Preparation of refractory calcium aluminate cement using the sonochemical process

Calcium aluminate cements (CAC) were prepared using the sonochemical process, followed by heat treatment. A study was made of the action of ultrasonic waves and the influence of thermal treatment conditions on two initial molar compositions of 1:1 and 1:2 of calcia:alumina. The aqueous suspension containing the raw materials (A-50 alumina and CaO) was subjected to an ultrasonic bath, followed by drying and burning at 1000, 1200 and 1300 ºC. These cements were characterized by SEM, XRD and the mechanical strength was evaluated by splitting tensile tests, using commercial cement as a reference. Furthermore, the phases were semi-quantified using the Rietveld method. The results show that hydration and sonochemical action increased the reactivity of the raw materials during firing and that phase formation is dependent on the thermal treatment conditions. The CAC cements were obtained at temperatures at least 200 ºC lower than those used in conventional methods, indicating the potential of this route of synthesis.

Caracterização dos resíduos cauliníticos das indústrias de mineração de caulim da Amazônia como matéria-prima para produção de pozolanas de alta reatividade

As regiões do Rio Capim e do Rio Jari são os principais distritos caulinitícos da Região Amazônica, detentores das maiores reservas brasileiras de caulim de alta qualidade para aplicações como cobertura de papel. O caulim é lavrado e beneficiado por três grandes companhias que são responsáveis pela geração de aproximadamente 500 mil de toneladas anuais de um resíduo decorrente da etapa de centrifugação. Esse resíduo, na forma de polpa, é depositado em lagoas de sedimentação que ocupam grandes extensões de áreas. O objetivo da pesquisa foi investigar as características físicas, químicas e mineralógicas dos resíduos processados da Região do Jari e do Capim, de modo a avaliar se atendem aos requisitos como matéria-prima para a produção de uma pozolana de alta reatividade, o metacaulim, adição mineral que incorporada ao cimento Portland proporciona alto desempenho às misturas de concreto e argamassas. Os resíduos foram caracterizados por difração de raios X, análise térmica, espectroscopia de infravermelho, microscopia eletrônica de varredura, fluorescência de raios X e difração a laser. Ambos os resíduos são constituídos por no mínimo 92% de caulinita de baixa granulometria, cujas áreas superficiais específicas são superiores a 8 m²/g e os diâmetros médios de partículas inferiores a 1 µm. Os teores de sílica livre (quartzo) não foram superiores a 3%. O alto grau de concentração de caulinita destes resíduos dispensa os rígidos parâmetros de controle de remoção de impurezas, normalmente empregados na produção deste tipo de pozolana. O caulim do Rio Jari, com quantidade de defeitos na estrutura cristalina superior ao da caulinita do Rio Capim, proporcinou maior grau de desidroxilação a uma temperatura mais baixa quando calcinado, indicando a possibilidade de redução de gastos com energia para a produção da adição mineral. Os resultados das análises foram convergentes e apontam ambos os caulins estudados como excelentes matérias-primas para a produção do metacaulim de alta reatividade.

Propriedades mecânicas e durabilidade do concreto branco com adições pozolânicas

O presente trabalho tem a finalidade de verificar o comportamento do concreto de cimento Portland Branco com adição de metacaulim e sílica ativa, avaliando o comportamento mecânico, a absorção de água e o nível de porosidade e durabilidade em concretos com este aglomerante. Para isso, foram realizados ensaios no estado plástico (consistência e massa específica) e endurecido (resistência à compressão axial, resistência à tração por compressão diametral, módulo de elasticidade, absorção de água, penetração de cloretos e carbonatação). Foram realizadas avaliações de sua resistência à compressão axial e à tração por compressão dimetral nas idades de 7 e 28 dias através do método IPT/EPUSP que utiliza os traços 1:5, 1:3,5 e 1:6,5. O módulo de elasticidade aos 28 dias. Além destes foi avaliada a permeabilidade por meio de ensaio de absorção; durabilidade através do ensaio acelerado de cloretos e da carbonatação; a porosidade foi verificada com a realização da microscopia eletrônica de varredura. De maneira geral, verificou-se que mesmo a resistência dos concretos de menor proporção agregado/aglomerante (traço pobre), está acima das resistências mais usuais na região metropolitana de Belém que é em torno de 25 a 30 MPa, visto que o cimento branco utilizado é o estrutural, por isso, justifica-se o alcance destes valores mesmo com traço pobre. Com relação à permeabilidade, os resultados demonstraram que assim como a resistência, esta é dependente do tipo de cimento empregado e das adições utilizadas. Os valores mais elevados de permeabilidade foram obtidos nos concretos referência (sem adição). Para estudar a porosidade viu-se que concreto referência apresenta-se menos compacto e com mais poros perceptíveis, principalmente os com maiores proporções agregado/aglomerante. Já nas micrografias dos concretos CMT e CSA, é possível observar uma menor quantidade de poros na região ocupada pela pasta Por fim, foi feita uma comparação das propriedades mecânicas, capacidade de absorção de água e porosidade do Cimento Portland Branco (CPB).

