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J Can Dent Assoc 2014;80:e12
l’Association dentaire canadienne 2010;76:aXXX

Effect of Preheating on Microhardness and

Viscosity of 4 Resin Composites
Karen V. Ayub, DDS, MSc; Gildo C. Santos, Jr., DDS, MSc, PhD;
Amin S. Rizkalla, BSc, MEng, PhD; Richard Bohay, DMD, MSc;
Luis Fernando Pegoraro, DDS, MSc, PhD; José H. Rubo, DDS, MSc, PhD;
M. Jacinta M.C. Santos, DDS, MSc, PhD

Abstract
Objective: This study was undertaken to determine the effect of temperature on the microhardness and viscosity of 4 resin
composite materials.
Methods: To investigate microhardness, samples of each of the 4 composite materials, prepared by standard insertion of resin
into prefabricated moulds, were divided into 2 groups (n = 10 per group). On the first group, the resin composite materials were
inserted into the moulds at room temperature and cured. On the second group, the resin composite materials were pre-heated
in a heating device, inserted into the moulds and immediately cured. Microhardness after curing (both immediately and after
24 hours of storage) was determined (using a 300 g load applied for 10 seconds) and averaged for 5 randomly selected points
on the top and bottom surfaces of each sample. To investigate viscosity, 0.5 g samples of room temperature or preheated resin
composite (n = 15 per group) were placed under a 454 g load for 45 seconds before light-curing (40 seconds). After curing, each
sample was photographed and the surface area calculated. Data were analyzed by t tests or one-way analysis of variance and
Tukey’s test.
Results: Preheating the resin composites increased the microhardness and decreased the viscosity of the samples. Filtek Supreme
Ultra resin composite had the highest mean microhardness, and Vit-l-escence resin composite had the lowest viscosity.
Conclusions: The effects of preheating resin composites may allow easier placement of restorations and greater monomer
conversion.

D
espite improvements in resin sion and wear, toxicity, marginal leak-
composite materials, some age and recurrent caries.1-5
drawbacks still compromise the To overcome these problems,
longevity of resin composite restora- attempts have been made to improve
tions. The most frequently reported the mechanical properties of these
limitations are related to shrinkage materials, including changes in the
during polymerization, mismatch in amount, size and type of fillers and/
thermal expansion, resistance to abra- or the use of non-methalcrylate-based

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Table 1: Characteristics of resin composites investigated in this study

jadc Average filler

Material Shade Composition Manufacturer Lot no. size (μm)
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Vit-l-escence A2 Resin: Bis-GMA, UDMA Filler: 71.5 % by wt. Ultradent (Salt B5YZB Publié par 0.7
l’Association dentaire canadienne
(microhybrid) silinated strontium borosilicate, silinated Lake City, UT,
silicon dioxide USA)
Tetric Ceram HB A2 Resin: Bis-GMA, dimethacrylates Filler: Ivoclar Vivadent P03082 0.04–3.0
(microhybrid) 68.4 wt% barium glass filler, Ba-Al- (Schaan,
fluorosilicate glass, dispersed silica Liechtenstein)
Filtek Supreme Ultra A2 Resin: Bis-GMA, UDMA, TEGDMA, Bis-EMA, 3M ESPE (St N277991 0.6–1.0
(nanofilled) PEGDMA Filler: 72.5 wt% zirconia/silica Paul, MN, USA)
Filtek LS Low Shrink A2 Resin: polysilorane Filler: 73 wt% quartz 3M ESPE (St N128586 0.1–2.0
Posterior Restorative Paul, MN, USA)
System (microhybrid)

Bis-EMA = ethoxylated bisphenol A glycol dimethacrylate, Bis-GMA = bisphenol A-glycidyl methacrylate, PEGDMA = polyethylene glycol dimethacrylate, TEGDMA =
tetraethylene glycol dimethacrylate, UDMA = urethane dimethacrylate.

