1
UNIVERSIDADE FEDERAL DE SANTA MARIA
CENTRO DE CIENCIAS DA SAÚDE
CURSO DE ODONTOLOGIA
EFEITO DO JATEAMENTO COM ALUMINA E DE
DIFERENTES SISTEMAS DE CIMENTAÇÃO NA
ADESÃO A ZIRCÔNIA
TRABALHO DE CONCLUSÃO DE CURSO
Rafaella Grasel
Santa Maria, RS, Brasil
2015
2
EFEITO DO JATEAMENTO COM ALUMINA E DE
DIFERENTES SISTEMAS DE CIMENTAÇÃO NA ADESÃO A
ZIRCÔNIA
Rafaella Grasel
Trabalho de Conclusão de Curso apresentado ao curso de Graduação em
Odontologia da Universidade Federal de Santa Maria (UFSM-RS) como
requisito parcial para obtenção do grau de Cirurgiã-Dentista.
Orientador: Professor Doutor Luiz Felipe Valandro Soares
Santa Maria, RS, Brasil
2015
3
AGRADECIMENTOS
À Universidade Federal de Santa de Maria (UFSM) e, de maneira especial, ao seu corpo
docente e técnicos administrativos, responsáveis pela minha formação profissional através do
Ensino Público. Apesar das dificuldades e limitações de recursos, formaram muito mais que
uma Cirurgiã-Dentista, mas também uma profissional mais humana, dinâmica e sensível.
À Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES) que, através de
Edital Público, financiou meu Estágio de Iniciação Científica no Exterior, na modalidade
Graduação Sanduíche, ao longo de três meses, viabilizando, desta forma, a execução deste
projeto de pesquisa e o início de uma nova fase na minha vida acadêmica.
À Mathematics of Information Technology and Complex Systems (MITACS) que, pelo
programa Globalink Research Internship, também financiou meu Estágio de Iniciação
Científica no Exterior e me proporcionou a oportunidade de conhecer um novo país, novas
culturas e novas pessoas, abrindo meus olhos a um novo mundo, de múltiplas possibilidades.
À University of Western Ontario (UWO), na pessoa da Prof. Dr. Maria Jacinta Santos, pelo
cuidado e atenção. Obrigada por me receber de braços abertos e me integrar, não só em seu
meio acadêmico e de pesquisa, mas também em seu meio familiar. Muito obrigada por sua
amizade.
Ao Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPQ) pelo benefício
da Bolsa de Iniciação Científica, como incentivo à continuidade e aprofundamento na
pesquisa científica.
4
RESUMO
Trabalho de Conclusão de Curso
Curso de Odontologia
Universidade Federal de Santa Maria
EFEITO DO JATEAMENTO COM ALUMINA E DE
DIFERENTES SISTEMAS DE CIMENTAÇÃO NA
ADESÃO A ZIRCÔNIA
AUTORA: RAFAELLA GRASEL
ORIENTADOR: PROF. LUIZ FELIPE VALANDRO
Data e Local da defesa: Santa Maria, 02 de Dezembro de 2015.
O presente estudo avaliou o efeito do jateamento com alumia e diferentes estratégias
de cimentação (primer/cimento resinoso) na adesão à zircônia. Oitenta blocos (4x4x3mm) de
Zirconia Y-TZP Lava Frame (3M ESPE) foram confeccionados e randomicamente
distribuídos em oito grupos (n = 10) de acordo com duas condições de tratamento de
superfície (sem tratamento ou jateamento com alumina 50 µm) e quatro estratégias de
cimentação (SU: Scotchbond Universal/RelyX Unicem 2; ZP: Z-prime Plus/Duo-link
Universal; MB: Monobond Plus/Variolink II; e AP: Alloy Primer/ED Primer II/Panavia F
2.0). Após o tratamento de superfície e aplicação do primer, o cimento resinoso foi
manipulado e aplicado sobre a zircônia, usando uma matriz para formar um cilindro (2 mm
diâmetro x 2 mm altura), seguido de fotoativação por 40 segundos. Os espécimes
foram, então, armazenados em água destilada (37 ° C) por 120 dias e submetidos ao teste de
cisalhamento, seguido da análise do modo de falha em microscópio ótico. ANOVA dois
fatores e teste de Tukey (α = 0.05) foram utilizados para análise dos dados. O jateamento com
alumina (Al) promoveu maiores valores de adesão para três estratégias de cimentação, exceto
para SU. Sem tratamento de superfície, SU foi a melhor estratégia de cimentação, enquanto
que, com jateamento, as estratégias de cimentação Al-SU, Al-ZP e Al-MB obtiveram valores
superiores comparado à Al-AP. Conclui-se que o jateamento com alumina da superfície da
zircônia parece ser dispensável para o grupo SU, enquanto o jateamento (alterações
topográficas) parece ser necessário para os grupos ZP, MB e AP.
