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This study evaluated the influence of silica coating, primer type and its heat treatment on bond strength durability between resin cement and an yttrium-stabilized polycrystalline tetragonal zirconia (Y-TZP). Eighty (80) Y-TZP blocks were allocated into 16 groups considering four factors: silica coating (without and with); type of primer (RelyX Ceramic Primer, a silane-based primer; Single Bond Universal, a universal MDP-based primer); heat treatment of the primer (without and with); aging (without and with). After zirconia treatments, resin cement cylinders (RelyX ARC) (n = 20; N = 320) were built. Half of the samples were tested after 24 h, and another half were subjected to aging (thermocycling 5-55°C/5.000, and storage in water for 6 months). Shear bond strength test and failure analysis were performed. Bond strength data were submitted to four-way ANOVA and Tukey test (p = 0.05). All factors were statistically significant (p < 0.001) for bond strength (MPa): silica coating (7.3 ± 5.9) > no-treatment (3.6 ± 4.3); universal primer (6.7 ± 4.8) > silane (4.2 ± 5.8); heat-treatment (6.5 ± 6.3) > no-heating (4.4 ± 4.3); no-aging (8.2 ± 5) > aging (2.7 ± 4.4). Tukey test revealed that the association of silica coating + universal primer + heat-treatment promoted higher and stable resin bond strength. Silica coating, universal adhesive application and heat treatment improve/increase durability and bond strength of zirconia. © 2018 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 107B: 104-111, 2019.

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Abstract This study aimed to investigate the effect of grinding and multi-stimuli aging on the fatigue strength, surface topography and the phase transformation of Y-TZP ceramic. Discs were manufactured according to ISO-6872:2008 for biaxial flexure testing (diameter: 15 mm; thickness: 1.2 mm) and randomly assigned considering two factors "grinding" and "aging": C- control (as-sintered); CA- control + aging; G- ground; GA- ground + aging. Grinding was carried out with coarse diamond burs under water-cooling. Aging protocols consisted of: autoclave (134°C, 2 bars pressure, 20 hours), followed by storage for 365 days (samples were kept untouched at room temperature), and by mechanical cycling (106 cycles by 20 Hz under a load of 50% from the biaxial flexure monotonic tests). Flexural fatigue strengths (20,000 cycles; 6 Hz) were determined under sinusoidal cyclic loading using staircase approach. Additionally, surface topography analysis by FE-SEM and phase transformation analysis by X-ray Diffractometry were performed. Dixon and Mood methodology was used to analyze the fatigue strength data. Grinding promotes alterations of topographical pattern, while aging apparently did not alter it. Grinding triggered t-m phase transformation without impacting the fatigue strength of the Y-TZP ceramic; and aging promoted an intense t-m transformation that resulted in a toughening mechanism leading to higher fatigue strength for as-sintered condition, and a tendency of increase for ground condition (C < CA; G = GA). It concludes that grinding and aging procedures did not affect deleteriously the fatigue strength of the evaluated Y-TZP ceramic, although, it promotes surface topography alterations, except to aging, and t-m phase transformation.

Resumo Este estudo objetivou investigar o efeito do desgaste e envelhecimento (estímulos combinados) na resistência à fadiga, topografia superficial e transformação de fase de uma cerâmica Y-TZP. Discos para teste de flexão biaxial foram confeccionados segundo as normas da ISO-6872:2008 (15 mm Ø; 1,2 mm espessura) e randomicamente distribuídos de acordo com os fatores "desgaste" e "envelhecimento": C- controle (sinterizado); CA- controle envelhecido; G- desgaste; GA- desgaste envelhecido. O desgaste foi feito com pontas diamantadas de granulação grossa sob irrigação com água. Os protocolos de envelhecimento consistiram em: autoclave (134°C, 2 bar de pressão, 20 horas), 365 dias armazenados em temperatura ambiente, e ciclagem mecânica (106 ciclos a 20 Hz em um intervalo de carga de até 50% da carga monotônica observada em testes estáticos). A resistência à fadiga foi determinada para 20.000 ciclos à 6 Hz sob carregamento sinusoidal através do método de escada. Adicionalmente, análises de topografia superficial em microscopia eletrônica de varredura e de transformação de fase por difração de raios-X foram executadas. A metodologia de Dixon e Mood foi usada para analisar os dados de resistência à fadiga. Foi observado que o desgaste promove uma alteração de padrão topográfico superficial; enquanto o envelhecimento aparentemente não demonstra influência. Em relação à transformação de fase e resistência à fadiga, o desgaste desencadeou um aumento de fase m sem impactar na resistência à fadiga da cerâmica Y-TZP; já o envelhecimento promoveu uma intensa transformação de fase, resultando no mecanismo de tenacificação, que gerou um aumento na resistência à fadiga para a condição sinterizada e uma tendência a aumento na condição desgaste (C < CA; G = GA). Os dados elucidam que o desgaste e o envelhecimento não impactaram negativamente na resistência à fadiga da cerâmica Y-TZP, apesar de promoverem alterações de topografia superficial e intensa transformação de fase de t-m respectivamente.

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OBJECTIVE: This study introduces an innovative method to enhance adhesion of methacrylate-based cements to yttria-stabilized zirconia (Y-TZP) by means of a silica-nanoparticle deposition process. METHODS: Two alkoxide organic precursors, tetraethyl-orthosilicate (TEOS) and zirconium tert-butoxide (ZTB) were diluted in hexane at different concentrations in order to obtain several experimental materials to enhance deposition of a SiO(x) reactive layer to Y-TZP. This deposition was attained via sintering alkoxide precursors directly on pre-sintered zirconia (infiltration method­INF) or application on the surface of fully sintered zirconia (coating method­COA). Untreated specimens and a commercial tribochemical silica coating were also tested as controls and all the treated Y-TZP specimens were analyzed using SEM-EDX. Specimens were bonded using silane, adhesive and dual-cure luting cement and submitted to shear bond strength test after different water storage periods (24 h, 3-, 6- and 12-months). RESULTS: SEM-EDX revealed Y-TZP surface covered by silica nanoclusters. The morphology of silica-covered Y-TZP surfaces was influenced by sintering method, employed to deposit nanoclusters. High bond strength (MPa) was observed when using COA method; highest TEOS percentage achieved the greatest bond strengths to Y-TZP surface (36.7±6.3 at 24 h). However, bonds stability was dependent on ZTB presence (32.9±9.7 at 3 months; 32.3±7.1 at 6 months). Regarding INF method, the highest and more stable resin-zirconia bond strength was attained when using experimental solutions containing TEOS and no ZTB. Both sintering methods tested in this study were able to achieve a bonding performance similar to that of classic tribochemical strategies. SIGNIFICANCE: This study demonstrates that it is possible to achieve a reliable and long-lasting bonding between yttria-stabilized zirconia ceramic and methacrylate-based cements when using this novel, simple, and cost-effective bonding approach.

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