Ceramic raw materials from the State of Maranhão, Brazil. Part 1: chemical and mineralogical characterization and technological properties of clays from São Luis, Rosário, Pinheiro and Mirinzal

Nesse trabalho, foram caracterizadas algumas argilas coletadas nos municípios de São Luís, Rosário, Pinheiro e Mirinzal. A caracterização foi realizada através dos ensaios de difração de raios X, massa específica real, capacidade de troca de cátions (CTC), área superficial, distribuição granulométrica, análise química, análise térmica (TG-DTA) e limites de Atterberg. Ensaios tecnológicos de retração linear, antes e após a queima, absorção de água e tensão de ruptura a flexão, em três pontos, foram realizados em corpos de prova prensados uniaxialmente a 20 MPa e tratados termicamente em 850, 950, 1050, 1150 e 1250ºC. Os resultados obtidos permitiram identificar duas argilas de queima branca, constituídas de quartzo, caolim, feldspato e anatásio, com excelentes propriedades para uso em cerâmica branca. As restantes são queima vermelha e possuem composição mineralógica de quartzo, caolim, feldspato, montmorilonita, hematita e goetita. Estas últimas apresentaram valores moderados de plasticidade e são adequadas para aplicações em cerâmica vermelha.

Variation in body size of Phanocerus clavicornis Sharp, 1882 (Coleoptera: Elmidae: Larainae) in Atlantic Rainforest streams in response to hydraulic disturbance

Neste estudo, padrões de tamanho do corpo de Phanocerus clavicornis Sharp, 1882 (Coleoptera: Elmidae: Larainae) foram investigados ao longo de um gradiente de variação de velocidade da corrente em córregos de baixa ordem da Mata Atlântica. Especificamente, buscou-se testar a hipótese de que a distribuição de larvas de P. clavicornis com diferentes tamanhos corpóreos respondem às variações na velocidade da corrente em córregos. As coletas das larvas foram realizadas com um amostrador de Surber durante dois períodos amostrais, definidos pelo regime de chuvas: agosto - estação seca e fevereiro - estação chuvosa. Possíveis diferenças nas medidas de tamanho do corpo foram testadas através de uma análise de variância (ANOVA). Os resultados daANOVAindicaram para todas as medidas das larvas coletadas nos córregos de primeira ordem (largura da cabeça, largura do protórax e comprimento total do corpo) encontramos diferenças significativas, indicando uma variação morfométrica com as mudanças das condições hidráulicas, onde as larvas menores foram associadas aos períodos de maior precipitação. No entanto, em córregos maiores (3a ordem), os eventos de chuva tiveram menor impacto no tamanho dos indivíduos, com a ocorrência de larvas com diferentes tamanhos. Os resultados deste estudo sugerem que os espaços intersticiais são importantes para a proteção das larvas contra a velocidade da corrente e que as populações de P. clavicornis possuem alta plasticidade, sendo uma característica fundamental para a ocupação desta espécie em ambientes instáveis. Esses resultados são importantes para a compreensão da história de vida e características comportamentais da espécie, que permitem persistir em córregos ao longo de gradiente de perturbação do fluxo.

Effect of Post-silanization Heat Treatments of Silanized Feldspathic Ceramic on Adhesion to Resin Cement

