Brazilian Dental Journal (2015) 26(5): 484-489 ISSN 0103-6440

http://dx.doi.org/10.1590/0103-6440201300180

Degree of Conversion and Mechanical

1Department of Operative Dentistry
and Dental Materials, Dental School,
UFU - Universidade Federal de
Properties of Resin Cements Cured Uberlândia. Uberlândia, MG, Brazil
2Department of Fixed Prosthodontics

Through Different All-Ceramic Systems and Dental Materials, Dental School,

UFU - Universidade Federal de
Uberlândia. Uberlândia, MG, Brazil
3Department of Dentistry, Health

and Biological Sciences Center,

Camila de Carvalho Almança Lopes1, Renata Borges Rodrigues1, André Luis UFSE - Universidade Federal de
Faria e Silva3, Paulo Cézar Simamoto Júnior2, Carlos José Soares1, Veridiana Sergipe, Aracaju, SE, Brazil
Resende Novais1
Correspondence: Veridiana Resende
Novais, Avenida Pará, 1720, Bloco
4L, Anexo A, Campus Umuarama,
The aim of this study was to verify the degree of conversion (DC), Vickers microhardness 38400-902 Uberlândia, MG, Brasil.
(VH) and elastic modulus (E) of resin cements cured through different ceramic systems. Tel: +55-34-3218-2222. e-mail:
[email protected]
One 1.5-mm-thick disc of each ceramic system (feldspathic, lithium dissilicate and zircônia
veneered with feldspathic) was used. Three dual-cured (Allcem, Variolink II and RelyX U200)
and one chemically-cured (Multilink) resin cements were activated through ceramic discs.
For dual-cured resin cements was used a conventional halogen light-curing unit (Optilux
501 at 650 mW/cm2 for 120 s). Samples cured without the ceramic disc were used as
control. The samples were stored at 37 °C for 24 h. ATR/FTIR spectrometry was used to
evaluate the extent of polymerization in the samples (n=5). Micromechanical properties - VH
and E - of the resin cements (n=5) were measured with a dynamic indentation test. Data
were statistically analyzed with two-way ANOVA, Tukey’s test and Pearson’s correlation
(α=0.05). DC was affected only by the type of resin cement (p=0.001). For VH, significant
interaction was detected between resin cement and ceramic (p=0.045). The dual-cured
resin cements showed no significant differences in mean values for E and significantly
higher values than the chemically-cured resin cement. The degree of conversion and the
mechanical properties of the evaluated resin cements depend on their activation mode and Key Words: resin cements,
the type of ceramics used in 1.5 mm thickness. The dual-cured resin cements performed ceramics, polymerization,
better than the chemically-cured resin cement in all studied properties. hardness, elastic modulus.