Reaproveitamento de cinzas de carvão mineral na formulação de argamassas

Este trabalho tem como objetivo o estudo da incorporação de cinzas provenientes da combustão do carvão mineral em caldeiras de leito fluidizado, na produção de argamassas, em substituição parcial do cimento. Foram elaborados corpos de prova utilizando-se os cimentos Portland com as especificações CPII-E-32 de características normais e areia de classificação abaixo da malha 100. Foram preparadas misturas na proporção 4 partes de agregado e 1 parte de cimento, com a inserção de cinzas nas proporções 0, 10, 20, 30, 40 e 50%. A argamassa foi desenvolvida em misturador e a moldagem foi feita em moldes de 5 cm x 10 cm. Foi analisado o comportamento de resistência à compressão após 28 dias. A resistência diminui conforme o aumento da porcentagem de cinzas. Foram feitas análises complementares de difração de raios X e constatou-se que a substituição desse resíduo pode ser feita com sucesso em argamassas com teores de até 30%.

Comparison of Physicochemical Surface Conditioning Methods for Adhesion of bis-GMA Resin Cement to Particulate Filler Composite and Surface Characterization

This study compared the effect of physicochemical surface conditioning methods on the adhesion of bis-GMA-based resin cement to particulate filler composite (PFC) used for indirect dental restorations. PFC blocks (N (block)=54, n (block)=9 per group) were polymerized and randomly subjected to one of the following surface conditioning methods: a) No conditioning (Control-C), b) Hydrofluoric acid (HF)etching for 60s (AE60), c) HF for 90s (AE90), d) HF for 120s (AE120), e) HF for 180s (AE180), and f) air-abrasion with 30 mu m silica-coated alumina particles (AB). The conditioned surfaces were silanized with an MPS silane, and an adhesive resin was applied. Resin composite blocks were bonded to PFC using resin cement and photo-polymerized. PFC-cement-resin composite blocks were cut under coolant water to obtain bar specimens (1mmx0.8mm). Microtensile bond strength test (mu TBS)was performed in a universal testing machine (1mm/min). After debonding, failure modes were classified using stereomicroscopy. Surface characterization was performed on a set of separate specimen surfaces using Scanning Electron Microscopy (SEM), X-Ray Dispersive Spectroscopy (XDS), X-Ray Photoelectron Spectroscopy (XPS), and Fourier Transform-Raman Spectroscopy (FT-RS). Mean mu TBS (MPa) of C (35.6 +/- 4.9) was significantly lower than those of other groups (40.2 +/- 5.6-47.4 +/- 6.1) (p<0.05). The highest mu TBS was obtained in Group AB (47.4 +/- 6.1). Prolonged duration of HF etching increased the results (AE180: 41.9 +/- 7), but was not significantly different than that of AB (p>0.05). Failure types were predominantly cohesive in PFC (34 out of 54) followed by cohesive failure in the cement (16 out of 54). Degree of conversion (DC) of the PFC was 63 +/- 10%. SEM analysis showed increased irregularities on PFC surfaces with the increased etching time. Chemical surface analyses with XPS and FT-RS indicated 11-70% silane on the PFC surfaces that contributed to improved bond strength compared to Group C that presented 5% silane, which seemed to be a threshold. Group AB displayed 83% SiO2 and 17% silane on the surfaces.

