RESEARCH ARTICLE

Color Stability and Polymerization Behavior of Direct

Esthetic Restorations
DAYANE CARVALHO RAMOS SALLES DE OLIVEIRA, DDS, MS, PhD*,
EDUARDO JOS SOUZA-JNIOR, DDS, MS, PhD*, LCIA TRAZZI PRIETO, DDS, MS, PhD*,
ERICK KAMIYA COPPINI, DDS, MS, PhD*, RODRIGO ROCHA MAIA DDS, MS, PhD,
LUS ALEXANDRE MAFFEI SARTINI PAULILLO, DDS, MS, PhD

ABSTRACT
Objectives: The current study evaluated the effect of accelerated artificial aging (AAA) on the color stability (CS) and
degree of conversion (DC) of nanofilled and nanohybrid resin composites associated to different adhesive systems in
direct esthetic restorations.
Material and Methods: Eighty bovine incisors were used to obtained dentin blocks (4 4 1 mm). The restorative
systems were bonded to the blocks and photoactivated according to the manufacturers instructions. Three adhesive
systems were used: Adper Scotchbond Multi-Purpose (conventional of three steps), Tetric N-Bond (conventional of
two steps) and ClearFill SE Bond (self-etching). Also, two composites were used: Filtek Z350 XT (nanofilled) and IPS
Empress Direct (nanohybrid). The restorations were made using a silicone mold placed on top of the prepared dentin
blocks (N = 10). CS was measured after 300 hours of AAA by means of ultraviolet light using a spectrophotometer
and CIE L*a*b* parameters on the top surface of the composite and at the bonded interface. The DC was performed
using Fourier transform infrared spectroscopy (N = 10). Data were analyzed using two-way analysis of variance and
Tukeys test ( = 0.05).
Results: The adhesive systems had no significant influence on the color stability (E) of either the restoration surface
( = 0.90) or the bonded interface ( = 0.78). However, composite influenced the color as measured by E and
isolated coordinates ( < 0.001). The nanohybrid composite showed increased DC values (67%) compared with the
nanofilled (61%) with statistically significant differences ( < 0.001).
Conclusions: The adhesive system did not affect the final color of direct esthetic restorations. The nanohybrid
composite demonstrated a higher DC and increased color stability after AAA compared to the nanofilled composite.

CLINICAL SIGNIFICANCE
The long-term color stability of composite restorations is a critical aspect of esthetic restorative procedures. Optimal
Polymerization behavior of resin composite as indicated by the degree of conversion also influence on the color
stability after artificial aging of composite restorations.
(J Esthet Restor Dent 26:288295, 2014)

INTRODUCTION
Resin composite materials have been widely used in
direct esthetic restorative procedures. The

clinical challenges of direct resin restorative

techniques include the attainment and maintenance of
color match with natural tooth structure. In fact, one of
the most common reasons for re-intervention and

*Student, Restorative Dentistry Department, Piracicaba Dental School State University of Campinas, 901 Limeira Ave, Areio, Piracicaba, 13414-903, SP, Brazil

Assistant Professor, Restorative Dentistry Department, College of Dentistry & Dental Clinics The University of Iowa, Iowa City 52242-1010, IA, USA

Full Professor, Operative Dentistry Department, Piracicaba Dental School State University of Campinas, 901 Limeira Ave, Areio, Piracicaba, 13414-903, SP, Brazil

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restoration replacement is failure in esthetics.1 The

color stability of direct restorations can be decreased by
the surface degradation of the resin material,24 and the
bond interface can also be degraded causing
color change as clinically observed in esthetic
restorations.5
The nal appearance of direct and indirect
restorations can be aected by the type of
materials and related physical properties, underlying
substrate, thickness, and translucency of restorative
materials and adequate polymerization.57 The clinical
relevance and the factors that inuence color
modication among direct resin composite
adhesives and restorations need further scientic
investigation.
Still, various factors can aect color data,
including the subjacent substrate of the restoration
through a translucent material.3,68 Restorative
studies of color analysis should consider
standardization not only of the tested materials, but
also the subjacent substrate to assure valid data.
Therefore, the aim of this study was to
evaluate the eect of accelerated articial aging on the
color stability and degree of conversion of nanolled
and nanohybrid resin composites associated with
dierent adhesive systems in direct esthetic
restorations using a standardized technique
proposed for color analysis. The tested hypotheses
were:
(1) The adhesive system will aect the nal
color of the direct composite
restorations
(2) Accelerated articial aging will compromise the
color stability of the direct restorations