Palavras chave: Tratamento de Superfície de Zircônia. Teste de Cisalhamento. Primers de
Zircônia.
5
SUMÁRIO
1. TITLE PAGE...................................................................................... 7
3. CLINICAL RELEVANCE................................................................. 8
4. ABSTRACT………………………………………………………. 8
5. INTRODUCTION.............................................................................. 9
6. METHODS AND MATERIALS....................................................... 10
6.1 Specimens’ preparation....................................................................................... 10
6.2. Cementation procedure....................................................................................... 11
6.3. Shear bond strength test..................................................................................... 11
6.4. Failure type analisys ........................................................................................... 11
6.5. Data analisys........................................................................................................ 11
7. RESULTS............................................................................................ 12
8. DISCUSSION..................................................................................... 12
9. CONCLUSION................................................................................... 15
10. REFERENCES................................................................................. 16
11. ACKNOWLEDGEMENTS............................................................. 21
12. TABLES............................................................................................ 22
14. FIGURES..........................................................................................
15. ANEXOS...........................................................................................
25
26
6
O presente Trabalho de Conclusão de Curso será apresentado na forma de Artigo Científico
e, para tanto, está formatado segundo as normas1 exigidas para publicação no periódico
Operative Dentistry – Qualis CAPES A1
com o título
“Luting systems with universal adhesive containing multiples bonding
promoters can be an alternative to alumina air-abrasion for resin bond
improvement to zirconia”
1 As normas de formatação exigidas pelo periódico constam no Anexo A deste trabalho.
7
Luting systems with universal adhesive containing multiples bonding promoters can be
an alternative to alumina air-abrasion for resin bond improvement to zirconia
Short title: resin adhesion to YTZP ceramic
Rafaella Grasel, Maria Jacinta Santos, Heleine Maria Chagas Rêgo, Marília Pivetta
Rippe, Luiz Felipe Valandro
*
Rafaella Grasel, DDS, Federal University of Santa Maria (UFSM), Faculty of Odontology,
Department of Prosthodontics, Santa Maria, Rio Grande do Sul State, Brazil. Address: 1184 Floriano
Peixoto St, 97015-372, Santa Maria/RS, Brazil. ([email protected]).
Maria Jacinta Santos, DDS, MSc, PhD, Associate Professor. University of Western Ontario (UWO),
Schulich School of Medicine & Dentistry, London, Ontario, Canada. Address: Dental Sciences
Building, Postal code N6A 5C1, London/ON, Canada. ([email protected]).
Heleine Maria Chagas Rêgo, DDS, MSc, PhD. Substitute Professor. Health Sciences and Biological
Centre, Department of Dentistry, Faculty of Odontology, Federal University of Sergipe, Sergipe State,
Brazil. Address: Claudio Batista St, 49060-100, Aracaju/SE, Brazil. ([email protected]).
Marília Pivetta Rippe, DDS, MSc, PhD, Adjunct Professor. Graduate Program in Oral Science,
Prosthodontics Unit, Faculty of Odontology, Federal University of Santa Maria, Rio Grande do Sul
State, Brazil. Address: 1184 Floriano Peixoto St, 97015-372, Santa Maria/RS, Brazil.
*Luiz Felipe Valandro, DDS, MSc, PhD, Associate Professor. Head of M.Sci.D./Ph.D. Graduate
Program in Oral Science, Prosthodontics Unit, Faculty of Odontology, Federal University of Santa
Maria, Rio Grande do Sul State, Brazil. ([email protected])
*Corresponding author:
Luiz Felipe Valandro, D.D.S., M.Sci.D., Ph.D., Associate Professor,
Federal University of Santa Maria
Faculty of Odontology
Head of Ph.D.-M.Sci.D. Graduate Program in Oral Science
Prosthodontics Unit
R. Floriano Peixoto, 1184, 97015-372,
Rio Grande do Sul State, Santa Maria, Brazil.
