Bond Strengths of Resin Cements to Ceramics
Bond Strengths of Resin Cements to Ceramics
Dental Materials
Abstract: This study evaluates the shear bond strength (SBS) of various
resin cements to different ceramics. Composite resin cylinders of Z100
David Cardoso Sandes FARIAS(a)
were fabricated and cemented to disks of feldspathic ceramic (Creation),
Letícia Machado GONÇALVES(b)
leucite-reinforced feldspathic ceramic (Empress I), and densely sintered
Ricardo WALTER(c)
aluminum oxide ceramic (Procera AllCeram) using five resin cements:
Yunro CHUNG(d) Panavia F (PAN), RelyX ARC (ARC), RelyX Unicem (RXU), RelyX Veneer,
Markus Bernhard BLATZ(e) and Variolink II. SBS was measured after three days of water storage
(baseline) and after artificial aging (180 days of water storage along with
(a)
Universidade CEUMA, Department of 12,000 thermal cycles). Failure mode of fractured specimens also was
Dentistry, São Luís, MA, Brazil.
evaluated. Data were analyzed with Kruskal-Wallis and Mann-Whitney
Universidade CEUMA, Postgraduate tests (α=0.05). RXU showed 1) the lowest baseline median SBS to
(b)
Declaration of Interests: The authors Keywords: Resin Cements; Ceramics; Aging; Aluminum Oxide; Shear
certify that they have no commercial or Strength.
associative interest that represents a conflict
of interest in connection with the manuscript.
Introduction
Corresponding Author:
David Cardoso Sandes Farias Recent progress in technology and research related to new dental
E-mail: davidcsfarias@[Link]
materials have resulted in an increasing number of all-ceramic materials
and systems commercially available for clinical use.1 In addition to
feldspathic porcelain, machinable glass ceramic, glass-infiltrated alumina
[Link]
ceramic, densely sintered high-purity alumina ceramic, and zirconia
ceramic are widely used in clinical practice. Clinical success of such
restorations relies on a strong and durable resin bond to the restorative
material and supporting tooth structures. A strong, durable resin bond
provides high retention,2 improves marginal adaptation and prevents
Submitted: April 21, 2019
microleakage,3 and increases fracture resistance of the restored tooth
Accepted for publication: September 1, 2019
Last revision: September 9, 2019 and the restoration.4
Bondi ng to cera m ics is faci l it ated by On the other hand, it is well accepted that
micromechanical interlocking and formation of airborne particle abrasion/silica coating followed
chemical bonds between resin cements and ceramic by silanization improves bonding of resin cements
substrates.5 To promote such interactions, surface to high-strength ceramics without any damage.20,21
modification by etching with hydrofluoric acid and The process of airborne particle abrasion with
subsequent silanization of the ceramic has been alumina particles coated with silica leaves the
advocated for use with silica-based ceramics.6,7 ceramic surface embedded with silica particles,
Selective use of hydrofluoric acid dissolves the which makes the chemically modified surface more
glassy matrix of silica-based ceramics producing reactive to bonding.14,22 Yet, bonding to airborne
a porous surface. That modified surface has particle abrasion/silica coated-treated oxide ceramics
increased surface area and may allow for better seems to suffer degradation over time.7,23 Likewise,
resin cement penetration.8,9 reduction in bond strengths over time may occur
Such procedure yields adequate micromechanical when the oxide surface is treated with a phosphate
bonding, whereas subsequent silanization of the monomer-containing primer (after airborne particle
etched ceramic facilitates chemical bonding between abrasion only).24
the resin cement and ceramic.10 After silanization, Used with any surface preparation protocol
the created bifunctional silane layer is capable of (airborne particle abrasion/silica coating followed by
chemically bonding to the hydrolyzed silicon dioxide silane agent or airborne particle abrasion followed
on the ceramic surface and copolymerizing with the by phosphate monomer-containing primer in
adhesive resin through its methacrylate-containing oxide ceramics, or hydrofluoric acid followed
group.10,11 Meanwhile, hydrofluoric acid etching by silane agent in silica-based ceramics), resin
and silanization of aluminum- or zirconium-oxide cements offer the advantage of sealing the created
ceramics are not reliable treatments. Such substrates internal surface roughness, which significantly
do not contain the silicon oxide phase, which makes st reng t hen s a nd i mproves t he longev it y of
the reaction between the hydrofluoric acid and glass restorations.25 In that regard, self-adhesive resin
in the ceramic possible,12 and may require alternative cements, which have been introduced to simplify
mechanical and chemical surface treatment techniques the application steps and minimize the time
to achieve reliable long-term resin-ceramic bonding.5,13 consumed during bonding procedures, can be
Various techniques have been investigated in utilized. According to the manufacturers, no
an attempt to roughen and activate the surface pretreatment is necessary, such as etching, priming,
of oxide ceramics in order to improve bonding. bonding or silanization, on the enamel, dentin, or
Studies have shown the positive effect of airborne ceramic substrate when using self-adhesive cements.
