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. (rafinha_grasel@hotmail.com).

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. (jacinta.santos@schulich.uwo.ca).

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. (heleine_rego@hotmail.com).

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.

(mariliarippe@mail.ufsm.br).

*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. (lfvalandro@hotmail.com)

*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: lfvalandro@hotmail.com (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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17

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dentistry 41(1) 31-41, http://dx.doi.org/10.1016/j.jdent.2012.09.013

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zirconia ceramics on the bond strength to resin cement The journal of adhesive

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roughness of zirconia-based ceramics and shear bond strength of veneering porcelain

Dental Materials Journal 33(6) 778-785

24. Amaral M, Belli R, Cesar PF, Valandro LF, Petschelt A & Lohbauer U (2014) The

potential of novel primers and universal adhesives to bond to zirconia Journal of

dentistry 42(1) 90-98, http://dx.doi.org/10.1016/j.jdent.2013.11.004

25. Blatz MB, Chiche G, Holst S & Sadan A (2007) Influence of surface treatment and

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27. Foxton RM, Cavalcanti AN, Nakajima M, Pilecki P, Sherriff M, Melo L & Watson TF

(2011) Durability of resin cement bond to aluminium oxide and zirconia ceramics

after air abrasion and laser treatment Journal of Prosthodontics 20(2) 84-92,

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28. Román-Rodríguez JL, Fons-Font A, Amigó-Borrás V, Granell-Ruiz M, Busquets-

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(2014) Influence of surface treatment of yttrium-stabilized tetragonal zirconium oxides

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33. Oyaqüe RC, Monticelli F, Toledano M, Osorio E, Ferrari M & Osorio R (2009) Effect

of water aging on microtensile bond strength of dual-cured resin cements to pre-

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34. Özcan M, Kerkdijk S & Valandro LF (2008) Comparison of resin cement adhesion to

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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

Manuscript submission

General Requirements

Operative Dentistry requires electronic submission of all manuscripts. All submissions must

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• The manuscript body MUST NOT include any:

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information, such as a signature at the end, etc.

o Figures

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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o Manuscripts that have major revisions requested (i.e. For English correction) are

entered as a resubmission of the original article.

28

• Spelling must conform to the American Heritage Dictionary of the English Language, and

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CORRESPONDING AUTHOR must provide a WORKING / VALID e-mail address which

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• full name of product

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29

MANUSCRIPTS must be provided as Word for Windows files. Files with the .doc and .docx

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30

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