Phone: +55-55-3220-9276, Fax: +55-55-3220-9272
E-mail: [email protected] (Dr LF Valandro)
8
Luting systems with universal adhesive containing multiples bonding
promoters can be an alternative to alumina air-abrasion for resin bond
improvement to zirconia
CLINICAL RELEVANCE
The alumina particle air-abrasion (topographical alterations) of the inner surface of Y-TZP
restorations and the application of universal primers (adhesives), containing multiple bond
promoters (methacrylates monomers, including phosphate monomers like 10-MDP, and
silane) optimize the adhesion of Y-TZP to resin cements.
ABSTRACT
This study aimed to evaluate the effect of different primer/resin luting agent
combinations and alumina air-abrasion on the adhesion to zirconia. Eighty blocks
(4x4x3 mm) of Lava Frame Zirconia (3M ESPE) were produced and randomly assigned
into eigth groups (n=10) according to two zirconia surface treatments (untreated or air-
abrasion with 50 µm alumina particles) and four luting systems (SU: Scotchbond
Universal/RelyX Unicem 2; ZP: Z-Prime Plus/Duo-link Universal; MB: Monobond
Plus/Variolink II; and AP: Alloy Primer/ED Primer II/Panavia F 2.0). After the
conditionings and primer applications, resin luting agents were manipulated and
applied on the zirconia, using a matrix, to form a cylinder (2 mm diameter x 2 mm
high), followed by photo-activation for 40 seconds. After that, the specimens were stored
in distilled water (37 °C) for 120 days and then submitted to shear bond strength test,
followed by failure mode evaluation under optical microscope (3X). A two-way ANOVA
and Tukey’s test (α = 0.05) were used for data analysis. The alumina air-abrasion (Al)
promoted higher bond values for three luting systems, exception for SU, which showed
the best results without air-abrasion, while using air-abrasion the Al-SU, Al-ZP, and Al-
MB presented higher values compared to Al-AP. It concludes that the alumina air-
abrasion of zirconia surface seems to be dispensable for SU group, while the air-
abrasion (topographical alterations) has enhanced the adhesion of ZP, MB and AP
groups.
Keywords: Surface Treatment of Zirconia, Shear Bond Strength, Zirconia Primers.
9
INTRODUCTION
The use of zirconia-based ceramics (Y-TZP) has increased over the last decade,
especially due to their superior mechanical and aesthetic properties used as frameworks and
monolithic restorations in posterior areas.1,2,3,4,5
Despite the large clinical application of
zirconia ceramics, the major drawback is related to its unpredictable bond with resin
cements.1,2,3,6
Zirconia is a densely sintered ceramic that offers chemical and dimensional
stability and desirable physical properties, such as high flexural strength, high elastic
modulus, and high fracture toughness compared to other ceramic materials.4 On the other
hand, polycrystalline ceramics are non-etchable by hydrofluoric acid since it does not contain
amorphous silica in its composition.4,5,6
Therefore, traditional surface treatments methods
indicated for silica-based ceramic, such as hydrofluoric acid followed by silane coupling
agent application, are impracticable on the zirconia-based ceramics due to their high
crystalline content and silica-free surface.2,4,5,6
The use of conventional cements, such as zinc phosphate or resin-modified glass
ionomer cements, had been initially recommended by the manufacturers for luting zirconia
restorations.4 However, adhesive cementation has been shown to increase fracture resistance,
4
the fatigue limit,7 and improve the longevity
of ceramic restorations,
8 besides sealing internal
surface defects created by airborne particle abrasion.9 Achieving a reliable adhesion to
zirconia-based ceramics would further expand the application of this great material.4
However, it requires surface treatments based on physical and/or chemical treatments, such as
air-abrasion and zirconium oxide dedicated primers, which will promote an interaction
between zirconia and luting substrate.
Air-abrasion with aluminum oxide particles aims to roughen the internal surface of the
ceramic restorations to optimize the adhesion area and promote better mechanical interlocking
with the resin cement.4,5
Although studies have shown that the particles air-abrasion promote a
resin bond improvement to zirconia materials,10,11
previous studies reported that this treatment
creates surface micro crack and defects which can damage the mechanical properties of the
material.12,13,14,15
Hence the use of zirconia primers has been studied as substitute to air-
abrasion in order to promote the chemical bond to zirconia trough phosphate monomers
without mechanical bond.
