RESEARCH ARTICLE

Polymerization Mode of Self-Adhesive, Dual-Cured

Dental Resin Cements Light Cured ThroughVarious
Restorative Materials
JI SUK SHIM, DDS, MSD *, JEONG KYUNG KANG, DDS, MSD*,†, NAYANSI JHA, DDS‡, JAE JUN RYU, DDS, PHD‡

ABSTRACT
Objective: The aim ofthis study was to investigate the polymerization mode of self-adhesive, dual-cured resin cements
light-cured through overlying materials with differentdegree oftranslucency by measuring the degree of conversion (DC).
Materials and Methods: Three kinds of self-adhesive, dual-cured resin cements (G-CEM LinkAceTM,Maxcem EliteTM,
R
and BisCemV) were light-cured through three different restorative materials that included porcelain-fused metal
(PFM), zirconia, and lithium disilicate.Polymerization kinetics were continuously evaluated using infrared spectroscopy
after 0, 5,10, and 30 min and 2 weeks of mixing.Data were statistically analyzed using two-way analysis of variance
(ANOVA), one-way ANOVA, and Tukey’s multiple-comparison test (a 5 0.05).
Results: Regardless of the kind of resin cement, the light-cured groups showed higher DCthan did the
autopolymerization group under PFM at any point of time (p < 0.05).The time taken by the cements to achieve
statistically similar DC between the zirconia and lithium disilicate groups increased in the following order: G-CEM
LinkAceTM,BisCemV, and Maxcem EliteTM (p < 0.05).
R

Conclusions: The degree of translucency of the restorative material can be a signif|cant variable determining the
polymerization aspects of self-adhesive, dual-cured resin cements.The resin cements light-cured through lithium
disilicate and zirconia showed higher DCthan that shown by cements cured under PFM at any measurementtime.
The lithium disilicate and zirconia groups showed differences in the early stage of polymerization for G-CEM
LinkAceTM and BisCemV; however, the differences diminished at 2 weeks.
R

CLINICAL SIGNIFICANCE
Chemical polymerization is not suff|cientto cause the resin cementto achieve the highest polymerization not only in
early stage, but also in late stage of polymerization.The sensitivity to the intensity of the light was different for each
resin cement. Special clinical steps to compensate for the attenuated light intensity seem to be necessary for the resin
cements which are susceptible to light intensity.
(J Esthet Restor Dent 00:00^00, 2017)

INTRODUCTION aspects of dual-cured resin composites have been shown

to be dependent on the amount of light exposure.4
Adequate polymerization is a prerequisite for not only Therefore, the translucency of restorative materials can
the mechanical properties but also the biocompatibility affect the amount of light transmission and the
of resin-based composites.1–3 The polymerization polymerization efficiency of dual-cured resin cements.

*Professor, Department of Dentistry, Korea University Ansan Hospital, Gyeonggi-do, Republic of Korea

Doctor, Department of Dentistry,VHS Medical Center, Seoul, Republic of Korea
`
Professor, Department of Dentistry, Korea University Anam Hospital, Seoul, Republic of Korea

C 2017 Wiley Periodicals, Inc.

V DOI 10.1111/jerd.12285 Journal of Esthetic and Restorative Dentistry Vol 00  No 00  00^00  2017 1
 POLYMERIZATION ASPECTS OF RESIN CEMENTS Shim et al

Self-adhesive resin cements, which can be polymerized DC of self-adhesive resin cements at every
in a dual-curing system, were developed to overcome measurement time.
the disadvantages of conventional resin cements whose
application was time-consuming, technical skill-
dependent, and complex.5–7 Most manufacturers of MATERIALS AND METHODS
these resin cements recommended using the products
with many different kinds of restorative materials,
Specimen Preparation
including porcelain-fused metal (PFM), lithium
disilicate, and zirconia. The chemical composition of
Figure 1 shows the method to prepare specimens.
self-adhesive resin cements is different from those of
Three kinds of self-adhesive, dual-cured resin cements
conventional resin cements, and previous studies have
were used: G-CEM LinkAceTM (GC America Inc,
shown the possibility of differences arising in the
Alsip), Maxcem EliteTM (Kerr Corporation, Orange,
polymerization characteristics of two types of resin R
CA), and BisCemV (Bisco, Inc. Schaumburg, IL)
cements.1
(Table 1). All resin cements were properly stored
according to the manufacturer’s instructions and
The observation period is an important factor for
mixed using automix mixing tips. Teflon molds with
evaluating the degree of conversion (DC) of dual-cured
2-mm thickness, a central opening of 10-mm diameter,
resin composites. This is because autopolymerization
and a channel of 4-mm width connected to the
continues until 2 weeks, even after light polymerization
opening were prepared. A slide glass was positioned
has been completed,8 and the rate of dual
under the mold, and mixed resin cements were slightly
polymerization differs according to the time after
overfilled in the opening. After injecting the cements
mixing. Therefore, multiple measurements have to be
obtained at various times for evaluating the DC of into the mold, a second slide glass was used to cover
dual-cured resin cements. However, most previous the top of the mold, taking care to avoid the
studies have measured the DC only once according to entrapment of air bubbles. Excess resin cement flowed
their study design. out to the connected channel without affecting the
thickness of the specimens, thereby ensuring a uniform
The purpose of this study was to evaluate the thickness for all specimens. The channel maintained a
polymerization mode of self-adhesive, dual-cured resin constant thickness of the resin cement specimens not
cements light-cured through overlying materials with only during their application but also during
different degree of translucency by measuring the DC polymerization, thereby minimizing the volume
at 0, 5, 10, and 30 min and 2 weeks after mixing. The changes in resin cement due to shrinkage.
null hypothesis was that the degree of translucency of
materials overlying resin cements would not affect the
Light Curing Through Various Materials

