Original Article

http://dx.doi.org/10.1590/1678-7757-2017-0528

Minimization of polymerization
shrinkage effects on composite resins
by the control of irradiance during the
photoactivation process

Abstract

Gabriel Felipe GUIMARÃES1 High levels of shrinkage stress caused by volumetric variations during

Edilmar MARCELINO2 the activation process are one of the main problems in the practical
application of composite resins. Objective: The aim of this study is to reduce
Ivana CESARINO1
the shrinkage stress and minimize the effects caused by composite resin
Fábio Bossoi VICENTE3
volumetric variation due to the photopolymerization. In this way, this work
Carlos Roberto GRANDINI3,4 proposes a systematic study to determine the optimal dimming function
Rafael Plana SIMÕES1 to be applied to light curing processes. Material and Methods: The study
was performed by applying mathematical techniques to the optimization
of nonlinear objective functions. The effectiveness of the dimming function
was evaluated by monitoring the polymerization shrinkage stress during the
curing process of five brands/models of composites. This monitoring was
performed on a universal testing machine using two steel bases coupled in
the arms of the machine where the resin was inserted and polymerized. The
quality of the composites cured by the proposed method was analyzed and
compared with the conventional photoactivation method by experiments to
determine their degree of conversion (DC). Absorbance measurements were
performed using Fourier-transform infrared spectroscopy (FT-IR). A T-test
was performed on DC results to compare the photoactivation techniques.
We also used scanning electron microscopy (SEM) to analyze in-vitro the
adhesion interface of the resin in human teeth. Results: Our results showed
that the use of the optimal dimming function, named as exponential, resulted
in the significant reduction of the shrinkage stress (~36.88% ±6.56 when
compared with the conventional method) without affecting the DC (t=0.86,
p-value=0.44). The SEM analyses show that the proposed process can
minimize or even eliminate adhesion failures between the tooth and the
resin in dental restorations. Conclusion: The results from this study can
promote the improvement of the composite resin light curing process by
the minimization of polymerization shrinkage effects, given an operational
Submitted: November 7, 2017 standardization of the photoactivation process.
Modification: February 21, 2018
Accepted: March 27, 2018
Keywords: Dental restoration. Composite resins. Light-curing of dental
adhesives.

Corresponding address: 1
Univ. Estadual Paulista, Faculdade de Ciências Agronômicas, Departamento de Bioprocessos e
Rafael Plana Simões Biotecnologia, Botucatu, SP, Brasil.
Phone: +55-14-3880-7512 - Fax: +55-14-3880-7162
e-mail: rafael@fca.unesp.br
2
Univ. Estadual Paulista, Instituto de Biociências, Botucatu, SP, Brasil.
3
Univ. Estadual Paulista, Faculdade de Ciências, Laboratório de Relaxações Anelásticas e
Biomateriais, Bauru, SP, Brasil.
4
Instituto de Biomateriais, Tribocorrosão e Nanomedicina - Ramo Brasileiro, Bauru, SP, Brasil.

J Appl Oral Sci. 1/9 2018;26:e20170528

 Minimization of polymerization shrinkage effects on composite resins by the control of irradiance during the photoactivation process

INTRODUCTION limited to the functions of conventional light curing

devices, which do not allow continuous variation of the

The composite resins emergence has provided irradiance during the activation.

higher aesthetic quality in dental restorations. However, Our hypothesis is that it can be possible to

the mechanical properties of the resins, especially the determine an optimal curve of irradiance variation

high levels of shrinkage stress caused by volumetric during the photoactivation, which will promote the

variations during the activation process, are the reduction of the shrinkage stress without affecting the

main problem in the practical application of these cured composites DC.

materials2,5. Considering the above, this project proposes a

Despite the chemical advances in resins for the systematic study to optimize the dimming function

minimization of the polymerization shrinkage, this in light curing processes. The study was performed

problem persists and can allow micro-infiltrations in by a mathematical approach to determine an optimal

the adhesive interface, which harm the restoration function for the irradiance modulation at the time

aesthetics and, in some extreme cases, favor the domain. This function was incorporated in a light

growth of bacteria due to marginal leakage4. curing unit, developed by our research group, which

