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Department of Dentistry and Stomatology, Cliniques Universitaires Saint-Luc, Universit catholique de Louvain, Brussels, Belgium
Institute of Condensed Matter and Nanosciences Bio & Soft Matter (IMCN/BSMA), Universit catholique de Louvain,
Louvain-la-Neuve, Belgium
c Center for Research and Engineering of Biomaterials (CRIBIO), Brussels, Belgium
b
a r t i c l e
i n f o
a b s t r a c t
Article history:
Objectives. The purpose of this study was to compare the mechanical and rheological prop-
erties of resin-based pit and ssure sealants to owable resin composites in order to dene
18 July 2011
Methods. Eight owable resin composites (Admira Flow, Filtek Supreme XT Flow, FlowLine,
Grandio Flow, Point-4 Flowable, Premise Flowable, Revolution Formula 2, X-Flow) and four
resin-based pit and ssure sealants (Clinpro, Delton FS+ , Estiseal F, Guardian Seal) were
used in this study. Their ller weight content was measured by thermogravimetric analy-
Keywords:
sis. Mechanical properties were measured: dynamic and static moduli of elasticity, exural
Resin composites
Flowable
Results. Flowable resin composites have by far better mechanical properties than pit and
Viscoelasticity
ssure sealants, except for Delton FS+ . All the materials tested are non-Newtonian, shear
Mechanical properties
thinning uids. They all showed elasticity even at the lowest frequencies but elasticity differs
Filler particles
1.
Introduction
Corresponding author at: School of Dentistry and Stomatology, Cliniques Universitaires Saint-Luc Universit catholique de Louvain,
Av. Hippocrate 10/5721, B-1200 Brussels, Belgium. Tel.: +32 2 764 57 30.
E-mail addresses: Sebastien.Beun@uclouvain.be, s.beun@skynet.be (S. Beun).
0109-5641/$ see front matter 2011 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.
doi:10.1016/j.dental.2011.11.001
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d e n t a l m a t e r i a l s 2 8 ( 2 0 1 2 ) 349359
resin modied glass ionomer cements, used as pit and ssure sealants is quite poor [68], the fact that they release
active F in the surrounding enamel is very important. Indeed,
they exert a cariostatic effect even after they have disappeared
macroscopically and this effect can reasonably be associated
to increased levels of F on the enamel surface as well as to
remnants of the material in the depths of the ssures [9]. For
these reasons, glass ionomer cements should be considered
more a F vehicle than a traditional ssure sealant [10] and
despite their lower retention rate as compared with resinbased pit and ssure sealants, there is today no conclusive
evidence that one material is superior to the other in preventing dental caries [11].
Compomers were developed to combine the advantages of
both glass ionomer cements and resins. Only little scientic
literature is available concerning the use of compomers as pit
and ssure sealants. It is known that the incorporation of uoride into resin and its release may compromise the integrity of
the material [12] and that the amount of F released from compomers is considerably less than for glass ionomers [1315].
However, Puppin-Rontani et al. showed comparability with
resin-based ssure sealants after a two year clinical study [16].
The caries preventive action of resin-based materials relies
on the establishment of an effective mechanical obstacle
to the leakage of nutrients to cariogenic microorganisms in
the deeper parts of ssures [10,17,18]. The major criterion
of success of these materials is thus based on their retention rate unlike glass ionomer sealants. They may be either
lled or unlled, and chemically or light-cured. Many studies have demonstrated the effectiveness of chemically cured
resin-based sealants in terms of retention rate [17,19,20]. The
performance levels of light-cured resin-based sealants are
similar to those of chemically cured ones within an observation period of up to 5 years [21,22]. However, for longer
observation periods, chemically cured sealants seem to give
better results [23] even if for obvious practical reasons lightcured materials are by far more popular among practitioners
nowadays than chemically cured ones. The addition of ller
particles to resin-based pit and ssure sealants seem to have
minor effect on clinical results and both lled and unlled
materials have similar retention rates [2426] but this is still
discussed [27].
2.
2.1.
Materials tested
2.2.
Percentage and morphology of the inorganic
fraction
2.2.1.
Manufacturer
Shade
Batch
A2
A3
A2
A3
A3
A3
A3
A3
500244
680934
10103
570666
408419
06-124102
4-1336
502000636
N/A
N/A
N/A
N/A
5FG
40825
10027
403412
d e n t a l m a t e r i a l s 2 8 ( 2 0 1 2 ) 349359
2.2.2.
Fillers morphology
The llers morphology was determined using SEM. Unpolymerized monomers were removed by a washing technique:
0.5 g of each material was dissolved in 4 ml of acetone and
centrifuged for 5 min at 700 g. This process was repeated
three times using acetone and three more with chloroform
for a further washing and to ensure a complete elimination
of the unpolymerized resin. The remaining llers including
prepolymerized llers were suspended in 2.5 ml of absolute
ethanol, smeared on a glass slide (7.5 cm 2.5 cm) and dried
at 37 C during 6 h. After gold-coating, llers were observed
by SEM (Leica Stereoscan S-260, Cambridge, UK) at 5000 and
10,000 magnications, operating at 20 kV under low-vaccuum.
2.3.
