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Purpose: This study evaluated the repair bond strength of differently surface-conditioned press-on-metal ceramic
to repair composites and determined the location of the accumulated stresses by finite element analysis.
Materials and Methods: Press-on-metal ceramic disks (IPS InLine PoM, Ivoclar Vivadent) (N = 45, diameter:
3 mm, height: 2 mm) were randomly divided into 3 groups (n = 15 per group) and conditioned with one of the
following methods: 9.5% hydrofluoric acid (HF) (Porcelain etch), tribochemical silica coating (TS) (CoJet), and an
unconditioned group acted as the control (C). Each group was divided into three subgroups depending on the repair
composite resins: a) Arabesk Top (V, a microhybrid; VOCO), b) Filtek Z250 (F, a hybrid;3M ESPE); c) Tetric Evo-
Ceram (T, a nanohybrid; Ivoclar Vivadent) (n = 5 per subgroup). Repair composites disks (diameter: 1 mm, height:
1 mm) were photopolymerized on each ceramic block. Microshear bond strength (MSB) tests were performed
(1 mm/min) and the obtained data were statistically analyzed using 2-way ANOVA and Tukey’s post-hoc test
(_ = 0.05). Failure types were analyzed under SEM. Vickers indentation hardness, Young’s modulus, and finite ele-
ment analysis (FEA) were performed complementary to MSB tests to determine stress accumulation areas.
Results: MSB results were significantly affected by the surface conditioning methods (p = 0.0001), whereas
the repair composite types did not show a significant effect (p = 0.108). The interaction terms between
the repair composite and surface conditioning method were also statistically significant (p = 0.0001).
The lowest MSB values (MPa ± SD) were obtained in the control group (V = 4 ± 0.8; F = 3.9 ± 0.7;
T = 4.1 ± 0.7) (p < 0.05). While the group treated with T composite resulted in significantly lower MSB val-
ues for the HF group (T= 4.1 ± 0.8) compared to those of other composites (V = 8.1 ± 2.6; F = 7.6 ± 2.2)
(p < 0.05), there were no significant differences when TS was used as a conditioning method (V = 5 ± 1.7;
F = 4.7 ± 1; T = 6.2 ± 0.8) (p > 0.05). The control group presented exclusively adhesive failures. Cohesive fail-
ures in composite followed by mixed failure types were more common in HF and TS conditioned groups. Elastic-
ity modulus of the composites were 22.9, 12.09, and 10.41 GPa for F, T, and V, respectively. Vickers hardness
of the composites were 223, 232, and 375 HV for V, T, and F, respectively. Von Mises stresses in the FEA
analysis for the V and T composites spread over a large area due to the low elastic modulus of the composite,
whereas the F composite material accumulated more stresses at the bonded interface.
Conclusion: Press-on-metal ceramic could best be repaired using tribochemical silica coating followed by silani-
zation, regardless of the repair composite type in combination with their corresponding adhesive resins, provid-
ing that no cohesive ceramic failure was observed.
Keywords: ceramic repair, finite element analysis, hydrofluoric acid, microshear bond strength, press-on-metal
ceramic, surface conditioning method, tribochemical silica coating.
J Adhes Dent 2014; 16: 63–70. Submitted for publication: 07.07.12; accepted for publication: 06.03.13
doi: 10.3290/j.jad.a30164
Part of this study was presented at the 16th Aegean Region Chambers of Dentists International Scientific Congress and Exhibition
(EBDO), 21-23 October, 2011, Izmir, Turkey.
a Research Assistant, Department of Prosthodontics, Faculty of Dentistry, Ege d Professor, University of Zurich, Dental Materials Unit, Center for Dental and
University, Izmir, Turkey. Performed experiments, analyzed data, prepared Oral Medicine, Clinic for Fixed and Removable Prosthodontics and Dental
draft of manuscript, discussed results, commented on manuscript at all Materials Science, Zurich, Switzerland. Designed study, wrote and edited
stages. manuscript, discussed results, commented on manuscript at all stages.
b Associate Professor, Department of Prosthodontics, Faculty of Dentistry, Ege e Professor, Department of Prosthodontics, Faculty of Dentistry, Ege University,
University, Izmir, Turkey. Designed study, wrote and edited manuscript, dis- Izmir, Turkey. Discussed results, commented on manuscript at all stages.
cussed results, commented on manuscript at all stages.