The output intensity of light curing unit (Dr’s Light;

Good Doctors Co., Incheon, Korea) was measured
with a radiometer (LED radiometer; ThreeH,
Zhengzhou, China), and the average of 10 measuring
was 714.8 mW/cm2 with 4.4 standard deviation.
Eighteen specimens were prepared for each kind of
resin cement and divided into three groups (n 5 6)
depending on the materials overlying the specimens
FIGURE 1. The illustration of methods to prepare the during light exposure: PFM, zirconia, and lithium
specimens; frontal and sagittal view. disilicate. The PFM group specimens were polymerized

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 POLYMERIZATION ASPECTS OF RESIN CEMENTS Shim et al

TABLE 1. Self-adhesive, dual-cured resin cements used in the experiment

Product Resin category Manufacturer Shade Lot
R
BisCemV Bis-GMA BISCO, Schaumburg, IL,USA A2 39213

G-CEM LinkAceTM UDMA GC Corporation, America Inc, Alsip,USA A2 1402251

Maxcem EliteTM Bis-GMA Kerr Corporation,Orange,CA,USA A2 557025

only by chemical curing because the curing light is (a 5 0.05). The influence of independent variables,
unable to penetrate through the metal disc in the including overlying materials and measurement times,
PFM. For the zirconia and lithium disilicate groups, was analyzed using a two-way analysis of variance
light curing was applied for 40 s through the blocks (ANOVA) (a 5 0.001). Comparison of the DC between
with 1-mm thickness and A2 shade was formed using groups was conducted using one-way ANOVA and
zirconia (LAVATM Plus; 3M Deutschland GmbH, Tukey’s multiple-comparison test (a 5 0.05). All
Neuss, Germany) or lithium disilicate (IPS e.max Press statistical analyses were conducted using SPSS for
HT ingots; Ivoclar-Vivadent AG, Schaan, Windows (release 12.01; SPSS Inc., Chicago, IL).
Liechtenstein) immediately after resin cement mixing.

RESULTS
Infrared Spectroscopy Measurements
The statistical analysis of the DC of each resin cement
The DC of the resin cements was examined using
measured at each time is summarized in Table 2. Two-
infrared spectroscopy (NIRSolutionsTM; BUCHI, Flawil,
way ANOVA revealed significant differences in the DC
Switzerland). Continuous evaluation was conducted
because of the overlying materials and the
according to the following timetable: 0 min (right after
measurement times (p < 0.001). In all resin cements,
exposure to curing light); 5, 10, and 30 min; and 2
autopolymerization continued until 2 weeks after light
weeks. The specimens were stored in a dark box at
curing at 0 min, and the DC of each resin cement
room temperature during the waiting period.
showed differences with increasing time. Regardless of
The absorbance spectrum was acquired by scanning the kind of resin cement used, the groups light cured
the specimens 10 times over a 10,000–4,000 cm21 through zirconia and lithium disilicate showed higher
range with a resolution of 4 cm21. To determine the DC than did the groups cured only with
DC, the area of the peak corresponding to vinyl autopolymerization under PFM at any measurement
stretching at 6,165 cm21 was used.9 The acquired peak time (p < 0.05). No statistical differences were observed
area in the 0-min spectrum was used as the area of between the zirconia and lithium disilicate groups at 2
resin in its monomeric state; the DC was calculated weeks after mixing; however, the lithium disilicate
from the ratio of the peak area in the monomeric to groups showed statistically higher DC than did the
polymeric states, according to the following formula: zirconia groups until 10 min after mixing with
R
BisCemV and until 30 min after mixing with G-CEM


DC 5 1 – areapolymer =areamonomer 3 100%:9 LinkAceTM (p < 0.05). No significant differences were
observed between the lithium disilicate and zirconia
Statistical Analysis groups used with Maxcem EliteTM at any
measurement time (p > 0.05). The differences between
The mean and standard deviation of the DC were the zirconia and lithium disilicate groups at each
calculated for each group. Data were evaluated for measurement time increased in the following order:
G-CEM LinkAceTM, BisCemV, and Maxcem EliteTM.
R
homogeneity of variance based on Levene’s test

C 2017 Wiley Periodicals, Inc.

