 

Dr. Yousef A. AlJehani

College of
Applied Medical Sciences
Dental Health Department
Dental Technology
Program
 ‫א‬‫א‬
Publications &
Researches
 Dental Materials 19 (2003) 393–398
www.elsevier.com/locate/dental

In vitro characterization of two laboratory-processed resin composites

A. Kakabouraa,*, C. Rahiotisa, S. Zinelisb, Y.A. Al-Dhamadic, N. Silikasc, D.C. Wattsc
a
Department of Operative Dentistry, University of Athens, Thivon 2, 115 27, Goudi, Athens, Greece
b
Biomaterials Laboratory, University of Athens, Greece
c
Dental School, University of Manchester, Manchester, UK
Received 15 January 2002; revised 20 May 2002; accepted 11 June 2002

Abstract
Purpose. To compare various characteristics of two new-generation laboratory-processed resin composites (BelleGlass HP/SDS-Kerr and
Sinfony/3M-ESPE). The properties evaluated were degree of CyC conversion, microhardness, roughness, biaxial flexural strength and
polymerization shrinkage-strain.
Materials and methods. All specimens were subjected to a first and a second polymerization cycle according to the manufacturers’
instructions. The degree of CyC conversion (DC) was recorded on rectangular (3 £ 2 £ 0.5 mm3) specimens (n ¼ 3) by FT-IR
micromultiple internal reflectance spectroscopy immediately after each of the two polymerization cycles. Twenty cylindrical specimens
(10 £ 2 mm2) of each material were prepared for surface microhardness (n ¼ 10, VHN, 200 g load, 20 s) and surface roughness (n ¼ 10, Ra)
measurements. The biaxial flexural strength and stiffness were determined on disk-shaped (n ¼ 8, 15 £ 0.7 mm2) specimens loaded to
fracture at 1 mm/min crosshead speed. The polymerization shrinkage-strain was calculated with the bonded-disk method. All values were
statistically analyzed by Student’s unpaired t-test ( p , 0.05).
Results. The second polymerization cycle significantly increased the degree of CyC conversion for both materials ( p , 0.05). BelleGlass
HP exhibited significantly higher degree of CyC conversion, surface microhardness, surface roughness, biaxial flexural strength and stiffness
values compared to Sinfony ( p , 0.05).
Significance. Several differences exist between the materials although both products are recommended for the same clinical applications.
q 2003 Academy of Dental Materials. Published by Elsevier Science Ltd. All rights reserved.
Keywords: Belleglass HP; Sinfony; Degree of cure; Microhardness; Roughness; Biaxial flexural strength; Shrinkage-strain; Load-to-failure rates

1. Introduction overcome some inherent deficiencies of direct composites

Although porcelain is a well-accepted esthetic material
for prosthodontic applications, the metal – ceramic and all-
ceramic restorations show some undesirable characteristics.
The opaque nature of metal substructure does not simulate
natural translucency; fabrication is time-consuming and
technically demanding and the abrasiveness of porcelain is
destructive to the opposing natural tooth structure [1].
Moreover, in all ceramic restorations, the absence of a metal
framework gives the potential for low fracture resistance,
limiting the clinical application in high stress areas.
In an effort to overcome some of these disadvantages, the
manufacturers, even in the early 1980s, introduced numer-
ous products of laboratory-processed resin composites [2].
These materials provided alternative ways for clinicians to
* Corresponding author. Tel.: þ 30-317788575; fax: þ 30-31-8033129.
E-mail address: afrodite1@otenet.gr (A. Kakaboura).
0109-5641/03/$ - see front matter q 2003 Academy of Dental Materials. Published by Elsevier Science Ltd. All rights reserved.
doi:10.1016/S0109-5641(02)00082-9
restorations, including polymerization shrinkage,
inadequate polymerization in deep interproximal areas and
restoration of proximal contacts and contour [3].
However, these resin composites were microfill materials
which demonstrated poor clinical performance due to low
flexural strength and wear characteristics attributed to the
low inorganic filler content [4]. In the early 1990s a second
generation of laboratory-processed resin composites was
developed, advocated for a wide range of fixed prosthodon-
tic applications such as inlays, onlays, veneering, metal-free
single unit crowns and short span anterior bridges [4]. A
variety of materials with remarkable differences in compo-
sition, polymerization modes and curing conditions com-
prise the second generation of the laboratory-processed
resin composites. Ultra-small filler particles and polyfunc-
tional methacrylate monomers are used in these composites.
They are processed by different laboratory techniques based
on combinations of heat, pressure, vacuum and light
394 A. Kakaboura et al. / Dental Materials 19 (2003) 393–398