Purpose: To evaluate the effect of post-silanization heat treatment of a silane agent and rinsing with hot water of silanized CAD/CAM feldspathic ceramic surfaces on the microtensile bond strength between resin cement and the ceramic, before and after mechanical cycling.Materials and Methods: Blocks measuring 10 x 5.7 x 3.25 mm(3) were produced from feldspathic ceramic cubes (VITA Mark II, VITA Zanhfabrik). Each ceramic block was duplicated in composite resin using a template made of polyvinylsiloxane impression material. Afterwards, ceramic and corresponding resin composite blocks were ultrasonically cleaned and randomly divided according to the 5 strategies used for conditioning the ceramic surface (n = 10): GHF: etching with hydrofluoric acid 10% + rinsing with water at room temperature + silanization at 20 degrees C; G20: silanization; G77: silanization + oven drying at 77 degrees C; G20r: silanization + hot water rinsing; G77r: silanization + oven drying at 77 C + hot water rinsing. The resin and ceramic blocks were cemented using a dual-curing resin cement. Every group was divided in two subgroups: aging condition (mechanical cycling, designated as a) or non-aging (designated as n). All the bonded assemblies were sectioned into microsticks for microtensile bond strength (mu TBS) testing. The failure mode of the tested specimens was assessed and mu TBS data were statistically analyzed in two ways: first 2-way ANOVA (GHF, G20 and G77 in non-aging/aging conditions) and 3-way ANOVA (temperature x rinsing x aging factors, excluding GHF), followed by Tukey's test (p = 0.05).Results: The 2-way ANOVA revealed that the mu TBS was significantly affected by the surface treatment (p < 0.001) but not by aging (p = 0.68), and Tukey's test showed that G77-n/G77-a (18.0 MPa) > GHF-n/GHF-a (12.2 MPa) > G20-n/G20-a (9.1 MPa). The 3-way ANOVA revealed that the mu TBS was significantly affected by the heat treatment and rinsing factors (p < 0.001), but not affected by aging (p = 0.36). The rinsing procedure decreased, while oven drying increased the bond strengths. Group G77, in both non-aging and aging conditions (18.6-17.4 MPa), had the highest bond values. Failure modes were mainly mixed for all groups.Conclusion: Oven drying at 77 degrees C improved the bond strength between the resin cement and feldspathic ceramic, but hot water rinsing reduced the bond strength and should not be recommended.

Effect of Resin Cement Type on the Microtensile Bond Strength to Lithium Disilicate Ceramic and Dentin Using Different Test Assemblies

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Effect of Surface Conditioning Modalities on the Repair Bond Strength of Resin Composite to the Zirconia Core / Veneering Ceramic Complex

Purpose: This study evaluated the effect of different surface conditioning protocols on the repair strength of resin composite to the zirconia core / veneering ceramic complex, simulating the clinical chipping phenomenon.Materials and Methods: Forty disk-shaped zirconia core (Lava Zirconia, 3M ESPE) (diameter: 3 mm) specimens were veneered circumferentially with a feldspathic veneering ceramic (VM7, Vita Zahnfabrik) (thickness: 2 mm) using a split metal mold. They were then embedded in autopolymerizing acrylic with the bonding surfaces exposed. Specimens were randomly assigned to one of the following surface conditioning protocols (n = 10 per group): group 1, veneer: 4% hydrofluoric acid (HF) (Porcelain Etch) + core: aluminum trioxide (50-mu m Al2O3) + core + veneer: silane (ESPE-Sil); group 2: core: Al2O3 (50 mu m) + veneer: HF + core + veneer: silane; group 3: veneer: HF + core: 30 mu m aluminum trioxide particles coated with silica (30 mu m SiO2) + core + veneer: silane; group 4: core: 30 mu m SiO2 + veneer: HF + core + veneer: silane. Core and veneer ceramic were conditioned individually but no attempt was made to avoid cross contamination of conditioning, simulating the clinical intraoral repair situation. Adhesive resin (VisioBond) was applied to both the core and the veneer ceramic, and resin composite (Quadrant Posterior) was bonded onto both substrates using polyethylene molds and photopolymerized. After thermocycling (6000 cycles, 5 degrees C-55 degrees C), the specimens were subjected to shear bond testing using a universal testing machine (1 mm/min). Failure modes were identified using an optical microscope, and scanning electron microscope images were obtained. Bond strength data (MPa) were analyzed statistically using the non-parametric Kruskal-Wallis test followed by the Wilcoxon rank-sum test and the Bonferroni Holm correction (alpha = 0.05).Results: Group 3 demonstrated significantly higher values (MPa) (8.6 +/- 2.7) than those of the other groups (3.2 +/- 3.1, 3.2 +/- 3, and 3.1 +/- 3.5 for groups 1, 2, and 4, respectively) (p < 0.001). All groups showed exclusively adhesive failure between the repair resin and the core zirconia. The incidence of cohesive failure in the ceramic was highest in group 3 (8 out of 10) compared to the other groups (0/10, 2/10, and 2/10, in groups 1, 2, and 4, respectively). SEM images showed that air abrasion on the zirconia core only also impinged on the veneering ceramic where the etching pattern was affected.Conclusion: Etching the veneer ceramic with HF gel and silica coating of the zirconia core followed by silanization of both substrates could be advised for the repair of the zirconia core / veneering ceramic complex.

