Journal of Oral Rehabilitation 2002 29; 257262
Mechanical properties of resin cements with different
activation modes
R. R. BRAGA, P. F. CESAR & C. C. GONZAGA
of Sa~o Paulo, Sa~o Paulo, Brazil
SUMMARY Dual-cured cements have been studied in
terms of the hardness or degree of conversion
achieved with different curing modes. However,
little emphasis is given to the inuence of the curing
method on other mechanical properties. This study
investigated the exural strength, exural modulus
and hardness of four proprietary resin cements.
Materials tested were: Enforce and Variolink II
(light-, self- and dual-cured), RelyX ARC (self- and
dual-cured) and C & B (self-cured). Specimens were
fractured using a three-point bending test. Pre-
failure loads corresponding to specic displace-
ments of the cross-head were used for exural
modulus calculation. Knoop hardness (KHN) was
measured on fragments obtained after the exural
Introduction
In the last two decades, bonding procedures have
expanded the indications of indirect restorations and
allowed the development of new treatment alternat-
ives. As examples, we have Maryland bridges in the
1980s, and ceramic restorations in the 1990s. The
advantages of bonded indirect restorations include
improved marginal sealing, reducing the risk of post-
operative sensitivity (Rosentiel et al., 1998), low solu-
bility and superior mechanical properties of resin
cements compared with zinc phosphate and glass
ionomer cements (White & Yu, 1993).
According to the activation mode, resin cements are
usually divided in three groups: chemically-activated
(self-cured), photo-activated and dual-cured cements.
Self-cured cements are indicated for xation of metallic
and metalloceramic restorations, Maryland bridges and
pre-fabricated or cast posts. As some of the self-cured
2002 Blackwell Science Ltd
Department of Dental Materials, School of Dentistry, University
test. Tests were performed after 24 h storage at
37 C. RelyX ARC dual-cured showed higher exural
strength than the other groups. RelyX ARC and
Variolink II depended upon photo-activation to
achieve higher hardness values. Enforce showed
similar hardness for dual- and self-curing modes.
No correlation was found between exural strength
and hardness, indicating that other factors besides
the degree of cure (e.g. ller content and monomer
type) affect the exural strength of composites. No
statistical difference was detected in the exural
modulus among the different groups.
KEYWORDS : degree of cure, exural modulus, ex-
ural strength, hardness, mechanical properties, resin
cements
cements are translucent, they may be used for xation
of ceramic restorations. Light-cured cements have
indication restricted to laminate veneers, because of
the severe reduction of light intensity during its
transmission through the restoration (Soderholm &
Reetz, 1996). Dual-cured cements were developed to
conciliate favourable characteristics of self-cured and
photo-activated cements. The rationale was to have a
material with extended working time and capable of
reaching a high degree of conversion either in the
presence or absence of light.
It is a common sense that composites with a high
degree of conversion also have good mechanical prop-
erties. For this reason, most of the research on dual-
cured cements has focused on comparing its cure
potential under different activation modes and/or
photo-activation parameters. Several studies have
shown that dual-cured cements depend on photo-
activation to achieve an optimal degree of conversion.
257
258 R . R . B R A G A et al.
Table 1. Resin cements tested
Material
(Manufacturer) Monomers
Enforce Bis-GMA, TEGDMA
(Dentsply Ind e Com, Sao Paulo, Brazil)
RelyX ARC Bis-GMA, TEGDMA
(3M Dental Products, St Paul, MN, USA)
Variolink II Bis-GMA, UEDMA, TEGDMA
(Vivadent Ets, Schaan, Liechstein)
C&B Ethoxilated Bis-GMA,
(Bisco Inc, Schawburg, IL, USA) Tri-EDMA, Bis-GMA
Harashima et al. (1991) studied the degree of conver-
sion of ve dual-cured cements, using Fourier Trans-
form Infrared spectrometry (FTIR), nding 5975%
after self-cure and 6681% after photo-activation.
Rueggeberg and Caughman (1993) tested four cements,
also by FTIR, and no one presented similar results
comparing self-cured and dual-cured samples.
Hardness values present a good correlation with
degree of conversion for a specic composite (Ferracane,
1985) and for this reason have been used to compare the
behaviour of dual-cured cements under different photo-
activation conditions. Hasegawa et al. (1991) afrmed
that the ultimate hardness of dual-cured cements
depend on the amount of exposure to the curing light.
Furthermore, they found that there are marked differ-
ences in the relative contents of photo-initiators and self-
curing components among materials. According to
Watts et al. (1994), some products are overdependent
on photo-activation, which may lead to inadequate cure
and clinical performance. More recently, El-Mowafy
et al. (1999) related that even the last generation of dual-
cured cements cannot overcome the lower hardness
values obtained in the self-cure mode.
Nevertheless, as important as the evaluation of dual-
cured cements by its relative hardness (or degree of
conversion) is to determine how the activation mode
inuences its mechanical properties. The degree of
conversion is not the sole factor responsible for the
mechanical properties of composites. Filler content
(Chung & Greener, 1990) and monomer type (Asmussen
& Peutzfeldt, 1998) was found to be determinant factors
on high diametral tensile strength. On the other hand,
diluent concentration, activation mode, type and content
of initiator did not show a signicant effect on several
mechanical properties of unlled resins (Ferracane
& Greener, 1986). Peutzfeldt (1995) studied the wear
2002 Blackwell Science Ltd, Journal of Oral Rehabilitation 29; 257262
Particle Filler content
size (lm) (% weight) Shade Batch
1 66 A2 42374 (base)
42259 (catalyst)
15 675 A1 AAAA
1 73 A3 A181166 (base)
A14492 (catalyst)
5 65 universal 089058
and the degree of conversion of eight proprietary resin
cements after self- and dual-curing. No signicant
correlation was found between these two variables.
Besides, dual-curing reduced the wear in only three out
of eight cements tested.
The purpose of the present study was to evaluate the
hardness, exural strength and exural modulus of
four resin cements: one self-cured, one in both self and
dual-curing modes and two cements in self-, light- and
dual-curing. The hypothesis to be tested was if there is a
positive correlation between hardness (as an indirect
measure of degree of conversion) and exural strength.
Methods and materials
The resin cements chosen for this study are described in
Table 1. Enforce* and Variolink II were tested as light-
cured, dual-cured and self-cured materials. When used
as light-cured cements, no mixing was required. RelyX
ARC is supplied in a dispenser that delivers two pastes
simultaneously and it does not have the option of use as
light-curedmaterial.Aself-curedlutingcomposite(C&B)
was also included in this investigation.
Rectangular cross-sectional area specimens with
10 mm length, 2 mm width and 1 mm height were
built using a stainless steel split mould. The mould was
placed on a mylar strip over a glass slab. For dual-cured
and self-cured specimens, equal amounts of base and
catalyst pastes were mixed with a plastic spatula on a
mixing pad for 10 s and inserted into the mould using
an explorator. Then, the resin cement was covered with
another mylar strip, gently pressed against the mould to
*Dentsply Ind e Com, Sao Paulo, Brazil.
3M Dental Products, St Paul, MN, USA.
Vivadent Ets, Schaan, Liechtenstein.
Bisco Inc, Schawburg, IL, USA.
 MECHANICAL PROPERTIES OF RESIN CEMENTS 259