polymerization. Although, second generation products

Second cycle: heat 140 8C, pressure 60 psi, N2

became available in 1995, their characteristics and clinical

(Visio Beta) up to 40 8C, vacuum, 15 min

performance have not been adequately investigated [2,
First cycle: photopolymerization (Light

First cycle: photopolymerization (Visio

5 – 10]. Additional products, such as Sinfony (3M-ESPE

(BelleGlass HP curing unit), 20 min

Second cycle: photopolymerization

Dental AG, Germany), were introduced claiming improved
performance and esthetics. The purpose of this study was to
Teklite) 650 mW/cm2, 40 s;

Alpha), 400 mW/cm2, 15 s;

evaluate the in vitro performance of two second-generation
laboratory-processed resin composites. Properties to be
Polymerization mode

examined include: the degree of CyC conversion, surface

microhardness, surface roughness, biaxial flexural strength
and polymerization shrinkage-strain which are acknowl-
edged to be related to the clinical performance of composite
restorations.
The null hypothesis to be tested, was that no significant
differences would be found in the properties examined,
between the two materials.
dimethacrylate oligomers, fillers: 74 wt% barium

2. Materials and methods

silicate glasses and SiO2, mean size: 0.6 mm
Aliphatic urethane dimethacrylate, aliphatic

The resin composites examined were BelleGlass HP

fillers: 50 wt% aluminum glass and SiO2
Aliphatic and cycloaliphatic monomers,

(SDS-Kerr, Orange, CA, USA) and Sinfony (3M-ESPE

Seefeld, Germany). The composition of each material and
their required polymerization mode are shown in Table 1.
The degree of CyC conversion (DC) was evaluated after the
first and second polymerization cycles with a reflectance
FT-IR spectroscopy (Perkin –Elmer, Norwalk, CT, USA).
mean size: 0.6 mm

Three rectangular specimens (3 £ 2 £ 0.5 mm3) were pre-

Composition

pared per material. Spectra of the original pastes and of the

directly irradiated surfaces were acquired after the first and
second polymerization cycle under the following con-
ditions: 4000 –400 cm21 range, 4 cm21 resolution, 458 para
edge KRS-5 minicrystal of seven internal reflections, 40
scans coaddition at 35 ^ 1 8C. The quantitative measure-
ments of DC were performed based on the two-frequency
method [11,12].
For surface microhardness measurements, the resin
Batch number #

composite pastes were packed into disk-shaped Teflon

FW0059863

molds (10 mm diameter, 2 mm height), pressed against

808B93
Composition and polymerization modes of the materials tested

transparent polyester matrix strips and subjected to the two

polymerization cycles. Ten specimens per material were
prepared. After the second polymerization cycle the speci-
mens were stored in water under dark conditions at 37 8C for
24 h, the flat surfaces were ground slightly with 1000 grit
size wet silicon carbide (SiC) papers and the microhardness
values were obtained after application of 200 g load for 20 s
BelleGlass HP shade: enamel natural

using a Microhardness instrument (HMV 2000, Shimadzu

Corp., Tokyo, Japan) equipped with a Vickers diamond
Sinfony shade: enamel natural

indenter.
For surface roughness measurements, 10 disk-shaped
specimens per material were prepared, as described above.
Mean roughness values (Ra) were measured using an
electronic profilometer (Diavite DH-5, Asmeto AG, Rich-
terswill, Germany) operated with a 5 mm diamond stylus,
Materials
Table 1

