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Article Porcelain veneer post-bonding crack repair by resin infiltration View project
All content following this page was uploaded by Daniel Alexandre Menezes Pedrosa Malta on 03 February 2016.
Purpose: To assess the resin microtensile bond strength (MTBS) and the degree of conversion (DC) of indirect
composite resin restorations polymerized with light and heat.
Materials and Methods: Two direct (Filtek Z100 and Premise) and one indirect (Premise Indirect) composite
resins were polymerized with a combination of light and heat (138°C for 20 min). For MTBS, 42 cylinders were
fabricated (n = 7). After the surface treatment, cylinders were bonded to each other using adhesive resin (Opti-
bond FL). Specimens were stored in water for 24 h. Another 15 cylinders (n = 5) were fabricated for determining
degree of conversion using Fourier Transform Infrared Spectrometry immediately and at 24 h. The MTBS and the
DC was submitted to two-way ANOVA. The interaction with existing data was explored with univariate ANOVA and
two-way ANOVA. Tukey’s HSD post-hoc test was used to detect pairwise differences (α = 0.05).
Results: The MTBS to light and heat polymerized Z100 was 75.7 MPa, significantly higher than that to Premise
(58.6 MPa) and Premise Indirect (63.9 MPa). The immediate DC for Z100, Premise, and Premise Indirect were
51.0%, 68.7%, and 61.8%, respectively. The DC at 24 h ranged from 53.4% (Z100) to 72.8% (Premise Indirect)
and significantly increased for Premise Indirect only. Comparison with previously published data revealed that
the heat treatment increased both MTBS and DC of Premise and Premise Indirect.
Conclusion: Z100 showed better bond strength but lower DC. Heat treatment and a 24-h delay before delivery
can benefit DC of Premise Indirect. The increase in DC of Premise and Premise Indirect did not affect their bond
strength.
Keywords: adhesion, bond strength, direct composite resin, dental materials, indirect composite resin, degree
of conversion.
J Adhes Dent 2015; 17: 559–566. Submitted for publication: 26.02.15; accepted for publication: 22.10.15
doi: 10.3290/j.jad.a35258
Table 1 Materials and polymerization protocol the polymerization protocol of the previously published
data (light only for Z100 and Premise, and light plus 10-
Material Polymerization protocol min heat polymerization for Premise Indirect) is termed
“standard” (Table 1).
Filtek Z100 40 s light polymerization + 20 min heat
Premise 40 s light polymerization + 20 min heat Microtensile Bond Strength (MTBS) Test
The MTBS samples were made from 42 cylindrical
Premise Indirect 40 s light polymerization + 20 min heat composite resin specimens using a plastic mold (8 mm
deep × 6 mm diameter) on a glass slide. The samples
were fabricated in pairs using two distinctive shades of
strated as a result of this extraoral treatment of a regular material (Table 2). Seven pairs (n = 7) were made for
composite resin material. each group (14 cylinders) and bonded to each other.
