Effect of ceramic surface treatment on the shear bond strength of a resin cement to different ceramic systems

This study evaluated three surface treatments and their effects on the shear bond strength between a resin cement and one of three ceramics. The ceramic surfaces were evaluated with scanning electron microscopy (SEM ) as well. Specimens were treated with 50 μm aluminum oxide airborne particles, 10% hydrofluoric acid etching, or a combination of the two. Using a matrix with a center hole (5.0 mm × 3.0 mm), the ceramic bonding areas were filled with resin cement following treatment. The specimens were submitted to thermal cycling (1,000 cycles) and the shear bond strength was tested (0.5 mm/minute). The failure mode and the effect of surface treatment were analyzed under SEM . Data were submitted to ANOVA and a Tukey test (α = 0.05). Duceram Plus and IPS Empress 2 composite specimens produced similar shear bond strength results (p > 0.05), regardless of the treatment method used. Hydrofluoric acid decreased the shear bond strength of In-Ceram Alumina specimens. For all materials, surface treatments changed the morphological surface. All treatments influenced the shear bond strength and failure mode of the ceramic/resin cement composites.

In vitro and in vivo investigation of the biological and mechanical behaviour of resin-modified glass-ionomer cement containing chlorhexidine

Objectives: To evaluate: (1) the in vitro antibacterial, cytotoxic and mechanical properties of a resin-modified glass ionomer cement (RMGIC) containing different concentrations of chlorhexidine (CHX) and (2) the in vivo microbiologic action of the best concentration of CHX associated with the RMGIC applied on remaining dentine after indirect pulp treatment (IPT). Methods: For the in vitro studies, RMGIC was associated with 0.2, 0.5, 1.25 and 2.5% CHX. Microbiologic evaluation consisted of an agar diffusion test on cariogenic bacteria for 24 h. Odontoblast-like cell metabolism and morphology analyses measured the cytotoxic effects of the RMGIC groups after 24 h. The same groups were submitted to compressive and diametral tensile strength. The in vivo treatment consisted of IPT using an RMGIC associated with the best CHX concentration. Clinical and microbiologic evaluations were performed before and after 3 months. Results: The use of 1.25% CHX significantly improved the antibacterial effects of the evaluated RMGIC, without causing any detrimental effects to the odontoblast-like cells and on the mechanical properties. This RMGIC and CHX combination completely eliminated mutans streptococci after 3 months of IPT. Conclusion: The RMGIC and 1.25% CHX mixture showed great biological and mechanical behaviour and could be a good treatment against caries progression. Clinical significance: The association of CHX with a liner RMGIC opens a new perspective for arresting residual caries after IPT. © 2012 Elsevier Ltd. All rights reserved.

Dielectric behavior of epoxy/BaTiO3 composites using nanostructured ceramic fibers obtained by electrospinning

Composite materials made of epoxy resin and barium titanate (BT) electrospun nanostructured fibers were prepared. BT fibers were synthesized from a sol based on barium acetate, titanium isopropoxide, and poly(vinyl pyrrolidone). The fibers were heat-treated at different temperatures and characterized by X-ray diffraction, scanning electron microscopy (SEM), and Raman spectroscopy. Mats of BT fibers heat-treated at 800 C were embedded in epoxy resin into suitable molds. The composites were characterized by SEM, and dielectric measurements were performed by means of dielectric spectroscopy. The dielectric permittivity and dielectric modulus of epoxy resin/BT-fiber composites were measured for two types of samples: with the electrodes parallel and perpendicular to the BT fiber layers. Interestingly, composite samples with electrodes perpendicular to the fiber layers and a BT content as low as 2 vol % led to dielectric permittivities three times higher than that of pure epoxy resin. © 2013 American Chemical Society.

Effect of ceramic shade on the degree of conversion of a dual-cure resin cement analyzed by FTIR

Objectives: The aim of this research was to evaluate the degree of monomer conversion of different resin cement shades when photocured under different feldspathic ceramic shades. The photocuring time was also evaluated as well as the translucency of each ceramic shade. Methods: Three VITA VM7 ceramic shades (Base Dentin 0M1, Base Dentin 2M2 and Base Dentin 5M3) were used to determine the translucency percentage. A spectrophotometer MiniScan was used to measure the opacity percentage of each specimen (2-mm-thick) and then the translucency was calculated. To measure the degree of conversion (DC), the resin cement (Variolink II; A3 Yellow and transparent) specimens (thickness: 100 μm) were photocured under a ceramic block (2-mm-thick) for 20 or 40 s. Specimens photocured without the ceramic block were used as control. Sixteen groups (n = 3) were evaluated. Micro-ATR/FTIR spectrometry was used to evaluate the extent of polymerization of all specimens after 24 h. The %DC was calculated of experimentally polymerized versus maximally polymerized composite. Results: The translucency percentages of 0M1, 2M2 and 5M3 ceramics were 12.41 (1.02)%, 5.75 (1.91)% and 1.07 (0.03)%, respectively. The %DC of both resin cement shades cured under ceramic 5M3 was significantly lower than the other groups (p < 0.05). The %DC of 0M1 groups exhibited no significant difference from 2M2 groups (p > 0.05), with the exception of the transparent cement photocured for 40 s. Conclusion: Photocuring under 2 mm ceramic showed that the increase in chroma saturation significantly decreased Variolink II resin cement %DC (100-μm-thick). © 2013 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Compressive strength of dental composites photo-activated with different light tips