Introduction Insufficient DC can negatively affect the mechanical

The interest in all-ceramic materials is on increase, since properties, alter dimensional stability, and decrease the
these materials have adequate physical and mechanical bonding of resin cements to tooth structures, impairing
properties, excellent esthetic and biocompatibility that the clinical longevity of restorations (1,7,8).
make them suitable for dental rehabilitation (1). However, The type of ceramics, their thickness, shade and
the success of all-ceramic restorations depends largely on translucency, the resin cement composition, mode of
the reliable bonding between ceramic and dental hard activation as well as the curing light output power,
tissues by luting materials. setting time and distance are factors that affect the
With the developments in adhesive dentistry, resin resin cement polymerization (1,5,9,10). The glass ceramic
cements became attractive because of their low solubility, systems, feldspathic, leucite and lithium disilicate systems
good esthetics, and proper bond strength to both tooth have pleasing aesthetics, are amenable to acid etching
substrate and restorative materials (2). These materials and present translucency that allows light transmission
can be classified according to their activation modes, through the restoration to underlying tooth structure.
since the activation can be chemical, physical (by light) However, higher strength ceramic systems, such as alumina
or combination of both (dual) (3). When the restoration or zirconia-based ceramics are required as substructure, as
thickness is above 1.5-2 mm or its opacity hinders these ceramics used as coping have high opacity and can
the light transmission, the use of dual- or chemically- hinder the light transmission (11).
cured resin cements has been advocated (4,5) to attain It is therefore important to assess the way in which
proper polymerization of resin cements. Inadequate the type of ceramic system may interfere in properties of
polymerization, characterized by low degree of conversion different resin cements, in order to better understand the
(DC), decreases the mechanical properties of cement and interaction between ceramic and luting material. Thus, the
increases water sorption and solubility. Furthermore, it aim of this study was to evaluate DC, Vickers microhardness
was shown that increased amount of residual monomers (VH) and elastic modulus (E) of resin cements cured under
may cause pulp irritation and irreversible pulpitis (6). different ceramic systems.
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The tested null hypothesis was that ceramic type and the Preparation of Resin Cement Samples through
type of resin cement would have no significant influence Ceramic Discs
on the mechanical properties of the resin cements. Three dual-cured (Allcem, Variolink II and RelyX U200)
and one chemically-cured (Multilink) resin cements were
Material and Methods selected for this study. All resin cements information is
Preparation of Ceramic Discs summarized in Table 1. The resin cements were manipulated
Three all-ceramic materials were selected for this study: as recommended by manufacturers and inserted into vinyl
feldspathic glass-ceramic (Noritake EX 3; Kuraray, Miyoshi, molds (1 mm thick x 2 mm inner diameter x 10 mm outer
Chugoku, Japan); low translucency lithium disilicate glass- diameter). Mylar strips (Quimidrol; Joinville, SC, Brazil) were
ceramic (IPS e-max Press LT; Ivoclar Vivadent, Schaan, used on the bottom and top surfaces of the sample to ensure
Liechtenstein) and polycrystalline zirconia ceramic (Lava smooth surfaces, allow the ceramic disc placement over the
All-Ceramic System; 3M ESPE, Seefeld, Bavaria, Germany). sample and avoid inhibition of polymerization by oxygen
For the last one, a feldspathic ceramic (Noritake EX 3) was (12). The cements were mixed in controlled temperature
applied over the core made from zirconia ceramic. For the 23(±1) °C and 40% relative humidity. The ceramic discs
feldspathic glass-ceramic, a machined metal pattern was were placed over the resin cement samples assisted with a
duplicated with silicon (Aerojet; São Paulo, SP, Brazil) and teflon positioning ring and waited five minutes for chemical
used to manufacture the feldspathic ceramic disc. The setting of the cements (13). The samples were shielded
feldspathic ceramic was sintered (Alumini Press II; EDG, from room light by positioning a dark compartment over
São Carlos, SP, Brazil) according to the manufacturer’s the samples, during the five minutes of chemical setting.
instructions. IPS e-max Press ceramic discs were prepared The light curing was performed for the dual-cured resin
by the heat-pressing technique in specific furnace (Ivoclar cements through the ceramic discs for 40 s on the top and

Resin cements cured through ceramics

Vivadent) following the manufacturer’s instructions. An on both sides of the samples to simulate light-activation
opaque zircon disc was milled in the Zirkonzahn CAD/ on the occlusal, lingual and buccal surfaces. Each sample
CAM (Zirkonzahn Worldwide, Gais, Italy) system using was submitted to light exposure for 120 s (12), using a
zircon blanks (0.3 mm thick) and a feldspathic ceramic halogen light-curing unit (Optilux 501; Kerr) at 650 mW/
was applied onto the fabricated 1.2-mm-thick zirconia cm2. Samples from each cement group cured without the
disc. Three ceramic discs were 1.5 mm thick, 10 mm in ceramic disc were used as control samples. All samples were
diameter and Vita shade A2 color. Next, the samples were stored under dry and dark conditions at 37 °C for 24 h.
stored at room temperature. The light transmission through
ceramics was measured with radiometer (Demetron; Kerr, Degree of Conversion
Orange, CA, USA). The DC of the samples (n=5) was determined using

Table 1. Resin cements assessed in this study

Classification/ Filler content

Material Manufacturer Composition*
activation mode (vol.%)

Bis-GMA, Bis-EMA, TEGDMA, co-initiators, initiators (camphorquinone

FGM, Joinvile, Regular/
Allcem and Dibenzoyl peroxide), inorganic fillers (Barium alumo- 66-67
SC, Brazil Dual-cured
silicate glass and silicon dioxide), pigments and stabilizers.

Base Paste - Methacrylate monomers containing phosphoric

3M ESPE, acid groups, methacrylate monomers, silanated fillers,
RelyX Self-adhesive/
Seefeld, initiator components, stabilizers, rheological additives; 72
U200 Dual-cured
Germany Catalyst Paste - Methacrylate monomers, alkaline (basic) fillers, silanated
fillers, initiator components, stabilizers, pigments, rheological additives.