particle abrasion when used with silica coating and Some of those single-step resin cements contain
silanization,14 and when followed by a ceramic primer functionalized monomers of phosphate groups and
in bonding to oxide ceramics.15 Airborne particle multifunctional acid methacrylates that are claimed
abrasion of oxide ceramics can be accomplished to react simultaneously with the calcium ions of
with different Al 2O3 particle sizes and has been hydroxyapatite26 and the ceramic surface.27 In vitro
reported to increase the surface roughness, thereby bonding studies have shown positive results for
increasing mechanical retention.5,16,17 It is a practical self-adhesive resin cements when applied to high-
and cost effective method to clean and activate strength aluminum-oxide,28,29 leucite-reinforced,27
the surface of high-strength ceramics prior to and lithium disilicate ceramics.30
bonding, and can be easily performed chairside.5,14,18 Despite the available literature on the effects
Yet, the effects of airborne particle abrasion on of surface modification techniques and the use of
bonding to high-strength ceramics are discussed self-adhesive resin cements in ceramics, limited
controversially as crack development potentially information is available on bond strengths of self-
may occur, weakening the ceramic substrate.16,19 adhesive resin cements to different ceramics after
artificial aging. Therefore, the purpose of this study North Haven, USA), as used for porcelain veneers;
was to evaluate the shear bond strength (SBS) of RelyX 80 leucite-reinforced feldspathic ceramic (Empress
Unicem (RXU, 3M ESPE, St. Paul, USA) to various I, Ivoclar Vivadent, Schaan, Liechtenstein), as used
ceramics after thermocycling. Four commercially for all-ceramic restorations; and 60 densely sintered
available resin cements were used for comparison. aluminum-oxide ceramic (Procera AllCeram;
It was hypothesized that the SBS of RXU to various Nobel Biocare, Gothenburg, Sweden), as used
ceramics would not be statistically different from for high-strength all-ceramic restorations. Resin
that of the other resin cements and that it would cement systems used are listed in Table 1. The
not be affected by thermocycling. ceramic specimens were randomly assigned into
groups of 20 according to Table 2. Subgroups of
Methodology 10 specimens were either stored in distilled water
for 3 days or thermocycled.
Two hundred and twenty ceramic specimens Specimens with dimensions of 10-mm x 10-mm
were fabricated for the study. Those were 80 x 2-mm were prepared and polished with 1,000-grit
feldspathic ceramic (Creation, Jenson Industries, silicon carbide abrasive paper to obtain a standardized
Table 2. Early and late shear bond strength (SBS) values (MPa).
Early SBS P value early vs. late* Late SBS
Group
Medians 25 /75 percentiles
th th
Medians 25th/75th percentiles
Feldspathic ceramic
VAR 23.5a 22.2/30.4 p = 1.0000 23.9a 13.9/31.1
VEN 22.8a 19.6/25.3 p = 0.0029 12.9a 10.8/15.4
PAN 18.6 ab
16.3/20.0 p = 0.6022 14.2 a
11.0/16.1
RXU 16.7b 13.7/17.3 p = 1.0000 13.7a 10.8/15.2
Leucite-reinforced feldspathic ceramic
VAR 29.9a 26.5/31.0 p = 0.0029 12.0a 11.1/12.8
ARC 27.3 ab
23.3/31.3 p = 0.0070 11.2 a
9.9/13.9
PAN 20.4 b
18.7/21.9 p = 0.0161 13.2 a
12.8/14.4
RXU 10.5c 9.4/14.2 p = 0.3381 16.4a 11.0/21.6
Densely sintered aluminum-oxide ceramic
PAN 19.8a 17.0/25.0 p = 0.9358 16.2a 8.1/21.2
ARC 16.8 a
15.5/18.8 p = 0.0012 0.0b
0.0/6.4
RXU 12.0b 10.3/14.8 p = 0.0016 2.6ab 1.5/3.5
VAR: Variolink II, VEN: RelyX Veneer, ARC: RelyX ARC, PAN: Panavia F, RXU: RelyX Unicem. Early SBS: specimens aged in distilled water for 3
days prior SBS testing, Late SBS: Specimens subjected to 12,000 thermocycles prior SBS testing. Identical superscript letters indicate that the
values are not significantly different within groups, within columns (p > 0.05).