To achieve both efficiency and quality, various can control the irradiance according to a mathematical

efforts have been made to reduce the effects of function. The effectiveness of the optimal function was

polymerization shrinkage. Current approaches include evaluated by monitoring the polymerization shrinkage

the improvement of the chemical composition of stress during the curing process. The quality of the

the resins, the photo-initiator molecules and the resins polymerized by the proposed method was

polymerization process catalysts3,11,17. experimentally analyzed to determine the conversion

However, studies have shown that the variation of degree of the monomers into polymers. The interface

some physical parameters can significantly change the adhesion between the teeth and resins was analyzed

resin shrinkage during the curing process, concluding by scanning electron microscopy (SEM).

that the radiant exitance (or emittance) of the curing

device has a correlation with the volumetric contraction
induction of photopolymerized composite resins9,15,18. It Materials and methods
has been observed a variation of shrinkage stress when
the composite is polymerized under different conditions This work has three major stages of development:
of exposure to the luminous source, being that some (1) determination of an optimal function for the
studies showed that the irradiance modulation during irradiance modulation using data from the variation
the photoactivation process has an influence on the pattern of the shrinkage stress in photoactivation
shrinkage stress modulus10. conventional processes, aiming to minimize the effects
Alternative light-activation protocols have been of the polymerization shrinkage; (2) evaluation of the
proposed to minimize the polymerization shrinkage cured composite quality by monitoring and comparing
effects . The soft-start techniques, for example,
2,10,17-19
the shrinkage stress during the polymerization and the
have been extensively studied. In this kind of DC for the conventional and proposed photoactivation
photoactivation, the polymerization is started with low methods and; (3) the use of SEM to evaluate the
irradiance for a few seconds, followed by increased adhesion interface between teeth and resins by also
irradiance for the remaining period of light-activation. comparing the conventional and proposed methods.
This process advocated as an approach to reduce the For all experiments, the following composite
shrinkage stress while maintaining proper degree of resins were analyzed: Z250 (3M Dental Products; St.
conversion (DC) of the composite3. However, there is no Paul, Minnesota, USA – Lot 386222, color A2); Z350
consensus about the time and irradiance parameters in (3M Dental Products; St. Paul, Minnesota, USA – Lot
the soft-start techniques. Therefore, in the literature, 545195, color A2D); Charisma (Heraeus Kulzer; Hanau,
it is possible to find soft-start protocols with different Hesse, Germany – Lot 010625A, color A3); NT Premium
values of irradiance and activation time, both for the (Coltene; Altstatten, St. Gallen, Switzerland – Lot
initial phase of low irradiance and for the final phase 1501559, color A2) and Ultrafill (Biodinâmica; Ibiporã,
of high irradiance16. In addition, this type of study is Paraná, Brazil – Lot 43815, color A2).