Ivoclar Vivadent, Bis-GMA, TEGDMA, UDMA, inorganic fillers (barium glass,

Regular/ Base - 46.7
Variolink II Schaan, ytterbium trifluoride, Ba-Al-fluorosilicate glass, and spheroid
Dual-cured Catalyst - 43.6
Liechtenstein mixed oxide), initiators, stabilizers, pigments, benzoyl peroxide.

Ivoclar Vivadent, Regular/ Bis-EMA, UDMA, Bis-GMA, HEMA, inorganic fillers

Multilink Schaan, Chemically- (barium glass, ytterbium trifluoride, spheroid mixed 39.7
Liechtenstein cured oxid), initiators, stabilizers and pigments.

* According to manufacturers. Bis-GMA: 2,2-bis[p-(2’-hydroxy-3’methacryloxypropoxy)phenyl]propane; TEGDMA: triethylene glycol dimethacrylate;

Bis-EMA: ethoxylated bisphenol A dimethacrylate; UEDMA: 1,6-bis(methacryloxy-2-ethoxycarbonylamino)-2,4,4-trimethylhexane; HEMA:
hydroxyethylmethacrylate.
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attenuated total reflectance/Fourier transform infrared hardness units:

spectroscopy (ATR/ FTIR Vertex 70; Bruker, Ettlingen, VHN = P
Germany). Preliminary reading for a small amount of each A
uncured material was recorded in absorbance spectrum where: P is the maximum load; A is the depth-sensing
acquired by scanning the samples 32 times over a 4,000 instrument.
to 400 cm-1 range with a resolution of 4 cm-1. Additional The indentation modulus was calculated from the
spectrum was obtained from cured specimen after dry slope of the indentation tangent depth-curve at maximum
storage at 37 °C for 24 h and shielded from the room force and is comparable with the elasticity modulus of
light. Shielding was performed by keeping the material the material.
inside the closed sample compartment. The ratio between
aliphatic carbon-to-carbon double bond (at 1,637 cm−1) Statistical Analysis
and aromatic component group (at 1,608 cm−1) for uncured DC, VH and E data were individually analyzed using
and cured samples were used to calculate the DC according two-way ANOVA, with ceramics and resin cement as the
to the following equation: factors. All post hoc multiple comparisons were performed
using Tukey’s test. Pearson’s correlation coefficient test was
%DC=1−[abs(C=C aliphatic)/abs(C=C aromatic)]polymer/ used to analyze a possible correlation between the analyzed
[abs(C=Caliphatic)/abs(C=Caromatic)] monomer x 100 three mechanical properties. Statistical significance was
set at α=0.05.
where DC is the degree of conversion, Abs (C=Carom) is
the height of the benzene ring peak, and Abs (C=Caliph) is Results
the height of the aliphatic C=C bond peak, for both cured Light transmission values of the ceramic discs are
and uncured resin cements (14,15). shown in Table 2.

Vickers Microhardness and Elastic Modulus Degree of Conversion

C.C.A. Lopes et al.

The samples were embedded in polyester resin The mean DC values and standard deviations according
(Instrumental; São Paulo, SP, Brazil). Prior to testing, the to the ceramic type and resin cement type are shown in Table
surfaces were finished with 600, 800, 1200 and 2000- 3. The factor resin cement type (p=0.001) was significant
grit silicon-carbide papers sizes (Norton; Campinas, SP, for DC. The factors ceramic type (p=0.703) and interaction
Brazil) and polished with metallographic diamond pastes between the study (p=0.056) were not significant. Tukey
with 6-, 3-, 1-, and ¼ µm- sizes (Arotec; São Paulo, SP,
Brazil) (16). Cement samples were ultrasonically cleaned
(Cristofoli; Campo Mourão, PR, Brazil) for 10 min. VH Table 2. Energy density values (mW/cm2) measured through different
measurements were performed on the top surface of resin types of ceramic discs
cement using micro-hardness dynamic indenter (Micro % of delivered
Ceramic type Energy density
Indentation Tester; CSM, Peseux, Switzerland). The test energy
load was increased and decreased at a constant speed Feldspathic 142 21.8
between 0 and 500 mN. The force increased from 0 to Lithium disilicate 135 20.8
500 mN in 20 s intervals, applied constantly for 5 s. Then
Zirconia + feldspathic 75 11.5
the force was gradually removed from 500 mN to 0 mN
in 20 s intervals. The load and the penetration
depth of the indenter were continuously
Table 3. Mean values and standard deviations of DC (%) for the experimental groups
measured while loading-unloading the force.
Five measurements were performed for each Ceramic
Resin Pooled
resin cement sample and the mean value was cement Lithium Zirconia + Control Average
Feldspathic
established as the Vickers hardness number disilicate Feldspathic
(VHN) for statistical analysis (n=5). Allcem 87.7 (0.8) 87.9 (1.2) 87.5 (1.5) 85.7 (2.2) 87.2 (1.4) A
From a multiplicity of measurements
Variolink II 68.1 (1.8) 60.5 (7.5) 63.0 (5.9) 66.6 (4.7) 64.5 (4.9) C
stored in a database supplied by the
RelyX U200 70.3 (2.8) 70.8 (5.6) 70.6 (2.9) 66.3 (3.6) 69.5 (3.7) B
manufacturer, a conversion factor between
hardness and VHN was calculated and Multilink 57.8 (4.1) 60.9 (2.2) 56.7 (7.9) 61.3 (3.6) 59.1 (4.4) D
introduced into the software, so that the * For pooled average, different letters represent statistically significant differences
measurements were expressed in Vickers (2-way ANOVA/Tukey, p<0.05).
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HDS showed differences among resin cements; chemically- similar values for E and significantly higher values than
cured resin cement exhibited the lowest values for DC. the chemically-cured resin cement.