Mechanical properties
2.4.
Dynamic modulus
The dynamic modulus of elasticity was measured nondestructively by the impulse excitation technique [30]. Each
sample was set in exural vibration by a light mechanical
impulse. The signal produced was captured via a microphone
placed underneath the sample by a special signal analyzer, the
Grindosonic (Lemmens Elektronics, Haasrode, Belgium). Modulus of elasticity (GPa) was calculated from the fundamental
frequency, the mass, the width, the length and the thickness
of the bar as follows:
Ed = 0.9465
mft2
b
L3
t3
2.5.
351
Fl3
4bh3 d
3Fl
2bh2
2.6.
Vickers microhardness
Microhardness measurements were carried out on the fractured samples issued from the previous test with a Durimet
microhardness tester (Leitz, Wetzlar, Germany). A load of 200 g
was applied during 30 s on their surface. The length of the
diagonal of each indentation was measured directly using a
graduated eye-lens. The Vickers Hardness Number is obtained
using the following equation:
H=
1854.4 P
d2
3.
Rheological properties
T1
where m is the mass of the bar, b the width of the bar, L the
length of the bar, t the thickness of the bar, ft the fundamental
frequency of the bar in exion which appears on the screen
of the machine, and T1 a correction factor for fundamental
exural mode to account for nite thickness of the bar, Poissons ratio and other constants. Poissons ratio is the ratio of
transverse strain (contraction) to axial strain (elongation) in a
uniaxial tensile test [31]. When applied to dental resin composites, its value lies around 0.30 [32], that value has been
taken as the mean value for all the materials tested in this
study.
3.1.
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d e n t a l m a t e r i a l s 2 8 ( 2 0 1 2 ) 349359
Fig. 1 Mean values and standard deviations of the percentage of llers by weight of all the materials tested. Vertical bars
connect values that are not statistically signicant (p < 0.05).
following measurements were made on fully structured materials so that the results can be compared from one composite
to another. After, a frequency sweep test was performed from
100 rad/s to 0.01 rad/s to determine the variation of the complex viscosity (* ), storage (elastic) shear modulus (G ), loss
(viscous) shear modulus (G ) and loss tangent (tan ) as a function of the frequency.
3.2.
4.
Statistical analysis
5.
Results
5.1.
Percentage and morphology of the inorganic
fraction
5.1.1.
The mean values and standard deviations of the weight percentage of llers of the materials tested are presented in Fig. 1.
For the owable resin composites, they ranged from 45.0% for
the Revolution Formula 2 to 77.8% for the Grandio Flow. For
the pit and ssure sealants, averages varied from 6.5% for the
Clinpro to 54.3% for the Delton FS+ .
5.1.2.
Fillers morphology
5.2.
Mechanical properties
d e n t a l m a t e r i a l s 2 8 ( 2 0 1 2 ) 349359
353
Fig. 2 Fillers by scanning-electron microscopy at 5000 magnication (10,000 in the inserts) (items marked with an
asterisk are from Beun et al. [36]).
5.3.
Rheological properties
5.3.1.
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d e n t a l m a t e r i a l s 2 8 ( 2 0 1 2 ) 349359
Fig. 3 Dynamic moduli of elasticity of the materials tested. Materials that are not statistically signicant (p < 0.05) are
connected by vertical bars.
Fig. 4 Static moduli of elasticity of the materials tested. Vertical bars connect materials that are not statistically signicant
(p < 0.05).
d e n t a l m a t e r i a l s 2 8 ( 2 0 1 2 ) 349359
355
Fig. 5 Flexural strength of the materials tested. The vertical bar connect the materials that are not statistically signicant
(p < 0.05).
5.3.2.
Fig. 6 Vickers microhardness of the materials tested. Materials that are not statistically signicant (p < 0.05) are connected
by vertical bars.
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d e n t a l m a t e r i a l s 2 8 ( 2 0 1 2 ) 349359
Fig. 7 Complex viscosity (* ) vs. frequency for the owable resin composites tested.
6.
Discussion
Fig. 8 Storage modulus (G ) vs. frequency for the owable resin composites tested.
d e n t a l m a t e r i a l s 2 8 ( 2 0 1 2 ) 349359
357
Fig. 9 Complex viscosity (* ) vs. frequency for the pit and ssure sealants tested.
From Beun et al. [36].
exhibit lower shrinkage strain values [42]. Filtek Supreme XT
Flow and Delton FS+ exhibit ller particles that are considerably larger than the other materials tested.
An optimal resin composite should mimic structural, physical and mechanical characteristics of dentin and enamel. Xu
et al. [43] measured the elastic modulus of human enamel and
dentin and obtained 94 GPa for the enamel while it depends
signicantly on tooth orientation. The dynamic and static
moduli of elasticity of all the materials tested in this study
are of course by far lower than that value. On the other hand,
it is most probably of minor importance in the case of pit and
Fig. 10 Storage modulus (G ) vs. frequency for the pit and ssure sealants tested.
From Beun et al. [36].
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d e n t a l m a t e r i a l s 2 8 ( 2 0 1 2 ) 349359
Acknowledgements
The authors would like to thank Thrse Glorieux and JeanJacques Biebuyck for their valuable technical help.
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