908 reading angle and 0.80 mm cut-off length. Six

recordings per specimen surface were recorded.
 A. Kakaboura et al. / Dental Materials 19 (2003) 393–398
Fig. 1. Schematic representation of the biaxial flexural method of fracture.
Eight disk-shaped specimens (15 mm diameter,
0.7 mm height) per material were prepared for the
biaxial flexural strength test, which were subjected to the
two individual polymerization cycles. The specimens
were ground, as described earlier and were immersed in
water at 37 ^ 1 8C for 24 h. Then, each specimen was
transferred on a biaxial flexure device consisting of three
stainless steel balls (3.2 mm in diameter) equally spaced
along the periphery of 10 mm diameter supporting circle
(Fig. 1). The specimens of each group were loaded at
the center with a stainless steel ball of 3.2 mm diameter
until fracture, in a universal testing machine (Model
6022, Instron Corp, Canton MA, USA) operating in
compression at 1 mm/min crosshead speed. The biaxial
flexural strength was calculated according to the
equation [13]
BS ¼ AP=h2 and
A ¼ ð3=4pÞ½2ð1 þ nÞlnða=r0p Þ þ ð1 þ nÞð2a2 2 r0p2 Þ=2b2
þ ð1 þ nÞ
r0p ¼ ð1:6r02 þ h2 Þ1=2 2 0:675h
where BS is the biaxial flexural strength, P the load at
failure, n the Poisson’s ratio (0.24) [14], a the radius of
supporting circle, b the radius of the specimen disk, h
the thickness of the sample and r0 the ball radius.
395
The load-to-failure rate was determined directly from the
load versus time graphs plotted as the ratio of the fractured
load to the failure time.
The polymerization shrinkage-strain during the pri-
mary cure cycle was measured with the bonded-disk
method [15,16].
Statistical analysis was performed by unpaired Student’s
t-test to define any significant differences in the properties
tested between the two resin composites for each testing
condition. A 95% confidence level was chosen ( p ¼ 0.05).
3. Results
The mean values of all the properties are shown in
Table 2. The second polymerization cycle significantly
improved the percentage degree of CyC conversion (DC) in
both materials ( p , 0.05). BelleGlass HP showed signifi-
cantly higher final DC values, higher surface microhardness
and higher roughness (Ra) values, compared to Sinfony
( p , 0.05). BelleGlass HP exhibited lower final shrinkage-
strain values compared to Sinfony during the primary cure
cycle, and also had remarkably lower shrinkage-strain
values in the early stages of the polymerization, 10– 40 s
(Tables 3 and 4). No statistically significant differences
were detected between the two materials regarding the
biaxial flexural strength. Nevertheless, BelleGlass HP
396 A. Kakaboura et al. / Dental Materials 19 (2003) 393–398
Table 2
Results (mean ^ SD) of all characteristics evaluated. The properties were measured after the second cure cycle
Material Degree of CyC Degree of CyC
conversion, first cycle conversion, second cycle
BelleGlass HP 60 (7.2) 80 (10.4)
Sinfony 50 (5.1) 66 (6.8)
exhibited a significantly higher load-to-failure rate com-
pared to Sinfony ( p , 0.05), an indication of higher
material stiffness.
4. Discussion
The null hypothesis was rejected. The two materials
exhibited significant differences in most of the properties
studied. The degree of CyC conversion for direct resin
composites has been reported to vary from 50 to 75% [17,
18]. The results of the present study indicate that after the
second polymerization, Sinfony reached a value within this
range, whereas BelleGlass HP demonstrated an even higher
degree of CyC conversion (80%), which is in accordance
with the results reported by Knobloch et al. [2]. Differences
in monomer composition and polymerization conditions
may explain the higher degree of CyC conversion provided
by BelleGlass HP. BelleGlass HP contains aliphatic
urethane monomers, which are known to provide an
increased degree of CyC conversion [18]. However, the
main differences are expected to arise from the temperatures
used in the second cure cycle. The polymerization of
BelleGlass HP during the second cycle was performed at a