Vickers Microhardness Pearson’s Correlation

There was statistical significance for resin cement The Pearson’s correlation test revealed a moderate
(p<0.001), ceramic (p<0.001) and interaction between these correlation between DC and VH (r2=0.594) and between
factors (p=0.045). The means and standard deviations for the DC and E (r2=0.389) and a strong correlation between
VH are in Table 4. The chemically-cured cement showed VH and E (r2=0.804).
lower VH values than the dual-cured cements. When cured
without the interposition of a ceramic disc or through Discussion
feldspathic ceramic, Allcem and RelyXU200 presented the Traditionally, DC is used to investigate factors
highest VH values Nevertheless, when cured through lithium affecting the polymerization reaction; whereas the final
disilicate and zirconia + feldspathic ceramic, RelyXU200 DC of a polymer has important effect on the mechanical
showed the highest values and Allcem resembled the other properties (17). It is important to emphasize that beyond
two dual-cured resin cements. The control group had the polymerization efficiency measured by DC, other factors
highest VH values for all studied cements or resembled affect the mechanical properties of resin cements and,
the ceramics. consequently, the clinical performance of adhesively
luted restorations (18). In the current study, mechanical
Elastic Modulus properties were assessed using a dynamic indentation test
The means and standard deviations for E are in Table that provides both hardness and modulus of elasticity of the
5. The factor resin cement was significant (p<0.001); no material directly from indentation load and displacement