V DOI 10.1111/jerd.12285 Journal of Esthetic and Restorative Dentistry Vol 00  No 00  00^00  2017 3
 POLYMERIZATION ASPECTS OF RESIN CEMENTS Shim et al

TABLE 2. The degree of conversion of resin cements with three different light-curing methods
0 min 5 min 10 min 30 min 2 weeks
R
BisCemV

PFM 0 (0)a 3.5 (0.7)a 9.8 (2.8)a 40.2 (3.8)a 75.5 (2.7)a

Zirconia 60.2 (1.6)b 63.7 (0.6)b 65.5 (0.5)b 68.5 (0.3)b 82.9 (0.6)b

Lithium 61.5 (1.1)c 65.1 (1.1)c 68 (0.5)c 71.1 (0.3)b 83.9 (0.7)b
disilicate

G-CEM LinkAceTM

PFM 0 (0)a 31.6 (1.9)a 40.1 (4.7)a 52 (1.6)a 69.2 (1.3)a

Zirconia 31.8 (1.2)b 41.1 (1.2)b 47.8 (1.6)b 51.4 (0.6)b 70.5 (2.3)b

Lithium 46.2 (1)c 51.8 (0.6)c 55.1 (1.8)c 60.9 (0.6)c 71.6 (0.9)b
disilicate

Maxcem EliteTM

PFM 0 (0)a 28.3 (1.3)a 39.9 (1.8)a 49.6 (0.3)a 76.9 (0.4)a

Zirconia 29.1 (1.5)b 52.6 (0.3)b 56.9 (1.6)b 67.2 (2.2)b 78.8 (0.7)b

Lithium 29.5 (3.2)b 54.6 (2.7)b 58.3 (1)b 69 (0.7)b 80.1 (0.8)b
disilicate

*Within each of the measurement times of each resin cements, similar superscript letters indicate homogenous subsets among the experimental
groups (p > 0.05).

The groups polymerized under PFM represented the lithium disilicate and zirconia groups also showed
autopolymerization aspects of each resin cement differences in the early stage of polymerization, which
R
without light curing. BisCemV showed the highest diminished at 2 weeks. Thus, the null hypothesis that
changes in the DC by autopolymerization between 10 the overlying materials on resin cements would not
and 30 min, whereas G-CEM LinkAceTM and Maxcem affect the DC of self-adhesive resin cements was
EliteTM showed the highest changes between 0 and 5 rejected.
min.
The results of this study showed that
autopolymerization without light curing did not induce
DISCUSSION the highest DC compared with dual-polymerization,
irrespective of the materials and measurement times.
The purpose of this study was to determine whether Similar results have been reported by previous studies
the differences in overlying materials can affect the DC that performed evaluations using mechanical properties
of self-adhesive, dual-cured resin cements on the basis and infrared spectroscopy.1,10,11 However, most
of the infrared spectroscopy (IR) results obtained at previous studies observed the polymerization aspects
multiple measurement times (0, 5, 10, and 30 min and for durations below 1 h, which is a relatively short
2 weeks after mixing). The specimens light cured time because autopolymerization is known to last 2
through translucent (lithium disilicate) and semi- weeks. In this study, the DC between the groups with
translucent (zirconia) overlying materials showed autopolymerization and dual-polymerization was
higher DC than did the groups with opaque overlying compared until 2 weeks, that is, the final DC of the
material (PFM) at all of the measurement times. The resin composite, and the findings confirmed the fact