Phosphate monomers act as bi-functional molecules, in which one tip connects with
the ceramic’s metal oxides (such as aluminum and zirconium), while the other extremity
copolymerizes with the resin cement matrix. Some examples of these bi-functional monomers
10
are the 10-MDP (10-methacryloyloxi-decyl-dihydrogen-phosphate), 2-MEP (2-
methacryloyloxyethyl dihydrogen), and 6-MHP (6-methacryloyloxyhexyl dihydrogen
phosphate).16
It has been found that MDP monomers promote a water-resistant chemical bond
to densely sintered zirconia ceramics.5,17
MDP monomers are also available in some resin
cements such as RelyX Unicem (3M ESPE, Maplewood, Minessota,USA) and Panavia
(Kuraray Noritake Dental Inc, Chiyoda-ku, Tokyo, Japan). Nowadays, several primers that
claim chemical adhesion to zirconia are available in the market. However, more studies are
necessary to verify their efficacy and long-term bond durability when combining different
primers and resin cements.18
Thus, the aim of this study was to evaluate the effect of alumina particle air-abrasion
and different luting systems (primer / resin luting agent) on bond strength to zirconia after
aging. The research hypotheses were: 1) Irrespective of the luting systems adopted, the
alumina air-abrasion would promote bond improvement; 2) There would be no difference in
bond strength among the different luting systems.
METHODS AND MATERIAL
The resin cements and primers used in this study are shown in Table 1.
Specimens’ preparation
Eighty blocks (4 x 4 x 3 mm) Lava Frame (3M ESPE) zirconia were obtained, sintered
as recommended by manufacturer, and embedded in auto-polymerizing acrylic resin cylinders
(Orthodontic Resin, Denstply Caulk, Milford, Delaware, USA), keeping free zirconia surface
for bond procedures. After the resin acrylic polymerization, the zirconia’s exposed surface
was ground-finished with a 800-grit silicon carbide abrasive (Auto Advanced, 3M ESPE)
under running water on a polishing machine (Buehler Metaserv, Buehler, Düsseldorf, North
Rhine-Westphalia, Germany) for 1 min. Afterwards, the specimens were ultrasonically
cleaned for 5 min in deionized water and then wiped with 95 vol.% ethanol.
Zirconia specimens were randomly allocated into eight groups (n=10), as described in
Table 2. Half of these groups did not receive zirconia surface treatment, while other groups
had the zirconia surface air-abraded (aluminum oxide, 50 microns, per 15 sec., device –
sample distance of 10 mm, pressure of 87 psi, perpendicular to the surface, by linear motion),
using a micro-etcher (Optiblast, Buffalo Dental Mfg Inc, New York, New York, USA).
11
Cementation procedure
After particle air-abrasion, the primer agents were applied over the treated zirconia
surface following the manufacturer’s instructions (Table 2). A cylinder of resin cement was
built on the ceramic surface using an Ultradent SBS device (Bisco, Schaumburg, Illinois,
USA) with an inner diameter of 2 mm and height of 2 mm. The resin cements were
manipulated following manufacturer’s instructions (Table 2). Resin cement cylinders were
light cured (Bluephase style, Ivoclar Vivadent, Schaan, Oberland, Liechtenstein) with
intensity of 1330 mW/cm² for 40 seconds. All specimens were prepared by the same operator
to avoid inter-operator variability.
Shear Bond Strength Test
After four months of storage in distillated water at 37°C for aging process, all
specimens were submitted to the shear bond strength test in a universal test machine
(Compact force gauge, Bisco, USA) at a crosshead speed of 0.5 mm/min, using a flat rod as
testing assembly. The bond strength “R” (MPa) was calculated using the following formula:
R=F/A, in which “F” means the load for specimen failure (N) and “A” is the cross sectional
interfacial area (mm²).
Failure type analysis
After the shear bond testing, the debonded surfaces were observed through an optical
microscope (Microview Canada, Markham, Ontario, Canada), at 3x magnification to
determinate and classify the failure mode. The evaluator was ‘blind’ for study conditions. The
failure types were classified into the following categories: (A) adhesive, at the zirconia-
cement interface; and (B) cohesive, in the resin cement structure. Some micrographs (S-2500
Hitachi Scanning Electron Microscope, Hitachi High Technologies America, Inc.,
Schaumburg, Illinois, USA) of tested samples were performed.
