Effect of ZrO2 paste, surface treatments, and storage on Weibull characteristics and resin bond strength to zirconia.

The objective is to evaluate the effect of different surface treatments and storage on the shear strength of ultratranslucent zirconia. 36 blocks of ultra-translucent zirconia were fabricated (7x7x2mm) and sintered. Then, divided into 12 groups according to the "surface treatment" (C -Primer; Al -Sandblasting with Al2O3 + Primer; Si -Silicate + Primer; Gl -Glaze + HF + Primer; Z -Zirlink; Zp -Zirlink + Primer) and "storage" factors (ST-with 150 days/37º and without). After surface treatment, five cylinders (Ø=2mm; h=2.0mm) of resin cement (n=15) were constructed in each ceramic block; at the end, the shear strength test was performed (1mm/min, 50Kgf), and analysis of surface failures. 60 additional samples (2x2x2mm) were made for extras analysis (surface roughness, MEV, and EDS). Bond strength and surface roughness data were statistically evaluated by ANOVA (2 factors/1 factor), Tukey test (5%), and Weibull analysis, respectively. ANOVA (2-way) revealed that all factors were statistically significant for bond strength. The silicatization groups (SiST: 30.47AMPa; Si: 29.21AMPa) showed the highest bond strength values, regardless of storage (Tukey's test). While the groups treated with Zirlink (ZST: 2.76FMPa; Z: 5.27EFMPa) showed the lowest values, just similar to the GlST group (5.14EFMPa). The Weibull modulus (m) showed a statistical difference between groups (p=0.000). ANOVA (1 factor) revealed that the "surface treatment" factor (p=0.0000) was statistically significant for surface roughness. Therefore, the application of Zirlink and Glaze on pre-sintered zirconia did not promote efficient adhesion of the ultratranslucent zirconia to the resin cement, even when associated with a primer containing MDP.

Effect of ZrO2 paste, surface treatments, and storage on Weibull characteristics and resin bond strength to zirconia

Abstract The objective is to evaluate the effect of different surface treatments and storage on the shear strength of ultratranslucent zirconia. 36 blocks of ultra-translucent zirconia were fabricated (7x7x2mm) and sintered. Then, divided into 12 groups according to the "surface treatment" (C -Primer; Al -Sandblasting with Al2O3 + Primer; Si -Silicate + Primer; Gl -Glaze + HF + Primer; Z -Zirlink; Zp -Zirlink + Primer) and "storage" factors (ST-with 150 days/37º and without). After surface treatment, five cylinders (Ø=2mm; h=2.0mm) of resin cement (n=15) were constructed in each ceramic block; at the end, the shear strength test was performed (1mm/min, 50Kgf), and analysis of surface failures. 60 additional samples (2x2x2mm) were made for extras analysis (surface roughness, MEV, and EDS). Bond strength and surface roughness data were statistically evaluated by ANOVA (2 factors/1 factor), Tukey test (5%), and Weibull analysis, respectively. ANOVA (2-way) revealed that all factors were statistically significant for bond strength. The silicatization groups (SiST: 30.47AMPa; Si: 29.21AMPa) showed the highest bond strength values, regardless of storage (Tukey's test). While the groups treated with Zirlink (ZST: 2.76FMPa; Z: 5.27EFMPa) showed the lowest values, just similar to the GlST group (5.14EFMPa). The Weibull modulus (m) showed a statistical difference between groups (p=0.000). ANOVA (1 factor) revealed that the "surface treatment" factor (p=0.0000) was statistically significant for surface roughness. Therefore, the application of Zirlink and Glaze on pre-sintered zirconia did not promote efficient adhesion of the ultratranslucent zirconia to the resin cement, even when associated with a primer containing MDP.