Stress distribution on dentin-cement-post interface varying root canal and glass fiber post diameters. A three-dimensional finite element analysis based on micro-C data

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

Interface of dentine to root canal sealers

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

Investigation of the Effect of Sealer Use on the Heat Generated at the External Root Surface during Root Canal Obturation Using Warm Vertical Compaction Technique with System B Heat Source

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

Bond Strength of Different Resin Cement and Ceramic Shades Bonded to Dentin

Purpose: To evaluate the microtensile bond strength (MTBS) of ceramic cemented to dentin varying the resin cement and ceramic shades.Materials and Methods: Two VITA VM7 ceramic shades (Base Dentine 0M1 and Base Dentine 5M3) were used. A spectrophotometer was used to determine the percentage translucency of ceramic (thickness: 2.5 mm). For the MTBS test, 80 molar dentin surfaces were etched and an adhesive was applied. Forty blocks (7.2 x 7.2 x 2.5 mm) of each ceramic shade were produced and the ceramic surface was etched (10% hydrofluoric acid) for 60 s, followed by the application of silane and resin cement (A3 yellow and transparent). The blocks were cemented to dentin using either A3 or transparent cement. Specimens were photoactivated for 20 s or 40 s, stored in distilled water (37 degrees C/24 h), and sectioned. Eight experimental groups were obtained (n = 10). Specimens were tested for MTSB using a universal testing machine. Data were statistically analyzed using ANOVA and Tukey's post-hoc tests (alpha <= 0.05).Results: The percentage translucency of 0M1 and 5M3 ceramics were 10.06 (+/- 0.25)% and 1.34 (+/- 0.02)%, respectively. The lowest MTBS was observed for the ceramic shade 5M3. For the 0M1 ceramic, the A3 yellow cement that was photocured for 20 s exhibited the lowest MTBS, while the transparent cement that was photocured for 40 s presented the highest MTBS.Conclusions: For the 2.5-mm-thick 5M3 ceramic restorations, the MTBS of ceramic cemented to dentin significantly increased. The dual-curing cement Variolink II photocured for 40 s is not recommended for cementing the Base Dentine 5M3 feldspathic ceramic to dentin.

Can Heat Treatment Procedures of Pre-hydrolyzed Silane Replace Hydrofluoric Acid in the Adhesion of Resin Cement to Feldspathic Ceramic?

Purpose: To evaluate the influence of heat treatment (HT) procedures of a pre-hydrolyzed silane on bond strength of resin cement to a feldspathic ceramic.Materials and Methods: Ceramic and composite blocks (N = 30) were divided into six groups (n = 5) and subjected to the following conditioning procedures: G1: 9.6% hydrofluoric acid (HF) for 20 s + silane (RelyX Ceramic Primer, 3M ESPE) + resin cement (Panavia F2.0, Kuraray) (control); G2: HF (20 s) + silane + heat treatment in furnace (HTF) (100 degrees C, 2 min) + resin cement; G3: silane + HTF + resin cement; G4-HF (20 s) + silane + heat treatment with hot air (HTA) (50 +/- 5 degrees C for 1 min) + resin cement; G5: silane + HTA + resin cement; G6: silane + resin cement. The microtensile bond strength (MTBS) test was performed using a universal testing machine (1 mm/min). After debonding, the substrate and adherent surfaces were analyzed using a stereomicroscope and SEM to categorize the failure types. The data were statistically evaluated using one-way ANOVA and Tukey's test (5%).Results: The control group (G1) showed no pre-test failures and presented significantly higher mean MTBS (16.01 +/- 1.12 MPa) than did other groups (2.63 +/- 1.05 to 12.55 +/- 1.52 MPa) (p = 0.0001). In the groups where HF was not used, HTF (G3: 12.55 +/- 1.52 MPa) showed significantly higher MTBS than did HTA (G5: 2.63 +/- 1.05 MPa) (p < 0.05). All failure types were mixed, ie, adhesive between the resin cement and ceramic accompanied by cohesive failure in the cement.Conclusion: Heat treatment procedures for the pre-hydrolyzed silane either in a furnace or with the application of hot air cannot replace the use of HF gel for the adhesion of resin cement to feldspathic ceramic. Yet when mean bond strengths and incidence of pre-test failures are considered, furnace heat treatment delivered the second best results after the control group, being considerably better than hot air application.

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 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.

