Novel protein stabilization in white wine: A study on thermally treated zirconia-alumina composites.

A major concern for wineries is haze formation in white wines due to protein instability. Despite its prevalent use, the conventional bentonite method has shortcomings, including potential alteration of color and aroma, slow processing times, and notable wine wastage. Zirconium oxide (ZrO2) effectively removes proteins without affecting wine characteristics. However, producing cost-effective ZrO2 materials with efficient protein removal capabilities poses a significant challenge. This research aims to assess the viability of designing a porous material impregnated with zirconia to remove turbidity-causing proteins effectively. For this purpose, the support material alone (Al2O3) and the zirconia-impregnated support (ZrO2/Al2O3) were subjected to different calcination temperatures. It was observed that high-temperature treatments (750 °C) enhanced wine stability and protein adsorption capacity. The optimal adsorbent achieved a notable reduction in turbidity, decreasing the ΔNTU from 42 to 18, alongside a significant 44 % reduction in the total protein content, particularly affecting proteins in the molecular weight range of 10 to 70 kDa. This result is attributed to modifying the textural properties of ZrO2/Al2O3, characterized by the reduction of acidic sites, augmented pore diameters from 4.81 to 7.74 nm, and the emergence of zirconia clusters across the surface of the porous support. In summary, this study presents the first application of zirconia on the alumina support surface for protein stabilization in white wine. Combining ZrO2/Al2O3 and a high-temperature treatment emerges as a promising, cost-efficient, and environmentally sustainable strategy for protein removal in white wine.

The optical behavior of pressable lithia-based glass-ceramics under two different heat treatment protocols / O comportamento óptico de vitrocerâmicas prensadas à base de lítio sob dois protocolos diferentes de tratamento térmico

Objective: This study aimed to evaluate the optical behavior of pressable lithia-silicate and lithia-zirconia-silicate glass ceramics toward additional heat treatment protocols. Material and Methods: 40 lithia-silicate discs (15mm x 1mm) were heat pressed following the manufacturers' instructions. Discs were divided into four groups (n=10) according to type as follows: two groups of lithia-silicate-glass ceramics; Gp(E) (IPS e.max Press; Ivoclar Vivadent AG), Gp(L) (GC Initial LiSi Press, GC), two lithia-zirconia-silicate pressable glass ceramics; Gp(C) (Celtra Press, Dentsply Sirona) and Gp(A) (VITA Ambria, VITA Zahnfabrik). Each group was subdivided into (n=5): Subgroup(T1): the thermal tempering temperature was set 9% below the pressing temperature, Subgroup(T2): the temperature was set 5% below the pressing temperature. Optical properties: color, translucency parameter (TP), and contrast ratio (CR) were evaluated by spectrophotometer (Aglient Cary 5000 UV-Vis­NIR) after pressing and after thermal tempering. Results: Thermal tempering regardless of temperature resulted in a color shift within the acceptability level as ΔE for Gp(E) (3.18±2) followed by ΔE for Gp(L) (2.47±0.19) by ΔE for Gp(C) (2.26±0.14) and the last ΔE for Gp(A) (1.62±0.13). Subgroup(T2) showed a significantly higher color shift with mean ΔE(2.55±0.63) compared to Subgroup(T1) ΔE(2.35±0.59). There was a statistically significant increase in TP after tempering for all tested groups parallelled with a decrease in CR values. Conclusion: Heat tempering of the tested lithia-silicate pressable ceramics had a significant effect on the optical outcome of these materials, being lithia-zirconia-silicate ceramics more stable and less affected optically than other lithia-silicate-glass ceramics.(AU)

Objetivo: Avaliar o comportamento óptico de cerâmicas pressionáveis de vidro de litia-silicato e litia-zircônia-silicato sob protocolos adicionais de tratamento térmico. Materiais e métodos: 40 discos de litia-silicato (15mm x 1mm) foram prensados a quente conforme instruções dos fabricantes. Material e Métodos: 40 discos de litia-silicato (15mm x 1mm) foram prensados e divididos em quatro grupos (n=10): dois de lithia-silicato-vidro, Gp(E) (IPS e.max Imprensa) e Gp(L) (GC inicial LiSi Press), e dois de vidro prensado de litia-zircônia-silicato, Gp(C) (Celtra Press) e Gp(A) (VITA Ambria). Cada grupo foi subdividido em (n=5): Subgrupo(T1): amostras temperadas a 9% abaixo da temperatura de prensagem, e Subgrupo(T2): a temperatura foi ajustada 5% abaixo da temperatura de prensagem. As propriedades ópticas, incluindo cor, translucidez (TP) e contraste (CR), foram avaliadas com um espectrofotômetro (Aglient Cary 5000 UV-Vis-NIR) após prensagem e temperagem térmica. Resultados: O tratamento térmico resultou em mudança de cor dentro do nível aceitável, com ΔE mais alto para Gp(E) (3,18±2), seguido por Gp(L) (2,47±0,19), Gp(C) (2,26±0,14), e Gp(A) (1,62±0,13). No subgrupo (T2), houve uma mudança de cor mais significativa, com ΔE médio de (2,55±0,63), comparado ao subgrupo (T1) com ΔE médio de (2,35±0,59). Houve aumento significativo na TP e redução nos valores de RC após o tratamento térmico em todos os grupos testados. Conclusão: O tratamento térmico das cerâmicas prensadas de litia-silicato teve um efeito significativo na sua qualidade ótica, com as cerâmicas de litia-zircônia-silicato mostrando-se mais estáveis e menos afetadas visualmente em comparação com outras cerâmicas de litia-silicato-vidro(AU)

