The ceramic artifacts in archaeological black earth (terra preta) from lower Amazon region, Brazil: Mineralogy

Sítios arqueológicos com Terra Preta, denominados de Terra Preta de Índio ou ainda Terra Preta Arqueológica (TPA) são muito freqüentes na Amazônia. As TPA geralmente contém fragmentos de vasos cerâmicos, por vezes abundantes, além de líticos, que são materiais de grande importância para os estudos arqueológicos. Para consubstanciar esses estudos, realizou-se pesquisas mineralógicas e químicas em fragmentos cerâmicos provenientes de dois sítios arqueológicos da região de Cachoeira-Porteira, Estado do Pará. Os fragmentos foram classificados segundo seus principais temperos em: cauixi, cariapé, areia+feldspatos e caco de vaso cerâmico. Mineralogicamente são compostos de quartzo, minerais de argila calcinados (especialmente caulinita), feldspatos (albita e microclínio), hematita, goethita, maghemita, variscita-estrengita, fosfatos amorfos, anatásio, e raramente apatita, rhabdophana e óxidos de Mn e Ba. Cauixi e cariapé são componentes orgânicos silicosos e amorfos a DRX. A composição mineralógica e a morfologia dos seus grãos indicam saprólito (material argiloso rico em quartzo) derivado de rochas ígneas félsicas de granulação fina ou rochas sedimentares ricas em argilominerais como matéria-prima dos vasos cerâmicos. Neste material argiloso cauixi, cariapé e/ou areias, ricas em sílica, foram intencionalmente adicionados. O elevado conteúdo de fosfatos de Al-Fe, amorfos ou como de baixa cristalinidade, originou-se a partir do contato entre a matriz argilosa da parede do vaso cerâmico com a solução aquosa quente durante o cozimento diário de alimentos de origem animal (principal fonte de fósforo). A cristalização dos fosfatos deve ter prosseguida mesmo depois que os vasos foram descartados, e juntos com os restos de matéria orgânica vegetal e animal incorporaram-se aos solos residuais. Participaram desta forma na formação dos solos tipo TPA.

Chemical and mineralogical characterization of portuguese ceramic tiles in the historic center of São Luís do Maranhão (Brazil): an approximation of the mineralogy and firing temperature of the raw materials

Nesse trabalho, foram caracterizados, pela primeira vez, azulejos históricos portugueses do Centro Histórico de São Luís (CHSL) do Maranhão. A caracterização foi realizada através dos ensaios de microscopia ótica, difração de raios X (DRX) e análise química, visando ao uso dessa informação para a determinação das possíveis matérias-primas utilizadas na sua fabricação, bem como a provável temperatura de queima desses materiais. Os resultados mostraram que a microestrutura desses materiais é constituída por poros de tamanhos variados, apresentando incrustações de calcita e grãos de quartzo de tamanhos inferiores a 500 µm, distribuídos numa matriz de cor rosa-amarelo, onde foram identificadas, por DRX, as fases minerais calcita, gelhenita, wollastonita, quartzo e amorfo. A partir da informação obtida, é possível inferir que as matérias-primas originais estiveram constituídas, provavelmente, por mistura de argilas caoliníticas (Al₂O₃•2SiO,₂•2H₂O), ricas em carbonatos de cálcio e quartzo ou misturas de argilas caoliniticas, quartzo e calcita. Essas matérias-primas originais não atingiram a temperatura de cocção de 950ºC.

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.

Síntese e caracterização elétrica de filmes varistores à base de 'SN''O IND.2' modificados superficialmente por difusão 'CR POT.3+' na região do contorno de grão

Pós-graduação em Química - IQ

Phase transitions and interface phenomena in the cryogenic temperature domain of a niobate nanostructured ceramic

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

Valorization of sugarcane bagasse ash: Producing glass-ceramic materials

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

Measurement of Radiant Energy using Pyroelectric Polymer/Ceramic Composite

Monitoring non-ionizing radiant energy is increasingly demanded for many applications such as automobile, biomedical and security system. Thermal type infrared (IR) sensors can operate at room temperature and pyroelectric materials have high sensitivity and accuracy for that application. Working as thermal transducer pyroelectric sensor converts the non-quantified thermal flux into the output measurable quantity of electrical charge, voltage or current. In the present study the composite made of poly(vinylidene fluoride) -PVDF and lead zirconate titanate (PZT) partially recovered with polyaniline (PAni) conductor polymer has been used as sensor element. The pyroelectric coefficient p(T) was obtained by measuring the pyroelectric reversible current, i.e., measuring the thermally stimulated depolarization current (TSDC) after removing all irreversible contribution to the current such as injected charge during polarization of the sample. To analyze the sensing property of the pyroelectric material, the sensor is irradiated by a high power light source (halogen lamp of 250 W) that is chopped providing a modulated radiation. A device assembled in the laboratory is used to change the light intensity sensor, an aluminum strip having openings with diameters ranging from 1 to 10 mm incremented by one millimeter. The sensor element is assembled between two electrodes while its frontal surface is painted black ink to maximize the light absorption. The signal from the sensor is measured by a Lock-In amplifier model SR530 -Stanford Research Systems. The behavior of the output voltage for an input power at several frequencies for PZT-PAni/PVDF (30/ 70 vol%) composite follows the inverse power law (1/ f) and the linearity can be observed in the frequency range used.

Influence of abutment-to-fixture design on reliability and failure mode of all-ceramic crown systems

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

Efficacy of Surface Treatments on the Bond Strength of Resin Cements to Two Brands of Zirconia Ceramic

Purpose: To compare the shear bond strength (SBS) of two cements to two Y-TZP ceramics subjected to different surface treatments.Materials and Methods: Zirconia specimens were made from Lava (n = 36) and IPS e.max ZirCAD (n = 36), and their surfaces were treated as follows: no treatment (control), silica coating with 30-mu m silica-modified alumina (Al2O3) particles (CoJet Sand), or coating with liners Lava Ceram for Lava and Intensive ZirLiner for IPS e.max ZirCAD. Composite resin cylinders were bonded to zirconia with Panavia F or RelyX Unicem resin cements. All specimens were thermocycled (6000 cycles at 5 degrees C/55 degrees C) and subjected to SBS testing. Data were analyzed by post-hoc test Tamhane T2 and Scheffe tests (alpha = 0.05). Failure mode was analyzed by stereomicroscope and SEM.Results: With both zirconia brands, CoJet Sand showed significantly higher SBS values than control groups only when used with RelyX Unicem (p = 0.0001). Surface treatment with liners gave higher SBS than control groups with both ceramic brands and cements (p < 0.001). With both zirconia brands, the highest SBS values were obtained with the CoJet and RelyX Unicem combination (> 13.47 MPa). Panavia F cement showed significantly better results when coupled with liner surface treatment rather than with CoJet (p = 0.0001, SBS > 12.23 MPa). In untreated controls, Panavia F showed higher bond strength than RelyX Unicem; the difference was significant (p = 0.016) in IPS e.max ZirCAD. The nontreated specimens and those treated with CoJet Sand exhibited a high percentage of adhesive and mixed A (primarily adhesive) failures, while the specimens treated with liners presented an increase in mixed A and mixed C (primarily cohesive) failures as well as some cohesive failure in the bulk of Lava Ceram for both cements.Conclusion: CoJet Sand and liner application effectively improved the SBS between zirconia and luting cements. This study suggests that different interactions between surface treatments and luting cements yield different SBS: in clinical practice, these interactions should be considered when combining luting cements with surface treatments in order to obtain the maximum bond strength to zirconia restorations.

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.

Characterization of a polymer-infiltrated ceramic-network material

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

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.