Influence of air-particle deposition protocols on the surface topography and adhesion of resin cement to zirconia

Objectives: This study evaluated the influence of air-particle abrasion protocols on the surface roughness (SR) of zirconia and the shear bond strength (SBS) of dual-polymerized resin cement to this ceramic. Materials and methods. Sintered zirconia blocks (n = 115) (Lava, 3M ESPE) were embedded in acrylic resin and polished. The specimens were divided according to the 'particle type' (Al: 110 mu m Al2O3; Si: 110 mu m SiO2) and 'pressure' factors (2.5 or 3.5 bar) (n = 3 per group): (a) Control (no air-abrasion); (b) Al2.5; (c) Si2.5; (d) Al3.5; (e) Si3.5. SR (Ra) was measured 3-times from each specimen after 20 s of air-abrasion (distance: 10 mm) using a digital optical profilometer. Surface topography was evaluated under SEM analyses. For the SBS test, 'particle type', 'pressure' and 'thermocycling' (TC) factors were considered (n = 10; n = 10 per group): Control (no air-abrasion); Al2.5; Si2.5; Al3.5; Si3.5; Control(TC); Al2.5(TC); Si2.5(TC); Al3.5(TC); Si3.5(TC). After silane application, resin cement (Panavia F2.0) was bonded and polymerized. Specimens were thermocycled (6.000 cycles, 5-55 degrees C) and subjected to SBS (1 mm/min). Data were analyzed using ANOVA, Tukey's and Dunnett tests (5%). Results. 'Particle' (p = 0.0001) and 'pressure' (p = 0.0001) factors significantly affected the SR. All protocols significantly increased the SR (Al2.5: 0.45 +/- 0.02; Si2.5: 0.39 +/- 0.01; Al3.5: 0.80 +/- 0.01; Si3.5: 0.64 +/- 0.01 mu m) compared to the control group (0.16 +/- 0.01 mu m). For SBS, only 'particle' factor significantly affected the results (p = 0.015). The SiO2 groups presented significantly higher SBS results than Al2O3 (Al2.5: 4.78 +/- 1.86; Si2.5: 7.17 +/- 2.62; Al3.5: 4.97 +/- 3.74; Si3.5: 9.14 +/- 4.09 MPa) and the control group (3.67 +/- 3.0 MPa). All TC specimens presented spontaneous debondings. SEM analysis showed that Al2O3 created damage in zirconia in the form of grooves, different from those observed with SiO2 groups. Conclusions. Air-abrasion with 110 mu m Al2O3 resulted in higher roughness, but air-abrasion protocols with SiO2 promoted better adhesion.

Bonding of Y-TZP to Dentin: Effects of Y-TZP Surface Conditioning, Resin Cement Type, and Aging

Purpose: To evaluate the effects of two surface treatments, aging, and two resin cements on shear bond strength between dentin and yttrium-stabilized tetragonal zirconia polycrystal ceramic (Y-TZP).Materials and Methods: Eighty human molars were embedded in acrylic resin and sectioned 3 mm below the occlusal plane. These teeth and 80 cylindrical Y-TZP specimens (height, 4 mm; diameter, 3.4 mm) were divided into eight groups (n=10) using the following factors: Y-TZP surface treatment (Vi: low-fusing porcelain [vitrification] + hydrofluoric acid etching + silanization or Si: tribochemical silicatization); cementation strategies (PF: Pan avia or CC: Clearfil); and storage (nonaging or aging). Bonding surfaces of 40 Y-TZP specimens received Vi treatment, and the rest received Si treatment. Half of the ceramic-tooth assemblies were cemented with Panavia, the rest with Clearfil. Shear tests were executed using 0.4-mm-thick wire at 0.5 mm/min. Data were analyzed by three-way analysis of variance and Tukey test (alpha=0.05). Fractures were analyzed.Results: Y-TZP surface treatments did not affect bond strength (p=0.762, Vi = Si), while resin cements (p<0.001, Panavia > Clearfil) and aging (p=0.006, nonaging > aging) showed a significant effect. Most failures were in adhesive at dentin-cement interfaces; no failure occurred between zirconia and cement.Conclusion: When Y-TZP ceramic is bonded to dentin, the weakest interface is that between dentin and resin cement. The resin cement/Y-TZP interface was less susceptible to failures, owing to Y-TZP surface treatments.