Data analysis
Statistical analysis was performed using the software Statistix 8.0 for Windows
(Analytical Software Inc, Tallahassee, Florida, USA). Bond strength data (MPa) were
subjected to two-way analysis of variance (ANOVA) and Tukey’s tests ( = 0.05). P values
less than 0.05 are considered to be statistically significant in all tests. Multiple comparisons
were made by repeated measures tests at a significance level of 0.05.
12
RESULTS
A two-way ANOVA revealed that the cementation approach (p < 0.0001) and the
zirconia surface treatment (p < 0.0001; Al2O3 > untreated) showed a significant effect on the
bond strength between the zirconia and the resin cement. Interaction between factors, surface
treatment x cementation strategy (p = 0.0062), was also significant.
Surface treatment by particle air-abrasion (Al2O3) increased statistically bond strength
values for all luting systems, except for Scotchbond Universal/RelyX Unicem 2 (Table 3).
Comparing the different luting systems without air-abrasion, the Scotchbond
Universal/RelyX Unicem 2 promoted the highest bond values, while evaluating the same
groups with treatment, the Alloy Primer/ED Primer II/Panavia F 2.0 presented the lowest
shear bond strength values (Table 3).
No pre-test failures occurred in this study. The percentages of adhesive and cohesive
failure after test are represented in Table 3. Representative micrographs of tested samples are
shown in the Figure 1.
DISCUSSION
The first hypothesis (bond improvement with the use of alumina air-abrasion
irrespective of the luting system) was partially accepted, once the zirconia surface treatment
increased bond strength values when compared to untreated surface, except for the luting
system that used Scotchbond Universal/RelyX Unicem 2.
Air-abrasion with aluminum oxide particles, microspheres cross-section between 50
mm and 125 mm, is considered as the main zirconia’s surface treatment prior to cementation
procedure due to the great results achieved and ease of chair-side procedure.19,20,21
The
alumina air-abrasion aims to roughen the zirconia surface, producing microretentions and
increasing the adhesion area.4,5,20
This way, alike the hydrofluoric acid treatment on silica-
based ceramics, alumina air-abrasion allows a mechanical interlocking between these acid
resistant ceramics and resin luting/ceramic primer.
Although air-abrasion has been proven to be a successful treatment, enhancing the
bond strength,10,11,22,23,24,25
its positive influence on resin adhesion to zirconia is contradictory.
Murthy et al. (2014)26
evaluated the effect of different surface treatments on shear bond
strength between zirconia and resin luting agents and observed no significant differences on
bond strength values between control (no surface treatment) and alumina air-abrasion (either
with 110 μm or 250 μm) groups. Foxton et al. (2011) 27
obtained a durable (six months) bond
13
to Procera All Ceram and Procera All Zirkon using a ceramic primer containing MDP-
phosphate monomer, without any additional surface treatment (alumina air-abrasion or
erbium-laser- treated). These findings are in accordance to the findings observed in the
present study when considering Scotchbond Universal/RelyX Unicem 2 luting system, in
which air-abrasion did not improve the adhesion to zirconia. Air-abrasion had a positive role
by increasing bonding values for the luting systems with Z-Prime Plus/Duo-link Universal,
Monobond Plus/Variolink II, and Alloy Primer/ED Primer II/Panavia F2.0, which is in
accordance with several studies.10,11,22,23,25,28,29
Furthermore, Amaral et al. (2014) 24
and
Inokoshi et al. (2014) 30
reported that air-abrasion is required when luting zirconia, even when
using novel primers and universal adhesives. Therefore, the fact that Scotchbond
Universal/RelyX Unicem 2 did not present increased bonding values after alumina air-
abrasion may be related to its chemical composition. This primer has been proposed as a
substitute to air-abrasion (morphological modifications) for zirconia surface treatment prior to
the luting procedure, due to the chemical adhesion to zirconia, given by its differentiated
chemical composition (Table 1), including multiple bond promoters, as reported below.