Resumo O objetivo é avaliar o efeito de diferentes tratamentos superficiais e do envelhecimento na resistência ao cisalhamento da zircônia ultratranslúcida. Foram confeccionados 36 blocos de zircônia ultratranslúcida (7x7x2mm) e sinterizados. Em seguida, divididos em 12 grupos de acordo com o "tratamento de superfície" (C-Primer; Al-Jateamento com Al2O3+Primer; Si-Silicato+Primer; Gl -Glaze+HF+Primer; Z-Zirlink; Zp-Zirlink+Primer) e fatores de "armazenamento" (ST-com, 150 dias/37º e sem). Após o tratamento superficial, foram construídos cinco cilindros (Ø=2mm; h=2,0mm) de cimento resinoso (n=15) em cada bloco cerâmico; ao final foi realizado o ensaio de resistência ao cisalhamento (1mm/min, 50Kgf) e análise de falhas superficiais. Foram confeccionadas 60 amostras adicionais (2x2x2mm) para análises extras (rugosidade superficial, MEV e EDS). Os dados de resistência de união e rugosidade superficial foram avaliados estatisticamente por ANOVA (2 fatores/1fator), teste de Tukey (5%) e análise de Weibull, respectivamente. ANOVA (2 fatores) revelou que todos os fatores foram estatisticamente significativos para a resistência de união. Os grupos de silicatização (SiST: 30,47AMPa; Si: 29,21AMPa) apresentaram os maiores valores de resistência de união, independente do armazenamento (Tukey). Enquanto os grupos tratados com Zirlink (ZST: 2,76FMPa; Z: 5,27EFMPa) apresentaram os valores mais baixos, apenas semelhantes ao grupo GlST (5,14EFMPa). O módulo de Weibull (m) apresentou diferença estatística entre os grupos (p=0,000). A ANOVA (1 fator) revelou que o fator "tratamento superficial" (p=0,0000) foi estatisticamente significativo para rugosidade superficial. Portanto, a aplicação de Zirlink e do Glaze na zircônia pré-sinterizada não promoveu adesão eficiente da zircônia ultratranslúcida ao cimento resinoso, mesmo quando associada a primer contendo MDP.

Novel organically linked ZnII hydrogenselenite coordination polymers: synthesis, characterization, and efficient TiO2 photosensitization for enhanced photocatalytic hydrogen production.

This study focused on the solvothermal synthesis, characterization, and photocatalytic activities of two novel coordination polymers, namely [Zn(µ-HSeO3)2(bipy)]n (1) and [Zn(µ-HSeO3)2(phen)]n (2). These compounds represent the first organically linked ZnII hydrogenselenite coordination polymers. The synthesis of compounds 1 and 2 involved the addition of 2,2'-bipyridine and 1,10-phenanthroline, respectively, to SeO2 and ZnO in methanol as the solvent. The novel hydrogenselenite compounds were thoroughly characterized using spectroscopic and crystallographic methods. The photocatalytic solids (TiO2-1A and TiO2-2A) were prepared by immobilizing compounds 1-2 onto TiO2 through the sol-gel approach. These photocatalysts were then evaluated for hydrogen evolution via water splitting using a 300 W Hg/Xe lamp as the irradiation source. Among the newly synthesized photocatalytic materials, TiO2-1A demonstrated auspicious photocatalytic performance for hydrogen gas production. Its catalytic activity overcame the observed for the pure solid support TiO2 and Degussa P25 (commercial titania), making compound 1 a particularly attractive TiO2 photosensitizer. Additionally, TiO2-1A exhibited superior photocatalytic activity compared to TiO2-2A. The latter performed better than freshly prepared TiO2, approaching that of Degussa P25. These findings highlight the potential of compound 1 as an effective photosensitizer for TiO2-based photocatalysis, making it a promising candidate for applications in clean energy generation, specifically in hydrogen production by water splitting.

Effect of calcium hypochlorite and sodium thiosulfate on the bond strength to pulp chamber dentin: A laboratory investigation.