Effect of laser irradiation on bond strength between zirconia and resin cement or veneer ceramic: A systematic review and meta-analysis.

Aim: This systematic review with meta-analysis aimed to evaluate the effect of the laser treatment on bond strength between Y-TZP and the resin cement or with the veneering ceramic, and the effect on the alteration of the Y-TZP surface roughness. Settings and Design: Systematic review and meta analysis following PROSPERO guidelines. Materials and Methods: A comprehensive review was performed up to September 2020 on four databases (PubMed/MEDLINE, Embase, Scopus, and Cochrane Library), using the combination of keywords: "laser AND zirconia AND surface treatment AND bond strength". Statistical Analysis Used: The meta-analysis was based on the Mantel-Haenszel and inverse variance methods. The continuous outcome was evaluated by mean difference and the corresponding 95% confidence intervals. Results: A total of 37 studies were identified for the inclusion of data, with only in vitro studies. The types of laser reported in the studies were: Er:YAG, Nd:YAG, Er,Cr:YSGG, CO2, Femtosecond, and Yb lasers. A random-effect model found statistically significant differences between lasers and control groups of Y-TZP (P < 0.00001; MD: 3.08; 95% CI: 2.58 to 3.58). Only the bond strength with the Er:YAG laser did not present statistical difference (P = 0.51; MD: 0.22; 95% CI: -0.44-0.88). In another analysis, a random-effect model found a statistically significant difference between the laser and control groups on surface roughness (P < 0.00001; MD: 0.96; 95% CI: 0.86 to 1.06). Conclusions: Laser irradiation is capable to improve the Y-TZP surface roughness and the bond strength of zirconia with resin cement and veneering ceramics. However, there is a lack of laser protocol for the zirconia surface, a fact that makes a simple and direct comparison difficult.

An evaluation of the effect of different veneer materials on fracture resistance of zirconia core / Avaliação dos diferentes efeitos de materiais de revestimento na resistência à fratura do núcleo de zircônia

Objectives: this in vitro study was done to evaluate the effect of packable P60 composite and Tetric N-Ceram composite veneer material on fracture strength of zirconia cores. Material and Methods:Twenty four zirconium cores (Vita, Germany) with 0.7 mm thickness were fabricated by CAD/CAM technology and then subjected to air abrasion with 50 µm of Al2O3. Cores were randomly divided into three groups according to veneering material (group A: control group sandblasted with 50 µm Al2O3 veneered by IPS E-max Ceram porcelain, group C: sandblasted with 50 µm Al2O3, etching with hydrofluoric acid and veneered with P60 composite, group E: sandblasted with 50 µm Al2O3, etching with hydrofluoric acid and veneered with Tetric N-Ceram composite). All crowns were subjected to fracture strength test in the testing machine, with load application by steel ball indenter and 0.5 mm/min. cross head speed. Results: statistical analysis was carried out utilizing one-way ANOVA, LSD. The results of fracture strength value test showed the highest mean value was registered for group (A), and the lowest mean for group (E). One-way ANOVA test represented that, there was a statistically high significant different among all groups. LSD results showed a high significant difference increase in fracture resistance for Group A at p value (*p < 0.001 High significant). Conclusions: Within the limitation of this study, sandblasting zirconia core with 50 µm Al2O3 and veneering with conventional ceramic produced restoration with acceptable fracture resistance value (AU)