monomers. As well, different clinical procedures Microhardness has often been used to assess
have been proposed to compensate for the stress the physical properties of restorative materials,
associated with polymerization shrinkage and to and this property correlates well with the degree
facilitate better marginal adaptation between the of conversion of resin composites.23,25-28 Therefore,
resin composite and the cavity walls. Several tech- this study was undertaken to determine the effect
niques for placing restorations 6-9 have been sug- of preheating on microhardness (measured as
gested to improve the seal of resin composite res- Knoop hardness number [KHN]) and viscosity
torations, such as incremental layering to reduce (measured as area after compression) of 4 resin
the configuration factor, 10 soft-start and pulsed- composite materials. The following null hypoth-
curing methods to modify the reaction rate11 and eses were considered:
use of flowable composites to promote better mar- 1. There is no significant difference in mean post-
ginal adaptation.7,8 Flowable composites, with their curing microhardness between preheated sam-
marked fluidity, have been frequently advocated as ples of resin composite and samples cured at
stress absorbers and adaptation promoters.7-9,12,13 room temperature without preheating.
However, because of the lower filler content of flow- 2. There is no significant difference in mean post-
able composite materials, greater polymerization- curing microhardness among different resin
induced stress is expected relative to standard composite restorative materials.
resin composites.14-16 3. There is no significant difference in the vis-
Studies have suggested that heating traditional cosity of different resin composites under dif-
resin composites can improve marginal adaptation ferent temperature conditions.
by enhancing fluidity.16,17 In addition, preheating
composites may improve their physical and Materials and Methods
mechanical properties through a higher degree
of monomer conversion,14,18-22 which has in turn Microhardness
been associated with greater mechanical strength, Four resin composite restorative materials
rigidity and resistance to degradation in the oral (Table  1), 3 methacrylate-based composites and
environment. 23 Conversely, incomplete polymer- 1 silorane-based composite, were used to prepare
ization can lead to increased wear due to reduced a total of 80 disk-shaped samples (20 samples of
mechanical strength, and unreacted monomers each composite). The samples were prepared by
may be cytotoxic, leading to allergic and sensi- inserting uncured resin composite into circular
tivity reactions.24 metallic moulds (5 mm diameter × 2 mm height).

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Table 2: Temperature of resin composites recorded after preheating at 68°C for 40 minutes

Time after end of preheating; temperature (°C) jadc

Decline in
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Material 0s 15 s 30 s 45 s temperature (°C)a
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Publié par
Vit-l-escence 54.4 53.4 51.5 49.2 5.2
l’Association dentaire canadienne

Tetric Ceram HB 54.8 52.7 50.1 46.1 8.7

Filtek Supreme Ultra 55.3 53.1 50.5 48.0 7.3
Filtek LS 55.6 53.1 49.8 47.1 8.5

Total decline in temperature from 0 to 45 seconds after end of heating.

a

The moulds were covered with a polyester strip Between measurements, the samples were stored
and a clear glass cover slip (Micro Slides, Gold at 37°C in distilled water in a darkened incubator.
Seal) on both upper and lower surfaces to remove
Viscosity
excess material and standardize surface finishing.
The viscosity of each of the 4 resin compos-
The samples of each composite were divided into
ites was measured at room temperature with and
2 groups of 10 samples each. For each composite,
without preheating. Preheating (to the same tem-
one group of samples was light-cured at room
perature as used for the microhardness tests) was
temperature (24°C ± 1°C) without pretreatment,
accomplished with a hot platform (Advanced
and the other group was light-cured after pre-
Hot Plate Stirrers, VWR). Sample temperature
heating. Light-curing was applied to the top sur-
was verified with a thermometer (HRC5A Heater
face of each sample for 40  seconds with a light-
Controller, Thermocouple). Viscosity was deter-
emitting diode curing unit (Valo, Ultradent).
mined by calculating and comparing the sur-
The light intensity was nominally 1200  mW/cm 2
face area of 0.5  g samples of each material. Each
and was checked with a radiometer (Patterson
sample (n  = 15 for each material) was placed
curing light meter). For the 4 groups of samples
between 2 glass slides under a load of 454  g for
that were preheated before light-curing, each
45  seconds to obtain a flat surface before light-
resin composite material was placed in a heating
curing for 40  seconds with the same light-curing
device (CalSet  3 temperature unit, AdDent) for unit described above. After curing, a digital photo-
40  minutes at the highest setting (68°C). Each graph of each sample was obtained and the surface
resin composite material was inserted into the area calculated using Image  J software (version
mould within 45  seconds after removal from the 1.44, National Institutes of Health, http://rsbweb.
heating device. The metallic moulds, clear glass nih.gov/ij/).
cover slips and plastic filling instrument were all Data were recorded in an Excel spread-
warmed to 37°C before insertion of the resin. The sheet (Microsoft Corp, Redmond, WA) and then
internal temperature of each preheated sample was imported into SPSS (IBM, Armonk, NY) for
determined by inserting a thermometer (HRC5A analysis. Three-way analysis of variance(ANOVA)
Heater Controller, Thermocouple) into the resin with the factors of material, time and preheating
composite syringe after the warming period. To for both top and bottom surfaces was used to
determine the rate of heat loss, additional tem- compare microhardness measurements, and 2-way
perature measurements were performed after 15, ANOVA with the factors of material and tem-
30 and 45  seconds (Table  2). The surface micro- perature was used to compare viscosity measure-
hardness was measured on the top and bottom ments. Because of significant interaction terms for
surfaces of each specimen (Knoop diamond with a both of these analyses, one-way ANOVA was used
300 g load for 10 seconds; Micromet, Buehler). Five to test for significant differences among the 4 com-
randomly selected points for each surface were posite materials. Tukey’s test was applied for pair-
measured immediately and 24 hours after curing. wise comparisons when the ANOVA result was