Effect of the Etching Duration and Ultrasonic Cleaning on Microtensile Bond Strength Between Feldspathic Ceramic and Resin Cement

This study assessed the effect of different etching durations of feldspathic ceramic with hydrofluoric acid (HF) and ultrasonic cleaning of the etched ceramic surface on the microtensile bond strength stability of resin to a feldspathic ceramic. The research hypotheses investigated were: (1) different etching times would not affect the adhesion resistance and (2) ultrasonic cleaning would improve the adhesion. Ceramic blocks (6 x 6 x 5 mm) (N = 48) were obtained. The cementations surfaces were duplicated in resin composite. The six study groups (n = 8) were: G1Etching with 10% aqueous HF (30 s) + silane; G 210% HF (1 min) + silane; G3-10% HF (2 min) + silane; G4-10% HF (30 s) + ultrasonic cleaning (4 min) in distilled water + silane; G5-10% HF (1 min) + ultrasonic cleaning + silane; G6-10% HF (2 min) ultrasonic cleaning + silane. The cemented blocks were sectioned into microbars for the microtensile test. The etching duration did not create significant difference among the groups (p = .156) but significant influence of ultrasonic cleaning was observed (p = .001) (Two-way ANOVA and Tukey's test, p > 0.05). All the groups after ultrasonic cleaning presented higher bond strength (19.38-20.08 MPa) when compared with the groups without ultrasonic cleaning (16.2117.75 MPa). The bond strength between feldspathic ceramic and resin cement was not affected by different etching durations using HF. Ultrasonic cleaning increased the bond strength between ceramic surface and resin cement, regardless of the etching duration.

Effect of LLLT on autogenous bone grafts in the repair of critical size defects in the calvaria of immunosuppressed rats

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

EVALUATION OF ROUGHNESS, WETTABILITY, AND MORPHOLOGY OF AN YTTRIA-STABILIZED TETRAGONAL ZIRCONIA POLYCRYSTAL CERAMIC AFTER DIFFERENT AIRBORNE-PARTICLE ABRASION PROTOCOL

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Effect of Ceramic Thickness and Shade on Mechanical Properties of a Resin Luting Agent

Purpose: This study aimed to investigate the influence of ceramic thickness and shade on the Knoop hardness and dynamic elastic modulus of a dual-cured resin cement.Materials and Methods: Six ceramic shades (Bleaching, A1, A2, A3, A3.5, B3) and two ceramic thicknesses (1 mm, 3 mm) were evaluated. Disk specimens (diameter: 7 mm; thickness: 2 mm) of the resin cement were light cured under a ceramic block. Light-cured specimens without the ceramic block at distances of 1 and 3mm were also produced. The Knoop hardness number (KHN), density, and dynamic Young's moduli were determined. Statistical analysis was conducted using ANOVA and a Tukey B rank order test (p = 0.05).Results: The bleaching 1-mm-thick group exhibited significantly higher dynamic Young's modulus. Lower dynamic Young's moduli were observed for the 3-mm-thick ceramic groups compared to bleaching 3-mm-thick group, and no difference was found among the other 3-mm groups. For the KHN, when A3.5 3-mm-thick was used, the KHN was significantly lower than bleaching and A1 1-mm-thick ceramic; however, no difference was exhibited between the thicknesses of the same shade.Conclusions: The dual-cured resin cement studied irradiated through the 1-mm-thick ceramic with the lightest shade (bleaching ceramic) exhibited a better elastic modulus, and there was no effect in KHN of the resin cement when light cured under different ceramic shades and thicknesses (1 and 3 mm), except when the A3.5 3-mm-thick ceramic was used.Clinical Significance: Variolink II irradiated through ceramic with the lowest chroma exhibited the highest elastic modulus; therefore, the light activation method might not be the same for all clinical situations.