Objetivo: o objetivo desse estudo in vitro foi avaliar o efeito dos compósitos P60 compactáveis e material laminado de compósitos Tetric-N Ceram na resistência à fratura de núcleos de zircônia. Material e métodos:Vinte e quatro núcleos de zircônia (Vita, Germany) com 0.7 mm de espessura fabricados por tecnologia de CAD/CAM e sinterizados em alta temperatura (1450ºC por 60 min) de acordo com as instruções do fabricante. Núcleos totalmente de zircônias foram submetidos a abração com 50 µm de Al2O3. Os núcleos de zircônia foram divididos de forma randomiza em três grupos de acordo com o material de revestimento (grupo A: grupo controle jateado com 50 µm Al2O3 folheado com porcelana IPS E-max Ceram, grupo C: jateado com 50 µm Al2O3 , coberto com concentração 9,5% de ácido fluorídrico e folheado com resina composta compatível, grupo E: jateado com 50 µm Al2O3 coberto com concentração 9,5% de ácido fluorídrico e folheado com porcelana IPS E-max Ceram. Todos os espécimes (coroas) foram submetidos a teste de resistência a fratura com máquina de teste universal, essa máquina utilizou para aplicação de carga bola de aço com 6mm de diâmetro 0,5 mm/min de velocidade da cruzeta. Resultados: análise estatística foi realizada utilizando One-way ANOVA, LSD. O resultado da resistência a fratura mostra que o maior valor médio foi registrado no grupo A e a menor média para o grupo E. O resultado do teste One-Way ANOVA representaram que houve uma diferença estatisticamente alta e significante entre todos os grupos. LSD foi executada para mostrar a fonte de significância. Os resultados do LSD mostraram um aumento da diferença significativa alta na resistência à fratura para o grupo A no valor de p (p < 0.001 signicancia alta). Conclusão: Dentro das limitações desse estudo o uso convencional de jateamento com 50 µm Al2O3 e estratificação com cerâmica convencional produziu restauração com valor aceitável de resistência a fratura (AU)

Influence of addition of zirconia on PMMA: A systematic review.

The objective of this systematic review is to evaluate the effect of the incorporation of zirconia (ZrO2) particles on the mechanical properties of PMMA (polymethyl methacrylate), and to establish which characteristics of this material yield the best results aiming their biomedical applicability. This study was carried out in accordance with the Items of Preferred Reports for Systematic Reviews and Meta-Analyzes (PRISMA) and is registered in PROSPERO under registration number: CRD42018095801. The searches were carried out in the PubMed, MEDLINE, Scopus and Cochrane Library databases for articles published up until April 2018. After the different stages of the article selection process, eight articles were selected for qualitative and quantitative analysis. All were in vitro studies, totaling 536 evaluated samples. The concentrations of zirconia ranged from 0.5% to 20% and the particle sizes were between 15 nm and 10 µm. The incorporation of zirconia particles did not increase the flexural strength of PMMA in only one study. While the concentration of zirconia influences PMMA, the type of acrylic resin, size, and silanization of zirconia particles did not influence the results. Thus, the addition of zirconia particles showed a positive effect on PMMA enhancing their use in the medical and dental field, especially when certain anatomical areas requires higher strength of the materials, providing longevity for the rehabilitation.

Gingival fibroblasts behavior on bioactive zirconia and titanium dental implant surfaces produced by a functionally graded technique

Abstract Adding a biological apatite layer to the implant surface enhances bone healing around the implant. Objective This study aimed to characterize the mechanical properties and test human gingival fibroblasts behavior in contact with Zirconia and Titanium bioactive-modified implant materials. Methodology 6 groups were considered: Titanium (Ti6Al4V), Ti6Al4V with 5% HA and 5% ßTCP, Zirconia (YTZP), YTZP with 5% HA and 5% ßTCP. For each group, we produced discs using a novel fabrication method for functionally graded materials, under adequate conditions for etching and grit-blasting to achieve equivalent surface microroughness among the samples. Surface roughness (Ra, Rz), water contact angle, shear bond strength, and Vickers hardness were performed. Human gingival fibroblasts immortalized by hTERT gene from the fourth passage, were seeded on discs for 14 days. Cell viability and proliferation were assessed using a resazurin-based method, and cellular adhesion and morphology using field emission gun scanning electron microscopy (FEG-SEM). After 3 days of culture, images of fluorescent nucleic acid stain were collected by confocal laser scanning microscopy (CLSM). Results Results were presented as mean ± standard deviation (SD). We compared groups using one-way ANOVA with Tukey's post-hoc test, and significance level was set at p<0.05. After 14 days of culture, cell viability and proliferation were significantly higher in YTZP group than in other groups (p<0.05). Samples of YTZP-ßTCP presented significantly higher wettability (p<0.05); yet, we observed no improvement in cell behavior on this group. Fibroblast spreading and surface density were more evident on YTZP specimens. Adding calcium-phosphate bioactive did not alter the tested mechanical properties; however, Ti6Al4V material shear bond strength was statistically higher than other groups (p<0.05). Conclusion Adding bioactive materials did not improve soft-tissue cell behavior. When compared to other zirconia and titanium groups, pure zirconia surface improved adhesion, viability and proliferation of fibroblasts. Cell behavior seems to depend on surface chemical composition rather than on surface roughness.