In this sense, the second null hypothesis (no difference in bond strength among the
different luting procedures) was denied since different luting systems resulted in different
bond strengths. Without surface treatment with air-abrasion, Scotchbond Universal/RelyX
Unicem 2 obtained the highest bond strength values. However, when alumina air-abrasion
was performed, it potentiated the adhesion of Z-Prime Plus/Duo-link Universal and
Monobond Plus/Variolink II, resulting in similar bond strength of Scotchbond
Universal/RelyX Unicem 2 (groups with the highest bond strength values). Even with an
increase in bond strength after air-abrasion, Alloy Primer/ED Primer II/Panavia F 2.0
presented the lowest bond values. Recent investigations have reported that the selection of the
luting agent is one of the most important factors for luting zirconia restorations.20,25,31,32,33,34
As aforementioned, another alternative surface treatment to zirconia is the use of
ceramic primers for chemical bond between zirconia surface and resin luting agent trough
phosphate monomers. They act as bi-functional molecules and improve the wettability of the
ceramic surface and bond strength to resin cements, by chemical interaction.35
Thereby, a
luting approach that includes phosphate monomers could enhance, for example, bond strength
and restorations longevity.24,25,28,29,32,36,37,38
Inokoshi et al. (2014)30
and De Souza et al.
(2014)35
observed that the application of an MDP-based adhesive might improve the bond
strength to zirconia. Differently, Cristoforides et al. (2012)39
observed that a MDP-containing
14
liner is not effective for zirconia Y-TZP composite repairs. The 10-MDP (10-
methacryloyloxi-decyl-dihydrogen-phosphate) is one of the well-known phosphate
monomers. Being in use for more than 20 years, it has achieved promising results in adhesion.
Its phosphoric acid group bonds chemically to zirconia atoms while the double bonds on the
other end of the molecule copolymerize with the resin monomers, as well as they are able to
create ionic bonds with calcium from hydroxyapatite.17,39,40
In the present study, it was
observed that primers/adhesives that associate multiples adhesion promoters, 10-MDP and
others, appear to promote efficient adhesion to zirconia.
Scotchbond™, as a universal adhesive, can be used in both tooth and indirect
restoration surfaces, including metals, composites, glass-containing ceramics and non-glass
ceramics. This property is given by its composition (Table 1) that contains multiple adhesion
promoters, such as methacrylate monomers, 10-MDP, polyalkenoic acid copolymer, and
silane. The resin cement RelyX Unicem 2 also presents (Table 1) methacrylate monomers
containing phosphoric acid groups. In the current study, this luting approach yielded the
highest bonding values, as observed by Amaral et al. (2014),24
De Souza et al. (2014),35
and
Seabra et al. (2014).41
This finding was assigned to the adhesive chemical composition, whose
MDP molecules may have interacted chemically to zirconium and aluminum (Al₂O₃) oxide
particles due to their affinity to metallic oxides. Amaral et al. (2014)24
have also observed that
Scotchbond Universal was effective in promoting durable bond to zirconia even without
previous air-abrasion with silica or alumina.
Hence, the present luting system may be a safe alternative for a stable bond to zirconia
without the need of additional surface treatments, as the use of air-abrasion may generate
damage to zirconia surface, including the presence of micro-cracks.12,13,14,15
Moreover, as an
universal adhesive, it simplifies the clinical procedures, reducing the number of steps
involved in an adhesive luting system.24
The superiority of the luting system using
Scotchbond Universal, despite the fact that Panavia F 2.0 (Table 1), Alloy Primer, and ED
Primer II (Table 1) also present 10-MDP and others phosphate monomers, methacrylates and
dimethacrylates in their compositions as adhesion promoters, was also observed
previously.25,42
On the other hand, several authors have observed that Panavia luting system
was superior to other luting agent/primer associations, such as AZ Primer/ResiCem (Shofu,
Kyoto, Japan),43
Metal/Zirconia Primer/Multilink (Ivoclar Vivadent),43
Monobond
S/Multilink (Ivoclar Vivadent),34
and Porcelain Liner M/SuperBond (SunMedical Co.,
Moriyama, Japan).34
Furthermore, Piwowarczyk et al. (2005) reported superior adhesion of
15
RelyX Unicem and Panavia F2.0 to zirconia after aging when compared to zinc phosphate and
modified glass-ionomer cements.44
The inferior results achieved by Panavia F in the present study might have been
affected by bonding procedures. During the bonding protocol, the Alloy Primer was applied
first on the zirconia surface, followed by ED Primer. The manufacturer recommends ED
Primer to be applied over the remaining tooth structure to keep contact with both tooth
structure and the Panavia luting agent, as well as, recommends Alloy Primer to be applied
over the zirconia to react with its surface and with the Panavia luting agent. Although no teeth
have been used in the present study, as aforementioned, ED Primer was applied after Alloy
Primer and may have interfered with the reaction between Alloy Primer and Panavia. A
previous study (Özcan et al. 2008)34
had also observed inferior or no adhesion to zirconia
after artificial aging when following the manufacturer’s instructions regarding Panavia F2.0.