Resin cements cured through ceramics

significant difference was found for the factor ceramic measurements (19). A strong correlation between these
type (p=0.287) and interaction between the ceramic and mechanical properties was shown, but weaker correlations
resin cement (p=0.259). Dual-cured resin cements showed were found between both mechanical properties and DC.
The polymerization depends on several
factors, including resin cement composition
and activation mode. Regarding activation-
Table 4. Mean values and standard deviations of VH (N/mm2)
mode, the lowest values of DC, VH and E
Ceramic were observed for the chemically-activated
Resin
Cement Lithium Zirconia + cement. The amount of initiators (usually
Feldspathic Control
disilicate Feldspathic benzoyl peroxide and an amine) added to
Allcem 70.6 (8.2) Aab 67.4 (13.6) ABb 71.1 (4.2) ABab 74.4 (4.7) Aa resin cements to produce chemical activation
Variolink II 59.0 (5.4) Bb 55.9 (4.4) Bb 67.9 (4.0) Ba 60.7 (7.6) Bab of the polymerization reaction is limited to
allow longer working time. Considering that
RelyX U200 67.6 (8.1) Ab 70.7 (8.0) Aab 76.2 (10.5) Aa 70.0 (10.4) Aab
the final DC of the chemically-activated
Multilink 44.4 (5.0) Ca 42.6 (3.2) Ca 43.7 (4.8) Ca 44.0 (6.3) Ca cement is proportional to the amount of
The means followed by different letters (upper case letters within the columns and lower chemical initiators, were expected reduced
case letters within the rows) are significantly different (statistical categories defined by values of DC (20). Chemical-activation
Tukey test; p<0.05).
also is present in dual cured cement, but
the light activation increases the amount
Table 5. Means and standard deviations of E (GPa) obtained according to the experimental
of free radicals available to initiate the
groups polymerization. Thus, the energy density
provided by light-curing unit may have
Ceramic
Resin Pooled significant effect on polymerization
Cement Lithium Zirconia + average
Feldspathic Control kinetics and final DC (21). To simulate a
disilicate Feldspathic
Allcem 10.3 (0.6) 8.9 (2.1) 10.0 (0.6) 10.5 (0.5) 9.9 (0.9) A
clinical condition of ceramic cementation,
light activation was performed through a
Variolink II 9.6 (1.1) 9.9 (0.7) 9.8 (0.6) 9.5 (0.5) 9.7 (0.7) A
1.5-mm-thick ceramic disc. The interposition
RelyX U200 10.3 (0.7) 10.0 (0.9) 10.0 (0.6) 10.1 (1.0) 10.1 (0.8) A of a ceramic can lead to some attenuation
Multilink 8.5 (0.6) 7.9 (0.6) 8.2 (0.6) 8.0 (1.1) 8.2 (0.7) B of light depending on ceramic crystalline
For pooled average, different letters represent statistically significant differences (2-way structure, light refractive index, shade and
ANOVA/Tukey, p<0.05). thickness (5,9). The ceramics used during
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the light activation of cements resulted in an energy loss resistance, and color stability should be taken into account
from light-curing unit varying from 11 to 22%. However, because they will also determine the clinical performance
this loss of energy did not result in reduction of DC of the material (25). Future research should consider the
irrespective the evaluated dual-cured cement (Table 2). polymerization of resin cements as function of time and
The increased time of light-curing (120 s) may help to ceramic thickness.
compensate the reduction of energy density, explaining
the outcomes. Therefore, when dual-cured cement is light- Resumo
cured through a ceramic system, extending light-curing O objetivo deste estudo foi mensurar grau de conversão (GC), microdureza
time accordingly may still be necessary to achieve optimal Vickers (VH) e módulo de elasticidade (E) de cimentos resinosos
polimerizados através de diferentes sistemas cerâmicos. Um disco de
polymerization (22). Furthermore, the 5 min of delay before 1,5 mm de espessura de cada sistema cerâmico (cerâmica feldspática,
the light-activation allows effective chemically activated dissilicato de lítio e zircônia coberto por cerâmica feldspática) foi utilizado.
polymerization (13). Três cimentos resinosos duais (Allcem, Variolink II e RelyX U200) e um
cimento resinoso quimicamente ativado (Multilink) foram ativados através
Among the dual-cured cements, Allcem showed the dos discos de cerâmica. Para os cimentos resinosos duais foi utilizado um
highest values and Variolink II the lowest one, irrespective the aparelho de lâmpada halógena (Optilux 501 a 650 mW/cm2 por 120 s).
conditions of light activation. Differences in composition, Amostras polimerizadas sem a interposição do disco de cerâmica foram
utilizadas como controle. As amostras foram armazenadas a 37 °C durante
including amount of chemicals and photo-initiators, 24 h. ATR/FTIR foi utilizado para avaliar a extensão da polimerização nas
monomeric composition, ratio of diluent monomers and amostras (n=5). Propriedades micromecânicas - VH e E – dos cimentos
filler content can explain the results. However, considering resinosos (n=5) foram medidas com um teste dinâmico de indentação. Os
dados foram analisados através de análise de variância a dois fatores, teste
that the exact concentration of each cement component is de Tukey e correlação de Pearson (α=0,05). O GC foi afetado somente
not provided by manufacturer, explanations of DC results pelo tipo de cimento resinoso (p=0,001). Para VH, houve interação entre
based on composition are speculative. It is important to o tipo de cimento resinoso e o tipo de cerâmica (p=0,045). Os cimentos
resinosos duais não apresentaram diferenças significativas nos valores
emphasize that differences of DC between resin cements do médios de E e valores significativamente maiores que o cimento resinoso
not necessarily indicate similar behavior when mechanical quimicamente ativado. O grau de conversão e as propriedades mecânicas
dos cimentos resinosos avaliados dependem do seu modo de ativação e
C.C.A. Lopes et al.

properties are evaluated (23). Interestingly, the behavior

do tipo de cerâmica usada na espessura de 1,5 mm. Os cimentos resinosos
of hardness between the cements was similar to those duais desempenharam melhor que o cimento resinoso quimicamente
observed for DC. In fact, beyond the compositional factors ativado em todas as propriedades estudadas.
and the developed polymer structure, DC has important
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J Appl Oral Sci 2003;11:162-167. Received April 1, 2015
19. Oliver WC, Pharr GM. Measurement of hardness and elastic modulus by Accepted July 7, 2015
instrumental indentation: Advances in understanding and refinements

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