J Appl Oral Sci. 2/9 2018;26:e20170528

 GUIMARÃES GF, MARCELINO E, CESARINO I, VICENTE FB, GRANDINI CR, SIMÕES RP

All the photoactivation processes were performed testing machine (Emic DL 3000, EMIC Equipamentos
using a polymerization unit developed by our research e Sistemas de Ensaios Ltda; São José dos Pinhais,
group (patent registration number BR1020160078245, Paraná, Brazil). An adaptation using two steel bases
INPI, Brazil). This device was equipped with a was coupled in the arms of the machine, which were
second generation Light Emitting Diode (LED) (LZ4- adjusted so that the resin could be inserted and
40B208-0000, LED Engin Inc; San Jose, California, polymerized for tests10. The gap between the two stents
USA). The LED device has a typical relative spectral in which the composite was inserted was regulated with
power distribution in wavelength range of 430–480 nm a width of 1 mm. Thus, the specimen to be polymerized
(with peak at 457 nm) and power rating of 10 W. This had the following dimensions: 6 mm × 2 mm × 1
device was coupled with an optical tip (diameter of 8 mm. The LED device tip was positioned on the 6 mm
mm) and the maximum output irradiance was adjusted side of the steel base, allowing the transmission of
to be 1000 mW/cm , which was calibrated using a
2
light to the full extent of the specimen. The distance
radiometer (RD7, Ecel Indústria e Comércio Ltda; of photopolymerization was 2 mm. The device driver
Ribeirão Preto, São Paulo, Brazil). The developed device software traced the shrinkage stress curve as a function
was connected to a personal computer containing of polymerization time. This experiment was performed
a computational interface that allows the control of in triplicate for each resin brand/model.
the LED emittance along the photoactivation process Curve fitting by the least squares method was
according to a mathematical function. applied to determine the average function ,
The experiments were performed according to ISO which was considered the objective function for the
4049:2009. optimization. The mathematical minimization of the
function consisted of calculating the polymerization
Determination of optimal dimming function and shrinkage-stress rate (MPa/s), obtained by the data
monitoring of instantaneous polymerization differentiation , and with this information,
shrinkage stress determining the inverse function of the contraction
The optimal mathematical dimming function in the rate, ( )-1 . This inverse function was taken as
time domain to minimize the shrinkage stress was the optimal dimming function to minimize the effects
formulated based on the dependence of shrinkage of the polymerization shrinkage. This optimal function
stress (fc) and the time (t) in a photoactivation process was named as the exponential photoactivation method.
by applying constant luminous intensity (i). Therefore, The referred optimal function was incorporated in
the existence of a mathematical function described as the photopolymerization device, and new experiments
fc (i,t) was assumed, which models the shrinkage stress for monitoring the shrinkage stress were performed.
behavior in a conventional photoactivation process. An average function of the shrinkage stress and its
Thus, the shrinkage stress minimization can then be standard deviation was determined for each brand/
modeled mathematically by an optimization problem model of resin. The results from these new experiments
of an objective function. showed the patterns of the composite shrinkage when
Recent studies have shown that stress data can the exponential photoactivation method (iopt) was
be displayed as a continuous time function usually for applied. These results were then compared with the
30-60 min. Measurements for longer periods, such as conventional photoactivation method by applying the
24 h, are also feasible due to the stable instrument T-test for equal sample sizes and equal variance. The
electronics . However, the major changes in the
6
level of significance for these statistical tests was 0.05.
shrinkage-stress rate occur in the first 5 min (300
seconds). In this way, the behavior of the function fc for Evaluation of cured resin quality
a conventional photoactivation method with constant Analyses to determine the conversion degree of
luminous irradiation (1000 mW/cm2 during 35 seconds) the monomers into polymers were applied to evaluate
was determined by monitoring the shrinkage stress the quality of the cured composites. A stainless-steel
during 300 seconds, of which only the initial 35 seconds matrix with a resin insertion cavity was used to perform
(corresponding to the photoactivation interval) were this experiment. The composite resins were packed
considered for the determination of the minimization on the cavity in a single increment. They were then
function. photoactivated using the conventional and exponential
The monitoring was performed with a universal

J Appl Oral Sci. 3/9 2018;26:e20170528

 Minimization of polymerization shrinkage effects on composite resins by the control of irradiance during the photoactivation process

methods. Five specimens were made for each orthodontics indication) were used to evaluate the
investigated group. The produced samples dimensions adhesion interface between tooth and polymerized
were the same as in the shrinkage stress tests (6 composites. All patients who provided teeth for the
mm × 2 mm × 1 mm). After the photoactivation, the present study completed a written consent form.
specimens were removed from the mold and stored Two teeth were used for each composite brand/
in a dry mean, in dark containers, at 37°C (±1°C) model and photoactivation method, resulting in 20
for 24 h. The specimens were then pulverized into samples for this analysis. Cavities with dimensions
a fine powder. The pulverized composite resins were similar to the specimens in the previous experiments
maintained in a dark box until the Fourier-transform (6 mm × 2 mm × 1 mm) were made in each tooth.
infrared spectroscopy (FT-IR) analysis. Five milligrams The cavities preparation was performed using water-
of the ground powder was thoroughly mixed with cooled diamond burs (4138, KG Sorensen; Barueri,
100 mg of the KBr powder salt 1,8,14
. The degree of São Paulo, Brazil), as it is conventionally performed in
conversion (DC) measurements were performed with dental restorations. A treatment with phosphoric acid
a spectrophotometer (Nicolet Nexus 470, Thermo was performed under each cavity and the remaining
Fisher Scientific; Vernon Hills, Illinois, USA) and were structure was conditioned by a primer adhesive solution
recorded in the absorbance, operating under the (Adapter Single Bond 2, 3M ESPE; Sumaré, São Paulo,
following conditions: 50 scans, a 4 cm –1
resolution Brazil). The resins were packed in the teeth cavity in
and a 300 to 4000 cm–1 wavelength. The DC was a single increment and then photoactivated for 35 s
determined according to equation: using the conventional or the exponential method. The
samples were later stored in 2% chlorhexidine solution
(1) for 1 week. Glutaraldehyde and sodium hypochlorite
were used as disinfectants after tooth extraction.
where the percentage of unreacted carbon-carbon For the SEM analyses, a longitudinal cut was made
double bonds (%C=C) was determined from the ratio in each restored tooth using a diamond cutting disc
of the absorbance intensities of aliphatic C=C (I1638cm-1) (Arotec; Cotia, São Paulo, Brazil) at 100 rpm. Note
and aromatic C–C (I1608cm-1), before and after curing that, after the cutting, the specimens did not have
of the specimen . The obtained DC results for each
13
their surfaces polished because the material removed
photoactivation technique were compared by applying from the teeth in this process could cover the possible
the T-test for equal sample sizes and equal variance. cracks in the interface of restoration.
The level of significance for these statistical tests was Afterwards, sputter coating for SEM was performed
0.05. by applying an ultra-thin coating of electrically-
conducting metal (gold, in this case) under each
Evaluation of adhesion interface between tooth specimen. This process was performed to make it
and resin susceptible to the emission of secondary electrons
Healthy molar human teeth (extracted by to obtain images by SEM (LS-15 EVO, Zeiss; Jena,