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Table 3: Microhardness of top surface of resin composite samples

Mean microhardness ± SD (KHN)a

% increase
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Material Not preheated Preheated with preheating p valueb
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Immediately Vit-l-escence 41.16 ± 1.19a 46.75 ± 1.26a 13.58 < 0.001
l’Association dentaire canadienne

after light-curing Tetric Ceram HB 43.70 ± 1.86b 49.07 ± 2.19a 12.29 < 0.001
Filtek Supreme Ultra 60.60 ± 1.03 70.62 ± 2.24 16.53 < 0.001
Filtek LS 42.38 ± 1.83a b
53.90 ± 2.02 27.18 < 0.001
24 hours after Vit-l-escence 52.07 ± 1.74a 57.21 ± 2.39 9.87 < 0.001
light-curing Tetric Ceram HB 52.31 ± 2.05a 53.07 ± 1.95 1.45 0.41
Filtek Ultra 70.81 ± 0.83 76.03 ± 2.24 7.37 < 0.001
Filtek LS 49.81 ± 1.26 60.14 ± 0.91 20.74 < 0.001
SD = standard deviation, KHN = Knoop hardness number.
a
Each value is the mean of 10 samples. Microhardness values for composite materials within a given column that have the same superscript capital letter are not
significantly different (p > 0.05).
b
The p value in the final column of each row refers to a comparison of mean KHN for samples of that particular resin composite that were and were not preheated.

Table 4: Microhardness of bottom surface of resin composite samples

Mean microhardness ± SD (KHN)a % of increase

Material Not preheated Preheated with preheating p valueb
Immediately Vit-l-escence 33.57 ± 2.02a 37.03 ± 1.52 10.31 < 0.001
after light-curing Tetric Ceram HB 35.52 ± 2.67ab 39.30 ± 1.83 10.64 0.002
Filtek Ultra 57.61 ± 1.06 67.61 ± 1.88 17.36 < 0.001
Filtek LS 34.33 ± 1.73ab 45.04 ± 2.02 31.20 < 0.001
24 hours after Vit-l-escence 42.60 ± 2.42a 48.13 ± 1.76 12.98 < 0.001
light-curing Tetric Ceram HB 43.19 ± 3.35ab 43.66 ± 3.90 1.09 0.78
Filtek Supreme Ultra 68.69 ± 1.71 72.27 ± 2.25 5.21 0.001
Filtek LS 44.03 ± 0.70ab 53.01 ± 1.98 20.40 < 0.001
SD = standard deviation, KHN = Knoop hardness number.
a
Each value is the mean of 10 samples. Microhardness values for composite materials within a given column that have the same superscript capital letter are not
significantly different (p > 0.05).
b
The p value in the final column of each row refers to a comparison of mean KHN for samples of that particular resin composite that were and were not preheated.

significant. Student t tests with Bonferroni correc- was a significant increase in microhardness on the
tion (p  ≤ 0.017) was used to compare microhard- top and bottom surfaces of samples of this resin
ness and viscosity measurements of samples cured composite immediately after curing, no signifi-
at room temperature with samples of the same cant increase was evident on either surface after
material cured after preheating. ` 24 hours.
Of the 4 resin composite materials tested,
Results Filtek Supreme Ultra displayed the highest micro-
hardness values under the various experimental
Microhardness
conditions.
For all but one of the resin composite materials,
mean microhardness of both the top (Table 3) and Viscosity
the bottom (Table 4) surfaces increased signifi- Preheating resin composites resulted in a sta-
cantly with preheating. The exception to this gen- tistically significant decrease in viscosity for all
eral finding was Tetric Ceram HB. Although there resin composites tested (Table  5). The materials

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Table 5: Flow area of resin composite samples prepared with and without preheating

Mean area ± SD (mm2)a % increase with jadc

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Material Not preheated Preheated preheating p value b
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Vit-l-escence 117.48 ± 17.30 151.95 ± 8.24 29.34 < 0.001
l’Association dentaire canadienne

