context, the
acid-etch procedure using phosphoric acid reduces
the surface micro-hardness of MTA and most likely
weakens its structure36), and this can be the explanation
of the greater frequency of cohesive failure in MTA for
specimens bonded with etch-and-rinse systems33).
The 1-step self-etch adhesive system has pH of
1.3 which is considered intermediary strong compared
with strong Phosphoric acid (pH=0.1–0.4)26). Since
Xeno V+ has lower acidity its use was associated with
lower number of cohesive failures in MTA as it does
not weaken the MTA structure. Moreover, the self-etch
adhesive systems do not etch the surface to the same
depth as phosphoric acid.
Within the limitation of this laboratory study it was
concluded that TheraCal LC produced the highest SBS
to resin composite compared with MTA and Fuji IX.
Moreover, its SBS was not affected by type of adhesive
system used. It would be clinically beneficial for patients
and dentists alike if the final adhesive restoration
can be placed over pulp capping material during the
same visit, decreasing time and cost. Therefore, the
simple application and high bond strength capacity of
TheraCal LC to resin composite may support its use and
consideration as the material of choice in direct pulp
capping. In addition, when placing composite materials
over MTA, it might be advisable to use an etch and rinse
system prior to composite resin bonding.
ACKNOWLEDGMENTS
This research was funded by Jordan University of
Science and Technology Research Grant Committee
(Grant Number 20150036). The authors would like to
thank Dr Joshua Cheetham, Research and Development
Director at SDI limited/Australia for providing shear
bond strength apparatus and metal molds used in the
current study.
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