Effect of surface and heat treatments on the biaxial flexural strength and phase transformation of a Y-TZP ceramic

To evaluate the effect of grinding and airborne-particle abrasion on the biaxial flexural strength (BFS) and phase transformation of a Y-TZP ceramic, and examine whether sintering the veneering porcelain renders the previous heat treatment recommended by the manufacturer unnecessary. Materials and Methods: Lava zirconia specimens (N = 108) were obtained with the following dimensions: 14.0 mm diameter × 1.3 mm thickness (n = 36) and 14.0 mm × 1.6 mm (n = 72). The thicker specimens were ground with diamond burs under irrigation and received (heat-treated groups) or not (non-heat-treated groups) a heat treatment (1000°C for 30 min) prior to the four firing cycles applied to simulate the sintering of the veneering porcelain. All specimens were air abraded as follows (n = 12): 1) 30-μm silica-modified Al2O3 particles (Rocatec Soft); 2) 110-μm silica-modified Al2O3 particles (Rocatec Plus); and 3) 120-μm Al2O3 particles, followed by Rocatec Plus. Three specimens of each group were analyzed by x-ray diffraction (XRD) to assess the monoclinic phase content (%). The BFS test was performed in a mechanical testing machine (Instron 8874). Data (MPa) were analyzed by two-way ANOVA (grinding × airborne-particle abrasion and heat treatment × airborne-particle abrasion) and Tukey's post-hoc test (α = 0.05). The strength reliability was analyzed using the Weibull distribution. Results: Grinding significantly decreased the BFS of the non-heat-treated groups (p < 0.01). Within the ground groups, the previous heat treatment did not influence the BFS (p > 0.05). Air abrasion only influenced the BFS of the ground/heat-treated groups (p < 0.01). For the non-heat-treated groups, the grinding did not decrease the Weibull modulus (m), but it did decrease the characteristic strength (σ0). For Rocatec Soft and 120-μm Al2O3 particles + Rocatec Plus, the heat-treated groups presented lower m and higher σ0 than the ground/non-heat-treated groups. The independent variables did not seem to influence phase transformation. Air-abraded surfaces presented higher monoclinic zirconia content than the as-sintered and ground surfaces, which exhibited similar content. Conclusion: Even under irrigation, grinding compromised the Y-TZP ceramic strength. The sintering of the veneering porcelain rendered the previous heat treatment recommended by the manufacturer unnecessary. Airborneparticle abrasion influenced the strength of heat-treated zirconia.

Effect of surface and heat treatments on the biaxial flexural strength and phase transformation of a y-tzp ceramic

To evaluate the effect of grinding and airborne-particle abrasion on the biaxial flexural strength (BFS) and phase transformation of a Y-TZP ceramic, and examine whether sintering the veneering porcelain renders the previous heat treatment recommended by the manufacturer unnecessary. Materials and Methods: Lava zirconia specimens (N = 108) were obtained with the following dimensions: 14.0 mm diameter × 1.3 mm thickness (n = 36) and 14.0 mm × 1.6 mm (n = 72). The thicker specimens were ground with diamond burs under irrigation and received (heat-treated groups) or not (non-heat-treated groups) a heat treatment (1000°C for 30 min) prior to the four firing cycles applied to simulate the sintering of the veneering porcelain. All specimens were air abraded as follows (n = 12): 1) 30-μm silica-modified Al2O3 particles (Rocatec Soft); 2) 110-μm silica-modified Al2O3 particles (Rocatec Plus); and 3) 120-μm Al2O3 particles, followed by Rocatec Plus. Three specimens of each group were analyzed by x-ray diffraction (XRD) to assess the monoclinic phase content (%). The BFS test was performed in a mechanical testing machine (Instron 8874). Data (MPa) were analyzed by two-way ANOVA (grinding × airborne-particle abrasion and heat treatment × airborne-particle abrasion) and Tukey's post-hoc test (α = 0.05). The strength reliability was analyzed using the Weibull distribution. Results: Grinding significantly decreased the BFS of the non-heat-treated groups (p < 0.01). Within the ground groups, the previous heat treatment did not influence the BFS (p > 0.05). Air abrasion only influenced the BFS of the ground/heat-treated groups (p < 0.01). For the non-heat-treated groups, the grinding did not decrease the Weibull modulus (m), but it did decrease the characteristic strength (σ0). For Rocatec Soft and 120-μm Al2O3 particles + Rocatec Plus, the heat-treated groups presented lower m and higher σ0 than the ground/non-heat-treated groups. The independent variables did not seem to influence phase transformation. Air-abraded surfaces presented higher monoclinic zirconia content than the as-sintered and ground surfaces, which exhibited similar content. Conclusion: Even under irrigation, grinding compromised the Y-TZP ceramic strength. The sintering of the veneering porcelain rendered the previous heat treatment recommended by the manufacturer unnecessary. Airborneparticle abrasion influenced the strength of heat-treated zirconia.