surface. Specimens then were treated according to (Table 1). Cementation procedures were performed
their respective group. The feldspathic ceramic and with the aid of an alignment apparatus consisting
leucite-reinforced feldspathic ceramic specimens were of parallel guides, a holder for the composite resin
etched with 4.8% hydrofluoric acid for 2 min. The cylinder, and an added weight of 1,000 g. The
densely sintered aluminum-oxide ceramic specimens setup ensured that the axis of the composite resin
were airborne particle abraded with 50 μm Al2O3 at specimen was perpendicular to the surface of the
a pressure of 2.5 bar and from a distance of 10-mm ceramic specimen and that a uniform layer of
for 12 s. Specimens then were cleaned ultrasonically resin cement was used. Specimens were placed in
in isopropyl alcohol for 3 min, rinsed, and stored in the alignment apparatus and a load of 1,000 g was
distilled water until use. applied for 10 min.6 Excess cement was removed
Composite resin cylinders (Z100, 3M ESPE) with the use of foam pellets (Disposable Mini-
serve as the substrate to be cemented to the ceramic Sponge Applicators, 3M ESPE) and microbrushes
specimens. They were made using an acrylic tube (Microbrush International, Grafton,
with an inner diameter of 2.9 mm and height of 3.0- USA). Materials were light-cured for 40 s from
mm, and light-cured for 40 s from the top and two three sides for a total of 120 s. In the Panavia F
sides for a total of 120 s. The Coltolux 4 (Coltène, (PAN) group, the oxygen-blocking gel Oxyguard II
Whaledent, Mahwah, (Kuraray Medical Inc., Tokyo, Japan) was applied at
USA) light-curing unit was used with its intensity the margins prior to light-curing procedures. After
being measured using the Coltolux 4 light meter to 10 min, specimens were removed from the alignment
ensure adequate output (above 450 mW/cm2). device and stored in distilled water. Half of the
Five minutes after light curing, the composite specimens (10/group) were tested in SBS after 3 days
resin cylinders were cemented to the treated ceramic (early SBS) while the other half was thermocycled.
specimens. The cements were used with their Thermocycling consisted of a total of 12,000 cycles
respective bonding/silane coupling agent and applied between 5 and 60ºC with a dwell time of 15 s. Two
according to the manufacturers’ recommendations thousand cycles were repeated every 30 days (total
of 180 days) as a method of stressing the bonding and for both pre- and post-thermocycling groups.
interface (late SBS). Mann-Whitney tests with Bonferroni correction
After aging, specimens were tested in shear with were then conducted to compare substrates and
the aid with a chisel-knife31 using an Instron 4441 cements pairwisely. The significance level was set
(Instron Corp., Norwood, at 0.05 and all analyses were performed using SAS
USA). Crosshead load speed was set at 1 mm/min. 9.3 (Cary, USA).