This study aimed to compare the effect of sodium hypochlorite (NaOCl) and calcium hypochlorite [Ca(OCl)2 ] on the bond strength to pulp chamber dentin when followed or not by the use of sodium thiosulfate (Na2 S2 O3 ). The pulp chamber of fifty human molars were divided into five groups (n = 10) according to the immersion protocol: 2.5% NaOCl; 2.5% NaOCl + 5% Na2 S2 O3 ; 2.5% Ca(OCl)2 ; 2.5% Ca(OCl)2 + 5% Na2 S2 O3 ; and 0.9% sodium chloride (NaCl; control). Subsequently, the samples were restored with resin composite. Three sticks each were obtained and subjected to microtensile testing. SEM/EDS analyses of the pulp chamber roof (n = 8) were carried out for mineral quantification. Elemental analysis data were investigated via one-way ANOVA and Tukey's post hoc, and bond strength data by post hoc pairwise comparisons using the Kruskal-Wallis test. Use of 2.5% NaOCl was associated with the lowest value of bond strength, while 2.5% Ca(OCl)2 had similar bond strength to that of the 0.9% NaCl control. Using 5% Na2 S2 O3 was able to increase the bond strength after 2.5% NaOCl, but not after 2.5% Ca(OCl)2 . The group treated only with 2.5% Ca(OCl)2 had a higher Ca/P ratio on the dentin surface. Dentin treated with Ca(OCl)2 was not affected by Na2 S2 O3 and showed bond strength similar to the 0.9% NaCl.

Development of microparticles and microparticulated tablets containing piperine

Abstract Piper nigrum (black pepper) is used in Indian traditional medicine and its main alkaloid, Piperine (PIP), presents antioxidant, antitumor and neuroprotective pharmacological properties. This substance is insoluble in aqueous media and can irritate the gastrointestinal tract. Aiming to avoid these inconvenient characteristics and enable PIP oral administration, this study suggested the PIP microencapsulation through the emulsion-solvent evaporation method and the preparation of microparticulated tablets by direct compression. An UV-spectroscopy method was validated to quantify PIP. Microparticles and microparticulated tablets were successfully obtained and the microparticles exhibited excellent flow. The scanning electron microscopy images showed that PIP microparticles were intact after compression. The in vitro release showed a controlled release of PIP from microparticles and PIP microparticles from tablets in comparison to PIP and PIP tablets. The release profiles of PIP microparticles and the microparticulated tablets were similar. Therefore, tablets containing PIP microparticles are promising multiparticulated dosage forms because a tablet allows microparticles administration and the intact ones promote a controlled release, decreasing its irritating potential on the mucosa.

Effect of pigmentation techniques on the fatigue mechanical behavior of a translucent zirconia for monolithic restorations.

This study aims to characterize the effect of pre- and/or post-sintering pigmentation techniques on the fatigue behavior of a 4YSZ ceramic (4 mol% yttrium stabilized zirconia). First, 4YSZ ceramic discs (IPS e.max ZirCAD, 15 mm diameter, and 1.2 mm thickness) were obtained and allocated according to the 'pigmentation technique' factor into 5 groups: Ctrl - unshaded ceramic disc (IPS e.max ZirCAD BL); Manuf - ceramic discs shaded by the manufacturer at block formation (IPS e.max ZirCAD MT A2); Brush - unshaded ceramic disc pigmented in the pre-sintered stage using a brush; Stain - unshaded ceramic disc pigmented in the post-sintering stage using a stain glaze (shade A2); Brush + Stain - combination of Brush and Stain techniques. The specimens were sintered and analyzed by a spectrophotometer (VITA Easyshade) for color differences (ΔE00 calculated according to CIEDE, 2000) to ensure that they present the same perceived color (ΔE00 ≤ 1.77, acceptability threshold). The specimens (n = 15) were submitted to biaxial flexural fatigue testing using a cyclic fatigue method (frequency of 20 Hz; 10,000 cycles per step; initial stress of 200 MPa; and step-size of 25 MPa) until specimen fracture. Fatigue strength (FS) and number of cycles until failure (CFF) were recorded with statistical purposes. Fractographic, complementary topography, elemental and roughness analyses were performed. The Ctrl shown the highest FS, CFF, and survival rates compared to the other conditions (p < 0.05), being only statistically similar to Brush. Stain showed the lowest FS, CFF and survival rates (p < 0.05). The Manuf and Brush + Stain shown intermediary performance. In regards of Weibull moduli, Brush shown the lowest values (lowest structural reliability), for both FS and CFF, being only statistically similar to Manuf. Topography analysis shown a uniform size of zirconia crystals in Ctrl, Manuf and Brush. In addition, a smooth glassy surface with some spots of impregnated pigment was observed in the groups where glaze was applied (Stain and Brush + Stain). This finding was corroborated by elemental analysis. Despite that, Stain and Brush + Stain presented the roughest surface (p < 0.05). In summary, the pigmentation techniques used to provide a Vita classical A2 color shade have a detrimental effect on the mechanical fatigue properties of a 4YSZ ceramic, except for the technique performed with the brush in the block pre-sintering stage. Despite this, the brush technique presents great variability in mechanical performance, resulting in lower structural reliability.