MN, USA) and a conventional of two steps (Tetric

N-Bond, Ivoclar Vivadent, Schaan, Lietchtenstein), and
a self-etching adhesive (ClearFill SE Bond, Kuraray,
Noritake, Japan). Two EA1 shade resin composites were
tested: a nanolled (Filtek Z350 XT, 3M ESPE, St. Paul,
MN, USA) and a nanohybrid (IPS Empress Direct,
Ivoclar Vivadent, Schaan, Lietchtenstein), as presented
in Table 1.
In vitro conditions were standardized to more
accurately evaluate the color stability of direct
restorations and control for confounding factors that
may aect color change. Shade A1E composite
was used for all specimens with a standard thickness of
1 mm. To standardize the dentin substrate, at
dentin blocks (4 4 mm and 1-mm thick) were
made from 80 bovine incisors and standardized to
similar L* parameter (10090) by a previous
color analysis in order not to aect the color
measurements.
The dentin specimens were restored with the respective
adhesive-resin composite system with each adhesive
system used according to the manufacturers
instructions (six groups, N = 10). A group of
non-bonded specimens (N = 10) were used as a control.
Each composite increment of 1 mm thick was
photoactivated by a light-emitting diode for 20 seconds
(Radii, SDI, Bayswater, Vic., Australia800 mW/cm2).
Irradiance was previously measured using a radiometer,
in order to standardize the energy dose. The restored
specimens were water stored at 37C for 24 hours to
ensure the stabilization of the polymer network. After
storage, specimens were polished using an abrasive
discs for 10 seconds (SofLex, 3M/ESPE, St. Paul, MN,
USA). The thickness of each specimen was veried
using a digital caliper (Digimess, Mitutoyo Corporation,
Tokyo, Japan).

MATERIAL AND METHODS

Color Analysis

Specimens Preparation

The color was measured according to the CIE L*a*b*

color scale relative to the standard illuminant D65 over
a white background using a spectrophotometer
(EasyShade Advanced, Vita Zahnfabrik, Bad Sckingen,
Germany)916 according to the readout region:

For this study, three adhesives systems were used: two

etch-and-rinse adhesives: a conventional of three steps
(Adper ScotchBond Multi-Purpose, 3M ESPE, St. Paul,

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TABLE 1. Material, product, manufacturer, and composition of resin composites and adhesive systems used
Material

Product

Manufacturer

Composition

Nanofilled resin
composite

Filtek Z350 XT, EA1

3M ESPE, St. Paul, MN,

USA

Similar mixture of Bis-GMA, Bis-EMA, UDMA and TEGDMA with

nanoparticles of non-agglomerated silica and zirconia/silica nanoclusters
(59.5 vol%).

Nanohybrid resin
composite

IPS Empress Direct,

EA1

Ivoclar Vivadent,
Schaan,
Lietchtenstein

Mixture of UDMA (1025%), Bis-GMA (2.510%) and TEG-DMA

(2.510%) with barium glass, ytterbium trifluoride, mixed oxide, silicone
dioxide and co-polymer (5259 vol%).

Conventional of three
steps adhesive
system

Adper Scotchbond
Multi-Purpose

3M ESPE, St. Paul, MN,

USA

Primer: HEMA, polyalkenoic acid copolymer and water.

Bond: Bis-GMA, HEMA and camphoroquinone.

Self-etching adhesive
system

ClearFill SE Bond

Kuraray, Noritake,
Japan

Primer: MPD, HEMA, hydrophilic dimethacrylates, camphoroquinone,

N-diethanol-p-toluidine, and water.
Bond: MDP, HEMA, Bis-GMA, hydrophobic dimethacrilates,
camphoroquinone, N-diethanol-p-toluidine, and silanized coloidal slica.