c Assistant Professor, Department of Material Engineering, Engineering Faculty, Correspondence: Dr. Burcu Kanat, Ege University, School of Dentistry, Depart-
Celal Bayar University, Manisa, Turkey. Conducted finite element analysis, ed- ment of Prosthodontics, Bornova 35100 Izmir, Turkey. Tel: +90-232-388-0327,
ited manuscript, discussed results, commented on manuscript at all stages. Fax: +90-232-388-0325. e-mail: burcukanat@hotmail.com
Table 1 The brands, abbreviations, manufacturers, chemical compositions, and batch numbers of the materials
used in this study
Hydrofluoric acid (HF) Porcelain Etch, Ultradent; Hydrofluoric acid (9.5%) 18005525512
South Jordan, UT, USA
CoJet-Sand (TS) 3M ESPE; Seefeld, Germany Aluminum trioxide particles coated with silica, particles 68421
size: 30 μm
Solobond M VOCO; Cuxhaven, Germany bis-GMA, HEMA, phosphate methacrylates, BHT, 0902048
acetone, CQ, amine accelerator
Arabesk Top (V) VOCO bis-GMA, UDMA and TEG-DMA monomers, microfillers, 750490
(microhybrid) and small particle fillers (56 vol%)
Filtek Z250 (F) 3M ESPE bis-GMA, UDMA, bis-EMA monomers, ZrO2, 8PR
(hybrid) SiO2 containing fillers (60 vol%)
Tetric EvoCeram (T) Ivoclar Vivadent Dimethacrylate monomers, barium glass, ytterbium K01495
(nanohybrid) trifluoride, mixed oxide and prepolymer fillers (55 vol%)
Bonding Procedures ure occurred between the ceramic and repair composite
The specimens in each conditioned group were ran- (MIX).5,24,31
domly divided into 3 subgroups (n = 15 per subgroup) to
be repaired with different resin composites, namely: Ara- Vickers Hardness and Finite Element Analysis
besk Top ([V], VOCO; Cuxhaven, Germany; microhybrid), The instrumented indentation method (Fischer-Cripps
Filtek Z250 ([F], 3M ESPE; hybrid), and Tetric EvoCeram indentation tester; Sydney, Australia) was employed,
([T], Ivoclar Vivadent; nanohybrid). which provides a continuous record of the variation of
The corresponding bonding agents of the resin compos- indentation load, P, as a function of the depth of pen-
ites (Solobond M, VOCO; Adper Scotchbond Multi-Purpose, etration (h), into the indented specimen through which
3M ESPE; Heliobond, Ivoclar Vivadent) were applied using a hardness and Young’s modulus of the materials under
microbrush, air thinned, and photopolymerized (Bluephase, applied peak load were calculated.20,42
Ivoclar Vivadent) for 10 s. Repair composites were applied During the loading step of the test, the response
in one layer (diameter: 1 mm, height: 1 mm) using a poly- generally follows the relation described by Kick’s Law:
ethylene mold on the conditioned ceramic surfaces and P=Ch2,where C is the loading curvature. The average
photopolymerized for 40 s. After polymerization, the poly- contact pressure (hardness), H=Pmax/Amax (Vickers hard-
ethylene molds were gently removed and the specimens ness at maximum load) can be identified with the hard-
were stored in dry conditions in the dark at 37°C. ness of the indented material.6 Using the initial part of
the unloading curve, both stiffness and contact depth
Microshear Bond Strength Test and Failure Analysis are determined at the maximum depth of penetration,
The microshear bond strength (MSBS) tests were per- h = hmax. Then, the stiffness of the contact is given by
formed in a universal testing machine (Autograph,
Shimadzu; Kyoto, Japan) at a crosshead speed of
S = dP = 2 Er √Ac
1 mm/min, with the shear force applied to the ceramic/ dh √/
composite interface until debonding occurred. After MSB
tests, all specimens were analyzed to identify the failure 1 1 – p2 1 – po2
= +
types using an optical microscope (MP 320, Carl Zeiss; Er E Eo
Jena, Germany) at 50X magnification.
After evaluating all specimens, the failure types were where Er = reduced elastic modulus, E = elastic modu-
defined as a) adhesive between the ceramic and repair lus of material, Eo = elastic modulus of indenter (dia-
composite (ADHES); b) cohesive in the repair composite mond), and p and po are the Poisson ratios of the
(COHES-com); c) mixed when cohesive and adhesive fail- material and indenter (diamond).27
N = 45 Polyethylene plate
control
HF
1 mm SiO
2
2 mm
POM ceramic
3 mm
n = 15 n = 15 n = 15
sil
an
Polyethylene plate Polyethylene plate Polyethylene plate
Fig 1 Schematic representation of specimen preparation for microshear bond strength test: press-on-metal ceramic disks were
prepared; polyethylene plates with 1-mm-diameter hole prepared in the middle; the specimens were divided into 3 groups (control
and two surface conditioning groups); silane was applied to all specimens; each main group was divided into 3 subgroups depend-
ing on the repair composite resin types; bonding agent specific to the composite resin systems was applied; the composites were
bonded using a polyethylene mold; ceramic block-resin composite specimens were obtained.
