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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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RESUMO

Abstract This study aimed to characterize and compare the effect of different aging regimens on surface characteristic (topography and roughness), structural stability (phase transformation) and mechanical performance (Weibull analysis) of a Y-TZP ceramic. Discs (15 × 1.2 mm; VITA In-Ceram YZ) were prepared according to ISO 6872-2015 for biaxial flexural strength testing and randomly assigned into five groups (n = 30): as-sintered, no aging treatment (CTRL); 20 h in autoclave at 134°C, 2 bar pressure (AUT); intermittent mechanical loading at 20 Hz/106 load pulses (MechLoad); AUT followed by MechLoad (AUT+MechLoad); and storage in distilled water at 37°C, for 1 year (STO). The following analyses were performed: roughness (n = 30), surface topography (n = 2), phase transformation (n = 2) and biaxial flexure strength (n = 30). Phase transformation (increase of m-phase content) was shown to be a spontaneous, unavoidable and time-dependent process, occurring even under ambient conditions (dry storage after 1 year = 6.0% increase), and is considerably accelerated in the presence of moisture (STO = 17.6%; AUT= 63.1%; and AUT+MechLoad = 59.9%). For roughness parameters, only Ra was affected by aging, and the highest values were observed for AUT+MechLoad (0.25 ± 0.07 µm). For Weibull analysis, structural reliability (Weibull moduli) and characteristic strength were not impaired after aging, and some aging conditions led to increased values (highest weibull moduli in AUT, and highest characteristic strength in STO). Phase transformation proves to be a time-dependent spontaneous mechanism that is accelerated in the presence of different stimuli. However, none of the aging regimens had a negative effect on the characteristic strength and structural reliability of Y-TZP ceramic.

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This study evaluated the effects of low-temperature aging on the surface topography, phase transformation, biaxial flexural strength, and structural reliability of a ground Y-TZP ceramic. Disc-shaped specimens were manufactured and divided according to two factors: "grinding" - without grinding (as-sintered, Ctrl), grinding with an extra-fine diamond bur (25 µm Xfine) and coarse diamond bur (181 µm Coarse); and "low-temperature-aging" (absence or presence). Grinding was performed using a contra-angle handpiece under water-cooling. Aging was performed in an autoclave at 134 °C, under 2 bar, over a period of 20 h. Surface topography analysis showed an increase in roughness based on grit-size (Coarse>Xfine>Ctrl), and aging promoted different effects on roughness (Ctrl AgCoarse). Grinding and aging promoted an increase in the amount of m-phase, although different susceptibilities to degradation were observed. Weibull analysis showed an increase in characteristic strength after grinding (Coarse=Xfine>Ctrl); however, distinct effects were observed for aging (CtrlCoarse Ag). Weibull moduli were statistically similar. Grinding promoted an increase in characteristic strength as a result of an increase in m-phase content; when the Y-TZP surface was ground by coarse diamond burs followed by aging, characteristic strength was reduced, meaning the low-temperature degradation appeared to intensify for rougher Y-TZP surfaces.

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The purpose of this study was to evaluate the influence of zirconia surface treatments on low-temperature degradation (LTD). Disc-shaped specimens were subjected to one of four surface treatments, denoted as C (control-no surface treatment), Si (air abrasion with 30 µm silica-modified alumina particles), Al (air abrasion with 30 µm alumina particles), and Gr (grinding with 120 grit diamond discs). Half of the samples were submitted to autoclave treatment for 12 h (127°C, 1.5 bar). Samples were characterized by x-ray diffraction and profilometer analysis and were subjected to biaxial flexural strength test. All of the groups exhibited an increase in the amount of monoclinic phase (m-phase) after LTD. The t→m transformation was remarkable for the specimens from the C group, which also exhibited a significant increase in strength. The Gr group also exhibited an increase in strength but lower initial roughness, which probably suppressed LTD on the zirconia surface. The specimens subjected to air abrasion exhibited higher initial amounts of m-phase and a small increase in m-phase after LTD; the strength was not affected in these groups. The effects of LTD were different with each surface treatment applied. Apparently, LTD may be suppressed by smoother surfaces or the presence of an initial amount of m-phase on zirconia surface.

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