Results were expressed in MPa and calculated
by dividing the failure load (N) by the bonding Results
area (mm 2). To assess failure mode, all specimens
were examined with a light microscope at 25X Medians, 25th and 75th percentiles of SBS values
magnification. Failure mode was categorized as in MPa are listed in Table 2. Shear bond strength
cohesive in ceramic (CCe), cohesive in composite values are illustrated in Figures 1–3. Based on the
resin (CCo), and adhesive (Ad). Kruskal-Wallis tests, MPa values were significantly
A review of the literature on ceramic bonding different among substrates (p < 0.05); and among
revealed that a sample size of 6 to 10 specimens per resin cements within feldspathic ceramic (p < 0.05),
group is commonly used. The data of study similar leucite-reinforced feldspathic ceramic (p<0.05),
to the present study was used for power analysis, and densely sintered aluminum-oxide ceramic
which indicated that a sample size of 4 specimens (p < 0.05). The results of the Mann-Whitney tests
per group would be sufficient to achieve 90% power showed no differences between feldspathic ceramic
in detecting differences between group means at and leucite-reinforced feldspathic ceramic (p>0.05).
least as large as observed in that study.6 Therefore a There were differences between feldspathic ceramic
sample size of 10 specimens per group was adequate and densely sintered aluminum-oxide ceramic (p
to provide sufficient power (more than 99%). < 0.05); and between leucite-reinforced feldspathic
Statistical analysis compared the SBS among ceramic and densely sintered aluminum-oxide
substrates and among cements within each substrate. ceramic (p < 0.05).
Since a small number of 10 disks were assigned for The fracture analysis revealed different failure
each group and normal assumption was violated, patterns among groups. The percentage distribution
Kruskal-Wallis tests were used to test the SBS among of the predominant failure mode for each group is
substrates; among cements within each substrate; presented in Table 3.
Feldspathic ceramic
50
VAR
Shear Bond Strenght (MPa)
40 VEN
PAN
30 *
RXU
20 *
10
0
VAR VER PAN RXU VAR VEN PAN RXU
Early Late
Figure 1. Boxplots of early and late shear bond strength of resin cements to feldspathic ceramic.
50
VAR
*
10
0
VAR VER PAN RXU VAR VEN PAN RXU
Early Late
Figure 2. Boxplots of early and late shear bond strength of resin cements to leucite-reinforced feldspathic ceramic.
50
PAN
Shear Bond Strenght (MPa)
40 ARC
RXU
30
*
*
20
*
10 *
0
PAN ARC RXU PAN ARC RXU
Early Late
Figure 3. Boxplots of early and late shear bond strength of resin cements to densely sintered aluminum-oxide ceramic.
lowest. That was not statistically significantly different surface showed low late SBS of 2.6 MPa after early
from PAN in the feldspathic ceramic group. The worse SBS of 12.0. In contrast, PAN showed stable SBS after
overall (early) bonding performance of RXU might be thermocycling. The functional monomer 10-MDP
attributed to its high viscosity or weight percentage may have promoted stable micromechanical and
of fillers (wt%), which may affect its wetting and chemical bonds creating a long-term durable bond
infiltrating abilities.32 Despite the lower early SBS for for PAN.6,29,36 The results for the densely sintered
RXU, the results obtained for this resin cement may aluminum-oxide ceramic are in partial agreement
be considered acceptable as 10–13 MPa is considered with a study by Piwowarczyk and colleagues27 that
the minimum needed for clinical bonding.33 demonstrated better bonding of PAN than ARC to
Regarding the densely sintered aluminum-oxide Procera AllCeram. Differently from the present study,
ceramic group, the resin cement PAN demonstrated however, RXU showed an increase in SBS over time.
bond strength values greater than that of the other The much shorter aging process in that project may
resin cements (not statistically different from ARC). explain the difference in results.