squeeze out the excess of material. In the experimental Five indentations were performed in each of the 10
groups for which photo-activation was required, a specimens.
composite spacer 2 mm thick (Z250, shade A3) was For hardness data, one-way ANOVA was performed
placed between the luting composite and the tip of the separately for Enforce (3 levels), RelyX ARC (2 levels)
light unit. Photo-activation was performed only on the and Variolink II (3 levels). Flexural strength and
upper surface of the specimen, using a halogen light unit exural modulus data were analysed by one-way ANOVA
with 550 mW cm2 intensity (Optilux 500), for 60 s. considering the nine experimental groups simulta-
Ten specimens were built in each group. The specimens neously. Tukey's test with a global signicance level
were stored in lightproof containers at 37 C for 24 h. of 5% was used for multiple comparisons. The existence
Three-point bending exural test was performed in a of signicant linear correlation between exural
universal testing machine** at a crosshead speed of strength and KHN was investigated by means of
05 mm min1. The distance between the supports was Pearson's correlation test.
6 mm. Before testing, specimens' dimensions were
determined using a digital calliper with 001 mm
Results
accuracy. Flexural strength was calculated using the
following formula: Average KHN is shown in Fig. 1. Enforce revealed
3Fl statistically similar hardness between self-cured and
r dual-cured groups. Light-cured specimens presented
2bh2
lower KHN compared with the other activation modes.
where r is the exural strength (in MPa), F is the
For RelyX ARC, the dual-cured group showed higher
failure load (in Newtons), l is the distance between
hardness than self-cured. Variolink II dual-cured also
the supports, b is the width and h is the height of the
presented higher KHN compared with self-cured and
specimen (all in mm).
light-cured groups. However, differently than Enforce,
During the test, the load values corresponding to
light-cured specimens demonstrated higher hardness
001 mm, 003 mm, 005 mm and 007 mm displace-
than self-cured specimens.
ment of the crosshead were recorded. These pre-failure
Flexural strength of RelyX ARC dual-cured was
load values were used to determine the exural
statistically higher than the other eight experimental
modulus according to the formula:
groups. All the other groups were statistically similar,
F1 l3 except for Variolink II self-cured, which showed
E
103
4bh3 d exural strength lower than RelyX ARC self-cured,
where E is the exural modulus (in GPa), F1 is the Variolink II light-cured, Variolink II dual-cured and
prefailure load (in Newtons), d is the displacement of
the crosshead at load F1 (in mm), l is the distance
between the supports, b is the width and h is the height
of the specimen (all in mm). The exural modulus of
each specimen was the average of the values calculated
using the four recorded loads and the corresponding
displacements.
Immediately after exural testing, half of the frac-
tured specimen was embedded in a PVC cylinder with
self-cured acrylic resin in a way that the upper surface
of the specimen was left exposed and parallel to the
horizontal plane. Knoop hardness (KHN) was meas-
ured using a load of 25 g with a dwell time of 15 s.