Tetric Ceram HB 44.24 ± 8.03a 62.15 ± 5.65a 40.48 < 0.001

Filtek Supreme Ultra 58.54 ± 2.70 64.63 ± 2.21a 10.40 < 0.001
Filtek LS 44.74 ± 3.41a 77.33 ± 18.01 72.84 < 0.001
SD = standard deviation.
a
Each value is the mean of 15 samples. Area values for composite materials within a given column that have the same superscript capital letter are not significantly
different (p > 0.05).
b
The p value in the final column of each row refers to a comparison of mean area for samples of that particular resin composite that were and were not preheated.

with the highest viscosity (smallest area) at room studies, 21,25,27 which have highlighted that poly-
temperature were Tetric Ceram HB (area  44.24 ± merization starts immediately after light exposure
8.03 mm 2) and Filtek LS (area 44.74 ± 3.41 mm 2), and continues for 24  hours and that during this
with no statistically significant difference between period, a reduction in the number of free radicals
them. Vit-l-escence exhibited the lowest viscosity and a slight but significant increase in the degree
at both temperatures. of conversion is observed. Post-irradiation curing
occurs because of unreacted species with free rad-
Discussion icals that become trapped within the more rigid
network during polymerization.19 The trapped
Microhardness
radicals are the result of self-deceleration, which
On the basis of the results reported here, the takes place because of reduced mobility of both
first null hypothesis, stating that there is no sig- monomer and unreacted pendant double bonds
nificant difference in mean postcuring microhard- in the viscous media. As the polymerization reac-
ness between samples of resin composite that have tion progresses, both propagation and termina-
been preheated and those cured at room temper- tion reactions become diffusion-controlled.19-21,33-35
ature without preheating, should be rejected. For Over time, these residual unpolymerized species
all 4 resin composites used in the present study, find pendant groups and are involved in further
mean microhardness increased with preheating, reaction. The post-irradiation hardening pattern
on both top and bottom surfaces of the samples. achieved by resin composites is characterized by
These findings are in accordance with the results enhanced polymer cross-linking.20
of previous studies. 26,28-32 The increase in mean The greater increase in microhardness achieved
microhardness of the top surface attained with at the top surface of samples relative to the bottom
preheating ranged from 1.45% (Tetric Ceram HB, surface can be explained by the attenuation of light
after 24  hours of storage) to 27.18% (Filtek LS, (because of reflection, absorption and dispersion
immediately after curing). For the bottom surface, phenomena) as it travels through the composite.
the increase in microhardness ranged from 1.09% In the current study, microhardness at the top and
(Tetric Ceram HB, after 24  hours of storage) to bottom surfaces was measured at 2  mm depth,
31.20% (Filtek LS, immediately after curing). All of the suggested increment thickness for composite
the increases were statistically significant, except placement.9,19 At a depth of 2 mm, the attenuation
that for Tetric Ceram HB resin composite after 24 of light may reduce irradiance to approximately
hours of storage. 75% of that reaching the top surface.9,32
As noted above, an increase in mean micro- It has been reported that, on average, resin
hardness was observed after 24  hours of storage composites can achieve 50% to 70% conversion of
(except with Tetric Ceram HB resin composite). monomers at room temperature. 36 During poly-
This finding is in agreement with the results of other merization, monomer conversion occurs as soon

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as exposure to light is initiated. As the reaction conversion was still superior to that achieved by
progresses, the viscosity of the resin composite
increases through the formation and growth The second null hypothesis, stating
jadc
resin composites cured at room temperature.
that there
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of polymer chains, which result in decreased are no significant differences in mean postcuring
Publié par

molecular movement. The increased viscosity pre- microhardness among the different resin compos-
l’Association dentaire canadienne