Conventional of two
steps adhesive
system

Tetric N-Bond

Ivoclar Vivadent,
Schaan,
Lietchtenstein

Phosphoric acid acrylate, HEMA, Bis-GMA, UDMA, ethanol, catalysts, and

stabilizers.

Bis-GMA = Bisphenol A glycidyl methacrylate; Bis-EMA = ethoxylated bis-phenol A methacrylate; MPD = methacryloyloxi-dihydrogen-phosphate;
UDMA = urethane dimethacrylate; TEGDMA = triethylene-glycol di-methacrylate; HEMA = 2-hydroxyethyl methacrylate.

290

E = ([ Lf Li ]2 + [ a f ai ]2 + [ bf bi ]2 )

0.5

(1) restoration top surface coupled to a teon specimen

holder (4 4 mm and 2-mm thick); (2) bonded interface
coupled to a dierent specimen holder (4 2 mm and
4-mm thick) at the following times: (2.1) 24 hours after
nishing and polishing procedures; (2.2) after 300 hours
of ultraviolet (UV) accelerated articial aging (AAA).
For the color evaluation of the bonded interface the
specimens were laterally placed and the
spectrophotometers tip was positioned at the
tooth/restoration interface to assure color measurement
of this specic area.

The isolated coordinates were also analyzed separately

to compare the variation of the color axes following the
formulas: L = L*f L*i; a = a*f a*i and b = b*f b *i,
in which i represents the initial analysis and f the
nal analysis of each specimen.17

All specimens had a spherical bur mark placed in

the opposite adhesive interface to ensure color
measurements were made at the same surface for
accurate comparison of the specimens initial and nal
color after aging. Spectrophotometers collect spectral
data from the reected light and automatically translate
these data into the three-color coordinates (L* =
lightness, +a* = red, a* = green, +b* = yellow, b* =
blue), according to CIE L*a*b* system. Color stability
was evaluated by color variation (E) using the
formula:

To evaluate color stability, the specimens were

submitted to accelerated articial aging EQ-UV
(Equilam, Diadema, So Paulo, SP, Brazil). The
standardized conditions of AAA consisted of 4 hours of
exposure to UV-B light at 50C and 4 hours of water
storage at 50C for a period of 300 hours.18 The color
change occurred in the rst 300 hours of the aging
process,19 which is considered equivalent to 1 year of
clinical service.6 After AAA, the color was measured
again using the same process previously described for
color assessment.

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Degree of Conversion by Fourier transform infrared

spectroscopy (FTIR) Spectrometry

RESULTS
Color Analysis

The DC was determined according to a method

previously reported20 using a FTIR spectrophotometer
(Spectrum 100, PerkinElmer, Waltham, MA, USA). The
transmission spectra were recorded using 16 scans at a
resolution of 1 cm1 of a non-polymerized resin sample
within a matrix (d = 4 1-mm thickness). After the
infrared spectral scan, the resin was irradiated (adjusted
to 800 mW/cm2) through the transparent discs for 20
seconds with the light-emitting diode (Radii). After 48
hours, the DC of the specimens was again scanned for
their FTIR spectra collection. The number of remaining
carbon double bonds was determined. The remaining
unconverted carbon double bonds were calculated by
comparing the percentage of aliphatic C = C (vinyl)
absorption (1638 cm1) with aromatic C = C absorption
(1608 cm1) between cured and uncured specimens
(N = 10), in which the aromatic double bond stretching
bands remain constant during polymerization reactions
and serve as an internal standard. The DC was
determined by subtracting the residual percentage of
polymerizable aliphatic double bond from 100% and by
the following equation:

DC (% ) = 1 Xa Ya Xb Yb 100

in which Xa and Xb are the bands of polymerizable

aliphatic double bond after (Xa) and before (Xb)
light activation, and Ya and Yb are the bands of
aromatic double bond after (Ya) and before (Yb) light
activation.

The E, L*, and b* presented statistically signicant

dierences among the resin composites (p < 0.0001) and
no signicant dierence was found for the E in
relation to the adhesive system, as shown in Table 2. For
the E values, Tukeys test showed that none of the
adhesive systems showed statistically signicant
dierences. The nanohybrid resin composite showed
greater color stability compared with the nanolled
Z350. Both composites had considerable color change
upon aging, even though the dierence between
composites was not signicant (Table 3).
The L* and b* mean values of Tukeys test (Tables 3)
revealed that the nanolled composite had greater
variation in blue-yellow and brightness coordinates, as
shown in Table 4, compared with the nanohybrid
composite, indicating that this composite presents
increased yellowing and opacity.