Pre-sintering pigmentation techniques do not affect the fatigue behavior of adhesively luted 4YSZ restorations.

This study aims to characterize the effect of shading techniques on the fatigue behavior of a 4YSZ ceramic (4 mol% yttrium stabilized zirconia) adhesively bonded to a dentin analogue (fiber-reinforced epoxy resin). 4YSZ ceramic discs (IPS e.max ZirCAD, Ø = 10 mm and 1 mm of thickness) were allocated according to the factor 'shading technique' into 4 groups: Brush- unshaded ceramic disc (IPS e.max ZirCAD BL) pigmented at the pre-sintered stage with pigment solution applied manually using a round liner brush; Immersion- unshaded ceramic disc pigmented through immersion in the solution for 1 s on only one side of the ceramic disc; Manufacturer- specimens already shaded by the manufacturer (IPS e.max ZirCAD MT A2 - Manufacturer group); Control- a control condition with absence of pigment (i.e. non-pigmented specimens). The specimens were sintered and a spectrophotometer (SP60, EX- Rite) was used to ensure that the same perceived color (i.e. pigment saturation) was achieved in the different shading strategies (Manufacturer, Brush or Immersion groups). To do so, the color differences (ΔE00) were calculated using the CIEDE 2000 equation; and an ΔE00 of up to 1.77 was considered as an acceptability threshold. Dentin analogue discs were obtained (Ø = 10 mm and 2.5 mm of thickness) and randomly allocated into pairs with the 4YSZ ceramic discs. Next, the pairs were adhesively bonded using a resin cement (Multilink N). The bonded assemblies (n = 15) were tested for fatigue using the step-stress test method (frequency of 20 Hz; 10,000 cycles per step, initial load 200 N; step-size of 100 N, up to 700 N; and after, step-size of 50 N, until specimen failure/fracture or radial cracks). Fatigue failure load (FFL) and number of cycles for failure (CFF) were recorded for statistical analysis. Fractographic features were accessed, and complementary roughness, topography, grain size and phase content analyses were performed. No statistical differences were observed in the fatigue behavior among the non-shaded condition (Control group - 880 N) and the shaded specimens (Manufacturer - 887 N, Brush - 820 N, and Immersion - 850 N groups; p > 0.05). However, the use of a brush shading technique induced slightly inferior fatigue mechanical behavior of the restorative set compared to the specimens already shaded by the manufacturer (p = 0.027). No differences in Weibull modulus were observed among the tested groups. The specimens pigmented by the brush technique demonstrated a rougher surface, with statistically higher Rz values, in addition to a larger grain size in comparison to all other conditions (p< 0.05). No m-phase content was identified (only t and c phases were detected). Thus, the shading techniques used to provide a Vita classic A2 shade does not negatively affect the mechanical fatigue properties of a bonded 4YSZ ceramic. However, the brush technique has detrimental effect on the fatigue behavior compared to when the ceramic was already provided in a shaded format by its manufacturer.