The aim of this study was to evaluate the compressive strength of microhybrid (Filtek™ Z250) and nanofilled (Filtek™ Supreme XT) composite resins photo-activated with two different light guide tips, fiber optic and polymer, coupled with one LED. The power density was 653 mW cm -2 when using the fiber optic light tip and 596 mW cm-2 with the polymer. After storage in distilled water at 37 ± 2 °C for seven days, the samples were subjected to mechanical testing of compressive strength in an EMIC universal mechanical testing machine with a load cell of 5 kN and speed of 0.5 mm min-1. The statistical analysis was performed using ANOVA with a confidence interval of 95% and Tamhane's test. The results showed that the mean values of compressive strength were not influenced by the different light tips (p > 0.05). However, a statistical difference was observed (p < 0.001) between the microhybrid composite resin photo-activated with the fiber optic light tip and the nanofilled composite resin. Based on these results, it can be concluded that microhybrid composite resin photo-activated with the fiber optic light tip showed better results than nanofilled, regardless of the tip used, and the type of the light tip did not influence the compressive strength of either composite. Thus, the presented results suggest that both the fiber optic and polymer light guide tips provide adequate compressive strength to be used to make restorations. However, the fiber optic light tip associated with microhybrid composite resin may be an interesting option for restorations mainly in posterior teeth. © 2013 Astro Ltd.

A brief discussion about image quality and SEM methods for quantitative fractography of polymer composites

The methodology for fracture analysis of polymeric composites with scanning electron microscopes (SEM) is still under discussion. Many authors prefer to use sputter coating with a conductive material instead of applying low-voltage (LV) or variable-pressure (VP) methods, which preserves the original surfaces. The present work examines the effects of sputter coating with 25 nm of gold on the topography of carbon-epoxy composites fracture surfaces, using an atomic force microscope. Also, the influence of SEM imaging parameters on fractal measurements is evaluated for the VP-SEM and LV-SEM methods. It was observed that topographic measurements were not significantly affected by the gold coating at tested scale. Moreover, changes on SEM setup leads to nonlinear outcome on texture parameters, such as fractal dimension and entropy values. For VP-SEM or LV-SEM, fractal dimension and entropy values did not present any evident relation with image quality parameters, but the resolution must be optimized with imaging setup, accompanied by charge neutralization. © Wiley Periodicals, Inc.

Effect of fiber surface on flexural strength in carbon fabric reinforced epoxy composites

The effect of carbon fiber surface characteristics on flexural properties of structural composites is studied in this work. Two types of intermediate modulus carbon fibers were used: T800HB and IM7. Results revealed that higher mechanical properties are linked with higher interfacial adhesion. Morphologies and chemical compositions of commercial carbon fibers (CF) were characterized by Fourier Transformed Infra Red (FTIR) and Scanning Electronic Microscopy (SEM). Comparing the results, the T800HB apparently has more roughness, since the IM7 seems to be recovered for a polymeric film. On other hand, the IM7 one shows higher interactivity with epoxy resin system Cycom 890 RTM. Composites produced with Resin Transfer Molding (RTM) were tested on a flexural trial. Interfacial adhesion difference was showed with SEM and Dynamic Mechanical Analyses (DMA), justifying the higher flexural behavior of composites made with IM7 fibers. © 2013 Elsevier B.V. All rights reserved.

Microtensile bond strength of resin cements to caries-affected dentin

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

Evaluation of the chemical interaction between carbon nanotubes functionalized with TGDDM tetrafunctional resin and hardener DDS

In this work, the chemical interaction between carbon nanotubes (MWCNT) functionalized with acyl chloride (SOCl2) and polymer chain tetrafuncional N,N,N′,N′-tetraglycidyl-4,4′- diaminodiphenylmethane (TGDDM) and hardener 4,4′diaminodiphenyl sulfone (DDS) has been monitored by Fourier transform infrared spectroscopy (FTIR) with a attenuated total reflectance (ATR) coupled. MWCNT were obtained from the pyrolysis of a mixture of camphor and ferrocene into a oven. The functionalization process was done by oxidative treatment in order to incorporate carboxylic group over the walls of MWCNT, before to be used SOCl2. The functionalized carbon nanotubes were evaluated by X-ray photoelectron spectroscopy (XPS), Raman and transmission electron microscopy (TEM). Nanostructured composites were processed by using epoxy resin with MWCNT in varying percentages. In this work it was observed that different percentages of functionalized nanotubes modify the interaction between the composite matrix and curing agent, where can be observed that in specimens with content less than 1 wt% MWCNT the chemical bond occurs preferentially from the opening of the SO double bond of the hardener and when is used MWCNT content higher than 1 wt% there is little chemical interaction with the SO bond of the hardener and most MWCNT binds to amine. © 2013 Elsevier Ltd.