Effect of Trigonella foenum Extract and ZiO2 Nanoparticles on Some Pathogenic Fungi and Bacteria

Aim: The current venture, were made to evaluate the inhibitory effect of Trigonella foenum seed Extract and ZiO2 Nanoparticles on some selected species of Fungi and Bacteria. Materials and Methods: two bacterial species included Pseudomonas aeruginosa and Staphylococcus aureus and three fungal species which is Cryptococcus neoformans, Candidda albicans and Chaetomium were used to evaluate the antibacterial activity of Trigonella foenum Extract and ZiO2 Nanoparticles. Results: This study showed that the Zirconium Oxide (ZiO2) nanoparticles have antifungal and antibacterial activities on the isolates of Cryptococcus neoformans, Candida alicans and Staphylococcus aureus, respectively. While the antimicrobial activity of Zirconium Oxide nanoparticles on the Chaetomium and Pseudomonas aeruginosa was negative. All tested fungi and bacterial isolates were found to be sensitive to Trigonella foenum seed extract, the results of the compination of the ZiO2 Nanoparticle and the Trigonella foenum seed extract were poisitive for all tested fungi isolates and bacterial isolates. The XRD analysis was done for Zirconium Oxide nanoparticles and the result showed that the biocrystallization on the surface of the Zirconium Oxide manoparticles. The average partides size was about (29.8) nm. Conclusions: This investigation conclude that the use of Trigonella foenum seed Extract has the effect of killing all bacteria and fungi under study, result indicate the Trigonella foenun seed Extract best antibacterial efficacy than the ZiO2 together (AU)

Adapted Pechini method to prepare DSA type electrodes of RuO2-ZrO2 doped with Sb2O5 over titanium plates.

This paper describes a thermal method to obtain metal oxides on a titanium substrate surface. This adapted Pechini method is a versatile, easy to handle and scalable technique to obtain electrodes for industrial uses, such as Dimensionally Stable Anodes (DSA). This method has advantages over other thermal methods like dip coating or sputtering, as it needs a smaller amount of polymeric mixture than dip coating method to cover the same area and is less expensive than sputtering method. The thermal method described herein to prepare DSA type electrodes of RuO2-ZrO2 doped with Sb2O5 over titanium plates needs no sophisticated equipment as spray pyrolysis technique does; a muffle, ultrasonic equipment, and a hot plate magnetic stirrer are the principal apparatus necessary to carry out the adapted Pechini method. On the other hand, this method allows metal oxides to disperse homogeneously. The cyclic voltammograms showed the stability of DSA, and the accelerated life test allowed establishing its useful life (18.18 years) at a current density of 10 mA cm-2.

Characterisation of a new plasma-enhanced film to improve shear bond strength between zirconia and veneering ceramic.

The aim of this study was to develop and characterise a new plasma-enhanced chemical vapor deposition (PECVD) film for improving shear bond strength (SBS) between yttria-stabilised tetragonal zirconia (Y-TZP) and veneering ceramic. In total, 192 Y-TZP samples (13 × 5.4 × 5 mm) were divided into 6 groups: control - no treatment (C), airborne-particle abrasion with 27 µm aluminum oxide particles (Al27), 110 µm aluminum oxide particles (Al110), and 250 µm aluminum oxide particles (Al250), application of liner for zirconia (L) and the PECVD film application (P). The Y-TZP surface was characterised by means of Scanning Electronic Microscopy (SEM), Energy-dispersive Spectroscopy (EDS), atomic force microscopy (AFM), surface profilometry and surface-free energy (SFE). SBS between Y-TZP and veneering ceramic was tested before and after thermocycling (20,000 cycles of 5 and 55 °C), and failure mode was also evaluated. Data were analysed by ANOVA and Tukey's HSD test (α = 0.05). Data analysis showed that PECVD film had no effect on surface roughness of Y-TZP (p > 0.05 vs control), whilst the other groups presented higher roughness values (p < 0.05). All treatments increased SFE, except the Al27 group. The highest SBS was presented by the P group (p < 0.05), and values were similar to those of the Al27 group (p = 0.107). Mixed failures were prevalent in all groups, and premature failures were found only in Al groups after thermocycling. Whilst PECVD treatment did not affect Y-TZP surface roughness, high SBS between Y-TZP and the veneering layer was observed. Therefore, PECVD treatment is a promising alternative to improve the performance of bi-layer zirconia-based restorations.