Demetron Res Corp, Danbury, CT, USA. Fig. 1. Knoop hardness number of the resin cements tested.
**Kratos Dinamometros, Sao Paulo, SP, Brazil. ANOVA was performed for Enforce, Variolink II and RelyX ARC

Mitutoyo Corp, Tokyo, Japan. separately. Columns joined by a horizontal bar are not statistically

Ernest Leitz, Durimet Wetzlar, Germany. different (P > 005).

2002 Blackwell Science Ltd, Journal of Oral Rehabilitation 29; 257262

260 R . R . B R A G A et al.

Table 2. Mean exural strength, in MPa, and s.d. (in parenthesis)
Light-cured Self-cured Dual-cured
a
C&B 1588 (1150)
Enforce 1536 (1732)a,b 1511 (1256)a,b 1548 (1163)a,b
RelyX ARC 1721 (1593)a 2008 (1301)
Variolink II 1682 (1652)a 1371 (1363)b 1646 (1858)a
Values followed by the same superscript are not statistically
different (P > 005).
C & B (Table 2). No statistically signicant correlation
between hardness and exural strength was found in
any experimental group. Pearson's correlation coef-
cients and respective P-values are shown in Table 3.
Flexural modulus ranged from 36 to 50 GPa
(Table 4). No statistical difference was detected
between groups (P 0091).
Discussion
The results of the hardness test are in accordance with
those of other similar studies with respect to the fact
that dual-cured cements depend on photo-activation to
achieve higher hardness values (Hasegawa et al., 1991;
Watts et al., 1994; Darr & Jacobsen, 1995; El-Badrawy &
El-Mowafy, 1995; El-Mowafy et al., 1999). In the
present study, the photo-activation was done through
a 2-mm-thick composite spacer, which was used to
approximate the conditions of the experiment to those
found in clinical practice. Even considering the attenu-
ated light intensity, only Enforce obtained statistically
similar values in the self-curing and dual-curing modes.
The other cements tested in more than one activation
mode presented lower hardness for the self-curing
mode. It is known that the light intensity reaching the
cement is drastically reduced when light is transmitted
through a composite or ceramic restoration. The inten-
sity decreases exponentially as a function of the
restoration thickness. An intensity of 600 mW cm2
may be reduced to approximately 120 mW cm2 when
light is transmitted through a 2-mm-thick porcelain
spacer (Prinsloo et al., 1997). Therefore, longer exposi-
Table 4. Mean exural modulus, in GPa, and s.d. (in parenth-
esis). All values are statistically similar (P = 0091)
Light-cured Self-cured Dual-cured
C&B 48 (118)
Enforce 43 (132) 42 (099) 49 (128)
RelyX ARC 42 (025) 42 (074)
Variolink II 49 (122) 36 (122) 50 (136)
tion times are recommended to diminish the effects of
the attenuation of the light that reaches the resin cement
(Rueggeberg & Caughman, 1993). There are evidences
that composites are less capable to transmit light than
a ceramic material of the same shade (El-Badrawy &
El-Mowafy, 1995). El-Mowafy et al. (1999) evaluated
the KHN of eight dual-cured cements and found that
Variolink II and Enforce showed opposite behaviours in
the absence of photo-activation. As it can be noticed in
Fig. 1, Variolink II did not present a substantial curing
potential when self-curing alone was used.
Statistical analysis of the hardness values was done
for each material separately, comparing the results
obtained from the different curing methods. When the
hardness test is used as an indirect assessment of the
degree of cure, the comparison among different com-
posites becomes meaningless, because the mechanical
properties of a polymer depend upon the cross-linking
density and the quality of the network which forms
during polymerization (Ferracane, 1985). In addition,
the ller content of the composite is also responsible for
its hardness (Chung & Greener, 1990). Hence there is
not an absolute hardness value that is able to predict an
absolute degree of conversion for all composite resins.
Notwithstanding, hardness tests permit the assessment
of the effectiveness of self- and light-curing components
which are present in the activation system of dual-
cured cements (Peutzfeldt, 1995).
Resin-based luting cements inadequately polymer-
ized are associated with problems such as post-opera-
tive sensitivity, microleakage and recurrent caries
(El-Mowafy et al., 1999), susceptibility to degradation,
discoloration and decrease in mechanical properties