4 Vol 00  No 00  00^00  2017 Journal of Esthetic and Restorative Dentistry DOI 10.1111/jerd.12285 V
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 POLYMERIZATION ASPECTS OF RESIN CEMENTS Shim et al

that the loss of light curing affects not only the early the remaining methacrylate groups include not only
stage of polymerization but also the final unreacted residual monomers, but also monomers that
polymerization of the resin cements. Although a have a single carbon bond at the end of polymer
clinically acceptable minimum DC has not yet been structures. Each resin cement has its own polymer
established, commercial resin composites show 50%– structure, and the specific bulk of the polymer strand
75% DC after polymerization.12,13 Therefore, all groups may affect the number of covalently bonded single
in the current study achieved relatively high DC at 2 carbon bond.
weeks, and the differences in the DC caused by the
loss of light curing may not be critical to the The groups polymerized under PFM show the
mechanical properties of resin cements. However, autopolymerization aspects of each resin cement
unreacted residual monomer can be an issue because it without light-curing. Therefore, the results show that
can cause poor biocompatibility.14,15 the time at which each resin cement is most
chemically active for polymerization is different.
With the same thickness and shade, zirconia attenuates Autopolymerization between 0 and 5 min after mixing
more light reaching the resin composite than does with G-CEM LinkAceTM and Maxcem EliteTM and
lithium disilicate because zirconia is more opaque than between 10 and 30 min after mixing with BisCemV
R

lithium disilicate.16 Therefore, the groups covered with seems critical for adequate DC when they are used in
lithium disilicate showed higher overall DC than did PFM restorations. In conclusion, clinical procedures
the groups covered with zirconia. However, the such as cementation removal and finishing in PFM
sensitivity to the amount of light exposure was
restorations should be delayed by at least 5 min for
different between the resin cements, and larger
G-CEM LinkAceTM and Maxcem EliteTM and 30 min
differences of DC in the early stage between lithium R
for BisCemV.
disilicate and zirconia groups were shown in the
following order: G-CEM LinkAceTM, BisCemV, and
R

A limitation of this study was that the experimental

Maxcem EliteTM. This result may be attributed to the
conditions were different from the intraoral conditions.
differences of required minimal irradiant energy
The storage temperature of the NIR machine should
between the resin cements because light intensity can
be lower (238C) than the temperature of the oral
be affected by the differences in the overlying
cavity; the differences in temperature can affect resin
restorative materials.17,18 Clinical attention, for
polymerization, which, in turn, affects the DC. The
example, providing higher intensity or longer duration
differences in the shape of the restorative materials
of irradiation, is necessary to compensate for the
could also have affected our findings. Additional
attenuated light intensity, and further study with
clinical research focusing on intraoral conditions may
variables of irradiation methods may be beneficial to
be necessary for verifying these results.
determine the appropriate irradiation method on
zirconia.

The final DC of each resin cement was shown to be CONCLUSION

different. Previous studies have also shown that the
polymerization potential can vary greatly according to The degree of translucency of the restorative material
the brand of cement used.19,20 The DC calculated can be a significant variable determining the
using IR data is a measurement of the amount of polymerization aspects of self-adhesive, dual-cured
reacted methacrylate groups, and it helps indirectly resin cements. The resin cements light-cured through
calculate the amount of remaining unreacted lithium disilicate and zirconia showed higher DC than
methacrylate groups. However, the differences in the that shown by cements cured under PFM at any
final DC between different brand resins may not measurement time. The lithium disilicate and zirconia
represent the amount of cytotoxicity. This is because groups showed differences in the early stage of

C 2017 Wiley Periodicals, Inc.

V DOI 10.1111/jerd.12285 Journal of Esthetic and Restorative Dentistry Vol 00  No 00  00^00  2017 5
 POLYMERIZATION ASPECTS OF RESIN CEMENTS Shim et al

polymerization for G-CEM LinkAceTM and BisCemV;

R
9. Stansbury JW, Dickens SH. Determination of double bond
however, the differences diminished at 2 weeks. conversion in dental resins by near infrared spectroscopy.
Dent Mater 2001;17:71–9.
10. Aguiar TR, Di Francescantonio M, Arrais CA, et al.
Influence of curing mode and time on degree of conversion
DISCLOSURE AND ACKNOWLEDGEMENTS of one conventional and two self-adhesive resin cements.
Oper Dent 2010;35:295–9.
11. Di Francescantonio M, Aguiar TR, Arrais CA, et al.
The authors do not have any financial interest in the
Influence of viscosity and curing mode on degree of
companies whose materials are included in this article. conversion of dual-cured resin cements. Eur J Dent 2013;7:
This study had no sources of support in the form of 81–5.
grants, equipment, products, or drugs. There are no 12. Bayne SC. Dental biomaterials: where are we and where are
competing interests or funding to declare. All authors we going? J Dent Educ 2005;69:571–85.
have approved the submission of this manuscript and 13. Ferracane JL, Greener EH. The effect of resin formulation
on the degree of conversion and mechanical properties of
have given necessary attention to ensure the integrity
dental restorative resins. J Biomed Mater Res 1986;20:121–
of the work. 31.
14. Moin Jan C, Nomura Y, Urabe H, et al. The relationship
between leachability of polymerization initiator and degree
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