The phosphate ester monomer 10-MDP may have In the feldspathic ceramic group, RelyX Veneer
helped creating better bonds to airborne particle (VEN) was the only resin cement to show decrease
abraded densely sintered aluminum-oxide ceramic34 in SBS after aging with 87% of the failures being
by chemical interaction with the oxide layer present adhesive. Water storage has shown detrimental effects
on the ceramic surface. 29 The phosphoric-acid (hydrolytic degradation) at the VEN/feldsphatic
methacrylates contained in RXU, which have been ceramic interface, despite the pretreatment with
shown to provide a “physical interaction” with the silane and hydrofluoric acid.38 The present study also
airborne-particle–abraded ceramic surface35,36 resulted showed decreased SBS for VAR, ARC, and PAN after
in SBS that were approximately 60% of that of PAN artificial aging in the leucite-reinforced feldspathic
(12.0 MPa vs. 19.8 MPa, respectively). ceramic group, while RXU showed a slight increase
To evaluate the influence of aging on bond in median SBS (not statistically significant). The
strength stability, a stress test comprising cyclic overall decrease in SBS in the leucite-reinforced
thermal fluctuations (thermocycling) is often carried feldspathic ceramic group may be due to weakening
out.6,27,29,37 Thermocycling utilizes differences in of the ceramic substrate.39
thermal coefficients of expansion of the ceramic and Another important indicator of the quality of
resin cements to stress the adhesive interface, which the adhesive interface is the analysis of fracture
has its resistance to hydrolytic degradation challenged modes. The 100% cohesive failures in ceramic for
by water storage.37 Long-term water storage along the feldspathic and leucite-reinforced feldspathic
with thermocycling (12,000 cycles performed over 180 ceramic groups suggests that the bonded interface
days) exhibited no impact on SBS for some of the test was stronger than those ceramics themselves when
resin cements. While the aging methodology might tested prior to thermocycling. The pattern somewhat
have exposed the adhesive interface to hydrolysis changed once the specimens were thermocycled with
and consequently weakened the adhesion for some cohesive failures (either in ceramic or composite)
test materials, it showed a tendency to increase the being noticed. On the other hand, adhesive failures
bond strength of RXU to leucite-reinforced feldspathic (100% of cases) were observed in the densely sintered
ceramic (not statistically significantly different). aluminum-oxide ceramic samples at baseline. This
Another interesting finding of this study was the can be explained by the fact that oxide ceramics have
reduction in bond strengths for ARC when bonded to flexural resistance higher than the other test ceramics.31
the densely sintered aluminum-oxide ceramic from It is evident that the SBS of resin cements to ceramics
16.8 MPa (early SBS) to 0 MPa (late SBS). The late is decreased by thermocycling, yet, surprising was
(lack of) bond strength resulted in most specimens the high spontaneous debonding rate for ARC and
debonding spontaneously before testing. Similarly, RXU after thermocycling in the densely sintered
specimens bonded with RXU to the same ceramic aluminum-oxide group.
The clinical relevance of bond strength tests is strength test methods. Indeed, failure modes were
often questioned because of the limitations of the predominantly cohesive within the ceramic for the
tests available. Moreover, comparison between silica-based ceramics. This fact, combined with the
studies may be challenging as different methods varying and non-axial forces applied in the standard
will result in different failure modes, for instance. shear bond strength test, indicates that shear bond
6,18,23,34,40,41,42,43,44
Yet, their value as screening tools for strengths are greater than inherent strength of
determination of the potential of resin cements, in the material and, indeed, question the validity of
the case of the present study, in the clinical setting the test set up. However, the applied set up with a
should not be ignored. In that regard, the shear bond shear load applied at the bonding interface through
strength test has been widely applied to compare a chisel is by far the most common bond strength
ceramics despite some researchers preferring test in dental material science and, at the very least,
modified tensile tests in order to eliminate the allows direct comparisons between materials and
occurrence of non uniform interfacial stresses. They also with other studies.
are typically present in conventional tensile and
shear bond strength tests. Non uniform distribution Conclusions
of stress may result in an excessive number of
cohesive failures in the ceramic substrate,45 which Within the limitations of this study, we concluded
compromises data interpretation. Controlled that resin cements perform differently when
clinical trials are ideal to test specific treatment bonded to different ceramic substrates. While
modalities and their long-term durability. However, all test resin cements worked similarly in the
in vitro investigations are indispensable to identify long-term to feldspathic and leucite-reinforced
superior materials before their clinical evaluation, feldspathic ceramics, only the 10-MDP-containing
especially for comparative studies of bonding resin cement provided durable bonds to densely
agents and cements. Additional in vitro and clinical sintered aluminum-oxide ceramic.
research is necessary before investigators can make
detailed recommendations on bonding methods to Acknowledgements
ceramic restorations. The work in this manuscript was performed in
In regards to the several of the failures occurring partial fulfillment of requirements for PhD degree.
within the ceramic substrate in the present study, David Farias was PhD candidate at the Universidade
cohesive failures should be expected for weaker Federal de Santa Catarina and completed the studies
ceramic substrates with the standard shear bond at the University of Pennsylvania.
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