During initial tests for the present study, it was tried to remove ED Primer II from the Alloy
Primer/Panavia F2.0 luting protocol, but no adhesion to zirconia was achieved.
The occurrence of cohesive failures by shear testing can be considered as a limitation
of this investigation, since it may lead to misinterpretation of bond performance of tested
materials.45,46,47
Instead of an indication of strong bonding, cohesive failures are explained by
the mechanics of the test and the brittleness of the materials involved.45
It may affect the
accurate assessment of the interfacial bond strength, precluding a correct evaluation of each
studied variable effect. Other limitation was the absence of thermocycling, since only water
storage at 37ºC temperature was performed, even though 150 and 300 days of distillated water
storage might be a useful method for aging cement-zirconia adhesion interfaces, producing
similar results to water storage associated to 12,000 thermocycling cicles.48
Although the use of ceramic primers seems to be part of a promising luting protocol
by enabling to reduce time-consuming and critical clinical steps, more studies are still
necessary to confirm the long-term efficiency of primers as bond promoters to zirconia.
CONCLUSION
The topographical alterations of the zirconia surface via alumina particle air-abrasion
provided enhanced resin bonding to the zirconia surface. Also, the luting systems that use
universal bonding agent (primers/adhesives) containing multiple bond promoters
(methacrylates monomers, phosphate monomers like 10-MDP, and silane), such as
16
Scotchbond Universal, are promising alternatives to alumina air-abrasion for the zirconia pre-
treatment.
REFERENCES
1. Reddy SM, Vijitha D, Deepak T, Balasubramanian R & Satish A (2014) Evaluation of
shear bond strength of zirconia bonded to dentin after various surface treatments of
zirconia Journal of Indian Prosthodontic Society 14(1) 38-41,
http://dx.doi.org/10.1007/s13191-012-0198-6
2. Shin YJ, Shin Y, Yi YA, Kim J, Lee IB, Cho BH, Son HH & Seo DG (2014)
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ACKNOWLEDGEMENTS
CAPES/MITACS and PIBIC/CNPq agencies financially supported the present study.
22
TABLES
Table 1 Information of resin cements and zirconia primers/bonding agents used in the present study
*Phosphate monomer 6-(4-Vinylbenzyl-N-propyl)amino-1,3,5-triazine-2,4-dithione.
Commercial Brand Lot Number Specifications
RelyX Unicem2
Translucenty, 3M ESPE 524950
Base paste: Methacrylate monomers containing phosphoric acid groups,
Initiator components, Silanated fillers, Stabilizers, Rheological additives.
Catalyst paste: Methacrylate monomers, Alkaline (basic) fillers, Silanated
fillers, Initiator components, Stabilizers, Rheological additives, Pigments.
Scotchbond Universal, 3M
ESPE 525058
MDP phosphate monomer, dimethacrylate resins, Vitrebond™ copolymer,
filler, ethanol, water, initiators and silane.
Duolink Universal, Bisco 1400003516 Base paste: Bis-GMA, Triethyleneglycol Dimethacrylate, Glass Filler.
Catalyst past: Bis-GMA, Triethyleneglycol Dimethacrylate, Glass Filler
Z-Prime Plus, Bisco 1400002857 Biphenyl dimethacrylate, MDP and Ethanol
Variolink II Transparent,
Ivoclar Vivadent
Base: T00900
Catalyst: T00901
Base: 26.3 %wt. monomer (Bis-GMA, urethane Dimethacrylate, and
triethylene glycol dimethacrylate), 73.4 %wt. filler.
Catalyst: 22.0%wt. monomer, 77.2%wt. filler
Monobond Plus, Ivoclar
Vivadent S55075
Alcohol solution of silane methacrylate, phosphoric acid methacrylate and
sulphide methacrylate.