Polishing of ground y-tzp ceramic is mandatory for improving the mechanical behavior

Abstract It evaluated the effect of aging by Low Temperature Degradation (LTD), executed after post- processing surface treatments (polishing, heat treatment and glazing), on the surface characteristics (micromorphology and roughness) and on the structural stability (phase transformation and mechanical behavior-flexural strength and structural reliability) of a ground yttrium-stabilized tetragonal zirconia polycrystal (Y-TZP) ceramic. Discs of Y-TZP (VITA In-Ceram YZ) were manufactured (ISO:6872-2015; 15 mm in diameter and 1.2 ± 0.2 mm in thickness) and randomly assigned into 10 groups according two factors: "aging" in 2 levels (with or without) and "surface treatment" in 5 levels (Ctrl: as-sintered; Gr: grinding with coarse diamond bur; Gr + HT: grinding plus heat treatment; Gr + Pol: grinding plus polishing; Gr + Gl: grinding plus glazing). Roughness (n=30), biaxial flexural test (n=30), phase transformation (n=2), and surface topography (n=2) analyses were performed. Aging led to an intense increase in monoclinic (m) phase content for all the tested conditions, being the as-sintered samples (Ctrl= 65.6%) more susceptible to the t-m phase transformation. Despite of increasing the m-phase content, aging was not detrimental for characteristic strength (except to the grinding condition). There was no significant reduction in the Weibull modulus after surface treatments. Additionally, heat treatment and glazing after grinding led to a decrease in characteristic strength, while polishing presented the highest characteristic strength values. Thus, polishing is mandatory after grinding the Y-TZP ceramic, while performing glazing or heat-treatment alone after grinding lead to the worst mechanical performance.

Resumo Este estudo avaliou o efeito do envelhecimento através da degradação a baixas temperaturas (low temperaturare degradation - LTD) após a realização de tratamentos de superfície pós- sinterização (polimento, tratamento térmico e glaze) nas características superficiais (micromorfologia e rugosidade), e na estabilidade estrutural (transformação de fase e comportamento mecânico - resistência flexural e confiabilidade estrutural) de uma cerâmica de zircônia tetragonal policristalina estabilizada por ítria (Y-TZP) desgastada. Discos de cerâmica Y-TZP (VITA In-Ceram YZ) foram confeccionados (ISO:6872-2015; 15mm de diâmetro e 1,2 ± 0,2mm de espessura) e randomicamente divididos em 10 grupos de acordo com dois fatores: "envelhecimento" (com e sem) e "tratamento de superfície" (Ctrl - sem tratamento; Gr - desgaste com ponta diamantada grossa; Gr + HT - desgaste mais tratamento térmico; Gr + Pol - desgaste mais polimento; Gr + Gl - desgaste mais glazeamento). Foram realizadas as análises de rugosidade (n=30), flexão biaxial (n=30), transformação de fase (n=2) e topografia de superfície (n=2). O envelhecimento levou a um aumento intenso no conteúdo de fase monoclínica (m) em todas as condições testadas, sendo observada uma maior susceptibilidade de transformação de fase t-m nas amostras do grupo controle (Ctrl= 65.6%). Apesar de provocar elevada transformação de fase, o envelhecimento não apresentou efeitos negativos nos desfechos avaliados. Não houve redução significativa do módulo de Weibull após os tratamentos. Além disso, o tratamento térmico e o glaze após desgaste levaram a uma redução da resistência característica, enquanto que o grupo polimento apresentou o mais alto valor de resistência característica. O glaze e o tratamento térmico geraram o pior desempenho mecânico, portanto a realização do polimento após desgaste de uma cerâmica Y-TZP é obrigatória.

Chemical and Microscopy Characterization of Trans-Endodontic Implants / Caracterización química y microscópica de implantes trans-endodónticos

Abstract Trans-endodontic implants are an artificial extension through root apex anchored in periradicular bone tissue. The aim is to improve the crown-root ratio and to provide stability to dental organ present. Zirconium oxide (ZrO2) is a material of great technological importance, having good natural color, high strength, high toughness, high chemical stability, does not suffer any corrosion, chemical and microbial resistance and excellent esthetic properties. Objective: The aim of this study was to evaluate chemical and microscopy of surface conditions of ZrO2 trans-endodontic implant. Materials and Methods: A blocks of ZrO2 were manufactured for produce trans-endodontic implants and divided in two groups: monoclinic and tetragonal phase. They were evaluated using Scanning Electroning Microscope (SEM), EnergyDispersive X-ray Spectroscopy (EDS), and Atomic Force Microscope (AFM) and Vickers Micro hardness. Results: The Monoclinic phase through AFM analysis showed roughness Ra = 0.320μm, whereas in the Tetragonal phase was 0.126μm, SEM/EDX indicated that the phases are not properly uniform and the addition of the Yttrium to favor the stabilization of the Tetragonal phase. The Vickers hardness analysis showed a value of 1500HV. Conclusion: The characterization of the surface of trans-endodontic zirconium oxide implants provides a guideline to know the surface characteristics of the material, since a greater roughness on the surface of the implant will favor the Osseo-integration capacity.