Degree of Conversion by FTIR Spectrometry

The two-way ANOVA showed signicant dierences
between the resin composites (p < 0.0001). Tukeys test
showed that the monomer conversion was higher (67%)
for nanohybrid composite when compared with

TABLE 2. E values (means and standard deviations) from

the top surface and the bonded interface of the tested
adhesives systems
Adhesive system

Top surface of
the composite

Bonded
interface

Self-etching

23.7 (5.2) a

16.1 (5.2) a

Conventional of three steps

24.0 (5.7) a

15.4 (4.7) a

Conventional of two steps

23.8 (4.6) a

15.6 (4.6) a

No adhesive system

23.1 (5.0) a

16.7 (4.4) a

Statistical Analysis
For statistical analysis, data were collected and
submitted to two-way analysis of variance (ANOVA)
and Tukeys test. These tests were used to assess the
mean dierences between the control and tested
groups, and also before and after aging using the type of
material and aging status as independent variables. In
all cases = 0.05 level of statistically signicant
dierences was selected.

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Mean value of 22 specimens with standard deviation in parentheses.

Same lowercase letters in same column indicate no statistically
significant differences.

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TABLE 3. E, L*, and b* (means and standard deviations) of the top surface of the resin composites tested
Resin composite

Color change values

E

L*

b*

a*

Nanofilled

26.7 (4.2) a

8.4 (1.8) a

+25.8 (3.9) a

+2.4 (0.7) a

Nanohybrid

20.6 (3.9) b

4.28 (1.6) b

+20.2 (3.8) b

0.3 (0.4) b

Same lowercase letters in the column indicates no statistically significant differences.

TABLE 4. L*, b*, and a* initial and final values (means and standard-deviations) of the top surface of the resin composites tested
Resin composite

Coordinate values
Li

Lf

bi

bf

ai

af

Nanofilled

91.53 (2.0)

86.02 (2.6)

19.04 (1.6)

46.26 (2.2)

1.00 (0.2)

1.81 (1.0)

Nanohybrid

90.64 (1.5)

87.68 (2.5)

22.2 (1.9)

41.97 (3.5)

0.30 (0.4)

0.16 (1.1)

Li, L* initial; Lf, L* final; bi, b* initial; bf, b* final; ai, a* initial; af, a* final.

TABLE 5. Degree of conversion values (means and standard

deviations) of resin composites evaluated
Resin composite

Degree of
conversion (%)

Nanofilled

61% (1.8) b

Nanohybrid

67% (0.8) a

Same lowercase letters in the column indicates no statistically

significant differences.

nanolled composite (61%), as can be observed in

Table 5.

DISCUSSION
The rst hypothesis stating that the adhesive system
would aect the nal color of the composite
restorations was rejected because neither of the
adhesives in the present study aected color change
under the resin composite. Studies have demonstrated
that the subjacent substrate can aect the nal
color of a translucent resin composite restoration.368
However, this study showed that unlike materials like
liners21 and luting cements,22 the adhesive interface of
direct restorations does not aect color stability.
As described in literature, liners and cements are not
able to promote color modication due limited

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thickness in relation to other materials studied.7,21,22 It

should be considered that dierences in color changes
among dierent studies may be related to variations in
samples thicknesses.23 For this reason, the present study
standardized the specimens thickness to 1 mm
simulating a minimally invasive esthetic restoration.
The second hypothesis stating that the accelerated
articial aging would compromise the color stability of
the direct restorations was accepted, once CIE Lab
coordinates values of all composite resins tested were
signicant dierent after submitted to articial
accelerated aging, as shown on Tables 3 and 4. Color
stability is an important property of composites used in
esthetic restorations, and several factors are associated
with alterations of this property, such as the
composition of the resin matrix,8,24,25 which can
interfere with the refractive index and consequently the
translucency.26 The material thickness also can aect
the translucence.26 Due to the standardization of the
thickness of the composites in the current study, it can
be assumed that the translucency was altered by the
refractive index modication, in which the nanolled
composite resin might have greater modications,
probably due to its inorganic pattern.3
Because the specimens were not exposed to any
staining agent, the related optical property alterations
resulted from internal physical-chemical reactions. The