Environmental ageing studies of chemically modified micro and nanofibril phenol formaldehyde composites

Cellulose micro and nano fibrils were extracted from banana macro fibres and chemically modified using sodium hydroxide, formic acid, 3-methacryloxy propyltrimethoxy silane. These untreated and chemically treated fibrils were incorporated into PF resin and the specimens were prepared. The composites were subjected to long-term water ageing, thermal ageing soil burial and outdoor weathering. The mechanical properties are reduced under all ageing conditions. The present study investigates the effects of different types of ageing on macro fibre, microfibril and nanofibril reinforced PF composites. The effect of chemical modifications of fibres on the degradability of the composites at different environments also has been analysed. © 2013 Elsevier B.V.

Effect of carbamide peroxide bleaching gel on composite resin flexural strength and microhardness

This study investigated the effect of 16% carbamide peroxide (Whiteness Perfect/FGM) on the Vickers microhardness and flexural strength of the restorative composites Filtek Z100 (hybrid), Filtek Z350 (nanofill), Brilliant (micro-hybrid) and Opallis (micro-hybrid). Discshaped (4×2 mm; n=5) and bar-shaped (12×2×1 mm; n=10) specimens of each restorative material were randomly divided into 2 groups: (G1) 16 weeks stored in distilled water; (G2) 16 weeks stored in distilled water, with 16% carbamide peroxide application during 6 h per day for the last 4 weeks. The mechanical properties were evaluated using a Vickers microhardness tester and a mechanical testing machine. Data were analyzed by twoway ANOVA and Tukey's (HSD) post-hoc test (α=0.05). Filtek Z100 presented the highest microhardness value, followed by Filtek Z350 and finally by Brilliant and Opallis (p=0.00). Filtek Z100 and Brilliant exhibited the highest flexural strength value, followed by Filtek Z350 and Opallis (p=0.00). Bleaching treatment decreased significantly microhardness of Brilliant and Opallis (p=0.00). The flexural strength of all studied materials was not affected by the home bleaching (p=0.28).

Avaliação da rugosidade superficial e resistência à flexão de três tipos de resina composta indireta após variação de tratamento da superfície

Neste estudo avaliou-se a rugosidade superficial em corpos-de-prova confeccionados com três tipos de resinas indicadas para confecção de restaurações indiretas, SR Adoro (Ivoclar-Vivadent) (GA), Signum Matrix (Heraeus-Kulzer) (GSM) e Signum⁺ (Heraeus-Kulzer) (GSP), assim como a resistência à flexão após serem utilizados diferentes tratamentos de superfície com o propósito de se verificar a influência dos mesmos na resistência mecânica dos materiais. Obteve-se 120 corpos-de-prova de cada tipo de resina de acordo com as recomendações dos fabricantes, os quais foram divididos e tratados com: A- Jateamento com óxido de alumínio a 50μm por 6 s a 60-80 libras (Grupo Controle); B- Jateamento e silanização com Monobond (Ivoclar Vivadent) e Excite DSC (Ivoclar Vivadent); C- Jateamento e condicionamento com ácido ortofosfórico a 37% por 3 minutos e D- Jateamento, condicionamento e silanização. Após a execução do tratamento superficial, analisou-se os corpos-de-prova em rugosímetro Mytutoyo no parâmetro Ra e teste de flexão por compressão em três pontos em máquina de ensaio universal Kratos. Submeteu-se os dados observados à análise estatística, tendo como nível de significância 5% para a construção dos resultados. Os resultados mostraram um comportamento bastante coerente com o que é visto na literatura com relação à composição das resinas estudadas, os quais apresentaram inicialmente lisura de superfície similar (p>0.05). Com a aplicação dos tratamentos de superfície, houve um comportamento bastante diversificado entre os materiais. Os grupos que receberam a aplicação de silano e adesivo apresentaram superfícies mais lisas e maiores valores de resistência flexural em todas as resinas. No entanto não houve correlação dos valores de rugosidade com a resistência flexural, a qual demonstrou ser maior nas resinas SR Adoro e Signum Matrix, sendo que nesta última, apenas após a silanização é que se observou melhoria deste aspecto flexural.

Experimental RTM manufacturing analysis of carbon/epoxy composites for aerospace application

The success of manufacturing composite parts by liquid composite molding processes with RTM depends on tool designs, efficient heat system, a controlled injection pressure, a stabilized vacuum system, besides of a suitable study of the preform lay-up and the resin system choice. This paper reports how to assemble a RTM system in a laboratory scale by specifying heat, injection and vacuum system. The design and mold material were outlined by pointing out its advantages and disadvantages. Four different carbon fiber fabrics were used for testing the RTM system. The injection pressure was analyzed regarding fiber volume content, preform compression and permeability, showing how these factors can affect the process parameters. The glass transition temperature (Tg) around 203 ºC matched with the aimed temperature of the mold which ensured good distribution of the heat throughout the upper and lower mold length. The void volume fraction in a range of 2% confirmed the appropriate RTM system and parameters choice.

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.

Resin composite characterizations following a simplified protocol of accelerated aging as a function of the expiration date

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)