Improved properties are attributed to increased mono- The different shades within each pair were necessary
mer conversion and stress annealing of polymerization to identify the adhesive interface and analyze the fail-
forces.21 A linear relationship should exist between heat ure mode. For Filtek Z100 and Premise, cylinders were
levels and degree of conversion. The degree of composite produced by incremental layering (2-mm-thick layers,
curing is determined by the ratio of aliphatic to aromatic light polymerized for 40 s each). For Premise Indirect, a
C=C absorbance of the methacrylate materials as deter- bulk placement technique was used because pilot tests
mined by Fourier transform infrared spectrometry, FT-IR. revealed lack of interlayer cohesion when using incre-
Still, at higher heat levels, a relatively high proportion of mental placement. All cylinders were light polymerized
aliphatic carbon double bonds (C=C) remain unutilized for 240 s through the plastic mold (40 s, 6 times). The
(30% to 50%). Some C=C units are present as pendant cylinders were then removed from the plastic mold and
methacrylate groups, covalently bonded to the polymer placed in the proprietary oven for 20 min at 138°C. All
network, and are incapable of leaching or evaporating. specimens were then reduced to a 6-mm height with a
Other C=C units are unreacted monomer, capable of leav- diamond saw (Diamond Wheel M4D220-N75M99-1/8,
ing the cured material. Heat treatment leads to the loss of Norton; Worcester, MA, USA) under water cooling on a
unreacted material at the composite surface by volatiliza- cutting machine (IsoMet Low Speed Saw, Buehler; Lake
tion. This would help make that area harder, denser, and Bluff, IL, USA). The fitting surface of each cylinder was
stronger. It would also help in reducing the leachability flatly wet ground with 400-grit silicon carbide paper (We-
of monomer into saliva following restoration bonding.3 tordry, 3M ESPE) for 5 s, followed by airborne particle
However, bonding to this surface with a methacrylate- abrasion using a fine airborne particle abrasion unit
based agent may be limited as a result of fewer C=C units (Kavo RONDOFlex Plus 360, Kavo; Biberach, Germany)
on the post-cure heated composite surface.4,24,33,48 A for 15 s at 2 bar with 50-μm aluminum oxide (Danville;
strong bond between the luting composite resin and the San Ramon, CA, USA) at a distance of approximately
fitting surface of the restoration is required for the clinical 10 mm and a 90-degree angle. The surfaces were then
success of nonretentive preparations, such as for inlays, cleaned by etching with 35% phosphoric acid (Ultra-
onlays, and veneers. Etch, Ultradent) and gentle scrubbing with a microbrush
The present study was designed to evaluate the degree for 1 min, followed by rinsing with water. Finally, the
of monomer conversion and bond strength of composite samples were placed in an ultrasonic bath with distilled
resins subjected to both light and prolonged heat poly- water for 2 min and air dried. A silane (Silane, Ultradent)
merization. Previously published data about light curing was applied for 5 s, then air and heat dried for 1 min
alone was included for comparison.29 The null hypothesis (D.I.-500, Coltène Whaledent; Altstätten, Switzerland).
is that there is no difference in bond strength and degree Seven pairs of cylinders of the same type of composite
of conversion between materials intended for direct or resin but dissimilar shades were bonded together using
indirect use, even when subjected to prolonged heat poly- a coat of adhesive resin (Optibond FL Adhesive; Kerr)
merization. on each fitting surface. A constant force of 1 kg was
applied to the blocks for 10 s before light polymerizing
for 40 s (2 × 20 s). The samples were stored in distilled
MATERIALS AND METHODS water for 24 h at room temperature before testing.
After storage, each specimen was individually secured
Two direct composite resins, Filtek Z100 (3M ESPE; St with sticky wax (Sticky Wax, Kerr) to a transparent plastic
Paul, MN, USA) and Premise (Kerr; Orange, CA, USA), sectioning block. Using the nontrimming technique de-
and one indirect composite resin, Premise Indirect veloped by Shono et al (1999),41 multiple beams were
(Kerr), were used in this study (Table 1). The composite prepared with the resin-to-resin adhesive interface in the
resins were polymerized with an LED unit (Valo Curing center of the beam. To do so, specimens were vertically
Light, Ultradent; South Jordan, UT, USA) in standard sectioned into 1-mm-thick slabs using a low-speed dia-
power mode with 1000 mW/cm2 intensity for 40 s, plus mond saw. The slabs were sectioned again into beams
additional heat treatment in a curing oven (Premise Indi- with approximately 1 mm2 cross-sectional areas. The
rect Curing Oven, Kerr) at 138°C for 20 min. This poly- specimens were attached to a table-top material tester
merization protocol is termed “prolonged” in this study; (The Micro Tensile Tester, Bisco; Schaumburg, IL, USA)
Table 2 Composition, batch numbers, and manufacturers of the resins used in this study
Premise Opaque A3/3435851 Bis-GMA, TEG-DMA, barium, 84 wt%, 70 vol% 0.4 μm Kerr; Orange,
Opaque B1/346919 silica, camphorquinone CA, USA
Premise Primary Dentin A3,5/3461351 Bis-GMA, TEG-DMA, barium, 87% wt%, 72 vol% 0.4 μm Kerr
Indirect Primary Dentin B1/3364736 silica, camphorquinone, pro-
prietary heat initiator
Fig 1 Microtensile specimen before loading. Fig 2 Composite resin cylinder placed in measuring device for
FT-IR.