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reduction in L* values after aging is due to the presence

of unreacted carbon double bonds, making the
composite more susceptible to degradation, according
to the degree of conversion,2 which also alters the
refractive index by a scattering pattern leading to
change in the opacity of the composite,3,27 thus
explaining the better results with the nanohybrid
compared with nanolled composite.
Commonly, the organic matrix of resin restorative
materials is composed primarily of Bisphenol A glycidyl
methacrylate (Bis-GMA, Mw = 512 g/mol), a highly
reactive molecule. However, the presence of phenolic
groups in its backbone, impairing rotation about the
bonds and the strong intermolecular interactions given
by hydroxyl groups result in a very viscous material and
lower degree of conversion28 compared with other
monomers.29 In order to increase conversion and allow
the incorporation of high ller levels, composite
formulations include one or more monomers with
lower viscosity, such as triethylene-glycol
di-methacrylate (TEGDMA, 286 g/mol), urethane
dimethacrylate (UDMA, 470 g/mol), or ethoxylated
bis-phenol A methacrylate (Bis-EMA, 540 g/mol).30
UDMA is an aliphatic high molecular weight monomer
that has two amine groups (-NH-), which form
intermolecular hydrogen bonds, increasing its viscosity.
The aliphatic molecule gives the polymer mobility,
thereby increasing the conversion degree.29 This study
demonstrated that the partial replacement of Bis-GMA
by UDMA leads to an increased degree of
conversion28,30,31 and lower plasticization of organic
matrix,31 as observed by the nanohybrid results
(Table 5).
Double bonds in aromatic amines may be a possible
explanation for the increase in yellowing because these
conjugate systems are capable of absorbing UV light,
thereby creating higher energy states. These active
molecules may react with oxygen, commonly with other
aromatic groups, or with small organic molecules that
may be incorporated during material manipulation.
From this reaction, bigger and more conjugated
systems, also called color centers or chromospheres are
formed, which increase visible light absorption,

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especially in the blue region of the electromagnetic

spectrum, thus yellowing the material.32
A greater yellowing eect is expected with a higher
amine rate because the excess of amine has a great
potential for darkness due to oxidative reactions.33 Even
if it is not possible to measure the concentration of
unreacted amine for each composite, it is predicted that
the increased yellowing with nanolled composite
occurred because of the lower conversion degree.
Furthermore, physical surface modications caused by
aging enable color change because of exposure to
staining agents.34 The higher plasticizing eect of the
nanolled composite35 possibly leads to the matrix resin
modication and greater staining in clinical situations
compared with a microhybrid composite such as the
nanohybrid composite.36
In general, E = 02 is considered clinically
imperceptible; E> 23, slightly noticeable change; E>
38, moderate noticeable change; and E> 8, severely
noticeable change.37 As observed in this study, either
nanohybrid or nanolled resin composites induced
clinical color change, although nanohybrid resin
composite achieved better color stability, possibly
predicting better clinical follow up outcomes.

CONCLUSIONS
In conclusion, the adhesive system tested did not aect
the nal color of direct resin composite restorations;
the nanohybrid resin composite demonstrated a higher
DC and increased color stability after AAA compared
to the nanolled composite, which were indicative of
better clinical performance.

DISCLOSURE AND ACKNOWLEDGEMENTS

The authors do not have any nancial interest in any of
the companies whose products are included in this
article.
This study was supported by the CAPES grants.

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Reprint requests: Dayane Carvalho Ramos Salles de Oliveira, DDS, MS,

PhD, Piracicaba Dental SchoolState University of Campinas,
Restorative Dentistry Department, 901 Limeira Av. Areio, Piracicaba
13414-903, SP. Brazil; Tel.: +55 19 21065200; email: dayoli87@gmail.com

Journal of Esthetic and Restorative Dentistry

Vol 26 No 4 288295 2014

295

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