Table 3. Pearson's correlation coef-

Light-cured Self-cured Dual-cured
cient between KHN and exural
C&B )0274 (P = 0512) strength
Enforce )0443 (P = 0200) )0489 (P = 0181) 0504 (P = 0137)
RelyX ARC 0516 (P = 0155) 0488 (P = 0152)
Variolink II 0054 (P = 0882) 0315 (P = 0409) )0315 (P = 0409)

2002 Blackwell Science Ltd, Journal of Oral Rehabilitation 29; 257262

 MECHANICAL PROPERTIES OF RESIN CEMENTS
(Uctasli et al., 1994). However, an under-polymerized
composite is not necessarily a `weak' material. In the
present study, differences detected in hardness values
did not correspond to differences in exural strength in
all cases. Enforce presented similar exural strength in
the three curing methods. Variolink II presented similar
exural strength in light- and dual-curing methods.
However, statistical differences were detected between
some of the corresponding hardness values. According
to Ferracane and Greener (1986), there would be a
`threshold' network quality which must be attained to
produce resins with high strength. After this network is
formed, the strength becomes less dependent upon the
degree of cure.
Several factors may affect the degree of cure, for
example the types of monomers which constitute the
polymeric chain and the inhibitor concentration
(Ferracane & Greener, 1986). Nevertheless, the degree
of conversion is not positively correlated with all types
of mechanical properties (Asmussen & Peutzfeldt,
1998). As mentioned above, ller type and content also
interfere in mechanical properties. With this respect,
it is interesting to notice the good performance of
Variolink II in exural strength in both light- and dual-
curing modes, even considering the low light intensity
that reached the cement and the small amount of
chemical activators veried in the hardness test. Besides
the high ller content compared with the other mate-
rials tested, another possible explanation for the beha-
viour of Variolink II would be the presence of urethane
dimethacrylate (UEDMA) in its composition. This
monomer is more exible than Bis-GMA because of the
urethane linkages and presents lower viscosity, which
facilitates the migration of free radicals, increasing the
degree of crosslinking (Asmussen & Peutzfeldt, 1998).
The exural modulus of the cements, also referred to
as `apparent modulus of elasticity' (ilo & Espevik,
1978), was around 45 GPa. This value is lower than
others found in the literature, between 7 and 12 GPa
(Oilo & Espevik, 1978; Asmussen & Peutzfeldt, 1998;
Li & White, 1999). This disagreement may be because of
differences in the method and specimen conguration.
The elastic modulus is related to the stress transmission
between the restoration and the tooth structure. It also
indicates the ability of the cement to resist elastic
deformation which could jeopardize the integrity of the
bonded interface. Theoretically, the luting agent should
have an intermediary elastic modulus between that of
dentin and the restorative material (Li & White, 1999).
2002 Blackwell Science Ltd, Journal of Oral Rehabilitation 29; 257262
261
However, the values found are much lower than those
reported for dentin, around 13 GPa (Watts, 1994).
When selecting a resin cement, some factors have to
be taken into account like the manipulation character-
istics, the aesthetic demand of the work and the stress
level to which the bonding interfaces will be submitted.
Concerning this last one, the results of this study
indicate that the evaluation of resin cements should not
be restricted to tests that estimate directly or indirectly
the degree of cure. It should also be considered that this
was a short-term study and more research on strength
of resin cements under different activation modes
should be carried out to verify if the mechanical
properties of these materials might be affected after
longer storage periods.
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Correspondence: Dr Paulo Francisco Cesar, Rua Barao do Triunfo,
464 apt.21, Sao Paulo, SP CEP 04602-001, Brazil.
E-mail: p-paulof@siso.fo.usp.br