Type of failure*
HF TS C
Composite ADHES COHES-com MIX ADHES COHES-com MIX ADHES COHES-com MIX
V 1 3 1 2 2 1 5 0 0
F 1 3 1 1 4 0 5 0 0
T 2 2 1 2 1 2 5 0 0
ADHES: Adhesive failure between the ceramic and repair composite; COHES-com: Cohesive failure in the repair composite; MIX: Cohesive failure of the
repair composite and adhesive failure between the ceramic and repair composite.
Fig 2a SEM image of the press-on- Fig 2b SEM image of the press-on- Fig 2c SEM image of the press-on-
metal ceramic surface (2000X) of an un- metal ceramic surface (2000X) of an metal ceramic surface (2000X) of a TS-
treated control specimen. Note the intact HF-etched specimen with visible leucite conditioned specimen. Note the rough
glassy phase. crystals due to glass matrix dissolution. surface irregularities.
Fig 3a FEA analysis of ceramic-composite combination show- Fig 3b FEA analysis of ceramic-composite combination show-
ing stress accumulation areas. Initial situation before force ing Von Mises stresses for V composite.
application.
Fig 3c FEA analysis of ceramic-composite combination show- Fig 3d F composite material accumulated stresses at the
ing T composite spreading on a large area due to low elasticity bonded interface possibly due to the alleged rigidity of this
modulus of the composite resin. composite.
on-metal ceramics, this study was undertaken to investi- greater bond strength of repair composite resin could
gate the most effective combination of surface condition- be obtained.3 HF acid dissolves the glassy matrix of
ing method and repair composite. Chipping or fractures the ceramic (SiO2) and remaining leucite or lithium dis-
of veneering ceramics have been attributed to a thermal ilicate, leading to microporosities. This is because the
mismatch between the ceramic and the framework, lack affinity of fluoride to silicon is higher than to oxygen:
of calibration of the ceramic furnace, laboratory mistakes, 4HF+SiO2ASiF4+2H2O.32 On the other hand, air abrasion
iatrogenic causes, brittleness of the ceramics, or trauma.29 with silica coating decreases the water contact angle,
The quality and durability of the bond between the ceramic which provides adsorption of the silane coupling agent;
veneer and the repair composite also affect the longevity this in turn facilitates the diffusion of the resin composite
and clinical success of a restoration.26 The key principles into micromechanical porosities of the ceramic due to
for successful adhesion of repair composite to a ceramic the increased surface roughness.17 Furthermore, silane
surface are preparation of a clean surface, providing a improves the interfacial adhesion of resin composite to
rough surface for micromechanical retention, supplying ceramic by about 25%.13 The silane (3-methacryloxypropyl
chemical retention with silane, adequate wetting of the trimethoxysilane) used in this study is a bifunctional mon-
ceramic by the bonding agent, creating enough surface omer containing a hydrolyzable methoxy group that bonds
energy, and wettability of the repair composite.10,18,29 to the SiO2 of the ceramic and involves a nonhydrolyzable
The viscosity of the resin composite and adhesive resin methacrylate group that copolymerizes with the organic
systems plays an important role in their wettability behav- matrix of the composite resin. The methoxy groups (-Si-
ior, due to variations in surface tension and contact angle O-CH3) of silane react with water to form three silanol
of the adhesive resin.9 In this study, resin composite and groups (-Si-OH), which eventually react with the silica layer
corresponding adhesive system combinations belonging deposited on the ceramic surface to form a siloxane (-Si-
to the same manufacturer were preferred in all groups O-Si-O) network. Methacrylate groups of the silane mol-
in order to eliminate possible chemical incompatibility ecules react with the methacrylate groups of composite
as well as wettability problems. Ceramic surfaces can resins.32 When silane is used without any surface condi-
be roughened in different ways to obtain micromechani- tioning methods, the bond strength is affected negatively
cal retention. HF acid roughens feldspathic ceramic, and due to insufficient mechanical retention.37 However, if
the initial bond strength is high, it has been shown that ture initiation from flaws at the interface or in high stress
it decreases over time10 because of the formation of a accumulation regions in the substrate.11 Bond strength
multimolecular layer of silane, which is less stable than tests have been used to predict the clinical performance
a monolayer of the deposited silane.19 Silanization after of repaired ceramic restorations in the oral environment.26
HF acid etching has been recommended for successful Shear stresses have been reported to be more clinically
bonding between ceramic and resin composite vs silane relevant due to similarity to the direction of the chewing
application alone.14,17 The MSB results obtained from the forces.36 It is assumed that the restorations which pos-
control group of the present study were significantly lower sess high resistance to MSB forces have high survival
with respect to HF acid and tribochemical silica coating rates under masticatory forces.15 However, bond strength