Resumen Los implantes trans-endodónticos son una extensión artificial a través del ápice radicular anclado en el tejido óseo periradicular. El objetivo es mejorar la relación corona-raíz y proporcionar estabilidad al órgano dental presente. El óxido de zirconio (ZrO2) es un material de gran importancia tecnológica, con buen color natural, alta resistencia, alta tenacidad, alta estabilidad química, no sufre corrosión, resistencia química y microbiana y excelentes propiedades estéticas. Objetivo: El objetivo de este estudio fue evaluar las condiciones superficiales de ZrO2 para su aplicación clínica a los implantes transendodónticos. Materiales y Métodos: se trituraron bloques de ZrO2 en implantes trans-endodónticos y se dividieron en: monoclínico y tetragonal. Luego se evaluaron mediante microscopía electrónica de barrido (SEM), espectroscopia de rayos X de energía dispersiva (EDS) y microscopio de fuerza atómica (AFM) y microdureza vickers. Resultados: La fase monoclínica a través del análisis AFM presenta Ra = 0.320 μm, mientras que en la fase Tetragonal es 0.126 μm, SEM / EDS muestra que las fases no son adecuadamente uniformes y la adición del Ytrio para favorecer la estabilización de la fase tetragonal. El análisis de microdureza mostro un valor de 1500HV. Conclusión: La caracterización de la superficie de los implantes trans-endodónticos de óxido de zirconio, brinda una pauta para conocer las características superficiales del material, ya que al haber una mayor rugosidad en la superficie del implante se verá favorecida la capacidad de oseointegración.

Micropatterned Silica Films with Nanohydroxyapatite for Y-TZP Implants.

This investigation aimed at developing micropatterned silica thin films (MSTFs) containing nanohydroxyapatite (nano-HA) microaggregates that were not completely covered by silica so that they could directly interact with the surrounding cells. The objectives were 1) to evaluate the effect of the presence of 2 films (MSTF with or without nano-HA addition) on the characteristic strength (σ0) and Weibull modulus ( m) of a yttria-stabilized tetragonal zirconia polycrystal (Y-TZP) and 2) to evaluate the effect of these 2 films, as applied onto the Y-TZP surface, on the morphology, orientation, and proliferation of MG63 cells. Sol-gel process and soft lithography were used to apply the MSTF onto the Y-TZP specimens. Three experimental groups were produced: Y-TZP, Y-TZP + MSTF, and Y-TZP + MSTF + sprayed nano-HA. All surfaces were characterized by scanning electron microscopy and energy-dispersive X-ray spectroscopy and tested for 4-point flexural strength ( n = 30) in water at 37 °C. Weibull analysis was used to determine m and σ0 (maximum likelihood method). In vitro biological behavior was performed with human osteoblast-like cells (MG63). Y-TZP was successfully coated with MSFT and MSFT + nano-HA. Scanning electron microscopy micrographs indicated that the microaggregates of nano-HA were not entirely covered by the silica. There was no statistically significant difference among the experimental groups for σ0 and m. In the groups containing the films, the cells were elongated and aligned along the lines. The MSFT + nano-HA group showed significantly higher cell metabolic activity than that obtained for the Y-TZP group at day 7. This investigation was successful in producing an MSTF containing nano-HA microaggregates that remained exposed to the environment. The developed films did not jeopardize the structural reliability of a commercial Y-TZP, as confirmed by the Weibull statistics. The MG63 cells seeded over the films became elongated and aligned along the films' micropatterned lines. Y-TZP specimens coated with MSTF and nano-HA showed a higher cell metabolic activity and proliferation after 7 d of culture when compared with uncoated Y-TZP.

Tissue Response and Immunoexpression of Interleukin 6 Promoted by Tricalcium Silicate-based Repair Materials after Subcutaneous Implantation in Rats.

INTRODUCTION: The aim of the present study was to evaluate the inflammatory response induced by experimental tricalcium silicate cement with 20% zirconium oxide (TSC) and MTA Plus (MTAP; Avalon Biomed Inc, Bradenton, FL) in rat subcutaneous tissues. METHODS: Polyethylene tubes were filled with TSC (n = 20) and MTAP (n = 20) and implanted in the dorsal subcutaneous tissues of 32 rats. Empty tubes were used as the control (control group [CG], n = 20). After 7, 15, 30, and 60 days, the tubes with connective tissue were removed, and the inflammatory cells and immunolabeled cells for interleukin 6 (IL-6) were counted. Data were statistically analyzed using analysis of variance and the Tukey test (P ≤ .05). RESULTS: An increased number of inflammatory and immunolabeled cells for IL-6 were observed at 7 days. The number of inflammatory cells was higher for TSC and MTAP than the CG (P < .001) at 7 days; after 30 and 60 days, no significant differences were observed among the TSC, MTAP, and CG (P = .955). The number of immunolabeled cells for IL-6 was similar for TSC, MTAP, and CG at all evaluated periods. A gradual and significant decrease was observed in the number of inflammatory cells and IL-6-immunopositive cells. At 60 days, the capsules adjacent to TSC and MTAP exhibited fibroblasts and bundles of collagen fibers. CONCLUSIONS: TSC and MTAP caused a similar subcutaneous reaction in rats, suggesting that they are biocompatible and present similar immune responses.