Figure 1- Illustration of: (a) shrinkage stress at the time domain for the conventional photoactivation method; (b) the conventional method
of photoactivation and theoretical optimized curve to minimize the effects of the polymerization shrinkage

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 GUIMARÃES GF, MARCELINO E, CESARINO I, VICENTE FB, GRANDINI CR, SIMÕES RP

Thuringia, Germany). at the beginning of the polymerization process.

The experimental data from the shrinkage stress

Results can be fitted by a first order exponential decay function:

The monitoring of shrinkage stress showed the (2)

function of the conventional polymerization

process (i.e., photoactivation with a constant luminous in which the determination coefficient is R2=0,99.

intensity of 1000 mW/cm2 for 35 s of irradiation) The mathematical optimization resulted in a

presented a logarithmic behavior, as illustrated in minimization function with exponential behavior:

Figure 1(a). The graph showed that the resins were

under an intensive stress in the initial seconds of the (3)

polymerization process, followed by stabilization,

where the stress tends to become constant. This where the parameters a, b and i0 can be adjusted to

behavior shows that the composite contraction occurs attempt the manufacturers’ recommendations for the

Figure 2- Comparison of the shrinkage stress between the conventional and exponential methods for composite resins: (a) Z-250; (b)
Z-350; (c) Charisma; (d) NT Premium and (e) Ultrafill

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 Minimization of polymerization shrinkage effects on composite resins by the control of irradiance during the photoactivation process

Table 1- Comparison of the shrinkage stress and degree of conversion for the conventional and exponential photoactivation methods

Composite Maximum Shrinkage Stress (MPa) Degree of Conversion (%)

Conventional Exponential Conventional Exponential
Z-250 2.46±0.06 1.48±0.23 59.72±4.97 64.46±7.01
Z-350 2.08±0.03 1.50±0.12 62.03±3.23 58.87±4.45
Charisma 1.39±0.18 0.78±0.15 63.86±2.99 64.64±2.65
NT Premium 1.36±0.15 0.96±0.07 79.22±5.02 66.39±6.92
Ultrafill 1.81±0.09 1.02±0.03 67.58±5.44 65.54±3.37
T-test True difference in mean is not equal to 0 No significant differences
(t=6.87, p-value=0.0023) (t=0.86, p-value=0.44)