groups, since only silane treatment without any surface interpretations should also be coupled with failure type
modification was employed. analysis. The control group demonstrated low MSB values
Subsequent application of bonding agent on the si- and showed only adhesive failures due to weak bonding
lanized ceramic surface produces a carbon-carbon double based on the lack of surface conditioning. This also indi-
bond between the nonhydrolyzable functional group of the cates the indispensability of surface modification prior to
silane and the methacrylate groups of the matrix resin. silane and/or adhesive resin application, irrespective of
In this way, the bifunctional activity of silane can provide the repair composite type. Cohesive failure in composite
successful adhesion between the organic bonding agent after debonding can indicate a stable bond compared
and fractured inorganic ceramic.25 When repairing resin- to mixed failures.7,23 The HF and TS groups presented
based composite restorations, the use of bonding agents mainly cohesive failure types in composites and mixed
containing hydrophobic monomers has been recom- failures. It should be noted than in none of the groups was
mended and higher shear bond strength values have been cohesive failure in the ceramic substrate observed. This
obtained for the repaired composite specimens with the implies that the bond strength obtained at the ceramic/
use of a bonding agent than without.40 Additionally, the composite interface did not exceed the cohesive strength
bonding agent wets the surface to be treated and alters of the ceramic substrate tested. Thus, adhesive promot-
surface tension, allowing deep penetration into pits and ers or conditioning methods for improved adhesion to this
grooves on the repair surface with the same mechanism ceramic require development.
for enamel and dentin.40 In this study, all repair compos- Complementary tests measuring Vickers hardness and
ites were applied in combination with their corresponding elasticity modulus in addition to implementing these data
adhesive resins, as clinicians often use the adhesives in the FEA model provided additional information on the
belonging to the composite system. Results may change stress distribution at the ceramic/composite interface.
when adhesives other than the respective ones are used. The elasticity modulus of V (10.41) and T (12.09) compos-
Except for the Tetric EvoCeram (T) composite in combina- ites were lower than that of F (22.9). In support of these
tion with HF conditioning, all other composites presented findings, FEA analysis – showing stress distributions of
nonsignificantly different results within each conditioning these materials at identical loading conditions – indicated
group. This could be attributed to the fact that the mono- larger stress areas both in the composite and the bonded
mer of the nanohybrid composite Tetric EvoCeram is com- area, compared to F, where a smaller stress area and
posed of bis-GMA and UDMA and the hybrid composite larger strain field were observed. Nevertheless, the inci-
Filtek Z250 contains TEG-DMA, UDMA, and bis-EMA. The dence of cohesive failures in this composite was not lower
maximum polymerization degrees of UDMA and bis-GMA than in the other composites, possibly indicating that its
were reported to be higher than for TEG-DMA and bis- corresponding adhesive resin provided better adhesion
EMA.38 However, a lower % filler content of the material which compensated for the cohesive strength of this ma-
might have led to some unreacted monomers in reacting terial. Clinical studies should report the location and sur-
with silanized silica particles and resulted in higher MSB vival of repairs in combination with the materials tested.
values and fewer adhesive failures. The resin composite
with low viscosity based on reduced filler content has
an effect on the adhesion due to decreased contact an- CONCLUSIONS
gle. Moreover, a rougher substrate has a greater surface
area, which promotes increased surface free energy and From this study, the following could be concluded:
thereby better wettability of the resin composite.33,34 In y When press-on-metal ceramic is repaired using hy-
future studies, surface roughness created as a function drofluoric acid followed by silanization, microhybrid
of deposition duration should be examined for correlation and hybrid composites in combination with their cor-
with bond strength. responding adhesive resins showed similar results,
Material properties, flaw distribution, level of stress, but the nanohybrid composite presented significantly
and environmental conditions are the main factors affect- lower results.
ing the fracture behavior of adhesive interfaces. Thus, the y Tribochemical silica-coated and silanized groups did
reliability of the bonded interfaces can be evaluated by not show significant differences between any of the
examining failed surfaces together with fracture mechan- repair composites tested.
ics analysis.4 The finite element stress analysis in the y After debonding, in both conditioning groups, mainly
present study revealed that nonuniform interfacial stress cohesive failures in the composite were observed, fol-
distribution caused by MSB tests might have led to frac- lowed by mixed failure types.