Fatigue limit of monolithic Y-TZP three-unit-fixed dental prostheses: Effect of grinding at the gingival zone of the connector.

OBJECTIVES: To determine the fatigue limits of three-unit monolithic zirconia fixed dental prosthesis (FDPs) before and after grinding of the gingival areas of connectors with diamond burs. MATERIAL AND METHODS: FDPs were milled from pre-sintered blocks of zirconia simulating the absence of the first mandibular molar. Half of the specimens were subjected to grinding, simulating clinical adjustment, and all of them were subjected to glazing procedure. Additional specimens were manufactured for roughness analysis. FDPs were adhesively cemented onto glass-fiber reinforced epoxy resin abutments. Fatigue limits and standard deviations were obtained using a staircase fatigue method (n=20, 100,000 loading cycles/5Hz). The initial test load was 70% of the mean load-to-fracture (n=3) and load increments were 5% of the initial test load for both the control and ground specimens. Data were compared by Student's T-test (α≤0.05). RESULTS: Both the control and ground groups exhibited similar values of load-to-fracture and fatigue limits. Neither the surface treatments nor ageing affected the surface roughness of the specimens. CONCLUSIONS: The damage induced by grinding with fine-grit diamond bur in the gingival area of the connectors did not decrease the fatigue limit of the three-unit monolithic zirconia FDP.

Mechanical behavior of yttria-stabilized tetragonal zirconia polycrystal: Effects of different aging regimens

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.

Fracture Strength of Implant-Supported Ceramic Crowns with Customized Zirconia Abutments: Screw Retained vs. Cement Retained.

PURPOSE: To compare the fracture resistance before and after cyclic fatigue assays of ceramic crowns with customized zirconia abutments when screw retained and cemented onto implants. MATERIALS AND METHODS: The sample of this study consisted of 40 ceramic crowns with zirconia infrastructure fixed onto external hexagonal implants. The crowns were distributed into two groups (n = 20): Screw-retained and cemented crowns. Half the crowns of each group (n = 10) underwent compression until fracture and the other half (n = 10) underwent cyclic fatigue and subsequent compression until fracture. The cyclic fatigue test was carried out using an electromechanical fatigue device (loads from 0 to 100 N, 2 Hz frequency, in distilled water, at 37 °C for a period of 1 million cycles). The compression test was carried out using a universal testing machine with a 0.5 mm/min speed and 5 KN load cell. After fracture, the crowns were classified according to the type of fracture. Student's t test (p < 0.05) was used for statistical analysis. RESULTS: The cyclic fatigue altered neither the mean fracture resistance of the screw-retained crowns (before = 1068.31 N, after = 891.49 N; p > 0.05) nor that of the cemented crowns (before = 2117.78 N; after = 2094.81 N; p > 0.05); however, the mean fracture resistance of the cemented crowns was higher than that of the screw-retained crowns both before (p < 0.001) and after (p < 0.001) the cyclic fatigue. Fractures occurred most frequently in the ceramic veneer, followed by fracture of some of the copings. CONCLUSION: The ceramic crowns cemented onto the customized zirconia abutments offered greater fracture resistance than ceramic crowns with customized zirconia abutments screw retained onto implants. The cyclic fatigue did not seem to influence the fracture resistance of these crowns, whether cemented or screw retained onto implants. Fracture of the veneering ceramic was the predominant failure in this study.

Marginal and internal fit of zirconia copings obtained using different digital scanning methods

Abstract The objective of this study was to evaluate the marginal and internal fit of zirconia copings obtained with different digital scanning methods. A human mandibular first molar was set in a typodont with its adjacent and antagonist teeth and prepared for an all-ceramic crown. Digital impressions were made using an intraoral scanner (3Shape). Polyvinyl siloxane impressions and Type IV gypsum models were also obtained and scanned with a benchtop laboratory scanner (3Shape D700). Ten zirconia copings were fabricated for each group using CAD-CAM technology. The marginal and internal fit of the zirconia copings was assessed by the silicone replica technique. Four sections of each replica were obtained, and each section was evaluated at four points: marginal gap (MG), axial wall (AW), axio-occlusal edge (AO) and centro-occlusal wall (CO), using an image analyzing software. The data were submitted to one-way ANOVA and Tukey's test (α = 0.05). They showed statistically significant differences for MG, AO and CO. Regarding MG, intraoral scanning showed lower gap values, whereas gypsum model scanning showed higher gap values. Regarding AO and CO, intraoral digital scanning showed lower gap values. Polyvinyl siloxane impression scanning and gypsum model scanning showed higher gap values and were statistically similar. It can be concluded that intraoral digital scanning provided a lower mean gap value, in comparison with conventional impressions and gypsum casts scanned with a standard benchtop laboratory scanner.