using cyanoacrylate glue (Professional Super Glue, Loctite slide was placed over the plastic and pressed to force
Henkel; Avon, Ohio, USA). A chemical accelerator (Zapit the composite to adapt to the metal matrix dimensions
Accelerator, DVA; Corona, CA, USA) was applied to the and yield a flat, and smooth surface.
cyanoacrylate glue with a microbrush. The specimens were The percent monomer conversion of the samples was
subjected to microtensile testing at a crosshead speed of collected between 1680 and 1550 cm-1 with the use of a
5.4 kg/min (Fig 1). After testing, the failure mode of each Fourier transform infrared spectrometer (Spectrum 100 FT-
beam was determined under a stereoscopic microscope IR Spectrometer, PerkinElmer; London, UK) using 4 scans
(MZ125, Leica Microsystems; Heerbrugg, Switzerland) at a resolution of 2 cm-1. The baseline measurement was
at 40X magnification. Failures were considered adhesive obtained from unpolymerized material by carefully remov-
when the fracture site was located entirely between the ing the glass slide and the plastic matrix and placing the
adhesive and the composite resin, cohesive when the sample on the spectrometer. The same procedure was
fracture occurred exclusively within the composite resin, repeated with polymerized samples (1000 mW/cm2 of
or mixed when fragments of composite resin were de- intensity for 40 s applied to top surface followed by heat
tected along the adhesive fracture. treatment by placing the assembly [metal matrix and com-
posite] into the proprietary oven for 20 min). The same
Fourier Transform Infrared Spectrometry samples were then stored in water at a room temperature
The closest shade of each material was selected (B2 until FT-IR measurements 24 h later (Fig 2).
for Z100; Opaque B1 for Premise; and Primary Dentin Monomer degree of conversion (DC, in %) was calcu-
B1 for Premise Indirect) for this part of the experiment. lated by standard methods from the absorbance intensi-
Cylindrical composite specimens (five per material) were ties of the aliphatic:aromatic (C=C) ratio, ie, between the
made in a metal matrix (3 mm deep × 6 mm diameter) nonpolymerized and polymerized composite resin spectra:
on a glass slide. The composite resin was put into the
matrix with a clean spatula in one bulk layer and cov- [Abs (aliphatic) / Abs (aromatic)]polymer
(%C=C) = × 100
ered with a sheet of clear plastic matrix. Another glass [Abs (aliphatic) / Abs (aromatic)]monomer
Table 3 Two-way ANOVA (composite and polymerization) of bond strength data (MPa) yielded by standard vs pro-
longed polymerization
Composite: Filtek Z100, Premise, and Premise Indirect. Standard polymerization: Filtek Z100 and Premise: 40 s of light polymerization; Premise Indirect:
40 s of light polymerization + 10 min heat (previous study). Prolonged polymerization: Filtek Z100, Premise, and Premise Indirect: 40 s of light polymerization
+ 20 min heat (present study).
Table 4 Two-way ANOVA (composite and time of measurement*) of degree of conversion data (%) of the present
study
Composite: Filtek Z100, Premise, and Premise Indirect. *Time of measurement: data collected immediately and after 24 h.