higher temperature (140 8C) than for Sinfony (40 8C).
In general, the additional cure-cycle and photothermal
annealing enhance the DC of the resin composites. Thus, the
physicomechanical properties of the materials can be
improved [19,20] and an increase in polymerization rate
can be achieved which yields and promotes an annealing
effect in the polymer. The high pressure (60 psi) applied
during BelleGlass HP polymerization may also increase the
extent of polymerization.
The positive influence of the additional cure on DC found
in this study has been noted in previous studies [21 – 23].
The second polymerization cycle will increase the molecu-
lar mobility of the residual monomer and the chain segments
after initial photopolymerization. However, an inherent
Table 3
Mean shrinkage-strain values for Sinfony, at three different temperatures during the first cure cycle, SD in parentheses (n ¼ 5)
Temperature (8C) Sinfony
10 s 20 s
23 2.60 (0.15) 3.30 (0.04)
37 2.90 (0.10) 3.55 (0.16)
60 3.34 (0.30) 3.94 (0.35)
Micro-hardness Roughness Biaxial flexural strength Load-to-failure rate
(VHN) (Ra, mm) (MPa) (MPa/s)
174 (22.1) 0.31 (0.05) 49.4 (9.4) 5.5 (0.4)
77.8 (16.5) 0.16 (0.03) 53.4 (8.1) 2.6 (0.3)
drawback of the increased CyC conversion may be the
reduction of remaining CyC bonds available for copoly-
merization with the resin luting cements. Jordan [24]
reported that the lack of air-inhibited layer and the limited
unsaturation of the laboratory-processed resins negatively
affect the composite-luting cement interfacial strength.
The proportional increase in DC after the second
polymerization cycle was found to be essentially equivalent
for both materials.
The volume fraction and type of inorganic fillers as well as
the DC of the organic matrix are important contributory
factors to the microhardness of composite materials [19,25,
26]. The higher inorganic volume fraction of BelleGlass HP,
the harder type of glasses contained [27] and the higher density
of the organic matrix, as a result of the enhanced conversion,
can explain the higher microhardness values obtained. Surface
microhardness is considered as an indicative factor of the
mechanical strength of a resin [28]. A positive correlation
between the hardness of a resin material and the wear
resistance has been reported [7,28,29] although such a
correlation has not been confirmed in other studies [30,31].
Resin composite restorations with smooth outer surfaces
lead to reduced plaque retention, surface staining and
secondary caries incidence [32,33]. The higher roughness
value obtained for BelleGlass HP may be partly explained
by the higher filler volume loading and the harder type of
fillers incorporated into the material. Moreover, curing of
BelleGlass HP under nitrogen pressure may provide
nitrogen entrapment, which may increase the porosity at
the surface region. On the other hand, polymerization of
Sinfony under vacuum eliminates such surface porosity.
Nevertheless, both materials investigated showed initial
roughness lower than the roughness values of
0.64 ^ 0.25 mm reported for enamel. Enamel roughness
of 0.64 mm at enamel-to-enamel occlusal contact areas is
considered as a standard for roughness measurements of
resin composites [34]. Plaque accumulation preferentially
occurs on composite surfaces with a roughness range of
40 s 30 min 60 min
3.50 (0.03) 4.30 (0.05) 4.34 (0.06)
3.80 (0.16) 4.40 (0.19) 4.44 (0.20)
4.10 (0.39) 4.66 (0.47) 4.73 (0.46)
 A. Kakaboura et al. / Dental Materials 19 (2003) 393–398
Table 4
Mean shrinkage-strain values for BelleGlass HP, at three different temperatures during the first cure cycle, SD in parentheses (n ¼ 5)
Temperature (8C) BelleGlass HP
10 s 20 s
23 0.28 (0.11) 0.96 (0.10)
37 0.24 (0.03) 1.27 (0.08)
60 0.34 (0.10) 1.96 (0.34)
0.7 –1.4 mm [32]. The lower roughness of Sinfony com-
pared to BelleGlass HP may be a contributory factor to the
higher reported color stability of Sinfony [6]. The roughness
of BelleGlass HP recorded by Soeno et al. [35] cannot be
compared with the results of the present study since a