Experimental Calcium Silicate-Based Cement with and without Zirconium Oxide Modulates Fibroblasts Viability

The aim of this study was to verify whether the use of zirconium oxide as a radiopacifier of an experimental calcium silicate-based cement (WPCZO) leads to cytotoxicity. Fibroblasts were treated with different concentrations (10 mg/mL, 1 mg/mL, and 0.1 mg/mL) of the cements diluted in Dulbecco's modified Eagle's medium (DMEM) for periods of 12, 24, and 48 h. Groups tested were white Portland cement (WPC), white Portland cement with zirconium oxide (WPCZO), and white mineral trioxide aggregate Angelus (MTA). Control group cells were not treated. The cytotoxicity was evaluated through mitochondrial-activity (MTT) and cell-density (crystal violet) assays. All cements showed low cytotoxicity. In general, at the concentration of 10 mg/mL there was an increase in viability of those groups treated with WPC and WPCZO when compared to the control group (p<0.05). A similar profile for the absorbance values was noted among the groups: 10 mg/mL presented an increase in viability compared to the control group. On the other hand, smaller concentrations presented a similar or lower viability compared to the control group, in general. A new dental material composed of calcium silicate-based cement with 20% zirconium oxide as the radiopacifier showed low cytotoxicity as a promising material to be exploited for root-end filling.

Resumo O objetivo deste estudo foi verificar se o uso do óxido de zircônia como radiopacificador de um cimento experimental à base de silicato de cálcio (WPCZO) levou a citotoxicidade. Os fibroblastos foram tratados com diferentes concentrações (10 mg/mL, 1 mg/mL e 0,1 mg/mL) dos cimento diluídos em meio Eagle modificado por Dulbecco (DMEM) durante períodos de 12, 24, e 48 horas. Os grupos testados foram: cimento Portland (WPC), cimento Portland branco com óxido de zircônio (WPCZO) e MTA Angelus branco (MTA). No grupo controle as células não foram tratadas. A citotoxicidade foi avaliada por meio da mitocondrial-atividade (MTT) e ensaio de densidade celular (cristal violeta). Todos os cimentos apresentaram baixa citotoxicidade. Em geral, na concentração de 10 mg/mL, houve um aumento na viabilidade desses grupos tratados com WPC e WPCZO quando comparado com o grupo controle (p <0,05). Um perfil semelhante para os valores de absorvância foi observado entre os grupos: 10 mg/mL apresentaram um aumento da viabilidade em relação ao grupo controle. Por outro lado, as concentrações menores apresentaram uma viabilidade semelhante ou inferior em comparação com o grupo controle, em geral. Um novo material odontológico composto de cimento à base de silicato de cálcio com 20% de óxido de zircônio, como o radiopacificador, apresentou baixa citotoxicidade e pode ser explorado como um material promissor para retrobturações.

Bacterial adhesion on amorphous and crystalline metal oxide coatings.

Several studies have demonstrated the influence of surface properties (surface energy, composition and topography) of biocompatible materials on the adhesion of cells/bacteria on solid substrates; however, few have provided information about the effect of the atomic arrangement or crystallinity. Using magnetron sputtering deposition, we produced amorphous and crystalline TiO2 and ZrO2 coatings with controlled micro and nanoscale morphology. The effect of the structure on the physical-chemical surface properties was carefully analyzed. Then, we studied how these parameters affect the adhesion of Escherichia coli and Staphylococcus aureus. Our findings demonstrated that the nano-topography and the surface energy were significantly influenced by the coating structure. Bacterial adhesion at micro-rough (2.6 µm) surfaces was independent of the surface composition and structure, contrary to the observation in sub-micron (0.5 µm) rough surfaces, where the crystalline oxides (TiO2>ZrO2) surfaces exhibited higher numbers of attached bacteria. Particularly, crystalline TiO2, which presented a predominant acidic nature, was more attractive for the adhesion of the negatively charged bacteria. The information provided by this study, where surface modifications are introduced by means of the deposition of amorphous or crystalline oxide coatings, offers a route for the rational design of implant surfaces to control or inhibit bacterial adhesion.

Effect of low-temperature aging on the mechanical behavior of ground Y-TZP.

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.