Table 5 Univariate analysis of variance (composite, time of measurment, and polymerization) of degree of conver-
sion data (%) of the comparison between standard and prolonged polymerization
Composite: Filtek Z100, Premise and Premise Indirect. Time of measurement: degree of conversion data collected immediately and after 24 h. Standard
polymerization: Filtek Z100 and Premise: 40 s of light polymerization; Premise Indirect: 40 s of light polymerization + 10 min heat (previous study). Prolonged
polymerization: Filtek Z100, Premise, and Premise Indirect: 40 s of light polymerization + 20 min heat (present study).
where Abs was the area of absorption band. Monomer The degree of conversion data of the present study
conversion was determined by subtracting the residual were submitted to two-way ANOVA (composite and imme-
percentage of aliphatic C=C from 100% (DC%=100- diate vs 24-h DC) (Table 4). Then, the interaction between
[%C=C]).1,14,31,39 “standard” and “prolonged” polymerization was explored
with univariate ANOVA with three fixed factors: composite
Statistical Analysis (3 levels, Filtek Z100, Premise and Premise Indirect), DC
The data were submitted to Lilliefors (bond strength) (2 levels, immediate and after 24 h), and polymerization
and Kolmogorov-Smirnov (monomer conversion) normal- method (standard and prolonged), and three interaction
ity tests. All data were considered normally distributed terms (material × 24-h DC, material × polymerization, and
(p > 0.05) and a parametric test was chosen. 24-h DC × polymerization) (Tables 5 and 6).
Two-way ANOVA (composite and polymerization) was When interactions were significant with the full facto-
conducted on the bond strength data to verify the interac- rial model, Tukey’s HSD post-hoc test was used to detect
tion between already published data29 and the present pairwise differences (α = 0.05).
study (Table 3).
Table 6 Two-way analysis of variance (polymerization and time of measurement*) of the degree of conversion
data yielded by standard and prolonged polymerization for each material
Two-way ANOVA (polymerization and time of measurement) of Premise degree of conversion data (%)
Two-way ANOVA (polymerization and time of measurement) of Premise Indirect degree of conversion data (%)
* Time of measurement: data collected immediately and after 24 h. Standard polymerization: Filtek Z100 and Premise: 40 s of light polymerization; Premise
Indirect: 40 s of light polymerization + 10 min heat (previous study). Prolonged polymerization: Filtek Z100, Premise, and Premise Indirect: 40 s of light poly-
merization + 20 min heat (present study).
100
Bond Strength (MPa)
80
60 72.24 75.69
80
Monomer conversion (%)
70
60
Fig 4 Mean and standard deviation of
monomer conversion (%).*Previous study:
50 for Filtek Z100 and Premise, 40 s of light
53.17 56.77 51.02 53.45 56.13 66.28 68.7 71.74 50.81 58.25 61.77 72.77 polymerization; for Premise Indirect, 40 s
40 of light polymerization + 10 min heat cur-
Z100 Premise Premise Indirect ing. **Present study: for all materials,
Composite resins 40 s of light polymerization + 20 min heat
curing.
Table 7 Analysis of fracture The silane works like a primer, improving the chemical
reaction between the methacrylate and the filler by the
Filtek Z100 Premise Premise In- formation of siloxane bonds.33,44,48
direct The high bond strength achieved with Filtek Z100 (in
Adhesive 86.59% 77.36% 83.58%
both methods of polymerization) may be explained by its
failure intrinsic mechanical properties and chemical composi-
tion, since heat treatment did not influence the monomer
Cohesive 12.20% 22.64% 10.45% conversion or MTBS values. The filler and the monomer it-
failure
self along with the monomer conversion play an important
Mixed failure 1.22% – 2.99% role in the physical behavior of composite resins.2,7,8,10,37
For Filtek Z100, the volume percent of filler is slightly
lower than in Premise or Premise Indirect, and the major
filler is spheroidal zirconia-silica, instead of barium-silica
DISCUSSION as in Premise and Premise Indirect. All materials tested
shared the same monomers, ie, bis-GMA and TEG-DMA.