Panavia F2.0 Light,
Kuraray 061229
Paste A: 10-Methacryloyloxydecyl dihydrogen phosphate, Hydrophobic
aromatic dimethacrylate, Hydrophobic aliphatic methacrylate, Hydrophilic
aliphatic dimethacrylate, Silanated silica filler, Silanated colloidal silica, dl-
Camphorquinone, Catalysts, Initiators, Others.
Paste B: Sodium fluoride, Hydrophobic aromatic dimethacrylate,
Hydrophobic aliphatic methacrylate, Hydrophilic aliphatic dimethacrylate,
Silanated barium glass filler, Catalysts, Accelerators, Pigments, Others.
Alloy Primer
ED Primer II. Kuraray
Alloy Primer:
0436AA
ED Primer II
Liquid A: 00322B
Liquid B: 00196A
Alloy Primer: Acetone, VBATDT* and 10-MDP.
ED Primer II Liquid A: 2-hydroxyethyl methacrylate, 10-
Methacryloyloxydecyl dihydrogen phosphate, N-Methacryloyl-5-
aminosalicylic acid, Water, Accelerators
ED Primer II Liquid B: N-Methacryloyl-5-aminosalicylic acid, Water,
Catalysts, Accelerators
23
Table 2 Testing groups according to the surface treatment and cementation strategy. The bonding procedures are
described as footnotes.
Cementation strategy
Surface treatment
Without With
Scotchbond Universal/RelyX Unicem 21 SU Al-SU
Z-Prime Plus/Duo-link Universal2 ZP Al-ZP
Monobond Plus/Variolink II3 MB Al-MB
Alloy Primer/ED Primer II/Panavia F 2.04 AP Al-AP
1Scotchbond Universal was applied on zirconia surface, with a microbrush, for 20 seconds and then air dried for 5 seconds. The specimen
was positioned on the Ultradent SBS device and RelyX Unicem cement was manipulated by equal parts of both pastes. 2Two layers of Z-Prime Plus were applied over the zirconia surface and air-dried for 5 seconds. Then the specimen was positioned on the
Ultradent SBS device and the Duo-link Universal cement was manipulated by equal parts of both pastes. 3Initially Monobond Plus was applied on the specimen free surface and let for 60 seconds, then it was air dried to remove possible primer
excess. The specimen was positioned on the Ultradent SBS device and the Variolink II cement was manipulated by equal parts of both
pastes during 10 seconds. 4Firstly Alloy Primer was applied with a microbrush and let dry by itself. Then ED Primer II (A & B) was applied, due its influence on resin
cement polymerization, let stay for 30 seconds and then gently air dried. Finally, the specimen was positioned on the Ultradent SBS device
and Panavia cement was manipulated by equal parts of both pastes mixed for 20 seconds.
24
Table 3 Means (and standard deviations, in MPa) and Tukey tests, as well as the percentages of adhesive (A)
and cohesive (B) failures in each group are presented.
Cementation strategy
BOND RESULTS* FAILURE TYPES
Alumina air-abrasion
Without With Without With
Scotchbond Universal/RelyX Unicem 2 19.595.58 Aa 23.185.17 Aa A: 60%, B: 40% A: 40%, B: 60%
Z-Prime Plus/Duo-link Universal 11.066.27 Bb 21.23 5.20 Aa A: 40%, B: 60% A: 30%, B: 70%
Monobond Plus/Variolink II 11.803.32 Bb 25.057.06 Aa A: 70%, B: 30% A: 40%, B: 60%
Alloy Primer/ED Primer II/Panavia F 2.0 4.671.31 Bc 9.152.02 Ab A: 100%, B: 0% A: 100%, B: 0%
*Line: different capital letters mean statistical difference between surface treatment groups, keeping unaltered the cementation strategy. *Column: different lowercase letters mean statistical difference among cementation strategy groups, keeping unaltered the surface treatment.
25
FIGURES
Figure 1 Representative micrographs of mainly adhesive fractures from debonded surfaces. It notes that the part of resin cement fractured (), due to typical biomechanical
behavior of the shear testing.
A B C
26
ANEXOS
Anexo A – Normas da “Operative Dentistry” para publicação de artigo no periódico2
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2 OPERATIVE DENTISTRY. Instructions to Authors. Indianápolis, 2014. Disponível em:
<https://www.jopdent.com/authors/authors.html>. Acesso em: 19 nov. 2015.
27
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28
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29
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