different polishing procedure of the specimens was used.
Mechanical strength is an important factor in the
clinical success of a restoration. Resin composites are
much weaker in tension than in compression. Therefore,
tensile strength is generally considered as a more
meaningful property for assessment of the clinical failure
potential of resin materials [36]. The traditional tensile
test has rarely been used for resins because of the
difficulty associated with gripping and aligning of the
specimens. Recently, the biaxial flexural test has been
used to determine the tensile strength of composite
materials [36]. In the present study, although BelleGlass
HP exhibited a higher DC and a higher filler volume
than Sinfony, similar biaxial flexural strength values were
recorded from both materials. It is well recognized that
several structural parameters, such as inclusions of voids,
cracks, flaws and stress gradients influence the fracture
strength of brittle materials [36]. A value of n ¼ 0.24
was taken as a selected value of Poisson’s ratio which is
consistent with previous measurements [14]. Other
restorative materials, such as glass-ionomer cements,
exhibited higher values of 0.30 [37]. If such a larger
value had been selected it would have enhanced the
values by 4.7%. Hence, even if the values for the
materials varied widely 0.24 – 0.30, this would not have
produced a very significant effect on the resultant
strength values. It is not known whether nitrogen
entrapment into BelleGlass HP during the second
polymerization cycle may induce flaws, which in
sequence may affect the material strength. So, despite
the fact BelleGlass HP presented a higher DC than
Sinfony, this cannot predict their relative strengths.
The load-to-failure rates measured show that Sinfony
is a more flexible material than BelleGlass HP. The
lower DC in Sinfony may generate a less stiff organic
network, which along with the lower filler volume
content may explain the more flexible nature of Sinfony.
The latter may permit higher energy absorption capacity
under loading, which may appear as plastic deformation.
This effectively blunts the crack tip, which then requires
more energy to propagate.
397
40 s 30 min 60 min
1.85 (0.10) 2.67 (0.12) 2.90 (0.10)
2.30 (0.08) 3.18 (0.10) 3.28 (0.10)
2.93 (0.32) 3.56 (0.35) 3.70 (0.40)
The polymerization shrinkage-strain during the primary
cure cycle showed that Sinfony had consistently higher
shrinkage values compared to Belleglass HP, despite its
lower DC. This could be attributed to the higher filler
percentage of Belleglass HP (74%), compared to that of
Sinfony (50%). The slower shrinkage response of Belleglass
HP is consistent with a lower concentration of the
photosensitizer. The rate of propagation Rp is proportional
to the photosensitizer concentration Cs [38]. This probably
accounts for the slower start in the polymerization of
Belleglass HP.
In conclusion, significant differences were determined
between the two second-generation laboratory-processed
resin composites evaluated in terms of DC, surface
microhardness, surface roughness, biaxial flexural strength
and stiffness, which may affect the clinical behavior of each
material. Nevertheless, controlled long-term clinical studies
are needed to confirm the clinical significance of these
differences. It is not known whether the greater compliance
of Sinfony may provide a better stress distribution pattern
and more efficiently preserve adjacent tissue integrity in
intracoronal restorations. However, the mechanical proper-
ties of these materials may be modified when veneering
metal frameworks, as the bonding capacity of the compo-
site-metal interface may strongly influence the mechanical
performance of the complex. Consequently, although the in
vitro characterization of material properties cannot yet
establish sound criteria for the prediction of their clinical
efficacy, it provides a basis for understanding the laboratory
and clinical performance of these materials and for the
development of new materials.
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