photoactivation process. In this work, these parameters Discussion

were adjusted as follows: a=0.58309, b=4.928 and
i0=300. This function represents an exponential growth The results from the monitoring shrinkage stress
of the luminous intensity in the photoactivation time showed that the exponential method significantly
domain. Figure 1(b) shows this exponential curve, reduces the stress for all resin models tested in this
which represents the theoretical optimal curve to work. This result can be interpreted because of the
minimize the effects of polymerization shrinkage. In control of luminous intensity during the photoactivation
this figure, the curve for the conventional method of that can change the polymerization reaction kinetics.
photoactivation was inserted for comparison purposes. The reduced irradiance at the beginning of the
By applying the exponential photoactivation method, photoactivation process can extend the pre-gel phase,
new contraction stress patterns for the resins were where the material may flow and undergo molecular
obtained. Figure 2 shows comparative graphs of the rearrangement, compensating shrinkages forces19.
shrinkage stress for the conventional and exponential Similar results were obtained from the soft-start
photoactivation methods. By analyzing the standard photoactivation protocol, which consists of an initial
deviation of the shrinkage stress quantification for the light exposure with reduced irradiance for a certain
conventional and exponential photoactivation methods time period, followed by full irradiance. However, the
at the end of the monitoring experiment (300 s) and soft-start technique does not have a rigid mathematical
the T-test result for these values (Table 1), it can be standardization for the contraction stress function
concluded that the exponential method promoted a optimization and, because of this, the results obtained
significant reduction of the shrinkage stress (~36.88% from this technique are not as significant as those
±6.56) for all analyzed composites brand/models. presented in this study. On this basis, the exponential
The result from T-test applied on DC values showed photoactivation method can improve the marginal
there are no significant differences comparing the adaptation of composite restorations16.
conventional and exponential photoactivation methods. The reduction of the contraction stress by itself
These results are also synthesized in Table 1. does not characterize an improvement in the
Figure 3 shows the SEM analyses for all resins in polymerization process of the composite resins. In
this study, comparing the two photoactivation methods. some situations, the low contraction stress may be
The SEM analyses showed that the reduction of the associated with partial polymerization of the composite.
shrinkage stress by the exponential method promoted In this context, the DC results showed there are no
the reduction of cracks at the resin/tooth interface for statistically significant differences for the ratio between
the Charisma and Ultrafill resins. In the other cases, residual monomers for conventional and exponential
i.e., for the Z250, Z350 and NT Premium composites, photoactivation techniques. Although this result is, by
the stress reduction was able to eliminate adhesion itself, very important, we should consider that the DC
failures. In the supplementary files, a SEM with lower might be associated with the hardness of the cured
magnification is shown, where it is observed that the resin composite, since there is a high correlation
elimination of cracks occurs throughout the extension between the two methods7,18. From this, it can be
of the adhesion interface between the tooth and the inferred that mechanical properties of the composite
resin. resins photoactivated by the proposed method are

J Appl Oral Sci. 6/9 2018;26:e20170528

 GUIMARÃES GF, MARCELINO E, CESARINO I, VICENTE FB, GRANDINI CR, SIMÕES RP

Figure 3- Scanning electron microscopy analyses of the conventional and exponential photoactivation methods for composite resins: (a)
Z-250; (b) Z-350; (c) Charisma; (d) NT Premium and (e) Ultrafill

J Appl Oral Sci. 7/9 2018;26:e20170528

 Minimization of polymerization shrinkage effects on composite resins by the control of irradiance during the photoactivation process

similar to those of the resins photoactivated by the Conclusions

conventional method. The DC results also show that
the irradiance used in the exponential light curing The results obtained in this study showed that
procedure provides sufficient energy for the adequate the control of irradiance during the photoactivation
resins polymerization. process by an optimized mathematical function is more
Finally, the SEM images show that exponential efficient than the conventional technique for reducing
photoactivation technique reduces or even eliminates the effects of polymerization shrinkage in composite
adhesion failures between the photopolymerized resins resins. According to the DC results, the proposed
and the teeth. We can note a significantly different photoactivation method does not cause damage to the
behavior of the composites photoactivated for the two cured resin, which is effective in converting monomers
presented methods and for all the composite resins in into polymers at the same level as for the conventional
this study. Considering the NT Premium and Ultrafill method. By the SEM analyses, we concluded that the
composites, the dimension of the gap at the resin/tooth exponential photoactivation method can reduce or
interfaces for the conventional photoactivation method eliminate the adhesion failure between the composite
was large enough (~10 µm) for microleakage and and the tooth.
even accumulation of bacteria, including Streptococcus
mutans. However, concerning the exponential method, Acknowledgements
only the Charisma and Ultrafill composites showed The authors would like to acknowledge the financial
adhesion failures. Meanwhile, the size of these gaps support of FAPESP (grant no. 2015/02136-2).
is lesser than that of the caries-causing bacteria. This
result has significant relevance and shows that the
technique is feasible for practical application.
In addition, note that we only have studied the
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