Effect of ceramic etching protocols on resin bond strength to a feldspar ceramic

This study sought to evaluate the resin micro-tensile bond strength (MTBS) stability of a leucite-reinforced ceramic after different ceramic etching protocols. The microtensile test had 40 ceramic blocks (5x5x6 mm) assigned to five groups (n=8), in accordance with the following surface etching protocols: NE nonetched (control); 9HF: hydrofluoric (HF) acid etching (9% HF)+wash/dry; 4HF: 4%HF+wash/dry; 5HF: 5%HF+wash/dry; and 5HF+N: 5%HF+neutralizer+wash/dry+ultrasonic-cleaning. Etched ceramic surfaces were treated with a silane agent. Next, resin cement blocks were built on the prepared ceramic surface and stored for 24 hours in distilled water at 37 degrees C. The specimens were then sectioned to obtain microtensile beams (32/block), which were randomly assigned to the following conditions, nonaged (immediate test) and aged (water storage for 150 days plus 12,000 thermal cycles), before the microtensile test. Bond strength data were submitted to one-way analysis of variance and Tukey test (alpha=0.05). Additional ceramic samples were subjected to the different ceramic etching protocols and evaluated using a scanning electron microscope (n=2) and atomic force microscopy (n=2). Aging led to a statistically significant decrease in the MTBS for all groups, except the untreated one (NE). Among the groups submitted to the same aging conditions, the untreated (NE) revealed inferior MTBS values compared to the 9HF and 4HF groups. The 5HF and 5HF+N groups had intermediate mean values, being statistically similar to the higher values presented by the 9HF and 4HF groups and to the lower value associated with the NE group. The neutralization procedure did not enhance the ceramic/resin cement bond strength. HF acid etching is a crucial step in resin/ceramic bonding.

Effect of the particle size of maize, rice, and sorghum in extruded diets for dogs on starch gelatinization, digestibility, and the fecal concentration of fermentation products

The influence of rice, maize, and sorghum raw material particle size in extruded dry dog food on the digestibility of nutrients and energy and the fecal concentration of fermentation products was investigated. Three diets with similar nutrient compositions were formulated, each with 1 starch source. Before incorporation into diets, the cereals were ground into 3 different particle sizes (approximately 300, 450, and 600 mu m); therefore, a total of 9 diets were in a 3 x 3 factorial arrangement (3 cereals and 3 particle sizes). Fifty-four beagle dogs (12.0 +/- 0.1 kg BW) were randomly assigned to the diets, with 6 dogs per diet. The digestibility was measured with the chromium oxide method. The data were evaluated with ANOVA considering the carbohydrate source, grinding effect, and interactions. The means were compared with the Tukey test and polynomial contrasts (P < 0.05). With the same grinding procedure, rice was reduced to smaller particles than other cereals. The cereal mean geometric diameter (MGD) was directly related to starch gelatini-zation (SG) during extrusion. For rice diets, the MGD and SG did not change nutrient digestibility (P > 0.05); only GE digestibility was reduced at the largest MGD (P < 0.01). For maize and sorghum diets, the total tract apparent nutrient digestibility was reduced for foods with greater MGD and less SG (P < 0.01). A linear reduction in nutrient digestibility according to cereal particle size was observed for sorghum (r(2) < 0.72; P < 0.01). Higher concentrations of fecal total shortchain fatty acids (SCFA) were observed for sorghum diets (P < 0.05) than for other diets. The rice diets led to the production of feces with less lactate (P < 0.05). The increase in raw material MGD did not influence fecal SCFA for rice diets, but for the dogs fed maize and sorghum foods, an increase in propionate and butyrate concentrations were observed as MGD increased (P < 0.05). In conclusion, for dogs fed different particle sizes of the cereal starches in the extruded diets, the digestibility and fecal characteristics were affected, and this effect was ingredient dependent.

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

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)