vents completion of the polymerization process ites tested, was also rejected. The Filtek Supreme
because movement of molecules in this vitrified Ultra resin composite exhibited the highest mean
state becomes limited.14,19 Conversely, preheated microhardness under the various experimental
composites exhibit increased monomer mobility, conditions investigated, and its microhardness
as a result of higher thermal energy, which was significantly greater than that of the other
leads to less viscosity and enhanced molecular materials (Table 3 and 4). These findings are in
motion.14,26,29,37 Also, any delay in both propaga- agreement with another study, in which the same
tion and termination of diffusion-controlled reac- resin composite was used.28 The high microhard-
tions will permit enhanced conversion. Such delay ness values achieved by Filtek Supreme Ultra resin
will result in a greater number of collisions, since composite may be related to the amount and type
free radicals are able to diffuse and react before of filler. This material has a high filler content
self-deceleration occurs, which in turn increases (72.5% by weight) and employs nanofiller tech-
the degree of monomer conversion before vitri- nology. Eliades and colleagues20 also found that
fication.14,19,22,31,33 Daronch and colleagues18 sug- hardness patterns are extended as inorganic
gested that curing time may be reduced by up to loading increases.
75% with preheating of composites. These authors This study included a silorane-based resin
reported that light-curing of a warmed resin com- composite (Filtek LS) for comparison with the
posite for 5 seconds resulted in a greater degree of methacrylate-based composites. Silorane resin
conversion than light-curing at room temperature composite contains a siloxane backbone with 4
for 40  seconds. Furthermore, in another study,19 attached oxirane rings that open to form a polymer
chain, which offsets the shrinkage resulting from
these authors showed that when resin compos-
monomer conversion into polymer. 38 Other studies
ites were polymerized at 3°C, the final conver-
have reported similar mechanical properties of
sion was less than 35%. The decreased monomer
siloranes relative to methacrylate-based compos-
conversion achieved at lower temperatures (e.g.,
ites. 38,39 In the present study, the mean microhard-
when resin composites are stored in the refriger-
ness of the silorane-based resin composite was
ator) was attributed to the higher viscosity of
similar to that of the methacrylate-based compos-
the material, which resulted in slower propaga-
ites tested, which is in accordance with previous
tion. A correlation between monomer conversion
reports. 38-40
and Knoop hardness values has been reported
in several studies.20,25,23,30,31 In one recent study, 25 Viscosity
the microhardness test was more sensitive than Viscosity is the property that determines
Fourier transform infrared spectroscopy in identi- the degree of molecular mobility of a resin
fying small changes in monomer conversion after composite. Preheating puts the monomers
24 hours. into a state of thermal agitation that increases
In the current study, the maximum resin tem- molecular motion, enhancing fluidity.14,26,29,37 It
perature achieved after 40  minutes of heating at has been reported that the use of low-viscosity
68°C ranged from a low of 54.4°C (Vit-l-escence) materials results in superior marginal adaptation
to a high of 55.6°C (Filtek LS). After 45  seconds, because of greater fluidity and capacity to pro-
the average temperature decline ranged from 5.2°C mote better contact with the prepared tooth sur-
to 8.7°C (Table  2). Heat loss was also reported faces.14,17 Although some studies have reported
in several other studies.19,28,29,33,37 Daronch and decreased microleakage when composites were
colleagues18 reported that even when preheated warmed,16,17 others have shown no significant dif-
composites had cooled to below 54°C, monomer ference with warming.14,37 Deb and colleagues 14

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observed that although marginal adaptation may

jadc
Dr. Pegoraro is associate professor, department
be better because of the enhanced flowability of of prosthodontics, Bauru School of Dentistry,
preheated resin composites, shrinkage may also be University of São Paulo, Bauru, SP, Brazil. DES CONNAISSANCES
DENTAIRES INDISPENSABLES
greater, because of higher monomer conversion. Publié par

They highlighted that increased shrinkage may l’Association dentaire canadienne

counteract the improved adaptation achieved by Dr. Rubo is associate professor, department
warming composites, leading to no difference in of prosthodontics, Bauru School of Dentistry,
University of São Paulo, Bauru, SP, Brazil.
microleakage of composites cured under different
temperature conditions.
The third null hypothesis, stating that there
Dr. JMC Santos is assistant professor, Schulich
is no significant difference in the viscosity of School of Medicine & Dentistry, Western
different resin composites under different tem- University, London, Ontario
perature conditions, was also rejected. Viscosity
declined with preheating for all resin composites Acknowledgments: The authors would like to thank the
MITACS Globalink Program – Western University and the
evaluated in the present study. This result is in
dental companies that kindly donated the materials for this
agreement with the results of previous investiga- study.
tions, which showed higher fluidity of preheated
composites.14,26,29,37 In addition, the extent of Correspondence to: Dr. M. Jacinta M.C. Santos, Schulich
flow differed among the resin composites tested. School of Medicine & Dentistry, Western University, Room
# 0149, Dental Sciences Building, London, ON N6A 5C1.
Vit-l-escence resin composite had the lowest Email: [email protected]
viscosity at both room temperature and after
preheating. The authors have no declared financial interests in any com-
pany manufacturing the types of products mentioned in this
Conclusions article.

Within the limitations of this in vitro study, This article has been peer reviewed.
it was determined that preheating resin compos-
ites increases their microhardness and flowability. References
These effects may result in easier placement and
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CONNAISSANCES
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INDISPENSABLES

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