The first part of the null hypothesis was partially re- The combination of zirconia, bis-GMA, and TEG-DMA might
jected. The bond strength to Filtek Z100 was signifi- be responsible for the high mechanical properties found
cantly higher than Premise and Premise Indirect, which in Z100. The use of a resin matrix with 50% bis-GMA and
showed similar behavior for both variables tested. The 50% TEG-DMA was found to present the highest strength
second part of the null hypothesis was partially rejected, and elastic modulus.2,43 Bis-GMA has high viscosity due
because prolonged heat treatment positively influenced to the hydrogen bonding interactions that occur between
the bond strength and monomer conversion of Premise the hydroxyl groups on the monomer molecules. Thus, bis-
and Premise Indirect, but not that of Z100. GMA must be diluted with TEG-DMA to decrease viscos-
The present research was designed to determine the ity and enhance copolymerization characteristics.2,18,24
bond strength and degree of monomer conversion of three Resin matrix strength is dependent upon monomer com-
light- and heat-polymerized composite resins used as in- position, being greatest when stiff bis-GMA molecules are
direct restorations. Previously published data generated used and the monomer conversion of the methacrylate
by the same operator under identical conditions (which groups is maximized.19 It appears that stiffness and hard-
includes the same batch of materials), but with a different ness of Filtek Z100 when only light cured exceeds that
method of polymerization (light only for Z100 and Premise, of indirect light and heat-polymerized composite resins.7
and only 10 min heat curing in proprietary oven for Prem- The flexural strength of the Filtek Z100 was also reported
ise Indirect) were included for comparison.29 Prolonged to be higher, approximately 180 MPa,7 compared to 128
heat treatment was used in the present study because it and 158 MPa for Premise and Premise Indirect, respect-
may enhance radical mobility and polymerization rate, re- ively (manufacturer’s information). It can be hypothesized
sulting in a superior cross-linking density and final degree that the proprietary spheroidal filler provided improved
of conversion.21,14,46 These in turn may lead to enhanced rheological properties and optimized bis-GMA:TEG-DMA
physical properties.3 After the polymerization procedures, ratios in Filtek Z100. Its slightly lower volume percent of
the composite resins received the appropriate surface filler might also explain the improved bond strength (more
treatment for indirect restorations, namely, airborne par- resin matrix exposed).
ticle abrasion and silane application.33 Airborne particle Based on the data from the present study, it might
abrasion is important to produce strong bonds by expos- seem that an inverse correlation exists between the bond
ing the fillers and roughening the surface (increases the strength and the amount of monomers available at the
surface area) for wetting and bonding.11,13,25,34,35,38,44,45 surface of the composite (Z100 compared to Premise and
Premise Indirect). Bond strength is dependent on uncov- wavelength range) have reduced the differences in mono-
ered C=C double bonds in the resin, which may be attrib- mer conversion between light- and heat-curing materials.
uted either to a low conversion rate or a high level of ma- However, it must be emphasized that the indirect compos-
trix resin. The high degree of conversion makes the attach- ite resins requiring a heat initiator must be placed in a cur-
ment of a new composite material more difficult.4,24,33 ing oven to eliminate benzoyl peroxide, which is toxic.18
However, the higher conversion rate of Premise and Prem-
ise Indirect following prolonged heat treatment did not
correlate with lower MTBS values. The explanation may lie CONCLUSION
in the fact that increased mechanical properties resulting
from heat treatment ultimately influence the results of the Filtek Z100 showed the highest MTBS and lowest mono-
MTBS. Increases in diametrical tensile strength, compres- mer conversion rate. Comparison with previously pub-
sive strength, modulus of elasticity, toughness, improved lished data revealed that prolonged heat treatment was
dimensional stability,49 wear,20,37 hardness, and color advantageous in terms of improved MTBS and monomer
stability49 have been observed following heat treatment. conversion for Premise and Premise Indirect.
The FT-IR analyses of this study showed degree of
conversion to range from 53.45% to 72.77%. This is in
total agreement with existing data about multifunctional ACKNOWLEDGMENTS
monomers used for dental restorations.1,14,20,24,37,46,48 The authors wish to thank the Kerr Sybron Corporation and 3M
The improvement in some of the properties (fracture ESPE for supplying the composites and adhesive used in this
toughness, flexural modulus, and flexural strength) ob- study. Moreover, a special thanks to Hector Garza and Al Kobash-
tained by heat treating light-polymerized composite resins igawa from Kerr Sybron for assistance with FT-IR analysis.
was found to be only short term, as it seems to be negated
by water sorption during aging.18 On the other hand, clinical
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